CN1298906A - Nm-class coating material and its preparing process - Google Patents
Nm-class coating material and its preparing process Download PDFInfo
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- CN1298906A CN1298906A CN 00129358 CN00129358A CN1298906A CN 1298906 A CN1298906 A CN 1298906A CN 00129358 CN00129358 CN 00129358 CN 00129358 A CN00129358 A CN 00129358A CN 1298906 A CN1298906 A CN 1298906A
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Abstract
the present invention relates to a nanometer coating film material and its preparation method. Said material is composed of (wt.%); tin oxide 40-95%, antimony oxide 0.5-35%, titanium oxide 0.1-15%, zirconium oxide 0.1-5% and silicon oxide 0.1-15%, the grain size of above mentioned oxides is between 5-30 nm, the raw material is dissolved in organic alcohol, reflaced, and alkali and organic protective agent are added, then proceed reaction under definite temperature and pressure, the reactant is filtered, spray-dried, calcined, ground, classified and concentrated into the product. Its characteristics include; high image clarity, low production cost, electrostatic resistant anti-dazzling, radiation resistant and high production efficiency.
Description
The invention belongs to the technical field of transparent continuous conductive films, and particularly relates to a nano coating material for a display and a kinescope and a preparation method thereof.
Conventionally, materials having a high dielectric constant, whose surfaces are liable to accumulate static charges and allow transmission of electromagnetic waves, such as glass, particularly for use in display screens ofcathode ray tubes and computer monitors, plasma displays, whose inner surfaces are bombarded with electrons to cause visibility to be reduced, whose surrounding objects are affected by radiation of electromagnetic waves, and whose definition of screen images is reduced under a certain light irradiation due to the mirror reflection effect of the glass surface to light, have conventionally been various transparent conductive films mainly containing ITO films, i.e., oxides such as indium tin oxide films, conductive films using noble metal nano conductive particles, such as silver-coated palladium, silver-coated gold, nickel-coated palladium, nickel-coated gold, etc., oxides containing indium tin oxide films, etc., which are generally adhered to the glass surface by a magnetron sputtering coating method or high-temperature thermal spraying, the transparent conductive film is formed by the method, when the antistatic requirement is met, the transparency of the conductive film is enough, because the high temperature and vacuum are required when the physical vapor deposition method or the chemical vapor deposition method is used for forming the film, the display device can not generally bear the high temperature of more than 450 ℃, therefore, the investment cost for forming the transparent conductive film on a large-area substrate is high, the production efficiency is low, the production cost is increased, and in addition, the cost of indium tin oxide is high, the production economy is poor, the noble metal is used as the conductive micro-particle, the prepared suspension liquid is not particularly complicated in coating process, but the value of the noble metal is high, and the amount of the transparent coating metal is at least 10 wt%, and the production cost of the method is also high.
The invention aims to overcome the defects of the prior art and provide a nano coating material with high image definition, low productioncost, antistatic property, anti-glare property, good radiation resistance and high production efficiency and a preparation method thereof
The invention aims to realize the purpose, and the nano coating material is characterized by comprising the following components in percentage by weight: 40-95% of tin oxide, 0.5-35% of antimony oxide, 0.1-15% of titanium oxide, 0.1-5% of zirconium oxide and 0.1-15% of silicon oxide, wherein the grain size of the oxides is 5-30 nm.
