|Publication number||US5606015 A|
|Application number||US 08/390,389|
|Publication date||Feb 25, 1997|
|Filing date||Feb 16, 1995|
|Priority date||Feb 16, 1995|
|Also published as||CA2169507A1, CN1137539A, DE69625733D1, DE69625733T2, EP0731128A1, EP0731128B1|
|Publication number||08390389, 390389, US 5606015 A, US 5606015A, US-A-5606015, US5606015 A, US5606015A|
|Inventors||Shang J. Chiou, Miao-Hsun L. Sheng|
|Original Assignee||Rohm And Haas Company|
|Export Citation||BiBTeX, EndNote, RefMan|
|Patent Citations (9), Referenced by (9), Classifications (11), Legal Events (5)|
|External Links: USPTO, USPTO Assignment, Espacenet|
The present invention relates to improved polymer powder stability. In particular, the present invention relates to improved stability of spray-dried emulsion polymers.
Polymers are known to be useful in many physical forms including powders. Several methods are known for preparing powders of polymers. One of the more practical methods for preparing powders of emulsion polymers is by spray-drying a polymer emulsion. However, spray-drying emulsion polymers has some drawbacks. For example, the yield of powder product may be low.
Another drawback to many spray-dried emulsion polymers is the poor storage stability of the spray-dried emulsion polymers. Poor stability may be manifested by clumping of the powder. In certain applications, such as cement modification, it is desirable to have the polymer powder be redispersible in the cement formulation. Poor storage stability may also be indicated by the degradation of performance, as manifested by the lack of redispersibility of the spray-dried emulsion polymer in the cement formulation.
One method for attempting to overcome the problems associated with spray-drying redispersible emulsion polymers was to add polyvinyl alcohol to the emulsion prior to spray-drying as taught in European Patent Application Number 0601518A. When polyvinyl alcohol is added to cement modifier emulsion polymers, there is a tendency for phase separation. Also, the addition of polyvinyl alcohol to the emulsion tends to impart poor rheology characteristics of cement compositions containing this mixture.
The present invention seeks to overcome the problems associated with known methods for providing redispersible polymer powders.
The present invention provides a method comprising
(i) providing an emulsion comprising at least one emulsion polymer and at least one surfactant having an HLB value below 7 wherein said surfactant is a nonionic surfactant selected from the group consisting of alkylphenoxy ethoxylates, acetylenic polyols, alkylene glycol alkylates, sorbitan alkalates, glycerol esters, polyglycerol esters, and combinations thereof; and
(ii) spray-drying the emulsion.
The method of the present invention provides spray-dried polymers having improved storage stability and redispersibility. The method of the present invention also improves the amount of polymer which is recovered during the spray-drying process.
As used herein and in the appended claims, "HLB" refers to hydrophile-lipophile balance. Surfactants which have a low HLB tend to be less water-soluble and more oil-soluble than surfactants which have a higher HLB.
Surfactants suitable for the present invention are nonionic surfactants having HLB below 7, preferably below 6, more preferably below 5. Nonionic surfactants tend to produce less foam than other classes of surfactants. Surfactants useful in the present invention include, for example: alkylphenoxy ethoxylates such as octylphenoxy ethoxylated alcohols; acetylenic polyols such as ethoxylated tetramethyl decynediol; alkylene glycol alkylates such as propylene glycol monolaurate; sorbitan alkalates such as sorbitan monostearate and sorbitan oleate; glycerol esters such as glycerol oleate; polyglycerol esters such as decaglycerol decastearate and decaglycerol decaoleate; and combinations thereof; which have an HLB below 7, preferably below 6, more preferably below 5. Nonionic surfactants such as ethylene oxide/propylene oxide block copolymers, even if the HLB is below 7, do not provide the benefits of the present invention. For example, ethylene oxide/propylene oxide block copolymers tend to result in high levels of caking on the walls of the spray-drying chamber.
The surfactants useful in the present invention may be added prior to the polymerization of the emulsion polymers, during the polymerization of the emulsion polymers, after the polymerization of the emulsion polymers or a combination thereof. Preferably, the surfactants useful in the present invention are used as the emulsifier for the emulsion polymerization and are thus added prior to the polymerization of the emulsion polymers. The surfactants useful in the present invention may also be used in combination with one or more conventional surfactants useful in emulsion polymerization. The surfactants useful in the present invention are preferably used at a level of from 0.1 to 20, more preferably from 0.2 to 18, most preferably from 0.5 to 15 percent by weight based on the total weight emulsion polymer.
The various aspects of emulsion polymerization are well known to those skilled in the art, such as the selection of the type and amount of monomer(s) and initiator, the selection of the type and amount of chain transfer agents, the control of pH, the rate of addition of the various components, the polymerization temperature, the level of solids, the heating profile, and the like. When preparing emulsion polymers intended for use as cement modifiers, it is preferred that the emulsion polymers are core-shell emulsion polymers, preferably core-shell polymers of the type disclosed in European Patent Application No. EP 522791 A1.
The various aspects of spray-drying are also well known to those skilled in the art, such as the selection of flow rates, inlet temperatures, outlet temperature, residence time, the type and amount of additives and type of carrier gas.
Preferably, the emulsion polymers are prepared via an aqueous emulsion process. Preferably, the aqueous emulsion is from 25 to 70 percent by weight polymer solids, more preferably from 30 to 60 percent by weight polymer solids, and most preferably from 35 to 55 percent by weight polymer solids. Preferably, the viscosity of the aqueous emulsion of the present invention is below 5,000 centipoises ("cps"), more preferably from 50 to 2,000 cps to allow for easier handling and pumping the emulsion through the nozzle of the spray drier.
The emulsion polymers prepared by the present invention are useful in the form of an aqueous emulsion and as a spray-dried polymer powder. The use of low HLB surfactants does not present foaming problems when the low HLB surfactant is used as an emulsifier during the emulsion polymerization, the low HLB surfactant improves the yield of product upon spray-drying, and the low HLB surfactant improves the stability of the spray-dried polymer powder.
The following procedure was used to prepare core-shell polymers. The surfactants used in each of the examples are set forth in Table V, below.
To a 5 liter, 4-necked round bottom flask equipped with a mechanical stirrer, thermocouple, condenser, and nitrogen sparge was added 700 grams of deionized water. The water was heated to 80° C. A monomer emulsion (ME#1) was prepared by combining the components set forth in Table I below. An initiator solution was prepared by combining the components set forth in Table II below. While stirring the contents of the kettle, ME#1 was added to the kettle followed by the initiator solution. After several minutes, the temperature of the kettle leveled off, a few grams of a catalyst solution containing t-butylhydroperoxide and sodium sulfoxylate formaldehyde was added to the kettle to reduce the residual monomer level. To the kettle was added the neutralizer slurry (as shown in Table III below) to solubilize the first stage (shell) polymer.
A monomer emulsion (ME#2) was prepared by combining the components set forth in Table IV below. To the kettle was added 114 grams of ME#2 and 10 grams of a 20 percent aqueous solution of ammonium persulfate. After the exotherm peaked, the remainder of ME#2 and 187 grams of a 3.7 percent aqueous solution of ammonium persulfate were separately added to the kettle at a constant rate over a period of two hours at a temperature in the range of 82°-86° C. The contents of the kettle temperature were then maintained at 82° C. for an additional thirty minutes, then cooled to 65° C. Residual monomer levels were reduced by adding a few grams of a catalyst solution containing t-butylhydroperoxide and sodium sulfoxylate formaldehyde to the kettle.
The emulsion polymers were spray-dried in a Bowen Model BLSA spray dryer under the following conditions: Inlet temperature 120° C.; Outlet Temperature 60° C.; Flow Rate 100-150 milliliters per minute; Air Pressure 100 pounds per square inch. In each of the examples, "Particle Size" is reported as diameter in nanometers ("nm") as measured by a Brookhaven BI-90 Particle Sizer. The Scrap Ratio reported in Table VII below is the amount of spray dried emulsion polymer, by weight, recovered relative to the amount of polymer which adhered to the walls of the spray drying chamber. The spray-dried emulsion polymers were evaluated as cement modifiers. Cement mortars were prepared according to the formulation set forth in Table VI below.
The following properties of the modified cements were evaluated, and the results are set forth in Table VII below:
Wet-out time: the time required for the mortar to reach a very workable consistency, reported in seconds ("sec.").
Thin section properties: a 1/16 inch (0.16 centimeter) thickness of mortar is placed on plywood and allow to cure for 24 hours. Toughness is rated qualitatively by scratching the center with a screw driver. Adhesion is rated qualitatively by evaluating how well the cement adhered to the plywood.
"Fresh" polymer refers to spray dried emulsion polymer incorporated into the cement formulations within 2 days of being spray-dried.
"Aged" polymer refers to spray dried emulsion polymer which has been placed in an oven at 60° C. for 5 days prior to being incorporated into the cement formulations.
