CN111943650B

CN111943650B - IWO target material for activated plasma deposition technology and preparation method thereof

Info

Publication number: CN111943650B
Application number: CN202010709846.8A
Authority: CN
Inventors: 陈明飞; 刘永成; 江长久; 陈明高; 徐胜利; 郭梓旋; 莫国仁; 李跃辉
Original assignee: Enam Optoelectronic Material Co ltd
Current assignee: Enam Optoelectronic Material Co ltd
Priority date: 2020-07-22
Filing date: 2020-07-22
Publication date: 2022-11-29
Anticipated expiration: 2040-07-22
Also published as: CN111943650A

Abstract

The invention discloses an IWO target material for an activated plasma deposition technology and a preparation method thereof. The oxide target material mainly comprises indium oxide and contains a doping element tungsten, the content of tungsten is 0.003-0.05 calculated by the atomic ratio of W/(In + W), the sintered body also contains a silicon element accounting for 5-600ppm of the total weight ratio of the sintered body besides the two elements, one or a combination of several metal elements of titanium (Ti), molybdenum (Mo), zirconium (Zr) and hafnium (Hf) can be further added as the doping element besides tungsten, the total content of tungsten and the combination of the metal elements is 0.003-0.05 calculated by the atomic ratio of (W + x)/(In + W + x), and the target material also contains the silicon element accounting for 5-600ppm of the total weight ratio of the sintered body besides the element metering ratios of the different combinations.

Description

IWO target material for activated plasma deposition technology and preparation method thereof

Technical Field

The invention belongs to the technical field of activated plasma deposition, and particularly relates to an IWO target material for an activated plasma deposition technology and a preparation method thereof.

Background

Among various film materials, the transparent conductive film can be widely applied to the fields of solar cells, building energy-saving glass, various sensors, flat panel display and the like. Among them, the indium oxide material is an n-type semiconductor material, and is widely used in solar cells because of its unique physical properties such as electrical conductivity close to that of metal, high visible light transmittance, and the like. The indium oxide material film is prepared by a plurality of methods, and the methods are vacuum thermal evaporation, electron beam evaporation, magnetron sputtering, plasma enhanced chemical vapor deposition, spraying method and sol-gel method. The first four methods need to be completed in a vacuum environment, and because the method is not influenced by various impurities in the air, purer materials can be obtained, the film forming quality is higher, the corresponding cost is higher, and the large-area preparation is more difficult. The latter two methods can be completed under atmospheric pressure, large-area preparation is easier and cost is lower, but it is difficult to obtain a pure high-quality film.

Activated Plasma Deposition (RPD) is a recently developed method of depositing thin films with significant advantages. Its main advantages include: (1) The low bombardment damage to the substrate, the RPD coating can be regarded as an ion auxiliary evaporation technology essentially, the particle energy is small in the coating process, high-energy particles hardly exist, and the low-energy particles avoid the damage to the surface of the substrate; (2) The high-quality film can be obtained at low temperature, and the specificity of the RPD deposition process ensures that the high-quality film can be obtained under the low-temperature condition; (3) The utilization rate of the source material is high, the RPD coating can control the power density of the plasma beam reaching the crucible, the utilization rate of the evaporation source material is finally improved and is far higher than that of the sputtering target material, and a foundation is laid for reducing the cost; (4) The RPD equipment has wide application, and can be used for preparing IWO, AZO, GZO and other transparent conductive films.

The RPD coating film is formed by vaporizing and dissociating the sintered body by plasma and reacting on the substrate. Compared with the sputtering process, the sintered body material is gasified by the heat energy of the plasma and diffused to the surface of the substrate in the form of ions, and has weak bombardment effect on the substrate. Unlike reactive magnetron sputtering, the "reaction" in reactive magnetron sputtering refers to the introduction of a reactive gas to obtain a compound thin film, for example, oxygen is introduced during the preparation of an indium tin oxide thin film, and the reactive substance in the RPD utilizes the source substance itself and reaches the substrate in the form of ions to perform a chemical reaction.

