Silicon-aluminum-zirconium-tungsten gradient doped target material and low-temperature sintering preparation method thereof

Abstract

The invention discloses a low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target material, which comprises the following steps: cleaning a substrate, and removing oil stains and impurities on the substrate; silicon, aluminum and zirconium are used as first target raw materials, tungsten is used as second target raw materials, the substance mass ratio of silicon to aluminum to zirconium to tungsten is 55: 5: 35: 5, the tungsten gradient target is formed, the sputtering power is 100 W, and the sputtering time is 1 h. According to the silicon-aluminum-zirconium-tungsten gradient doping target material, low-temperature sintering is conducted, silicon, aluminum and zirconium serve as first target material raw materials, tungsten serves as second target material raw materials, sputtering treatment is conducted, meanwhile, ultrasonic liquid treatment is conducted, yttrium oxide bodies and modified liquid in ultrasonic liquid are evenly mixed and subjected to ball milling improvement, yttrium oxide, nanometer silica sol and urea in the yttrium oxide bodies are co-matched for improvement, and the silicon-aluminum-zirconium-tungsten gradient doping target material is obtained. And the modified liquid is modified, so that the conductivity and transparency of the prepared gradient doped target material are coordinated, and the corrosion-resistant stability effect of the product is remarkable.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and in particular to a silicon-aluminum-zirconium-tungsten gradient-doped target material and a low-temperature sintering preparation method thereof. Background Art

[0002] The requirements for sputtering targets are higher than those in the traditional materials industry. General requirements include size, flatness, purity, impurity content, density, N / O / C / S, grain size and defect control; higher or special requirements include: surface roughness, resistance value, grain size uniformity, composition and structure uniformity, foreign matter (oxide) content and size, magnetic permeability, ultra-high density and ultra-fine grains, etc.

[0003] For the application of existing target products in the high-end glass industry, it is necessary to optimize the conductivity of the target products and improve the transparency of the products. The coordination of the two performances and the corrosion resistance and stability of the products are the technical difficulties of the present invention. Based on this, the present invention provides a silicon-aluminum-zirconium-tungsten gradient doped target material and a low-temperature sintering preparation method thereof. Summary of the Invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide a silicon-aluminum-zirconium-tungsten gradient doped target material and a low-temperature sintering preparation method thereof to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solutions: The present invention provides a low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient-doped target material, comprising the following steps: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

[0006] Preferably, the ultrasonic power of the ultrasonic treatment is 200-250W, and the ultrasonic treatment is performed for 1 hour; the sintering temperature of the sintering improvement treatment is 1050-1100° C., and the sintering is performed for 2 hours.

[0007] Preferably, the preparation method of the ultrasonic liquid is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

[0008] Preferably, the mass fraction of the urea solution is 2-5%; the rotation speed of the mixing ball milling treatment is 1500 r / min, and the ball milling is performed for 2 hours.

[0009] Preferably, the preparation method of the modified liquid is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution which is 3-5 times the total amount of zinc oxide, and then titanium oxide which is 10-15% of the total amount of zinc oxide and a silane coupling agent which is 3-5% of the total amount of zinc oxide are added, and stirred evenly to obtain a modified solution.

[0010] Preferably, the silane coupling agent is silane coupling agent KH550.

[0011] Preferably, the carboxymethyl cellulose sodium solution is prepared by uniformly blending sodium carboxymethyl cellulose, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of (2-5):5:(1-2).

[0012] Preferably, the mass fraction of the sodium silicate solution is 3-6%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

[0013] The present invention also provides a silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by a low-temperature sintering preparation method of the silicon-aluminum-zirconium-tungsten gradient-doped target material.

[0014] Compared with the prior art, the present invention has the following beneficial effects: The silicon-aluminum-zirconium-tungsten gradient doped target material of the present invention is sintered at low temperature, silicon, aluminum and zirconium are used as the first target material raw materials and tungsten is used as the second target material raw material, and is sputtered. At the same time, it is treated with ultrasonic liquid, the yttrium oxide body and the modifying liquid in the ultrasonic liquid are mixed and ball milled for improvement, the yttrium oxide, nano-silica sol and urea in the yttrium oxide body are co-blended and improved, and the modifying liquid is re-blended for improvement. The conductivity and transparency of the prepared gradient doped target material are coordinated, and the corrosion resistance and stability of the product are remarkable. DETAILED DESCRIPTION

[0015] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0016] A low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient-doped target material in this embodiment includes the following steps: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

[0017] The ultrasonic power of the ultrasonic treatment in this embodiment is 200-250W, and the ultrasonic treatment is performed for 1 hour. The sintering temperature of the sintering improvement treatment is 1050-1100° C., and the sintering is performed for 2 hours.