TABLE I______________________________________Materials ME #1______________________________________Deionized water 290.00Triton XN-45S 1.3Surfactant 35.60Methyl Methacrylate 294.00Allyl Methacrylate 5.60Methacrylic Acid 75.00Methyl 3-mercaptopropionate 13.1______________________________________
TABLE II______________________________________0.1 percent aqueous solution of FeSO4.7 H2 O 10.0 g14.9 percent aqueous solution of t-butyl 25.4 ghydroperoxide7.8 percent aqueous solution of sodium sulfoxylate 43.4 gformaldehyde______________________________________
TABLE III______________________________________deionized water 110.0 g50 percent aqueous solution of sodium 35.0 ghydroxideCa(OH)2 16.1 g______________________________________
TABLE IV______________________________________Materials ME #2______________________________________Deionized water 326.00 gramsSurfactant 11.30 gramssodium lauryl sulfate 10.80 gramsButyl Acrylate 762.00 gramsMethyl Methacrylate 739.00 grams______________________________________
TABLE V______________________________________Example Surfactant HLB______________________________________1 Octylphenyl ethoxylated alcohol (1-2 3.6 EO units)2 tetramethyl decylnediol 4.03 Ethoxylated tetramethyl decynediol 4.04 C12-13 linear primary alcohol 3.7 ethoxylate5 polyglycol monolaurate 3.2Comparative 6 Octylphenoxy ethoxylated alcohol (˜16 15.8 EO units)Comparative 7 C 11-15 secondary alcohol ethoxylate 8.0Comparative 8 C 12-13 linear primary alcohol 7.9 ethoxylateComparative 9 Block copolymers of EO/PO 1-7Comparative 10 Block copolymers of EO/PO 12-18______________________________________
TABLE VI______________________________________Type I Portland cement 15.0 grams60 mesh sand 22.5 gramsSpray dried emulsion 1.0 grams (based on polymerpolymer solids)water 6.0 grams______________________________________
TABLE VII__________________________________________________________________________ Comp. Comp. Comp. Comp. Comp.Example 1 2 3 4 5 6 7 8 9 10__________________________________________________________________________HLB 3.6 4.0 4.0 3.7 3.2 15.8 8.0 7.9 1-7 12-18Particle 172 161 149 161 158 156 164 150 161 161size (nm)Scrap Ratio 25.0 27.3 24.0 13.8 19.3 10.4 10.9 10.0 16.1 8.8Wet-out 20 15 15 15 20 25 15 15 20 15time (sec.)Thin SectionToughnessFresh good very very good very poor fair fair fair poor good good goodAged good/ good good/ fair/ fair very poor poor good very fair fair poor poor fair poorThin SectionAdhesionFresh good very very good good fair good good very fair good good goodAged good good good fair fair- very poor poor good very good poor poor__________________________________________________________________________
The data in Table VII show, for example, that spray-dried polymer powders prepared from emulsions containing emulsion polymers and low HLB nonionic surfactants, namely alkylphenoxy ethoxylates, acetylenic polyols, or alkylene glycol alkylates, exhibit an improved balance of properties with regard to scrap ratio and stability.
|Cited Patent||Filing date||Publication date||Applicant||Title|
|US4171428 *||Jun 6, 1977||Oct 16, 1979||Stauffer Chemical Company||Method for manufacturing plastisol resins using spray-drying|
|US4203879 *||Sep 1, 1978||May 20, 1980||The Firestone Tire & Rubber Company||Plastisol resins having improved clarity|
|US5342897 *||Mar 19, 1993||Aug 30, 1994||Basf Aktiengesellschaft||Aqueous polymer dispersions and polymer powders prepared therefrom by spray drying|
|US5403894 *||Jul 11, 1991||Apr 4, 1995||Rohm And Haas Company||A redispersible core-shell polymer powder|
|DE4317036A1 *||May 21, 1993||Nov 24, 1994||Basf Ag||Polymerisatpulver|
|EP0239084A2 *||Mar 24, 1987||Sep 30, 1987||S.C. JOHNSON & SON, INC.||Non-homogenized multi-surface polish compositions|
|EP0601518A1 *||Dec 6, 1993||Jun 15, 1994||Air Products And Chemicals, Inc.||Redispersible acrylic polymer powder for cementitious compositions|
|GB1525864A *||Title not available|
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|Citing Patent||Filing date||Publication date||Applicant||Title|
|US6900259 *||Aug 22, 2003||May 31, 2005||Celanese Emulsions Gmbh||Redispersible dispersion powder composition, its use, and process for its preparation|
|US9169382||Mar 5, 2013||Oct 27, 2015||Dow Global Technologies Llc||Carboxyl group containing acrylic RDP and dry mix cement formulations containing them|
|US9296653||Dec 15, 2011||Mar 29, 2016||Dow Global Technologies Llc||Dry mix formulations containing carboxylated styrene-butadiene redispersible polymer powders and alumina rich containing cements|
|US9334388 *||Oct 25, 2007||May 10, 2016||Wacker Chemie Ag||Dispersion powder compositions comprising gemini surfactants|
|US20030164478 *||Sep 27, 2001||Sep 4, 2003||Wolfgang Fiedler||Redispersible dispersion powder composition method for the production and use thereof|
|US20040048961 *||Aug 22, 2003||Mar 11, 2004||Heinz-Peter Klein||Redispersible dispersion powder composition, its use, and process for its preparation|
|US20060160937 *||Dec 21, 2005||Jul 20, 2006||Rhodia Chimie||Solid composition containing at least one low-melting surfactant|
|US20080098933 *||Oct 25, 2007||May 1, 2008||Wacker Polymer Systems Gmbh & Co. Kg||Dispersion powder compositions comprising gemini surfactants|
|US20140000540 *||Jun 25, 2013||Jan 2, 2014||Shell Oil Company||Fuel and engine oil composition and its use|
|U.S. Classification||528/495, 528/498, 528/502.00E|
|International Classification||C08F6/14, C08F6/00, C04B24/26, C08J3/12|
|Cooperative Classification||C08J3/122, C04B24/26|
|European Classification||C08J3/12A, C04B24/26|
|Sep 30, 1996||AS||Assignment|
Owner name: ROHM AND HAAS COMPANY, PENNSYLVANIA
Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:CHIOU, SHANG JAW;SHENG, MIAO-HSUN;REEL/FRAME:008164/0793
Effective date: 19950215
|May 18, 2000||FPAY||Fee payment|
Year of fee payment: 4
|Aug 25, 2004||FPAY||Fee payment|
Year of fee payment: 8
|Aug 25, 2008||FPAY||Fee payment|
Year of fee payment: 12
|Sep 1, 2008||REMI||Maintenance fee reminder mailed|


Copper Additive Manufacturing is continuously expanding – what are the latest trends and why this material could enable the emergence of new applications?
by Benjamin Delignon, Head of Innovation at AMEXCI
In the last two years, more and more additive manufacturing technologies claimed to print copper. At first sight, it is now possible to produce small to large components, even with high accuracy. Does copper printing already reached its mature age?
Copper printing – for what applications?
Traditionally, Copper alloys are used in the industry for applications where heat or electrical conductivity plays a major role, such as heat exchangers or coils – often with complex shapes to optimise their function, leading to rather expensive manufacturing methods.
Thermal and Electric conductivities highly depend on the material produced (e.g., alloy composition, density, thermal history), but these functions can also be enhanced through the design of the component: that is where Additive Manufacturing plays a major role. Complex structures and shapes can now be manufactured, and at a relatively low cost compared to the function improvement they provide.
AM technologies producing copper applications
Several AM techniques are currently available to produce pure Copper* components. Laser Powder Bed Fusion (with Green or Blue lasers, or high power infrared lasers) is struggling with the low heat absorptivity of the laser, which complexifies the production parameters definition – but promising results are already available from companies like Trumpf, EOS and more recently Reinshaw. Furthermore, a potential solution might lay in the powder: the Swedish company Graphmatec is currently studying the effect of graphene addition, with highly promising results.
What about Electron Beam Melting? Using no lasers, it is not facing the same challenges as LPBF, but has its own – such as a limited process window and the removal of the sintered powder surrounding the part. However, some products are already on the market, for instance inductor coils, manufactured by Spanish company 3D Inductors. For larger components where productivity is the key word, cold spray companies such as Spee3D are pushing the limits and getting more interest, as shown by their increasing number of machines set up.
On the other side, for small parts, Metal FDM and Metal Binder Jetting are showing great promises for high-accuracy components. Digital Metal just announced the addition of copper to their material portfolio, and Markforged Metal X machines have already been set up all around the globe.
Machine and feedstock are available – but are they industrial solutions?
As part of one of our Multi Owner projects, we investigated the material properties of various AM technologies, with diverse results. In this project, the Metal FDM samples were produced by Marcel Escursell, AM expert at SKF, in their Göteborg facility. He accepted to share his feedback on their machine, and especially on Copper printing:
What type of applications lead to this investment, and why this Metal X machine in particular?
