CN109971413B - Preparation method of high-refractive-index LED packaging adhesive material - Google Patents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
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Abstract
The invention discloses a preparation method of a high-refractive-index LED packaging adhesive material. By using the phase transfer technique, the nanoparticles dispersed in the aqueous phase can be transferred into the organic phase because the nano zirconia particles coated with the phosphoric acid-based modifier are more soluble in a solvent having a small polarity and thus are easily transferred from water into the organic phase. Compared with other methods, the phase transfer method has the advantages of lower environmental requirements, simpler operation and lower cost, and is very suitable for preparing a large amount of nano zirconia particles with high dispersibility and high-refractive-index composite packaging adhesive materials. The method can prepare the nano zirconia particles with good dispersibility, small and uniform particles, and can enrich zirconia in a solvent to form a nano zirconia dispersion with high solid content. And the reaction condition is easy to control, and the method has large-scale industrial production conditions.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to a preparation method of an LED packaging adhesive material with high refractive index, high transparency and high cohesiveness.
Background
Zirconium dioxide, also known as zirconic anhydride or zirconium oxide, is a solid that is difficult to dissolve in water, but can dissolve in hot concentrated sulfuric and hydrofluoric acids. Zirconium dioxide has a melting point of about 2700 c, a boiling point of about 4300 c and a flash point of about 5000 c. Compared with the oxides of the same family, the zirconium dioxide has stable properties and no photocatalysis, and is widely researched and applied due to five major effects of volume effect, surface effect, quantum size, quantum tunnel, dielectric confinement and the like of the nano material, wherein the nano zirconium dioxide particles can be applied to manufacturing biological materials, ceramic materials and the like and can also be used as a synthesis catalyst or a cocatalyst in certain chemical reactions. The nanometer zirconium dioxide particles can be particularly used in the photoelectric field, for example, the zirconium dioxide nanoparticles can be added into the packaging adhesive of the LED light-emitting device to improve the refractive index of the packaging adhesive, so as to improve the light-emitting rate of the device and achieve the effects of energy conservation and emission reduction. However, it is worth noting that, if some special surface particle modification techniques are not performed, the nano zirconia particles are easily agglomerated in the organic base material, and the agglomeration phenomenon causes overlarge local particles and uneven dispersion, so that the transmittance of the composite base material is greatly reduced, and the light emitting performance of the LED device is reduced. Therefore, the key point of the technical field is to prepare the transparent zirconium dioxide dispersion which has excellent dispersion performance in an organic solvent system and can be stable for a long time. The dispersion can be mixed with an LED packaging adhesive material by a simple solvent blending method, and can uniformly disperse the nano zirconia particles in the organic base material after the solvent is removed, and the characteristics of high transparency, high refractive index and the like are maintained.
Some methods for preparing aqueous dispersions of nano zirconia with small particle size are described in the prior patents, such as patent CN106277049B, in which alkaline zirconium salt solution is heated, and the obtained solution is dialyzed to remove impurities and then undergoes hydrothermal reaction to obtain the product; patent No. cn201810836953.x adopts a method of adding hydrogen peroxide to a strongly basic zirconium salt solution for reaction, and then washing and precipitating with an acid solution and water respectively to obtain products, but LED packaging materials are generally epoxy resins and organic silicone adhesives, and these two organic polymers cannot form a uniformly dispersed transparent nano composite adhesive with hydrophilic nano zirconia. There is therefore a need for a process for preparing nano-zirconia particles of small diameter while achieving good dispersion thereof in organic solvents. The method combines the preparation technology of the aqueous phase dispersion and the surface modification technology of the organic acid, and prepares the transparent nano zirconium dioxide particle organic phase dispersion with high dispersion, small particle size, uniformity and small agglomeration degree by a phase transfer method. After the packaging adhesive material is added into the dispersion, the solvent is removed, and the packaging adhesive uniformly doped with the nano zirconia can be obtained, wherein the refractive index of the packaging adhesive is obviously improved compared with that of the packaging adhesive material without the nano zirconia.
