A preparation method of a high-purity aluminum target

Abstract

The present invention discloses a preparation method of a high-purity aluminum target, which comprises the following steps: spraying and treating with a complex-adjusted chitosan solution of aluminum borate whiskers until the product of step two is completely wetted, and then ending; placing the product of step three at 310-320 °C for heat treatment for 10-20 minutes, and then treating in a salt bath agent for 10-20 minutes, and ending the treatment; finally, performing a heat temperature improvement treatment, and ending the treatment to obtain a high-purity aluminum target. The high-purity aluminum target of the present invention uses pure aluminum to be melted and cooled to form an aluminum ingot body, and then the activity of the product is optimized and activated by the heat treatment in step two, and then cooled at a constant temperature to make the product performance mild, so that the grain size, density and conductivity of the product are coordinately improved.

Description

Technical Field

[0001] The present invention relates to the technical field of aluminum target materials, and particularly relates to a preparation method of a high-purity aluminum target material. Background Art

[0002] Aluminum is widely used in the field of sputtering target materials and is currently mainly applied to TFT liquid crystal displays through sputtering coating technology. In sputtering coating technology, the performance of sputtering target materials is mainly reflected in the sputtering deposition efficiency, the utilization rate of sputtering target materials, the quality of sputtered thin films, and conductivity.

[0003] In the prior art, the aluminum target materials prepared have poor grain size and compactness, and it is difficult to improve the conductivity of the products, which limits the use efficiency of the products. Summary of the Invention

[0004] Aiming at the defects of the prior art, the purpose of the present invention is to provide a preparation method of a high-purity aluminum target material to solve the problems raised in the above background art.

[0005] The present invention adopts the following technical solutions to solve the technical problems:

[0006] The present invention provides a preparation method of a high-purity aluminum target material, including the following steps:

[0007] Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting. After complete melting, obtain high-purity aluminum, and then place it in a mold for shaping to obtain an aluminum ingot body;

[0008] Step 2: Heat-treat the aluminum ingot body at 130 - 140 °C for 10 - 20 min, and then cool it to 50 - 55 °C at a rate of 1 - 3 °C / min and keep it warm;

[0009] Step 3: Subsequently, spray and treat with a boric acid aluminum whisker complexed chitosan solution until the product of Step 2 is completely wetted, and then end;

[0010] Step 4: Heat-treat the product of Step 3 at 310 - 320 °C for 10 - 20 min, and then treat it in a salt bath agent for 10 - 20 min, and then end the treatment;

[0011] Step 5: Finally, perform heat-temperature improvement treatment, and after the treatment ends, obtain a high-purity aluminum target material.

[0012] The inventor of the present invention found that without using the boric acid aluminum whisker complexed chitosan solution treatment, without using the salt bath agent treatment, and without using the heat-temperature improvement treatment, the performance of the product deteriorates significantly. By using the three in combination, the performance of the product can achieve synergistic effects.

[0013] Preferably, the preparation method of the boric acid aluminum whisker complexed chitosan solution is as follows:

[0014] S01: Add 2-6 parts of 3% lanthanum nitrate solution and 1-3 parts of phosphate buffer solution to 10-15 parts of 6% chitosan aqueous solution, stir evenly, then add 1-2 parts of sodium alkyl sulfonate, stir well, and obtain chitosan adjustment solution;

[0015] S02: heat-treating the aluminum borate whisker at 110-120°C for 5-10 minutes, then cooling to 45°C at a rate of 1-3°C / min, then adding a ball milling solution of 10-15% of the total amount of the aluminum borate whisker, and performing ball milling modification treatment. After the treatment is completed, washing and drying are performed to obtain an aluminum borate whisker ball milling agent;

[0016] S03: Add the aluminum borate whisker ball mill into the chitosan adjustment solution at a weight ratio of 1:5, stir thoroughly, and obtain an aluminum borate whisker compounded chitosan solution.

[0017] Preferably, the ball milling speed of the ball milling modification treatment is 1000-1500 r / min, and the ball milling time is 1-2 h.

[0018] Preferably, the pH value of the phosphate buffer solution is 5.0-6.0.

