WO2022156636A1 - 一种高热导、净尺寸氮化硅陶瓷基片的制备方法 - Google Patents

一种高热导、净尺寸氮化硅陶瓷基片的制备方法 Download PDF

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WO2022156636A1
WO2022156636A1 PCT/CN2022/072352 CN2022072352W WO2022156636A1 WO 2022156636 A1 WO2022156636 A1 WO 2022156636A1 CN 2022072352 W CN2022072352 W CN 2022072352W WO 2022156636 A1 WO2022156636 A1 WO 2022156636A1
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silicon nitride
powder
preparation
green body
ceramic substrate
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PCT/CN2022/072352
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English (en)
French (fr)
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张辉
刘学建
蒋金弟
姚秀敏
黄政仁
陈忠明
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中国科学院上海硅酸盐研究所
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Priority to JP2023544057A priority Critical patent/JP2024503523A/ja
Priority to US18/273,332 priority patent/US20240116821A1/en
Publication of WO2022156636A1 publication Critical patent/WO2022156636A1/zh

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Definitions

  • the invention relates to a preparation method of a silicon nitride ceramic substrate with high thermal conductivity and net size, and belongs to the field of ceramic material preparation.
  • semiconductor devices have developed rapidly along the direction of high power, high frequency and integration.
  • the heat generated by the operation of the semiconductor device is a key factor that causes the failure of the semiconductor device, and the thermal conductivity of the insulating substrate is the key to affecting the heat dissipation of the overall semiconductor device.
  • semiconductor devices often face complex mechanical environments such as bumps and vibrations during use, which imposes strict requirements on the mechanical reliability of the materials used.
  • Silicon nitride (Si 3 N 4 ) ceramics with high thermal conductivity have excellent mechanical and thermal properties.
  • the excellent mechanical properties and good high thermal conductivity make silicon nitride ceramics promising to make up for the deficiencies of existing substrate materials such as alumina and aluminum nitride. , it has great market prospects in the application of high-end semiconductor devices, especially high-power semiconductor devices.
  • the thickness requirements of silicon nitride ceramic substrates for commercial applications are concentrated at about 0.2 to 0.8 mm. For such thin samples, it is very difficult to form. Therefore, the molding of substrates is the core technology to realize its mass production and subsequent application.
  • the forming methods of ceramic substrates mainly include tape casting, dry pressing, and rolling. Among them, the dry-pressed substrates often have problems such as difficulty in directly preparing ceramic substrates with a thickness of less than 0.5 mm, inability to accurately control the thickness, and uneven thickness due to the non-uniformity of powder flow and the technological characteristics of mechanical pressure. Therefore, subsequent machining is required.
  • the rolling film forming process is complex, and it is necessary to repeatedly roll the film to eliminate the uneven thickness caused by the limitations of the process itself and the lumps caused by the agglomeration of the raw materials, resulting in the prepared substrates prone to blistering and surface unevenness.
  • Only mechanical processing can meet the requirements of the subsequent copper cladding process.
  • the tape casting process has high production efficiency, low cost, can be fully automated, and is convenient for continuous batch production. It is the most promising and potential process technology for ceramic substrate molding, but there are also prepared tape casting.
  • the film is prone to blistering, cracking, deformation, uneven thickness, etc., resulting in problems such as low yield, low flatness, uneven thickness, and the need for subsequent machining.
  • the ceramic substrate has the characteristics of high flatness, uniform thickness and smooth surface, which are the technological requirements for its subsequent copper cladding.
  • the present invention provides a method for preparing a high thermal conductivity, clean size silicon nitride ceramic substrate, comprising:
  • ( 2 ) tape casting and drying are carried out in a nitrogen atmosphere to obtain a first green body; the drying is to use a flowing heat N atmosphere with increasing temperature for drying;
  • the crucible used for the gas pressure sintering is a high-purity BN crucible Or a graphite crucible with a high-purity BN isolation layer attached to the surface.
  • the problem of the ease of casting substrates is solved. Blistering, cracking, deformation, uneven thickness and other problems, realize the net size forming of high thermal conductivity silicon nitride ceramic substrate.