In order to further achieve the object of the present invention, the present invention is carried out by a production method comprising the steps of:
a. weighing required tin chloride, antimony chloride, titanium chloride and zirconium chloride, and completely dissolving in organic alcohol:
b. heating, and refluxing with alcohol at 60-150 deg.C for 1-8 hr;
c. then adding alkali, adjusting the pH value to be 9.5-10, and reacting to generate a precipitate, wherein the reaction formula is as follows:
a represents Sn, Sb, Zr and Ti, and X represents a natural number;
d. adding organic protective agent into the filtered liquid, controlling the reaction temperature at 60-300 deg.C and the pressure at 0.1-30Mpa, and hydrolyzing to obtain precipitate with particle size of 5-30 nm;
e. washing and filtering the precipitate, adding acid and an organic protective agent, and dispergating to form emulsion;
f. spraying and drying the emulsion at the drying temperature of 300 ℃ to form composite hydroxide particles;
g. roasting the composite hydroxide particles at the temperature of 250-900 ℃ to form loosely agglomerated particles with the grain size of less than 30nm and the granularity of less than 2 mu m, wherein the reaction formula is as follows:
h. grinding the generated particles for 4-12 hours, putting the particles into a centrifuge, and controlling the rotating speed at 10000-15000 r/min for classification and sorting.
g. Adding a silane coupling agent and a surface coating agent which account for 0.3-45% of the weight of the raw materials into a qualified product to generate a final product, wherein the reaction formula is as follows:
m represents Ti, Zr, Si, Sn, Sb, Et represents one or more C fatty alcohol groups.
h. And concentrating the final product to obtain the invention.
In order to further achieve the purpose of the invention, the organic protective agent can also be polyvinyl alcohol, polyvinylpyrrolidone, potassium sodium tartrate, polyacrylamide, citric acid, EDTA, fluorocarbon surfactant, and can be used singly or mixed by any two or more than two.
In order to further achieve the purpose of the invention, the surface coating agent can also be a titanate coupling agent, an aluminate coupling agent, a zirconate coupling agent or a boroaluminate coupling agent.
The invention adopts coprecipitation method, combines surface treatment and mechanical dispersion treatment, uses traditional material, uses some special dispersant, and uses coating treatment, and finally achieves antistatic, anti-glare and anti-radiation effects in use performance, through controlling precipitation condition, raising precipitation temperature between 60-150 ℃, using atomization adding method for reactant to accelerate reaction speed, and adding protective agent in system, using high temperature and high pressure baking method, controlling temperature at 250-900 ℃ to form composite metal oxide nano crystal, the aggregate is loose, using mechanical grinding dispersion treatment, adding special surfactant, high grinding dispersion efficiency and stable system, the invention is different from previous single metal oxide crystal ion preparation, and the invention compounds four metal oxides together, the proportion of the metal oxide and the metal oxide is controlled to meet the requirement of low electrical conductivity, and the finally formed conductive film can generate an uneven meteorite pit structure by adding the metal oxide with low refractive index, so that the aim of preventing glare is fulfilled.
The present invention will be described in further detail with reference to examples.
Example 1, 69.2g of tin chloride, 49.3g of antimony chloride, 35.6g of titanium chloride and 9.5g of zirconium chloride are weighed and completely dissolved in organic alcohol to prepare a solution, the organic alcohol can be methanol, the heating temperature is 150 ℃ for refluxing, the refluxing time is 8 hours, ammonia water is added to adjust the pH value to 10, precipitation is generated by reaction, an organic protective agent is added after the precipitate isfiltered out, in the embodiment, the organic protective agent is EDTA and potassium sodium tartrate, the hydrolysis is carried out at the temperature of 300 ℃ and the pressure of 30Mpa to generate the precipitate with the particle size of 5-30nm, the generated precipitate is washed with water and filtered, nitric acid, the EDTA and the potassium sodium tartrate are added to decompose the precipitate to form emulsion, then spray drying and granulation are carried out at the drying temperature of 300 ℃ to form composite hydroxide particles, the composite hydroxide particles are roasted at the temperature of 900 ℃ to form the particle size of less than 30nm, grinding the generated particles for 12 hours, placing the particles into a centrifuge, controlling the rotating speed at 10000-15000 r/min for grading and sorting, adding 30g of silane coupling agent and surface coating agent into the qualified products after grading, and concentrating to obtain the invention, wherein the surface coating agent is isopropyl tri (isostearoyl) titanate in the titanate coupling agent, the silane coupling agent is vinyl silane, and the final product contains 40g of tin oxide, 35g of antimony oxide, 15g of titanium oxide, 5g of zirconium oxide and 9g of silicon oxide.
