CN115536383B - High-density ITO green body sintering method with accurate process control - Google Patents
High-density ITO green body sintering method with accurate process control Download PDFInfo
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Abstract
The invention relates to the technical field of ITO green body sintering, and particularly discloses a high-density ITO green body sintering method with accurate process control, which comprises the following steps of: the method comprises the following steps: taking 55-65 parts of ITO powder and 3-6 parts of modified hydroxyapatite; step two: uniformly mixing the raw materials in the step one, then adding the raw materials into 2-3 times of graphene compounded nano silicon dioxide modified solution, stirring and reacting, and performing step three: selecting a substrate, and then carrying out sputtering treatment; step four: and finally, sintering at 1550-1650 ℃ for 25-35min, and cooling to room temperature to obtain the high-density ITO green body after sintering. The modified hydroxyapatite and the graphene compounded nano silicon dioxide modified liquid are synergistic, so that the density and the transmission performance of the product are enhanced, and the use efficiency of the product is improved.
Description
Technical Field
The invention relates to the technical field of ITO green body sintering, in particular to a high-density ITO green body sintering method with accurate process control.
Background
The main component of ITO (indium tin oxide) is a composite oxide in which tin oxide is solid-dissolved in indium oxide. ITO has excellent photoelectric properties, and ITO-containing films have high conductivity and visible light transmittance, and are widely used in various fields such as solar cells, liquid crystal display devices, and touch panels. Methods for preparing ITO thin film include sputtering method, vacuum evaporation method, sol-gel method, cluster deposition method, and PLD method
The existing ITO green body is sintered to improve the density of a product, but the infrared transmission performance of the product is reduced, and therefore, the invention optimizes the density and the infrared transmission performance of the product in a coordinated and improved mode, and further improves the treatment process based on the optimization.
Disclosure of Invention
In view of the defects of the prior art, the present invention aims to provide a sintering method for a high-density ITO green body with precise process control, so as to solve the problems in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a high-density ITO green body sintering method with accurate process control, which comprises the following steps:
the method comprises the following steps: taking 55-65 parts of ITO powder and 3-6 parts of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, then adding the mixture into 2-3 times of graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1550-1650 ℃ for 25-35min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
Preferably, the temperature of the stirring reaction treatment in the second step is 55-65 ℃, the stirring speed is 450-500r/min, and the stirring time is 30-40min.
Preferably, the temperature of the sputtering treatment is 185-188 ℃, the sputtering time is 1.2-1.3h, the vacuum degree is 5-7Pa, and the target base distance is 6.3-6.5cm.
Preferably, the preparation method of the modified hydroxyapatite comprises the following steps:
s01: adding hydroxyapatite into 3-5 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 1-3 parts of lanthanum sulfate, 1-5 parts of sodium alkyl sulfate and 3-5 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 5-10% of the total amount of the S01 product, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The inventor finds that the relative density and the average transmittance in a near infrared region of a product have a remarkably poor trend without adding modified hydroxyapatite and adopting graphene compounded nano silicon dioxide modified liquid for treatment;
the modified hydroxyapatite is replaced by hydroxyapatite, the performance of the product is not changed greatly, meanwhile, no additive is added in the preparation of the modified hydroxyapatite, no sodium alkyl sulfate is added in the preparation of the additive, the silane coupling agent solution is replaced by the silane coupling agent KH560 and deionized water according to the weight ratio of 1.
Preferably, the particle size of the hydroxyapatite is 3.5-4.5um.
Preferably, the preparation method of the silane coupling agent liquid comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to a weight ratio of 1; then adding hydrochloric acid accounting for 10-20% of the total amount of the silane coupling agent and sodium alginate accounting for 1-5% of the total amount of the silane coupling agent, and fully stirring and mixing to obtain silane coupling agent liquid.
Preferably, the silane coupling agent is a coupling agent KH560.
The inventor finds that only when the modified hydroxyapatite prepared by the method is matched with the graphene compounded nano silicon dioxide modified solution for treatment, the density and the average transmittance in a near infrared region of the product can form a coordinated improvement effect, and the performance effect of the product is not as obvious as that of the method provided by the invention when the modified hydroxyapatite is replaced by other methods.
