CN113233872A - Amorphous indium tungsten oxide target and preparation method thereof - Google Patents
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Abstract
The invention discloses an amorphous indium tungsten oxide target and a preparation method thereof, and relates to the technical field of amorphous oxide semiconductors. The preparation method of the amorphous indium-tungsten oxide target material comprises the following steps: (1) preparing a fine mixed material of indium oxide and tungsten trioxide; (2) taking part of the fine mixed material for granulation, and preparing a coarse mixed material; (3) respectively sintering the fine mixed material and the coarse mixed material; (4) ball-milling the sintered fine mixed material, mixing the fine mixed material with the sintered coarse mixed material, adding water, and standing; (5) pressing the standing materials into a green body; (6) and sintering the blank to obtain the amorphous indium tungsten oxide target. The amorphous indium tungsten oxide target material prepared by the method is free of other additives, the process is more environment-friendly, and the target material is not cracked or continuously splashed in the evaporation process.
Description
Technical Field
The invention relates to the technical field of amorphous oxide semiconductors, in particular to an amorphous indium tungsten oxide target and a preparation method thereof.
Background
Amorphous Oxide Semiconductors (AOS) are widely considered as an active layer material of Thin Film Transistors (TFTS) that can replace conventional Amorphous silicon as a next generation display technology. Oxide semiconductors which are popular and mature in technology currently belong to amorphous indium gallium zinc oxide thin film transistors (a-IGZO TFTs), but now the resolution requirements of display devices are higher and higher, and the mobility of the a-IGZO TFTs can no longer meet the requirements. Amorphous indium tungsten oxide (IWO) has higher carrier concentration and better stability, so that the amorphous indium tungsten oxide (IWO) is possible to become a new generation of oxide semiconductor material for replacing a-IGZO TFTs, and the magnetron sputtering technology is an important technology for preparing high-performance thin film materials and is applied to various high-end electronic industries.
The indium tungsten oxide (IWO) film is mainly obtained by evaporation in an indium tungsten oxide target evaporation coating mode, and the performance of the IWO target has great influence on the performance of the IWO film. The common target material is not environment-friendly and has high cost because organic binder is often required to be added in the preparation process, and the target material is easy to crack in the use process because the binder is not used.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the amorphous indium-tungsten oxide target material and the preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of an amorphous indium-tungsten oxide target material comprises the following steps:
(1) carrying out ball milling on indium oxide, then adding tungsten trioxide accounting for 1-5% of the mass of the indium oxide, continuing ball milling to obtain a uniformly mixed material, and dividing the material into a material A and a material B according to the weight ratio of 5-7: 3-5;
(2) adding water into the material B, standing and granulating to obtain a material B';
(3) respectively sintering the material A and the material B' to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) carrying out ball milling on the indium tungsten oxide A, then, homogenizing and mixing the indium tungsten oxide A and the indium tungsten oxide B, then, adding water into the mixture, and standing;
(5) pressing the standing material to obtain a blank;
(6) and sintering the blank to obtain the amorphous indium tungsten oxide target.
According to the invention, firstly, the mixture of indium oxide and tungsten trioxide is divided into two parts, one part is used as fine powder, the other part is prepared into coarse powder through granulation, the mass ratio of the fine powder to the coarse powder is selected, the prepared target material has enough density, the coarse powder and the fine powder are mixed to form pores in the target material, and the target material is prevented from cracking due to overlarge internal stress generated by thermal expansion in the evaporation process. Meanwhile, the raw materials are sintered for the second time, the first sintering aims at preparing tungsten-doped indium oxide, and because the volume of the mixture of indium oxide and tungsten trioxide is changed after sintering, the product of the first sintering is firstly subjected to ball milling and then is pressed into a blank with the required size for secondary sintering, and at the moment, the size of the material is not obviously changed. If the raw materials are only pressed into a green body and then sintered once, the target material prepared by sintering needs to be cut and polished, and the process is more complicated.
