CN114436642A - Preparation method of indium tin oxide alloy target material - Google Patents
Preparation method of indium tin oxide alloy target material Download PDFInfo
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- CN114436642A CN114436642A CN202011233273.2A CN202011233273A CN114436642A CN 114436642 A CN114436642 A CN 114436642A CN 202011233273 A CN202011233273 A CN 202011233273A CN 114436642 A CN114436642 A CN 114436642A
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- tin oxide
- alloy target
- indium tin
- indium
- target material
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 83
- 239000000956 alloy Substances 0.000 title claims abstract description 83
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000013077 target material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910001887 tin oxide Inorganic materials 0.000 claims abstract description 41
- 229910003437 indium oxide Inorganic materials 0.000 claims abstract description 36
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000007731 hot pressing Methods 0.000 claims abstract description 16
- 238000007750 plasma spraying Methods 0.000 claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 15
- 238000003825 pressing Methods 0.000 claims abstract description 15
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 2
- 238000001771 vacuum deposition Methods 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000035939 shock Effects 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 2
- 230000003068 static effect Effects 0.000 abstract description 2
- 238000005299 abrasion Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 21
- 238000000576 coating method Methods 0.000 description 18
- 239000011248 coating agent Substances 0.000 description 17
- 239000010408 film Substances 0.000 description 16
- 238000005507 spraying Methods 0.000 description 16
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 13
- 239000011261 inert gas Substances 0.000 description 11
- 229910001128 Sn alloy Inorganic materials 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000002834 transmittance Methods 0.000 description 7
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 229910052738 indium Inorganic materials 0.000 description 5
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 5
- NQBRDZOHGALQCB-UHFFFAOYSA-N oxoindium Chemical compound [O].[In] NQBRDZOHGALQCB-UHFFFAOYSA-N 0.000 description 5
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000010288 cold spraying Methods 0.000 description 3
- 238000005034 decoration Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000003754 machining Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000004506 ultrasonic cleaning Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 239000011812 mixed powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
- C04B35/457—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates based on tin oxides or stannates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3286—Gallium oxides, gallates, indium oxides, indates, thallium oxides, thallates or oxide forming salts thereof, e.g. zinc gallate
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- C04B2235/3293—Tin oxides, stannates or oxide forming salts thereof, e.g. indium tin oxide [ITO]
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Abstract
The invention provides a preparation method of an indium tin oxide alloy target material, which comprises the following steps: A) placing indium oxide and tin oxide in a vacuum rolling mixer for mixing to obtain a mixture; B) vacuumizing the mixture, performing cold isostatic pressing to obtain a rough blank, and performing secondary pressing on the rough blank to obtain an alloy target green blank; C) carrying out vacuum hot-pressing sintering on the alloy target green body to obtain an indium tin oxide alloy target crude product; D) annealing the crude indium tin oxide alloy target, and plasma spraying the mixture obtained in the step A) onto the surface of the annealed crude indium tin oxide alloy target to obtain the indium tin oxide alloy target. The indium tin oxide alloy target material with uniform structure, fine crystal grains and high thermal shock resistance is prepared, and the alloy target material can be used as a rotary target vacuum coating film to obtain a high-quality film with high resistance, electromagnetic interference resistance, static electricity resistance and abrasion resistance, so that the uniformity of the film can be increased, and the utilization rate of the target material can be improved.
Description
Technical Field
The invention relates to the technical field of alloy targets, in particular to a preparation method of an indium tin oxide alloy target.