[0018] The preparation method of the ultrasonic liquid of the present embodiment is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

[0019] The mass fraction of the urea solution in this embodiment is 2-5%; the rotation speed of the mixing and ball milling treatment is 1500 r / min, and the ball milling is performed for 2 hours.

[0020] The preparation method of the modified liquid of this embodiment is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution which is 3-5 times the total amount of zinc oxide, and then titanium oxide which is 10-15% of the total amount of zinc oxide and a silane coupling agent which is 3-5% of the total amount of zinc oxide are added, and stirred evenly to obtain a modified solution.

[0021] The silane coupling agent in this embodiment is silane coupling agent KH550.

[0022] The carboxymethyl cellulose sodium solution of this embodiment is prepared by uniformly blending sodium carboxymethyl cellulose, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of (2-5):5:(1-2).

[0023] The mass fraction of the sodium silicate solution in this embodiment is 3-6%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

[0024] The present embodiment provides a silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by a low-temperature sintering preparation method of the silicon-aluminum-zirconium-tungsten gradient-doped target material.

[0025] Example 1. A low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient-doped target material in this embodiment includes the following steps: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

[0026] The ultrasonic power of the ultrasonic treatment in this embodiment is 200W, and the ultrasonic treatment is performed for 1 hour. The sintering temperature of the sintering improvement treatment is 1050° C., and the sintering is performed for 2 hours.

[0027] The preparation method of the ultrasonic liquid of the present embodiment is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

[0028] The mass fraction of the urea solution in this embodiment is 2%; the rotation speed of the mixing ball milling treatment is 1500 r / min, and the ball milling is performed for 2 hours.

[0029] The preparation method of the modified liquid of this embodiment is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution 3 times the total amount of zinc oxide, and then titanium oxide 10% of the total amount of zinc oxide and a silane coupling agent 3% of the total amount of zinc oxide are added and stirred evenly to obtain a modified solution.

[0030] The silane coupling agent in this embodiment is silane coupling agent KH550.

[0031] The carboxymethyl cellulose solution of this embodiment is prepared by uniformly blending sodium carboxymethyl cellulose, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of 2:5:1.

[0032] The mass fraction of the sodium silicate solution in this embodiment is 3%; the mass fraction of the dopamine hydrochloride solution is 2%.

[0033] The present embodiment provides a silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by a low-temperature sintering preparation method of the silicon-aluminum-zirconium-tungsten gradient-doped target material.

[0034] Example 2. A low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient-doped target material in this embodiment includes the following steps: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

[0035] The ultrasonic power of the ultrasonic treatment in this embodiment is 250W, and the ultrasonic treatment is performed for 1 hour. The sintering temperature of the sintering improvement treatment is 1100° C., and the sintering is performed for 2 hours.

[0036] The preparation method of the ultrasonic liquid of the present embodiment is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

[0037] The mass fraction of the urea solution in this embodiment is 5%; the rotation speed of the mixing ball milling treatment is 1500 r / min, and the ball milling is performed for 2 h.

[0038] The preparation method of the modified liquid of this embodiment is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution 5 times the total amount of zinc oxide, and then titanium oxide 15% of the total amount of zinc oxide and a silane coupling agent 5% of the total amount of zinc oxide are added and stirred evenly to obtain a modified solution.

[0039] The silane coupling agent in this embodiment is silane coupling agent KH550.

[0040] The carboxymethyl cellulose sodium solution of this embodiment is prepared by uniformly blending sodium carboxymethyl cellulose, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of 5:5:2.

[0041] The mass fraction of the sodium silicate solution in this embodiment is 6%; the mass fraction of the dopamine hydrochloride solution is %.

[0042] The present embodiment provides a silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by a low-temperature sintering preparation method of the silicon-aluminum-zirconium-tungsten gradient-doped target material.

[0043] Example 3. A low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient-doped target material in this embodiment includes the following steps: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

[0044] The ultrasonic power of the ultrasonic treatment in this embodiment is 225W, and the ultrasonic treatment is performed for 1 hour. The sintering temperature of the sintering improvement treatment is 1075° C., and the sintering is performed for 2 hours.

[0045] The preparation method of the ultrasonic liquid of the present embodiment is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

[0046] The mass fraction of the urea solution in this embodiment is 3.5%; the rotation speed of the mixing and ball milling treatment is 1500 r / min, and the ball milling is performed for 2 h.

[0047] The preparation method of the modified liquid of this embodiment is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution that is 4 times the total amount of zinc oxide, and then titanium oxide that is 12.5% of the total amount of zinc oxide and a silane coupling agent that is 4% of the total amount of zinc oxide are added and stirred evenly to obtain a modified solution.