Preferably, in the step (1), indium oxide is firstly ball-milled to ensure that the specific surface area of indium oxide particles is more than or equal to 2m2Adding tungsten trioxide into the mixture, and then performing ball milling to ensure that the specific surface area of the mixture particles is more than or equal to 2.5m2/g。
Preferably, in the step (2), the adding amount of water is 7-10% of the mass of the material B, and the standing time is not less than 20 h. Too little water is used, the powder is difficult to granulate, too much water is used, the powder is bonded into a dough shape, and the powder is difficult to granulate and passes through a 0.5mm screen.
Preferably, in the step (2), the maximum particle size of the material B' is 0.5 mm.
Preferably, in the step (3), the sintering method of the material a and the material B' is: heating to 800-1000 ℃ at the speed of 1-5 ℃/min, preserving heat for 0.5-1.5 h, heating to 1300-1450 ℃ at the speed of 0.5-3 ℃/min, preserving heat for 3-5 h, cooling to room temperature (15-35 ℃) at the speed of 3-5 ℃/min, and continuously introducing oxygen during the sintering process, wherein the flow of the oxygen is 50-100L/min.
Preferably, in the step (4), after ball milling, the mixture is subjected to ball millingThe specific surface area of the indium tungsten oxide A is more than or equal to 10m2The addition amount of water is 4-7% of the mass of the mixture, and the standing time is more than or equal to 20 h.
Preferably, in the step (6), the sintering method of the green body is as follows: heating to 100-200 ℃ at the speed of 0.1-1 ℃/min, preserving heat for 0.5-1.5 h, heating to 1300-1450 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 3-5 h, and then cooling to room temperature at the speed of 3-5 ℃/min.
The reason for selecting the conditions of the primary sintering and the secondary sintering is that firstly, the heat preservation time is too short, the tungsten-doped indium oxide required by the invention cannot be formed, the heat preservation time is too long, the density can be further increased, but simultaneously, the porosity is also reduced, so that the target material is easy to crack in the using process; the selection of the temperature also conforms to a similar law; in addition, the heating rate has a great influence on the structure of the target material, and the target material is cracked due to improper heating rate. According to the invention, sintering conditions are researched, it is determined that the amorphous indium-tungsten oxide target prepared by the scheme has higher density and stability, the particle size of powder is widened by mixing coarse powder and fine powder, a prepared product has certain pores, internal stress generated by heating is effectively reduced in the heating evaporation process, and the phenomena of cracking and continuous splashing are avoided in the using process.
Meanwhile, the invention also discloses the amorphous indium-tungsten oxide target material prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, no additive is added in the process of preparing the amorphous indium-tungsten oxide target material, the amorphous indium-tungsten oxide target material is prepared under the action of pure water, no waste gas, waste water and waste solids are generated in the process, the preparation method is more environment-friendly, meanwhile, the target material with required density can be accurately prepared, the precision is higher, and the target material is not cracked in the evaporation process.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In an embodiment of the amorphous indium-tungsten oxide target material of the present invention, the method for preparing the amorphous indium-tungsten oxide target material includes the following steps:
(1) weighing 4kg of indium oxide, ball-milling for 26 hours, wherein the specific surface area of the particles is 2.87m2Per g, 40.4g of tungsten trioxide was added and ball milling was continued for 4 hours to obtain a specific surface area of 2.89m2The mixture is divided into a material A and a material B according to the weight ratio of 7: 3;
(2) adding 96g of pure water into the material B, standing for 24 hours, granulating, and sieving by a 0.5mm sieve to obtain a material B'.
