A method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices

Abstract

The application discloses a preparation method of high-thermal-conductivity tungsten-nickel-chromium sputtering target material for semiconductor equipment, and comprises the following steps of substrate selection: uniformly blending tungsten, nickel and chromium according to a weight ratio of 65:28:7 to prepare a substrate; adding 10-15% of the total amount of the substrate of nano additives and 2-5% of the total amount of the substrate of rare earth agents into the substrate, then uniformly mixing and sufficiently ball milling to obtain a ball milling body. The tungsten-nickel-chromium sputtering target material is prepared by using tungsten, nickel and chromium to form a substrate, and the nano additives and the rare earth agents are added at the same time, and the target material is prepared by sintering improvement, and the balance and coordination of dielectric property and thermal conductivity of the target material are modified, and the anti-radiation stability effect is remarkable.

Description

Technical Field

[0001] This invention relates to the field of sputtering target technology, and more specifically to a method for preparing a high thermal conductivity tungsten nickel-chromium sputtering target for semiconductor devices. Background Technology

[0002] Targets can be used as insulating layers in semiconductor devices to isolate components and prevent interference and short circuits. In integrated circuits, targets can also form capacitor structures for functions such as charge storage, filtering, and compensation.

[0003] In order to optimize the thermal conductivity of existing semiconductor equipment sputtering targets, the dielectric properties of the products are easily limited. Therefore, the balance and coordination of dielectric properties, thermal conductivity, and radiation resistance are the technical challenges of this invention. Based on this, this invention provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, thereby solving the problems mentioned in the background art.

[0005] The present invention solves the technical problem by adopting the following technical solution:

[0006] This invention provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, comprising the following steps:

[0007] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0008] Step 2: Add 10-15% of the total matrix amount of nano-additives and 2-5% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0009] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0010] Preferably, the ball milling process involves a ball milling speed of 1000-1500 r / min for 2 hours to achieve thorough mixing.

[0011] Preferably, the preparation method of the nano-additive is as follows:

[0012] 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added to 5-8 parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano additives.

[0013] The preparation method of aluminum nitride liquid is as follows:

[0014] Aluminum nitride, nano-bismuth titanate and sodium silicate solution were mixed evenly in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride solution.

[0015] Preferably, the ultrasonic power of the ultrasonic treatment is 400-450W, and the ultrasonic treatment lasts for 20-30 minutes.

[0016] Preferably, the sodium silicate solution has a mass fraction of 2-5%.

[0017] Preferably, the rare earth agent is prepared by:

[0018] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0019] Preferably, the heat treatment temperature is 350-400℃, and the treatment time is 1 hour.

[0020] Preferably, the specific operation steps of the hot pressing sintering improvement treatment are as follows: first, sinter at a temperature of 500-550℃ for 1 hour, then raise the temperature to 800℃ at a rate of 1-3℃ / min, hold for 20-30 minutes, then raise the temperature to 1250℃ at a rate of 2-5℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

[0021] Preferably, the temperature is cooled to room temperature at a rate of 5-8°C / min.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] This invention relates to a tungsten-nickel-chromium sputtering target. The matrix is ​​made of tungsten, nickel, and chromium, and the addition of nano-additives and rare earth agents, combined with sintering, results in a target material with significantly improved dielectric and thermal conductivity, as well as enhanced radiation resistance. The nano-additives are made by blending nano-titanium dioxide with aluminum nitride solution and silane coupling agent KH550, followed by ultrasonic treatment. The aluminum nitride solution contains aluminum nitride, nano-bismuth titanate, and sodium silicate solution, which are then optimized and improved. Furthermore, a rare earth agent, composed of lanthanum oxide, cerium oxide, and neodymium oxide, is used for further synergistic effects. Finally, hot pressing and sintering are performed to further enhance the performance of the resulting target material, achieving a coordinated improvement in performance and significant stability. Detailed Implementation

[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to specific examples. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0025] This embodiment provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, including the following steps:

[0026] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0027] Step 2: Add 10-15% of the total matrix amount of nano-additives and 2-5% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0028] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0029] In this embodiment, the ball milling is performed at a speed of 1000-1500 r / min for 2 hours to ensure thorough mixing.

[0030] The preparation method of the nano-additive in this embodiment is as follows:

[0031] 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added to 5-8 parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano additives.

[0032] The preparation method of aluminum nitride liquid is as follows:

[0033] Aluminum nitride, nano-bismuth titanate and sodium silicate solution were mixed evenly in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride solution.

[0034] In this embodiment, the ultrasonic power for ultrasonic treatment is 400-450W, and the ultrasonic treatment lasts for 20-30 minutes.

[0035] The sodium silicate solution in this embodiment has a mass fraction of 2-5%.

[0036] The preparation method of the rare earth agent in this embodiment is as follows:

[0037] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0038] In this embodiment, the heat treatment temperature is 350-400℃, and the treatment time is 1 hour.