Mostly tooling, we chose MetalX since we already had good experience with MarkForged composite printers. We’re mainly targeting tooling, sometimes we print non-functional prototypes but not so often.
When did you set up the machine and how easy was it to learn how to use it?
We installed the printer in 2019 and it was fairly easy to learn how to use it. However, it’s considerably more complex to handle than a polymer or composite printer since there are 3 steps involved: printing, de-binding and sintering. The machine set up took 2-3 days and training only half a day. Knowing that the software is the same as for Markforged composite printing (Eiger), our previous experience helped.
Are you globally satisfied with the machine?
We succeed to print the components we planned for, but we were surprised by the total leadtime (printing, de-binding, sintering took 1 to 2 weeks in total) and the printer speed, which is significantly slower than those for MarkForged composite printers. The maintenance costs are also higher than for composite printing.
What machine evolution are you expecting?
Like other Metal FDM suppliers, a great step to shorten the leadtimes would be to skip the de-binding (washing) step. When printing solid parts the de-binding takes several weeks, which is too long for our needs. Printing larger parts would also be a great addition, but I guess the sintering step remains a challenge.
For the moment we haven’t confirmed the maximum potential for the MetalX. The main limitations are the cost and time as well as the component size. Knowing we don´t have a CNC machine in our department, as soon as a machining operation is needed, then using the MetalX is not relevant due to the high total leadtimes. For other components, using the Metal X is often a valuable option.
As for any AM challenge, one of the first question should be: what for? Why print in Copper? The component function, size, and accuracy required, will already filter the list of AM materials and technologies compatible with your need. Following these first technical considerations (“is it feasible?”), comes the economic question. Compare to conventional solutions, AM is also often more expensive – especially true for Copper printing which requires expensive feedstocks. Its high cost has to be compensated with high value add(s), such as a great function improvement (exceptional increase in thermal or electric conductivity through material properties and redesign), additional advantages in the supplychain (e.g, low MOQ, shorter leadtimes) and other improvements specific to your application and company – for instance reducing the carbon footprint of your component. As always in AM, a look at the big picture is needed to see the global impact of this Copper printing solution.
Nonetheless, the technologies might not match your requirements (yet), but numerous projects are trying to solve this challenge, to finally have a reliable, accurate and mature solution – industrial, in a sense.
* In this article, we only consider all the materials marketed as “pure copper” – e.g. not the CuCrZr alloy, well established in the AM Space industry.


Mondi Fibre Packaging is the developer and supplier of the new perFORMing line of tray material, which is shipped as rollstock to REWE’s dairy producer Salzburgmilch. There the material is fed into a highly automated packaging line from GEA that thermoforms the trays 8-up, robotically loads the slices of cheese with Weber pickers, evacuates ambient air, backflushes the tray with CO2, and applies a clear lidding material.
The Austrian retail stores BILLA, MERKUR, ADEG, and Sutterlüty — all part of REWE Group — are all offering the organic cheese slices on these new paper trays. In Austria, these can be recycled as waste paper because they’re made of 80 percent virgin fiber and only 20 percent plastic. The new packaging reduces plastic consumption by 70 percent and carbon footprint by around two-thirds compared with the previous solution, according to Mondi.
The natural brown paper of the new cheese packaging is produced by Mondi Frantschach, Carinthia, predominantly from Austrian wood. Rolls of paper then go to Mondi Styria, about 30 miles away. Here the paper is given an extrusion coating of EVOH. Once the coating is applied, the total weight of the paper is 290 gsm.
When the coated paper reaches Salzburgmilch, it’s fed into a GEA PowerPak form/fill/seal system. It includes three Weber robots that load the cheese into the thermoforms. Clear lidding material is heat-sealed over the cheese, but details on what that film is were not available. Once the individual packs have been cut from the web, they’re packed into corrugated secondary packaging.
“One nice feature of this material is that it performs on the same thermoforming machinery that is used for plastics,” says Falk Paulsen, Mondi’s sales director of extrusion coatings. “Yes, there are minor adjustments to make, but it would have been unrealistic to expect food companies like Salzburgmilch to disrupt their entire f/f/s systems just to be able to run our material.”
After a nine-month test phase in cooperation with dairy producer Salzburgmilch, the new packaging is now being used for cheese slices in the varieties Bio Alpkönig, Bio Gouda, Bio Emmentaler, Bio Butterkäse and Bio Bergkäse. The new paper-based packaging solution will soon be appearing in national supermarket chains in France and Poland as well.
Switching from conventional packaging to paper-based solutions delivers multiple benefits. First, paper has the lowest carbon footprint of all packaging types,and second, it is recyclable, with paper recycling rates across Europe already at over 80 percent. The EU and consumers are increasingly demanding solutions that are more readily recyclable and more sustainable. According to a 2018 survey in Austria, around 50 percent of consumers seek to avoid plastic packaging as much as possible. It is clear that brand manufacturers and packaging companies will face huge changes in the future.
Martina Hörmer, managing director at Ja! Natürlich, says, “Consumer expectations concerning sustainability in the food industry have changed dramatically over the last couple of years. Our customers are currently taking a keen interest in packaging. Brands such as Ja! Natürlich are expected to act in an environmentally aware manner. Against this backdrop, this topic has been extremely important to us for several years, and we have been gradually switching to more sustainable packaging alternatives since 2011. We are now delighted to have found a solution, together with Mondi, which significantly reduces the product’s carbon footprint, curbs the use of plastic, and is capable of substantially enhancing recyclability.”
Cost is always difficult to pin down since it can often depend on the diameter of the real of material supplied. But in this case, the upcharge over what was used in the past is 30 to 40 percent. This would certainly suggest that REWE and Salzburgmilch are willing to invest when it comes to meeting their sustainable packaging objectives.


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SBC: SENVOL LLC Topic: DLA18A001
The Department of Defense (DoD) has a demand for out-of-production parts to maintain mission readiness of various weapons platforms. Additive manufacturing (AM) is an exciting and promising manufacturing technique that can make out-of-production parts and holds the potential to solve supply chain issues, such as high costs (i.e. for low-volume parts) and sole sourcing risks. The ability of AM to s ...STTR Phase I 2018 Department of DefenseDefense Logistics Agency
SBC: ARCTOS Technology Solutions, LLC Topic: DLA18A001
Universal Technology Corporation (UTC) has teamed with the University of Dayton Research Institute (UDRI), Stratonics, and Macy Consulting to demonstrate not only the transitionability into commercial systems, but also to develop the data analytics and monitoring and control requirements to extract the full value fromseveral sensors, including the Stratonics ThermaViz, acoustic and profilometry se ...STTR Phase I 2018 Department of DefenseDefense Logistics Agency
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Signature Research, Inc. (SGR) and Michigan Technological University (MTU) propose a Phase I STTR effort to develop a learning algorithm which exploits the spatio-spectral characteristics inherent within IR imagery and motion imagery.Our archive of modelled and labeled data sets will allow our team to thoroughly capture the variable elements that will drive machine learning performance.The overall ...STTR Phase I 2018 Department of DefenseNational Geospatial-Intelligence Agency
SBC: Clear Carbon Innovations Topic: MM
This STTR Phase I project will develop a process to produce silica products from the waste stream of a patent pending activated carbon manufacturing process (carbonxt process). The project focuses on using the silica for Silica-Titania Composites but would also take into account markets that employ precipitated or gel silica which would have differing properties than the silica used in Silica-Tit ...STTR Phase I 2010 National Science Foundation
SBC: CSD Nano Topic: MM
This Small Business Technology Transfer (STTR) Phase I project aims to fabricate anti-reflective coatings (ARC) for solar energy applications. The approach is to use a convective and evaporation-induced assembly to deposit organized nanostructures and create sub-wavelength quasi repeating structures at lower cost than the repeating structures from photolithography. In this project, a Microreacto ...STTR Phase I 2010 National Science Foundation
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This Small Business Technology Transfer (STTR) Phase I project aims to develop a highly-efficient and cost-effective plasma-based method for graphene mass production. The approach is to utilize unique properties of magnetically controlled arc discharge to couple the plasma production of carbon species and the synthesis of graphene. The broader/commercial impact of this project will be the potenti ...STTR Phase I 2010 National Science Foundation
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This Small Business Technology Transfer Phase I project will develop a new system for fabrication and manipulation of carbon nanotube (CNT) composites. The system will use holographic optical trapping (HOT) with a spatial light modulator (SLM) and a new form of nano-controlled photo-polymerization. This tool will allow the creation of a new class of carbon-nanotube polymer composite materials wit ...STTR Phase I 2010 National Science Foundation
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This Small Business Technology Transfer Phase I project will develop a new type of nanostructured substrate for applications in arsenide detection using surface enhanced Raman spectroscopy (SERS). Arsenic is a well known toxic chemical which exists in both nature and industrial processes, and its detection and monitoring at very low concentration is highly desired. SERS, which relies on Raman sig ...STTR Phase I 2010 National Science Foundation
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You're a Diamond! This uniquely designed tumbler is in a glass of its own < see what we did there? :) and it's a perfect house gift for friends and family.