(3) Placing the material A and the material B' into a sintering furnace for sintering, heating to 800 ℃ at the speed of 2 ℃/min, preserving heat for 1h, continuing heating to 1300 ℃ at the speed of 0.5 ℃/min, preserving heat for 4h, then cooling to room temperature at the speed of 5 ℃/min, and continuously introducing oxygen in the sintering process, wherein the oxygen flow is 50L/min, so as to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) ball milling indium-tungsten oxide A for 10h to make the specific surface area more than or equal to 10m2Mixing the mixture with indium tungsten oxide B for 0.5h, adding pure water accounting for 5% of the mixture by mass, and standing for 24 h;
(5) weighing 23g of the mixture after standing, putting the mixture into a mold for tabletting, adjusting the height of the mold, and pressing to obtain an indium tungsten oxide biscuit with the thickness of 25.01mm multiplied by 10.0mm, wherein the tabletting pressure is 78kN, putting the biscuit into a sintering furnace, heating to 150 ℃ at the speed of 0.3 ℃/min, preserving heat for 1h, heating to 1300 ℃ at the speed of 0.5 ℃/min, preserving heat for 5h, and cooling to room temperature at the speed of 3 ℃/min to obtain the indium tungsten oxide biscuit with the density of 4.65g/cm3The amorphous indium tungsten oxide target material.
Example 2
In an embodiment of the amorphous indium-tungsten oxide target material of the present invention, the method for preparing the amorphous indium-tungsten oxide target material includes the following steps:
(1) weighing 4kg of indium oxide, ball-milling for 24 hours, wherein the specific surface area of the particles is 2.67m2102.56g of tungsten trioxide is added and the ball milling is continued for 3 hours, and the specific surface area of the mixture particles is 2.72m2The mixture is prepared from the following raw materials in parts by weight of 6:4, dividing the mixture into a material A and a material B;
(2) 144g of pure water is added into the material B, and the mixture is kept stand for 20 hours, granulated and sieved by a 0.5mm screen to obtain a material B'.
(3) Placing the material A and the material B' into a sintering furnace for sintering, heating to 900 ℃ at the speed of 1 ℃/min, preserving heat for 1h, continuing heating to 1450 ℃ at the speed of 0.8 ℃/min, preserving heat for 5h, then cooling to room temperature at the speed of 5 ℃/min, and continuously introducing oxygen in the sintering process, wherein the oxygen flow is 80L/min, so as to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) ball milling indium-tungsten oxide A for 8h to make the specific surface area more than or equal to 10m2Mixing the mixture and indium tungsten oxide B for 1h, adding pure water accounting for 5% of the mixture by mass, and standing for 24 h;
(5) weighing 22.5g of the mixture after standing, putting the mixture into a mold for tabletting, adjusting the height of the mold, and pressing to obtain an indium tungsten oxide biscuit with the thickness of 25.01mm multiplied by 10.0mm, wherein the tabletting pressure is 62kN, putting the biscuit into a sintering furnace, heating to 150 ℃ at the speed of 0.2 ℃/min, preserving heat for 1h, heating to 1450 ℃ at the speed of 0.8 ℃/min, preserving heat for 5h, and cooling to room temperature at the speed of 3 ℃/min to obtain the indium tungsten oxide biscuit with the density of 4.45g/cm3The amorphous indium tungsten oxide target material.
Example 3
In an embodiment of the amorphous indium-tungsten oxide target material of the present invention, the method for preparing the amorphous indium-tungsten oxide target material includes the following steps:
(1) weighing 4kg of indium oxide, ball-milling for 22 hours, wherein the specific surface area of the particles is 2.58m2166.67g of tungsten trioxide is added, the ball milling is continued for 3 hours, and the specific surface area of the mixture is 2.72m2The mixture is divided into a material A and a material B according to the weight ratio of 5: 5;
(2) adding 180 parts of pure water into the material B, standing for 24 hours, granulating, and sieving by a 0.5mm sieve to obtain a material B'.
