JP2008516015A - Aluminum phosphate compositions, coatings and related composites - Google Patents

Abstract

A composite comprising a substrate and a coating component thereon, the coating component comprising an aluminum phosphate compound, wherein the compound has an aluminum to phosphorus ratio of about 0.5 to about 1 to about 25 to about 1 And the composite is arranged around a substantially vertical axis with respect to the configuration.

Description

  The present invention relates to an aluminum phosphate coating deposited on a substrate to provide the desired electrical, chemical, mechanical and physical properties. The present invention can teach a method of sealing to a porous material and also teaches novel compositions and modifications of aluminum phosphate materials.

  This application is a continuation-in-part of pending patent application 10745955 filed on December 23, 2003 and enjoys priority (incorporated herein by reference in its entirety). That application enjoys the priority of provisional applications 60/615920 and 60/615986 filed on December 23, 2002 (incorporated herein by reference in its entirety).

  There are many prior art patents related to the synthesis of aluminum phosphate materials that are primarily used as catalyst supports including crystalline and amorphous forms. Most synthetic methods use sol-gel methods with raw materials including commonly available aluminum salts and various phosphorus sources including phosphoric acid, diammonium hydrogen phosphate, phosphorous acid and the like. Many of these methods produce crystalline forms and some thermally stable amorphous compositions (US Pat. No. 4,289,863, Hill et al; 5698758, Racer et al; 6022513, Pecaro et al.). Prior art materials cannot be used, for example, as a coating to protect the substrate from corrosion or oxidation at elevated temperatures.

  In order to protect various substrates in industrial and consumer use applications, it is desirable to use a thermally durable and stable amorphous high density coating. Prior art coatings are not durable under certain atmospheric conditions where the material is subjected to heat treatment or exposed to a corrosive environment or under certain harsh industrial or use environments. Amorphous coatings based on silicon dioxide have been developed and recent patents define a unique method for depositing such coatings (US Pat. No. 6,162,498). However, the coating is not durable under certain harsh conditions, is not thermally stable at high temperatures, or does not function properly as a transparent coating on glass. A high temperature stable glassy or vitreous coating first coats the substrate with a slurry of glass frit and then treats the coating at a sufficiently high temperature to dissolve the glass frit to form a vitreous coating. It is manufactured by. Vitreous enamel coatings have existed for decades in many different compositions. However, they are usually cloudy and deform at high temperatures. The high temperature processing requirements to melt the glass frit may cause the substrate to degrade, and if a low melting glass composition is selected, they may not be durable.

  Vapor-deposited inorganic coatings are currently used in many applications, but they require expensive equipment and are not suitable for non-line of sight substrate shapes (eg, US Pat. No. 3,442,686, US Pat. No. 4,702,963, US Pat. No. 5,434,008, US Pat. No. 5,792,550). Solution-derived inorganic coatings provide conformability at a low cost for coating substrates.

  Also, some of the prior art inorganic coatings are completely suitable for use on glass where the transmission properties are affected or on other substrates where the substrate's aesthetic properties (metallic appearance) need to be preserved. Not transparent.

  Brushed steel and other related solid surfaces are widely used on the front in buildings, malls, elevators, table lamps, bathtub fittings, cabinet doors, wall plates and others. The desirable properties of these surfaces are easy to clean and resistant to fingerprints, in addition to being durable enough to heat exposure or heat, sunlight, various solvents and ordinary detergents, exposure to ultraviolet radiation. Other related properties, such as being resistant to food and not sticking to food.

  Porous surfaces are susceptible to contamination when used for storage purposes. Enamel, granite, marble, floor tiles, glass, porcelain fossilware, ovens and related cooking equipment in ovens, oven interior panels, food trays, cooktops and other ceramic surfaces are microscopic in their end use And macro holes and scratches. Sealing the granite holes will help provide anti-staining properties, for example, in a kitchen worktop. The hermetic seal of these holes also helps reduce gas permeability, which is important in certain applications. Surface treatment with polymers is a well-known technique for sealing porcelain surfaces, but their durability is limited by exposure to heat, cleaning solvents or agents and is relatively flexible. A suitable thin inorganic coating that is chemically inert and thermally stable is desired. Many of these applications symbolize a high degree of mass sales, for which reason low-cost coating technology is important in considering solution immersion or spray coating, which is the preferred method of application. Such treatment can also allow for antibacterial properties combined with self-cleaning surfaces, easy cleaning, biological safety, aesthetic value, hardness and abrasion resistance, solvent resistance. Furthermore, such sealants must have good thermal shock properties (e.g. hot pan on granite table) and thermal stability, and even if the sealant is worn, the effect of plugging pores on the surface is Will help extend the durability of the equivalent coating.

  Inventive materials in anodized aluminum parts and other related materials can improve performance and durability in addition to environmental and energy savings. The inventive material is a hermetic seal and adhesion promoter for ceramics (monolithic, composite and glass-ceramic) in various applications including tiles, electrical packaging substrates and refractory bricks to improve resistance and low gas permeability Can be used as

  Silicon carbide has excellent properties as a space and aerial platform optical material, but the brittle nature along with the high hardness of the material makes it difficult to finish to the required resistance. Depending on the size and shape of the substrate, it can take weeks to months to polish the surface to the wavelength fraction of the reflected light.

Current low dielectric materials do not have the required dielectric constant in combination with thermal and mechanical stability. New low-k materials are required to improve the current state of the semiconductor field.
Researchers are working on combining polymer and metal-foil substrates with printable TFT backplanes to bring flexible displays closer to commercialization. Although not yet available, for many years the “best goal” of the display industry is a thin film, transparent, flexible substrate with barrier properties comparable to that of glass sheets. That is, the prior art is somewhat insufficient in this regard.

  A photomask is a high precision plate containing a microimage of an electronic circuit. A structure to achieve a defect-free photomask must be put in place. Problems arise when the chromium layer is affected by the environment or interlayer reactions. All need to be avoided, but there are surface defects including scratches on the chromium outside the array, damage or removal of the AR coating, contamination on the chromium, and glass tips on the mask edge. The coating must be very thin and free of defects, in the range of about 10 nanometers.

  Plastic materials are generally susceptible to wear, moisture attack, UV radiation, oxygen atoms, exposure to solvents, degradation from chemicals, and the like. However, inorganic coatings deposited on plastics are currently used for many applications and require expensive equipment, such as non-line-of-sight substrate shapes (eg, US Pat. No. 3,442,686, US Pat. No. 4,702,963, US Pat. No. 5,434,008, US Pat. No. 5,792,550). Thus, low cost solution-derived protective coatings (inorganic and inorganic-organic composites) on plastic substrates with an appropriate treatment plan, along with the ability to coat composite processed substrates, provide continuous reel-reel or roll-roll processing. Necessary to develop.

  However, unlike glass and metal, all polymers are quite permeable to gases and vapors. Many technologies have been developed to reduce polymer permeability, thus increasing the applicability to food and beverage packaging. Also, the permeable barrier layer is important whenever the material to penetrate must be transferred. Tubes and hoses (important in automotive and equipment applications) for gasoline, fluorocarbon vapors, etc. require barrier performance beyond that currently available. Similarly, inorganic barrier coatings against moisture and oxygen, without fine defects and pinholes, are necessary for these display applications.

  In view of the above, an object of the present invention is to provide compounds, compositions, coatings and related composites or products based on aluminum phosphate, together with their use and methods of manufacture, whereby Various deficiencies and disadvantages of the prior art, including those outlined above, can be overcome.

  It will be appreciated by those skilled in the art that one or more aspects of the present invention may meet a particular purpose, while one or more other aspects may address certain other objectives. In all aspects of the invention, in each respect, each objective may not apply equally. Thus, the following objectives can alternatively be considered with respect to any one aspect of the present invention.

  For the purposes of the present invention, the term “inventive material”, its description or its citation refers to any aluminum phosphate-based compound of the present invention over all possible ranges of Al: P stoichiometry, or Means a composition and can be used with the methods, composites or articles of the invention and / or the films, layers or coatings associated therewith or described below, prepared as described herein, or Like the characterized compounds or compositions, or the references incorporated above and / or US Pat. Nos. 6,036,762 and 6,461,415 and pending patent application 10/362869 (July 15, 2003). Application) and 10/627194 and PCT / US03 / 36976 (filed July 24, 2003 and 11 November 2003, respectively) No. 10/642069 and PCT / US03 / 25542 (filed Aug. 14, 2003) (incorporated herein by reference in its entirety) and featured. As an aluminum phosphate compound and composition applied and / or applied, it will be understood as the compounds and compositions shown respectively.

  Without limitation, as indicated herein and / or throughout one or more of the above-incorporated patents or applications, the material of the present invention is on a molar basis and has a stoichiometric ratio of aluminum to phosphoric acid. Organic molecules, polymers, carbon, silicon, metals, metal oxides and / or other metal ions / salts (including non-oxides), whether less than stoichiometric or greater than stoichiometric Further, a compound and a composition mainly composed of aluminum phosphate containing particles and / or inclusions can be included. Specific examples of the inventive material are available from Applied Thin Films under the Cerablak trademark.

  “Inventive material” also includes materials based on aluminum phosphate and can be deposited as a thin film on a substrate using a custom-made precursor solution that produces a unique form of amorphous aluminum phosphate. . US Pat. Nos. 6,036,762 and 6,461,415 (Sambasivan et al.) And the above-mentioned patent applications provide details regarding precursor synthesis and provide chemistry, properties and other processing details. Also, various additions or modifications to the surface coated with the inventive material are considered examples of the present invention, examples of which are given below.

  Similarly, the term “substrate” or “solid substrate” includes polymers, plastics, earthenware, metals, alloys, silicon carbide, silicon, oxides, chalcogenides, pinicides, quartz, glass, etc. Without limitation, any solid material is included.

  One or more of the following objectives are coating the inventive material on various substrates that protect the substrate from various environmental factors including moisture, oxygen, ultraviolet light, etc. (particularly emphasized is the roll of substrate) -Roll continuous coating). Accordingly, such inventive material coatings can serve as protective and functional coatings.

  It is an object of the present invention to use an inventive material coating as an insulating layer having an effective insulating strength used in various applications such as optoelectronic devices on conductive substrates that require electrical isolation.