  • the purpose of reducing or eliminating air bubbles in the slurry and reducing the agglomeration in the slurry is achieved by fully ball-milling and mixing under a protective atmosphere during the preparation of the casting slurry, combined with low-vacuum and long-term degassing treatment.
  • the preparation of high-quality, defect-free cast films and their uniform thickness are achieved by the precise control of the cylindrical doctor blade and its height during the casting process, and the continuous hot N2 atmosphere with increasing temperature to dry the cast film blanks. precise control of sex.
  • the secondary oxidation of the silicon nitride powder raw material is suppressed by measures such as ball-milling mixing and N 2 protective atmosphere in the process of tape casting, so as to ensure that the prepared silicon nitride ceramic substrate has the characteristics of high thermal conductivity.
  • the density, thickness uniformity and flatness of the prepared cast film are further improved.
  • the micro-positive pressure debonding process is adopted, and by precisely controlling the escape rate of the gas generated by the decomposition of organic matter during the debonding process, the cracking, surface peeling and bubble generation during the debonding process of the green body are prevented, and the surface of the green body on the substrate is avoided. defect.
  • high nitrogen pressure sintering in the sintering process the deformation of the substrate blank during the sintering process is controlled, the decomposition of silicon nitride is suppressed, and the surface roughness of the silicon nitride substrate is precisely adjusted.
  • the sintering aids are rare earth oxides and alkaline earth metal oxides, and the amount added is the total mass of silicon nitride powder, silicon nitride formed by nitriding silicon powder, and sintering aids of 4.0 to 5.0 wt%.
  • the rare earth oxide contains Y 2 O 3 and the alkaline earth metal oxide contains MgO.
  • the dispersing agent is selected from at least one of polyethylene glycol (PEG) and triethyl phosphate (TEP), and the amount added is silicon nitride powder, silicon powder completely nitrided.
  • the defoaming agent may be oleic acid, and the amount added is 0.2-1.0 wt% of the total mass of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder, and sintering aids .
  • the binder may be polyvinyl butyral (PVB), and the amount added is the total of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder, and sintering aids. 5-9wt% of the mass.
  • the plasticizer is selected from at least one of diethyl phthalate (DEP), dibutyl phthalate (DBP) and polyethylene glycol (PEG).
  • DEP diethyl phthalate
  • DBP dibutyl phthalate
  • PEG polyethylene glycol
  • the amount added is 2-6 wt% of the total mass of silicon nitride powder, silicon nitride formed by complete nitridation of silicon powder and sintering aid.
  • the protective atmosphere is a nitrogen atmosphere or an inert atmosphere, and the pressure of the protective atmosphere is 0.1 MPa.
  • the mixing method is ball milling mixing, the rotation speed of the ball milling mixing is 30-100 rpm, and the total time is 6-24 hours; the vacuum degree of the vacuum degassing is -0.1 ⁇ -10kPa, the time is 6 ⁇ 24 hours.
  • at least one of silicon nitride powder and silicon powder, sintering aid, dispersant and defoaming agent are ball-milled and mixed for 3 to 12 hours, and then the binder and The plasticizer is continuously ball-milled and mixed for 3 to 12 hours to obtain the mixed slurry.
  • the pressure of the nitrogen atmosphere is 0.1-0.2 MPa.
  • the pressure is 0.1-0.2MPa
  • the temperature is 40-85°C
  • the total drying time is 15-60 minutes; preferably , the drying is carried out in at least two stages, and the nitrogen temperature in the latter stage is greater than the nitrogen temperature in the previous stage; more preferably, the number of stages is 3, including: the temperature of the first stage is 40-60 ° C, the drying time 5 to 20 minutes, the temperature range of the second stage is 55 to 70 ° C, the drying time is 5 to 20 minutes, the temperature range of the third stage is 65 to 85 ° C, and the drying time is 5 to 20 minutes, and the first stage The temperature of ⁇ the temperature of the second stage ⁇ the temperature of the third stage.