In the prior art, the IWO target has low density and belongs to a non-compact body, the problem of powder falling exists in the use process, after the problem of powder falling occurs, hidden dangers can be brought to continuous production, the continuous production can be continued after the machine is stopped to clean the track, and the production efficiency is reduced. The patent CN103347836A discloses that an indium oxide sintered body doped with tungsten is applied to an RPD technology for coating, and the core of the method is that a sintered body with a dual-phase structure is obtained by mixing and sintering indium oxide crystalline phase powder and indium oxide powder which have a bixbyite structure and are solid-dissolved with tungsten, so that the problems of cracking and splashing of the sintered body in the coating process are avoided. However, the problem that a small amount of powder falls off during the use process of the client still occurs, and hidden troubles are brought to continuous production.

Meanwhile, as a transparent conductive film for a solar cell, it is required to have high light transmittance at a cut-off wavelength of 1200 nm and to have good conductivity. The light transmittance of the ITO film widely used at present in 1200 nm is difficult to be greatly improved, and the material which is high in conductivity and suitable for RPD coating is prepared, so that the conversion efficiency of the solar cell is favorably improved.

Disclosure of Invention

Problems to be solved by the invention

The invention provides an IWO target material for an activated plasma deposition technology and a preparation method thereof. The invention aims to solve the problem that the IWO target material has low density, so that the powder falling problem in the using process is caused, and the continuous operation of the coating process is influenced, so that the production efficiency is reduced. The invention solves the problem of sintered body powder falling in the coating process by adding trace silicon element of the binding phase on the premise of not reducing the coating quality.

Means for solving the problems

In order to solve the above problems, the present inventors have made detailed studies on the influence of the relationship between the amount of silicon element added and the temperature on the density of the sintered body, and on the influence of the occurrence of cracks, or splashes in the RPD plating film.

Therefore, the invention provides an IWO target material for an activated plasma deposition technology and a preparation method thereof.

The first aspect of the invention provides an IWO target material, which comprises indium oxide and tungsten doped with element; the content of the doping element tungsten is 0.003 to 0.05 In terms of the atomic ratio of W/(In + W); besides the two elements, the IWO target material also contains silicon element accounting for 5 to 600ppm of the total weight of the IWO target material.

According to some embodiments of the invention, the method further comprises doping the element x while doping the metal tungsten, wherein the doping element x is at least one of titanium, molybdenum, zirconium and hafnium, and the total content of the tungsten and the doping element x In combination is 0.003 to 0.05 In terms of an atomic ratio of (W + x)/(In + W + x).

According to some embodiments of the invention, the content of the elemental silicon in the sintered body is 5 to 600 ppm.

According to some embodiments of the invention, the content of the elemental silicon in the sintered body is 20 to 60ppm.

The second aspect of the present invention provides a method for preparing the above IWO target, comprising the following steps:

s1: weighing the indium oxide, the doping element tungsten and the doping element x according to the proportion, uniformly mixing the indium oxide, the doping element tungsten and the doping element x, and then carrying out certain high-temperature treatment to obtain indium oxide crystalline phase powder with a bixbyite structure and tungsten and the doping element x in solid solution;

s2: adding nano silicon oxide powder or silicon dioxide sol into the indium oxide crystalline phase powder which has the bixbyite structure and is solid-dissolved with tungsten and doping element x and is obtained in the step S1 according to the amount of silicon of 5-600ppm of the total weight, uniformly mixing, and then pressing and forming to obtain a blank body with the required size;

s3: and (3) sintering the blank obtained in the step (S2) to obtain the IWO target material for activating the plasma deposition technology.

According to some embodiments of the invention, the temperature of the high temperature treatment in step S1 is 1300 to 1600 ℃.

According to some embodiments of the invention, in step S1, the high temperature treatment time is 2 to 72 hours.

According to some embodiments of the invention, in step S3, the sintering temperature is 650 to 1450 ℃.

According to some embodiments of the invention, in the step S3, the sintering temperature is 700 to 1100 ℃.

According to some embodiments of the invention, in step S3, the sintering time is 2-72h.

The IWO target material according to the embodiment of the invention at least has the following technical effects:

the invention has the following effects:

in the technical scheme of the invention, the silicon element has no doping effect, the content of the silicon element in the sintered body is 5-600ppm, and the addition mode of the silicon element is at least one of nano silicon oxide powder and silicon dioxide sol. According to the technical scheme, the extremely trace silicon element is added, a binding phase is formed after sintering, and the problem of powder falling of a sintered body in the using process is solved on the premise of not reducing the quality of a coating film.