[0019] Preferably, the preparation method of the ball milling liquid is:

[0020] Preheat the Re powder to 45-55°C, keep it warm, then add it to the sodium alginate aqueous solution at a weight ratio of 1:5, then add silane coupling agent KH560 (10-15% of the total Re powder) and sodium oxalate (2-5% of the total Re powder), stir evenly, and obtain a ball milling solution.

[0021] The inventors of the present invention also found that in the preparation of the aluminum borate whisker double-tuned chitosan solution, the chitosan regulating solution used a chitosan aqueous solution with a mass fraction of 6%, no lanthanum nitrate solution was added in the preparation of the chitosan regulating solution, the aluminum borate whisker double-tuned chitosan solution did not use aluminum borate whiskers to be sent to 115°C for heat treatment for 6 minutes and then cooled to 45°C at a rate of 2°C / min in the preparation of the aluminum borate whisker double-tuned chitosan solution, and the aluminum borate whisker double-tuned chitosan solution did not use ball milling liquid treatment. The preparation methods of the ball milling liquid are different, and the performance of the products all have a tendency to deteriorate. Only the aluminum borate whisker double-tuned chitosan solution prepared by the method of the present invention has the most significant performance effect of the product.

[0022] Preferably, the mass fraction of the sodium alginate aqueous solution is 5-8%.

[0023] Preferably, the preparation method of the salt bath agent is:

[0024] S11: adding potassium nitrate to the yttrium nitrate solution at a weight ratio of 1:5 and stirring evenly, then adding potassium chloride in an amount of 4-8% of the total amount of potassium nitrate and stirring thoroughly;

[0025] S12: Add sodium dodecyl sulfate solution into the product of S11 at a weight ratio of 1:5 and stir thoroughly to obtain a salt bath agent.

[0026] Preferably, the mass fraction of the sodium dodecyl sulfate solution is 10-15%.

[0027] Preferably, the specific operation steps of the thermal warming improvement treatment are:

[0028] S11: heat treating the product of step 4 at 400-420°C for 10-20 min, and first cooling to 210-220°C at a rate of 1-3°C / min;

[0029] S12: Then perform water cooling, reduce the temperature to 120°C at a rate of 20-25°C / min, and finally reduce the temperature to room temperature at a constant rate.

[0030] Preferably, the constant temperature in S12 is reduced to room temperature at a rate of 3-6°C / min.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] The high-purity aluminum target material of the invention adopts pure aluminum to be melted and cooled to form an aluminum ingot body, and then optimizes and activates the activity of the product through the heat treatment in step 2, and then cools at a constant temperature to make the product performance mild. At the same time, in step 3, the aluminum borate whisker compound chitosan liquid is sprayed, and the optimized and improved aluminum borate whisker is loaded on the surface of the product, which is convenient for improving the conductivity of subsequent products and improving the density of the product. Through the heat treatment in step 4 and then the salt bath treatment, the salt bath agent and the aluminum borate whisker compound chitosan liquid are coordinated and improved, and the performance of the product is coordinated and improved. Finally, the product is subjected to the thermal temperature improvement treatment, and the performance of the product is further improved, so that the grain size, density and conductivity of the product are coordinated and improved. DETAILED DESCRIPTION

[0033] 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 creative work are within the scope of protection of the present invention.

[0034] A method for preparing a high-purity aluminum target material in this embodiment includes the following steps:

[0035] Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting, obtain high-purity aluminum after complete melting, and then place it in a mold to form an aluminum ingot;

[0036] Step 2: Heat-treat the aluminum ingot body at 130 - 140 °C for 10 - 20 min, then cool it to 50 - 55 °C at a rate of 1 - 3 °C / min and keep it warm.

[0037] Step 3: Subsequently, spray-treat with the borate whisker complex-adjusted chitosan solution until the product in Step 2 is completely wetted, and then end.

[0038] Step 4: Heat-treat the product in Step 3 at 310 - 320 °C for 10 - 20 min, and then treat it in a salt bath agent for 10 - 20 min, and then end the treatment.