Another object of the present invention is to provide a coating or film of the above characteristics that can maintain a predetermined moisture content within the packaged amount.
The object of the present invention is to use the inventive material as an anti-iridescent and anti-fogging coating.

  The present invention is suitable for an improved method of forming an inventive material layer on a metal surface to provide an interface to enhance adhesion between the metal surface and the organic polymer coating, resulting as a result of being coated on the metal surface Suitable for oxide layer. The method includes applying an inventive material to a metal surface. The resulting coating layer can function as an interface to increase adhesion between the metal surface and the organic polymer coating.

  It is also an object of the present invention to use an inventive material coating in a housing for a moisture sensitive device, such as a moisture sensitive optical device, which includes a plurality of soldered at their ends defining the housing. Including a metal plate, an organic polymer coating is applied at least to the outer surface of the housing at the joint to provide a moisture barrier that prevents corrosion at the joint.

  One of the objects of the present invention is to use the present material coating as a thin, airtight, microstructurally dense, uniform and transparent coating using a simple dipping, rotating, spraying, brushing or flow coating process. It is to provide a method of depositing.

The object of the present invention is to use inventive material coatings to protect solid substrates from moisture, light, gases, chemicals and other environmental effects.
It is also an object of the present invention to protect the surface of a solid substrate during processing and utility at room temperature and elevated temperature.

  Further objects of the invention include, but are not limited to, solid substrates including scratch resistance, rust resistance, wear resistance, erosion resistance, high speed particles, damage caused by rain, water, liquid and other object impacts Is to improve the mechanical properties of

An object of the present invention is to protect space solid materials from a low earth orbit environment such as a high bundle of atoms and molecules such as oxygen, hydrogen, nitrogen and the like.
The object of the present invention is to use the inventive material as a primer or adhesion promoting layer on the polymerized surface.

The object of the present invention is to use the inventive material as a primer or adhesion promoting layer on a metal surface.
The object of the present invention is to use the inventive material as a primer or adhesion promoting layer on a ceramic surface.

The object of the present invention is to use the inventive material as a primer or adhesion promoting layer on the surface of a metal chalcogenide.
The object of the present invention is to use the inventive material as a primer or adhesion promoting layer on a solid surface.

The object of the present invention is to use the inventive material as an adhesive or binder with two similar or different types of materials.
The object of the present invention is to use the inventive material as an adhesive or binder for two identical or different optical materials.

The object of the present invention is to use the inventive material to coat surface defects and seal pores on the surface of solid substrates.
An object of the present invention is to planarize the surface of a coated solid substrate.

An object of the present invention is to reduce friction at the surface of a coated solid substrate.
The object of the present invention is to use the inventive material as an antistatic film on a solid substrate.
An object of the present invention is to use an inventive material layer as a low dielectric layer of a solid substrate.

The object of the present invention is to use inventive materials and modified inventive material coatings as antireflective layers on substrates such as polymers.
The object of the present invention is to use the inventive material coating as a moisture and oxygen barrier for flexible display structures.

The object of the present invention is to use the inventive material coating as a barrier against mechanical damage of the solid substrate.
The object of the present invention is to use inventive material coatings to adapt the optical properties of solid materials.

The object of the present invention is to use inventive material coatings to protect polymeric thermoplastics and other materials from photodegradation.
The object of the present invention is to use inventive material coatings to protect solid substrates against harmful microorganisms.

The object of the present invention is to use inventive material coatings on medical devices and parts made of solid materials against chemical and physical damage.
An object of the present invention is to use inventive material coatings on medical devices and parts made of solid materials against body fluid corrosion.

It is an object of the present invention to use inventive material coatings and modified inventive materials on medical devices, devices, implants and other parts to provide biocompatibility.
It is an object of the present invention to be used in the development of biocompatible materials that incorporate inventive materials and inventive material coatings on solid substrates.

An object of the present invention is to provide a highly colorless and transparent barrier film and a method for producing the same.
Another object of the present invention is to provide a film of the above character having a thickness in the range of about 10 to about 500 nm.

Another object of the present invention is to provide a coating or film of the above character having low friction.
Another object of the present invention is to provide a coating or film of the above character that can be produced at low cost.

Another object of the present invention is to provide a coating or film of the above character which reduces the total amount of solid material required in the device.
Another object of the present invention is to provide a coating or film of the above character which reduces the difficulty of recycling.

Another object of the present invention is to provide a coating or film of the above character that can be used in food packaging that can be used in a microwave oven.
Another object of the present invention is to provide a coating or film of the above character that can be used in packaged foods that can be used in microwave units and that can remain transparent with a long shelf life. .

Another object of the present invention is to provide a coating or film having the above characteristics that can maintain a predetermined moisture content for the contents wrapped in the barrier film.
Another object of the present invention is to provide a coating or film capable of producing a barrier film at high speed.

Another object of the present invention is to provide a coating that can planarize the polymer surface and can help reduce light scattering.
The object of the invention is to provide a functional coating, preferably an electrically conductive or magnetic coating, on a solid substrate by dispersion of additives in a precursor solution of inventive material.

  It is an object of the present invention to provide improved aircraft transparency by using an inventive material coating on a solid substrate and an electrically conductive metal oxide coating deposited on the solid substrate.

The object of the present invention is to provide aircraft transparency with a protective and adhesion promoting layer.
The object of the present invention is to develop inventive materials mixed with inorganic polymers and molecules (eg P and B containing materials such as phosphazene, borazine or borozole).

  It is an object of the present invention to develop inventive materials and inventive material coatings in which boron nitride, molybdenum silicide, molybdenum sulfide or other lubricating oil materials are dispersed to form a high temperature lubricating oil layer.

  The object of the present invention is to develop inventive materials of low dielectric constant by appropriately modifying the microstructure of the inventive materials, in particular by increasing the porosity of the inventive material coating.

  The present invention relates to the use of inorganic and inorganic-organic composite coatings of compositions based on aluminum phosphate on plastics or polymerized substrates for wear or abrasion and for improved protection from environmental attacks. Directed to.

  In particular, the present invention relates to chemical or curable coating compositions of precursor solutions that are utilized to derive the structure and properties of protective coatings deposited on plastics or polymerized substrates.

  The object of the present invention is to adapt precursor chemistry containing Al, P, O and other species to form a substantially inorganic coating with good adhesion under relatively low temperature cure conditions. Was that.

  A further object of the present invention is to include the presence of supplemental water, hydroxyl groups, organics and some nitrates or other salts in the substantially inorganic coating to increase the flexibility and strength of the coating.

  It is a further object of the present invention to generally provide a curable coating composition containing an aluminum phosphate compound in order to suitably adapt the curing conditions to minimize stress and add other functionality to the coating. The addition of organic and inorganic additives.

  A further object of the present invention is to provide adhesion promoting underlayers such as layers that are substantially inorganic or inherently inorganic-organic hybrids, and a) barrier properties such as layers that are substantially inorganic or inherently inorganic-organic hybrids. Sealing a microcrack in the underlying layer to be improved, and b) using a multi-layer comprising a top layer containing certain inorganic or organic additives to improve solvent resistance or wear of the coating system, the total film of the multi-layer system The thickness does not exceed about 15 microns, preferably about 10 microns, and most preferably about 5 microns.

  A further object of the present invention is to develop a stable sprayable formulation that can be cured with heat or UV or IR radiation or microwave treatment. Curing can function by one or more of one or more treatment methods.

A further object of the present invention is to develop a coating based on aluminum phosphate that is substantially transparent to the visible spectrum of electromagnetic radiation.
A further object of the present invention is either to deposit an organic layer on top or to incorporate specific organic additives into the curable formulation to promote durable hydrophilicity or hydrophobicity.

  It is a further object of the present invention to utilize a coating composition based on aluminum phosphate as an adhesive for bonding plastic substrates to other metals, ceramics, glasses and other plastic materials.

  One of the objects of the present invention is that the material of the present invention as a thin, airtight, microstructurally dense, uniform, transparent coating using a simple dipping, rotating, spraying, brushing or flow coating process. A method is provided for depositing a coating.

The object of the present invention is to use inventive material coatings to protect particles, polymers, etc. from moisture, light, gas and other environmental effects.
The object of the present invention is invented as a barrier film against inert gases (eg oxygen, nitrogen, hydrogen), chemically active gases (eg water, carbon dioxide), liquids and vapors (eg fragrances, fine chemicals, gasoline). The material is to be used.

The object of the present invention is to protect the polymer surface during processing and utility at room temperature and elevated temperature.
An object of the present invention is to improve mechanical properties including, but not limited to, scratch resistance, abrasion resistance, high velocity particles and damage resulting from impact of other objects.

The object of the present invention is to protect space polymers from a low earth orbit environment such as a high bundle of atoms and molecules such as oxygen, hydrogen, nitrogen and the like.
The object of the present invention is to use the inventive material as a primer or adhesion promoter on the polymerized surface.

The object of the present invention is to use the inventive material to cover surface defects and seal pores in the polymer surface.
The object of the present invention is to planarize the coated polymer surface.

An object of the present invention is to reduce friction at the coated polymer surface.
The object of the present invention is to use the inventive material as an antistatic film for polymers and related substrates.

The object of the present invention is to use an inventive material coating as the dielectric layer.
The object of the present invention is to use inventive materials and modified inventive coatings as antireflective layers in substrates such as polymers.

The object of the present invention is to use the inventive material coating as a moisture and oxygen barrier for flexible display structures.
The object of the present invention is to use an inventive material coating as a barrier against mechanical damage.

The purpose of the present invention is to use inventive material coatings to adapt the optical properties of materials such as polymerization.
The object of the present invention is to use inventive material coatings to protect polymers, thermoplastics and other materials from photodegradation.

The object of the present invention is to use inventive material coatings to protect against harmful microorganisms.
It is an object of the present invention to protect against chemical and physical damage by using inventive material coatings on medical devices and parts made of polymers.

The objective of this invention is providing the barrier film which has high colorless transparency, and its manufacturing method.
Another object of the present invention is to provide a barrier film having the above characteristics and having high transparency.

Another object of the present invention is to provide a coating or film of the above character which reduces the film thickness as a whole.
Another object of the present invention is to provide a coating or film of the above character having a film thickness in the range of about 10 to about 500 nm.

Another object of the present invention is to provide a coating or film of the above character in which the coated polymeric flexible substrate does not curl.
Another object of the present invention is to provide a coating or film of the above character having low friction.

