Preparation method of silicon-molybdenum alloy target material
By using high-purity raw materials in the preparation of silicon-molybdenum alloy targets, a vacuum mixer combined with ultrasonic-assisted dispersion, cold-pressing molding of thermally sprayed boron nitride coating molds, microwave-assisted heating and atmosphere control sintering processes, as well as high-precision CNC processing and chemical cleaning, the problems of wide distribution of raw materials, low mixing efficiency, and poor molding accuracy in traditional preparation methods are solved, and the effects of uniform target composition, stable electrical performance and uniform film deposition are achieved.
Patent Information
- Application Number
- CN202411970309.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-30
- Publication Date
- 2025-03-28
- Estimated Expiration
- 2044-12-30
AI Technical Summary
The traditional silicon-molybdenum alloy target preparation method has problems such as broad particle size distribution, limited purity, low mixing efficiency, poor molding accuracy, unsatisfactory sintered tissue structure and incomplete post-treatment process, resulting in unstable target density and electrical properties, affecting the quality of film deposition.
High-purity molybdenum powder and chemical vapor deposition are prepared by airflow crushing and grading screening technology. The vacuum mixer combines ultrasonic-assisted dispersion and temperature control, and the thermally sprayed boron nitride coating mold for cold pressing molding, microwave-assisted heating and atmosphere control sintering process, as well as high-precision CNC processing, chemical cleaning and plasma treatment post-treatment processes.
It achieves uniform target composition, stable electrical performance, high film deposition uniformity, improved product yield, improved target strength and extended service life, meeting the high-tech industry's demand for high-quality target materials.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of silicon-molybdenum alloy target material preparation, and in particular to a method for preparing a silicon-molybdenum alloy target material. Background Art
[0002] In today's era of booming high-tech industries, the application of thin film materials is becoming more and more extensive. From semiconductor chip manufacturing, flat panel displays to solar photovoltaic fields, high-quality thin film deposition technology is indispensable. As the key raw material for thin film deposition, the performance of target materials directly determines the quality of the film and the characteristics of the final product.
[0003] Silicon-molybdenum alloy targets have unique advantages in many cutting-edge fields due to their characteristics of both silicon and molybdenum. Silicon has good semiconductor properties and can provide precise electrical control for electronic devices; molybdenum has a high melting point, high hardness and excellent thermal conductivity, making the alloy target stable and reliable under high temperature and high power conditions. The silicon-molybdenum alloy target formed by the combination of the two can meet the needs of special application scenarios such as high-temperature semiconductor devices and high-power electronic components.
[0004] However, the traditional method of preparing silicon-molybdenum alloy targets has many drawbacks and is difficult to adapt to the modern industry's requirements for high-quality and high-precision targets. In the early stage of raw material preparation, conventional crushing and simple purification methods were often used to obtain molybdenum powder and silicon powder, resulting in a wide distribution of powder particle size and limited purity, which seriously affected the density and electrical properties of subsequent targets. For example, coarse-grained powders are prone to uneven pores during the molding process, which in turn causes problems such as uneven film thickness and fluctuations in electrical properties during thin film deposition.
[0005] In the past, the mixing process often relied on ordinary mechanical stirring, which had low mixing efficiency and poor uniformity. It was impossible to fully and evenly disperse the molybdenum powder and silicon powder, which easily caused component segregation, resulting in inconsistent performance in different parts of the target material, local defects during thin film deposition, and reduced product yield.
[0006] The molding and sintering processes also face challenges. Traditional cold press molding has rough pressure control, unreasonable mold design, difficult demoulding and easy damage to the blank, affecting the dimensional accuracy and surface quality of the target. During the sintering process, the heating rate, holding time and atmosphere control lack precise regulation, making it difficult to achieve an ideal microstructure, resulting in stress concentration and uneven grain size inside the target. This not only reduces the strength of the target, but also causes cracking of the target due to the release of thermal stress during use, shortening its service life.
[0007] The post-processing process also has shortcomings, such as low machining accuracy, incomplete chemical cleaning, and simple packaging materials that cannot effectively isolate the external environment from erosion, making the target material susceptible to contamination and oxidation during storage and transportation, further reducing its performance. In summary, a new, fully optimized silicon-molybdenum alloy target preparation method is urgently needed to break through these bottlenecks and meet the growing industrial needs. Summary of the invention
[0008] 1. Technical issues to be solved
[0009] In view of the deficiencies in the prior art, the present invention provides a method for preparing a silicon-molybdenum alloy target.
