A preparation method of a silver target with high density

Abstract

The present invention discloses a preparation method of a silver target with high density, which comprises the following steps: thermally improving the ball milling agent, and obtaining a thermally improved material after the treatment; subsequently, performing homogenizing, refining and denaturing treatment on the thermally improved material, and the silver target of the present invention can be obtained after the treatment. The silver target of the present invention uses a modified regulator to perform ball milling modification to obtain a ball milling agent, and then cooperates with thermal improvement treatment, and finally performs homogenizing, refining and denaturing treatment to obtain a target material. The modified regulator is prepared by wollastonite in cooperation with a chitosan aqueous solution and adjusted by yttrium nitrate and carboxymethyl cellulose. Through the optimization of wollastonite, the silver raw material is ball milled and adjusted to improve the density of the raw material product.

Description

Technical Field

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

[0002] Target materials are basic consumables in the magnetron sputtering process. They not only have a large usage amount, but also the quality of the target materials plays a crucial decisive role in the performance of the thin film. Target materials are widely used in various fields, mainly including optical target materials, target materials for display thin films, target materials for the semiconductor field, target materials for recording media, superconducting target materials, etc. Among them, target materials for the semiconductor field, target materials for display, and target materials for recording media are the three most widely used target materials at present.

[0003] In the prior art, the density performance of the prepared target materials is poor, the wear resistance is poor, it is difficult to coordinately improve the density and wear resistance, and the performance stability of the product is low under acid corrosion conditions, which limits the use efficiency of the product. 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 silver target material with high density to solve the problems raised in the above background art.

[0005] The present invention solves the technical problems by adopting the following technical solutions:

[0006] The present invention provides a preparation method of a silver target material with high density, including the following steps:

[0007] Step 1: Add 10 - 15 parts of wollastonite to 35 - 45 parts of a chitosan aqueous solution with a mass fraction of 6%, then add 3 - 5 parts of carboxymethyl cellulose and 1 - 5 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator;

[0008] Step 2: Add the modified regulator accounting for 10 - 15% of the total amount of the silver raw material to the silver raw material, and then perform ball milling modification treatment. The rotation speed of the ball milling modification is 1000 - 1500 r / min, and the ball milling time is 1 - 2 h. After the ball milling is completed, wash with water and dry to obtain a ball milling agent;

[0009] Step 3: Perform heat improvement treatment on the ball milling agent, and after the treatment is completed, obtain a heat-improved material;

[0010] Step 4: Subsequently, perform uniform refinement and denaturation treatment on the heat-improved material, and after the treatment is completed, the silver target material of the present invention can be obtained.

[0011] Preferably, the mass fraction of the yttrium nitrate solution is 5 - 9%.

[0012] Preferably, the specific operation steps of the heat improvement treatment are as follows:

[0013] S01: Feed the ball milling agent and heat-treat it at 140 - 150 °C for 1 - 2 h; then heat it up to 210 - 220 °C at a rate of 1 - 3 °C / min;

[0014] S02: Then cool the product of S01 to 45 - 50 °C at a rate of 3 - 5 °C / min, keep it warm for standby;

[0015] S03: Immerse the product of S02 in the salt bath agent for salt bath improvement treatment, and after the treatment is completed, wash it with water and dry it.

[0016] Preferably, the salt bath agent is prepared from a lanthanum chloride solution with a mass fraction of 5 - 7% and a sodium dodecyl sulfate solution in a weight ratio of 2:5.

[0017] Preferably, the mass fraction of the sodium dodecyl sulfate solution is 10 - 15%.

[0018] Preferably, the method of the salt bath improvement treatment is: perform ionization treatment at a current density of 110 - 115 A / dm 2 and a voltage of 210 - 215 V for 2 - 5 min.

[0019] Preferably, the specific operation steps of the uniform refinement and modification treatment are as follows:

[0020] S11: Add 2 - 5 parts of aluminum borate whiskers to 15 - 20 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 1 - 4 parts of an aqueous sodium alginate solution and 2 - 5 parts of a silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent;

[0021] S12: Heat-treat the heat-improved material at 210 - 230 °C for 10 - 20 min, then cool it to 45 °C at a rate of 1 - 3 °C / min, and perform infiltration treatment by spraying the aluminum borate whisker agent, and the treatment is completed;

[0022] S13: Place the product of S12 under hot pressing conditions for treatment, and after the treatment is completed, wash it with water and dry it.