Example 2, weighing 164.3g of tin chloride, 0.71g of antimony chloride, 0.24g of titanium chloride and 0.18g of zirconium chloride, completely dissolving the tin chloride in organic alcohol ethanol to prepare a solution, heating the solution to 60 ℃ for reflux, adding triethanolamine to adjust the pH value to 9.5, reacting to generate a precipitate, filtering the precipitate to remove precipitates, adding organic protective agents polyvinyl alcohol and polyvinyl pyrrolidone, hydrolyzing the solution at the temperature of 60 ℃ and the pressure of 0.1 Mpa to generate a precipitate with the particle size of 5-30nm, washing and filtering the generated precipitate, adding oxalic acid and a protective agent citric acid to decompose the precipitate to form an emulsion, then performing spray drying and granulation at the drying temperature of 300 ℃ to form composite hydroxide particles, roasting the composite hydroxide particles at the temperature of 250 ℃ to form loosely agglomerated particles with the particle size of less than 30nm and the particle size of less than 2 μm, grinding the generated particles for 4 hours, placing the particles into a centrifuge, controlling the rotating speed at 10000-15000 r/min for grading and sorting, adding 16.7g of silane coupling agent ureido silane and surface coating agent aluminum titanate into the qualified products after grading, and concentrating to obtain the product, wherein the final product contains 95g of tin oxide, 0.5g of antimony oxide, 0.1g of titanium oxide, 0.1g of zirconium oxide and 5g of silicon oxide.
Example 3, weighing 116.8g of tin chloride, 25g of antimony chloride, 18g of titanium chloride and 4.84g of zirconium chloride, completely dissolving the tin chloride, the antimony chloride, the titanium chloride and the zirconium chloride in isopropanol organic alcohol to prepare a solution, heating the solution to 110 ℃ for refluxing, wherein the refluxing time is 4.5 hours, adding diethylenetriamine to adjust the pH value to 9.6, reacting to generate a precipitate, filtering the precipitate to remove precipitates, adding an organic protective agent fluorocarbon surfactant FC-4, controlling the temperature to 180 ℃ and the pressure to hydrolyze under 15Mpa to generate a precipitate with the particle size of 5-30nm, washing and filtering the generated precipitate with water, adding phosphoric acid and a protective agent polyvinyl alcohol, peptizing to form an emulsion, spray drying and granulating at a drying temperature of 300 ℃ to form composite hydroxide particles, roasting the composite hydroxide particles at 550 ℃ to form loosely agglomerated particles with the particle size of less than 30nm and the particle sizeof less than 2 μm, grinding the generated particles for 8 hours, putting the particles into a centrifuge, controlling the rotating speed at 10000-15000 r/min for grading and sorting, adding 23.3g of silane coupling agent amido silane and surface coating agent triethanolamine titanate into the qualified products after grading, and concentrating to obtain the product, wherein the final product contains 67.5g of tin oxide, 17.8g of antimony oxide, 7.6g of titanium oxide, 2.6g of zirconium oxide and 7g of silicon oxide.