  • the shaping pretreatment is to treat the first green body by cold isostatic pressing; the pressure of the cold isostatic pressing is 40-200 MPa, and the time is 2-10 minutes.
  • the atmospheric pressure of the slightly positive nitrogen atmosphere is 0.1-0.2 MPa; the debonding time is 1-3 hours.
  • the quality of the silicon powder is not less than 75% of the mass of the original powder, wherein the quality of the original powder is the nitrogen generated after the silicon nitride powder and the silicon powder are completely nitrided.
  • the pressure of the nitrogen atmosphere in the gas pressure sintering is 0.5-10 MPa; the holding time of the gas pressure sintering is 4-12 hours.
  • the crucible used for the gas pressure sintering is a high-purity BN crucible or a graphite crucible with a high-purity BN isolation layer attached to the surface.
  • the purity of the high-purity BN crucible is greater than 99%.
  • the purity of the high-purity BN isolation layer is >99%.
  • the present invention provides a high thermal conductivity, net size silicon nitride ceramic substrate prepared according to the above preparation method, wherein the high thermal conductivity, net size silicon nitride ceramic substrate has a thickness of 0.2-1.0 mm and a uniform thickness.
  • the property is ⁇ 0.04mm, the flatness is 0-0.002mm/mm, and the surface roughness is 0.3-0.8 ⁇ m; the thermal conductivity of the silicon nitride ceramic substrate is greater than 80W ⁇ m -1 ⁇ K -1 .
  • the flatness, thickness uniformity and surface roughness of the substrate are respectively controlled in the range of 0.002mm/mm, ⁇ 0.04mm and 0.3-0.8 ⁇ m, it can be directly used in the subsequent copper cladding process without machining.
  • the size of the silicon nitride ceramic substrate is at least 90 mm ⁇ 90 mm, preferably (114-140) mm ⁇ (114-190) mm.
  • the distinctive feature of the invention is that the prepared silicon nitride ceramic substrate can realize precise control of sintering size and surface quality, can be used directly without subsequent processing, and has the characteristics of simple preparation process, economical and practicality.
  • Another notable feature of the present invention is that high thermal conductivity of the silicon nitride ceramic substrate is achieved by controlling oxidation and impurity introduction during the preparation process.
  • FIG. 1 is the silicon nitride ceramic substrate prepared in Example 1.
  • FIG. 2 is the microstructure of the silicon nitride ceramic substrate prepared in Example 1.
  • FIG. 3 is a silicon nitride ceramic substrate prepared in Comparative Example 3.
  • FIG. 3 is a silicon nitride ceramic substrate prepared in Comparative Example 3.
  • FIG. 4 is a silicon nitride ceramic substrate prepared in Comparative Example 5.
  • Table 1 in FIG. 5 is the process parameters of the silicon nitride ceramic substrate prepared by the present invention.
  • Table 2 in FIG. 6 is the performance parameters of the silicon nitride ceramic substrate prepared by the present invention.
  • the silicon nitride ceramic base is solved.
  • the problems of easy blistering, cracking, deformation, and uneven thickness of the sheet are realized, and the preparation of silicon nitride ceramic substrates with uniform thickness, no surface pores and stains, no subsequent machining, and can be directly used in the subsequent copper cladding process .
  • the following exemplifies the preparation method of the high thermal conductivity, neat size silicon nitride ceramic substrate.
  • Preparation of agglomeration-free, bubble-free slurries At least one of silicon nitride powder and silicon powder, sintering aids, dispersants, defoaming agents, binders and plasticizers are ball-milled and mixed in a protective atmosphere (such as N2 atmosphere, the pressure can be 0.1MPa) After the material is degassed, vacuum degassing is carried out to prepare a mixed slurry without agglomeration and bubbles. In the ball milling process, silicon nitride ceramic grinding balls are used.
  • the sintering aids can be rare earth oxides and alkaline earth metal oxides.
  • the rare earth oxide contains at least Y 2 O 3
  • the alkaline earth metal oxide contains at least MgO.
  • the molar ratio between the rare earth oxide and the alkaline earth metal oxide may be (1.0-1.4):(2.5-2.9).
