Preparation method of high-thermal-conductivity tungsten-nickel-chromium sputtering target material for semiconductor equipment

Abstract

The invention discloses a preparation method of a high-thermal-conductivity tungsten-nickel-chromium sputtering target material for semiconductor equipment. The preparation method comprises the following steps: selection of a substrate: uniformly blending tungsten, nickel and chromium according to a weight ratio of 65: 28: 7 to prepare the substrate; the preparation method comprises the following steps: adding a nano additive accounting for 10-15% of the total amount of a matrix and a rare earth agent accounting for 2-5% of the total amount of the matrix into the matrix, and then uniformly mixing and fully ball-milling to obtain a ball-milled body; according to the tungsten-nickel-chromium sputtering target material disclosed by the invention, tungsten, nickel and chromium are matched to prepare a matrix, and meanwhile, the target material which is prepared by sintering and improving the added nano additive and rare earth agent has remarkable effects of balanced and coordinated modification of dielectricity and thermal conductivity and anti-radiation stability.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and in particular to a method for preparing a high thermal conductivity tungsten-nickel-chromium sputtering target material for semiconductor equipment. Background Art

[0002] Target materials 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 charge storage, filtering, compensation, and other functions.

[0003] In order to optimize the thermal conductivity of the product, the target materials used in existing semiconductor equipment can easily limit the dielectric properties of the product. Therefore, the balance and coordination of dielectric properties and thermal conductivity, as well as radiation resistance stability are technical difficulties of the present invention. Based on this, the present invention provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target. Summary of the Invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solutions: The present invention provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 10-15% of the total amount of the matrix to the nano-additive and 2-5% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0006] Preferably, the mixing and ball milling is carried out at a speed of 1000-1500 r / min and the ball milling is carried out for 2 hours.

[0007] Preferably, the preparation method of the nano additive is: 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added into 5-8 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are uniformly blended in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride liquid.

[0008] Preferably, the ultrasonic treatment is performed at an ultrasonic power of 400-450W and for 20-30 minutes.

[0009] Preferably, the mass fraction of the sodium silicate solution is 2-5%.

[0010] Preferably, the preparation method of the rare earth agent is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0011] Preferably, the heat treatment temperature is 350-400° C., and the treatment time is 1 hour.

[0012] Preferably, the specific operating steps of the hot pressing sintering improvement treatment are: first sinter at a temperature of 500-550°C for 1 hour, then heat to 800°C at a rate of 1-3°C / min, keep warm for 20-30 minutes, then heat to 1250°C at a rate of 2-5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0013] Preferably, cooling to room temperature is performed at a cooling rate of 5-8°C / min.

[0014] Compared with the prior art, the present invention has the following beneficial effects: The tungsten-nickel-chromium sputtering target material of the present invention adopts tungsten, nickel and chromium to form a matrix, and nano-additives and rare earth agents are added to adjust the target material through sintering to improve the dielectric property and thermal conductivity of the target material, and the radiation resistance stability effect is remarkable; the nano-additive adopts nano-titanium dioxide to adjust aluminum nitride liquid and silane coupling agent KH550 through ultrasonic treatment, the aluminum nitride, nano-bismuth titanate and sodium silicate solution in the aluminum nitride liquid are coordinated and optimized, and the rare earth agent prepared by rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide is synergistically adjusted, and finally hot pressing sintering is improved to achieve the target material product performance effect coordinated improvement and the performance stability effect is remarkable. DETAILED DESCRIPTION

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

[0016] The present embodiment provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 10-15% of the total amount of the matrix to the nano-additive and 2-5% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0017] The mixing and milling in this embodiment is thorough, with a ball milling speed of 1000-1500 r / min and ball milling for 2 h.

[0018] The preparation method of the nano additive of this embodiment is: 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added into 5-8 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are uniformly blended in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride liquid.

[0019] The ultrasonic treatment in this embodiment has an ultrasonic power of 400-450W and an ultrasonic treatment time of 20-30 minutes.

[0020] The mass fraction of the sodium silicate solution in this embodiment is 2-5%.

[0021] The preparation method of the rare earth agent of this embodiment is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0022] The heat treatment temperature in this embodiment is 350-400° C., and the treatment time is 1 hour.