In the preparation of organic phase dispersions of transparent nano-zirconia particles, the chemical bonds of the zirconia nano-particles can be combined with a modifier by using a surface modifier with a bond functional group at the end, thereby increasing the dispersibility in the dispersoid, and therefore, the selection of a suitable modifier is a very critical step. In previous studies, some modifiers have been selectively used to modify the surface of the nano zirconia. Patent CN102448888A adopts aryl sulfonyloxy modifier to modify the nano zirconia particles, the method has the defects that the raw materials are easy to obtain and the process is simple, but the aryl sulfonyloxy organic matter is generally too stable and difficult to remove, and the impurities in the product are possibly too much; patent CN102031026A discloses that nano zirconia is modified by amino silane to obtain zirconia dispersion with good dispersibility, but because the dispersant is single in type, the preparation process is complex, and the reaction condition requires high, it is difficult to realize industrial mass preparation.
The invention selects organic acid represented by phosphoric acid to modify the surface of the zirconia nano-particles, and the organic acid has more excellent properties compared with other modifiers as a novel modifier to be developed. Taking a phosphoric acid modifier as an example, the modification method is to form Zr-O-P bonds on the surface of zirconia, and because phosphate radicals in phosphoric acid have higher thermal stability, contact among zirconia particles is effectively hindered, so that growth and agglomeration of zirconia nanoparticles are inhibited in a phase transfer reaction, and the dispersion degree of the nanoparticles is increased.
The phase transfer method employed in the present invention can be used to transfer nanoparticles between two liquid phases. By using the phase transfer technique, the nanoparticles dispersed in the aqueous phase can be transferred into the organic phase because the nano zirconia particles coated with the phosphoric acid-based modifier are more soluble in a solvent having a small polarity and thus are easily transferred from water into the organic phase. Compared with other methods, the phase transfer method has the advantages of lower environmental requirements, simpler operation and lower cost, and is very suitable for preparing a large amount of nano zirconia particles with high dispersibility and high-refractive-index composite packaging adhesive materials.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a preparation method of a transparent organic phase nano zirconium oxide particle dispersion. According to the preparation method, firstly, a hydrothermal method and other methods are used for preparing the nano zirconia water-phase dispersion, then the surface of zirconia is bonded by an organic acid modification method, so that a phase transfer reaction occurs, and nano zirconia particles are enriched in an organic phase to form the transparent zirconia nano particle dispersion. The method can prepare the nano zirconia particles with good dispersibility, small and uniform particles, and can enrich zirconia in a solvent to form a nano zirconia dispersion with high solid content. And the reaction condition is easy to control, and the method has large-scale industrial production conditions.
The second technical problem to be solved by the invention is to provide a transparent organic phase nano zirconium oxide particle dispersion. The solid content of the transparent organic phase dispersoid is 0.01-50 wt%, the grain diameter of the zirconia crystal is small, the distribution is uniform, and the average grain diameter is 6.23 nanometers; in addition, the liquid phase dispersion has good stable dispersion effect, high solid content, is suitable for long-time storage, and can be widely applied to industrial production.
The third technical problem to be solved by the invention is to provide an application description of the transparent organic phase nano zirconium oxide particle dispersion.
In order to solve the first technical problem, the invention adopts a technical scheme that a preparation method of a transparent organic phase nano zirconium oxide particle dispersion is provided, and the preparation method comprises the following steps:
step 1) preparing a water-phase nano zirconium oxide particle dispersoid which is not subjected to surface modification; the nano zirconia particle dispersion is prepared according to the methods of patents CN106277049B and cn201810836953. x.
Step 2) mixing the prepared water-phase non-surface-modified nano zirconium oxide particle dispersoid, inorganic acid, an organic acid surface modifier and an organic solvent according to a proper proportion to obtain acidic layered liquid;
step 3) placing the acidic layered liquid in a stirring reactor for phase transfer reaction for a proper time, and obtaining a product transparent organic phase nano zirconium oxide particle dispersoid through reaction;
and 4) uniformly mixing the prepared transparent organic phase nano zirconium oxide particle dispersoid with an organic base material of the packaging adhesive in a certain proportion, and removing the solvent in the mixture to obtain the final product, namely the high-refractive-index LED packaging adhesive material.