[0023] Preferably, the mass fraction of the aqueous sodium alginate solution is 8 - 12%.

[0024] Preferably, the hot pressing conditions are treatment at 10 - 15 Mpa and 85 - 95 °C for 40 - 50 min.

[0025] Preferably, the infiltration treatment by spraying the aluminum borate whisker agent is to infiltrate the surface of the heat-improved material cooled to 45 °C with the aluminum borate whisker agent until complete infiltration.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] The silver target material of the present invention is subjected to ball milling modification with a modified regulator to obtain a ball milling agent, and then combined with heat improvement treatment, and finally subjected to uniform refinement and denaturation treatment to obtain a target material. The modified regulator is prepared by combining wollastonite with an aqueous chitosan solution and adjusting with yttrium nitrate and carboxymethyl cellulose. Through the optimization of wollastonite, the silver raw material is ball milled to improve the density of the raw material product. At the same time, through heat improvement treatment, the density of the product is further improved. Combined with uniform refinement and denaturation treatment, the heat-improved material is heat-treated at 210-230 °C for 10-20 min, and then cooled to 45 °C at a rate of 1-3 °C / min, and infiltrated with a borate whisker agent. The borate whisker is used to adjust and improve the product, so that the wear resistance of the product is improved. The optimized product can achieve coordinated improvement of wear resistance and density, and at the same time, the acid corrosion resistance of the product is further improved. Specific Embodiments

[0028] 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 a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative work shall fall within the protection scope of the present invention.

[0029] A method for preparing a silver target material with high density in this embodiment includes the following steps:

[0030] Step 1: Add 10-15 parts of wollastonite to 35-45 parts of an aqueous chitosan solution with a mass fraction of 6%, then add 3-5 parts of carboxymethyl cellulose and 1-5 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator.

[0031] Step 2: Add the modified regulator accounting for 10-15% of the total amount of the silver raw material to the silver raw material, and then perform ball milling modification. The rotation speed of the ball milling modification is 1000-1500 r / min, and the ball milling time is 1-2 h. After the ball milling is completed, wash with water and dry to obtain a ball milling agent.

[0032] Step 3: Perform heat improvement treatment on the ball milling agent, and obtain a heat-improved material after the treatment.

[0033] Step 4: Subsequently, perform uniform refinement and denaturation treatment on the heat-improved material, and the silver target material of the present invention can be obtained after the treatment.

[0034] The mass fraction of the yttrium nitrate solution in this embodiment is 5-9%.

[0035] The specific operation steps of the heat improvement treatment in this embodiment are as follows:

[0036] S01: Feed the ball milling agent and heat-treat it at 140 - 150 °C for 1 - 2 h; then heat it up to 210 - 220 °C at a rate of 1 - 3 °C / min;

[0037] S02: Then cool the product of S01 to 45 - 50 °C at a rate of 3 - 5 °C / min, keep it warm for standby;

[0038] S03: Immerse the product of S02 into the salt bath agent for salt bath improvement treatment, after the treatment, wash it with water and dry it.

[0039] The salt bath agent in this example is prepared from a lanthanum chloride solution with a mass fraction of 5 - 7% and a sodium dodecyl sulfate solution according to a weight ratio of 2:5.

[0040] The mass fraction of the sodium dodecyl sulfate solution in this example is 10 - 15%.

[0041] The method of salt bath improvement treatment in this example is: the salt bath improvement treatment is carried out at a current density of 110 - 115 A / dm 2 and a voltage of 210 - 215 V for ionization treatment for 2 - 5 min.

[0042] The specific operation steps of the uniform refinement and modification treatment in this example are as follows:

[0043] S11: Add 2 - 5 parts of aluminum borate whiskers to 15 - 20 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 1 - 4 parts of an aqueous sodium alginate solution and 2 - 5 parts of a silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent;

[0044] S02: Place the heat-improved material at 210 - 230 °C for heat treatment for 10 - 20 min, then cool it to 45 °C at a rate of 1 - 3 °C / min, and carry out infiltration treatment by spraying the aluminum borate whisker agent, and the treatment is completed;

[0045] S03: Place the product of S02 under hot pressing conditions for treatment, after the treatment, wash it with water and dry it, then it is ready.

[0046] The mass fraction of the aqueous sodium alginate solution in this example is 8 - 12%.

[0047] The hot pressing conditions in this example are treatment at 10 - 15 Mpa and 85 - 95 °C for 40 - 50 min.

