CN117902880A - ITO target material with high transparency and preparation method thereof - Google Patents
ITO target material with high transparency and preparation method thereof Download PDFInfo
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- CN117902880A CN117902880A CN202410309499.8A CN202410309499A CN117902880A CN 117902880 A CN117902880 A CN 117902880A CN 202410309499 A CN202410309499 A CN 202410309499A CN 117902880 A CN117902880 A CN 117902880A
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- hydroxyapatite
- ito target
- high transparency
- nitrate solution
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- 239000013077 target material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims description 18
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 56
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 24
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 20
- 230000004048 modification Effects 0.000 claims abstract description 20
- 238000012986 modification Methods 0.000 claims abstract description 20
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 15
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical group [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 15
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims abstract description 14
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 8
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000001509 sodium citrate Substances 0.000 claims abstract description 8
- 239000008117 stearic acid Substances 0.000 claims abstract description 8
- 238000000498 ball milling Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 238000005245 sintering Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000007654 immersion Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000002715 modification method Methods 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 238000002834 transmittance Methods 0.000 abstract description 5
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to the technical field of ITO targets, and particularly discloses an ITO target with high transparency, wherein the ITO target is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1. The ITO target material is prepared from indium oxide and tin oxide, sodium citrate solution, silane coupling agent, yttrium nitrate solution and modified hydroxyapatite in the modified liquid are mutually prepared through ultrasonic modification and infiltration treatment of the modified liquid, a target material matrix is jointly optimized, and meanwhile, the adopted hydroxyapatite is jointly ball-milled and improved through raw materials such as nano silica sol, stearic acid, lanthanum nitrate solution, nano titanium dioxide and the like, so that the target material improved by the modified hydroxyapatite obtained through matching with the modified liquid can realize coordinated improvement of light transmittance and conductivity of a product.
Description
Technical Field
The invention relates to the technical field of ITO targets, in particular to an ITO target with high transparency and a preparation method thereof.
Background
ITO thin films are commonly used in the fields of liquid crystal displays, photovoltaic cells, etc., and therefore, their transparency is an important performance index. The increase of the indium content in the target material can improve the transparency of the film. This is because indium has a higher electron affinity and can promote the formation of a dense lattice structure in the oxide, thereby reducing scattering.
The existing ITO target material has poor light transmittance, so that the light transmittance of the product is improved, the poor conductivity of the product is easily caused, the light transmittance and conductivity coordination of the product are difficult to realize, and the use efficiency of the product is limited.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide an ITO target material with high transparency and a preparation method thereof, so as to solve the problems in the prior art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides an ITO target with high transparency, which is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1.
The invention also provides a preparation method of the ITO target with high transparency, which comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying solution for modification treatment, washing with water, drying, sintering the dried product at 1150-1250 ℃ for 1-2h, cooling to 210-230 ℃ at a speed of 2-5 ℃/min after sintering, preserving heat for 5-10min, and finally cooling to room temperature at a speed of 1-3 ℃/min.
Preferably, the operation steps of the immersion modification treatment are as follows:
Adding 2-5 parts of silane coupling agent into 6-10 parts of sodium citrate solution with the mass fraction of 10%, then adding 1-3 parts of yttrium nitrate solution and 2-4 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
Immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 350-400W, the ultrasonic time is 15-20min, and the method comprises the steps of ultrasonic finishing, water washing and drying.
The inventor of the invention finds that the performance of the product is obviously degraded without immersing in the modified liquid, the modified hydroxyapatite is not added in the modified liquid, the modified hydroxyapatite is replaced by the hydroxyapatite, the nano titanium dioxide, the nano silica sol is not added in the preparation of the modified hydroxyapatite, the lanthanum nitrate solution is replaced by deionized water in the preparation of the modified hydroxyapatite, and the performance of the product is degraded.
Preferably, the silane coupling agent is a silane coupling agent KH560.
Preferably, the yttrium nitrate solution has a mass fraction of 2-5%.
Preferably, the modification method of the modified hydroxyapatite comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 6-10 parts of the hydroxyapatite, 1-3 parts of nano silica sol, 2-4 parts of stearic acid, 5-7 parts of lanthanum nitrate solution and 0.25-0.30 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
Preferably, the lanthanum nitrate solution has a mass fraction of 2-5%.
Preferably, the lanthanum nitrate solution has a mass fraction of 3.5%.
Preferably, the ball milling speed of the ball milling treatment is 1000-1500r/min, and the ball milling time is 1-2h.
Compared with the prior art, the invention has the following beneficial effects:
The ITO target material is prepared from indium oxide and tin oxide, sodium citrate solution, silane coupling agent, yttrium nitrate solution and modified hydroxyapatite in the modified liquid are mutually prepared through ultrasonic modification and infiltration treatment of the modified liquid, a target material matrix is jointly optimized, and meanwhile, the adopted hydroxyapatite is jointly ball-milled and improved through raw materials such as nano silica sol, stearic acid, lanthanum nitrate solution, nano titanium dioxide and the like, so that the target material improved by the modified hydroxyapatite obtained through matching with the modified liquid can realize coordinated improvement of light transmittance and conductivity of a product.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
An ITO target material with high transparency in this embodiment is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1.