Both glasses stand at an angle which allows you to rotate them in a way in which you enjoy a full bodied flavour of your favourite whiskey. The Diamond Glasses are made from Borosilicate glass, a high quality material with high tolerance to heat. Despite the glasses being thin and lightweight they are extremely durable and also resistant to chemical corrosion.


- A large area of the ladder terrace, equipped with a trough and coconut trees
- Senior environmental PVC material to ensure the hardness of the product
- Portable and easy to carry design cover, bottom non-slip design
- 360-degree ventilation opening to ensure adequate oxygen
- Larger feeding port for easy feeding, easy to watch, easy to clean.
Product descriptionSize: Large
Every detail of this product is so perfect, each of which is carefully designed.
Environmentally friendly sturdy material, portable design, 360-degree ventilation, larger feeding mouth, not easy to fall off the lid, non-slip bottom design.


Date of Graduation
Master of Science in Materials Science
Physics, Astronomy, and Materials Science
A combination of thermal decomposition and surfactant-assisted synthesis route was utilized to synthesize novel CoO/MnFe2O4 heterostructured nanoparticles. Four samples of varying CoO core size were synthesized with variable extent of overgrowth phase. XRD, XPS, SEM and TEM data show evidence of MnFe2O4 spinel phase overgrowth on CoO rock-salt structured nanoparticles. XPS and magnetic data reveal partial oxidation and formation of Co3O4 phase on 7 nm and 19 nm size CoO-based nanoparticles. The remaining samples having 22 nm and 34 nm dimensions show a higher percentage of FiM materials overgrowth on the nanoparticle surface and no Co3O4 phase formation. The variation in core size, extent of MnFe2O4 overgrowth and Co3O4 formation significantly impacts the magnetic properties and exchange bias interactions of the heterostructured nanoparticles. The largest exchange bias of 6.2 KOe was measured from the 7 nm sized sample whereas largest coercivity of 3.26 KOe was measured from the 19 nm sized sample, at 5 K. Interface crystallinity, surface effect, uncompensated spins play a crucial role to achieve better exchange bias. The exchange bias showed sensitivity to core size and relative percentage of AFM and FiM materials. This effort in the synthesis technique of heterostructure core-shell system as well as understanding the large exchange bias effect may lead to the potential use of heterostructured nanoparticles in magnetic devices and biomedical applications.
heterostructure, magnetic, exchange bias, anisotropy, coercivity, hysteresis
Nanoscience and Nanotechnology | Other Materials Science and Engineering
© Mohammad Tauhidul Islam
Islam, Mohammad Tauhidul, "Synthesis of Novel CoO/MnFe2O4 Heterostructured Nanoparticles and the Effects of Variable Size and Extent of Overgrowth on Their Magnetic Properties" (2020). MSU Graduate Theses. 3573.


Submitted to: European Symposium on Industrial Crops and Products
Publication Type: Abstract Only
Publication Acceptance Date: 3/25/1999
Publication Date: N/A
Technical Abstract: Market potential for biodegradable lubricants is expected to grow with the increase of environmental regulations. Biodegradability is a property of lubricant basestock (80% of total lubricant), and presents an opportunity for veg. oils to be utilized at large scale. Applicability of a given base- stock is determined by viscometrics, oxidative stability, deposit formation, volatility, low temp. solidification, hydrolytic stability, solvency, miscibility and seal compatibility. Major concerns for veg. oils are their low oxidative stability and poor low temp. performance. Oxidative stability tests using Pressurized Differential Scanning, Oxidative Stability Index and Microoxidation (heating thin film of oil on metal surface under controlled air flow) showed that veg. oils perform not as well as their main biodegradable competitors, such as polyol esters, poly alpha olefins and isoalkyl adipates. Methylene interrupted polyunsaturation is the main factor causing unacceptable oxidative stability. Presence of multiple reactive sites in triglyceride molecules results in oxidative gelation under microoxidation conditions, unlike other fluids. Volatilities of those fluids were much higher than those of veg. oils. Low temp. behavior was monitored using pour point measurement and extended cold storage tests. Presence of saturated fatty acids and high molecular weight of triglycerides were main reasons of rapid crystalli- zation. Veg. oils were modified chemically to reduce their Iodine Value and improve viscometric properties without compromising biodegradability. Although oxidative stability testing did not show desired improvement, low temp. properties in many respects was better than that of original oils.


1mm thick steel sheet in coils secondary quality
Being quality-centric firm, we are engaged in presenting a high-class range of 409 Stainless Steel Sheets. General Properties Alloy 409 is a general purpose, chromium, titanium stabilized, ferritic stainless steel whose primary application is automotive exhaust systems.
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As new building and insulation materials have entered the market, confusion over the nature and meaning of R-Value has raised questions among building professionals and consumers alike. What exactly is R-Value? Is it an effective and objective measure of the thermal performance of an insulation product or construction system? And how should the marketplace use it to compare the benefits of one insulation material over another?
During the 1970's demand for quality building insulation soared, when an oil crisis sent heating and cooling costs skyward, With many new products on the market -- and with so many conflicting claims pertaining to the insulating abilities of those products -- the Federal Trade Commission, with the participation and support of the insulation industry, created an objective method for reporting the performance of residential insulation materials. This method is called the R-Value Rule.
The rule provides requirements for product labeling (R-Value) and advertising, and mandates specific ASTM methods for thermal testing. The R-Value rule attempted to create a level-playing field for competing insulation materials. "The R-Value Rule has been helpful in comparing different brands of the same type of insulating material," said Betsy de Campos, executive director of EPSMA, "but as more sophisticated materials and higher technology construction systems are introduced into the building industry we find that the R-Value of a material does not tell the whole story."
R-Value is based on a mathematical term known as R-Factor. The term R-Value was developed to represent the ability of an insulation material to restrict heat flow. It is determined by placing test specimens between two plates in a laboratory apparatus and measuring heat-flow through the insulation. The test specimen usually consists of a square foot of material exactly one inch thick whose surfaces have a temperature differential of 1degree Fahrenheit. The thermal conductivity (k) of a material is expressed as the rate of heat flow in BTUs per hour.
R-Value then, is the R-Factor of an insulation material multiplied by the amount of material used. For instance, if the specified insulation has an R-Factor of 3.8 and you are using 3.5 inches of insulation, the R-Value is 13.3. Thermal resistance (R) of a material is its resistance to heat flow, and R-Value is expressed as the reciprocal of the materials thermal conductivity.
Pretty technical stuff, but the idea that a consumer should be able to compare insulation is essential to ensuring homeowners and building professionals are capable of making informed product decisions. Simply put, the greater the R-Value the better the insulation.
But, there is more to consider when making those decisions today.


Patent application title: ENGINEERED FLUORIDE-COATED ELEMENTS FOR LASER SYSTEMS
Jue Wang (Fairport, NY, US)
Jue Wang (Fairport, NY, US)
Horst Schreiber (Rochester, NY, US)
Horst Schreiber (Rochester, NY, US)
IPC8 Class: AC23C1414FI
Class name: Direct application of electrical, magnetic, wave, or particulate energy ion plating or implantation silicon present in substrate, plating, or implanted layer
Publication date: 2011-08-25
Patent application number: 20110206859
The invention is directed to elements having fluoride coated surfaces
having multiple layers of fluoride material coatings for use in laser
systems, and in particular in laser systems operating at wavelength
<200 nm. In a particular embodiment the invention is directed to
highly reflective mirrors for use in wavelengths <200 nm laser
systems. The invention describes the mirrors and a method of making them
that utilizes a plurality of periods of fluoride coatings, each period
comprising one layer a high refractive index fluoride material and one
layer low refractive index fluoride material, and additionally at least
one layer of an amorphous silica material. The silica material can be
inserted between each period, inserted between a stack consisting of a
plurality of periods, and, optionally, can also be applied as the final
layer of the finished element to protect the element.
1. A method for making a fluoride coated element suitable for use <200
nm laser systems, said method comprising the steps of: providing a
substrate; coating, using an energetic deposition technique, the
substrate with one or a plurality of periods of fluoride coating
materials using an energetic deposition technique, and further coating,
using an energetic deposition technique, with an amorphous SiO2
material to thereby form a fluoride coated element suitable for use in
<200 nm laser systems; wherein coating the substrate with one or a
plurality of periods of fluoride coating materials means coating such
that each period comprises a layer of a high refractive index fluoride
coating material and a layer of a low refractive index coating material.
2. The method according to claim 1, wherein said method further comprises coating said substrate with a layer of an amorphous SiO2 material prior to the application of the first period of fluoride coating materials.
