A method for preparing IZrO target material

Abstract

The present invention relates to the technical field of target material manufacturing, and in particular to a method for preparing an IZrO target material. The method for preparing an IZrO target material of the present invention comprises powder preparation, powder molding, green embryo sintering and heat treatment; the powder preparation is to first hydrolyze indium oxide powder and zirconium oxide powder, and then prepare IZrO nanopowder by a sol-gel method. The IZrO target material obtained by the method for preparing an IZrO target material of the present invention uses a composite complexing agent instead of traditional salicylic acid in the sol-gel process, so that the particle distribution is more uniform, and the target material finally obtained has excellent density and low resistivity, and the surface of the target material is relatively flat, and the uniformity is greatly improved.

Description

Technical Field

[0001] The invention relates to the technical field of target material manufacturing, and in particular to a method for preparing an IZrO target material. Background Art

[0002] Transparent conductive oxide (TCO) materials, such as indium tin oxide (ITO), are widely used in photovoltaic cells, displays and other fields. However, ITO materials have problems such as high cost, low near-infrared transmittance and brittleness, which limit the further expansion of their applications. Therefore, studying new transparent conductive materials to replace or improve the performance of existing materials has become a current research hotspot.

[0003] Patent document CN202310998914.0 discloses a method for preparing a high-density, low-mobility indium zinc oxide rare earth doped target material, including raw material selection, ball milling, calcination, ball milling, granulation, molding, and sintering, so that the final indium zinc oxide target material has a good density; Patent document CN202010755647.0 discloses a method for preparing a molybdenum-doped indium oxide target material and a molybdenum-doped indium oxide target material. The target material prepared by the invention has a high density and good uniformity of component distribution. The transparent conductive film prepared by the target material is conducive to the transmission of infrared light. Although the target materials obtained by the above inventions have excellent density, the particle size and composition obtained by ball milling are not uniform, and the surface of the target material formed is uneven, which is bound to affect the subsequent sputtering effect. Summary of the invention

[0004] In view of this, the purpose of the present invention is to provide a method for preparing an IZrO target material to solve the problem that the surface of the target material prepared in the prior art is not smooth and uniform enough.

[0005] Based on the above purpose, the present invention provides a method for preparing an IZrO target, comprising the following steps:

[0006] S1 powder preparation: indium oxide powder and zirconium oxide powder are mixed to obtain mixed powder, and then the mixed powder is dispersed in an ethanol solution, a stabilizer and a complex complexing agent are added, and the mixture is reacted at 75-85°C for 3-4 hours, centrifuged, and dried to obtain IZrO nanopowder;

[0007] S2 powder molding: IZrO nanopowder is pressed into blanks using cold isostatic pressing technology;

[0008] S3 green embryo sintering: plasma-assisted sintering of the green embryo;

[0009] S4 heat treatment: The sintered green body is first kept at 450°C for 1 hour, and then cooled to room temperature at 100°C / h to obtain the IZrO target;

[0010] The composite complexing agent in step S1 is a mixture of acetic acid and salicylic acid in a weight ratio of 3-5:1.

[0011] Preferably, in step S1, the weight ratio of the indium oxide powder to the zirconium oxide powder is 10-20:1.

[0012] Preferably, the particle sizes of the indium oxide powder and the zirconium oxide powder in step S1 are both 50-300 μm.

[0013] Preferably, the weight ratio of the mixed powder, ethanol solution, stabilizer and composite complexing agent in step S1 is 1-1.5:100-200:0.1-0.2:0.5-1.

[0014] Preferably, the stabilizer in step S1 is sodium acetate.

[0015] Preferably, the purity of the indium oxide powder and the zirconium oxide powder in step S1 is 4N.

[0016] Preferably, the pressure of the cold isostatic pressing in step S2 is 300-400 MPa.

[0017] Preferably, the parameters of the plasma-assisted sintering in step S3 are: 1300° C., sintering time of 6-8 h, plasma power of 5 kW, and magnetic field strength of 1 T.

[0018] Beneficial effects of the present invention:

[0019] The present invention prepares IZrO powder by first hydrolyzing indium oxide powder and zirconium oxide powder and then performing a sol-gel method, so that the component distribution and particle size of the IZrO powder are more uniform, thereby significantly improving the surface uniformity of the target material finally obtained.