[0010] (II) Technical solution
[0011] A method for preparing a silicon-molybdenum alloy target comprises the following steps:
[0012] S1. Raw material preparation: select metallic molybdenum powder with a purity of not less than 99.9% and a particle size of 1-10μm, prepared by air flow crushing and classification screening technology, and silicon powder with a purity of not less than 99.9% and a particle size of 0.5-5μm, prepared by chemical vapor deposition method, and weighed according to the silicon content mass fraction of 10%-50%;
[0013] S2. Mixing treatment: Place the weighed molybdenum powder and silicon powder in a vacuum mixer, evacuate to 0.01-0.1Pa, stir at a speed of 100-500 rpm for 1-5 hours, use ultrasonic assisted dispersion, the ultrasonic frequency is 20-60kHz, and the ultrasonic generator has an intelligent frequency adjustment function, which is adjusted in real time according to the powder mixing state to ensure that the powders are fully mixed and uniform. At the same time, a temperature control system is provided inside the mixer. The temperature is controlled at 25-40°C during the mixing process, and the circulating water cooling system is used for precise temperature control to prevent the powder from overheating and oxidation due to friction;
[0014] S3, molding process: put the mixed powder into the mold, and coat the inner wall of the mold with boron nitride coating, the coating thickness is 0.05-0.2mm, and the thermal spraying process is used. The coating has strong bonding force, and the mold is cold pressed at a pressure of 200-500MPa, and the pressure holding time is 5-20 minutes. The cold pressing equipment is equipped with a pressure sensor and an automatic compensation system to obtain a blank. The mold is a detachable structure for easy demoulding. The mold material is cemented carbide with a hardness of not less than HRA85, and the mold surface is treated with ion implantation;
[0015] S4, sintering process: put the green blank into a vacuum sintering furnace, first heat it to 1000-1200℃ at a heating rate of 5-15℃ / min, keep it warm for 1-3 hours, use microwave assisted heating to make the green blank heated evenly, then heat it to 1500-1800℃ at a heating rate of 2-8℃ / min, keep it warm for 2-6 hours, maintain the vacuum degree at 0.001-0.01Pa during the whole sintering process, and then cool it with the furnace; the vacuum sintering furnace is equipped with an atmosphere control system, and a small amount of argon gas can be introduced in the later stage of sintering, and the argon gas flow rate is 1-5ml / min, and the gas flow automatic regulating valve is used for precise control to adjust the internal structure of the target material;
[0016] S5. Post-processing process: The sintered target material is mechanically processed by CNC processing equipment with a processing accuracy of ±0.05-±0.2mm. Polycrystalline diamond tools are used as processing tools. Then chemical cleaning is carried out using a mixed solution of hydrofluoric acid and nitric acid. The concentration of hydrofluoric acid is 5%-15%, and the concentration of nitric acid is 10%-25%. The cleaning time is 10-30 minutes. It is carried out with the assistance of ultrasonic oscillation to remove surface impurities. After chemical cleaning, plasma treatment is also carried out using argon plasma with a power of 100-500W and a processing time of 5-15 minutes. The plasma processing equipment is equipped with a radio frequency matching network to automatically optimize the discharge parameters. Finally, vacuum packaging is carried out and high-purity nitrogen is filled in the package. The purity of nitrogen is not less than 99.99%. A vacuum nitrogen filling packaging machine is used.
[0017] Furthermore, the stirring blades of the vacuum mixer adopt a special double-layer spiral structure. The inner blades perform preliminary mixing, and the outer blades enhance the dispersion effect. The surface of the stirring blades is also coated with a ceramic wear-resistant coating with a thickness of 0.02-0.1mm, and the coating has self-lubricating properties.
[0018] Furthermore, in step S3, the detachable structure of the cold pressing mold is connected by a dovetail groove, and an automatic release agent spraying device is provided inside the mold. The release agent is sprayed evenly before demolding to further optimize the demolding effect. At the same time, the release agent is a high-temperature resistant and pollution-free silicone release agent, and the release agent spraying amount can be accurately controlled by the CNC system. According to the mold size and powder characteristics, the spraying amount accuracy is controlled within ±0.1g / cm 2 .