Another object of the present invention is to provide a coating or film of the above character that can be produced at low cost.
Another object of the present invention is to provide a coating or film of the above character which reduces the total amount of plastic or polymer required in the device.

Another object of the present invention is to provide a coating or film of the above character which reduces the difficulty of recycling.
It is another object of the present invention to provide a coating or film of the above character that can be utilized for food packaging that can be used in a microwave oven.

  Another object of the present invention is to provide a coating or film of the above character that can be used to package food that can be used in microwave units and can remain transparent with a long shelf life. It is to be.

Another object of the present invention is to provide a coating or film having the above-described characteristics that allows the contents wrapped by the barrier film to maintain a predetermined moisture content.
Another object of the present invention is to provide a coating or film of the above character which can produce a barrier film at high speed.

Another object of the present invention is to provide a coating that can planarize the polymer surface and can help reduce light scattering.
Another object of the present invention is to provide an electronic or photoelectric device with an improved polymeric substrate by inventive material coating, which can avoid or at least reduce the problems of the prior art.

  The object of the invention is to provide a functional coating, preferably an electrically conductive or magnetic coating, on a solid substrate by dispersing additives in a precursor solution of inventive material.

  It is an object of the present invention to provide improved aircraft transparency by using an inventive material coating on a solid substrate and an electrically conductive metal oxide coating dispersed on the solid substrate.

The object of the present invention is to provide aircraft transparency with a protective and adhesion promoting layer.
Accordingly, the present invention relates to developing materials that are inorganic, organic-inorganic composites or inorganic dominant compositions. In certain embodiments, it is a material based on aluminum phosphate that can be useful in many applications that can be used in powder, bulk, fiber and as a coating. The present invention is primarily based on aluminum phosphates on a variety of solid substrates including, but not limited to, plastics, polymers, metals, alloys, ceramics, silicon, silicon carbide, quartz, sapphire, glass and other substrate materials. The application of the coating as a component. The present invention is not limited to such as reflection of metals or other reflective surfaces with a material coating based on aluminum phosphate under various exposure conditions, including but not limited to high temperature processing, UV radiation, moisture and others. It relates to maintaining the properties on the surface.

  The present invention relates to applying a coating based on aluminum phosphate as a barrier coating against the diffusion of gases, water and other fluids on various substrates. The present invention uses a precursor solution based on aluminum phosphate as a spin-on glass (SOG) material in a system having a structure consisting of narrow gaps and non-uniform surfaces (eg, semiconductor devices and optical layers). It can also be related. The present invention relates generally to the surface treatment or coating of polymer or plastic solid substrates utilizing a material composition based on aluminum phosphate. The present invention relates to a method for improving adhesion between polymers and other types of materials.

  In part, the present invention can be directed to a configured composite comprising a substrate and coating components thereon. The coating component comprises an aluminum phosphate compound having an aluminum to phosphorus ratio that can range from about 0.5 or less: about 1, about 10: about 1, about 20: about 1, or about 25: about 1. Can be included. Such a composite can be positioned about an axis that is substantially perpendicular to the configuration provided.

  In certain embodiments, the substrate is morphologically flexible so that the composite with such a coating component can then be unwound and / or unwound on a spool to produce a product. It can be. Thus, as understood in the art, such a substrate can be selected from metals, metal alloys and plastics. In certain embodiments, such metal substrates can be selected from stainless steel and brushed stainless steel. Nevertheless, as described elsewhere, the coating components of the present invention can be substantially transparent in the visible spectrum and / or provide an iridescent appearance to the composite. can do. Alternatively, such coating components can include one or more additive components or agents to provide the composite with an antimicrobial function, such agents understood by those skilled in the art who recognize the present invention. It is like that. Further, as described herein, function or action can be induced by interposing one or more intermediate components, such as interlayer components, between the substrate and the coating component.

In certain other embodiments, the substrate may comprise a plastic material comprising one or more of polycarbonate and / or copolymer thereof, polyimide and / or copolymer thereof, polyester and / or copolymer thereof. . Without limitation, other such polymeric materials are described elsewhere herein and will be understood by one of ordinary skill in the art to recognize the present invention. Regardless of the identity of the substrate, the coating component can provide a permeable barrier to moisture, gases and / or other permeates. Alternatively, with respect to the adverse effects of organic solvents, such components can provide a protective function for plastic substrates. Regardless of the functional benefit provided by the substrate, an upper layer component can be deposited on or over the coating component to provide additional functional benefits to the composite. As described elsewhere, depending on the identity of the substrate and the various compositional aspects of the coating component, the coating component includes a structural portion that absorbs radiation in the infrared spectrum at about 1230 cm ^−1. Can be confirmed.

  In certain other embodiments, the substrate component can include a metal foil. Without limitation, such substrates can be sized as required by end use applications (less than approximately 100 mils). Such a foil-like substrate can be selected from an alloy and a superalloy mainly composed of aluminum, stainless steel, titanium, magnesium and nickel. As noted above, such composites can further include various intermediate layer components and upper layer components. For example, without limitation, a metal top layer component in such a coating component can provide a reflective surface such as a mirror, benefiting such composites for use in a variety of lighting applications. give.

  For one thing, the present invention can also provide a method of using an aluminum phosphate phosphor composition to seal a porous substrate surface. Such a method provides a substrate comprising a surface component, contacting the surface component with a composition containing an aluminum phosphate phosphorous compound comprising at least one phosphate ester moiety, wherein at least a portion of the ester moiety is Heating the composition at a temperature and for a time sufficient to partially remove and / or oxidize. Without limitation, in such embodiments, the substrate can be selected from granite, marble, designed or engineered stone, porcelain, and various ceramic materials. Nevertheless, such a method can provide a substantially planarized surface component with a contact composition that is substantially thermally stable up to a temperature of about 1000 ° C.

  In certain embodiments, such compositions can be sprayed onto surface components. Depending on the particular application or processing conditions, such compositions can include at least one water-soluble carrier component, a non-aqueous elemental component, and an aerosol spray. Such components will be understood by those skilled in the art who recognize the present invention. As contemplated within the broader aspects of the present invention, such methods can be used with a variety of kitchen applications and counters, bathroom counters and equipment, floor and wall tile members, such as The compositions can be applied to them during or after manufacture of such articles.

  Enamel surfaces used in kitchen applications such as ovens are chemical complexes with various alkalis mixed with aluminoborosilicate and are susceptible to chemical reactions with various food chemicals. The reaction product strongly adheres to the surface and requires a strong cleaning solution (caustic treatment) that is inherently toxic and cannot be easily removed. Moreover, the surface has a degree of porosity that causes mechanical bonding of particles that are difficult to remove. No solution to surface treatment has been attempted due to the lack of a low cost solution that provides a stable, inert, low surface energy sealing action. The use of inventive material films as seal coats represents a key innovation for this application.

  For oven cavity applications, the baked food is difficult to clean and reduces surface porosity by at least 50% with an inventive material coating to avoid mechanical bonding to the enamel surface. It is necessary. In addition, reducing the surface energy of enamel facilitates cleaning and is similar to using a non-stick frying pan with a Teflon coating. A surface energy of less than 35 dynes / cm is desired for this type of application.

  Enamel coupons and ceramic tile studies have shown the coating ability of inventive materials to sufficiently coat ceramic or metal surfaces with sub-micron thick coatings. Mechanical bonding is considered to be the main concern for this application because it has a relatively rough surface morphology of the enamel surface. The relatively inert surface chemistry of the inventive material is expected to be stable by interacting with various food materials at high temperatures in the oven.

  Food processing equipment is a source of bacterial / biofilm adhesion and growth that can turn into a serious health problem. One reason for bacterial attachment is the roughness of the surface that promotes biofilm structure by mechanical bonding. The other is the presence of moisture. Both sources of bacterial adhesion can be eliminated using inventive material coatings and inventive material coatings with organic hydrophobic layers. Thus, an anti-bacterial coating can be formed using an inventive material coating by reducing the metal surface finish to an electropolishing level, for example, by a factor of 5. Inventive material coatings can also be used for cryomachined surfaces (in-lathe spray coatings and IR lamps). Inventive materials can also be used as abrasion resistant coatings on lenses and glass mirrors.

  Inventive material can function as a non-stick coating on polyester and other food packaging plastic substrates. As discussed below, the roll-roll coating process can be utilized with flash curing to achieve high throughput of the coated product.

  Another embodiment of the present invention is to use a low surface energy layer (eg, organometallic silane, fluorosilane, organic molecule or polymer on the inventive material coating layer). This surface layer can facilitate several methods including, but not limited to, reducing or eliminating the formation of glue-like residues from food at cooking temperatures. These overcoats can be reapplied very easily by spray technology.

Another embodiment of the present invention is the use of the inventive material as a spray product for commercial or home applications.
It is important that technical obstacles result in uniform application at the targeted film thickness (50-500 nm) using spray formulations. Most commercial spray coatings are relatively thick (several mils) and the process is not suitable for forming high quality thin films. Developing a suitable aqueous formulation, which is preferred for safety and environmental reasons, is even more difficult than an alcohol formulation. Many risks, toxicity, flammability and waste associated with the use of alcoholic precursors will be mitigated. Aqueous formulations do not provide adequate wetting properties and the aqueous formulations have poor storage stability.

  Another embodiment of the invention is a modification of the precursor to develop a suitable spray formulation. Aerosol technology is very suitable for various environments and users. Continuous, sub-micron thick deposition is our biggest challenge to the prior art. Furthermore, atomization parameters that will change based on solvent and additives, surface coverage and wetting will vary from substrate to substrate.

  Another exemplary embodiment of the present invention is the development of a solution of the inventive material in an aqueous or water-ethanol mixture. Wetting properties can be improved by increasing the polymer chain length by refluxing, thereby increasing the polymerization properties of the precursor solution. In order to further improve the wettability, a small amount of commercially available surfactant (less than 2% by weight) and / or a mixture of water / alcohol solvent can be used. Useful surfactants reduce the surface tension of water, but are chemically compatible with the precursor during curing (ease of solvent removal). Fine coatings can be applied to solid substrates including, but not limited to, enamel, stainless steel, glass, ceramics and polymers with known aerosol techniques of alcohol solutions.