[0020] In the present invention, a composite complexing agent is used to replace salicylic acid in the sol-gel process, so that the uniformity of the sol is improved, the component distribution of the formed IZrO powder is more uniform and stable, and thus the surface uniformity of the target material is improved. DETAILED DESCRIPTION

[0021] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0022] Embodiment 1: A method for preparing an IZrO target, the specific steps are as follows:

[0023] (1) mixing acetic acid and salicylic acid in a weight ratio of 3:1, stirring evenly, and obtaining a composite complexing agent;

[0024] (2) indium oxide powder and zirconium oxide powder were mixed uniformly at a weight ratio of 10:1 to obtain a mixed powder, and then 10 g of the mixed powder was dispersed in 1000 g of ethanol solution, 1 g of a stabilizer and 5 g of a composite complexing agent were added, and the mixture was reacted at 75° C. for 3 h, centrifuged, and dried to obtain IZrO nanopowder;

[0025] (3) Using cold isostatic pressing technology to press the IZrO nanopowder into a blank, wherein the cold pressing pressure is 300 MPa;

[0026] (4) Plasma-assisted sintering of the green embryo, wherein the sintering temperature is 1300° C., the sintering time is 6 h, the plasma power is 5 kW, and the magnetic field strength is 1 T;

[0027] (5) The sintered green body is first kept at 450°C for 1 hour, and then cooled to room temperature at 100°C / h to obtain the IZrO target.

[0028] Embodiment 2: A method for preparing an IZrO target, the specific steps are as follows:

[0029] (1) mixing acetic acid and salicylic acid in a weight ratio of 4:1, stirring evenly, and obtaining a composite complexing agent;

[0030] (2) indium oxide powder and zirconium oxide powder were mixed uniformly at a weight ratio of 15:1 to obtain a mixed powder, and then 13 g of the mixed powder was dispersed in 1500 g of ethanol solution, 1.5 g of a stabilizer and 7.5 g of a complexing agent were added, and the mixture was reacted at 80° C. for 4 h, centrifuged, and dried to obtain IZrO nanopowder;

[0031] (3) Using cold isostatic pressing technology to press the IZrO nanopowder into a blank, wherein the cold pressing pressure is 350 MPa;

[0032] (4) Plasma-assisted sintering of the green embryo, wherein the sintering temperature is 1300° C., the sintering time is 7 h, the plasma power is 5 kW, and the magnetic field strength is 1 T;

[0033] (5) The sintered green body is first kept at 450°C for 1 hour, and then cooled to room temperature at 100°C / h to obtain the IZrO target.

[0034] Embodiment 3: A method for preparing an IZrO target, the specific steps are as follows:

[0035] (1) mixing acetic acid and salicylic acid in a weight ratio of 5:1, stirring evenly, and obtaining a composite complexing agent;

[0036] (2) indium oxide powder and zirconium oxide powder were mixed uniformly at a weight ratio of 20:1 to obtain a mixed powder, and then 15 g of the mixed powder was dispersed in 2000 g of ethanol solution, 2 g of stabilizer and 10 g of composite complexing agent were added, reacted at 85° C. for 4 h, centrifuged, and dried to obtain IZrO nanopowder;

[0037] (3) Using cold isostatic pressing technology to press the IZrO nanopowder into a blank, wherein the cold pressing pressure is 400 MPa;

[0038] (4) Plasma-assisted sintering of the green embryo, wherein the sintering temperature is 1300° C., the sintering time is 8 h, the plasma power is 5 kW, and the magnetic field strength is 1 T;

[0039] (5) The sintered green body is first kept at 450°C for 1 hour, and then cooled to room temperature at 100°C / h to obtain the IZrO target.

[0040] Comparative Example 1: A method for preparing an IZrO target, the specific steps are as follows:

[0041] (1) After indium oxide powder and zirconium oxide powder were mixed uniformly in a weight ratio of 15:1 to obtain a mixed powder, 1 g of polyethylene glycol and 9 g of deionized water were added to the mixture, and the mixture was ball-milled at 450 rpm for 9 h to obtain a ball-milled slurry, which was granulated to obtain a composite powder;

[0042] The remaining steps are the same as in Example 2.

[0043] Comparative Example 2: A method for preparing an IZrO target, the specific steps are as follows:

[0044] Indium nitrate and zirconium nitrate (molar ratio of indium to zirconium is 95:5) are dissolved in 1000 g of deionized water, followed by adding 7.5 g of a composite complexing agent, reacting at 80° C. for 4.5 h, followed by drying at 120° C. for 24 h, grinding, calcining at a high temperature of 1200° C. for 20-50 h, and grinding to obtain IZrO powder;

[0045] The remaining steps are the same as in Example 2.

[0046] Comparative Example 3: A method for preparing an IZrO target, the specific steps are as follows:

[0047] The difference from Example 2 is that the composite complexing agent is replaced by an equal amount of salicylic acid.