[0019] Furthermore, in step S4, the frequency of the microwave-assisted heating system of the vacuum sintering furnace is 2.45 GHz, and the power is intelligently adjusted according to the size and material of the blank. In addition, during the microwave-assisted heating process, the sintering furnace is also equipped with a temperature field homogenization device, which consists of a multi-layer metal reflector and a heat-averaging medium. It reflects and scatters microwaves to control the temperature field deviation in the furnace within ±2°C.
[0020] Furthermore, in step S5, the target material after chemical cleaning is first subjected to cold air drying treatment to remove residual moisture on the surface before entering the plasma processing equipment. The cold air drying equipment adopts low-temperature cold air circulation technology. The cold air temperature is controlled at 5-15°C and the wind speed is 2-5m / s. At the same time, a humidity sensor is installed inside the drying equipment to monitor the degree of drying in real time. When the humidity is lower than the set value of 10%, the drying is automatically stopped.
[0021] Furthermore, in step S5, the packaging material used for vacuum packaging is a multi-layer composite aluminum foil bag, which has high barrier properties and corrosion resistance, and the inner layer of the multi-layer composite aluminum foil bag is adhered with a layer of deoxidizer sustained-release film, which can slowly release the deoxidizer during storage, so that the oxygen content in the package is always maintained below 0.01%.
[0022] Furthermore, after step S1 is completed, the mixed powder is pre-compacted by using low-frequency vibration compaction technology with a vibration frequency of 10-30 Hz, an amplitude of 0.5-2 mm, and a compaction time of 10-20 minutes to initially compact the powder, reduce powder movement in subsequent molding processes, and improve the uniformity of green billet density.
[0023] Furthermore, during the S4 sintering process, when the temperature rises to 1300-1500°C, hydrogen is intermittently introduced into the vacuum sintering furnace with a hydrogen flow rate of 0.5-2 ml / min. Each introduction time is 2-5 minutes, with an interval of 10-20 minutes. The reducing property of hydrogen is used to remove trace oxide impurities that may exist inside the target material, thereby improving the purity of the target material. At the same time, by controlling the hydrogen introduction time and interval, excessive reaction of hydrogen with molybdenum and silicon can be avoided.
[0024] (III) Beneficial technical effects
[0025] First of all, in terms of raw material processing, air flow crushing and graded screening technology is used to prepare molybdenum powder, and chemical vapor deposition method is used to prepare silicon powder, which ensures that the raw material particle size is uniform and the purity is extremely high (both not less than 99.9%), laying a solid foundation for the subsequent preparation of high-quality target materials, making the target material composition uniform and the electrical performance stable and reliable.
[0026] During the mixing process, the vacuum mixer combines ultrasonic assisted dispersion with intelligent frequency regulation and precise temperature control to allow the molybdenum powder and silicon powder to be fully and evenly mixed, effectively avoiding component segregation, greatly improving the mixing efficiency and uniformity, and thus ensuring that the performance of the target material is consistent everywhere, forming a uniform, high-quality film layer during thin film deposition, and improving product yield.
[0027] In the molding process, the boron nitride coating mold prepared by thermal spraying and the precision cold pressing molding equipment not only facilitate demolding, but also ensure the high size accuracy and excellent surface quality of the blank, provide a good blank for subsequent sintering, and reduce the problem of target material performance degradation caused by molding defects.
[0028] The sintering process uses microwave-assisted heating, precise heating rate and atmosphere control to achieve the ideal microstructure of the target material, evenly distribute internal stress, and make the grains small and uniform, which greatly improves the strength of the target material, effectively prevents cracking during use, and extends the service life of the target material.
[0029] The post-processing process guarantees the quality of the target materials in all aspects. High-precision CNC machining, thorough chemical cleaning and plasma treatment remove surface impurities and improve surface cleanliness. Vacuum packaging is combined with multi-layer composite aluminum foil bags and deoxidizer slow-release films to isolate external moisture and oxygen, maintain the stability of target material performance, and keep it in good condition during storage and transportation, meeting the high-tech industry's stringent demands for high-quality target materials. DETAILED DESCRIPTION
[0030] Embodiment 1:
[0031] Raw materials preparation:
[0032] The metal molybdenum powder with a purity of 99.95% is selected, and the particle size is controlled at 3-7μm. It is made by advanced air flow crushing and fine classification and screening technology to ensure highly uniform particle size. The silicon powder has a purity of 99.93% and a particle size of 1-3μm, and is prepared by optimized chemical vapor deposition. It is accurately weighed according to the mass fraction of silicon content of 30%.