[0039] The specific operation steps of the hot pressing sintering improvement treatment in this embodiment are as follows: first, sinter at a temperature of 500-550℃ for 1 hour, then raise the temperature to 800℃ at a rate of 1-3℃ / min, hold for 20-30 minutes, then raise the temperature to 1250℃ at a rate of 2-5℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

[0040] In this embodiment, the temperature is cooled to room temperature at a rate of 5-8°C / min.

[0041] Example 1.

[0042] This embodiment provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, including the following steps:

[0043] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0044] Step 2: Add 10% of the total matrix amount of nano-additives and 2% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0045] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0046] In this embodiment, the ball milling process is performed at a speed of 1000 r / min for 2 hours to ensure thorough mixing.

[0047] The preparation method of the nano-additive in this embodiment is as follows:

[0048] Three parts of nano-titanium dioxide and one part of silane coupling agent KH550 were mixed and added to five parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano-additives.

[0049] The preparation method of aluminum nitride liquid is as follows:

[0050] Aluminum nitride, nano-bismuth titanate, and sodium silicate solution were mixed evenly in a weight ratio of 2:1:4 to obtain aluminum nitride solution.

[0051] In this embodiment, the ultrasonic power for ultrasonic treatment is 400W, and the ultrasonic treatment lasts for 20 minutes.

[0052] The sodium silicate solution in this embodiment has a mass fraction of 2%.

[0053] The preparation method of the rare earth agent in this embodiment is as follows:

[0054] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0055] In this embodiment, the heat treatment temperature is 350°C, and the treatment time is 1 hour.

[0056] The specific operation steps of the hot pressing sintering improvement treatment in this embodiment are as follows: first, sinter at 500℃ for 1 hour, then raise the temperature to 800℃ at a rate of 1℃ / min, hold for 20 minutes, then raise the temperature to 1250℃ at a rate of 2℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

[0057] In this embodiment, the temperature is cooled to room temperature at a rate of 5°C / min.

[0058] Example 2.

[0059] This embodiment provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, including the following steps:

[0060] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0061] Step 2: Add 15% of the total matrix amount of nano-additives and 5% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0062] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0063] In this embodiment, the ball milling process is performed at a speed of 1500 r / min for 2 hours to ensure thorough mixing.

[0064] The preparation method of the nano-additive in this embodiment is as follows:

[0065] Five parts of nano-titanium dioxide and two parts of silane coupling agent KH550 were mixed and added to eight parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano-additives.

[0066] The preparation method of aluminum nitride liquid is as follows:

[0067] Aluminum nitride, nano-bismuth titanate, and sodium silicate solution were mixed evenly in a weight ratio of 4:1:6 to obtain aluminum nitride liquid.

[0068] In this embodiment, the ultrasonic power for ultrasonic treatment is 450W, and the ultrasonic treatment lasts for 30 minutes.

[0069] The sodium silicate solution in this embodiment has a mass fraction of 5%.

[0070] The preparation method of the rare earth agent in this embodiment is as follows:

[0071] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0072] In this embodiment, the heat treatment temperature is 400°C and the treatment time is 1 hour.

[0073] The specific operation steps of the hot pressing sintering improvement treatment in this embodiment are as follows: first, sinter at 550°C for 1 hour, then raise the temperature to 800°C at a rate of 3°C / min, hold for 30 minutes, then raise the temperature to 1250°C at a rate of 5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0074] In this embodiment, the temperature is cooled to room temperature at a rate of 8°C / min.

[0075] Example 3.

[0076] This embodiment provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, including the following steps:

[0077] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0078] Step 2: Add 12.5% ​​of the total matrix amount of nano-additives and 3.5% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0079] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0080] In this embodiment, the ball milling process is performed at a speed of 1250 r / min for 2 hours to ensure thorough mixing.

[0081] The preparation method of the nano-additive in this embodiment is as follows:

[0082] Four parts of nano-titanium dioxide and 1.5 parts of silane coupling agent KH550 were mixed and added to 6.5 parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano-additives.

[0083] The preparation method of aluminum nitride liquid is as follows:

[0084] Aluminum nitride, nano-bismuth titanate, and sodium silicate solution were mixed evenly in a weight ratio of 3:1:5 to obtain aluminum nitride solution.

[0085] In this embodiment, the ultrasonic power for ultrasonic treatment is 420W, and the ultrasonic treatment lasts for 25 minutes.

[0086] The sodium silicate solution in this embodiment has a mass fraction of 3.5%.

[0087] The preparation method of the rare earth agent in this embodiment is as follows:

[0088] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0089] In this embodiment, the heat treatment temperature is 375°C, and the treatment time is 1 hour.