Preferably, in step 2), the organic acid surface modifier is one or more selected from the following substances: 2-ethylhexyl phosphate, diisobutyl phosphate, cetyl alcohol phosphate, dihexadecyl phosphate, mono-n-dodecyl phosphate, cetostearyl phosphate, dimethylhydrogen phosphate, bis (butoxyethyl) phosphate, bis (2-ethylhexyl) phosphate, n-butyl phosphate, 2-ethylhexyl phosphate, isooctyl phosphate, 9-octadecen-1-ol phosphate; more preferably, one or more of 2-ethylhexyl phosphate, mono-n-dodecyl phosphate, n-butyl phosphate and cetyl alcohol phosphate are selected.
Preferably, in step 2), the inorganic acid is one or more selected from the group consisting of: hydrochloric acid, nitric acid, boric acid, hydrocyanic acid, hydrofluoric (halogen) acid, nitrous acid, perhalogenic acid, halous acid, hypohalous acid, and metaaluminic acid.
Preferably, the stirring reactor in step 3) is used for fully mixing the substances participating in the chemical reaction, and the stirring reactor includes a gas flow stirring reactor, a jet stirring reactor, a static pipeline stirring reactor, an electromagnetic stirring reactor, and the like. The reaction speed is 50-300 revolutions, and more preferably, the reaction speed is 70-150 revolutions; most preferably, the reaction speed is 100 revolutions.
Preferably, in step 3), the organic solvent is selected from one or more of the following substances: benzene, toluene, xylene, phenol, aniline, benzoic acid, nitrobenzene, diethyl ether, petroleum ether, tetrahydrofuran, dichloromethane, chloroform, carbon tetrachloride, n-pentanol, methyl acetate, ethyl acetate, phenyl acetate, methyl benzoate, butyl acetate, octyl acrylate, isoamyl acetate, methyl benzoate, methyl salicylate, glycerol esters.
Preferably, in step 4), the organic substrate is selected from one or more of the following: methyl organic silica gel, phenyl organic silica gel, glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin and alicyclic epoxy resin.
In order to solve the second technical problem, the invention adopts the following technical scheme: a transparent organic phase nano zirconium oxide particle dispersoid comprises an organic phase medium and nano zirconium oxide particles, wherein the nano zirconium oxide particles are obtained by the preparation method of the transparent organic phase nano zirconium oxide particle dispersoid; the solids content of the dispersion is from 0.01 to 50% by weight; the one-dimensional size of the nano zirconia particles is 6.2 nm; the liquid phase medium is one or more of benzene, toluene, xylene, phenol, aniline, benzoic acid, nitrobenzene, diethyl ether, petroleum ether, tetrahydrofuran, dichloromethane, trichloromethane, carbon tetrachloride, n-amyl alcohol, methyl acetate, ethyl acetate, phenyl acetate, methyl benzoate, butyl acetate, octyl acrylate, isoamyl acetate, methyl benzoate, methyl salicylate and glyceride.
The third technical problem to be solved by the invention is to provide an application of the transparent organic phase nano zirconium oxide particle dispersion. The transparent organic phase nano zirconium oxide dispersoid has good dispersibility, good stabilizing effect and high solid content of liquid phase dispersoid, is suitable for long-term storage and can be widely applied to industrial production, so the transparent organic phase nano zirconium oxide dispersoid can be used as ceramic materials, such as dental materials, artificial joints, oxygen sensors, ceramic ferrules, sensor materials, polishing materials, fuel cells, structural materials and the like; or for synthesizing catalyst components, such as main catalysts, cocatalysts, and the like; meanwhile, the nano-zirconia in the aqueous nano-zirconia dispersion prepared by the method has the characteristic of high refractive index, so that the method has the important application of improving the refractive index of the composite material on the premise of keeping the original high light transmittance of the resin material, and particularly has excellent performance in the aspect of manufacturing and application of optical elements.