[0023] The specific operating steps of the hot pressing sintering improvement treatment of this embodiment are: first sinter at a temperature of 500-550°C for 1 hour, then heat to 800°C at a rate of 1-3°C / min, keep warm for 20-30 minutes, then heat to 1250°C at a rate of 2-5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0024] The cooling to room temperature in this embodiment is performed at a cooling rate of 5-8°C / min.

[0025] Example 1. The present embodiment provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: adding 10% of the total amount of the matrix to the nano-additive and 2% of the total amount of the matrix to the matrix, and then mixing and ball milling to obtain a ball mill; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0026] The mixing in this embodiment was thoroughly ball-milled at a speed of 1000 r / min for 2 h.

[0027] The preparation method of the nano additive of this embodiment is: 3 parts of nano titanium dioxide and 1 part of silane coupling agent KH550 were mixed and added into 5 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are uniformly blended in a weight ratio of 2:1:4 to obtain aluminum nitride liquid.

[0028] The ultrasonic treatment in this embodiment was performed with an ultrasonic power of 400 W and ultrasonic treatment for 20 min.

[0029] The mass fraction of the sodium silicate solution in this embodiment is 2%.

[0030] The preparation method of the rare earth agent of this embodiment is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0031] The heat treatment temperature in this embodiment is 350° C. and the treatment time is 1 hour.

[0032] The specific operating steps of the hot pressing sintering improvement treatment of this embodiment are: first sinter at a temperature of 500°C for 1 hour, then heat to 800°C at a rate of 1°C / min, keep warm for 20 minutes, then heat to 1250°C at a rate of 2°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0033] The cooling to room temperature in this embodiment was performed at a cooling rate of 5°C / min.

[0034] Example 2. The present embodiment provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 15% of the total amount of the matrix to the nano-additive and 5% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0035] The mixing and milling in this embodiment was complete at a speed of 1500 r / min for 2 h.

[0036] The preparation method of the nano additive of this embodiment is: 5 parts of nano titanium dioxide and 2 parts of silane coupling agent KH550 were mixed and added into 8 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are evenly blended in a weight ratio of 4:1:6 to obtain aluminum nitride liquid.

[0037] The ultrasonic treatment in this embodiment was performed with an ultrasonic power of 450 W and for 30 min.

[0038] The mass fraction of the sodium silicate solution in this embodiment is 5%.

[0039] The preparation method of the rare earth agent of this embodiment is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0040] The heat treatment temperature in this embodiment is 400° C. and the treatment time is 1 hour.

[0041] The specific operating steps of the hot pressing sintering improvement treatment of this embodiment are: first sinter at a temperature of 550°C for 1 hour, then heat to 800°C at a rate of 3°C / min, keep warm for 30 minutes, then heat to 1250°C at a rate of 5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0042] The cooling to room temperature in this embodiment was performed at a cooling rate of 8°C / min.

[0043] Example 3. The present embodiment provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 12.5% of the total amount of the matrix to the nano-additive and 3.5% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0044] The mixing was thoroughly ball-milled at a speed of 1250 r / min for 2 h.

[0045] The preparation method of the nano additive of this embodiment is: 4 parts of nano titanium dioxide and 1.5 parts of silane coupling agent KH550 were mixed and added into 6.5 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are evenly blended in a weight ratio of 3:1:5 to obtain aluminum nitride liquid.

[0046] The ultrasonic treatment in this embodiment was performed with an ultrasonic power of 420 W and for 25 min.

[0047] The mass fraction of the sodium silicate solution in this embodiment is 3.5%.

[0048] The preparation method of the rare earth agent of this embodiment is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0049] The heat treatment temperature in this embodiment is 375° C. and the treatment time is 1 hour.

[0050] The specific operating steps of the hot pressing sintering improvement treatment of this embodiment are: first sinter at a temperature of 525°C for 1 hour, then heat to 800°C at a rate of 2°C / min, keep warm for 25 minutes, then heat to 1250°C at a rate of 3.5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0051] The cooling to room temperature in this example was performed at a cooling rate of 6.5°C / min.

[0052] Example 4. The present embodiment provides a method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, comprising the following steps: Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 11% of the total amount of the matrix to the nano-additive and 3% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

[0053] The mixing and ball milling in this embodiment was performed at a speed of 1100 r / min for 2 h.

[0054] The preparation method of the nano additive of this embodiment is: 4 parts of nano titanium dioxide and 2 parts of silane coupling agent KH550 were mixed and added into 6 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are evenly blended in a weight ratio of 3:1:4 to obtain aluminum nitride liquid.