[0048] The infiltration treatment by spraying the aluminum borate whisker agent in this example is to infiltrate the surface of the heat-improved material cooled to 45 °C with the aluminum borate whisker agent until complete infiltration.

[0049] Example 1.

[0050] The preparation method of a high-density silver target in this example includes the following steps:

[0051] Step 1: Add 10 parts of wollastonite into 35 parts of chitosan aqueous solution with a mass fraction of 6%, then add 3 parts of carboxymethyl cellulose and 1 part of yttrium nitrate solution, and stir evenly to obtain a modified regulator.

[0052] Step 2: Add 10% of the modified regulator in the total amount of silver raw materials to the silver raw materials, and then perform ball milling modification treatment. The rotation speed of ball milling modification is 1000 r / min, and the ball milling time is 1 h. After ball milling, wash with water and dry to obtain a ball milling agent.

[0053] Step 3: Perform heat improvement treatment on the ball milling agent, and after the treatment, obtain a heat-improved material.

[0054] Step 4: Subsequently, perform uniform refinement and denaturation treatment on the heat-improved material. After the treatment, the silver target of the present invention can be obtained.

[0055] The mass fraction of the yttrium nitrate solution in this example is 5%.

[0056] The specific operation steps of the heat improvement treatment in this example are as follows:

[0057] S01: Feed the ball milling agent into a heat treatment at 140 °C for 1 h; then heat it up to 210 °C at a rate of 1 °C / min.

[0058] S02: Then cool the product of S01 to 45 °C at a rate of 3 °C / min and keep it warm for standby.

[0059] S03: Immerse the product of S02 in a salt bath agent for salt bath improvement treatment. After the treatment, wash with water and dry.

[0060] The salt bath agent in this example is prepared from a lanthanum chloride solution with a mass fraction of 5% and a sodium dodecyl sulfate solution in a weight ratio of 2:5.

[0061] The mass fraction of the sodium dodecyl sulfate solution in this example is 10%.

[0062] The method of salt bath improvement treatment in this example is: The salt bath improvement treatment is carried out with a current density of 110 A / dm 2 and a voltage of 210 V for ionization treatment for 2 min.

[0063] The specific operation steps of the uniform refinement and denaturation treatment in this example are as follows:

[0064] S11: Add 2 parts of aluminum borate whiskers into 15 parts of hydrochloric acid solution with a mass fraction of 2%, then add 1 part of sodium alginate aqueous solution and 2 parts of silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent.

[0065] S02: Place the heat-improved feedstock in a heat treatment at 210 °C for 10 min, then cool it to 45 °C at a rate of 1 °C / min, and perform a dipping treatment with an aluminum borate whisker agent. The treatment is completed.

[0066] S03: Place the product of S02 under hot pressing conditions for treatment. After the treatment is completed, wash it with water and dry it to obtain the product.

[0067] In this example, the mass fraction of the sodium alginate aqueous solution is 8%.

[0068] The hot pressing conditions in this example are treatment at 10 Mpa and 85 °C for 40 min.

[0069] In this example, the dipping treatment with the aluminum borate whisker agent is to dip the surface of the heat-improved feedstock cooled to 45 °C with the aluminum borate whisker agent until complete dipping.

[0070] Example 2.

[0071] A preparation method of a high-density silver target in this example includes the following steps:

[0072] Step 1: Add 15 parts of wollastonite to 45 parts of a chitosan aqueous solution with a mass fraction of 6%, then add 5 parts of carboxymethyl cellulose and 5 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator.

[0073] Step 2: Add 15% of the modified regulator based on the total amount of the silver raw material to the silver raw material, and then perform ball milling modification treatment. The rotation speed of the ball milling modification is 1500 r / min, and the ball milling time is 2 h. After the ball milling is completed, wash it with water and dry it to obtain a ball milling agent.

[0074] Step 3: Perform heat improvement treatment on the ball milling agent. After the treatment is completed, obtain a heat-improved feedstock.

[0075] Step 4: Subsequently, perform uniform refinement and denaturation treatment on the heat-improved feedstock. After the treatment is completed, the silver target of the present invention can be obtained.

[0076] In this example, the mass fraction of the yttrium nitrate solution is 9%.

[0077] The specific operation steps of the heat improvement treatment in this example are as follows:

[0078] S01: Feed the ball milling agent into a heat treatment at 150 °C for 2 h; then heat it to 220 °C at a rate of 3 °C / min.