  The present invention also provides an inexpensive and rapid process for processing the surface of silicon carbide optical components. This new process is suitable for various types of SiC and can be used to planarize SiC surfaces for space and ground optical systems, regardless of manufacturing technology. Due to the low melting eutectic between aluminum phosphate and silicon dioxide, the inventive material coating can planarize the SiC surface by reaction with the substrate.

  The use of a thin film of inventive material can be a significant improvement in current surface finishing techniques in terms of reducing cost and time required to planarize SiC reflections, either alone or by reaction mechanism. The surface roughness of the sintered SiC piece was reduced by 100 times (polishing to a 2.7 nm rms roughness of the 1 μm diamond abrasive surface) by an investment of about 0.5 man-hours. Furthermore, a thin coating of inventive material can be used to planarize the surface of an aluminum or silver mirror, as well as other non-optical substrates, without resorting to reaction mechanisms.

The advantages of the inventive material based on the surface finishing process are as follows.
Substantially lower cost to achieve a smooth surface (less than 10 nm rms roughness),
Reducing the time required to produce optical quality finishes,
-Applicability to many ceramic and metal optical systems, regardless of ultimate mission,
No significant investment in processing equipment would be necessary to achieve an optical quality finish,
-The deposition method of the inventive material is very simple and versatile. The precursor solution used to make the coating is low viscosity, transparent, stable (extending shelf life) and suitable for dip and spin coating methods.
The resulting surface is glassy in nature and conventional or MRF-based finishing techniques can be used to further reduce surface roughness.

  Thus, the present invention can be finished in a similar manner used for glass mirrors while taking advantage of the superior mechanical and thermal properties of ceramics such as, but not limited to, SiC and silicon nitride. An opportunity to obtain a glass layer on the ceramic surface through heat treatment of the inventive material film that can be done or through direct deposition.

Without wishing to be bound by any theory, the inventive material coating on silicon carbide appears to promote the formation of aluminophosphosilicate glass upon high temperature annealing. From the prior art it is known that there is an eutectic of the AlPO ₄ —SiO ₂ system with 70 mol% of SiO ₂ melting at 1400 ° C. After annealing at 1400 ° C., the inventive material coating applied on the sintered SiC appears to form a vitreous phase. Without wishing to be bound by any theory, the oxidation of SiC to SiO ₂ appears to give silicon dioxide to form the reaction phase. The phase on the surface appears to be glassy and lacks a crystalline shape. It is clear that the surface is considerably smoother than the initial substrate or uncoated annealed sample under an optical microscope and evaluation of the surface by SEM.

   Hexoloy SiC is polished with 1 μm diamond slurry and surface-finished on the order of 1 to 3 μm. Hexoloy SA is 99% pure sintered SiC. Hexoroy was somewhat porous compared to SiC by CVD, and these pores were effectively sealed with the inventive material coating. This substrate was coated and heat treated with the uncoated sample. After heat treatment, the coated sample has a high reflectivity and exhibits a smooth surface. As measured by AFM, the rms roughness of the coated sample was reduced to about 2.7 nm. The uncoated, annealed and finished surface maintained a very rough and relatively porous surface morphology. Without the initial polishing and coating steps and heat treatment, about 0.5 man-hours are required. (In this case, the polished silicon carbide substrate (with 1 μm diamond abrasive) was ultrasonically cleaned, dip coated with the inventive material solution, and then heat treated in a laboratory furnace.) It should not be bound by any theory For example, the aluminum phosphate present in the inventive material appears to react with silicon dioxide formed from the oxidation of silicon carbide. Furthermore, after cooling, no cracks are observed, and the glass shows a relatively good CTE match to the SiC substrate.

  In addition, the inventive material allowed excellent protection of SiC from oxidation at high temperatures. A substantial reduction in weight gain was observed in the coated material compared to the as-obtained silicon carbide after exposure to 1400 ° C. for 100 hours. By incorporating silicon into the inventive material, it may function as a silicon source to form an aluminosilicate phosphate glass composition. After high temperature annealing, some loss of phosphorus was observed, but the surface appears to be well sealed to provide environmental protection. The modified method can be used on other substrates by first depositing a SiC coating and then treating the surface with the inventive material described above by any known method including CVD. C / C and C / SiC composites used in high temperature applications need protection against oxidation. Such treatment can be viewed as enhancing the protection of these and other non-oxidative and oxidative complex systems.

  The present invention can be used to promote good adhesion between metal surfaces that may or may not produce an organic polymer coating and an oxide layer. Phosphate and aluminate groups can be covalently bonded to metal atoms at the metal surface. In addition, the coating composition of the present invention may include an upper layer of at least another organic substance or an organic silane or an organic phosphate in order to improve the bonding between the organic substance and the polymer. Alternatively, another organic or organic silane or organophosphate layer having at least one reactive site capable of binding with the organic resin may be applied separately as the other top layer. Inventive material that promotes adhesion between a relatively inert metal surface (such as noble metal surfaces such as gold, silver, platinum, palladium, iridium, rhenium, ruthenium and osmium) and an organic polymer coating. To provide an interface. The adhesion promoting effect of the inventive material coating is not limited to metal-polymer materials. This can include metal-ceramic, ceramic-polymer, glass-polymer, glass-ceramic, ceramic-glass, ceramic-ceramic and other systems as well.

  The present invention also relates to a rainbow-colored, non-rainbow-colored, anti-fogging, and highly reflective (high reflectance) coating on a surface such as stainless steel. Antioxidant coatings on stainless steel with a thickness of less than 1 micron exhibit an iridescent color due to the difference in refractive index of the substrate relative to the coated layer. Inventive material amorphous aluminum phosphate thin film coating on stainless steel is effective against oxidation at high temperatures, thus preventing fogging. They also maintain or improve the reflectivity of the coated metal surface. This coating also exhibits an iridescent color that can be utilized as a decorative coating on the article. Without wishing to be bound by any theory, the inventor believes that the iridescence observed in the coating depends on the chemistry, thickness and uniformity of the coating.

  The inventive coating material can be used with undercoats and overcoats to modify reflectivity, glow, gloss, and other optical effects for thin coatings. As the undercoat, any phosphorus material containing trivalent or tetravalent phosphorus atoms can be used. The phosphorus compound may be either organic or inorganic. The organic phosphate is not limited to an organic phosphite. For example, phosphate, phosphonate, hydrogen phosphite, hydrogen phosphate, polyphosphate, polyphosphonate, phosphate esters, Phosphate esters, phosphines, alkyl chlorophosphines, chlorophosphates and mixtures thereof can be used. Inorganic phosphates can be, but are not limited to, for example, metal phosphates, phosphoric acid mixed with a suitable solvent, phosphorus pentoxide solution, phosphorus halides, phosphorus and mixtures thereof. The overcoat can be an organic or inorganic or hybrid coating. The organic overcoat layer can be, but is not limited to, a self-assembled monolayer of organic molecules or polymers. The silane-based coating can be used as an overcoat. The inventive material itself can function as an under and overcoat. Inventive material coatings can also contain organic or inorganic additives. The inorganic additive can be a metal ion such as, but not limited to, silicon, iron, zinc and manganese and / or mixtures thereof. The nanocrystalline oxide can be, but is not limited to, for example, zinc oxide, titanium oxide, and mixtures thereof.

  Inventive material layers can be manufactured as porous bulk materials using organic templates (eg, polymers and organic macromolecules). Especially for silicon carbide which is a high temperature semiconductor and requires a thermally stable low-k dielectric layer, the designed porous inventive material as a low-k dielectric and silicon, gallium arsenide and It can be used as a coating for other semiconductors. The spin-on glass process as a process can be used to deposit inventive material layers that function as effective diffusion barriers. The porosity of the inventive material can be designed to be nanoscale so that the coating can maintain good mechanical properties. The organic content in the coating composition can be modified not only to minimize cracking for the process, but also to help improve the strength of the layer.

  By using the inventive material coating, sealing of surface defects of glass, polymers and other related substrates used in semiconductors, solar cells, flexible displays can be effectively achieved. In addition, the inventive material coating can also function as a barrier layer against diffusion of oxygen, moisture, sodium and other environmental factors.

  It is also useful for sealing defects on quartz, glass and other substrates used as photo blanks in the semiconductor industry. Inventive materials can also be etched on a submicron scale using chemical or physical methods, if necessary.

  A shiny glass coating on steel or other surfaces can enhance the aesthetic value of the surface. When coated on a metal surface, the inventive material exhibits an iridescent color. Such coatings may be applied as shapes, signs, partial labeling and many others.

  Realizing a continuous crack-free coating at the microscale level using a solution-based process is a very difficult task. More difficult with structures containing gaps and non-uniform surface structures. In the prior art, such coatings are provided by spin-on-glass coatings of silicate, borosilicate and phosphosilicate in semiconductor devices. However, they have drawbacks such as cracks and sodium diffusion and other problems. The semiconductor industry is exploring low-cost technologies that can replace existing ones with a combination of multiple properties in a single material that reduces manufacturing costs and is of equal or higher performance.

  The coating must be sufficiently thick, air tight and crack free to prevent or limit sodium diffusion. The combination of both is difficult to achieve using sol-gel coating techniques. These situations can be achieved by appropriate modification of the coating technology and the inventive coating materials. The coating must be able to planarize the coated substrate to form a multilayer film on the coating. The coating material must be stable with high breakdown strength. Using the appropriate additives, inventive materials and modified inventive material precursor compositions, viscosities and concentrations, the surface tension function of liquids that may cause problems in achieving continuous coverage or edge coating Can be minimized or eliminated.

  Inventive materials can be used as spin-on-glass coatings on substrates such as, but not limited to, quartz, silicon, silicon carbide, gallium arsenide, and other substrates. Inventive material coatings have essential properties for coatings on semiconductor devices such as, but not limited to, insulation, low dielectric constant, planarization and ion barrier. Similar coatings can be formed on any kind of non-uniform surface regardless of their surface chemistry due to the strong tacky nature of the inventive materials. The inventive material and its modified precursors can be used as both conformal and planarization coatings, depending on the coating thickness and method. Inventive material coatings can also be combined with other planarization techniques, such as MRF or CMP, if desired, to achieve a better surface. Also, the coating can protect the semiconductor device from problems due to sodium diffusion from the handling environment. Inventive and modified inventive material precursors can be used as flowable gap-filling materials using spin-on-glass technology. Thus, the inventive material can be used to produce flowable spin-on insulators. Based on spin-on-glass technology, but not limited to small products with complex shapes such as fasteners from electrolytic corrosion (e.g., steel fasteners to aluminum chassis) and decomposition from solvents, chemicals and other environmental attacks. To protect, it can be coated with inventive material.