3. The method according to claim 1, wherein coating using an energetic deposition technique comprises coating using deposition techniques selected form the group consisting of plasma ion-assisted deposition, ion-assisted deposition and ion beam sputtering.
4. The method according to claim 1, wherein the method further comprises coating said element with a final layer of an amorphous silica after the coating with a plurality of fluoride materials is completed.
5. The method according to claim 1, wherein coating with said amorphous silica material means coating with a silica material selected from the group consisting of silica, F-doped SiO2, N-doped SiO2 and Al2O3-doped SiO.sub.2.
CROSS-REFERENCE TO RELATED APPLICATIONS
 This is a divisional of U.S. patent application Ser. No. 12/072,427 filed on Feb. 26, 2008, which claims the benefit of priority under 35 U.S.C. §119(e) of U.S. Provisional Application Ser. No. 60/904,132 filed on Feb. 28, 2007, the content of which is relied upon and incorporated herein by reference in its entirety, and the benefit of priority under 35 U.S.C. §120 is hereby claimed.
 The invention is directed to fluoride coated surfaces and elements having multiple layers of fluoride material coatings for use in laser systems. In particular, the invention is directed to surfaces, for example, highly reflective mirrors for use with 193 nm lasers that have multiple layers of coatings of fluoride materials.
 ArF excimer lasers are the illumination sources of choice for the microlithographic industry. The industry constantly demands more performance from excimer laser sources. As a result, greater demands are constantly placed on excimer laser optical components, for example, the highly reflective mirrors that are used in 193 nm wavelength excimer lasers that operate at high repetition rates. These highly reflective mirrors are typically made using at least one high refractive index material and one low refractive index material. Among the very limited number of materials that can be used for such mirrors, GdF3 and LaF3 are considered as high refractive index materials and MgF2 and AlF3 are the low refractive index materials that are used for wavelengths below 200 nm. [see D. Ristau et al., "Ultraviolet optical and microstructural properties of MgF2 and LaF3 coating deposited by ion-beam sputtering and boat and electron-beam evaporation", Applied Optics 41, 3196-3204 (2002); R. Thielsch et al., "Development of mechanical stress in fluoride multi-layers for UV-applications", Proc. SPIE 5250, 127-136 (2004); C. C. Lee et al., "Characterization of AlF3 thin films at 193 nm by thermal evaporation", Applied Optics 44, 7333-7338 (2005); R. Thielsch et al, "Optical, structural and mechanical properties of gadolinium tri-fluoride thin films grown on amorphous substrates", Proc. SPIE 5963, 59630O1-12 (2005); and Jue Wang and Robert L. Maier, "Nano-structure of GdF3 thin film evaluated by variable angle spectroscopic ellipsometry", Proc. SPIE 6321, p6321071-10 (2006)]. At the present time there is renewed research interest in wide band-gap fluoride thin films for ArF laser optics applications. The application of energetic deposition processes, such as plasma ion-assisted deposition (PIAD), ion assisted deposition (IAD) and ion beam sputtering (IBS), are restricted for fluoride materials because of the nature of fluoride materials. As a result, the industry has accepted thermal resistance evaporation for fluoride film deposition without introducing fluorine depletion. However, when thermal resistance evaporation is used as the film deposition method, the resulting fluoride film packing density is low (that is, it is porous) and the film structure is inhomogeneous. Neither of these is desirable because a porous structure can harbor environmental contamination and increases scatter losses. Various approaches have been applied to improve fluoride film structure including substrate temperature and deposition rate. Recently, the effect of substrate crystal orientation has also been taken into account, but no significant improvements have been reported. [see Y. Taki and K. Muramatsu, "Hetero-epitaxial growth and optical properties of LaF3 on CaF2", Thin Solid Films 420-421, 30-37 (2002), and U.S. Pat. No. 6,809,876 to Y. Taki et al., titled "OPTICAL ELEMENT EQUIPPED WITH LANTHANUM FLUORIDE FILM"].
 Another problem arises from the fact that many periods of high index and low index layers (one period equals one high and one low refractive index layer) are required in order to get high reflectivity at 193 nm. However, the surface/interface roughness and inhomogeneity increase as number of layers and the overall thickness increases. The control of the multilayer fluoride film structure is critical for achieving high reflectivity at 193 nm. In addition to their use in microlithography, fluoride coated mirrors are also required for those areas where ArF excimer laser have other, non-lithographic application, for example minimal invasive brain-, vascular- and eye surgery; ultra-precision machining & measurement; large-scale integrated electronic devices; and components for communication. In view of the problems extant with the present fluoride coated elements, for example mirrors, that are used in below 200 nm, and particularly in 193 nm, lithography, it is desirable to have fluoride coated elements that overcome these problems. In addition to mirrors, the invention can also be applied to beamsplitters, prisms, lenses, output couplers and similar elements used in <200 nm laser systems.
 The invention is directed to elements for use in <200 nm laser systems, the element comprising a substrate; one or a plurality of periods of fluoride coating materials, each of said periods comprising at least one layer of a high refractive index fluoride material and at least one layer of a low refractive fluoride material; and at least one layer of an amorphous SiO2 material selected from the group consisting of amorphous silica, amorphous F-doped SiO2, amorphous Al2O3-doped SiO2, and amorphous N-doped SiO2. In accordance with the invention the amorphous SiO2 material can be inserted after each period of the fluoride coating material or after a stack consisting of a plurality of periods of fluoride coating material. Optionally, a layer of the amorphous SiO2 material can be applied to the substrate prior to the application of the first period of fluoride coating materials. The fluoride coating materials are metal fluoride materials having a high refractive index and low refractive index, and these materials are applied in alternating layers to the substrate or amorphous SiO2 coated substrate. In some embodiments the high refractive index fluoride material has an index in the range of 1.65 to 1.75 and said low refractive fluoride material has an index in the range of 1.35 to 1.45. Substrates that can be used for the elements are glass and glass-ceramic substrates; alkaline metal fluoride single crystal substrates; metallic substrates, for example without limitation, substrates made from aluminum, titanium, and other metals known in the art that are know to be resistant to deterioration in a 200 nm laser environment such as found in ArF and F2 lasers; and other materials resistant to deterioration in a 200 nm laser environment such as found in ArF and F2 lasers, for example silicon nitride (Si3N4). The amorphous SiO2 material includes amorphous SiO2 itself and doped amorphous SiO2 materials such as silica materials doped with fluorine (F), silica materials doped with Al2O3, and silica materials doped with nitrogen (N), fluoride (F) and Al2O3. Each period of fluoride coating has a thickness in the range of 50 nm to 90 nm, and within the period the high refractive index material has a thickness in the range of 20 nm to 40 nm, and the low refractive index material has a thickness in the range of 30 nm to 50 nm. The SiO2 layer applied to the substrate before coating (optional), or after a period or stack of periods, has a thickness in the range of 5 nm to 75 nm. The final layer of SiO2 applied to element after the deposition of all the fluoride coating periods has a thickness in the range of 10 nm to 150 nm.
 The invention is further directed to a method for preparing fluoride coated elements and in particular highly reflective fluoride coated mirrors for use in <200 nm laser systems. The method has at least the steps of providing a substrate; coating the substrate with one or a plurality of periods of fluoride coating materials using an energetic deposition technique, each such period having at least one layer of a high refractive index fluoride material and at least one layer of a low refractive index fluoride coating material; and further coating using an amorphous SiO2 material including amorphous SiO2 material itself and doped amorphous SiO2 materials. In one embodiment of the method the SiO2 is applied as a layer after each fluoride coating period. In another embodiment of the method the SiO2 layer is applied after a stack of a plurality of fluoride coating material periods. In another embodiment of the method a SiO2 layer is applied to the substrate prior to the applying the first period of fluoride coating materials. Energetic deposition techniques that can be used in practicing the invention include PIAD (plasma ion-assisted deposition), IAD (ion-assisted deposition), and IBS (ion beam sputtering).
BRIEF DESCRIPTION OF THE DRAWINGS
 FIG. 1 (Prior Art) is a graph illustrating the refractive index depth profile of a GdF3 film grown on CaF2 (111).
 FIGS. 2A and 2B (Prior Art) are AFM images of GdF3 single layer grown on a CaF2 (111) single crystal.
 FIG. 3 (Prior Art) is a graph illustrating the absorbance of a GdF3 film at 193 nm as a function of air exposure time.
 FIG. 4 (Prior Art) is a schematic diagram illustrating of a standard fluoride mirror having high and low refractive index materials coated on a substrate.
 FIG. 5 (Prior Art) is a graph illustrating the surface roughness of standard fluoride mirrors as a function of stack period.
 FIG. 6 (Prior Art) is a graph illustrating the scatter loss of standard fluoride mirrors as a function of stack period.
 FIG. 7 (Prior Art) is a graph illustrating the reflectance of standard fluoride mirrors as a function of stack period.