Preferably, the preparation method of the graphene compounded nano silicon dioxide modified liquid comprises the following steps:
s11: adding nano silicon dioxide into 4-6 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 10-20% of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 1-5% of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding the graphene into a heat treatment furnace for thermal reaction for 10-20min, wherein the thermal reaction temperature is 300-350 ℃, and recovering to room temperature after the thermal reaction is finished;
s13: placing the graphene in 2-3 times of potassium permanganate aqueous solution, carrying out heat treatment at 45-55 ℃ for 10-20min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
Preferably, the mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution are respectively 10-20% and 20-30%.
Preferably, the pH value of the phosphoric acid buffer solution is 4.5-5.5.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, ITO powder is matched with modified hydroxyapatite, then graphene compounded nano silicon dioxide modification liquid is used for stirring, dispersing and modifying, graphene sheet-shaped structure in the graphene compounded nano silicon dioxide modification liquid is matched with nano silicon dioxide with high specific surface area for coordination, and the raw materials of the modified ITO powder, the modified hydroxyapatite and the graphene compounded nano silicon dioxide modification liquid are coordinated and enhanced, so that the density and the transmission performance of the product are enhanced, and the use efficiency of the product is improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The high-density ITO green body sintering method with accurate process control in the embodiment comprises the following steps:
the method comprises the following steps: taking 55-65 parts of ITO powder and 3-6 parts of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, then adding the mixture into 2-3 times of graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1550-1650 ℃ for 25-35min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
In the second step of this embodiment, the temperature of the stirring reaction treatment is 55-65 ℃, the stirring speed is 450-500r/min, and the stirring time is 30-40min.
The temperature of the sputtering treatment of the embodiment is 185-188 ℃, the sputtering time is 1.2-1.3h, the vacuum degree is 5-7Pa, and the target base distance is 6.3-6.5cm.
The preparation method of the modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding hydroxyapatite into 3-5 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 1-3 parts of lanthanum sulfate, 1-5 parts of sodium alkyl sulfate and 3-5 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 5-10% of the total amount into the product S01, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The particle size of the hydroxyapatite in this example is 3.5-4.5um.
The preparation method of the silane coupling agent liquid in the embodiment comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to a weight ratio of 1; then adding hydrochloric acid accounting for 10-20% of the total amount of the silane coupling agent and sodium alginate accounting for 1-5% of the total amount of the silane coupling agent, and fully stirring and mixing to obtain silane coupling agent liquid.
The silane coupling agent of the present example is a coupling agent KH560.
The preparation method of the graphene compounded nano silicon dioxide modification liquid comprises the following steps:
s11: adding nano silicon dioxide into 4-6 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 10-20% of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 1-5% of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding the graphene into a heat treatment furnace for thermal reaction for 10-20min, wherein the thermal reaction temperature is 300-350 ℃, and recovering to room temperature after the thermal reaction is finished;
s13: placing the graphene in 2-3 times of potassium permanganate aqueous solution, carrying out heat treatment at 45-55 ℃ for 10-20min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
The mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution in the embodiment are 10-20% and 20-30%, respectively.
The pH of the phosphate buffer solution of this example was 4.5-5.5.
Example 1.
The high-density ITO green body sintering method with accurate process control in the embodiment comprises the following steps:
the method comprises the following steps: taking 55 parts by weight of ITO powder and 3 parts by weight of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, adding the mixture into 2-time graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1550 ℃ for 25min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
In the second step of this example, the temperature of the stirring reaction treatment is 55 ℃, the stirring speed is 450r/min, and the stirring time is 30min.
The temperature of the sputtering treatment in this example was 185 ℃, the sputtering time was 1.2 hours, the degree of vacuum was 5Pa, and the target base distance was 6.3cm.
The preparation method of the modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding hydroxyapatite into 3 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 1 part of lanthanum sulfate, 1 part of sodium alkyl sulfate and 3 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 5 percent of the total amount into the product S01, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The hydroxyapatite of this example had a particle size of 3.5um.