  Metal and polymer foil substrates can be used in a variety of applications including displays, photovoltaic devices, heat shields and others. Thermally stable coatings of inventive materials can be continuously deposited on these substrates to provide desirable properties. The multifunctionality of the inventive coating material can provide significant benefits over prior art materials at low processing costs and high throughput. For example, the inventive material can be deposited to provide electrical insulation and provide a smooth surface. This avoids the expensive PVD or CVD process commonly used to deposit an alumina layer with an additional coating layer that is required to provide sufficient flatness. For the food packaging industry, the inventive material can be deposited on a plastic substrate in a continuous roll-roll process, giving the food non-stick properties. Inventive materials also provide suitable barrier properties against gases diffusing into or out of the food packaging material.

  Vacuum-based coatings inherently contain pinholes and other defects due to the processing method. Inventive material coatings of vacuum-based thin films can eliminate these defects and can effectively increase the barrier properties of the coating. Furthermore, the inventive material coating can serve as a planarizing template to produce other types of coatings.

  Devices, especially micro and nanofluid devices, include blow molding, dip molding, film insertion molding (FIM), gas assist molding, reaction injection molding, resin transfer molding, rotational molding, SF molding, thermoplastic injection molding, vacuum assist molding, A mold is used that is molded from a plastic material by compression molding, stretch blow molding, thermoforming, UV reaction molding or embossing or other molding methods. These devices find application in various fields such as, but not limited to, biomedical devices, optical communication systems (some diameters are 1 mm or less, tolerance is 1 μm or less) and others. Micro-optics with nanostructured surfaces, complete transparency and long-term automotive windows with long-term resistance to friction are at the forefront of plastic processing technology. Microfluidic lab-on-a-chip systems have great potential for many laboratory applications, including clinical diagnostics and life science research. Various devices have been developed that are very suitable for handling the difficult requirements of actual clinical samples such as whole blood and other body fluids. The device can be used in a stand-alone application as a self-contained passive disposable product for quantitative and semi-quantitative analytical and separation applications, or they can be used as a component of advanced instrument systems. Can do.

  Rapid and effective release of molded parts from the tool is key to any efficient molding process. During processing, high temperature resins (eg, polyetherimide) may reach temperatures above 700 ° F. that cause the degradation of many standard release additives. New high temperature mold releases require the opening of process windows to allow for better regeneration on some surfaces and rapid mold cycles with some low slopes. The molding surface includes metal, silicon and others.

  Plastic processing also requires that the mold release the coating used in the permanent mold. Other objectives are better coatings for wear resistance, corrosion resistance and improved resin flow. A successful coating results in improved partial release and partial quality, protection of the mold against wear from rough materials and reduced deposition build-up, allowing faster mold cleaning. Also, considerable economic benefits are obtained by eliminating downtime due to improper working machine parts such as partial sticking to the mold, breakage of the ejector pins, and backflow valves. The net effect can reduce cycle time and make maintenance intervals longer.

  For example, a P-20 mold with a hardness of 40 Rockwell C and a perimeter of 12 cavities every 18 inches is suitable for Teflon nickel layer, lapping compound and wire brushing and pre-release application per shot Regardless, it is a molding part that is difficult to release. Furthermore, it involves the worker manually and cautiously pulling it away from the mold in the final step in the 72 second cycle while trying to avoid causing any distortion or warping. Peeling from parts is time consuming and has proven to be expensive. The scrap rate varied from 30 to 40 percent. It has been found that a 6 μm finish on the tool surface is necessary for this type of speaker grid application that releases automatically. Using conventional EDM technology, it is possible to achieve a finish of only 12 to 14 μm after 150 hours of finishing work. After 150 hours, any better surface finish could be achieved.

  Inventive material technology may be effective as a permanent release coating. Inventive materials can benefit from reduced surface roughness below 6 μm with very little work and cost required for conventional polishing techniques. Along with reducing the surface roughness, the surface energy of the coated surface can also be reduced with an organic overlayer that can be self-assembled or overlying itself. Improved energy and finishing with inventive material coatings on 12 micron surfaces can be very beneficial to the plastic and microfluidic industries. Various materials such as polymers, metals, alloys, high temperature stable polymers, etc. are used during molding depending on the application requirements.

  A military aircraft window, whether it is a jet fighter canopy or an infrared sensor cover, resists being bombarded by debris at high speed, allowing pilots to look out or reach infrared signals In addition, it must be fairly robust in order to maintain sufficient transparency. Conventional yttria windows tend to crack depending on flight conditions. Inventive materials can be used as media to disperse such nanoparticles and apply as a coating at high loads. This can be used as a cost effective method for infrared store scanners and other application coatings. It also helps extend the life of the canopy with jet fighters.

Various other uses and applications of the present invention include:
Inventive material coatings can be used in the thermal spray coating industry. For example, the inventive material can be used as an osmotic sealer for spray coating of MCrAlY-based turbine blades and as a feedstock for cold spray coating applications.

With or without a hydrophobic overphase, the inventive material coating can be used as a low-wetting windshield coating.
Low temperature amorphous inventive material coatings / Al ₂ O ₃ coatings can be used in various fields including, but not limited to, electronics, textiles and polymers.

The inventive material can be used as an anti-catalytic coating for Ni-rich components used in systems handling hot gases.
The material of the present invention can be used as a wetting agent for powder metallurgy constituents (sintered product curability).

Inventive materials can be used as coating compositions in fuel cells and gas reforming parts (hot surfaces).
Inventive material coating on metal can be used as an interfacial layer for improved adhesive with corrosion protection and improved lacquer adhesive.

  Inventive material coatings are also useful for photoelectric and other sensors in terms of their low dielectric constant characteristics. Electrically insulating inventive material coatings require the design of solar cells on metal foils. The inventive material coating serves as a protective layer between the solar cell electrical back contact and the conductive substrate.

The thickness requirements for inventive material coatings will vary depending on the application.
The following table lists the applications along with practicality and required non-limiting layer thicknesses.

Applications / Layer thickness High reflection and antireflection coating optical layer laminate / 10 nm to 200 nm
Transparent gas barrier coating on plastic web / 30nm-100nm
Abrasion resistant coating on polycarbonate sheet / 4-6 microns
Interfacial layer for improving adhesion (some substrates) / 5 to 20 nm
Conversion layer on steel (corrosion prevention, lacquer adhesion) /0.3-0.4 micron Dielectric coating (sensor, solar cell backside protection) / 2-5 micron It can be very beneficial to adjust the properties. For example, glass slides manufactured by different companies may not have the same composition. Different batches of slides may not necessarily match, even from the same manufacturer. For example, the surface roughness may vary depending on the processing that these samples have undergone. For example, having almost the same surface characteristics in a sample such as a microarray is very important for some applications. Inventive material coatings can provide uniform surface features (eg, uniform surface chemical uniform surface roughness, etc.).

Metals and alloys (eg, titanium, Ti ₆ Al ₄ V, CoCr) are widely used as materials for orthopedic tissue due to their superior mechanical properties and non-toxic behavior. High strength and fatigue resistance and effectiveness, ease of processing and low cost prove the important role played by metals in implant dentistry. These metals may integrate with surrounding structures, especially hard structures, alloys. Special importance is given to titanium and its alloys and CoCr alloys in order to show chemical and mechanical bonding and to show good biocompatibility / histocompatibility and biofunctionality. Differences in corrosion and high rates influence the choice of graft material, especially because fretting disease contributes strongly to the generation of wear particles that may lead to particle disease and subsequent graft detachment. Also, the affinity of metal surfaces for microbial contaminants and biofilms is a significant problem. The rate of transplanted tissue infection requires risky implant replacement, and even a good clinic may reach 2% to 3%. Careful design for initial implants and implant replacements faces problems of stress shielding and bone line loss. In most prior art, the coating is cracked and the glass-metal interface is unreliable. Therefore, a coating that adheres strongly, is protective and biocompatible would be very beneficial.

  In the prior art, various methods have been developed to modify the surface of polymers, metals and alloys or other biocompatible materials used in the device industry. Examples are conventional coating processes (eg spraying or dipping), vacuum deposition techniques, surface modification techniques such as diffusion, laser and plasma processes, chemical plating, grafting or bonding, hydrogel encapsulation and high energy particle bombardment. Is mentioned. In general, it was an objective to achieve improved physical or mechanical properties in a part or device, for example by adding a non-adhering coating to the catheter for easier insertion. Increasingly, however, surface modification is aimed at inducing certain desirable biological responses or preventing potential side effects. Low friction, hydrophobic, hydrophilic or other functionalized coatings are used to treat carotid and biliary obstruction, peripheral vascular disease, invasive for use on carotid stents, guidewires, catheters, etc. There is a need for instruments, products and accessory coatings.

  The present invention relates to developing protective, functional, biocompatible coatings based on inventive materials. Inventive material compositions can be tailored to meet the need for coating on medical devices and implants. Inventive material coatings on metal or polymer substrates can significantly reduce the coefficient of friction. After coating and curing, the surface of the inventive material is either hydrophilic or hydrophobic. By using a self-assembled organic layer or organic layer coating on the inventive material coating, appropriate functionality can be provided. Hydroxyapatite or other bioactive nanoparticles can be incorporated into the inventive material coating to improve biocompatibility. A bioactive layer, such as hydroxyapatite, can be deposited using vacuum, plasma or sol-gel based coating techniques. In this case, the inventive material coating can act as an adhesive layer that improves the adhesion between the metal or polymerized medical device substrate with the bioactive material.

  Inventive material coatings can effectively prevent or reduce devitrification from reaction of fused silica or quartz and other amorphous materials used in surgical probes, lighting products, etc. with alkali or other species, for example. .

  Boundary lubrication is known to enhance the lubrication properties of many systems. The present invention addresses the deposition of alkyl fluorosilanes on inventive material coating surfaces and the stability of such organic layers. A smooth surface is highly desirable for low friction properties, but requires considerable surface preparation, and the presence of surface defects, such as pits on the alloy surface, limits the quality of the surface finish. A good adhesion, abrasion resistant coating that can planarize the surface is very useful for tribological applications. The inventive material film can prevent corrosion of the substrate from both the lubricating oil and the atmosphere. The hermetic inventive material coating can protect the substrate from lubricants and corrosive species present in the atmosphere.