Example 4, weighing 140.6g of tin chloride, 12.9g of antimony chloride, 9.12g of titanium chloride and 2.5g of zirconium chloride, completely dissolving the tin chloride, the antimony chloride, the titanium chloride and the zirconium chloride in n-butanol, preparing a solution, heating to 85 ℃ for refluxing, adding diethanolamine to adjust the pH value to 9.7, reacting to generate a precipitate, filtering to remove the precipitate, adding polyvinylpyrrolidone serving as an organic protective agent, controlling the temperature to 120 ℃ and the pressure to hydrolyze under 8 Mpa to generate a precipitate with a particle size of 5-30nm, washing and filtering the generated precipitate with water, adding citric acid and fluorocarbon surfactant FC-3 serving as a protective agent to decompose the precipitate to form an emulsion, then performing spray drying and granulation at a drying temperature of 300 ℃ to form composite hydroxide particles, roasting the composite hydroxide particles at 400 ℃ to form loosely agglomerated particles with a crystal size of less than 30nm and a particle size of less than 2 μm, grinding the generated particles for 6 hours, putting the particles into a centrifuge, controlling the rotating speed at 10000-15000 r/min for grading and sorting, adding 20g of silane coupling agent aminopropyl silane and surface coating agent polybutyl titanate into the qualified products after grading, and concentrating to obtain the product, wherein the final product contains 81.3g of tin oxide, 9.2g of antimony oxide, 3.9g of titanium oxide, 1.4g of zirconium oxide and 6g of silicon oxide.
Example 5, 93g of tin chloride, 37g of antimony chloride, 27g of titanium chloride and 7.2g of zirconium chloride are weighed, and are completely dissolved in organic alcohol methanol to prepare a solution, the solution is heated to 240 ℃ for reflux, the reflux time is 7 hours, sodium hydroxide is added to adjust the pH value to 9.8, a precipitate is generated by reaction, an organic protective agent polyacrylamide is added after the precipitate is filtered out, hydrolysis is performed at the temperature of 240 ℃ and the pressure of 23Mpa to generate a precipitate with the particle size of 5-30nm, the generated precipitate is washed with water and filtered, sulfamic acid and a protective agent fluorocarbon surfactant FN-2 are added to be peptized to form emulsion, then spray drying and granulation are performed at the drying temperature of 300 ℃ to form composite hydroxide particles, the composite hydroxide particles are roasted at the temperature of 750 ℃ to form loose agglomerated particles with the particle size of less than 30nm and the particle size of less than 2 μm, grinding the generated particles for 10 hours, putting the particles into a centrifuge, controlling the rotating speed at 10000-15000 r/min for grading and sorting, adding 13.3g of silane coupling agent KH-560 and surface coating agent into the qualified product after grading, and then concentrating the aluminum tristearate to obtain the product, wherein the final product contains 53.8g of tin oxide, 26g of antimony oxide, 11.3g of titanium oxide, 3.8g of zirconium oxide and 4g of silicon oxide.
Claims (4)
1. A nanometer coating material is characterized by comprising the following components in percentage by weight: 40-95% of tin oxide, 0.5-35% of antimony oxide, 0.1-15% of titanium oxide, 0.1-5% of zirconium oxide and 0.1-15% of silicon oxide, wherein the grain size of the oxides is 5-30 nm.
2. The method for preparing a nano coating material according to claim 1, wherein the method comprises the following steps:
a. weighing required tin chloride, antimony chloride, titanium chloride and zirconium chloride, and completely dissolving in organic alcohol;
b. heating, and refluxing with alcohol at 60-150 deg.C for 1-8 hr;
c. then adding alkali, adjusting the pH value to be 9.5-10, and reacting to generate a precipitate, wherein the reaction formula is as follows:
a represents Sn, Sb, Zr and Ti, and X represents a natural number;
d. adding organic protective agent into the filtered liquid, controlling the reaction temperature at 60-300 deg.C and the pressure at 0.1-30Mpa, and hydrolyzing to obtain precipitate with particle size of 5-30 nm;
e. washing and filtering the precipitate, adding acid and an organic protective agent, and dispergating to form emulsion;
f. spraying and drying the emulsion at the drying temperature of 300 ℃ to form composite hydroxide particles;
g. roasting the composite hydroxide particles at the temperature of 250-900 ℃ to form loosely agglomerated particles with the grain size of less than 30nm and the granularity of less than 2 mu m, wherein the reaction formula is as follows:
h. grinding the generated particles for 4-12 hours, putting the particles into a centrifuge, and controlling the rotating speed at 10000-15000 r/min for classification and sorting.
g. Adding a silane coupling agent and a surface coating agent which account for 0.3-45% of the weight of the raw materials into a qualified product to generate a final product, wherein the reaction formula is as follows:
M(OH)x→MnOx+H2O
m represents Ti, Zr, Si, Sn, Sb, Et represents one or more C fatty alcohol groups.
h. And concentrating the final product to obtain the invention.