Background
The vacuum coating technology is a new technology for material synthesis and processing, and is an important component in the technical field of surface engineering. With the rapid development of the global manufacturing industry, the application of the vacuum coating technology is more and more extensive. From the development of semiconductor integrated circuit, LED, display, touch screen, solar photovoltaic, chemical and pharmaceutical industries, the products of vacuum coating technology relate to a plurality of products, including electrical films for manufacturing large scale integrated circuits, digital data recording and storing films which can be magnetized longitudinally and transversely, optical films which can fully show and apply various optical characteristics, photosensitive films for computer display, conductive films and antireflection films on TFT and PDP flat displays, glass coating and decoration films applied in the building and automobile industries, protective films and barrier films used in the packaging field, functional films with various functional decoration effects on decoration materials, wear-resistant super-hard films applied on the surfaces of tools and molds, and various functional films in the research aspect of nano materials, and the like, and the requirements of the films are higher and higher, so the requirements on vacuum coating equipment, technology and materials are continuously increased, meanwhile, with the continuous development of industrial technology, the comprehensive performance requirement of the material is also continuously improved, and the performance requirement of the working machine under certain specific environments cannot be met by the performance of a single material.
After decades of development, domestic vacuum ion coating machines have made certain progress in automation degree and technology compared with foreign high-end coating equipment, but need to be improved in the aspects of stability and accuracy of coating products. The high cost performance of vacuum coating and the environmental pollution caused by traditional electroplating force vacuum coating to become the mainstream, and vacuum coating equipment for various coating processes is increasing continuously. The indium-tin alloy is an alloy formed by adding other elements into titanium; indium tin has two homogeneous crystals: 231.89 deg.C. The high-hardness high-resistance film has the advantages of static electricity resistance, radiation resistance, magnetic interference resistance, high brightness and high contrast, is one of basic materials in various industries, and is widely applied to the fields of solar cells, liquid crystal displays and plasma displays. In recent years, with the rapid development of high-grade displays, indium tin alloy rotary targets become important materials for preparing high-hardness and high-resistance thin films. The core technical difficulty of the high-hardness and high-resistance target material is cracking in the forming process and uniformity control in the sintering process.
Disclosure of Invention
The invention aims to provide a preparation method of an indium tin oxide alloy target material, and the alloy target material provided by the invention has the properties of uniform structure, fine crystal grains, high thermal shock resistance and the like, and can be suitable for producing large-area high-hardness high-resistance films.
In view of the above, the present application provides a method for preparing an indium tin oxide alloy target, comprising the following steps:
A) placing indium oxide and tin oxide in a vacuum rolling mixer for mixing to obtain a mixture;
B) vacuumizing the mixture, performing cold isostatic pressing to obtain a rough blank, and performing secondary pressing on the rough blank to obtain an alloy target green blank;
C) carrying out vacuum hot-pressing sintering on the alloy target green body to obtain an indium tin oxide alloy target crude product;
D) annealing the crude indium tin oxide alloy target, and plasma spraying the mixture obtained in the step A) onto the surface of the annealed crude indium tin oxide alloy target to obtain the indium tin oxide alloy target.
Preferably, in the step A), the mass ratio of the indium oxide to the tin oxide is (6-8): (2-4), the Fischer-Tropsch average particle size of the indium oxide is 1-7 mu m, and the Fischer-Tropsch average particle size of the tin oxide is 1-7 mu m.
Preferably, in the step B), the pressure of the cold isostatic pressing is 10-60 MPa, the pressure of the secondary pressing is 50-200 MPa, and the density of the alloy target green body is greater than 98%.
Preferably, in the step C), the vacuum hot-pressing sintering is carried out in a hydrogen protection atmosphere, the pressure is 20-30 MPa, and the temperature is 200-300 ℃.
Preferably, step D) further comprises, before plasma spraying:
ball milling the mixture obtained in step A) and sieving.
Preferably, when the ito target is a target with a hollow cylinder, the plasma spraying of the mixture onto the surface of the annealed ito target crude product further includes:
vacuumizing the obtained indium tin oxide alloy target material, and carrying out plasma spraying on the mixture obtained in the step A) in an inert atmosphere to a cavity of the target material.
Preferably, in the step D), the annealing temperature is 100-300 ℃ and the annealing time is 3-5 h.
Preferably, in the step a), the vacuum pressure in the vacuum rolling mixer is 2 × 10 ° Pa, and the rotation speed is 50 to 80 r/min.