[0079] S02: Then cool the product of S01 to 50 °C at a rate of 5 °C / min and keep it warm for standby.

[0080] S03: Immerse the product of S02 in a salt bath agent for salt bath improvement treatment. After the treatment is completed, wash it with water and dry it.

[0081] The salt bath agent in this embodiment is prepared by mixing a lanthanum chloride solution with a mass fraction of 7% and a sodium dodecyl sulfate solution in a weight ratio of 2:5.

[0082] The mass fraction of the sodium dodecyl sulfate solution in this embodiment is 15%.

[0083] The method for improving the salt bath treatment in this embodiment is: the salt bath improvement treatment is carried out at a current density of 115 A / dm 2 and a voltage of 215 V for ionization treatment for 5 minutes.

[0084] The specific operation steps of the homogenization refinement and denaturation treatment in this embodiment are as follows:

[0085] S11: Add 5 parts of aluminum borate whiskers to 20 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 4 parts of sodium alginate aqueous solution and 5 parts of silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent;

[0086] S02: Place the heat-improved material at 230 °C for heat treatment for 20 minutes, then cool it to 45 °C at a rate of 3 °C / min, and spray and infiltrate it with the aluminum borate whisker agent to complete the treatment;

[0087] S03: Place the product of S02 under hot pressing conditions for treatment, wash with water and dry after the treatment to obtain the finished product.

[0088] The mass fraction of the sodium alginate aqueous solution in this embodiment is 12%.

[0089] The hot pressing conditions in this embodiment are treatment at 15 Mpa and 95 °C for 50 minutes.

[0090] The spraying and infiltration treatment with the aluminum borate whisker agent in this embodiment is to infiltrate the surface of the heat-improved material cooled to 45 °C with the aluminum borate whisker agent until complete infiltration.

[0091] Example 3.

[0092] A method for preparing a high-density silver target in this embodiment includes the following steps:

[0093] Step 1: Add 12.5 parts of wollastonite to 40 parts of a chitosan aqueous solution with a mass fraction of 6%, then add 4 parts of carboxymethyl cellulose and 2.5 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator;

[0094] Step 2: Add the modified regulator accounting for 12.5% of the total amount of the silver raw material to the silver raw material, then carry out ball milling and modification treatment. The rotation speed of the ball milling and modification is 1250 r / min, and the ball milling time is 1.5 h. After the ball milling is completed, wash with water and dry to obtain a ball milling agent;

[0095] Step 3: Carry out heat improvement treatment on the ball milling agent. After the treatment is completed, obtain a heat-improved material;

[0096] Step 4: Subsequently, perform homogenization, refinement, and denaturation treatment on the heat-improved feedstock. After the treatment is completed, the silver target material of the present invention can be obtained.

[0097] In this embodiment, the mass fraction of the yttrium nitrate solution is 7%.

[0098] The specific operation steps of the heat improvement treatment in this embodiment are as follows:

[0099] S01: Feed the ball milling agent into a heat treatment at 145°C for 1.5 h; then raise the temperature to 2150°C at a rate of 2°C / min.

[0100] S02: Then cool the product of S01 to 47°C at a rate of 4°C / min, keep it warm, and set it aside for use.

[0101] S03: Immerse the product of S02 in a salt bath agent for salt bath improvement treatment. After the treatment is completed, wash it with water and dry it.

[0102] In this embodiment, the salt bath agent is prepared from a lanthanum chloride solution with a mass fraction of 6% and a sodium dodecyl sulfate solution according to a weight ratio of 2:5.

[0103] In this embodiment, the mass fraction of the sodium dodecyl sulfate solution is 12.5%.

[0104] The method of the salt bath improvement treatment in this embodiment is: the salt bath improvement treatment is carried out with a current density of 112 A / dm 2 and a voltage of 212 V for ionization treatment for 3.5 min.

[0105] The specific operation steps of the homogenization, refinement, and denaturation treatment in this embodiment are as follows:

[0106] S11: Add 3.5 parts of aluminum borate whiskers to 17.5 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 2.5 parts of an aqueous sodium alginate solution and 3.5 parts of a silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent.

[0107] S02: Place the heat-improved feedstock in a heat treatment at 220°C for 15 min, then cool it to 45°C at a rate of 2°C / min, and perform infiltration treatment by spraying the aluminum borate whisker agent. After the treatment is completed.

