BRPI0806015A2 - process for the preparation of thin or ultra thin films and nanocomposites of metal oxide and / or metal oxide nanoparticles impregnated and / or deposited on glassy, polymeric, wood, metal and other substrates - Google Patents

Abstract

PROCESS FOR PREPARATION OF FINE OR ULTRA FINE FILMS AND NANOCOMPOSITES OF METALLIC AND / OR METAL IMPREGNED AND / OR METAL NANOPARTICULES, CONTAINED IN METHODS, POLYMERICES, METALS AND METHODS and or metals on diversified substrates. The results of this process are exemplified in this patent and are thin film generators, ultra thin substrate surface composite films, glass surface substrate nanocomposites in the form of nanocomposites from metal oxides and / or pulverized metals. . The proposed procedure differs from the methodologies currently applied by applying metal oxides and / or metals exactly in the chemical composition intended to be obtained as the final product of the film at temperatures below: glass transition temperature for glass substrates softening temperature for polymer substrates, flash point for wood substrate and oxidation state change temperature for metals.

Description

PREPARATION OF PREPARATION OF GOLDEN FINAL FILMS AND NANOCOMPOSITES OF IMPREGNED AND / OR DEPOSIT METAL, METAL, WOOD AND OIL SUBSTRATES

The present invention comprises a method for the manufacture of thin or ultra-thin films and nanocomposites of metal oxide nanoparticles and / or metals in interaction with glass or polymeric substrates or wood, metals or any other substrate which may or may pore its surface. by a process of impregnating and / or depositing powders of metal oxides and / or metals previously constituted at a temperature below the glass transition or softening or flash point or below any temperature which results in a change in the physical state of the material when associated with influence of the time at which the assay is processed.

It is common to find in the scientific literature studies concerning the properties of materials related to surface structure. The surface properties of materials can be modified from various deposition techniques capable of forming thin, thick or still ultra thin films. Some of these techniques are described below.

Thin films can be produced by saline deposition through the effect of temperature. Ag + ion deposition films have already been prepared on the glass surface from Ag2SO4, CuSO4, Na2SO4 solution in the presence of organic compounds dispersed in oil. The treatment temperature was 300 ° C, 320 ° C and 350 ° C, with time ranging from 1 to 48 h.

Another way to obtain films is from electrostatic spray deposition, sputtering method followed by thermal treatment. The filtered cathodic arc plasma and oxygen flow technique was also applied to deposit thin surface zinc oxide films. and temperature of 200 ° C.

Still another way of altering the surface properties of the materials is in the direct addition of dopants during the synthesis process that form new materials with new properties, consequently also changing the surface properties.

Currently, 3 types of substrates are used in the development of thin films: 1) Metal foils, used to make thin films for capacitors on printed circuit boards through coatings such as nickel or copper. 2) Ceramic substrates. 3) Silicon crackers, paraffin fabrication of metal oxide thin films. It is known that a basic condition for the selection of a thin film substrate is low surface roughness.

Among the many existing methods for thin film manufacturing we can mention: Sputtering, Chemical Vapor Deposition (CVD), Sol-Gel, Spray Pyrolysis, etc. All these methods have advantages and disadvantages, but in general they have difficulties such as high cost, difficulties in reproducing results, superficial cracks and porosities.

It should also be noted that the methods described above may constitute the oxides to be obtained in the form of films only mixed during the synthesis process of these materials. For the formation of films on already processed substrates, oxides are formed from precursor substances deposited on the substrates that, by treatment (usually thermal), form the oxide films to be obtained.

It is noteworthy that the vitreous materials when subjected to high temperatures reach a state of "softening" which, by definition, is known as glass transition (Tg). This glass transition is often a limiting factor for filmmaking methods and impregnation of particulate materials on the glass surface, and if it is a polymeric substrate softening can be achieved and if it is wood the flash point and metal oxidation etc. The present invention comprises a method for the manufacture of thin or ultra-thin films and nanocomposites of metal oxide nanoparticles in interaction with glass or polymeric substrates or woods, metals or any other substrate which presents or may generate porosity on its surface by means of a surface. a process of impregnation and / or deposition of previously constituted metal oxide powders at a temperature below the glass transition or softening or flash point or below any temperature resulting in a change in the physical state of the material when associated with the influence of the time at which the test is performed .