 FIGS. 8A and 8B are AFM images comparing the PIAD smoothed SiO2 film of FIG. 8A with the uncoated SiO2 substrate of 8B.
 FIG. 9 is a schematic diagram illustrating the surface and interface of an engineered fluoride mirror.
 FIG. 10 is a schematic diagram illustrating the surface and interface of an engineered fluoride-enhanced-oxide mirror.
 FIG. 11 is a schematic diagram illustrating the surface and interface engineered fluoride-enhanced-Al mirror.
 As used herein, the terms "fluoride coated mirrors" and "fluoride mirrors" include mirrors in which the fluoride coating is applied to substrates such as alkaline earth metal fluoride single crystal materials (single crystals of CaF2, BaF2, SrF2, BaF2), glass materials (for example SiO2, HPSF® (Corning Incorporated), BK7® and SF10® (Schott Glass)), metallic materials (for example, aluminum, titanium) and other materials (for example, Si, Si3N4). Also as used herein, the term "period" as applied to fluoride coatings means one high refractive index layer and one low refractive index layer. The term "stack" as used herein means two or more periods of fluoride materials coated on the substrate which lie between the substrate and the SiO2 films of the invention or between two SiO2 films.
 In wavelengths <200 nm laser systems, for example, ArF laser systems which operate at 193 nm, scatter and contamination are the main factors that degrade the performance of fluoride mirrors and fluoride enhanced mirrors. Fluorine depletion generates significant absorption at 193 nm if advanced energetic deposition processes are used to improve fluoride film structure and reduce scatter loss. Among the problems associated with standard fluoride mirrors, including fluoride-enhanced-oxide mirrors and fluoride-enhanced-Al mirrors are:  (1) it is difficult to obtain a reflectivity over 97% at 193 nm,  (2) the reflectivity is environmental sensitive,  (3) the porous structure of fluoride films harbors contamination, leading to absorption at 193 nm, and  (4) laser durability is low The present invention overcomes these problems by insertion of amorphous silica (SiO2) layers between a period or stack of periods of the high and low refractive index materials that are use to coat the mirror blanks (substrates). In general, the invention is directed to using a PIAD smoothed SiO2 layer is periodically inserted into fluoride stacks and also use SiO2 as the top, capping or final layer. More specifically, the invention relates to:  (1) inserting amorphous SiO2 layer to eliminate the growth of inhomogeneous fluoride film structure,  (2) using PIAD to smooth the amorphous SiO2 layer surface,  (3) continuously growing fluoride films on the smoothed SiO2 surface, and  (4) using the dense smoothed SiO2 as capping layer to reduce the fluoride exposed surface area by a factor of ˜10-5 and thus to seal the engineered fluoride mirror.
 . The Surface Roughness of a Fluoride Single Layer
 Standard fluoride mirrors comprise multiple layers of fluoride materials; in particular, alternating layers of a high refractive index material and a low refractive index material. The fluoride film growth mechanism was investigated using a GdF3 single layer as an example, and the results indicate that the layer has an inhomogeneous structure and a rough surface. FIG. 1 (Prior Art) shows the refractive index (at 193 nm) depth profile of a GdF3 film grown on CaF2 (111) surface. The refractive index is proportional to film packing density. In general for the GdF3 film, high refractive index originates from a dense film, whereas low refractive index corresponds to a porous film structure. As can be seen in FIG. 1, at the beginning of the GdF3 film formation a dense thin layer is formed on the substrate leading to a refractive index of 1.738. As the film thickness increases, the growth mechanisms of columnar and polycrystalline microstructure may introduce gaps between crystal grains. As a consequence, the film density decreases as the layer thickness accumulates. At the end of film growth the refractive index has further dropped to 1.62, corresponding to a mean porosity of 15.8%. A refractive index of 1.35 represents a 3.5 nm surface roughness layer in FIG. 1. High refractive index fluoride materials have an index of refraction n in the range of 1.65 to 1.75, and low refractive index fluoride material has an index on the range of 1.35 to 1.45.
 FIGS. 2A and 2B (Prior Art) exhibits AFM (atomic force microscopy) images over 1μ×1μ and 5μ×5μ scanning areas of the GdF3 layer, respectively. The grain and the pore sizes shown in FIGS. 2A and 2B range from 300 nm to 350 nm. The AFM images clearly reveal the nano-porous morphology of GdF3 film growth on a CaF2 (111) surface. As can be seen in the 1μ×1μ image of FIG. 2A, there are some gaps between the accumulated dense grains, leading to the formation of porous structure. By increasing AFM scanning size to 5μ×5μ as shown in FIG. 2B, the porous network is obvious on the film growth plane. As predicted by ellipsometric modeling, the inhomogeneity of the GdF3 film is a result of film porosity changes during growth. The randomly distributed porous structure with relatively high internal surface area may connect to each other to some degree and may harbor environmental contamination.
 FIG. 3 (Prior Art) shows the absorbance of the GdF3 film at 193 nm as a function of laboratory ambient exposure (air exposure). The film absorbance increases over exposure time to air. In summary, fluoride films are inhomogeneous and porous in general. As layer thickness increases, film surface roughness increases. The porous film structure and rough surface lead to high absorption and scatter loss at 193 nm wavelength.
 . Surface and Interface of Standard Fluoride Mirror
 Based on our experimental results, the surface roughness of standard fluoride mirror, Rm, can be described by Equation (1),
where α and β are fluoride material and deposition process related parameters, Rs is the surface roughness of the substrate, and p is the stack period. A stack period is defined as a combination of low refractive index and high refractive index layers. Parameter α is related to the high and the low refractive fluoride layers used for the period such as GdF3/MgF2, LaF3/MgF2, GdF3/AlF3 and LaF3/AlF3, the deposition rate and substrate temperature for each material. Parameter β is dominated by the substrate material properties and surface finishing condition. Using standard fluoride mirrors, for example, at a normal angle of incidence, i.e., 0°, the fluoride mirrors compromise stacks of high and low refractive index layers as represented by Formula (2):
where H and L corresponds to a quarter-wave high index GdF3 and a quarter-wave low index AlF3, respectively, and p is a stack period. A schematic of the mirror is shown in FIG. 4 (Prior Art). [Note: In all the figures, the substrate is numbered as 20; H is numbered as 30; L is numbered as 40, the SiO2 layer 2M is numbered as 50.]
 FIG. 5 (Prior Art) is a graph showing the surface roughness of standard fluoride mirrors as a function of stack period. The surface roughness is linearly proportional to the stack period as described in formula (1). That is, the more periods a standard mirror contains the rougher the surface becomes. FIG. 6 (Prior Art) shows surface and interfacial scatter loss of fluoride mirrors as a function of stack period. Generally, a large number of stack periods (p>16) are required in order to achieve high reflectivity in the final mirror product. As can be seen from FIG. 6, scatter loss increases slowly when the stack period is a small number. However, FIG. 6 shows that the slope of the curve increases along with an increasing number of stack periods. In other words, scatter loss increases faster than the additional reflectivity gain due to adding more stack periods into standard fluoride mirror. As a result, there is an optimized number of stack periods which offers the highest reflectivity when one takes into account of scatter loss.
 FIG. 7 (Prior Art) shows reflectance of standard fluoride mirror as a function of stack period. According to the design calculations (design curve is numeral 80), the reflectance as a function of stack period can be separated into 3 zones which are:
 1. a fast increasing region (up to 6 periods),
 2. a slow increasing region (more than 16 periods) and
 3. transition region from the fast increase to the slow increase.
 The achievable reflectance (numeral 82), which also has 3 zones, is plotted in the same figure for comparison. The fast increasing region of the achievable reflectance is almost the same as that of the design reflectance. The transition zone for the achievable reflectance is very similar to the design, but there is a small separation when the stack period number is located at the high end of the zone. The main difference between the achievable reflectance and the design reflectance is located in the region where the period number is greater than 16. Instead of a slow increase of reflectance as shown for the design reflectance, a slow decrease of reflectance appears in the high period region for the achievable reflectance because of scatter loss. Consequently, in order to successfully make a high reflectance fluoride mirror it is necessary to eliminate surface and interface roughness. As discussed above, energetic deposition techniques cannot be used to make dense smooth fluoride films without generating fluorine depletion. The invention describes high reflectance fluoride mirrors which utilize SiO2 based oxide layers to smooth-out fluoride films to achieve high reflectivity.