Preferably, the step a) further comprises, after the mixing:
selecting a plurality of different areas from the mixed material to respectively detect the contents of indium oxide and tin oxide until the ratio error of the indium oxide content to the tin oxide content of each detection point is 0.01-0.3%, and completing mixing.
Preferably, in step B), before the vacuum-pumping, the step of placing the mixture into a tubular rubber sleeve and then sealing the rubber sleeve.
The application provides a preparation method of an indium tin oxide alloy target, which comprises the steps of taking indium oxide and tin oxide as raw materials, mixing the indium oxide and the tin oxide, carrying out cold isostatic pressing, and then carrying out secondary pressing to obtain an alloy target green body, carrying out vacuum hot-pressing sintering on the alloy target green body to obtain an indium tin oxide alloy target crude product, annealing, and then carrying out plasma spraying on the surface of the alloy target crude product to obtain an indium tin oxide alloy target; in the preparation process, firstly, a crude indium tin oxide alloy target material is preliminarily prepared, and then a mixture of indium oxide and tin oxide is sprayed on the surface of the crude indium tin oxide alloy target material, so that the indium tin oxide alloy target material with uniform structure, fine crystal grains and high thermal shock resistance can be obtained.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Aiming at the problems of cracking and uniformity in the preparation process of a high-hardness and high-resistance target material in the prior art, the application provides a preparation method of an indium tin oxide alloy target material. Specifically, the application provides a preparation method of an indium tin oxide alloy target, which comprises the following steps:
A) placing indium oxide and tin oxide in a vacuum rolling mixer for mixing to obtain a mixture;
B) vacuumizing the mixture, performing cold isostatic pressing to obtain a rough blank, and performing secondary pressing on the rough blank to obtain an alloy target green blank;
C) carrying out vacuum hot-pressing sintering on the alloy target green body to obtain an indium tin oxide alloy target crude product;
D) annealing the crude indium tin oxide alloy target, and plasma spraying the mixture obtained in the step A) onto the surface of the annealed crude indium tin oxide alloy target to obtain the indium tin oxide alloy target.
In the preparation process of the indium tin oxide alloy target material, firstly, indium oxide and tin oxide are placed in a vacuum rolling mixer to be mixed to obtain a mixture; the indium oxide is added in a powder state, the theoretical density of the indium oxide is more than 98%, the Fisher's average particle size is 1-7 mu m, the tin oxide exists in a powder state, the theoretical density of the tin oxide is more than 98%, and the Fisher's average particle size is 1-7 mu m. The mass ratio of the indium oxide to the tin oxide is (6-8): (2-4), more specifically, the mass ratio of the indium oxide to the tin oxide is 6:4, 7:3 or 8:2, and in specific embodiments, the mass ratio of the indium oxide to the tin oxide is 7:3, so as to satisfy both the conductivity and the high impedance performance; further, the good conductivity of indium is better than that of tin, and the 7:3 ratio is favorable for the performance requirement of high resistance and high transmittance of the thin film. Mixing indium oxide and tin oxide according to a certain mass ratio, and then placing the mixture into a vacuum rolling mixer for mixing to obtain a mixture; the vacuum pressure of the vacuum rolling mixer is 2 x 100Pa, the rotating speed is 50-80 r/min, more specifically, the rotating speed is 60-75 r/min. The raw materials are mixed in a vacuum rolling mixer to keep the materials dry and remove residual gas, so that the materials are mixed more uniformly to be beneficial to obtaining groupsWeaving an alloy target material with uniform and fine grains.
In order to ensure the uniformity of the alloy target, the content of the oxygen indium and the content of the tin oxide are preferably detected at a plurality of randomly selected points of the mixed material until the ratio error of the content of the indium oxide to the content of the tin oxide at each detection point is 0.01-0.03%, and the mixing is completed.