[0055] The ultrasonic treatment in this embodiment was performed with an ultrasonic power of 410 W and for 22 min.

[0056] The mass fraction of the sodium silicate solution in this embodiment is 3%.

[0057] The preparation method of the rare earth agent of this embodiment is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

[0058] The heat treatment temperature in this embodiment is 360° C. and the treatment time is 1 hour.

[0059] The specific operating steps of the hot pressing sintering improvement treatment of this embodiment are: first sinter at a temperature of 520°C for 1 hour, then heat to 800°C at a rate of 2°C / min, keep warm for 22 minutes, then heat to 1250°C at a rate of 3°C / min, continue sintering for 1 hour, and finally cool to room temperature.

[0060] The cooling to room temperature in this embodiment was performed at a cooling rate of 6°C / min.

[0061] Comparative Example 1. The difference from Example 3 is that no nano additives are added.

[0062] Comparative Example 2. The difference from Example 3 is that no aluminum nitride liquid is added during the preparation of the nano-additive.

[0063] Comparative Example 3. The difference from Example 3 is that no aluminum nitride or nano-bismuth titanate is added to the aluminum nitride liquid.

[0064] Comparative Example 4. The difference from Example 3 is that no rare earth agent is added.

[0065] Comparative Example 5. The difference from Example 3 is that rare earth cerium oxide and neodymium oxide are not added to the rare earth agent.

[0066] The product performance tests of Examples 1-4 and Comparative Examples 1-5 are as follows:

[0067] It can be seen from Examples 1-4 and Comparative Examples 1-5 that the breakdown strength and thermal conductivity of the product of Example 3 of the present invention are improved in a coordinated manner, and the radiation stability of the product is also significantly improved; however, without the addition of rare earth agents and nano-additives, the performance of the product deteriorates significantly, among which the nano-additives have the greatest impact on the product performance. At the same time, without the addition of aluminum nitride liquid in the preparation of the nano-additives, without the addition of aluminum nitride and nano-bismuth titanate to the aluminum nitride liquid, and without the addition of rare earth cerium oxide and neodymium oxide to the rare earth agent, the performance of the product tends to deteriorate. The product raw materials obtained by the specific method of the present invention have the most significant performance effect.

[0068] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0069] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment, characterized in that: The following steps are included Step 1: Selection of a matrix: Tungsten, nickel, and chromium are uniformly mixed in a weight ratio of 65:28:7 to form a matrix; Step 2: Add 10-15% of the total amount of the matrix to the nano-additive and 2-5% of the total amount of the matrix to the matrix, then mix and ball-mill thoroughly to obtain a ball-milled body; Step three: hot pressing and sintering the ball mill to obtain the target material of the present invention.

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

3. The method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 1, characterized in that: The preparation method of the nano additive is: 3-5 parts of nano titanium dioxide and 1-2 parts of silane coupling agent KH550 are mixed and added into 5-8 parts of aluminum nitride solution for ultrasonic treatment, and then filtered and dried to obtain a nano additive; The preparation method of aluminum nitride liquid is as follows: Aluminum nitride, nano-bismuth titanate and sodium silicate solution are uniformly blended in a weight ratio of (2-4):1:(4-6) to obtain aluminum nitride liquid.

4. The method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 3, characterized in that: The ultrasonic treatment is performed with an ultrasonic power of 400-450W and an ultrasonic treatment time of 20-30 minutes.

5. The method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 3, characterized in that: The mass fraction of the sodium silicate solution is 2-5%.

6. The method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 1, characterized in that: The preparation method of the rare earth agent is: Rare earth lanthanum oxide, rare earth cerium oxide and neodymium oxide are mixed in a weight ratio of 3:2:1, and then heat-treated to obtain a rare earth agent.

7. A method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 6, characterized in that: The heat treatment temperature is 350-400° C., and the treatment time is 1 hour.

8. The method for preparing a high thermal conductivity tungsten nickel chromium sputtering target for semiconductor equipment according to claim 1, characterized in that: The specific operating steps of the hot pressing sintering improvement treatment are: first sinter at a temperature of 500-550°C for 1 hour, then heat to 800°C at a rate of 1-3°C / min, keep warm for 20-30 minutes, then heat to 1250°C at a rate of 2-5°C / min, continue sintering for 1 hour, and finally cool to room temperature.

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

Images