 . Smoothed Amorphous SiO2 by Energetic Deposition
 In accordance with the invention, an amorphous but dense and smooth, SiO2 film is inserted into a fluoride stack by means of energetic deposition. Dense smooth SiO2 films can be deposited by PIAD, IAD and IBS. Here PIAD deposited SiO2 is used as an example. FIG. 8A is an AFM image of PIAD smoothed SiO2 film on a SiO2 substrate. The surface roughness of the uncoated substrate is 0.35 nm. After depositing a 200 nm SiO2 film, the surface roughness has been reduced to 0.29 nm. The result shows that the smoothed SiO2 film reduces roughness of an uncoated substrate. FIG. 8B illustrates how a SiO2 film can be also used to improve, that is, decrease, the surface smoothness of a coated substrate. In accordance with the invention, at least one PIAD deposited SiO2 layer has been inserted into standard fluoride mirror to protect fluoride films from plasma ion direct bombardment, and to smooth out the fluoride film's accumulated rough structure. Fluoride stacks can be continuously deposited on the smoothed SiO2 film layer. In preferred embodiments the final layer is a SiO2 film layer. In FIG. 8B, the surface roughness is 0.29 nm after application of the SiO2 film. Before application of the SiO2 film the surface roughness was 0.35 nm.
 . Surface and Interface Engineered Fluoride Mirror
 Surface and interface engineered fluoride mirrors can be described by Formula (3):
Sub_H(LH)i2M(LH).sup.j2M . . . (LH).sup.k2M (3)
where 2M represents a half-wave SiO2 layer; H and L are high index and low index fluoride layers, respectively; and i, j . . . and k are stack periods. According to Equation (3), a SiO2 layer is inserted into standard fluoride mirror every i, j . . . k stack periods. FIG. 9 shows a schematic of surface and interfacial engineered fluoride mirror as represented by Formula (3). Table 1 lists a comparison of standard and surface/interface engineered fluoride mirrors with a stack period of 21, where 3 nm surface and interface roughness is used for the engineered mirror.
TABLE-US-00001 TABLE 1 Comparison of standard and surface/interface engineered mirrors Standard mirror Engineered mirror Scatter loss (%) 5.69 1.16 Reflectance design (%) 99.96 99.57 Reflectance achievable 94.27 98.41 (%)
 Although the designed reflectance of the standard mirror (99.96%) is higher than the engineered mirror (99.57%), the scatter loss of the standard mirror is 4.9 times greater than that of the engineered mirror. The final achievable reflectance is 94.27% and 98.41% for the standard and the engineered mirrors, respectively. In some embodiments of the invention the top layer of the engineered mirror ends with a dense SiO2 layer as shown in formula (3). This top layer of SiO2 seals and smoothes the porous structure as is shown in the AFM images of FIGS. 8A and 8B. In addition, as a result of applying a dense SiO2 film as described herein, the risk for environmental contamination penetrating into the porous fluoride structure is eliminated. This is a further difference between the surface/interface engineered mirrors of the invention as compared to the standard fluoride mirror which can easily be contaminated due to porosity as is illustrated by GdF3 single layer data shown in FIG. 3 (Prior Art).
 . Surface/Interface Engineered Fluoride-Enhanced-Oxide Mirror
 The invention, in another embodiment, is also directed to fluoride-enhanced-oxide mirrors in which the fluoride enhanced stacks are smoothed by inserting PIAD deposited SiO2 layers in a Formula (4)
Sub_H0(L0H0)i(LH).sup.j2M . . . (LH).sup.k2M (4)
or Formula (5)
Sub_(H0L0)iH(LH).sup.j2M . . . H(LH).sup.k2M (5)
where H0 and L0 corresponds to a quarter-wave high index Al2O3 and a quarter-wave low index SiO2, respectively; 2M represents a half-wave SiO2 layer; and H and L are high index and low index fluoride layers, respectively. A schematic of surface and interface engineered fluoride-enhanced-oxide mirror is shown in FIG. 10 where H0 is numeral 32; L0 is numeral 42; and H, L and 2M are represented by numerals as previously indicated.
 . Surface/Interface Engineered Fluoride-Enhanced-Aluminum Mirror
 The invention, in another embodiment, is also directed to fluoride-enhanced-aluminum mirror, in which the fluoride enhanced stacks are smoothed by inserting PIAD deposited SiO2 layers as represented by Formula (6):
Sub_A(LH).sup.j2M . . . (LH).sup.k2M (6)
or Formula (7)
Sub_AH(LH).sup.j2M . . . (LH).sup.k2M (7)
where A is a thickness aluminum (Al) layer; 2M represents a half-wave SiO2 layer; and H and L are high index and low index fluoride layers, respectively. A schematic of surface and interface engineered fluoride-enhanced-Al mirror is shown in FIG. 11, the aluminum layer (Al) being represented by numeral 70; and H, L and 2M are represented by numerals as previously indicated.
 To summarize the characteristics of the invention:  H can be any high refractive index fluoride material, for example, GdF3, LaF3, and other high refractive index metal fluoride materials known in the art.  L can be any low refractive index fluoride material, for example, AlF3, MgF2, CaF2 and other low refractive metal fluoride materials known in the art  SiO2 based layer can be SiO2 or modified SiO2, for example, F-doped SiO2, N-doped SiO2, and Al2O3-doped SiO2,  Energetic smoothing technique that can be used in practicing the invention can be PIAD (plasma ion-assisted deposition), IAD (ion assisted deposition), IBS (ion beam sputtering), and similar energetic techniques known in the art as being useful for the deposition of the oxide materials and particularly oxide materials.  The layer order of H and L in Formulas (3)-(7) can be changed. For example, the order in Formula (3) may change from
 Sub_H(LH)i2M(LH).sup.j2M . . . (LH).sup.k2M (3)
Sub_(HL)i2MH(LH).sup.j2M . . . (LH).sup.k2M (8)
Sub_(LH)i2M(LH).sup.j2M . . . (LH).sup.k2M (9)  Formulas 4-7 may similarly be changed.  Changing the optical thickness in Formulas (3)-(7) enables one to apply the invention to S-polarization or P-polarization mirrors at high angle of incidence at 193 nm. Typically the thickness of the high refractive index layer is in the range of 20 to 35 nm, and the thickness of the low refractive index material is in the range of 30 to 45 nm. The thickness of the SiO2 film inserted, in accordance with the invention, after a period or a stack of periods is typically in the range of 5 to 75 nm. The thickness can be changed to 22 to 39 nm for the high refractive index material and 36 to 54 nm for the low refractive index material for applications to S-polarization or P-polarization mirrors at high angle of incidence at 193 nm.  The element can be selected from the group consisting of reflective mirrors, beamsplitters, prisms, lenses, and output couplers.  The high refractive index material can be selected from the group consisting of GdF3 and LaF3.  The low refractive index material can be selected from the group consisting of MgF2, CaF2 and AlF3.  The thickness of the amorphous SiO2 layer inserted between the periods of high and low refractive index materials can be in the range of 5 nm to 75 nm. Changing optical thickness in Equations (3)-(7) also enables one to apply the invention to other DUV laser wavelengths, for example, other <200 nm laser systems that operate at such <200 nm wavelengths such as 157 nm, 198.5 nm.
 While the invention has been described with respect to a limited number of embodiments, those skilled in the art, having benefit of this disclosure, will appreciate that other embodiments can be devised which do not depart from the scope of the invention as disclosed herein. Accordingly, the scope of the invention should be limited only by the attached claims.
Patent applications by Horst Schreiber, Rochester, NY US
Patent applications by Jue Wang, Fairport, NY US
Patent applications in class Silicon present in substrate, plating, or implanted layer
Patent applications in all subclasses Silicon present in substrate, plating, or implanted layer


We want to briefly present the benefits and positive improvements that the use of synthetic materials, especially high-grade polyvinyl chloride known as PVC, has brought to our daily lives. There are a few facts that need to be mentioned. Synthetic materials have become more widely used for making building elements by adopting the extrusion technology for multi-chamber hollow profiles.
The first windows were made about 50 years ago, but the first larger buildings were equipped in the mid 1960s. Since then, the use of PVC in the manufacture of window elements has revolutionized the construction industry. This is no wonder, because the quality, durability, ease of use and maintenance of PVC joinery are the properties that can hardly be achieved by using any other material. Today, in the homeland of PVC windows, Germany, synthetic materials occupy approximately 54% of the market of windows and other building joinery elements. The situation is similar in other European countries, including our country. There is no wonder for it, because there are many benefits of joinery that are made of synthetic materials, and the price is moderate, so the price-quality ratio is by far the most favorable.
SISTEM S8000 IQ
6 chamber insulation with curved construction, profile depth 74 mm and sash 85 mm with galvanized steel reinforcement with curved slats with gray gaskets seals is very good thermal and acoustic insulation with thermal permeability of Uf = 1.2 W/m2K (with appropriate glazing up to 0.84 W/m2K). Sound insulation: 32 dB (with appropriate glass up to 40 dB)
Benefits from installing low-E glass are additional thermal insulation.
The joinery standard equipment includes G-U Uni-Jet D tilt-turn hardware for 1 leaf and 2 leaf windows and balcony doors in the basic security design that can be easily upgraded to a higher level of security. The hardware is also characterized by simplicity and safety of handling and exclusive surface protection ferGUard*silver.
The standard paint for the manufacture of joinery is white, but we can offer the same product in a wide range of acrylic paints and wood decorations.