According to the invention, the mixture is subjected to cold isostatic pressing after being vacuumized to obtain a rough blank, and the rough blank is subjected to secondary pressing to obtain an alloy target green blank. In the process, the mixture is preferably placed in a rubber sleeve provided with a tubular flexible mold, indium disulfide powder is coated on the contact surface of the mold and the mixed material, then the rubber sleeve is sealed and vacuumized, the vacuumized rubber sleeve is placed on a cold isostatic press, primary pre-pressing is carried out under the pressure of 10-60 MPa to form a rough blank, secondary pressing is carried out under the pressure of 50-200 MPa until the density of the rough blank reaches 60-62% of the theoretical density, and the alloy target green blank is obtained and is also a tubular cavity alloy target due to the fact that the mold is tubular. More specifically, the pressure of the primary prepressing is 15-40 MPa, and more specifically, the pressure of the primary prepressing is 20-35 MPa. More specifically, the pressure of the secondary pressing is 80-160 MPa, and further the pressure of the secondary pressing is 100-140 MPa.
And then carrying out vacuum hot-pressing sintering on the alloy target green body to obtain the indium tin oxide alloy target. In this process, the vacuum hot press sintering is a technical means well known to those skilled in the art, and the technical embodiment thereof is not particularly limited in this application. Specifically, the vacuum hot-pressing sintering is carried out in a hydrogen atmosphere, the pressure is 20-30 MPa, the temperature is 200-300 ℃, and more specifically, the pressure of the vacuum sintering is 23-28 MPa, and the temperature is 230-280 ℃. And demolding at 100-200 ℃ after vacuum hot-pressing sintering, and cooling to room temperature to obtain the crude indium tin oxide alloy target.
Annealing the crude indium tin oxide alloy target after the crude indium tin oxide alloy target is obtained, wherein the annealing temperature is 100-300 ℃, and the annealing time is 2-4 hours; more specifically, the annealing temperature is 140-220 ℃.
The obtained alloy target is still not suitable for preparing a thin film by using a rotary target, and further, the mixture of indium oxide and tin oxide is preferably subjected to ball milling, the ball milling is carried out for 2-4 hours, then the mixture is sieved by a 1000-mesh sieve, and then the mixed powder after ball milling is sprayed on the surface of the annealed alloy target by using plasma spraying under an inert atmosphere, so that the indium tin oxide alloy target is obtained.
The alloy target material is used as a rotary target material to prepare a film, on the basis, in order to be used as the rotary target material, the alloy target material after plasma spraying is vacuumized again, mixed powder of indium oxide and tin oxide after ball milling is sprayed into a cavity of the alloy target material in an inert atmosphere, the spraying thickness is 0.1-0.3 mm, and therefore the rotary target material which can be etched uniformly at 360 degrees is obtained. In the above process, the inert gas of the inert atmosphere is introduced at a flow rate of 400 to 1200sccm, and more specifically, the inert gas is introduced at a flow rate of 700 to 1000 sccm.
The rotary target prepared by the method can rotate around the fixed strip-shaped magnet assembly in the sputtering process, flies in all directions, has good uniformity, large sputtering area, convenient replacement and operation, high production efficiency and high target utilization rate, and has unique superiority on the deposition of the inner wall of a part.