[0039] Step 5: Finally, perform heat-temperature improvement treatment, and then end the treatment to obtain a high-purity aluminum target.

[0040] The preparation method of the borate whisker complex-adjusted chitosan solution in this example is as follows:

[0041] S01: Add 2 - 6 parts of a 3% lanthanum nitrate solution and 1 - 3 parts of a phosphate buffer solution to 10 - 15 parts of a 6% chitosan aqueous solution by mass fraction. First, stir evenly, and then add 1 - 2 parts of sodium alkyl sulfonate and stir well to obtain a chitosan adjustment solution.

[0042] S02: Send the borate whiskers to be heat-treated at 110 - 120 °C for 5 - 10 min, then cool them to 45 °C at a rate of 1 - 3 °C / min. Subsequently, add 10 - 15% of the total amount of the borate whiskers of the ball-milling liquid and perform ball-milling modification treatment. After the treatment ends, wash with water and dry to obtain a borate whisker ball-milling agent.

[0043] S03: Add the borate whisker ball-milling agent to the chitosan adjustment solution according to a weight ratio of 1:5 and stir well to obtain a borate whisker complex-adjusted chitosan solution.

[0044] The ball-milling speed of the ball-milling modification treatment in this example is 1000 - 1500 r / min, and the ball-milling time is 1 - 2 h.

[0045] The pH value of the phosphate buffer solution in this example is 5.0 - 6.0.

[0046] The preparation method of the ball-milling liquid in this example is as follows:

[0047] Preheat the Re powder to 45 - 55 °C and keep it warm. Then, add it to the sodium alginate aqueous solution according to a weight ratio of 1:5. Then, add 10 - 15% of the total amount of the Re powder of the silane coupling agent KH560 and 2 - 5% of the total amount of the Re powder of sodium oxalate, and stir evenly to obtain a ball-milling liquid.

[0048] The mass fraction of the sodium alginate aqueous solution in this example is 5 - 8%.

[0049] The preparation method of the salt bath agent in this embodiment is as follows:

[0050] S11: Potassium nitrate is added to the yttrium nitrate solution according to a weight ratio of 1:5, stirred evenly first, and then 4-8% of potassium chloride based on the total amount of potassium nitrate is added and stirred thoroughly;

[0051] S12: The sodium dodecyl sulfate solution is added to the product of S11 according to a weight ratio of 1:5 and stirred thoroughly to obtain the salt bath agent.

[0052] The mass fraction of the sodium dodecyl sulfate solution in this embodiment is 10-15%.

[0053] The specific operation steps of the heat temperature improvement treatment in this embodiment are as follows:

[0054] S11: The product of step four is heat-treated at 400-420 °C for 10-20 min and cooled to 210-220 °C at a rate of 1-3 °C / min first;

[0055] S12: Then water cooling treatment is carried out, cooled to 120 °C at a rate of 20-25 °C / min, and finally cooled to room temperature at a constant temperature rate, and that's it.

[0056] In S12 of this embodiment, the constant temperature rate is cooled to room temperature at 3-6 °C / min.

[0057] Example 1.

[0058] The preparation method of a high-purity aluminum target in this embodiment includes the following steps:

[0059] Step 1: The high-purity aluminum ingot is remelted in a vacuum furnace, and after complete melting, high-purity aluminum is obtained, and then it is formed in a mold to obtain an aluminum ingot body;

[0060] Step 2: The aluminum ingot body is heat-treated at 130 °C for 10 min first, and then cooled to 50 °C at a rate of 1 °C / min and kept warm;

[0061] Step 3: Subsequently, it is sprayed with a boron aluminum whisker complexed chitosan solution until the product of step two is completely wetted, and then it ends;

[0062] Step 4: The product of step three is heat-treated at 310 °C for 10 min, and then treated in the salt bath agent for 10 min, and the treatment ends;

[0063] Step 5: Finally, heat temperature improvement treatment is carried out again, and after the treatment ends, a high-purity aluminum target is obtained.