The invention has the beneficial effects that:
1. the modified nano-zirconia particles prepared by the method have the characteristics of high dispersibility, high stability, high solid content and the like in an organic phase. Compared with the existing method of dispersing the nano zirconia particles by using the aqueous phase, the method has the advantages that the obtained zirconia nano particles are small in particle size and uniform in distribution, the one-dimensional size is 6.2nm, the application range of the nano zirconia is widened, and the nano zirconia can be used for preparing the high-refractive-index LED packaging adhesive material.
2. The dispersant of the transparent organic phase nano zirconium oxide liquid phase dispersion body obtained by the invention selects various organic matters or mixtures thereof, so that the dispersant has higher selectivity in preparation, has better adaptability to various organic solvents in the dispersion process, and can be better applied to industrial production.
3. When the modified zirconia nano-particles obtained by the invention are added into the LED packaging adhesive, the refractive index is obviously improved.
4. The preparation method has the advantages of simple preparation process, good product quality, wide and easily-obtained raw materials, simple process, convenient condition control, pure obtained product, easy mass preparation and large-scale industrial production potential.
Drawings
FIG. 1 is a graph of the dynamic light scattering laser particle size of the modified nano zirconia particles of example 1;
FIG. 2 is a graph of the dynamic light scattering laser particle size of the modified nano zirconia particles of example 2;
FIG. 3 is a transmission electron microscope image of modified nano-zirconia particles in example 1;
FIG. 4 is a transmission electron microscope image of modified nano-zirconia particles in example 2;
FIG. 5 is a transmission electron microscope image of modified nano-zirconia particles in example 3;
FIG. 6 is a transmission electron microscope image of modified nano-zirconia particles in example 4;
FIG. 7 is a schematic representation of a modified nano zirconia dispersion of example 1;
FIG. 8 shows the refractive index of silica gel to which the modified nano-zirconia of example 1 was added;
FIG. 9 shows the refractive index of the epoxy resin to which the modified nano zirconia of example 1 was added;
Detailed Description
The present invention will be further described with reference to the drawings and examples, but the present invention is not limited to the following examples or other similar examples.
Example 1
1) Preparing an aqueous phase non-surface modified nano zirconium oxide particle dispersion according to the method described in patent cn201810836953. x;
2) 5 ml of zirconium oxide nano-particle aqueous phase dispersion liquid with the solid content of 1 wt%, 2 ml of trichloromethane and 0.5 ml of 2-ethylhexyl phosphate are put into a bottle and are kept stand until the zirconium oxide nano-particle aqueous phase dispersion liquid and the trichloromethane are layered.
3) Adding magnetons at the bottom of the bottle, placing the bottle on a magnetic stirrer, and stirring at the speed of 100 revolutions per minute for phase transfer reaction for 1 hour to obtain the final product, namely the transparent organic phase nano zirconium oxide particle dispersoid. Wherein the particle size of the nano particles under an electron microscope is 3-8 nanometers. Dynamic light scattering laser particle size analysis the average particle size of the nanoparticles was 6.23 nm.
4) The transparent organic phase nano zirconia particle dispersion was mixed with a pure colloidal material, wherein the weight of the modified nano zirconia was fifty percent of the total solids weight (excluding the solvent portion), and the refractive index was measured after spin coating of the colloidal film to obtain a refractive index profile, which resulted in a refractive index of 1.558 at 633 nm and maintained a transmittance of 98%.
Example 2
1) An aqueous phase non-surface modified nano-zirconia particle dispersion obtained according to the method described in patent CN 106277049B;
2) 5 ml of zirconium oxide nano-particle aqueous phase dispersion liquid with the solid content of 1 wt%, 2 ml of trichloromethane and 0.5 ml of mono-n-dodecyl phosphate are put into a bottle and kept stand until the zirconium oxide nano-particle aqueous phase dispersion liquid and the trichloromethane are layered.