The preparation method of the silane coupling agent liquid in the embodiment comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to a weight ratio of 1; then adding hydrochloric acid accounting for 10% of the total amount of the silane coupling agent and sodium alginate accounting for 1% of the total amount of the silane coupling agent, and fully stirring and mixing to obtain a silane coupling agent solution.
The silane coupling agent of the present example is a coupling agent KH560.
The preparation method of the graphene compounded nano silicon dioxide modification liquid comprises the following steps:
s11: adding nano silicon dioxide into 4 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 10 percent of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 1 percent of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding graphene into a heat treatment furnace for thermal reaction for 10min, wherein the thermal reaction temperature is 300 ℃, and after the thermal reaction is finished, recovering the temperature to room temperature;
s13: placing graphene in 2 times of potassium permanganate aqueous solution, carrying out heat treatment at 45 ℃ for 10min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
The mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution in this example were 10% and 20%, respectively.
The pH of the phosphate buffer solution of this example was 4.5.
Example 2.
The high-density ITO green body sintering method with accurate process control in the embodiment comprises the following steps:
the method comprises the following steps: taking 65 parts by weight of ITO powder and 6 parts by weight of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, adding the mixture into 3 times of graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1650 ℃ for 35min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
In the second step of this example, the temperature of the stirring reaction treatment is 65 ℃, the stirring speed is 500r/min, and the stirring time is 40min.
The temperature of the sputtering treatment in this example was 188 ℃, the sputtering time was 1.3 hours, the degree of vacuum was 7Pa, and the target pitch was 6.5cm.
The preparation method of the modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding hydroxyapatite into 5 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 3 parts of lanthanum sulfate, 5 parts of sodium alkyl sulfate and 5 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 10 percent of the total amount into the product S01, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The particle size of the hydroxyapatite in this example was 4.5um.
The preparation method of the silane coupling agent liquid in the embodiment comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to a weight ratio of 1; then adding hydrochloric acid accounting for 20% of the total amount of the silane coupling agent and sodium alginate accounting for 5% of the total amount of the silane coupling agent, and fully stirring and mixing to obtain a silane coupling agent solution.
The silane coupling agent of the present example is a coupling agent KH560.
The preparation method of the graphene compounded nano silicon dioxide modification liquid comprises the following steps:
s11: adding nano silicon dioxide into 6 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 20 percent of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 5 percent of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding the graphene into a heat treatment furnace for thermal reaction for 20min, wherein the thermal reaction temperature is 350 ℃, and recovering to room temperature after the thermal reaction is finished;
s13: placing graphene in 3 times of potassium permanganate aqueous solution, carrying out heat treatment at 55 ℃ for 20min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
The mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution in the examples were 20% and 30%, respectively.
The pH of the phosphate buffer solution of this example was 5.5.
Example 3.
The high-density ITO green body sintering method with accurate process control in the embodiment comprises the following steps:
the method comprises the following steps: taking 60 parts by weight of ITO powder and 4.5 parts by weight of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, then adding the mixture into 2.5 times of graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1600 ℃ for 30min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
In the second step of this example, the temperature of the stirring reaction treatment is 60 ℃, the stirring speed is 470r/min, and the stirring time is 35min.
The temperature of the sputtering treatment in this example was 186 ℃, the sputtering time was 1.25 hours, the degree of vacuum was 6Pa, and the target pitch was 6.4cm.
The preparation method of the modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding hydroxyapatite into 4 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 2 parts of lanthanum sulfate, 3 parts of sodium alkyl sulfate and 4 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 7.5 percent of the total amount into the product S01, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The particle size of the hydroxyapatite in this example was 4.0um.
The preparation method of the silane coupling agent liquid in the embodiment comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to the weight ratio of 1; then adding hydrochloric acid accounting for 15% of the total amount of the silane coupling agent and sodium alginate accounting for 3% of the total amount of the silane coupling agent, and fully stirring and mixing to obtain a silane coupling agent solution.
The silane coupling agent of the present example is a coupling agent KH560.