In the technical scheme of the invention, the target material is a non-compact body with the relative density of about 60% (theoretical density is 7.18g/cm < 3 >), and is suitable for RPD evaporation.

The IWO target prepared by the invention can continuously and stably obtain the crystalline transparent conductive film with low resistivity and high infrared light transmittance through RPD evaporation, is applied to the solar cell, can obtain higher light transmittance in the range of 940-1200 nm compared with the ITO film widely used at present, and has higher photoelectric conversion efficiency.

Drawings

Fig. 1 is an XRD test pattern of indium oxide crystalline phase powder having a bixbyite structure with tungsten solid-dissolved therein.

Detailed Description

The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.

Example 1

In this example, a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours at an atomic ratio of W/(In + W) of 0.03 to obtain a powder of indium oxide crystal phase having a bixbyite structure and containing tungsten In a solid solution, as shown In FIG. 1. Then mixing with 5 ppm silicon dioxide sol, pressing into blank with relative density of 58%, sintering at 900 deg.C for 5 hr to obtain target with sintering density of 60%. The sintered target material is loose, has obvious powder falling phenomenon, is not beneficial to transportation, and does not utilize continuous production.

Example 2

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixed material of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 10 ppm, and pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 3

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixture of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten solid-dissolved therein, and then mixed with a silica sol having a total weight content of 20 ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 4

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixed material of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 5

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixture of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten solid-dissolved therein, and then mixed with a silica sol having a total weight content of 100ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 6

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixed material of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 200 ppm, and pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 7

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixture of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten solid-dissolved therein, and then mixed with a silica sol having a total weight content of 600ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 63%. After sintering, the shrinkage is too large, the density is higher, the size is smaller, and the size control requirement is not met.

Example 8

In this example, a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten solid-dissolved therein, mixed with a silica sol containing 50ppm by weight, and then pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%, wherein the atomic ratio of W/(In + W) was 0.003. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 9

In this example, the atomic ratio of W/(In + W) was 0.008, and a mixture of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol containing 50ppm by weight and pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 10

In this example, a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystal phase powder having a bixbyite structure and having tungsten dissolved therein, mixed with a silica sol having a total weight content of 50ppm, and then pressed into a green body having a relative density of 58%, and sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%, wherein the atomic ratio of W/(In + W) was 0.015. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 11

In this example, the atomic ratio of W/(In + W) was 0.02, and a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture was pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 12

In this example, the atomic ratio of W/(In + W) was 0.04, and a mixture of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain a powder of indium oxide crystal phase having a bixbyite structure and having tungsten dissolved therein, and the powder was mixed with a silica sol containing 50ppm by weight and then pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 13

In this example, a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and containing tungsten as a solid solution, and the indium oxide crystalline phase powder was mixed with a silica sol containing 50ppm by weight and pressed into a green body having a relative density of 58%, and then sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%, wherein the atomic ratio of W/(In + W) was 0.05. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 14

In addition to the first oxide target material, a Ti element is further added In addition to indium and tungsten, the total content of tungsten and the Ti element is 0.03 In terms of the atomic ratio of (W + Ti)/(In + W + Ti), the oxide mixed material is treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder which has a bixbyite structure and is dissolved with tungsten, and then the indium oxide crystalline phase powder is mixed with silica sol with the total weight content of 50ppm, pressed into a blank with the relative density of 58 percent and sintered at 900 ℃ for 5 hours to obtain the target material with the sintering density of about 60 percent. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 15

In addition to indium and tungsten, the first oxide target material further contains Hf element In addition, the total content of tungsten and Hf element is 0.03 In terms of the atomic ratio of (W + Hf)/(In + W + Hf), the oxide mixture is treated at 1200 ℃ for 8 hours to obtain indium oxide crystal phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with 50ppm by weight of silica sol, pressed into a green body having a relative density of 58%, and sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 16