  Inventive material coatings on materials such as polymers a) good protection against light irradiation (eg UV irradiation), b) good protection against acids, alkalis, organic solvents and other chemicals, c) The coating properly seals the defects (eg pits) on the polymer surface and coats the particles so as to flatten the coated surface and reduce the surface roughness, d) inert gases (eg oxygen, nitrogen, hydrogen) Against chemical active gases (eg water, carbon dioxide) and good barriers to liquids and vapors (eg atoms, fine chemicals, gasoline), e) atomic oxygen, nitrogen, oxygen, hydrogen and low earth orbits Good barriers to other elements found in or developed in the laboratory, f) polymers originating from various sources (eg routine handling materials, impact with high speed materials, etc.) Good protection against surface mechanical damage, g) good protection against oxidation, h) good protection against corrosion, i) good protection against moisture, j) used in medical applications against corrosion from body fluids, chemicals and microorganisms Give good protection of the biomedical polymer obtained, k) reduce the coefficient of friction of the polymer surface by planarization and l) increase the abrasion resistance of the coated polymer surface. Of these, if not wishing to be bound by theory, suitable and innovative properties are dense, continuous, smooth, strong, sticky inorganic, mainly inorganic or inorganic-organic composites Inventive material's ability to promote the formation of body coatings.

  For examples of polymers that form plastic films or substrates, cellulose esters (eg, triacetyl cellulose, diacetyl cellulose, propionyl cellulose, butyryl cellulose, acetyl propionyl cellulose, nitrocellulose), polyamides, polycarbonates, polyesters (eg, poly (Ethylene terephthalate), poly (ethylene naphthalate), poly (1,4-cyclohexanedimethylene terephthalate), polyethylene-1,2-diphenoxyethane-4,4′-dicarboxylate, poly (butylene terephthalate)), Polystyrene (eg, syndiotactic polystyrene), polyolefin (eg, polypropylene, polyethylene, polymethylpentene), polysulfone, poly (ethers) Hong), polyarylate, poly (ether imide), poly (methyl methacrylate) and poly (ether ketone) is. Triacetylcellulose, polycarbonate, poly (ethylene terephthalate) and polyethylene naphthalate) are preferred. Examples of the packaging material made of polymer include polypropylene PP, polyethylene PE, polyamide PA, PET, and laminated films made of various polymer materials (eg, PP / PE, PET / PP, PET / PE, PE / PA). .

  Plastic layers used in flexible display devices include, for example, polyester, polycarbonate, polyvinyl butyrate, polyethylene and substituted polyethylene, polyhydroxybutyrate, polyhydroxyvinyl butyrate, polyetherimide, polyamide, polyethylene naphthalate, It can be made from polyamide, polyether, polysulfone, polyvinyl acetylene, transparent thermoplastic, transparent polybutadiene, polycyanoacrylate, cellulosic polymer, polyacrylate and polymethacrylate, polyvinyl alcohol, polysulfide and polysiloxane.

  The substrate can also be in the form of a laminate, and the plastic layer of the composite is coated on the glass layer by any suitable method. That is, (i) the plastic already exists as a film and is laminated to the glass, and (ii) the plastic is not in film form but may be in a different state coated on the glass by dipping, spraying and other methods. Is possible. The prepolymer described above follows, for example, the case of (ii). However, some of the other plastics mentioned above may be coated for case (ii). In this example, the polymer can be coated on glass substantially by coating from solution, melt or prepolymer.

  The substrate can also be any organic material, desirably an organic polymer, that has high temperature thermal stability. The polymer may be a thermoplastic or thermosetting material, desirably a high temperature thermoplastic material (eg, polyimide, polyamideimide, polyetherimide, bismaleimide), fluororesin (eg, polytetrafluoroethylene), ketone-based resin, polyphenylene. Sulfides, polybenzimidazoles, aromatic polyesters, and liquid crystal polymers may be used. Furthermore, polyolefins, in particular crystalline high molecular weight types, can be used.

  Curing can occur by any method that can condense and result in the formation of Al-O-Al, P-O-Al groups. For example, heat treatment, exposure to UV light at the relevant frequency, increasing the pH of the solution to 3 or higher, exposure to IR radiation, exposure to microwave radiation, exposure to chemicals capable of hydrolyzing P-OR groups Addition of appropriate chemicals that can increase the condensation rate or any combination of the above methods.

  The adhesion of inorganic coatings to polymers is a significant problem that limits the use of coatings reported in the prior art. Measuring adhesive strength with a tape test was performed on polyimide samples coated with inventive material (similar to ASTM D-3359 test). 3M ™ Scotch ™ tape was applied over the coating and then peeled off quickly. There was no removal of inventive material on the polyimide film or loss of adhesion. Optical cracking of the polyimide coated with the inventive material after bending to 180 ° did not show any cracking of the coating. These results show the strong adhesion of Cerablak ™ on the polymer. Phosphate-based coatings are known to exhibit strong adhesion on polymers. For example, calcium phosphate on polyethylene and poly (tetrafluoroethylene) showed adhesive strengths of 6.4 and 5.8 MPa, respectively. Without wishing to be bound by any theory, it is believed that strong adhesion is due to the formation of C—O bonds between the phosphate groups and the polymer interface during coating curing. The adhesive strength can be improved by pretreating the substrate with Ar ions. The precursor solution of the inventive material is slightly acidic but does not damage the acid sensitive polymer substrate surface during the coating process.

  The organic group that binds to phosphorus in the precursor solution can be reduced or eliminated completely by replacing the P-OR group with a P-OH group. However, any chemical changes in the precursor solution may affect condensation and thin film formation. In some embodiments of the inventive precursor solution, an aluminophosphate complex with a characteristic [O = P—O—Al—O—Al] bond can be retained. If one does not wish to be bound by any theory, the organic content can be significantly reduced by increasing the relative content of the “P—OH” species. In addition to using water or other non-alcoholic chemicals as the solvent, the organic content can also be reduced using configurationally hindered alcohols (eg, isobutyl alcohol as a solvent for aluminum nitrate). it can. The reaction rate of isobutyl alcohol by the aggregated phosphate (P—O—P) group is low. Even if P-O-i-Bu groups are formed in solution, they can be removed at reflux, forming 2-methylpropene (boiling point: 6.6 ° C.), a gas at room temperature.

  Wetting of low surface energy polymers with alcohols is a challenge. Adhesion is a concern because high cure temperatures may be necessary to improve adhesion. In the case of a polyimide film, the inventive material coating adhesion force is good without any surface treatment. If the coating adhesion to any polymer is weak, modification of the polymer surface can be employed. Several techniques, primer deposition, use of surface assembly monolayer SAM, oxygen plasma etching and sulfochromic bath treatment can be used to improve wetting. Inventive material coatings can also be used with other metals, for polymers and inorganic coatings, layers that promote primer or adhesion.

The lower and upper layers can be selected from any organic polymer coating, inorganic-organic composite coating, or metal coating. These layers can also be formed from the same inventive material with different compositions. These layers can also be formed by inventive material precursors modified with any inorganic or organic functionalizing agent. For example, UV absorbers for UV radiation protection, scatterers such as ZnO, CeO ₂ , TiO ₂ , Ag ions for antibacterial activity, transparent metal oxides such as ITO for electrical properties, mechanical properties Examples include photocatalytic species such as SiO ₂ , Al ₂ O ₃ , ZrO ₂ for improving TiO ₂ or TiO ₂ for imparting hydrophilicity. Several layers of these lower layers and upper layers can be formed as needed. Inventive material coatings can planarize the polymer surface with an appropriately modified refractive index, helping to reduce light scattering from the coated polymeric substrate.

  The following non-limiting examples and data illustrate various aspects and features relating to the composites, products and methods of the present invention, including the use of various aluminum phosphate compounds and related compositions therewith. That is obtained through the synthetic methodology described herein. Compared to the prior art, the compositions, composites, products and related methods of the present invention are unexpected and provide unexpectedly contrasting results and data. While the usefulness of the present invention is illustrated by using several composites / products used therewith and coating compositions based on aluminum phosphate, the corresponding results have been demonstrated with various other composites / It is well understood by those skilled in the art that it can be obtained in products and coating compositions. This corresponds to the scope of the present invention.

Example 1
One preferred method of depositing the amorphous aluminum phosphate coating uses a transparent chemical precursor solution, preferably a solution comprising an aluminum salt and a phosphate ester in an organic solvent. Aluminum: phosphorus ratio of 2: A solution used to deposit the first amorphous aluminum phosphate coating is prepared by 264g dissolving _{Al (NO 3) 3 · 9H} 2 O in 300mL ethanol. In a separate container, dissolve 25 g of P ₂ O ₅ in 100 mL ethanol. Mix these solutions. The resulting solution is diluted with ethanol to a concentration of 0.2 molar Al / L solution. This solution is used to deposit amorphous aluminum phosphate on the substrate.

Example 2
Aluminum: phosphorus ratio of 4: A solution used to deposit the first amorphous aluminum phosphate coating is prepared by 528g dissolving _{Al (NO 3) 3 · 9H} 2 O in 300mL ethanol. In a separate container, dissolve 25 g of P ₂ O ₅ in 100 mL ethanol. Mix these solutions. The resulting solution is diluted with ethanol to a concentration of 0.2 molar Al / L solution.

Example 3
The stainless steel plate was cleaned with detergent and water followed by ultrasonication in methanol. It was immersed in the solution prepared in Example 1. Dry using a heat gun. The dried sample was heated for 1 minute at 400 ° C. and cooled to room temperature. The hardened stainless steel surface showed a strong iridescent color. This type of inventive material coating can be applied as a decorative coating on articles.

Example 4
The stainless steel plate was cleaned with detergent and water followed by ultrasonication in methanol. Subsequently, it was immersed in the alcohol solution containing a phosphoric acid and aluminum mixture. Next, it was dried using a heat gun. The dried sample was heated for 1 minute at 400 ° C. and cooled to room temperature.

Example 5
The IR absorption spectrum of the sample produced in Example 4 was recorded with a Perkin Elmer Spectrum One Spectrometer using an 80 ° grazing angle accessory (FIG. 1).