[0108] S03: Place the product of S02 under hot pressing conditions for treatment. After the treatment is completed, wash it with water and dry it.

[0109] In this embodiment, the mass fraction of the aqueous sodium alginate solution is 10%.

[0110] In this embodiment, the hot pressing conditions are treatment at 12.5 Mpa and 90°C for 45 min.

[0111] In this embodiment, the spraying and infiltration treatment of the aluminum borate whisker agent is to infiltrate the surface of the hot improved material cooled to 45 °C with the aluminum borate whisker agent until complete infiltration.

[0112] Example 4.

[0113] A preparation method of a high-density silver target in this embodiment includes the following steps:

[0114] Step 1: Add 12 parts of wollastonite to 38 parts of a 6% chitosan aqueous solution by mass, then add 4 parts of carboxymethyl cellulose and 2 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator;

[0115] Step 2: Add the modified regulator accounting for 12% of the total amount of the silver raw material to the silver raw material, and then perform ball milling and modification treatment. The rotation speed of the ball milling and modification is 1220 r / min, and the ball milling time is 1.2 h. After the ball milling is completed, wash with water and dry to obtain a ball milling agent;

[0116] Step 3: Perform hot improvement treatment on the ball milling agent, and after the treatment is completed, obtain a hot improved material;

[0117] Step 4: Subsequently, perform uniform refinement and denaturation treatment on the hot improved material, and after the treatment is completed, the silver target of the present invention can be obtained.

[0118] The mass fraction of the yttrium nitrate solution in this embodiment is 6%.

[0119] The specific operation steps of the hot improvement treatment in this embodiment are as follows:

[0120] S01: Feed the ball milling agent into a heat treatment at 142 °C for 1.2 h; then raise the temperature to 212 °C at a rate of 2 °C / min;

[0121] S02: Then cool the product of S01 to 46 °C at a rate of 4 °C / min, keep warm, and reserve for use;

[0122] S03: Immerse the product of S02 in a salt bath agent for salt bath improvement treatment, and after the treatment is completed, wash with water and dry.

[0123] The salt bath agent in this embodiment is prepared from a 6% lanthanum chloride solution and a sodium dodecyl sulfate solution in a weight ratio of 2:5.

[0124] The mass fraction of the sodium dodecyl sulfate solution in this embodiment is 12%.

[0125] The method of the salt bath improvement treatment in this embodiment is: the salt bath improvement treatment is carried out with a current density of 112 A / dm 2 and a voltage of 212 V for ionization treatment for 3 min.

[0126] The specific operation steps of the uniform refinement and denaturation treatment in this embodiment are as follows:

[0127] S11: Add 3 parts of aluminum borate whiskers into 18 parts of hydrochloric acid solution with a mass fraction of 2%, then add 2 parts of sodium alginate aqueous solution and 3 parts of silane coupling agent KH560, and stir evenly to obtain the aluminum borate whisker agent;

[0128] S02: Place the heat-improved material for heat treatment at 212 °C for 14 min, then cool it to 45 °C at a rate of 2 °C / min, and spray and infiltrate it with the aluminum borate whisker agent to complete the treatment;

[0129] S03: Place the product of S02 under hot pressing conditions for treatment, wash and dry after the treatment to obtain the product.

[0130] The mass fraction of the sodium alginate aqueous solution in this example is 9%.

[0131] The hot pressing conditions in this example are treatment at 12 Mpa and 86 °C for 42 min.

[0132] The spraying and infiltration treatment of the aluminum borate whisker agent in this example is to infiltrate the surface of the heat-improved material cooled to 45 °C with the aluminum borate whisker agent until complete infiltration.

[0133] Example 5.

[0134] A preparation method of a high-density silver target in this example includes the following steps:

[0135] Step 1: Add 14 parts of wollastonite into 42 parts of chitosan aqueous solution with a mass fraction of 6%, then add 4 parts of carboxymethyl cellulose and 4 parts of yttrium nitrate solution, and stir evenly to obtain the modified regulator;

[0136] Step 2: Add the modified regulator accounting for 14% of the total amount of the silver raw material into the silver raw material, then perform ball milling and modification treatment. The rotation speed of the ball milling and modification is 1400 r / min, and the ball milling time is 1.8 h. After the ball milling is completed, wash and dry to obtain the ball milling agent;

[0137] Step 3: Perform heat improvement treatment on the ball milling agent, and obtain the heat-improved material after the treatment;

[0138] Step 4: Then perform uniform refinement and denaturation treatment on the heat-improved material, and the silver target of the present invention can be obtained after the treatment.