[0064] The preparation method of the boron aluminum whisker complexed chitosan solution in this embodiment is as follows:

[0065] S01: Add 2 parts of 3% by mass lanthanum nitrate solution and 1 part of phosphate buffer solution to 10 parts of 6% by mass chitosan aqueous solution, stir evenly, then add 1 part of sodium alkyl sulfonate, stir thoroughly, and obtain chitosan adjustment solution;

[0066] S02: heat-treating the aluminum borate whisker at 110°C for 5 minutes, then cooling to 45°C at a rate of 1°C / min, then adding a ball milling solution of 10% of the total amount of the aluminum borate whisker, and performing ball milling modification treatment. After the treatment is completed, washing and drying are performed to obtain an aluminum borate whisker ball milling agent;

[0067] S03: Add the aluminum borate whisker ball mill into the chitosan adjustment solution at a weight ratio of 1:5, stir thoroughly, and obtain an aluminum borate whisker compounded chitosan solution.

[0068] The ball milling speed of the ball milling modification treatment in this embodiment is 1000 r / min, and the ball milling time is 1 h.

[0069] The pH value of the phosphate buffer solution in this example is 5.0.

[0070] The preparation method of the ball milling liquid of this embodiment is:

[0071] The Re powder was preheated to 45°C, kept warm, and then added to the sodium alginate aqueous solution at a weight ratio of 1:5. Then, 10% of the total amount of Re powder was added with silane coupling agent KH560 and 2% of the total amount of Re powder was added with sodium oxalate. The mixture was stirred evenly to obtain a ball milling solution.

[0072] The mass fraction of the sodium alginate aqueous solution in this embodiment is 5%.

[0073] The preparation method of the salt bath agent of the present embodiment is:

[0074] S11: adding potassium nitrate to the yttrium nitrate solution in a weight ratio of 1:5 and stirring evenly, then adding potassium chloride which is 4% of the total amount of potassium nitrate and stirring thoroughly;

[0075] S12: Add sodium dodecyl sulfate solution into the product of S11 at a weight ratio of 1:5 and stir thoroughly to obtain a salt bath agent.

[0076] The mass fraction of the sodium lauryl sulfate solution in this embodiment is 10%.

[0077] The specific operation steps of the thermal temperature improvement treatment of this embodiment are:

[0078] S11: heat treating the product of step 4 at 400°C for 10 min, and first cooling to 210°C at a rate of 1°C / min;

[0079] S12: Then perform water cooling, reduce the temperature to 120°C at a rate of 20°C / min, and finally reduce the temperature to room temperature at a constant rate.

[0080] In S12 of this embodiment, the constant temperature rate is reduced to room temperature at 3°C / min.

[0081] Example 2.

[0082] A method for preparing a high-purity aluminum target material in this embodiment includes the following steps:

[0083] Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting, obtain high-purity aluminum after complete melting, and then place it in a mold to form an aluminum ingot;

[0084] Step 2: heat-treat the aluminum ingot at 140°C for 20 minutes, then cool to 55°C at a rate of 3°C / min and keep warm;

[0085] Step 3: Then, the aluminum borate whisker-modified chitosan solution is sprayed until the product of step 2 is completely wetted;

[0086] Step 4: heat-treat the product of step 3 at 320°C for 20 minutes, and then treat it in a salt bath for 20 minutes, and then the treatment is completed;

[0087] Step 5: Finally, heat and warm the target to obtain a high-purity aluminum target.

[0088] The preparation method of the aluminum borate whisker multiplex chitosan solution of the present embodiment is:

[0089] S01: Add 6 parts of 3% by mass lanthanum nitrate solution and 3 parts of phosphate buffer solution to 15 parts of 6% by mass chitosan aqueous solution, stir evenly, then add 2 parts of sodium alkyl sulfonate, stir well, and obtain chitosan adjustment solution;

[0090] S02: heat-treating the aluminum borate whisker at 120°C for 10 minutes, then cooling to 45°C at a rate of 3°C / min, then adding a ball milling solution of 15% of the total amount of the aluminum borate whisker, and performing ball milling modification treatment. After the treatment is completed, washing and drying are performed to obtain an aluminum borate whisker ball milling agent;

[0091] S03: Add the aluminum borate whisker ball mill into the chitosan adjustment solution at a weight ratio of 1:5, stir thoroughly, and obtain an aluminum borate whisker compounded chitosan solution.