In addition to indium and tungsten, zr element is further added to the first oxide target material, and the total content of tungsten and Zr element is 0.05 In terms of (W + Zr)/(In + W + Zr) atomic ratio, the oxide mixture is treated at 1200 ℃ for 8 hours to obtain indium oxide crystal phase powder having a bixbyite structure and having tungsten dissolved therein, and the indium oxide crystal phase powder is mixed with a silica sol having a total weight content of 50ppm, pressed into an embryo having a relative density of 58%, and sintered at 900 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 17

In addition to indium and tungsten, the first oxide target material further contains Mo element, the total content of tungsten and Mo element is (W + Mo)/(In + W + Mo) atom ratio is 0.05, the oxide mixed material is treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder which has a bixbyite structure and is dissolved with tungsten, and then mixed with 50ppm silica sol by weight, pressed into a blank with the relative density of 58%, and sintered at 900 ℃ for 5 hours to obtain the target material with the sintering density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 18

In addition to indium and tungsten, the first oxide target material further contains Mo element, the total content of tungsten and Mo element is (W + Mo + Zr)/(In + W + Mo + Zr) atom ratio is 0.05, the oxide mixed material is treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder which has a bixbyite structure and is dissolved with tungsten, and then the indium oxide crystalline phase powder is mixed with silica sol with the total weight content of 50ppm and is pressed into a blank with the relative density of 58 percent, and the blank is sintered at 900 ℃ for 5 hours to obtain the target material with the sintering density of about 60 percent. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 19

In this example, the atomic ratio of W/(In + W) was 0.03, and a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture was pressed into a green body having a relative density of 58%, and then sintered at 650 ℃ for 5 hours to obtain a target having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 20

In this example, the atomic ratio of W/(In + W) was 0.03, and a mixed material of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture was pressed into a green body having a relative density of 58%, and then sintered at 750 ℃ for 5 hours to obtain a target having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 21

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixture of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten solid-dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 1050 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 22

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixed material of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 1250 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Example 23

In this example, the atomic ratio of W/(In + W) is 0.03, and a mixture of indium oxide and tungsten oxide is subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and having tungsten dissolved therein, and then mixed with a silica sol having a total weight content of 50ppm, and the mixture is pressed into a green body having a relative density of 58%, and then sintered at 1450 ℃ for 5 hours to obtain a target material having a sintered density of about 60%. The RPD evaporation experiments were performed without causing cracking, or splashing and dusting problems.

Comparative example 1

This example differs from example 1 in that no silica was added. When the RPD evaporation experiment is carried out, cracks or splashing are not caused, but the powder falling problem exists, so that the continuous production is not facilitated.

Comparative example 2

This example differs from example 8 in that no silica was added. When the RPD evaporation experiment is carried out, cracks or splashing are not caused, but the powder falling problem exists, so that the continuous production is not facilitated.

Comparative example 3

This example differs from example 14 in that no silicon oxide was added. When the RPD evaporation experiment is carried out, cracks or splashing are not caused, but the powder falling problem exists, so that the continuous production is not facilitated.

Detection example 1

Table 1 shows the detailed formulation and the test results of the targets of examples 1 to 22 and comparative examples 1 to 3.

TABLE 1

Remarking: OK indicates qualified, and meets the requirements, and NG indicates unqualified.

In examples 1 to 7, indium oxide powder and tungsten oxide powder were used as raw material powders, indium oxide was used as a main component, tungsten was used as an additive element, and the content of tungsten was 0.03 In terms of the atomic ratio of W/(In + W). Treating the mixed material of indium oxide and tungsten oxide at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder which has a bixbyite structure and is dissolved with tungsten, mixing the indium oxide crystalline phase powder with silicon dioxide sol with the total weight content of 3-650ppm, pressing the mixture into a blank with the relative density of 58%, and sintering the blank at 900 ℃ for 5 hours to obtain the target with the sintering density of about 60%. In examples 1 to 7, the RPD vapor deposition experiments were carried out, and there were no problems such as cracking, splashing, and powder falling.