3. The method of claim 2, wherein the organic protective agent is selected from the group consisting of polyvinyl alcohol, polyvinylpyrrolidone, potassium sodium tartrate, polyacrylamide, citric acid, EDTA, and fluorocarbon surfactant, and the organic protective agent can be used alone or in combination of two or more.
4. The method of claim 2, wherein the surface coating agent is selected from the group consisting of titanate coupling agent, aluminate coupling agent, zirconate coupling agent, and boroaluminate coupling agent.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351323C (en) * | 2005-03-17 | 2007-11-28 | 中南大学 | Coating material and prepn. thereof |
| CN102815872A (en) * | 2012-09-06 | 2012-12-12 | 中电电气（南京）太阳能研究院有限公司 | Preparation method of antimony doped tin oxide nanopore transparent conducting film |
| CN105906895A (en) * | 2016-04-15 | 2016-08-31 | 佛山市聚成生化技术研发有限公司 | Preparation method of composite packing antistatic agent and antistatic agent prepared by method |
| CN109929344A (en) * | 2017-12-19 | 2019-06-25 | 中国科学院化学研究所 | Low-surface-energy high molecular material composite construction with high-adhesion and preparation method thereof |
| CN110499083A (en) * | 2019-09-05 | 2019-11-26 | 特普罗(深圳)应用科技有限公司 | A kind of display screen and its display material and preparation process of use |
| US12002602B2 (en) | 2019-07-29 | 2024-06-04 | Jiangsu Nanomeida Optoelectronics Technology Co., Ltd. | Optically consistent transparent conductive film and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100418394C (en) * | 2006-09-14 | 2008-09-10 | 同济大学 | Inorganic non-metallic conductivity, electromagnetic shielding powder and method for making same and application |
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2000
- 2000-11-24 CN CNB001293583A patent/CN1137223C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100351323C (en) * | 2005-03-17 | 2007-11-28 | 中南大学 | Coating material and prepn. thereof |
| CN102815872A (en) * | 2012-09-06 | 2012-12-12 | 中电电气（南京）太阳能研究院有限公司 | Preparation method of antimony doped tin oxide nanopore transparent conducting film |
| CN105906895A (en) * | 2016-04-15 | 2016-08-31 | 佛山市聚成生化技术研发有限公司 | Preparation method of composite packing antistatic agent and antistatic agent prepared by method |
| CN105906895B (en) * | 2016-04-15 | 2018-05-04 | 佛山市南海区承欣塑料助剂有限公司 | A kind of preparation method of compound filler antistatic agent and the antistatic agent prepared by this method |
| CN109929344A (en) * | 2017-12-19 | 2019-06-25 | 中国科学院化学研究所 | Low-surface-energy high molecular material composite construction with high-adhesion and preparation method thereof |
| CN109929344B (en) * | 2017-12-19 | 2020-07-14 | 中国科学院化学研究所 | Low-surface-energy polymer material composite structure with high cohesiveness and preparation method thereof |
| US12002602B2 (en) | 2019-07-29 | 2024-06-04 | Jiangsu Nanomeida Optoelectronics Technology Co., Ltd. | Optically consistent transparent conductive film and preparation method thereof |
| CN110499083A (en) * | 2019-09-05 | 2019-11-26 | 特普罗(深圳)应用科技有限公司 | A kind of display screen and its display material and preparation process of use |
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| CN1137223C (en) | 2004-02-04 |
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