[0092] The ball milling speed of the ball milling modification treatment in this embodiment is 1500r / min, and the ball milling time is 2h.

[0093] The pH value of the phosphate buffer solution in this example is 6.0.

[0094] The preparation method of the ball milling liquid of this embodiment is:

[0095] The Re powder was preheated to 55°C, kept warm, and then added to the sodium alginate aqueous solution at a weight ratio of 1:5. Then, 15% of the total amount of Re powder was added with silane coupling agent KH560 and 5% of the total amount of Re powder was added with sodium oxalate. The mixture was stirred evenly to obtain a ball milling solution.

[0096] The mass fraction of the sodium alginate aqueous solution in this embodiment is 8%.

[0097] The preparation method of the salt bath agent of the present embodiment is:

[0098] S11: adding potassium nitrate to the yttrium nitrate solution in a weight ratio of 1:5 and stirring evenly, then adding potassium chloride which is 8% of the total amount of potassium nitrate and stirring thoroughly;

[0099] S12: Add sodium dodecyl sulfate solution into the product of S11 at a weight ratio of 1:5 and stir thoroughly to obtain a salt bath agent.

[0100] The mass fraction of the sodium lauryl sulfate solution in this embodiment is 15%.

[0101] The specific operation steps of the thermal temperature improvement treatment of this embodiment are:

[0102] S11: heat treating the product of step 4 at 420°C for 20 min, and first cooling to 220°C at a rate of 3°C / min;

[0103] S12: Then perform water cooling, reduce the temperature to 120°C at a rate of 25°C / min, and finally reduce the temperature to room temperature at a constant rate.

[0104] In S12 of this embodiment, the constant temperature rate is reduced to room temperature at 6°C / min.

[0105] Example 3.

[0106] A method for preparing a high-purity aluminum target material in this embodiment includes the following steps:

[0107] Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting, obtain high-purity aluminum after complete melting, and then place it in a mold to form an aluminum ingot;

[0108] Step 2: heat-treat the aluminum ingot at 135°C for 15 minutes, then cool to 52°C at a rate of 2°C / min and keep warm;

[0109] Step 3: Then, the aluminum borate whisker-modified chitosan solution is sprayed until the product of step 2 is completely wetted;

[0110] Step 4: Heat-treat the product of Step 3 at 315 °C for 15 min, then treat it in a salt bath agent for 15 min, and the treatment is completed.

[0111] Step 5: Finally, perform hot temperature improvement treatment, and after the treatment is completed, a high-purity aluminum target is obtained.

[0112] The preparation method of the aluminum borate whisker complex-adjusted chitosan solution in this example is as follows:

[0113] S01: Add 4 parts of lanthanum nitrate solution with a mass fraction of 3% and 2 parts of phosphate buffer solution to 12 parts of chitosan aqueous solution with a mass fraction of 6%. First, stir evenly, and then add 1.5 parts of sodium alkyl sulfonate and stir thoroughly to obtain a chitosan adjustment solution.

[0114] S02: Send the aluminum borate whiskers for heat treatment at 115 °C for 7.5 min, then cool to 45 °C at a rate of 2 °C / min. Subsequently, add 12% of the total amount of the ball milling liquid of the aluminum borate whiskers for ball milling modification treatment. After the treatment is completed, wash with water and dry to obtain the aluminum borate whisker ball milling agent.

[0115] S03: Add the aluminum borate whisker ball milling agent to the chitosan adjustment solution according to a weight ratio of 1:5 and stir thoroughly to obtain the aluminum borate whisker complex-adjusted chitosan solution.

[0116] The ball milling speed of the ball milling modification treatment in this example is 1250 r / min, and the ball milling time is 1.5 h.

[0117] The pH value of the phosphate buffer solution in this example is 5.5.