The preparation method of the graphene compounded nano silicon dioxide modification liquid comprises the following steps:
s11: adding nano silicon dioxide into 5 times of chitosan aqueous solution, and then adding 15% of carboxymethyl cellulose and 3% of phosphoric acid buffer solution of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding graphene into a heat treatment furnace for thermal reaction for 15min, wherein the thermal reaction temperature is 325 ℃, and after the thermal reaction is finished, recovering to room temperature;
s13: placing graphene in 2.5 times of potassium permanganate aqueous solution, carrying out heat treatment at 50 ℃ for 15min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
The mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution in the embodiment are 10-20% and 20-30%, respectively.
The pH of the phosphate buffer solution of this example was 4.5-5.5.
Example 4.
The high-density ITO green body sintering method with accurate process control in the embodiment comprises the following steps:
the method comprises the following steps: taking 57 parts by weight of ITO powder and 4 parts by weight of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, then adding the mixture into 2.2 times of graphene compounded nano silicon dioxide modified solution, stirring for reaction treatment,
step three: selecting a substrate, and then carrying out sputtering treatment;
step four: and finally, sintering at 1570 ℃ for 28min, and cooling to room temperature to obtain the high-density ITO green body after sintering.
In the second step of this example, the temperature of the stirring reaction treatment is 57 ℃, the stirring speed is 460r/min, and the stirring time is 32min.
The temperature of the sputtering treatment in this example was 186 ℃, the sputtering time was 1.2 hours, the degree of vacuum was 6Pa, and the target pitch was 6.4cm.
The preparation method of the modified hydroxyapatite of the embodiment comprises the following steps:
s01: adding hydroxyapatite into 4 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 2 parts of lanthanum sulfate, 2 parts of sodium alkyl sulfate and 4 parts of silica sol to obtain an additive;
s03: and (3) adding an additive accounting for 6 percent of the total amount into the product S01, stirring and mixing fully, washing with water, and drying to obtain the modified hydroxyapatite.
The particle size of the hydroxyapatite in this example was 3.6um.
The preparation method of the silane coupling agent liquid in the embodiment comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to the weight ratio of 1; then, hydrochloric acid accounting for 12% of the total amount of the silane coupling agent and sodium alginate accounting for 2% of the total amount of the silane coupling agent are added, and the mixture is stirred and fully mixed to obtain silane coupling agent liquid.
The silane coupling agent of the present example is a coupling agent KH560.
The preparation method of the graphene compounded nano silicon dioxide modification liquid comprises the following steps:
s11: adding nano silicon dioxide into 5 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 12 percent of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 2 percent of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding graphene into a heat treatment furnace for thermal reaction for 12min, wherein the thermal reaction temperature is 310 ℃, and recovering to room temperature after the thermal reaction is finished;
s13: placing graphene in 2.2 times of potassium permanganate aqueous solution, carrying out heat treatment at 46 ℃ for 12min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
The mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution in this example were 12% and 20-30%, respectively.
The pH of the phosphate buffer solution of this example was 4.6.
Comparative example 1.
In contrast to example 3, no modified hydroxyapatite was added.
Comparative example 2.
The difference from the embodiment 3 is that the modified hydroxyapatite is replaced by hydroxyapatite.
Comparative example 3.
The difference from example 3 is that no additive was added in the preparation of the modified hydroxyapatite.
Comparative example 4.
The difference from example 3 is that no sodium alkyl sulphate was added in the preparation of the additive.
Comparative example 5.
The difference from the example 3 is that the silane coupling agent solution is replaced by a silane coupling agent KH560 and deionized water according to the weight ratio of 1.
Comparative example 6.
Different from the embodiment 3, the method does not adopt the graphene compounded nano silicon dioxide modified solution for treatment.
Comparative example 7.
Different from the embodiment 3, the pre-modified graphene is not added in the preparation of the graphene compounded nano silicon dioxide modified solution.