Example 6
An overcoat of the precursor solution prepared in Example 1 was applied by dip coating on the sample prepared in Example 2. The sample was then heat treated for 15 minutes at 500 ° C. and cooled to room temperature. The uncoated part of the plate changes color due to oxidation. The coating was shining and kept silver. Precursor solution concentration, composition and coating state are strongly dependent on the surface morphology of the coated surface. Thus, the iridescent effect of the inventive material coating may be removed by appropriate modification of the precursor and coating methods.

Example 7
The IR absorption spectrum of the sample produced in Example 6 was recorded with a Perkin Elmer Spectrum One Spectrometer using an 80 ° grazing angle accessory (Figure).

Example 8
A fingerprint trace was formed on one surface of stainless steel coated with the inventive material by pressing the thumb against the surface. A clean cloth was then used to wipe the traces. The thumb trace could be removed from the coated surface very easily, leaving an aesthetic, pleasant, clean surface. Using similar cleaning methods, fingerprint traces could not be removed from the uncoated surface.

Example 9
The effect of resisting coloration of inventive material coatings on solid substrates is demonstrated in this example. Inventive material covers various materials (eg ketchup, H ₂ O + NaCl, tomato, lemon, tea, coffee, milk, acetic acid, citric acid 20%, lard + oleic acid, jam, butter, olive oil and other items) It was attached to a stainless steel coupon and dried at room temperature and 90 ° C. It was then washed with water and subsequently examined for any stains visually attached to the coated surface. The surface coated with the inventive material did not show any dirt.

Example 10
A pencil hardness test was performed on the stainless steel sample coated with the inventive material prepared in Example 5. The pencil hardness was observed to exceed 6H.

Example 11
The reflectance of the surface coated with the inventive material was measured before and after heat treatment at 700 ° C. The reflectivity was maintained at the coated surface compared to the uncoated control sample.

Example 12
A small sample of crystalline alumina (sapphire) was washed with deionized water, acetone and methanol. It was then dip coated using the precursor solution prepared in Example 2 (4: 1 Al: P ratio). The drawing speed of the dip coat is 2 cm / second. Then, it was cured at 800 ° C. for 10 minutes. A clear coating was obtained.

Example 13
The TEM image of the inventive material coating on sapphire shows an airtight, dense and uniform inventive coating (FIG. 3). Electron diffraction patterns obtained from inventive material coatings exhibit coating amorphous properties. The inventive material film is uniform with a film thickness of 140 nm or less. High resolution TEM showed typical amorphous contrast in the film. There is an interface layer (5 nm or less) between the inventive material and sapphire.

Example 14
In tests of enamel coupons partially coated with inventive material, tomato sauce cured at 300 ° C. for 15 minutes was compared in the coated area using only water and a soft cloth compared to the uncoated area. This shows that it was easily removed (FIG. 4). This residue appeared to bind well to the substrate when observed under an optical microscope.

Example 15
The 1 μm polished uncoated SiC surface after heat treatment and the SiC coated with the inventive material showed a reflective surface compared to the uncoated (FIG. 15).

Example 16
The AFM image of SiC coated with the inventive material and heat treated showed a very smooth surface (FIG. 6).

Example 17
Based on the hermetic properties of inventive material films observed for several metals, alloys and glass substrates, it is expected that inventive materials will be quite useful in sealing microscale surface defects on polymers. The FIG. 7 shows an AFM image of a metal alloy surface coated with an inventive material that exhibits a significant planarization effect induced by the film. A reduction of 4X in surface roughness is seen in the presence of the film.

  Micron scale surface defects on the metal surface (even after micron finish polishing) are used as the starting site for oxidation. These small surface defects are used as a starting point for oxidation as the metal substrate is oxidized during high temperature oxidation. These small defects become large pits. However, these defects are covered by sufficiently depositing a relatively thin inventive material film so that pitting is essentially eliminated. These results show the potential of the inventive material for sealing micron scale defects (scratches, pits, etc.) on the coated surface.

Example 18
A copper block 1 × 3 diameter was cleaned by sonication in acetone and methanol. It was then dip coated in the inventive material precursor solution. It dried in the air and heat-processed for 15 minutes in a 200 degreeC oven. The action of the inventive material coating after this heat treatment is shown in the photograph (FIG. 8). The parts coated with the inventive material remain bright and shining. On the other hand, the uncoated side is completely cloudy. Similarly, copper, brass and other metal wires can be coated with inventive materials and can be protected against oxidation and environmental damage.

Example 19
An AFM image of a slide glass coated with the inventive material is shown in FIG. 9 along with the uncoated glass. The surface coated with the inventive material is very smooth and the rms roughness is on the order of magnitude less than uncoated glass.

Example 20
Formation of a crack-free coating of ceramic material on the polymerized substrate is a technical challenge due to the large thermal expansion coefficient mismatch and the heat sensitive properties of the polymerized substrate. In particular, if the coating cures at high temperatures, the remaining thermal stress will cause the film to crack. This can be minimized if the coating thickness is kept to a minimum and the adhesion energy of the membrane to the substrate is increased. Both of these forms of the inventive material can be achieved because of the low viscosity and the phosphoric acid based precursor solution which is easily decomposed by thermal decomposition at relatively low temperature. An optical image of the inventive material coating on the polyimide composite showed a planarizing effect on the coated surface. Inventive materials also cover defects and make the surface airtight without creating such gaps.

Example 21
Polyvinyl pyrrolidone, PVP (MW 630000) was dissolved in the precursor solution of inventive material prepared in Example 2. The amount of PVP in the solution can vary from 0 to 100% by weight. The concentration of the solution increases with increasing PVP content. Alternatively, the solution can be prepared directly by mixing PVP with Al (NO ₃ ) ₃ and P ₂ O ₅ solutions. Other molecular weight PVPs can also be used.

Example 22
A polycarbonate sample (1 × 1 diameter) was immersed in a chromium sulfide bath for 30 seconds. It was then washed with a large amount of deionized water. Subsequently, dip coating was performed with the precursor solution of the inventive material prepared in Example 2. The coated sample was dried with a heat gun. Subsequently, it heat-processed in 130 degreeC oven. After curing for a while, a clear coating was formed.

Example 23
A polycarbonate sample (1 × 1 diameter) was immersed in a chromium sulfide bath for 30 seconds. It was then washed with a large amount of deionized water. Subsequently, dip coating was performed with the precursor solution of the modified inventive material prepared in Example 3. The coated sample was dried with a heat gun. Subsequently, it heat-processed in 130 degreeC oven. After curing for a while, a clear coating was formed.

Example 24
The methyl ethyl ketone solution was dropped onto the surface of the polycarbonate film coated with the inventive material prepared in Example 5. No reaction with polycarbonate was observed. This suggests the ability of the inventive material coating to protect against chemicals and its good barrier properties.

Example 25
Nano-sized zinc oxide particles dispersed in a medium were mixed with the inventive precursor solution prepared in Example 2. The amount of zinc oxide can be varied. Alternatively, the solution can be prepared directly by mixing zinc oxide with Al (NO ₃ ) ₃ and P ₂ O ₅ solutions.

Example 26
To measure the curing state of the inventive material coating, the FTIR reflectance spectrum of the stainless steel foil coated with the inventive material was recorded as a function of temperature and heat treatment time (FIG. 10). The intensity of the organic absorption peaks for phosphate esters (1370, 1432, 1473 1720, 2987 cm ⁻¹ ) is reduced and a single strong absorption for fully bound PO ₄ groups is observed at cure temperature and time. It appeared in the vicinity of 1200 cm ⁻¹ with the increase. As the curing temperature increases, the required heat treatment can be shortened. Based on FTIR data, a cure temperature of 325 ° C. is necessary to obtain a complete inorganic coating with some water. A crack-free coating was obtained by curing the polyimide coated with the inventive material up to 340 ° C. The curing temperature and stability of the coating can be varied depending on the nature, thickness and pre-treatment morphology of the substrate. The curing temperature can be varied according to the composition of the precursor solution of the inventive material. FTIR data of samples heat treated at 200 ° C. for a longer time will show that the coating is sufficiently dense and airtight even when cured at 200 ° C. It is interesting to note that there was a slight change in the residual moisture content in the coating. According to this study, a curing temperature of 200 ° C. must be sufficient as it forms a protective coating on the polymer. However, higher temperatures will give better adhesion and better airtight quality.

Example 27
A clean stainless steel foil was coated with the precursor solution prepared in Example 1. The sample was heat treated for several seconds in a furnace above 800 ° C. The grazing angle infrared reflection spectrum of the flash cured inventive material coating shows the absence of organic and water molecules and the formation of a fully cured inorganic metal phosphate layer (FIG. 11). During this flash curing process, the surface coating reaches a temperature above 500 ° C, while the substrate is below 250 ° C. This flash cure technique is preferred for certain coating processes (eg, roll-roll, etc.) and heat sensitive substrates such as polymers.

Example 28
Polyimides are classified as organic resins and are used in engineering applications due to their special thermal and chemical resistance. In the semiconductor industry, these materials are used primarily for flexible printed circuit substrates and as substrates for integrated circuit applications in the wireless, digital and computer industries. The surface finish of these materials has a direct impact on their performance and it is therefore important to optimize their morphology. Inventive material is coated on a cleaned polyimide film and cured at 300 ° C. for 1 hour. The SEM image of the polyimide film coated with the inventive material showed the crack-free properties of the coating. Also, the particles on the polyimide surface are coated with an inventive material coating.

Example 29
Reduction of UV absorption by 40% addition of nanoscale ZnO (less than 10 mol%) to inventive material coating. This example demonstrates the effect of adding a UV absorber to the inventive material. UV-visible transmission spectrum of ZnO dispersed in inventive material and inventive material coated on a sapphire plate (FIG. 13).

Example 30
Inventive material coatings or quartz glass products containing surface treatments can prevent silicate reactions in the environment for utility. The results of this example show this effect of the inventive material coating on the fused silica sample. Fused silica samples were partially coated with the inventive material and treated with sodium sulfate at 900 ° C. for 15 hours. Under this processing condition, the uncoated fused quartz becomes opaque due to reaction with sodium ions, the parts coated with the inventive material remain transparent, and the barrier of the inventive material coating against sodium ion diffusion. The effect is shown (FIG. 14).