[0118] The preparation method of the ball milling liquid in this example is as follows:

[0119] Preheat the Re powder to 42 °C for heat preservation treatment, then add it to the sodium alginate aqueous solution according to a weight ratio of 1:5, and then add 12.5% of the total amount of the Re powder of the silane coupling agent KH560 and 3.5% of the total amount of the Re powder of sodium oxalate, and stir evenly to obtain the ball milling liquid.

[0120] The mass fraction of the sodium alginate aqueous solution in this example is 6.5%.

[0121] The preparation method of the salt bath agent in this example is as follows:

[0122] S11: Add potassium nitrate to the yttrium nitrate solution according to a weight ratio of 1:5, stir evenly first, and then add 6% of potassium chloride of the total amount of potassium nitrate and stir thoroughly;

[0123] S12: Add the sodium dodecyl sulfate solution to the product of S11 according to a weight ratio of 1:5 and stir thoroughly to obtain the salt bath agent.

[0124] The mass fraction of the sodium lauryl sulfate solution in this embodiment is 12.5%.

[0125] The specific operation steps of the thermal temperature improvement treatment of this embodiment are:

[0126] S11: heat treating the product of step 4 at 410°C for 15 min, and first cooling to 215°C at a rate of 2°C / min;

[0127] S12: Then perform water cooling, reduce the temperature to 120°C at a rate of 22°C / min, and finally reduce the temperature to room temperature at a constant rate.

[0128] In S12 of this embodiment, the constant temperature rate is reduced to room temperature at 4.5° C. / min.

[0129] Example 4.

[0130] A method for preparing a high-purity aluminum target material in this embodiment includes the following steps:

[0131] Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting, obtain high-purity aluminum after complete melting, and then place it in a mold to form an aluminum ingot;

[0132] Step 2: heat-treat the aluminum ingot at 132°C for 12 minutes, then cool to 2°C at a rate of 2°C / min and keep warm;

[0133] Step 3: Then, the aluminum borate whisker-modified chitosan solution is sprayed until the product of step 2 is completely wetted;

[0134] Step 4: heat-treat the product of step 3 at 312°C for 12 minutes, and then treat it in a salt bath for 15 minutes, and then the treatment is completed;

[0135] Step 5: Finally, heat and warm the target to obtain a high-purity aluminum target.

[0136] The preparation method of the aluminum borate whisker multiplex chitosan solution of the present embodiment is:

[0137] S01: Add 3 parts of 3% lanthanum nitrate solution and 2 parts of phosphate buffer solution to 12 parts of 6% chitosan aqueous solution, stir evenly, then add 1.2 parts of sodium alkyl sulfonate and stir thoroughly to obtain chitosan adjustment solution;

[0138] S02: heat-treating the aluminum borate whisker at 115°C for 6 minutes, then cooling to 45°C at a rate of 2°C / min, then adding a ball milling solution of 12% of the total amount of the aluminum borate whisker, and performing ball milling modification treatment. After the treatment is completed, washing and drying are performed to obtain an aluminum borate whisker ball milling agent;

[0139] S03: Add the aluminum borate whisker ball milling agent to the chitosan regulating solution at a weight ratio of 1:5, and stir well to obtain the aluminum borate whisker compounded chitosan solution.

[0140] In this example, the ball milling speed for the ball milling modification treatment is 1200 r / min, and the ball milling time is 1.2 h.

[0141] The pH value of the phosphate buffer solution in this example is 5.2.

[0142] The preparation method of the ball milling liquid in this example is as follows:

[0143] Preheat the Re powder to 42 °C and perform heat preservation treatment, then add it to the sodium alginate aqueous solution at a weight ratio of 1:5, and then add 12% of the silane coupling agent KH560 based on the total amount of Re powder and 3% of sodium oxalate based on the total amount of Re powder, and stir evenly to obtain the ball milling liquid.

[0144] The mass fraction of the sodium alginate aqueous solution in this example is 6%.

[0145] The preparation method of the salt bath agent in this example is as follows:

[0146] S11: Add potassium nitrate to the yttrium nitrate solution at a weight ratio of 1:5, stir evenly first, and then add 5% of potassium chloride based on the total amount of potassium nitrate, and stir well;

[0147] S12: Add the sodium dodecyl sulfate solution to the product of S11 at a weight ratio of 1:5 and stir well to obtain the salt bath agent.