(3) Placing the material A and the material B' into a sintering furnace for sintering, heating to 800 ℃ at the speed of 2 ℃/min, preserving heat for 1h, continuing heating to 1400 ℃ at the speed of 0.5 ℃/min, preserving heat for 4h, then cooling to room temperature at the speed of 5 ℃/min, and continuously introducing oxygen in the sintering process, wherein the oxygen flow is 90L/min, so as to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) ball milling indium-tungsten oxide A for 5h to make the specific surface area more than or equal to 10m2Mixing the mixture with indium tungsten oxide B for 0.5h, adding pure water accounting for 5% of the mixture by mass, and standing for 24 h;
(5) weighing 22g of the mixture after standing, putting the mixture into a mold for tabletting, adjusting the height of the mold, and pressing to obtain an indium tungsten oxide biscuit with the thickness of 25.00mm multiplied by 10.0mm, wherein the tabletting pressure is 55kN, putting the biscuit into a sintering furnace, heating to 150 ℃ at the speed of 0.5 ℃/min, preserving heat for 1h, heating to 1400 ℃ at the speed of 0.5 ℃/min, preserving heat for 5h, and cooling to room temperature at the speed of 3 ℃/min to obtain the indium tungsten oxide biscuit with the density of 4.23g/cm3The amorphous indium tungsten oxide target material.
Example 4
In an embodiment of the amorphous indium-tungsten oxide target material of the present invention, the method for preparing the amorphous indium-tungsten oxide target material includes the following steps:
(1) 4kg of indium oxide was weighed and ball-milled for 20 hours, and the specific surface area of the particles was 2.46m2210.52g of tungsten trioxide is added, the ball milling is continued for 5 hours, and the specific surface area of the mixture is 2.63m2The mixture is divided into a material A and a material B according to the weight ratio of 5.5: 4.5;
(2) and adding 190g of pure water into the material B, standing for 20 hours, granulating, and sieving by using a 0.5mm sieve to obtain a material B'.
(3) Placing the material A and the material B' into a sintering furnace for sintering, heating to 900 ℃ at the speed of 1 ℃/min, preserving heat for 1h, continuing heating to 1350 ℃ at the speed of 0.8 ℃/min, preserving heat for 5h, then cooling to room temperature at the speed of 5 ℃/min, and continuously introducing oxygen in the sintering process, wherein the oxygen flow is 100L/min, so as to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) ball milling indium-tungsten oxide A for 6h to make the specific surface area more than or equal to 10m2Mixing the mixture and indium tungsten oxide B for 1h, adding pure water accounting for 5% of the mixture by mass, and standing for 24 h;
(5) weighing 21.5g of the mixture after standing, putting the mixture into a die for tabletting, setting the pressure to be 50kN to obtain an indium tungsten oxide biscuit with the thickness of 25.00mm multiplied by 10.02mm, putting the biscuit into a sintering furnace, and putting the biscuit at the speed of 0.5 ℃/minHeating to 150 deg.C at a speed of 1h, heating to 1350 deg.C at a speed of 0.9 deg.C/min, maintaining for 5h, and cooling to room temperature at a speed of 3 deg.C/min to obtain a density of 4.08g/cm3The amorphous indium tungsten oxide target material.
Comparative example 1
The preparation method of the amorphous indium-tungsten oxide target material is different from that of the amorphous indium-tungsten oxide target material in embodiment 1 only in that the ratio of the material A to the material B is 4:6, and the density of the amorphous indium-tungsten oxide target material prepared by the method is 4.58g/cm3。
Comparative example 2
The preparation method of the amorphous indium-tungsten oxide target material is different from that of the amorphous indium-tungsten oxide target material in embodiment 1 only in that the ratio of the material A to the material B is 8:2, and the density of the amorphous indium-tungsten oxide target material prepared by the method is 4.45g/cm3。
Comparative example 3
The preparation method of the amorphous indium-tungsten oxide target material is different from that of the example 1 only in that coarse materials are not prepared, the step (2) is omitted, sintering, ball milling, pressing and secondary sintering are carried out according to the same process as that of the example 1 to obtain the amorphous indium-tungsten oxide target material, and the density of the amorphous indium-tungsten oxide target material prepared by the method is 4.45g/cm3。
Comparative example 4
An amorphous indium-tungsten oxide target material, the preparation method of which differs from that of example 1 only in that the sintering method in step (5) is: heating to 150 ℃ at the speed of 0.3 ℃/min, preserving heat for 1h, heating to 1500 ℃ at the speed of 0.5 ℃/min, preserving heat for 5h, cooling to room temperature at the speed of 3 ℃/min, and introducing oxygen in the sintering process, wherein the oxygen flow is 30L/min. The density of the amorphous indium-tungsten oxide target material prepared by the method is 4.45g/cm3。
The evaporation resistance of the amorphous indium tungsten oxide targets of examples 1 to 4 and comparative examples 1 to 4 was tested under the conditions shown in table 1, and the results are shown in table 2 by visual observation of whether cracking or continuous sputtering occurred during the evaporation process.