3) Adding magnetons at the bottom of the bottle, placing the bottle on a magnetic stirrer, and stirring at the speed of 100 revolutions per minute for phase transfer reaction for 1 hour to obtain the final product, namely the transparent organic phase nano zirconium oxide particle dispersoid. Wherein the particle size of the nano particles under an electron microscope is 2-7 nanometers. Dynamic light scattering laser particle size analysis the average particle size of the nanoparticles was 5.17 nm.
4) Mixing the transparent organic phase nano-zirconia particle dispersion with a pure glue material, wherein the weight of the modified nano-zirconia accounts for fifty percent of the total solid weight (no solvent part), spin-coating the mixture to form a glue film, measuring the refractive index of the glue film to obtain a refractive index curve, wherein the refractive index at 633 nm is 1.543, and the transmittance is 97%.
Example 3
1) Preparing an aqueous phase non-surface modified nano zirconium oxide particle dispersion according to the method described in patent cn201810836953. x;
2) 5 ml of zirconium oxide nano-particle aqueous phase dispersion liquid with the solid content of 1 wt%, 2 ml of trichloromethane and 0.5 ml of n-butyl phosphate are put into a bottle and kept stand until the zirconium oxide nano-particle aqueous phase dispersion liquid and the trichloromethane are layered.
3) Adding magnetons at the bottom of the bottle, placing the bottle on a magnetic stirrer, and stirring at the speed of 100 revolutions per minute for phase transfer reaction for 10 hours to obtain the final product, namely the transparent organic phase nano zirconium oxide particle dispersoid. Wherein the particle size of the nano particles under an electron microscope is 4-6 nanometers. The average particle size of the nanoparticles was 5.98 nm as determined by dynamic light scattering laser particle size analysis.
4) Mixing the transparent organic phase nano zirconia particle dispersion with a pure glue material, wherein the weight of the modified nano zirconia accounts for forty percent of the total solid weight (the part without solvent), measuring the refractive index of the glue film after spin coating to obtain a refractive index curve, wherein the refractive index is 1.542 at 633 nm, and the transmittance is 97%.
Example 4
1) Preparing an aqueous phase non-surface modified nano zirconia particle dispersion according to the method described in patent CN 106277049B;
2) 5 ml of zirconium oxide nano-particle aqueous phase dispersion liquid with the solid content of 1 wt%, 2 ml of toluene and 0.5 ml of n-butyl phosphate are put into a bottle and kept stand until the zirconium oxide nano-particle aqueous phase dispersion liquid is layered.
3) Adding magnetons at the bottom of the bottle, placing the bottle on a magnetic stirrer, and stirring at the speed of 100 revolutions per minute for phase transfer reaction for 10 hours to obtain the final product, namely the transparent organic phase nano zirconium oxide particle dispersoid. Wherein the particle size of the nano particles under an electron microscope is 3-9 nanometers. Dynamic light scattering laser particle size analysis the average particle size of the nanoparticles was 6.77 nm.
4) Mixing the transparent organic phase nano zirconia particle dispersion with a pure glue material, wherein the weight of the modified nano zirconia accounts for thirty percent of the total solid weight (no solvent part), measuring the refractive index of the glue film after spin coating to obtain a refractive index curve, wherein the refractive index at 633 nm is 1.531, and the transmittance is 98%.
Example 5
1) Preparing an aqueous phase non-surface modified nano zirconium oxide particle dispersion according to the method described in patent cn201810836953. x;
2) 5 ml of zirconium oxide nano-particle aqueous phase dispersion liquid with the solid content of 1 wt%, 2 ml of tetrahydrofuran and 0.5 ml of hexadecanol phosphate are put into a bottle and kept stand for layering.
3) Adding magnetons at the bottom of the bottle, placing the bottle on a magnetic stirrer, and stirring at the speed of 200 revolutions per minute for phase transfer reaction for 5 hours to obtain the final product, namely the transparent organic phase nano zirconium oxide particle dispersoid. Wherein the particle size of the nano particles under an electron microscope is 2-6 nanometers. Dynamic light scattering laser particle size analysis the average particle size of the nanoparticles was 5.41 nm.