[0148] The mass fraction of the sodium dodecyl sulfate solution in this example is 12%.

[0149] The specific operation steps of the thermal aging improvement treatment in this example are as follows:

[0150] S11: Heat-treat the product of step four at 410 °C for 12 min, and first cool it to 212 °C at a rate of 2 °C / min;

[0151] S12: Then perform water cooling treatment, cool it to 120 °C at a rate of 22 °C / min, and finally cool it to room temperature at a constant rate, and that's it.

[0152] In S12 of this example, the constant rate is cooled to room temperature at 4 °C / min.

[0153] Comparative Example 1.

[0154] The difference from Example 3 is that the treatment with the aluminum borate whisker compounded chitosan solution is not adopted.

[0155] Comparative Example 2.

[0156] Different from Example 3, in the preparation of the aluminum borate whisker complex-adjusted chitosan solution, the chitosan regulating solution uses a 6% by mass chitosan aqueous solution.

[0157] Comparative Example 3.

[0158] Different from Example 3, lanthanum nitrate solution was not added in the preparation of the chitosan regulating solution.

[0159] Comparative Example 4.

[0160] Different from Example 3, in the preparation of the aluminum borate whisker complex-adjusted chitosan solution, the aluminum borate whiskers were not sent for heat treatment at 115°C for 6 min and then cooled to 45°C at a rate of 2°C / min.

[0161] Comparative Example 5.

[0162] Different from Example 3, in the preparation of the aluminum borate whisker complex-adjusted chitosan solution, ball milling liquid treatment was not used.

[0163] Comparative Example 6

[0164] Different from Example 3, the preparation method of the ball milling liquid was different. Re powder was added to the sodium alginate aqueous solution at a weight ratio of 1:5, and then 12% of the total amount of Re powder of the silane coupling agent KH560 was added and stirred evenly to obtain the ball milling liquid.

[0165] Comparative Example 7

[0166] Different from Example 3, salt bath agent treatment was not used.

[0167] Comparative Example 8

[0168] Different from Example 3, heat temperature improvement treatment was not used.

[0169] The performance measurement results of Examples 1-4 and Comparative Examples 1-8 are as follows

[0170] <![CDATA[Resistivity (10 -2 Ω.cm)]]> <![CDATA[Density (g / cm 3 )]]> Grain size (nm) Example 1 1.6 5.95 0.3 Example 2 1.3 5.97 0.3 Example 3 1.2 5.98 0.2 Example 4 1.5 5.96 0.3 Comparative Example 1 7.8 4.12 0.8 Comparative Example 2 4.9 5.03 0.5 Comparative Example 3 4.0 5.14 0.4 Comparative Example 4 5.3 4.87 0.6 Comparative Example 5 6.9 4.54 0.6 Comparative Example 6 5.7 4.79 0.5 Comparative Example 7 7.1 4.65 0.7 Comparative Example 8 6.3 5.05 0.6

[0171] It can be obtained from Examples 1-4 and Comparative Examples 1-8 that the products of Example 3 of the present invention have excellent electrical conductivity, density and small grain size performance, and at the same time, the performance of the products can be coordinately improved;

[0172] Without using the aluminum borate whisker complex-adjusted chitosan solution treatment, without using the salt bath agent treatment, and without using the heat temperature improvement treatment, the performance of the products deteriorates significantly. By using the three in harmony, the performance of the products can achieve synergistic effects;

[0173] Meanwhile, it is found that in the preparation of the composite-adjusted chitosan solution with aluminum borate whiskers, the chitosan adjusting solution uses an aqueous chitosan solution with a mass fraction of 6%. No lanthanum nitrate solution is added during the preparation of the chitosan adjusting solution. During the preparation of the composite-adjusted chitosan solution with aluminum borate whiskers, the aluminum borate whiskers are not sent for heat treatment at 115°C for 6 minutes and then cooled to 45°C at a rate of 2°C / min. The composite-adjusted chitosan solution with aluminum borate whiskers is not treated with ball milling liquid. Different preparation methods of the ball milling liquid result in a deteriorating trend in the product performance. Only the composite-adjusted chitosan solution with aluminum borate whiskers prepared by the method of the present invention has the most significant product performance effect.