The following drawings refer to results in the exemplary form of the invention of the methodology for manufacturing thin oxide or ultra-thin films and nanocomposites of metal oxide nanoparticles in interaction with glass or polymeric substrates or woods, metals, or any other substrate presenting or porosity can be generated on its surface by a process of impregnation and / or deposition of metal oxide powders previously constituted at a temperature below the glass transition or from the softening or the flash point or even below any temperature that results in the change of physical state associated with the influence of the time at which the test is submitted, in which:

fig. 1 is a sequence of 3,000 X magnification scanning electron micrographs from pure glass substrate to the deposition of unparticulated Sn02 film treated at 485 ° C.

fig. 2 represents an example of decobalt oxide deposition by SEM.

fig. 3 represents an example of iron oxide III deposition by SEM.

fig. 4 depicts an example of deposition of titanium oxide by SEM.

fig. 5 depicts an example of deposition of aluminum oxide by SEM. FIG. 6 represents an example of deposition of copper oxide by SEM.

The present invention comprises a process for the manufacture of thin films of metal oxides of films at temperatures below the glass transition temperature, the softening temperature, the glow point or the change in oxidation state depending on the substrate, high pressure as a function of rehearsal time. The process consists of: (a) deposition of metal powders on the substrate surface, (b) application of high pressure cooled degassing, (c) infiltration and / or deposition of powders on the substrate surface and (d) heating temperature below transition temperature glass (for glass), softening (for polymers), flash point (for wood) and oxidation (for metals) as a function of time. After impregnation and / or deposition under high pressure, metal oxides will form a second phase, such as depending on factors such as substrate chemical constitution, particle size and specific surface area of metal oxide powders, applied gas pressure, gas type, treatment time and temperature, may be in a amorphous or nanocrystalline state and may therefore form a thin film consisting of non-nanocomposite materials.

Figure 1 shows an example of thin film of metal oxides impregnated and / or deposited by high limit pressure (P1) on substrate. From this figure 1 it can be seen that even at the pressure P1, at point (1) the substratum is not treated (temperature To = O and time to = 0), consequently, the metal oxide and / or metal is not deposited.

With the application of the limit pressure or higher than Pl, in a heat treatment at a temperature Ti> T0 and time ti> to it can be seen that it begins to occur to the impregnation and / or deposition of metal oxide and / or metal with the substrate leading to the point ( 2) of figure 1.

When the limit pressure is kept constant, film adhesion and / or impregnation can be improved by raising the temperature from Ti to T2 or raising the time from ti to X2 or raising the temperature and time to T2 and respectively. However, keeping the temperature constant at Ti and the time at Ti, but by increasing the pressure higher than Pl it is also possible to reach a film indicated by stage (3) of Figure 1.

Similarly, still in figure 1, stage 3 can be reached if: the limit pressure is kept constant and the temperature of T2 is raised to T3 or even if the time is increased from t2 to k or raise both to T3 and t3 respectively. In this same example, it is also reached the same result if the temperature at T2 and the time at t2 remain constant, but if the applied pressure is greater than the pressure exerted at stage (2).

Thus, it is shown that by applying a very high pressure, and a temperature Tn (where η is greater than zero) which varies for, temperature below the glass transition temperature when the substrate is glass, temperature below the softening temperature when the substrate for polymer, temperature below flash point when substrate for wood and temperature below oxidation temperature for metals and a tm time (where m is greater than zero) can have a different methodology for obtaining thin or ultra thin films. - finose nanocomposites of metal oxide and / or metal nanoparticles in interaction with glass or polymeric substrates or woods, metals or any other substrate which may or may generate porosity on its surface by a high pressure impregnation and / or deposition process of time

In turn, the figures from figure 2 to figure 6 demonstrate the possibility of applying different substrate oxides when a pressure of P1 or greater, a temperature of Ti or greater and a time of at least you.