Example 31
Inventive material embodiments can be used as chemically or thermally stable binders or adhesives. In these experiments, the modified precursor solution was applied to one surface to be bonded and the other surface was pressed first to make sure that the precursor solution had sufficiently covered the two pieces to be bonded. The two pieces were fixed together and heat treated to form an inorganic material. The manufactured joints showed a relatively good bond strength considering the low level of effort in these preliminary experiments. The phosphorus content will affect both permeability and adhesive strength. The phosphorus-rich composition of the inventive material showed some absorption in the IR range due to its relatively high phosphorus content, but the binding may be stronger. Binding experiments were performed on glass and stainless steel coupons. The glass had a very smooth surface, while the steel had a # 3 finish. These experiments demonstrated that inventive material-based adhesives can bond substrate materials with different surface finishes.

  To provide further evidence of a direct link to this application, a sapphire plate (rectangular) was bonded to a ZnS disk coupon. The bond was annealed at 450 ° C. in air for 1 hour to test the thermal stability of the joint. The material maintains a good bond and suggests the strong properties of the inventive material adhesive. In the transmission spectrum measurement of the binding pair, the transmittance at 6 μm or more is decreased due to the opacity of sapphire, but good transmittance is shown at 3 to 5 μm (FIG. 15).

Example 32
Inventive materials can be synthesized with a wide range of Al / P ratios (eg 0.5 / 1 to 10/1 and 25/1) including the addition or doping of other elements (eg silicon) It may be necessary to induce the functional properties of As shown in FIG. 16, in the comparison of the permeability of two inventive material films of various compositions on ZnS, an Al / P ratio of 6/1 indicates that silicon addition (silicon dioxide also absorbs around the same region) It can be seen that it exhibits negligible phosphate absorption compared to a relatively phosphate rich composition. However, since good adhesion is provided by the phosphate species, it may be necessary to find a balance between permeability and high adhesion strength. In this way, the inventive material system allows for flexible configuration variations to rework special properties.

Example 33
Applications for coatings on polymers

実施例３４
１以上の上述又は実施例に関して、種々の複合体及び／又は製品要素を、公知のロール−ロール又は連続的製造方法を用いて製造することができ、この発明を認識する当業者に理解されるであろう。従って、上述したリン酸アルミニウム組成物のコーティング及び組み込まれた引例の方法（例えば、Cerablak（商標）化合物及び製品、アプライド・シン・フィルム・インク、エバンストン、ＩＬ）を、広範囲にわたる基材材料に適用することができる。そのような器材装置及び構成は、米国特許第６，９５１，７７０号及び第６，８７８，８７１号でより完全に記述されている（それぞれ全趣旨を参照することによりここに取り込む）。

Example 34
With respect to one or more of the above or examples, various composite and / or product elements can be manufactured using known roll-roll or continuous manufacturing methods and will be understood by those skilled in the art who recognize this invention. Will. Thus, the coating of aluminum phosphate compositions described above and incorporated reference methods (eg, Cerablak ™ compounds and products, Applied Thin Film Ink, Evanston, IL) can be applied to a wide range of substrate materials. Can be applied. Such equipment devices and configurations are more fully described in US Pat. Nos. 6,951,770 and 6,878,871, each incorporated herein by reference in its entirety.

  Optionally, the substrate is first degreased with a suitable organic or aqueous solution (eg, alcohol or detergent / water) using one or more spraying or dip coating methods, first removing the stripped surface debris. Water and / or alcohol rinsing can be performed. A drying oven (at a temperature range of about 50 ° C. to 500 ° C.) can be used to remove all the solvent, using a stream of air, dry air, oxygen, nitrogen or any other inert gas it can.

  As indicated above and / or in the incorporated citations, the precursor solution of the aluminum phosphate composition can be sprayed onto the substrate. Alternatively, the substrate can be immersed in one or more tanks or storage tanks of the precursor solution. Where both many or all sides of such a substrate are coated, one or more spray nozzles can thus be constructed. Alternatively, all substrate sides can be coated with dip coating. The precursor composition is not limited and can vary with respect to Al / P stoichiometry, viscosity, support (eg, aqueous or non-aqueous) and presence of additives (either organic or inorganic). For example, a slurry can be made with a solvent (aqueous or non-aqueous) carrier component since it may be advantageous for high emissivity coatings.

  In view of various volume and throughput requirements, the coating composition can be cured in one or more ovens or heating / curing sources for lengths up to about 100 feet or more. For example, a sufficiently long oven or furnace that can be dried and cured according to a set schedule is effective at about 50 ° C. to 1000 ° C., depending on the rate and length of the heating / curing zone in which the residence time is effective. A temperature range can be given. Such bands can be varied with one or more sources (e.g., UV / IR, air, etc., a heated stream of inert gas or a resistance heating source).

  The cured applied coating can be cleaned with a suitable solvent and then dried prior to subsequent coating application. Alternatively, it can be used in composites or high-throughput systems consisting of temperature sensitive substrates (eg, certain plastics), and curing is sufficient for coating effects without detrimental impact or action on the substrate. Using a suitable heat source in a manner that allows the coated component to be heated at a relatively high temperature while maintaining the substrate at a relatively low temperature (eg, less than about 250 ° C.) for a time (eg, within about 1 hour) It can be carried out.

  Because of various process related considerations, it may be desirable to roll the substrate at a right angle before being moved with or by the heating / curing source. If the substrate is fairly wet or uncured, coating damage from bending will be minimal. Depending on the initial surface roughness, the substrate can be electropolished or mechanically polished as understood in the art prior to cleaning and coating application. Nevertheless, for further explanation of the roll-roll / continuous coating process, it is carried out as in FIGS. 17 and 18, resulting in a non-limiting wound or roll composite form.

6 is an FTIR image of the sample produced in Example 4 showing absorption peaks corresponding to phosphate and water groups in the coating. 7 is an FTIR image of the sample produced in Example 6 showing absorption peaks corresponding to phosphate and water groups in the coating. 2 is a cross-sectional TEM image of an inventive material coating on sapphire showing airtight, high density and uniform properties. The electron diffraction pattern corresponding to the inventive material coating exhibits amorphous properties. Figure 2 is a photograph of an enamel coupon partially coated with inventive material after a food-adhesion test. 1 μm polished (left) uncoated silicon carbide surface and photograph of SiC coated with inventive material after heat treatment (right), showing the reflective surface. Figure 2 shows an AFM image of heat treated silicon carbide coated with inventive material. 2 shows an AMF image of a heat treated metal alloy coated with an inventive material. 2 is a photograph of a copper plate partially coated with the inventive material. Shown are uncoated glass (rms 1-2 nm) (left) and inventive material coating (rms 0.1-0.2 nm) (right). Figure 5 shows the FTIR spectrum of the inventive material coating on stainless steel as a function of the temperature length of the heat treatment at 200 ° C. Figure 3 shows an FTIR spectrum of an inventive material coating flash cured on a stainless steel foil. It is a SEM micrograph of the surface coat | covered with the invention material of the polyimide film. Figure 2 shows the UV-visible absorption spectrum of an undoped inventive material and a zinc oxide particle diffusion inventive material coating. Fig. 3 is a photograph of a molten quartz sample partially coated with inventive material, showing the barrier effect of the coating against environmental attack. It is a transmission spectrum of a sapphire / ZnS bond pair. The reduced transmission above 6 μm is due to sapphire. It is a transmission spectrum of the inventive material on ZnS. Figure 2 shows the roll-roll process according to the invention and the resulting composite shape. Figure 2 shows the roll-roll process according to the invention and the resulting composite shape.

Claims (26)

A composite comprising a substrate, a coating component thereon, wherein the coating component comprises an aluminum phosphate compound, wherein the compound has an aluminum to phosphorus ratio of about 0.5 to about 1 to about 25 to about 1 Range of
The composite is a structural composite that is disposed about a vertical axis substantially with respect to the configuration.   The composite of claim 1 wherein the substrate is selected from metals, metal alloys and plastics.   The composite of claim 2 wherein the substrate is selected from stainless steel and brushed stainless steel.   The composite of claim 3 wherein the coating component is substantially transparent to the visible spectrum.   The composite of claim 3 wherein the coating component imparts a iridescent appearance to the composite.   The composite of claim 3, wherein the coating component comprises an antimicrobial component.   The composite of claim 2 comprising at least one interlayer component between the substrate and the coating component.   The composite of claim 2, wherein the substrate comprises a plastic comprising one of polycarbonate, polycarbonate copolymer, polyimide, polyimide copolymer, polyester and polyester copolymer.   The composite of claim 8, wherein the coating component is an osmotic barrier.   The composite of claim 8, wherein the coating component is at least partially insoluble in the organic solvent.   9. The composite of claim 8, comprising at least one upper layer component over the coating component, wherein the coating component is adhesive to the upper layer component. The composite of claim 11 wherein the coating component comprises a structural site that absorbs radiation at about 1230 cm ^-1 in the IR spectrum.   The composite of claim 2 wherein the substrate comprises a metal foil having a thickness of about 100 mils or less.   14. The composite of claim 13, wherein the foil is selected from aluminum, stainless steel, titanium, magnesium, nickel-based alloy and superalloy.   15. The composite of claim 14, comprising a reflective metal upper layer component over the coating component.   The composite of claim 2 wherein the substrate is a wire.   The composite of claim 1 wound with a spool.   The composite of claim 1 manufactured into a product. A method of sealing a porous substrate surface using an aluminum phosphate composition,
Preparing a substrate containing surface components;
Contacting the surface component with an aluminum phosphate compound, the compound comprising at least a phosphate ester moiety, and heating the composition at a temperature and for a time sufficient to partially remove the ester moiety.   20. The method of claim 19, wherein the substrate is selected from granite, marble, artificial stone, porcelain and ceramic.   20. The method of claim 19, wherein the surface component is substantially flat.   20. The method of claim 19, wherein the contacted composition is thermally stable to a temperature of substantially about 1000 <0> C.   20. The method of claim 19, wherein the composition is sprayed onto the surface component.   24. The method of claim 23, wherein the composition comprises at least one aqueous carrier component, a non-aqueous carrier component and an aerosol spray.   25. The method of claim 24, wherein the composition comprises an aerosol spray.   20. The method of claim 19, wherein the substrate is selected from kitchen utensils and counters, bathroom fixtures and floor and wall tile members.

Images