TABLE 1
TABLE 2
According to the test results, the evaporation resistance of the comparative examples 1-4 is relatively poor, and the coating is easy to crack in the using process. According to the test results, the amorphous indium-tungsten oxide target material with the required size and density can be prepared according to the requirements by selecting the proportion of the fine material and the coarse material and the sintering conditions, and the amorphous indium-tungsten oxide target material also has good evaporation resistance.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. The preparation method of the amorphous indium-tungsten oxide target is characterized by comprising the following steps:
(1) carrying out ball milling on indium oxide, then adding tungsten trioxide accounting for 1-5% of the mass of the indium oxide, continuing ball milling to obtain a uniformly mixed material, and dividing the material into a material A and a material B according to the weight ratio of 5-7: 3-5;
(2) adding water into the material B, standing and granulating to obtain a material B';
(3) respectively sintering the material A and the material B' to obtain indium tungsten oxide A and indium tungsten oxide B;
(4) carrying out ball milling on the indium tungsten oxide A, then, homogenizing and mixing the indium tungsten oxide A and the indium tungsten oxide B, then, adding water into the mixture, and standing;
(5) pressing the standing material to obtain a blank;
(6) and sintering the blank to obtain the amorphous indium tungsten oxide target.
2. The method for preparing the amorphous indium tungsten oxide target material according to claim 1, wherein in the step (1), indium oxide is ball-milled to make the specific surface area of indium oxide particles larger than or equal to 2m2Adding tungsten trioxide into the mixture, and then performing ball milling to ensure that the specific surface area of the mixture particles is more than or equal to 2.5m2/g。
3. The method for preparing the amorphous indium-tungsten oxide target material according to claim 1, wherein in the step (2), the addition amount of water is 7-10% of the mass of the material B, and the standing time is not less than 20 h.
4. The method for preparing an amorphous indium tungsten oxide target material according to claim 1, wherein in the step (2), the maximum particle size of the material B' is 0.5 mm.
5. The method for preparing the amorphous indium tungsten oxide target material according to claim 1, wherein in the step (3), the sintering method of the material a and the material B' comprises the following steps: heating to 800-1000 ℃ at the speed of 1-5 ℃/min, preserving heat for 0.5-1.5 h, heating to 1300-1450 ℃ at the speed of 0.5-3 ℃/min, preserving heat for 3-5 h, cooling to room temperature at the speed of 3-5 ℃/min, and continuously introducing oxygen in the sintering process.
6. The method for preparing the amorphous indium tungsten oxide target material according to claim 5, wherein the flow rate of the oxygen is 50 to 100L/min.
7. The method for preparing an amorphous indium tungsten oxide target material according to claim 1, wherein in the step (4), the oxidation is performed after the ball millingThe specific surface area of the indium-tungsten A is more than or equal to 10m2The addition amount of water is 4-7% of the mass of the mixture, and the standing time is more than or equal to 20 h.
8. The method for preparing the amorphous indium tungsten oxide target material according to claim 1, wherein in the step (6), the sintering method of the blank comprises the following steps: heating to 100-200 ℃ at the speed of 0.1-1 ℃/min, preserving heat for 0.5-1.5 h, heating to 1300-1450 ℃ at the speed of 0.5-2 ℃/min, preserving heat for 3-5 h, and then cooling to room temperature at the speed of 3-5 ℃/min.
9. An amorphous indium tungsten oxide target material prepared by the method of any one of claims 1 to 8.
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