[0048] Comparative Example 4: A method for preparing an IZrO target, the specific steps are as follows:

[0049] Indium nitrate and zirconium nitrate (molar ratio of indium to zirconium is 95:5) are dissolved in 1000 g of deionized water, followed by adding 7.5 g of salicylic acid, reacting at 80 °C for 4.5 h, followed by drying at 120 °C for 24 h, grinding, calcining at a high temperature of 1200 °C for 20-50 h, and grinding to obtain IZrO powder;

[0050] The remaining steps are the same as in Example 2.

[0051] Performance Testing

[0052] Target density: The obtained samples were tested according to the Archimedes drainage method, and the test results are shown in Table 1;

[0053] Resistivity: The resistivity of the obtained samples was measured by a four-probe test method. The test results are shown in Table 1.

[0054] Surface roughness: The surface roughness of the obtained samples was measured using a surface profiler. The test results are shown in Table 1.

[0055] Table 1 Performance test results

[0056] Density(%) Resistivity (Ω·cm) Roughness(nm) Example 1 98.8 <![CDATA[5.5×10 -3 ]]> 7 Example 2 99.2 <![CDATA[5.3×10 -3 ]]> 6 Example 3 98.5 <![CDATA[6×10 -3 ]]> 7 Comparative Example 1 97.1 <![CDATA[6.4×10 -3 ]]> 25 Comparative Example 2 96.4 <![CDATA[5.7×10 -3 ]]> 14 Comparative Example 3 97.4 <![CDATA[6.6×10 -3 ]]> 11 Comparative Example 4 98.5 <![CDATA[7.9×10 -3 ]]> 17

[0057] Data analysis shows that the IZrO target obtained by the preparation method of the IZrO target of the present invention has a higher density and a lower resistivity, and its density is not less than 98%, and its resistivity is not higher than 6×10 -3 Ω·cm, and most importantly, the target surface has a high uniformity and the surface roughness does not exceed 7nm.

[0058] It can be seen from Example 2 and Comparative Examples 1 and 2 in Table 1 that the present invention prepares IZrO powder by hydrolysis followed by sol-gel method, so that the composition and particle size of the IZrO powder are more uniform, and the surface uniformity of the target material finally obtained is significantly improved.

[0059] It can be seen from Example 2 and Comparative Examples 3 and 4 in Table 1 that the present invention uses a composite complexing agent to replace salicylic acid in the sol-gel process, so that the uniformity of the sol is improved, and the final particles are more uniform and stable. After pressing and sintering, the surface uniformity of the target material is improved.

[0060] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

Claims

1. A method for preparing an IZrO target, characterized in that: The following steps are involved: S1 powder preparation: indium oxide powder and zirconium oxide powder are mixed to obtain mixed powder, and then the mixed powder is dispersed in an ethanol solution, a stabilizer and a complex complexing agent are added, and the mixture is reacted at 75-85°C for 3-4 hours, centrifuged, and dried to obtain IZrO nanopowder; S2 powder molding: IZrO nanopowder is pressed into blanks using cold isostatic pressing technology; S3 green embryo sintering: plasma-assisted sintering of the green embryo; S4 heat treatment: The sintered green body is first kept at 450°C for 1 hour, and then cooled to room temperature at 100°C / h to obtain the IZrO target; The composite complexing agent in step S1 is a mixture of acetic acid and salicylic acid in a weight ratio of 3-5:

1.

2. The method for preparing an IZrO target according to claim 1, characterized in that: The weight ratio of the indium oxide powder to the zirconium oxide powder in step S1 is 10-20:

1.

3. The method for preparing an IZrO target according to claim 1, characterized in that: The particle sizes of the indium oxide powder and the zirconium oxide powder in step S1 are both 50-300 μm.

4. The method for preparing an IZrO target according to claim 1, characterized in that: The weight ratio of the mixed powder, ethanol solution, stabilizer and composite complexing agent in step S1 is 1-1.5:100-200:0.1-0.2:0.5-1.

5. The method for preparing an IZrO target according to claim 1, characterized in that: The stabilizer in step S1 is sodium acetate.

6. The method for preparing an IZrO target according to claim 1, characterized in that: The purity of the indium oxide powder and the zirconium oxide powder in step S1 is both 4N.

7. The method for preparing an IZrO target according to claim 1, characterized in that: The pressure of the cold isostatic pressing in step S2 is 300-400 MPa.

8. The method for preparing an IZrO target according to claim 1, characterized in that: The parameters of the plasma assisted sintering in step S3 are: 1300° C., sintering time of 6-8 h, plasma power of 5 kW, and magnetic field strength of 1 T.