The preparation method of the ITO target with high transparency comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying solution for modification treatment, washing with water, drying, sintering the dried product at 1150-1250 ℃ for 1-2h, cooling to 210-230 ℃ at a speed of 2-5 ℃/min after sintering, preserving heat for 5-10min, and finally cooling to room temperature at a speed of 1-3 ℃/min.
The immersion operation steps of this embodiment are:
Adding 2-5 parts of silane coupling agent into 6-10 parts of sodium citrate solution with the mass fraction of 10%, then adding 1-3 parts of yttrium nitrate solution and 2-4 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
Immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 350-400W, the ultrasonic time is 15-20min, and the method comprises the steps of ultrasonic finishing, water washing and drying.
The silane coupling agent of this example is a silane coupling agent KH560.
The mass fraction of the yttrium nitrate solution in the embodiment is 2-5%.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 6-10 parts of the hydroxyapatite, 1-3 parts of nano silica sol, 2-4 parts of stearic acid, 5-7 parts of lanthanum nitrate solution and 0.25-0.30 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
The mass fraction of the lanthanum nitrate solution in the embodiment is 2-5%.
The lanthanum nitrate solution of this example has a mass fraction of 3.5%.
The ball milling speed of the ball milling treatment in the embodiment is 1000-1500r/min, and the ball milling time is 1-2h.
Example 1
An ITO target material with high transparency in this embodiment is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1.
The preparation method of the ITO target with high transparency comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying liquid for modification treatment, washing with water, drying, thermally sintering the dried product at 1150 ℃ for 1h, cooling to 210 ℃ at a speed of 2 ℃/min after sintering, preserving heat for 5min, and finally air-cooling to room temperature at a speed of 1 ℃/min.
The immersion modification treatment of this embodiment comprises the following steps:
Adding 2 parts of silane coupling agent into 6 parts of sodium citrate solution with the mass fraction of 10%, then adding 1 part of yttrium nitrate solution and 2 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 350W, the ultrasonic time is 15min, and the method comprises the steps of ultrasonic ending, water washing and drying.
The silane coupling agent of this example is a silane coupling agent KH560.
The mass fraction of the yttrium nitrate solution of this example was 2%.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 6 parts of the hydroxyapatite, 1 part of nano silica sol, 2 parts of stearic acid, 5 parts of lanthanum nitrate solution and 0.25 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
The lanthanum nitrate solution of this example has a mass fraction of 2%.
The ball milling speed of the ball milling treatment in this example was 1000r/min and the ball milling time was 1h.
Example 2
An ITO target material with high transparency in this embodiment is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1.
The preparation method of the ITO target with high transparency comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying liquid for modification treatment, washing with water, drying, thermally sintering the dried product at 1250 ℃ for 2 hours, cooling to 230 ℃ at a speed of 5 ℃/min after sintering, preserving heat for 10min, and finally air-cooling to room temperature at a speed of 3 ℃/min.
The immersion modification treatment of this embodiment comprises the following steps:
adding 5 parts of silane coupling agent into 10 parts of sodium citrate solution with the mass fraction of 10%, then adding 3 parts of yttrium nitrate solution and 4 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
Immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 400W, the ultrasonic time is 20min, and the method comprises the steps of ultrasonic ending, water washing and drying.
The silane coupling agent of this example is a silane coupling agent KH560.
The mass fraction of the yttrium nitrate solution of this example was 5%.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 10 parts of the hydroxyapatite, 3 parts of nano silica sol, 4 parts of stearic acid, 7 parts of lanthanum nitrate solution and 0.30 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
The lanthanum nitrate solution of this example was 5% by mass.
The ball milling speed of the ball milling treatment in this example was 1500r/min and the ball milling time was 2h.
Example 3
An ITO target material with high transparency in this embodiment is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1.
The preparation method of the ITO target with high transparency comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying solution for modification treatment, washing with water, drying, thermally sintering the dried product at 1200 ℃ for 1.5h, cooling to 220 ℃ at a speed of 3.5 ℃/min after sintering, preserving heat for 7.5min, and finally cooling to room temperature at a speed of 2 ℃/min.
The immersion modification treatment of this embodiment comprises the following steps:
adding 3.5 parts of silane coupling agent into 8 parts of sodium citrate solution with the mass fraction of 10%, then adding 2 parts of yttrium nitrate solution and 3 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
Immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 370W, the ultrasonic time is 17min, and the method comprises the steps of ultrasonic ending, water washing and drying.
The silane coupling agent of this example is a silane coupling agent KH560.
The mass fraction of the yttrium nitrate solution of this example was 3.5%.
The modification method of the modified hydroxyapatite of the embodiment comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 8 parts of the hydroxyapatite, 2 parts of nano silica sol, 3 parts of stearic acid, 6 parts of lanthanum nitrate solution and 0.28 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
The lanthanum nitrate solution of this example has a mass fraction of 3.5%.