The target materials of examples 8 to 13 were prepared by using indium oxide powder and tungsten oxide powder as raw material powders, using indium oxide as a main component and tungsten as an additive element, wherein the content of tungsten is 0.003 to 0.05 In terms of an atomic ratio of W/(In + W), subjecting a mixture of indium oxide and tungsten oxide to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and containing tungsten dissolved therein, mixing the indium oxide crystalline phase powder with a silica sol containing 50ppm by weight, pressing the mixture into a green body having a relative density of 58%, and sintering the green body at 900 ℃ for 5 hours to obtain a target material having a density of about 60%. The sintered sheet body has good strength and no powder falling condition, and an RPD evaporation experiment is carried out. Without causing cracking, or splashing and dusting problems. The performance completely meets the use performance requirements of customers. The content of tungsten is preferably 0.003 to 0.05 In terms of the atomic ratio of W/(In + W), and the film has stable properties.

In examples 14 to 18, in addition to indium and tungsten, other metal elements were further added, and the total content of tungsten and the other metal elements was 0.003 to 0.05 In terms of the atomic ratio of (W + x)/(In + W + x), and the oxide mixture was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and containing tungsten as a solid solution, and then mixed with 50ppm by weight of a silica sol, pressed into a green body having a relative density of 58%, and sintered at 900 ℃ for 5 hours to obtain a target having a sintered density of about 60%, which was free from a powder drop problem by performing an RPD evaporation test.

In examples 19 to 23, indium oxide powder and tungsten oxide powder were used as raw material powders, indium oxide was used as a main component, tungsten was used as an additive element, the content of tungsten was 0.03 In terms of the atomic ratio of W/(In + W), a mixture of indium oxide and tungsten oxide was treated at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and containing tungsten dissolved therein, and the indium oxide crystalline phase powder was mixed with a silica sol containing 50ppm by weight and pressed into a green body having a relative density of 58%, and then sintered at 650 to 1450 ℃ to obtain sintered sheets. RPD evaporation experiments were performed. No powder falling.

In comparative examples 1 to 3, indium oxide powder and tungsten oxide powder were used as raw material powders, indium oxide was used as a main component, tungsten was used as an additive element, the content of tungsten was 0.003 to 0.05 In terms of the atomic ratio of W/(In + W), a mixture of indium oxide and tungsten oxide was subjected to high-temperature treatment at 1200 ℃ for 8 hours to obtain indium oxide crystalline phase powder having a bixbyite structure and containing tungsten In a solid solution, and a green body having a relative density of 58% was directly pressed without adding silica sol and silica nanopowder, and then sintered at 900 ℃ for 5 hours. The strength of the sintered pellet was good. The RPD evaporation experiment is carried out, the powder falling phenomenon is obvious in the using process, and hidden danger is brought to equipment continuous production.

Claims

1. An IWO target material for activating a plasma deposition technology is characterized by comprising indium oxide and doped element tungsten; the content of the doping element tungsten is 0.003 to 0.05 In terms of the atomic ratio of W/(In + W); the IWO target also comprises silicon element accounting for 5-600ppm of the total weight of the IWO target;

the silicon element is added in at least one of nano silicon oxide powder and silicon dioxide sol;

the preparation method of the IWO target for the activated plasma deposition technology comprises the following steps:

s1: weighing indium oxide and tungsten-doped oxide according to a ratio, uniformly mixing the indium oxide and the tungsten-doped oxide, and performing high-temperature treatment to obtain indium oxide crystalline phase powder which has a bixbyite structure and is in solid solution with tungsten;

s2: adding a silicon element into the indium oxide crystalline phase powder which is obtained in the step S1, has a bixbyite structure and is solid-dissolved with tungsten, uniformly mixing, and then pressing and forming to obtain a blank body with a required size;

s3: sintering the blank obtained in the step S2 to obtain the IWO target material for activating the plasma deposition technology;

in step S3, the sintering temperature is 700-1100 ℃.

2. The IWO target according to claim 1, further comprising a doping element x, the doping element x being at least one of titanium (Ti), molybdenum (Mo), zirconium (Zr) and hafnium (Hf), and the total content of tungsten and the doping element x being 0.003 to 0.05 In terms of an atomic ratio of (W + x)/(In + W + x).

3. The IWO target according to claim 1, wherein the elemental silicon is present in the IWO target in an amount of 20 to 60ppm.

4. The IWO target according to claim 1, wherein the high temperature treatment temperature in step S1 is 1300-1600 ℃.

5. The IWO target according to claim 1, wherein the high temperature treatment time in step S1 is 2-72h.

6. The IWO target according to claim 1, wherein in step S3, the sintering time is 2-72h.