For further understanding of the present invention, the following examples are provided to illustrate the preparation method of the indium tin oxide alloy target material provided by the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
a) The furnace volume of a vacuum rolling mixer is 10.00kg, indium oxide powder with the theoretical density of more than 99.9 percent and the Fisher's average particle size of 7 mu m and tin oxide powder with the theoretical density of more than 99.9 percent and the Fisher's average particle size of 7 mu m are respectively selected, the mass ratio of indium oxide to tin oxide is 7:3, 7.00kg of indium oxide and 3.00kg of tin oxide are weighed and put into a vacuum (the vacuum pressure is 2 Pa) rolling mixer according to the mass ratio, and the materials are fully mixed under the condition that the rotating speed is 50 r/min;
b) randomly selecting five points from the mixed material obtained in the step a) to detect the indium oxide content and the tin oxide content until the error of the ratio of the indium oxide content to the tin oxide content at each detection point is 0.01%, and completing mixing;
c) filling the mixed material treated in the step b) into a rubber sleeve provided with a tubular flexible mold, coating indium disulfide powder on the contact surface of the mold and the mixed material, sealing the rubber sleeve, vacuumizing, placing the vacuumized rubber sleeve on a cold isostatic press, performing primary prepressing under the condition of 40MPa of pressure to form a rough blank, performing secondary pressing on the prepared rough blank under the condition of 100MPa until the density of the rough blank reaches 60 percent of the theoretical density, and releasing the pressure to normal pressure;
d) placing the indium tin alloy target green compact pressed in the step c) in a vacuum hot-pressing sintering furnace, carrying out hot-pressing sintering under the conditions of hydrogen protection atmosphere, pressure of 20MPa and temperature of 200 ℃, carrying out demoulding at 100 ℃ by adopting a high-temperature demoulding process after heat preservation and pressure maintaining for 5 hours, and cooling to room temperature to obtain a crude indium tin oxide alloy target;
e) machining the crude indium tin alloy target material prepared in the step d) to a required size, then placing the crude indium tin alloy target material in a vacuum annealing furnace, and heating to 100 ℃ for annealing for 3 hours;
f) carrying out chemical and physical detection on the crude indium tin oxide alloy target material obtained in the step e), and then carrying out ultrasonic cleaning to ensure that the target material reaches qualified roughness;
g) b), taking the mixed material treated in the step b), putting the mixed material into a ball mill for ball milling for 3 hours, and sieving through a 1000-mesh sieve to obtain indium tin oxide spraying powder;
h) spraying the indium tin oxide spraying powder prepared in the step g) on the outer surface of the step f) by using a plasma spraying method under the inert gas protection atmosphere;
i) vacuumizing the target material cavity prepared in the step h), introducing inert gas with the flow of 400-1200 sccm, and cold spraying the indium tin spraying powder obtained in the step g) into the cavity of the target material under the inert gas atmosphere, wherein the spraying thickness is 0.1mm, so as to prepare the indium tin oxide alloy target material.
Adopt the aboveThe prepared In30Sn alloy target material is used as a rotary target material, the Ar flow of the coating chamber is 200-220sccm, the oxygen flow is 0.5sccm, and the vacuum degree of the coating chamber is 3.0 multiplied by 10-1Pa, total air pressure of 0.30Pa, coating temperature of 300 deg.C, thickness of 1nm, and resistance of 3 x 107European transmittance and transmittance>97％。
Example 2
a) The furnace amount of the vacuum rolling mixer is 10.00kg, indium oxide powder with the theoretical density of more than 98 percent and the Fisher's average particle size of 7 mu m and tin oxide powder with the theoretical density of more than 99.9 percent and the Fisher's average particle size of 1-7 mu m are respectively selected, the mass ratio of indium oxide to tin oxide is 6:4, 6.00kg of indium oxide and 4.00kg of tin oxide are weighed and put into a vacuum (the vacuum pressure is 2 Pa rolling mixer, and the materials are fully mixed under the condition of the rotating speed of 60 r/min;
b) randomly selecting five points from the mixed material obtained in the step a) to detect the oxygen indium content and the tin oxide content until the error of the ratio of the oxygen indium content to the tin oxide content at each detection point is 0.02%, and completing mixing;
c) filling the mixed material treated in the step b) into a rubber sleeve provided with a tubular flexible mold, coating indium disulfide powder on the contact surface of the mold and the mixed material, sealing the rubber sleeve, vacuumizing, placing the vacuumized rubber sleeve on a cold isostatic press, performing primary prepressing under the condition of 40MPa to form a rough blank, performing secondary pressing on the prepared rough blank under the condition of 100MPa until the density of the rough blank reaches 61% of the theoretical density, and releasing the pressure to normal pressure;