[0090] The specific operation steps of the hot pressing sintering improvement treatment in this embodiment are as follows: first, sinter at 525℃ for 1 hour, then raise the temperature to 800℃ at a rate of 2℃ / min, hold for 25 minutes, then raise the temperature to 1250℃ at a rate of 3.5℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

[0091] In this embodiment, the temperature is cooled to room temperature at a rate of 6.5°C / min.

[0092] Example 4.

[0093] This embodiment provides a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, including the following steps:

[0094] Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix;

[0095] Step 2: Add 11% of the total matrix amount of nano-additives and 3% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body;

[0096] Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material of the present invention.

[0097] In this embodiment, the ball milling process is performed at a speed of 1100 r / min for 2 hours to ensure thorough mixing.

[0098] The preparation method of the nano-additive in this embodiment is as follows:

[0099] Four parts of nano-titanium dioxide and two parts of silane coupling agent KH550 were mixed and added to six parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano-additives.

[0100] The preparation method of aluminum nitride liquid is as follows:

[0101] Aluminum nitride, nano-bismuth titanate, and sodium silicate solution were mixed evenly in a weight ratio of 3:1:4 to obtain aluminum nitride solution.

[0102] In this embodiment, the ultrasonic power for ultrasonic treatment is 410W, and the ultrasonic treatment lasts for 22 minutes.

[0103] The sodium silicate solution in this embodiment has a mass fraction of 3%.

[0104] The preparation method of the rare earth agent in this embodiment is as follows:

[0105] Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

[0106] In this embodiment, the heat treatment temperature is 360°C, and the treatment time is 1 hour.

[0107] The specific operation steps of the hot pressing sintering improvement treatment in this embodiment are as follows: first, sinter at 520℃ for 1 hour, then raise the temperature to 800℃ at a rate of 2℃ / min, hold for 22 minutes, then raise the temperature to 1250℃ at a rate of 3℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

[0108] In this embodiment, the temperature is cooled to room temperature at a rate of 6°C / min.

[0109] Comparative Example 1.

[0110] Unlike Example 3, no nano-additives were added.

[0111] Comparative Example 2.

[0112] Unlike Example 3, aluminum nitride liquid was not added in the preparation of the nano-additive.

[0113] Comparative Example 3.

[0114] Unlike Example 3, aluminum nitride and nano-bismuth titanate were not added to the aluminum nitride solution.

[0115] Comparative Example 4.

[0116] Unlike Example 3, no rare earth agent was added.

[0117] Comparative Example 5.

[0118] Unlike Example 3, rare earth cerium oxide and neodymium oxide were not added to the rare earth agent.

[0119] The product performance tests for Examples 1-4 and Comparative Examples 1-5 are as follows:

[0120]

[0121] As can be seen from Examples 1-4 and Comparative Examples 1-5, the product of Example 3 of the present invention shows coordinated improvement in breakdown strength and thermal conductivity, and significant improvement in radiation resistance. However, without the addition of rare earth agents and nano-additives, the performance of the product deteriorates significantly. Among them, nano-additives have the greatest impact on product performance. Furthermore, the absence of aluminum nitride liquid in the preparation of nano-additives, the absence of aluminum nitride and nano-bismuth titanate in the aluminum nitride liquid, and the absence of rare earth cerium oxide and neodymium oxide in the rare earth agents all show a trend of deterioration in product performance. The product raw materials obtained by the specific method of the present invention have the most significant performance effect.

[0122] 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 implemented 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 exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0123] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider 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 thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices, characterized in that, Includes the following steps Step 1, Selection of matrix: Tungsten, nickel and chromium are blended uniformly in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 10-15% of the total matrix amount of nano-additives and 2-5% of the total matrix amount of rare earth agent to the matrix, then mix and ball mill thoroughly to obtain the ball milled body; Step 3: Improve the ball mill body by hot pressing and sintering to obtain the target material; The preparation method of the nano-additive is as follows: 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added to 5-8 parts of aluminum nitride solution, ultrasonically treated, then filtered and dried to obtain nano additives. The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution were mixed evenly in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride solution; The rare earth agent is prepared by: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, then heat-treated to obtain a rare earth agent.

2. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, The ball milling process is performed at a speed of 1000-1500 r / min for 2 hours to ensure thorough mixing.

3. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, The ultrasonic power for the ultrasonic treatment is 400-450W, and the ultrasonic treatment lasts for 20-30 minutes.

4. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, The sodium silicate solution has a mass fraction of 2-5%.

5. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, The heat treatment temperature is 350-400℃, and the treatment time is 1 hour.

6. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, The specific operating steps of the improved hot pressing sintering treatment are as follows: first, sinter at a temperature of 500-550℃ for 1 hour, then raise the temperature to 800℃ at a rate of 1-3℃ / min, hold for 20-30 minutes, then raise the temperature to 1250℃ at a rate of 2-5℃ / min, continue sintering for 1 hour, and finally cool to room temperature.

7. The method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target for semiconductor devices according to claim 1, characterized in that, Cool to room temperature at a rate of 5-8°C / min.

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