[0174] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and the present invention can be implemented in other specific forms without departing from the spirit or basic characteristics of the present invention. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be encompassed by the present invention.

[0175] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing a high-purity aluminum target, It is characterized in that The following steps are involved: Step 1: Place the high-purity aluminum ingot in a vacuum furnace for remelting, obtain high-purity aluminum after complete melting, and then place it in a mold to form an aluminum ingot; Step 2: Heat treat the aluminum ingot at 130-140°C for 10-20 minutes, then cool to 50-55°C at a rate of 1-3°C / min, and keep warm; Step 3: Then, the aluminum borate whisker-modified chitosan solution is sprayed until the product of step 2 is completely wetted; Step 4: heat-treat the product of step 3 at 310-320°C for 10-20 minutes, then treat in a salt bath for 10-20 minutes, and then the treatment is completed; Step 5: Finally, heat and improve the treatment, and the treatment is completed to obtain a high-purity aluminum target; The preparation method of the aluminum borate whisker multiplexed chitosan solution is: S01: Add 2-6 parts of 3% lanthanum nitrate solution and 1-3 parts of phosphate buffer solution to 10-15 parts of 6% chitosan aqueous solution, stir evenly, then add 1-2 parts of sodium alkyl sulfonate, stir well, and obtain chitosan adjustment solution; S02: heat-treating the aluminum borate whisker at 110-120°C for 5-10 minutes, then cooling to 45°C at a rate of 1-3°C / min, then adding a ball milling solution of 10-15% of the total amount of the aluminum borate whisker, and performing ball milling modification treatment. After the treatment is completed, washing and drying are performed to obtain an aluminum borate whisker ball milling agent; S03: adding the aluminum borate whisker ball mill into the chitosan adjustment solution at a weight ratio of 1:5, stirring sufficiently to obtain an aluminum borate whisker compounded chitosan solution; The specific operation steps of the thermal temperature improvement treatment are: S11: heat treating the product of step 4 at 400-420°C for 10-20 min, and first cooling to 210-220°C at a rate of 1-3°C / min; S12: Then water cooling is performed to reduce the temperature to 120°C at a rate of 20-25°C / min, and finally to room temperature at a constant temperature rate. The preparation method of the ball milling liquid is as follows: Preheat the Re powder to 45-55°C, keep it warm, then add it to the sodium alginate aqueous solution at a weight ratio of 1:5, then add silane coupling agent KH560 (10-15% of the total amount of Re powder) and sodium oxalate (2-5% of the total amount of Re powder), stir evenly, and obtain a ball milling solution.

2. The method for preparing a high-purity aluminum target according to claim 1, It is characterized in that The ball milling speed of the ball milling modification treatment is 1000-1500r / min, and the ball milling time is 1-2h.

3. The method for preparing a high-purity aluminum target according to claim 1, It is characterized in that The pH value of the phosphate buffer solution is 5.0-6.

0.

4. The method for preparing a high-purity aluminum target according to claim 1, It is characterized in that The mass fraction of the sodium alginate aqueous solution is 5-8%.

5. The method for preparing a high-purity aluminum target according to claim 1, It is characterized in that The preparation method of the salt bath agent is: S11: adding potassium nitrate to the yttrium nitrate solution in a weight ratio of 1:5 and stirring evenly, then adding potassium chloride in an amount of 4-8% of the total amount of potassium nitrate and stirring thoroughly; S12: Add sodium dodecyl sulfate solution into the product of S11 at a weight ratio of 1:5 and stir thoroughly to obtain a salt bath agent.

6. The method for preparing a high-purity aluminum target according to claim 5, It is characterized in that The mass fraction of the sodium dodecyl sulfate solution is 10-15%.

7. The method for preparing a high-purity aluminum target according to claim 1, It is characterized in that In the S12, the temperature is lowered to room temperature at a constant rate of 3-6°C / min.