[0033] Hybrid Processing:
[0034] Molybdenum powder and silicon powder are placed in a mixer with high-precision vacuum (vacuumed to 0.05Pa) and stirred at 300 rpm for 3 hours. During this period, ultrasonic waves assist in dispersion, and the ultrasonic frequency is dynamically adjusted at 30-50kHz, which is intelligently adjusted according to the real-time mixing state of the powder. The internal temperature control system of the mixer uses high-precision temperature sensors and efficient circulating water cooling to accurately maintain the temperature at 30°C, effectively preventing powder oxidation.
[0035] Molding process:
[0036] The mixed powder is loaded into a mold with a 0.1mm boron nitride coating (prepared by thermal spraying process, the coating bonding strength exceeds 50MPa) on the inner wall. The mold is a detachable carbide mold (hardness HRA88) connected by a dovetail groove. The surface is treated with ion implantation, and the wear resistance is improved by 30%. Cold pressing is carried out at a pressure of 350MPa, and the pressure is maintained for 12 minutes. The pressure sensor accuracy of the cold pressing equipment reaches ±0.5MPa, and the automatic compensation system calibrates the pressure in real time.
[0037] Sintering process:
[0038] The blank was placed in a vacuum sintering furnace, first heated to 1100°C at 10°C / min, microwave-assisted heating (frequency 2.45GHz, power intelligently regulated according to blank size), and kept warm for 2 hours; then heated to 1650°C at 5°C / min, kept warm for 4 hours, and the vacuum degree during the sintering process was 0.005 Pa. Later, 3ml / min of argon gas was introduced, and a high-precision gas flow automatic regulating valve was used for precise control to adjust the target material microstructure.
[0039] Post-processing process:
[0040] After sintering, the target material is processed by high-precision CNC processing equipment, and the processing accuracy is controlled at ±0.1mm. The sharpness retention of the cutting edge of the polycrystalline diamond tool is improved by 20%. Chemical cleaning uses a mixed solution of 10% hydrofluoric acid and 18% nitric acid, and ultrasonic oscillation assists cleaning for 20 minutes. After that, plasma treatment (argon plasma, power 300W, radio frequency matching network optimizes discharge parameters) for 5 minutes. Finally, it is vacuum packaged in a multi-layer composite aluminum foil bag, and the bag is filled with 99.995% pure nitrogen. The inner layer of deoxidizer slow-release film stabilizes the oxygen content in the package below 0.005%.
[0041] After testing, the density uniformity deviation of the prepared silicon-molybdenum alloy target is less than 0.5%, the grain size is uniform, the average particle size is 20μm, the film thickness uniformity deviation after thin film deposition is less than 3%, and the electrical performance is stable, meeting the needs of high-end semiconductor chip manufacturing.
[0042] Embodiment 2:
[0043] Raw materials preparation:
[0044] Select metal molybdenum powder with a purity of 99.92% and a particle size of 2-8μm, and use air flow pulverization combined with graded screening to ensure the particle size. Silicon powder with a purity of 99.94% and a particle size of 0.8-2μm is prepared by chemical vapor deposition. Weigh according to the mass fraction of silicon content of 40%.
[0045] Hybrid Processing:
[0046] Place in a mixer with a vacuum degree of 0.08Pa, stir at 250 rpm for 4 hours, intelligently adjust the ultrasonic frequency to 25-45kHz, and control the temperature at 35°C.
[0047] Molding process:
[0048] Loaded with 0.15mm boron nitride coating mold (thermal spraying, bonding strength exceeds 60MPa), dovetail groove removable carbide mold (hardness HRA86), ion implantation treatment. 300MPa pressure cold press molding, pressure holding for 15 minutes, pressure sensor accuracy ±0.8MPa, automatic compensation system calibration.
[0049] Sintering process:
[0050] The vacuum sintering furnace was first heated to 1050°C at 8°C / min, with microwave-assisted heating (frequency 2.45GHz, intelligent power control), and kept warm for 2.5 hours; then heated to 1700°C at 4°C / min, kept warm for 5 hours, with a vacuum degree of 0.008Pa, and then precisely controlled by passing 2ml / min of argon gas.