As can be seen from comparative examples 1 to 7 and examples 1 to 4; according to the invention, no modified hydroxyapatite is added, and no graphene compounded nano silicon dioxide modification solution is adopted for treatment, so that the relative density and the near infrared region average transmittance of the product have a remarkable deterioration trend;
the modified hydroxyapatite is replaced by hydroxyapatite, the performance of the product is not changed greatly, meanwhile, no additive is added in the preparation of the modified hydroxyapatite, no sodium alkyl sulfate is added in the preparation of the additive, the silane coupling agent solution is replaced by the silane coupling agent KH560 and deionized water according to the weight ratio of 1;
only when the modified hydroxyapatite prepared by the method is matched with the graphene compounded nano silicon dioxide modified solution for treatment, the density and the average transmittance in a near infrared region of the product can form a coordinated improvement effect, and other methods are adopted for substitution, so that the performance effect of the product is not as obvious as that of the method.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A sintering method of a high-density ITO green body with accurate process control is characterized by comprising the following steps:
the method comprises the following steps: taking 55-65 parts of ITO powder and 3-6 parts of modified hydroxyapatite;
step two: uniformly mixing the raw materials in the step one, then adding the raw materials into 2-3 times of graphene compounded nano silicon dioxide modified solution, and stirring for reaction treatment;
step three: finally, carrying out sintering treatment again, wherein the sintering temperature is 1550-1650 ℃, the sintering time is 25-35min, and cooling to room temperature after sintering;
step four: selecting a substrate, and then carrying out sputtering treatment; obtaining a high-density ITO green body;
the preparation method of the modified hydroxyapatite comprises the following steps:
s01: adding hydroxyapatite into 3-5 times of silane coupling agent liquid, and stirring and dispersing uniformly;
s02: stirring and mixing 1-3 parts of lanthanum sulfate, 1-5 parts of sodium alkyl sulfate and 3-5 parts of silica sol to obtain an additive;
s03: s01, adding an additive accounting for 5-10% of the total amount into the product, stirring and mixing fully, washing with water, and drying to obtain modified hydroxyapatite;
the preparation method of the silane coupling agent liquid comprises the following steps:
stirring, preparing and mixing a silane coupling agent and deionized water according to a weight ratio of 1; then adding hydrochloric acid accounting for 10-20% of the total amount of the silane coupling agent and sodium alginate accounting for 1-5% of the total amount of the silane coupling agent, and stirring and mixing fully to obtain silane coupling agent liquid;
the preparation method of the graphene compounded nano silicon dioxide modified liquid comprises the following steps:
s11: adding nano silicon dioxide into 4-6 times of chitosan aqueous solution, and then adding carboxymethyl cellulose accounting for 10-20% of the total amount of the nano silicon dioxide and phosphoric acid buffer solution accounting for 1-5% of the total amount of the nano silicon dioxide to obtain nano silicon dioxide solution;
s12: feeding the graphene into a heat treatment furnace for thermal reaction for 10-20min, wherein the thermal reaction temperature is 300-350 ℃, and recovering to room temperature after the thermal reaction is finished;
s13: placing the graphene in 2-3 times of potassium permanganate aqueous solution, carrying out heat treatment at 45-55 ℃ for 10-20min, washing with water, and drying to obtain pre-modified graphene;
s14: and (3) fully stirring and mixing the pre-modified graphene and the nano silicon dioxide solution according to the weight ratio of 1.
2. The sintering method of the high-density ITO green body with the accurate process control according to claim 1, wherein the temperature of the stirring reaction treatment in the second step is 55-65 ℃, the stirring speed is 450-500r/min, and the stirring time is 30-40min.
3. The sintering method of the high-density ITO green body with the accurate process control according to claim 1, wherein the sputtering temperature is 185-188 ℃, the sputtering time is 1.2-1.3h, the vacuum degree is 5-7Pa, and the target base distance is 6.3-6.5cm.
4. The sintering method of the high-density ITO green body with the accurate process control according to claim 1, wherein the particle size of the hydroxyapatite is 3.5-4.5 μm.
5. The sintering method of the high-density ITO green body with accurate process control according to claim 1, wherein the silane coupling agent is KH560.
6. The sintering method of the high-density ITO green body with the accurate process control according to claim 1, wherein the mass fractions of the chitosan aqueous solution and the potassium permanganate aqueous solution are 10-20% and 20-30%, respectively.
7. The sintering method of the high-density ITO green body with the accurate process control according to claim 1, wherein the pH value of the phosphoric acid buffer solution is 4.5-5.5.
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