The ball milling speed of the ball milling treatment in this example was 1250r/min and the ball milling time was 1.5h.
Comparative example 1.
Unlike example 3, the immersion modification liquid treatment was not employed.
Comparative example 2.
The difference from example 3 is that no modified hydroxyapatite was added to the modified liquid.
Comparative example 3.
The difference from example 3 is that the modified hydroxyapatite is replaced with hydroxyapatite.
Comparative example 4.
The difference from example 3 is that no nano titanium dioxide or nano silica sol is added in the preparation of the modified hydroxyapatite.
Comparative example 5.
The difference from example 3 is that the lanthanum nitrate solution was replaced with deionized water in the preparation of the modified hydroxyapatite.
The results of the performance measurements of examples 1-3 and comparative examples 1-5 are as follows
From examples 1 to 3 and comparative examples 1 to 5,
The product of the embodiment 3 has high light transmission performance and excellent electric conduction performance, and the compatibility effect of the two performances is obvious;
As can be seen from comparative examples 1 to 5, the performance of the product is obviously degraded without being treated by immersing in the modified liquid, and meanwhile, modified hydroxyapatite is not added in the modified liquid, the modified hydroxyapatite is replaced by hydroxyapatite, nano titanium dioxide, nano silica sol and lanthanum nitrate solution in the preparation of the modified hydroxyapatite are not added in the preparation of the modified hydroxyapatite, deionized water is replaced, the performance of the product is degraded, and the modified liquid prepared by the method has the most obvious performance effect;
The invention has the innovation points that the performance of the product is obviously deteriorated without immersing in the modified liquid, the modified hydroxyapatite is not added in the modified liquid, the modified hydroxyapatite is replaced by the hydroxyapatite, the nano titanium dioxide, the nano silica sol is not added in the preparation of the modified hydroxyapatite, the lanthanum nitrate solution is replaced by the deionized water in the preparation of the modified hydroxyapatite, and the performance of the product is deteriorated.
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 characteristics 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 disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (6)
1. An ITO target material with high transparency is characterized in that the ITO target material is indium oxide: the tin oxide is prepared according to the weight ratio of 99:1;
the preparation method of the ITO target with high transparency comprises the following steps:
Mixing indium oxide and tin oxide thoroughly, immersing in a modifying solution for modification treatment, washing with water, drying, sintering the dried product at 1150-1250 ℃ for 1-2h, cooling to 210-230 ℃ at a speed of 2-5 ℃/min after sintering, preserving heat for 5-10min, and finally cooling to room temperature at a speed of 1-3 ℃/min;
The immersion modification treatment comprises the following operation steps:
Adding 2-5 parts of silane coupling agent into 6-10 parts of sodium citrate solution with the mass fraction of 10%, then adding 1-3 parts of yttrium nitrate solution and 2-4 parts of modified hydroxyapatite, and stirring fully to obtain modified liquid;
Immersing the ITO target material into a sufficient amount of modifying liquid for ultrasonic modification treatment, wherein the ultrasonic power is 350-400W, the ultrasonic time is 15-20min, and the method comprises the steps of ultrasonic finishing, water washing and drying;
the modification method of the modified hydroxyapatite comprises the following steps:
And (3) uniformly stirring and mixing the hydroxyapatite in a sufficient amount of potassium permanganate solution with the mass fraction of 5%, washing with water and drying, and then ball-milling 6-10 parts of the hydroxyapatite, 1-3 parts of nano silica sol, 2-4 parts of stearic acid, 5-7 parts of lanthanum nitrate solution and 0.25-0.30 part of nano titanium dioxide in a ball mill, wherein the ball milling is finished, washing with water and drying to obtain the hydroxyapatite.
2. The ITO target material having high transparency according to claim 1, wherein the silane coupling agent is a silane coupling agent KH560.
3. An ITO target having high transparency according to claim 1, wherein the mass fraction of the yttrium nitrate solution is 2-5%.
4. An ITO target having high transparency according to claim 1, wherein the lanthanum nitrate solution has a mass fraction of 2-5%.
5. An ITO target having high transparency according to claim 1, wherein the lanthanum nitrate solution has a mass fraction of 3.5%.
6. The ITO target with high transparency according to claim 1, wherein the ball milling speed of the ball milling treatment is 1000-1500r/min and the ball milling time is 1-2h.
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| CN202410309499.8A CN117902880B (en) | 2024-03-19 | ITO target material with high transparency and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202410309499.8A CN117902880B (en) | 2024-03-19 | ITO target material with high transparency and preparation method thereof |
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| CN117902880B CN117902880B (en) | 2024-05-28 |
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| CN114956790A (en) * | 2022-07-28 | 2022-08-30 | 广州市尤特新材料有限公司 | Near-infrared high-transmittance TCO (transparent conductive oxide) target material and preparation method thereof |
| CN115536383A (en) * | 2022-11-02 | 2022-12-30 | 株洲火炬安泰新材料有限公司 | High-density ITO green body sintering method with accurate process control |
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