[0051] Post-processing process:
[0052] The CNC machining accuracy is ±0.15mm, chemical cleaning is carried out with a mixed solution of 8% hydrofluoric acid and 22% nitric acid, ultrasonic oscillation for 25 minutes, plasma treatment (power 400W, 5 minutes), multi-layer composite aluminum foil bag vacuum packaging, filled with 99.992% purity nitrogen, and the inner layer of deoxidizer slow-release film controls oxygen below 0.008%.
[0053] Tests show that the target material density uniformity deviation is less than 0.6%, the average grain size is 22μm, and the film thickness uniformity deviation is less than 4%, which is suitable for the field of high-performance flat panel displays.
[0054] Comparative Example:
[0055] Traditional preparation method:
[0056] The raw materials are ordinary mechanically crushed molybdenum powder (purity 99%, particle size 5-20μm) and simply purified silicon powder (purity 99%, particle size 2-8μm), roughly weighed according to the silicon content of 25%. The mixture is stirred by ordinary machinery for 2 hours without vacuum and ultrasonic assistance, and the ambient temperature is uncontrollable. A simple steel mold is used for molding, without coating, and cold pressing at 200MPa pressure. The pressure is maintained for 10 minutes, and demolding is difficult and the blank is damaged. Sintering is done in a simple electric furnace, and the heating rate fluctuates arbitrarily at 3-8℃ / minute, there is no atmosphere control, and the insulation time is inaccurate. Post-processing is manual grinding, and the accuracy can only reach ±0.5mm. Chemical cleaning is simply soaked in a single acid solution for 10 minutes, and then packaged in ordinary plastic bags after natural drying.
[0057]
[0058]
[0059]
[0060] Performance test results:
[0061] The density uniformity deviation of the prepared target material is greater than 3%, the grain size is uneven, the maximum particle size exceeds 50μm, the film thickness uniformity deviation is greater than 10%, the electrical performance fluctuates greatly, and problems such as target material cracking and film layer defects are prone to occur during use. It cannot meet the needs of high-end industries, which is in sharp contrast to Examples 1 and 2.
[0062] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a silicon-molybdenum alloy target, characterized in that: The following steps are involved: S1. Raw material preparation: select metallic molybdenum powder with a purity of not less than 99.9% and a particle size of 1-10μm, prepared by air flow crushing and classification screening technology, and silicon powder with a purity of not less than 99.9% and a particle size of 0.5-5μm, prepared by chemical vapor deposition method, and weighed according to the silicon content mass fraction of 10%-50%; S2. Mixing treatment: Place the weighed molybdenum powder and silicon powder in a vacuum mixer, evacuate to 0.01-0.1Pa, stir at a speed of 100-500 rpm for 1-5 hours, use ultrasonic assisted dispersion, the ultrasonic frequency is 20-60kHz, and the ultrasonic generator has an intelligent frequency adjustment function, which is adjusted in real time according to the powder mixing state to ensure that the powders are fully mixed and uniform. At the same time, a temperature control system is provided inside the mixer. The temperature is controlled at 25-40°C during the mixing process, and the circulating water cooling system is used for precise temperature control to prevent the powder from overheating and oxidation due to friction; S3, molding process: put the mixed powder into the mold, and coat the inner wall of the mold with boron nitride coating, the coating thickness is 0.05-0.2mm, and the thermal spraying process is used. The coating has strong bonding force, and the mold is cold pressed at a pressure of 200-500MPa, and the pressure holding time is 5-20 minutes. The cold pressing equipment is equipped with a pressure sensor and an automatic compensation system to obtain a blank. The mold is a detachable structure for easy demoulding. The mold material is cemented carbide with a hardness of not less than HRA85, and the mold surface is treated with ion implantation; S4, sintering process: put the green blank into a vacuum sintering furnace, first heat it to 1000-1200℃ at a heating rate of 5-15℃ / min, keep it warm for 1-3 hours, use microwave assisted heating to make the green blank heated evenly, then heat it to 1500-1800℃ at a heating rate of 2-8℃ / min, keep it warm for 2-6 hours, maintain the vacuum degree at 0.001-0.01Pa during the whole sintering process, and then cool it with the furnace; the vacuum sintering furnace is equipped with an atmosphere control system, and a small amount of argon gas can be introduced in the later stage of sintering, and the argon gas flow rate is 1-5ml / min, and the gas flow automatic regulating valve is used for precise control to adjust the internal structure of the target material; S5. Post-processing process: The sintered target material is mechanically processed by CNC processing equipment with a processing accuracy of ±0.05-±0.2mm. Polycrystalline diamond tools are used as processing tools. Then chemical cleaning is carried out using a mixed solution of hydrofluoric acid and nitric acid. The concentration of hydrofluoric acid is 5%-15%, and the concentration of nitric acid is 10%-25%. The cleaning time is 10-30 minutes. It is carried out with the assistance of ultrasonic oscillation to remove surface impurities. After chemical cleaning, plasma treatment is also carried out using argon plasma with a power of 100-500W and a processing time of 5-15 minutes. The plasma processing equipment is equipped with a radio frequency matching network to automatically optimize the discharge parameters. Finally, vacuum packaging is carried out and high-purity nitrogen is filled in the package. The purity of nitrogen is not less than 99.99%. A vacuum nitrogen filling packaging machine is used.
2. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: In step S2, the stirring blades of the vacuum mixer adopt a special double-layer spiral structure. The inner blades perform preliminary mixing, and the outer blades enhance the dispersion effect. The surface of the stirring blades is also coated with a ceramic wear-resistant coating with a thickness of 0.02-0.1mm, and the coating has self-lubricating properties.
3. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: In step S3, the detachable structure of the cold-pressed mold is connected by a dovetail groove. An automatic release agent spraying device is installed inside the mold. The release agent is sprayed evenly before demolding to further optimize the demolding effect. At the same time, the release agent is a high-temperature resistant and pollution-free silicone release agent. The amount of release agent sprayed can be accurately controlled by the CNC system. According to the mold size and powder characteristics, the spraying amount accuracy is controlled within ±0.1g / cm 2 .
4. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: In step S4, the frequency of the microwave-assisted heating system of the vacuum sintering furnace is 2.45 GHz, and the power is intelligently adjusted according to the size and material of the blank. In addition, during the microwave-assisted heating process, the sintering furnace is also equipped with a temperature field homogenization device, which consists of a multi-layer metal reflector and a heat-averaging medium. It reflects and scatters microwaves to control the temperature field deviation in the furnace within ±2°C.
5. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: In step S5, the target material after chemical cleaning is first subjected to cold air drying treatment before entering the plasma processing equipment to remove residual moisture on the surface. The cold air drying equipment adopts low-temperature cold air circulation technology. The cold air temperature is controlled at 5-15°C and the wind speed is 2-5m / s. At the same time, a humidity sensor is installed inside the drying equipment to monitor the degree of drying in real time. When the humidity is lower than the set value of 10%, the drying is automatically stopped.
6. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: In step S5, the packaging material used for vacuum packaging is a multi-layer composite aluminum foil bag, which has high barrier properties and corrosion resistance, and the inner layer of the multi-layer composite aluminum foil bag is adhered with a layer of deoxidizer slow-release film, which can slowly release the deoxidizer during storage, so that the oxygen content in the package is always maintained below 0.01%.
7. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: After the S1 step is completed, the mixed powder is pre-compacted using low-frequency vibration compaction technology with a vibration frequency of 10-30 Hz, an amplitude of 0.5-2 mm, and a compaction time of 10-20 minutes to initially compact the powder, reduce powder movement in the subsequent molding process, and improve the uniformity of the green billet density.
8. The method for preparing a silicon-molybdenum alloy target according to claim 1, characterized in that: During the S4 sintering process, when the temperature rises to 1300-1500°C, hydrogen is intermittently introduced into the vacuum sintering furnace with a hydrogen flow rate of 0.5-2 ml / min. Each introduction time is 2-5 minutes, with an interval of 10-20 minutes. The reducing property of hydrogen is used to remove trace oxide impurities that may exist inside the target material, thereby improving the purity of the target material. At the same time, by controlling the hydrogen introduction time and interval, excessive reaction of hydrogen with molybdenum and silicon can be avoided.
Citation Information
Patent Citations
Manufacturing method of molybdenum-silicon target material
CN104513953A
Manufacturing method for molybdenum-silicon target and combination thereof
CN105483624A
Preparation method of integral tubular molybdenum target material for magnetron sputtering
CN108517498A
Molybdenum-silicon target material and powder mixing method and preparation method for improving density of molybdenum-silicon target material
CN117024124A
Metal silicide target material
JP1999256322A
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