[0139] The mass fraction of the yttrium nitrate solution in this example is 8%.

[0140] The specific operation steps of the heat improvement treatment in this example are:

[0141] S01: Feed the ball milling agent into a heat treatment at 148 °C for 1.8 h; then heat it to 218 °C at a rate of 2 °C / min;

[0142] S02: Then cool the product of S01 to 48°C at a rate of 4°C / min, hold the temperature, and reserve for use.

[0143] S03: Immerse the product of S02 in the molten salt agent for molten salt improvement treatment. After the treatment is completed, wash with water and dry.

[0144] The molten salt agent in this example is prepared from a lanthanum chloride solution with a mass fraction of 6% and a sodium dodecyl sulfate solution according to a weight ratio of 2:5.

[0145] The mass fraction of the sodium dodecyl sulfate solution in this example is 14%.

[0146] The method of the molten salt improvement treatment in this example is: the molten salt improvement treatment is carried out with a current density of 114 A / dm 2 and a voltage of 214 V for ionization treatment for 4 minutes.

[0147] The specific operation steps of the uniform refinement and denaturation treatment in this example are as follows:

[0148] S11: Add 4 parts of aluminum borate whiskers to 18 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 3 parts of an aqueous sodium alginate solution and 4 parts of a silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent.

[0149] S02: Place the heat-improved material at 228°C for heat treatment for 18 minutes, then cool it to 45°C at a rate of 2°C / min, and carry out infiltration treatment with the aluminum borate whisker agent. After the treatment is completed.

[0150] S03: Place the product of S02 under hot pressing conditions for treatment. After the treatment is completed, wash with water and dry.

[0151] The mass fraction of the aqueous sodium alginate solution in this example is 11%.

[0152] The hot pressing conditions in this example are treatment at 14 Mpa and 92°C for 48 minutes.

[0153] The infiltration treatment with the aluminum borate whisker agent in this example is to infiltrate the surface of the heat-improved material cooled to 45°C with the aluminum borate whisker agent until complete infiltration.

[0154] Comparative Example 1.

[0155] The difference from Example 3 is that the modified regulator treatment is not adopted.

[0156] Comparative Example 2.

[0157] The difference from Example 3 is that the yttrium nitrate solution is not added in the preparation of the modified regulator.

[0158] Comparative Example 3.

[0159] Different from Example 3, wollastonite was not added in the preparation of the modification regulator.

[0160] Comparative Example 4.

[0161] Different from Example 3, thermal improvement treatment was not adopted.

[0162] Comparative Example 5.

[0163] Different from Example 3, salt bath improvement treatment was not adopted in the thermal improvement treatment.

[0164] Comparative Example 6.

[0165] Different from Example 3, the S02 step treatment was not adopted in the thermal improvement treatment.

[0166] Comparative Example 7.

[0167] Different from Example 3, homogeneous refinement modification treatment was not adopted.

[0168] Comparative Example 8.

[0169] Different from Example 3, the specific conditions of the homogeneous refinement modification treatment were different:

[0170] S01: Heat-treat the thermally improved material at 228 °C for 18 min, and then cool it to room temperature at a rate of 2 °C / min;

[0171] S02: Place the product of S01 under hot pressing conditions for treatment, wash with water and dry after the treatment to obtain the product.

[0172] The hot pressing conditions in this example were treatment at 14 Mpa and 92 °C for 48 min.

[0173] Use a friction and wear testing machine to evaluate the wear resistance of each product. The load is 5 N, the friction pair is a GCr15 steel ball with a diameter of 5 mm, the friction frequency is 6 Hz, the friction stroke is 2 mm, the friction time is 30 min, and use an electronic balance to weigh the mass before and after wear to calculate the wear amount.

[0174] The performance measurement results of Examples 1-5 and Comparative Examples 1-8 are as follows

[0175]

[0176]

[0177] It can be obtained from Examples 1-5 and Comparative Examples 1-8 that the products of Example 3 of the present invention have excellent wear resistance and density performance, and the two can achieve coordinated improvement;

[0178] Without being treated with a modification regulator, without undergoing heat improvement treatment, and without undergoing uniform refinement and modification treatment, the performance of the product shows an obvious trend of deterioration. By combining the three and achieving synergistic effects, the performance effect of the product is the most significant.