d) placing the indium tin alloy target green compact pressed in the step c) in a vacuum hot-pressing sintering furnace, carrying out hot-pressing sintering under the conditions of hydrogen protection atmosphere, pressure of 25MPa and temperature of 250 ℃, carrying out demoulding at 150 ℃ by adopting a high-temperature demoulding process after heat preservation and pressure maintaining for 5 hours, and cooling to room temperature to obtain a crude indium tin oxide alloy target;
e) machining the crude indium tin alloy target material prepared in the step d) to a required size, then placing the crude indium tin alloy target material in a vacuum annealing furnace, and heating to 150 ℃ for annealing for 3 hours;
f) carrying out chemical and physical detection on the crude indium tin oxide alloy target material obtained in the step e), and then carrying out ultrasonic cleaning to ensure that the target material reaches qualified roughness;
g) b), taking the mixed material treated in the step b), putting the mixed material into a ball mill for ball milling for 3 hours, and sieving through a 1000-mesh sieve to obtain indium tin oxide spraying powder;
h) spraying the indium tin oxide spraying powder prepared in the step g) on the outer surface of the step f) by using a plasma spraying method under the inert gas protection atmosphere;
i) vacuumizing the target material cavity prepared in the step h), introducing inert gas with the flow of 800sccm, and cold spraying the indium tin spraying powder obtained in the step g) into the cavity of the target material under the atmosphere of the inert gas to obtain the indium tin oxide alloy target material with the spraying thickness of 0.1 mm.
The prepared In40Sn alloy target is used as a rotary target, the Ar flow of a coating chamber is 210sccm, the oxygen flow is 0.6sccm, and the vacuum degree of the coating chamber is 4.0 multiplied by 10-1Pa, total air pressure of 0.40Pa, coating temperature of 350 deg.C, thickness of 1.2nm, and resistance of 4 ANG 106European transmittance and transmittance>93.6％。
Example 3
a) The furnace amount of the vacuum rolling mixer is 10.00kg, indium oxide powder with the theoretical density of more than 98 percent and the Fisher's average particle size of 7 mu m and tin oxide powder with the theoretical density of more than 99.9 percent and the Fisher's average particle size of 1-7 mu m are respectively selected, the mass ratio of indium oxide to tin oxide is 8:2, 8.00kg of indium oxide and 2.00kg of tin oxide are weighed and put into a vacuum (the vacuum pressure is 2 Pa rolling mixer, and the materials are fully mixed under the condition of the rotating speed of 70 r/min;
b) randomly selecting five points from the mixed material obtained in the step a) to detect the oxygen indium content and the tin oxide content until the error of the ratio of the oxygen indium content to the tin oxide content at each detection point is 0.02%, and completing mixing;
c) filling the mixed material treated in the step b) into a rubber sleeve provided with a tubular flexible mold, coating indium disulfide powder on the contact surface of the mold and the mixed material, sealing the rubber sleeve, vacuumizing, placing the vacuumized rubber sleeve on a cold isostatic press, performing primary prepressing under the condition of 40MPa to form a rough blank, performing secondary pressing on the prepared rough blank under the condition of 100MPa until the density of the rough blank reaches 61.5 percent of the theoretical density, and releasing the pressure to the normal pressure;
d) placing the indium tin alloy target green compact pressed in the step c) in a vacuum hot-pressing sintering furnace, carrying out hot-pressing sintering under the conditions of hydrogen protection atmosphere, pressure of 27MPa and temperature of 280 ℃, carrying out demoulding at 180 ℃ by adopting a high-temperature demoulding process after heat preservation and pressure maintaining for 5 hours, and cooling to room temperature to obtain a crude indium tin oxide alloy target;
e) machining the crude indium tin oxide alloy target material prepared in the step d) to a required size, then placing the crude indium tin oxide alloy target material in a vacuum annealing furnace, and heating to 280 ℃ for annealing for 3 hours;
f) carrying out chemical and physical detection on the crude indium tin oxide alloy target material obtained in the step e), and then carrying out ultrasonic cleaning to ensure that the target material reaches qualified roughness;
g) b), taking the mixed material treated in the step b), putting the mixed material into a ball mill for ball milling for 3 hours, and sieving through a 1000-mesh sieve to obtain indium tin oxide spraying powder;
h) spraying the indium tin oxide spraying powder prepared in the step g) on the outer surface of the step f) by using a plasma spraying method under the inert gas protection atmosphere;
i) vacuumizing the target material cavity prepared in the step h), introducing inert gas with the flow of 900sccm, and cold spraying the indium tin spraying powder obtained in the step g) into the cavity of the target material under the inert gas atmosphere to obtain the indium tin oxide alloy target material with the spraying thickness of 0.1 mm.