Still referring to the figures already mentioned and, according to the proposal of this process of preparing films on substrates, it is possible to verify the possibility of impregnating and / or depositing cobalt oxide (figure 2), iron oxide III (figure 3), titanium oxide (figure 4), aluminum oxide (figure 5), copper oxide (figure 6) or any other type of metal and / or metal oxide on glass, polymer, wood or metal substrates, provided pressure, temperature and time proposed in this inventive process.

Claims (8)

1. PROCESS FOR PREPARATION OF FINE OR ULTRA FINE FILMS NANOPOMETRIES OF METALICOSIS OR METAL IMPREGNED AND / OR MIXED SUBSTRATES 1 POLYMERIC, WOOD, METAL AND OTHER METHODS: deposition of metal oxide and / or metal powders on the substrate of glass, polymer, wood, metals or their composition, infiltration and / or deposition of metal oxide and / or metal powders in the substrate by the high pressure action of gas and temperature lower than: glass transition temperature for glass, polymer softening temperature, flash point for wood, temperature of change of oxidation state for metals at a given time forming a thin layer of metal oxides and / or infiltrated metal and / or deposited on the substrate. 2. PROCESS FOR PREPARATION OF FINE OR ULTRA FINE FILMS NANOPOMETRIES OF METALICOSIS OR METAL IMPREGNED IMPREGNED OXIDE NANOParticles, SUBSTRATES VITRE, POLYMERIC, WOOD, METALS AND OTHER MATERIALS, COMPONENTS from a group consisting of the definition of pure oxide ceramics or mixtures thereof or the definition of metal bonding to metals comprising all natural elements listed in the periodic table even in different proportions. 3. PROCESS FOR PREPARING FINE OR ULTRA FINE FILMS NANOPOMPOSITES OF METALLICOSE / OR METAL IMPREGNED AND / OR METAL NONOParticles, SUBSTRATES VITRE, POLYMERIC, WOOD, WHICH MAY BE SUBSTITUTED BY, be classified as: glass, polymer, wood, metal or pure, or mixtures of different proportions. 4. PROCESS FOR PREPARING FINE OR ULTRA FINE FILMS NANOPOMPOSITES OF METALICOSIS / OR METAL IMPREGNED AND / OR METAL OXIDE NANOParticles, WHERE, METALS AND OTHER PRESSURES APPLIED TO METALICOSIS AND OTHER PRESSURES OF THE METALS Metals against the surface of the substrate is 1-200 bar, or more preferably between 5-50 bar, or more preferably between 15-25 bar. 5. PROCESS FOR PREPARATION OF FINE OR ULTRA FINE FILMS AND NANOPOMETRIES OF METALICOSIS / OR METAL IMPREGNED AND / OR METAL NONOParticles, POLYMERIC, WOOD, TEMPERATURE, AND OTHER TEMPERATURES where temperature is required at controlled temperatures deposition and / or impregnation of metal oxides or metals and below the temperature of: glass transition to glass substrates, softening to polymer substrates, flash point for wood substrates and temperature of oxidation state change and, in the case of its composition, which the lowest temperature is respected. 6. PROCESS FOR PREPARING FINE OR ULTRA FINE FILMS NANOPOMPOSITES OF METALLICOSE / OR METAL IMPREGNED AND / OR METAL NONOParticles, SUBSTRATES VITRE, POLYMERIC, WOOD is selected as a group of high pressure and a group of selected air. atmospheric, neutral, reducing or oxidizing atmospheres and their combinations in any proportion. 7. PROCESS FOR PREPARATION OF FINE OR ULTRA FINE FILMS NANOPOMETRIES OF METALLICOSE / OR IMPREGNED AND / OR METAL OXIDE NANOParticles, POLYMERIC, WOOD, METHODS, POWERS, AND METHODS and / or metals, substrate constitution, applied pressure and temperature and heat treatment time. 8. PROCESS FOR PREPARING FINE OR ULTRA FINE FILMS ENANOCOMPOSITS OF METALICOSIS / OR METAL IMPREGNED AND / OR METAL NANOParticles, SUBSTRATES VITRE, POLYMERIC, WOOD, METALS AND OTHER PRODUCTS metals deposited together with the substrate.