Intelligent automatic ventilation system GECCO may be installed at request.
Maintenance is simple and easy due to extremely smooth surfaces and large channel of the frame.
The goal of the development of this system was to achieve optimal thermal insulation that enables the production of windows suitable for passive houses. With the achieved heat insulation value profile of Uf = 0.92 W/m2K, and with the standard steel reinforcement and triple insulated glazing, the Ug-value of 0.6 W/m2K can achieve the Uw-value of 0.78 W/m2K which is suitable for passive houses.
The money invested in purchasing windows suitable for passive houses will give you energy savings with new windows in a short period of time.
Suitable for supporting triple functional glazing with a maximum thickness of 54 mm.
Narrow profile elevation width and design-oriented 15° incline.
Intelligent sealing concept with three end-to-end sealing levels.
Optimized for using STV® in order to dry glue window and sash projection.
Very good thermal and sound insulation through 6-chamber design and large installation depth for window frame and sash.
INNOVATION IN WINDOW PRODUCTION – STV ®
(STATISCHE – TROCKNEN – VERGLASUNG) = STATIC DRY GLAZING
The profile is suitable for using the STV technology which achieves the following:
- more stable elements and for producing unprecedented element sizes
- enhancement of the thermal insulation
- anti-burglary protection.
The profiles are delivered with the integrated adhesive tape which allows for producing unprecedented element sizes. By gluing the glass to the sash profile, the stability of the glass window is transferred into the sash and the entire system becomes more intrinsically stable.
In the combination of STV® with steel in the sash, particularly large window elements can be produced and the protection from burglars can be improved by gluing of glass and sash.


As a leading global manufacturer of crushing equipment, milling equipment,dressing equipment,drying equipment and briquette equipment etc. we offer advanced, rational solutions for any size-reduction requirements, including quarry, aggregate, grinding production and complete planGet Price
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In order for producing products meeting various customers’ needs, TOCOS develops a positive consciousness of our corporate motto “Think and Create” and pursue R&D based on accumulated technologies.
As to our main products (potentiometers, trimmer potentiometers), demands for downsizing and longer rotational life have always been in the market.
Working on the development of ink (resistive paste) which plays a key role for printing resistive element, we continuously address engineering development as well as R&D to conduct functional improvement in engineering resource.
For automotive applications, not only resistive element, wipers are one of the most important components and the shape and the material properties are to be characterized as an important research terms.
Integrating hardware and software technologies into all products, we address various themes like improving the high-accuracy and the efficiency in design through CAD and computing structure analysis including material, manufacturing process, geometric design.


Iron chalcogenide superconductor, FeSe, has attracted much attention for high tunability of the superconducting transition temperature (Tc). Although Tc of FeSe is 8 K in bulk form, it increases up to approximately 40 K by applying hydrostatic pressure, intercalation etc. Furthermore, ARPES measurements reported that a monolayer epitaxial film grown on SrTiO3 (STO) substrate shows superconductivity  with Tc as high as 65 K . The high Tc in the monolayer FeSe/STO is attributed to interface effects such as electron doping from STO substrate and electron-phonon interaction via the substrate. One important problem in the high Tc superconductivity in monolayer FeSe/STO is discrepancy in reported values of Tc depending on the measurement techniques. The 65 K Tc was reported by ARPES measurements. However, almost all of resistivity measurements reported the onset Tc (Tconset) of about 40 K and much lower zero-resistance Tc (Tczero) [1,3]. The only exception is the report of 109 K Tczero by Ge et al., for which a skepticism was proposed in terms of reproducibility and reliability . The disagreement between resistance Tc and those obtained by ARPES measurements casts a question whether the real Tc in monolayer FeSe/STO is 65 K or not. We have worked on the growth of epitaxial thin films of FeSe by a pulsed laser deposition (PLD) technique . We investigated electron doping effect by fabricating electric double layer transistor (EDLT) structure on the films, and found that even only electron doping increases Tczero up to 46 K [7,8]. This is the highest Tczero of FeSe ever reported including monolayer FeSe/STO except for ref. . Thus, it is intriguing how Tc of FeSe films grown by PLD changes as the thickness of FeSe films is reduced. It should be noted that all reports of high Tc in monolayer FeSe/STO is obtained in films grown by molecular-beam epitaxy (MBE). It might be possible that Tczero of monolayer FeSe/STO is higher than those ever reported when fabricated by PLD. In this work, we report growth and transport properties of FeSe/STO ultrathin films by the PLD technique.
Prior to the deposition, the STO substrates were thermally treated so that the step and terrace structure on the surface was observed. This is very important to obtain films with good superconducting properties. Fig. 1 shows the temperature dependence of resistivity for three films with different thicknesses, namely 30 nm, 20 nm, and 11 nm. All films show superconducting transition at low temperatures. Tconset increases as the thickness is reduced, and the 11-nm-thick film shows the highest Tconset = 26 K and Tczero = 11 K. These results are remarkable since these Tconset values are exceptionally high in terms of the relationship between Tc and in-plane strain reported for bulk superconductivity in FeSe films . All of these films have in-plane lattice constant, a ≧ 3.77 Å, leading to Tc < 8K according to the relationship reported in ref. . In addition, the behavior that Tconset increases with decreasing thickness is in good agreement with those of MBE-grown films  even quantitatively. These results indicate that the high Tc in the grown films is the result of the interface effects other than the lattice strain. In other words, we succeeded in realizing interface superconductivity in FeSe/STO by the PLD technique for the first time.
In the presentation, we will also show results of thinner films.
Figure 1 : Temperature dependence of resistivity for 30, 20, 11 nm films of FeSe/STO
 Q. Y. Wang et al., Chin. Phys. Lett. 29, 037402 (2012)
 S. He et al., Nat. Mater. 12, 605 (2013)
 A. K. Pedersen et al., Phys. Rev. Lett. 124, 227002 (2020)
 J. F. Ge et al., Nat. Mater. 14, 285 (2014)
 I. Bozovic and C. Ahn, Nat. Phys. 10, 892 (2014)
 Y. Imai, F. Nabeshima, A. Maeda Condens. Matter 2, 25 (2017)
 N. Shikama et al., Appl. Phys. Express 13, 083006 (2020)
 N. Shikama et al., Phys. Rev. B 104, 094512 (2021)
 F. Nabeshima et al., JJAP 57, 120314 (2018)
 Q. Wang et al., 2D Mater. 2, 044012 (2015)
Keywords: Iron chalcogenide, Pulsed laser deposition, Supercondutivity, ultrathin films


The paradoxical nature of black pearlescent pigments is due to the contradictory facts that 1) the color black is characterized by the absence of light and 2) the iridescence of pearlescent pigments is due to the structure-induced interference of light. Due to this apparent contradiction, the current black pearl technology is limited to pigments that either have a jet, matte-black appearance with no iridescence, or to iridescent black pearls that have blue, violet or green undertones and lack sufficient jetness. None of these pigments show the sparkle that pearlescent pigments are traditionally known for. A new black pearlescent pigment has been developed that has exceptional luster an sparkle and is sufficiently jet. The new pigments can be incorporated into a range of plastics with no reduction in effect. The properties of this pigment with respect to plastics will be described.
Biography – Jonathan Doll
Jonathan received a Ph.D. in polymer science from the University of Connecticut in 2011. During his studies, he researched the synthesis and/or manipulation of many varieties conducting and semiconducting nanomaterials including quantum dots, carbon nanotubes, iron oxide nanoparticles, metallic nanoparticles and conductive polymers. His published technical work includes papers in the journals Nature Nanotechnology and Nano Letters as well as presentations at multiple international conferences. Jonathan joined the Sun Chemical team in 2012 as a Senior Chemist in the Effect Pigments group. In 2014, he became the Leader of the Effect Pigments team at Sun Chemical. His research at Sun involves the synthesis and design of new metallic and pearlescent effects pigments as well as improving the properties of existing effects pigments. In his five years at Sun Chemical, Jonathan has filed over eleven provisional patents and published three papers.


All galvanised hollows are manufactured from AS/NZS 1365 cold rolled coil. Galvanised coating Z275.
MECHANICAL PROPERTIES – G250
Standard precision tube is manufactured from G250 steel.
Tensile strength expected min 320 Mpa.
Elongation expected min 25%.
MECHANICAL PROPERTIES – G310
Grade 310 hollows is manufactured from G310 steel.
Tensile strength expected min 340 Mpa.
Tensile strength typically above 450 Mpa.
Elongation typically above 25%.
Precision tube standard length is 5.5m but available ex-mill rolling in various lengths.
Heavy wall range available in 6.0m lengths but available ex-mill rolling in various lengths.
Common stock lines
Non stock material - available ex-mill rolling
Weights are theoretical and rounded to two decimal points
Precision Tube - Round
Precision Tube - Square
Precision Tube - FSO
Metric SHS G310
Metric RHS G310
Industrial Tube Colour Chart
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