The prepared In20Sn alloy target is used as a rotary target, the Ar flow of a coating chamber is 220sccm, the oxygen flow is 01.0sccm, and the vacuum degree of the coating chamber is 5.0 multiplied by 10-1The total air pressure is 0.5Pa, the coating temperature is 450 ℃, and the thickness of the film obtained after coating is 1-1.5 nm, thus obtaining the filmThe resistance of the obtained coated product is 6 ANG 106European transmittance and transmittance>93.9％。
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of an indium tin oxide alloy target material comprises the following steps:
A) placing indium oxide and tin oxide in a vacuum rolling mixer for mixing to obtain a mixture;
B) vacuumizing the mixture, performing cold isostatic pressing to obtain a rough blank, and performing secondary pressing on the rough blank to obtain an alloy target green blank;
C) carrying out vacuum hot-pressing sintering on the alloy target green body to obtain an indium tin oxide alloy target crude product;
D) annealing the crude indium tin oxide alloy target, and plasma spraying the mixture obtained in the step A) onto the surface of the annealed crude indium tin oxide alloy target to obtain the indium tin oxide alloy target.
2. The preparation method according to claim 1, wherein in the step A), the mass ratio of the indium oxide to the tin oxide is (6-8): (2-4), the Fischer-Tropsch average particle size of the indium oxide is 1-7 mu m, and the Fischer-Tropsch average particle size of the tin oxide is 1-7 mu m.
3. The preparation method according to claim 1, wherein in the step B), the cold isostatic pressing pressure is 10-60 MPa, the secondary pressing pressure is 50-200 MPa, and the density of the alloy target green body is greater than 98% of the relative density.
4. The preparation method according to claim 1, wherein in the step C), the vacuum hot-pressing sintering is performed under a hydrogen protective atmosphere, the pressure is 20-30 MPa, and the temperature is 200-300 ℃.
5. The method according to claim 1, wherein the step D) further comprises, before the plasma spraying:
ball milling the mixture obtained in step A) and sieving.
6. The method according to claim 1, wherein when the ito target is a target with a hollow cylinder, the method further comprises, after the plasma spraying of the mixture on the surface of the annealed ito target crude product:
vacuumizing the obtained indium tin oxide alloy target material, and carrying out plasma spraying on the mixture obtained in the step A) in an inert atmosphere to a cavity of the target material.
7. The preparation method according to claim 1, wherein in the step D), the annealing temperature is 100-300 ℃ and the annealing time is 3-5 h.
8. The preparation method according to claim 1, wherein in the step A), the vacuum pressure in the vacuum rolling mixer is 2 x 10 degrees Pa, and the rotating speed is 50-80 r/min.
9. The method of claim 1, further comprising, after the mixing in step a):
selecting a plurality of different areas from the mixed material to respectively detect the contents of indium oxide and tin oxide until the ratio error of the indium oxide content to the tin oxide content of each detection point is 0.01-0.3%, and completing mixing.
10. The method according to claim 1, wherein the step B) further comprises placing the mixture in a tubular rubber sleeve and sealing the rubber sleeve before the step of evacuating.
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