4) Mixing the transparent organic phase nano zirconia particle dispersion with a pure glue material, wherein the weight of the modified nano zirconia accounts for twenty percent of the total solid weight (no solvent part), spin-coating the mixture to form a glue film, measuring the refractive index of the glue film to obtain a refractive index curve, wherein the refractive index at 633 nm is 1.529, and the transmittance is 96%.
Claims (3)
1. A preparation method of a high-refractive-index LED packaging adhesive material is characterized by comprising the following steps: the preparation method comprises the following steps of,
step 1) preparing a water-phase nano zirconium oxide particle dispersoid which is not subjected to surface modification;
step 2) mixing the prepared water-phase non-surface-modified nano zirconium oxide particle dispersoid, inorganic acid, an organic acid surface modifier and an organic solvent according to a proper proportion to obtain acidic layered liquid;
step 3) placing the acidic layered liquid in a stirring reactor for phase transfer reaction for a proper time, and obtaining a product transparent organic phase nano zirconium oxide particle dispersoid through reaction;
step 4) uniformly mixing the prepared transparent organic phase nano zirconium oxide particle dispersoid with an organic base material of the packaging adhesive in a certain proportion, and removing the solvent in the mixture to obtain a final product, namely the high-refractive-index LED packaging adhesive material;
in the step 2), the organic acid surface modifier is one or more selected from the following substances: 2-ethylhexyl phosphate, diisobutyl phosphate, cetyl alcohol phosphate, dihexadecyl phosphate, mono-n-dodecyl phosphate, cetostearyl phosphate, dimethyl hydrogen phosphate, diphosphate, n-butyl phosphate, isooctyl phosphate, 9-octadecen-1-ol phosphate;
in the step 2), the inorganic acid is one or more selected from the following substances: nitric acid, boric acid, hydrocyanic acid, hydrofluoric acid, nitrous acid, perhalogenic acid, halous acid, hypohalous acid, and metaaluminic acid;
step 3) the stirring reactor is used for fully mixing substances participating in chemical reaction, and comprises an airflow stirring reactor, a jet stirring reactor, a static pipeline stirring reactor and an electromagnetic stirring reactor; the reaction speed is 50-300 rpm;
in step 2), the organic solvent is selected from one or more of the following substances: benzene, toluene, xylene, aniline, nitrobenzene, diethyl ether, petroleum ether, dichloromethane, trichloromethane, carbon tetrachloride, n-pentanol, methyl acetate, ethyl acetate, phenyl acetate, butyl acetate, octyl acrylate, isoamyl acetate, methyl benzoate, methyl salicylate.
2. The method for preparing the high-refractive-index LED packaging adhesive material according to claim 1, wherein the method comprises the following steps: in step 4), the organic substrate is selected from one or more of the following substances: methyl organic silica gel, phenyl organic silica gel, glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin and alicyclic epoxy resin.
3. A transparent organic phase nano zirconia particle dispersion characterized by: which is prepared by the preparation method of the transparent organic phase nano zirconium oxide particle dispersion as claimed in claim 1, comprising an organic phase medium and nano zirconium oxide particles, wherein the solid content of the dispersion is 0.01-50 wt%; the one-dimensional size of the nano zirconia particles is 6.2 nm; the organic phase medium is one or more of benzene, toluene, xylene, aniline, nitrobenzene, diethyl ether, petroleum ether, dichloromethane, trichloromethane, carbon tetrachloride, n-amyl alcohol, methyl acetate, ethyl acetate, phenyl acetate, butyl acetate, octyl acrylate, isoamyl acetate, methyl benzoate and methyl salicylate.
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| "Unique Hydrophobization and Hybridization via Direct Phase Transfer of ZrO2 Nanoparticles from Water to Toluene Producing Highly Transparent Polystyrene and Poly(methyl methacrylate) Hybrid Bulk Materials";Kazushi Enomoto等;《Macromolecules》;20171204(第50期);第9713-9725页 * |
| He Xianglei等."High-gravity-assisted scalable synthesis of zirconia nanodispersion for light emitting diodes encapsulation with enhanced light extraction efficiency".《Chemical Engineering Science》.2018,(第195期),第1-10页. * |
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