[0048] The silane coupling agent in this embodiment is silane coupling agent KH550.

[0049] The carboxymethyl cellulose solution of this embodiment is prepared by uniformly blending sodium carboxymethyl cellulose, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of 3.5:5:1.5.

[0050] The mass fraction of the sodium silicate solution in this embodiment is 4.5%; the mass fraction of the dopamine hydrochloride solution is 3.5%.

[0051] The present embodiment provides a silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by a low-temperature sintering preparation method of the silicon-aluminum-zirconium-tungsten gradient-doped target material.

[0052] Comparative Example 1. The difference from Example 3 is that ultrasonic liquid treatment was not used.

[0053] Comparative Example 2. The difference from Example 3 is that no yttrium oxide is added to the ultrasonic liquid.

[0054] Comparative Example 3. The difference from Example 3 is that no modifying liquid is added to the ultrasonic liquid.

[0055] Comparative Example 4. The difference from Example 3 is that the carboxymethyl cellulose sodium solution in the modification solution is replaced by water.

[0056] Comparative Example 5. The difference from Example 3 is that titanium oxide and silane coupling agent are not added to the modified solution.

[0057] The product performance tests of Examples 1-3 and Comparative Examples 1-5 are as follows:

[0058] It can be seen from Examples 1-3 and Comparative Examples 1-5 that the product of Example 3 of the present invention has excellent conductivity, transparency and corrosion resistance stability; however, when ultrasonic liquid treatment is not used, the performance of the product deteriorates significantly. At the same time, no yttrium oxide body is added to the ultrasonic liquid, no modifying liquid is added to the ultrasonic liquid, the carboxymethyl cellulose sodium liquid in the modifying liquid is replaced by water, and titanium oxide and silane coupling agent are not added to the modifying liquid. The performance of the product tends to deteriorate to varying degrees. The ultrasonic liquid prepared by combining the modifying liquid obtained by the specific method of the present invention with the yttrium oxide body has the most significant performance effect.

[0059] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0060] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient doped target, characterized in that: The following steps are involved: Step 1: Clean the substrate to remove oil and impurities; Step 2: Using silicon, aluminum, and zirconium as the first target material and tungsten as the second target material, wherein the mass ratio of silicon, aluminum, zirconium, and tungsten is 55:5:35:5, sputtering treatment is performed to form a tungsten gradient target, the sputtering power is 100 W, and the sputtering time is 1 hour; Step 3: ultrasonically treating the tungsten gradient target in an ultrasonic liquid, and then completing the ultrasonic treatment to obtain a gradient target after ultrasonic treatment; Step 4: Finally, the gradient target material after ultrasonic treatment is sintered and improved, and the sintering is completed to obtain the gradient doped target material of the present invention.

2. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 1, characterized in that: The ultrasonic power of the ultrasonic treatment is 200-250W, and the ultrasonic treatment is performed for 1 hour; the sintering temperature of the sintering improvement treatment is 1050-1100° C., and the sintering is performed for 2 hours.

3. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 1, characterized in that: The preparation method of the ultrasonic liquid is: Yttrium oxide, nano-silica sol and urea solution are uniformly mixed in a weight ratio of 3:2:3 to obtain yttrium oxide body; yttrium oxide body and modified liquid are uniformly mixed in a weight ratio of 5:3 and ball milled to obtain ultrasonic liquid.

4. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 3, characterized in that: The mass fraction of the urea solution is 2-5%; the rotation speed of the mixing ball milling treatment is 1500 r / min, and the ball milling is performed for 2 hours.

5. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 3, characterized in that: The preparation method of the modified liquid is: Zinc oxide is first stirred thoroughly in a carboxymethyl cellulose solution which is 3-5 times the total amount of zinc oxide, and then titanium oxide which is 10-15% of the total amount of zinc oxide and a silane coupling agent which is 3-5% of the total amount of zinc oxide are added, and stirred evenly to obtain a modified solution.

6. The low-temperature sintering method for preparing a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 5, characterized in that: The silane coupling agent is silane coupling agent KH550.

7. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 5, characterized in that: The carboxymethyl cellulose sodium solution is prepared by uniformly blending carboxymethyl cellulose sodium, sodium silicate solution and dopamine hydrochloride solution in a weight ratio of (2-5):5:(1-2).

8. The low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient doped target according to claim 7, characterized in that: The mass fraction of the sodium silicate solution is 3-6%; the mass fraction of the dopamine hydrochloride solution is 2-5%.

9. A silicon-aluminum-zirconium-tungsten gradient-doped target material prepared by the low-temperature sintering preparation method of a silicon-aluminum-zirconium-tungsten gradient-doped target material as described in any one of claims 1 to 8.

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