[0179] In the preparation of the modification regulator, yttrium nitrate solution is not added, and wollastonite is not added. In the heat improvement treatment, salt bath improvement treatment is not adopted, and the S02 step treatment is not adopted. The specific conditions of the uniform refinement and modification treatment are different.

[0180] The performance of the product shows a trend of deterioration. Only by adopting the method and process of the present invention, the performance effect of the product is the most significant. The effects of using other substitutes are not as obvious as that of the present invention.

[0181] Place the test product under the condition of 2% hydrochloric acid mist for 12 h and then test its performance effect.

[0182]

[0183]

[0184] From the acid and corrosion resistance performance, it can be seen that under acid and corrosion conditions, the performance of the product deteriorates significantly. Only the product prepared by the method of the present invention has the most obvious stability in performance under acid and corrosion conditions.

[0185] 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 included in the present invention.

[0186] 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 preparation method of a silver target with high density, characterized in that, it includes the following steps: Step 1: Add 10 - 15 parts of wollastonite into 35 - 45 parts of an aqueous chitosan solution with a mass fraction of 6%, then add 3 - 5 parts of carboxymethyl cellulose and 1 - 5 parts of yttrium nitrate solution, and stir evenly to obtain a modified regulator; Step 2: Add the modified regulator accounting for 10 - 15% of the total amount of silver raw materials to the silver raw materials, then perform ball - milling modification treatment. The rotation speed of ball - milling modification is 1000 - 1500 r / min, and the ball - milling time is 1 - 2 h. After ball - milling ends, wash with water and dry to obtain a ball - milling agent; Step 3: Perform heat improvement treatment on the ball - milling agent. After the treatment ends, obtain a heat - improved material; Step 4: Subsequently, perform uniform refinement and denaturation treatment on the heat - improved material. After the treatment ends, the silver target can be obtained; The specific operation steps of the heat improvement treatment are: S01: Feed the ball - milling agent into a heat treatment at 140 - 150 °C for 1 - 2 h; then heat up to 210 - 220 °C at a rate of 1 - 3 °C / min; S02: Then cool the product of S01 to 45 - 50 °C at a rate of 3 - 5 °C / min, keep warm, and reserve; S03: Immerse the product of S02 in a salt bath agent for salt bath improvement treatment. After the treatment ends, wash with water and dry; The specific operation steps of the uniform refinement and denaturation treatment are: S11: Add 2 - 5 parts of aluminum borate whiskers into 15 - 20 parts of a hydrochloric acid solution with a mass fraction of 2%, then add 1 - 4 parts of an aqueous sodium alginate solution and 2 - 5 parts of silane coupling agent KH560, and stir evenly to obtain an aluminum borate whisker agent; S12: Place the heat - improved material at 210 - 230 °C for heat treatment for 10 - 20 min, then cool to 45 °C at a rate of 1 - 3 °C / min, and perform infiltration treatment by spraying the aluminum borate whisker agent. After the treatment ends; S13: Place the product of S12 under hot - pressing conditions for treatment. After the treatment ends, wash with water and dry. The method of the salt bath improvement treatment is: The salt bath improvement treatment is carried out with an ionization treatment at a current density of 110 - 115 A / dm and a voltage of 210 - 215 V for 2 - 5 min.

2. The preparation method of a silver target with high density according to claim 1, characterized in that, the mass fraction of the yttrium nitrate solution is 5 - 9%.

3. The preparation method of a silver target with high density according to claim 1, characterized in that, the salt bath agent is prepared from a lanthanum chloride solution with a mass fraction of 5 - 7% and a sodium dodecyl sulfate solution according to a weight ratio of 2:

5.

4. The preparation method of a silver target with high density according to claim 3, characterized in that, the mass fraction of the sodium dodecyl sulfate solution is 10 - 15%.

5. The preparation method of a silver target with high density according to claim 1, characterized in that, the mass fraction of the aqueous sodium alginate solution is 8 - 12%.

6. The preparation method of a silver target with high density according to claim 1, characterized in that, the hot - pressing conditions are treatment at 10 - 15 Mpa and 85 - 95 °C for 40 - 50 min.

7. A method for preparing a silver target with high density according to claim 1, characterized in that, in the spray treatment of aluminum borate whisker agent infiltration, the surface of the hot improved material cooled to 45°C by the aluminum borate whisker agent infiltration is infiltrated until complete.

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