  • the content of the silicon powder may be 75-100 wt%.
  • the prepared slurry is vacuumed to remove air bubbles, the vacuum degree can be -0.1 ⁇ -10kPa, and the degassing time can be 6 ⁇ 24h.
  • Preparation of cast film blanks with uniform thickness and no bubbles on the surface Cast molding under N2 atmosphere (0.1-0.2MPa). Drying is carried out in a flowing hot N 2 atmosphere (the flow rate can be 10-1000 liters/min) to achieve the preparation of a cast film green body with uniform thickness and no bubbles on the surface.
  • a cylindrical doctor blade is used for tape casting under N 2 atmosphere, and the thickness of the cast film green body can be adjusted by controlling the height of the doctor blade.
  • the casting film green body is dried by using a flowing hot N2 atmosphere with increasing temperature, the temperature range of the hot N2 atmosphere can be 40-85 DEG C, and the atmosphere pressure can be 0.1-0.2MPa.
  • the number of passing temperature stages is 2, including: the temperature of the first stage can be 40-65°C, the drying time is 15-30 minutes, the temperature range of the second stage can be 60-85°C, and the drying time is 15- 30 minutes, and the temperature of the first stage ⁇ the temperature of the second stage.
  • the number of passing temperature stages is 3, including: the temperature of the first stage can be 40-60°C, the drying time can be 5-20 minutes, the temperature range of the second stage can be 55-70°C, and the drying time can be 5-20 minutes, the temperature range of the third stage can be 65-85°C, the drying time can be 5-20 minutes, and the temperature of the first stage ⁇ the temperature of the second stage ⁇ the temperature of the third stage.
  • Shaping pretreatment of cast film green body Under a certain pressure (40-200MPa), cold isostatic pressing pretreatment is performed on the cut cast film blank (substrate blank) to ensure the thickness uniformity and flatness of the cast film.
  • the time of shaping pretreatment may be 2-10 minutes.
  • the substrate blank is heat-treated.
  • a slight positive pressure is generated by passing in an N 2 atmosphere
  • the atmospheric pressure may be 0.1-0.2 MPa
  • the processing temperature is 500-900° C.
  • the processing time is 1-3 h.
  • the mass of the silicon powder is not less than 75% of the original powder mass, wherein the original powder mass is the mass of silicon nitride generated after the silicon nitride powder and the silicon powder are completely nitrided sum.
  • the substrate blank is nitrided in a hydrogen/nitrogen mixed atmosphere with a hydrogen content not higher than 5 vol% and a certain temperature.
  • the atmosphere pressure may be 0.1-0.2 MPa
  • the nitriding temperature may be 1350-1450° C.
  • the nitriding time may be 3-6 hours.
  • Gas pressure sintering was carried out under high pressure N2 atmosphere.
  • the sintering of the substrate green body is carried out by placing it in a BN crucible and performing gas pressure sintering under the condition of high-pressure N 2 atmosphere, wherein the N 2 atmosphere pressure is preferably 0.5-10 MPa, which is more conducive to improving the mechanical properties of the material within this range.
  • the N 2 atmosphere pressure is preferably 0.5-10 MPa, which is more conducive to improving the mechanical properties of the material within this range.
  • Thermal / electrical properties reduce the roughness of the substrate surface.
  • the sintering temperature can be 1800-2000°C, and the holding time can be 4-12 hours.
  • the preparation process of the high thermal conductivity, clean size silicon nitride ceramic substrate in the present invention is all carried out in a nitrogen atmosphere.
  • the thickness uniformity of the silicon nitride ceramic substrate obtained by using a micrometer test is ⁇ 0.04mm.
  • the flatness of the silicon nitride ceramic substrate obtained by testing with a profilometer can range from 0 to 0.002 mm/mm.
  • the surface roughness of the silicon nitride ceramic substrate obtained by testing with a profiler can be 0.3-0.8 ⁇ m.
  • the thermal conductivity of the silicon nitride ceramic substrate obtained by testing the silicon nitride ceramic substrate obtained by using a laser thermal conductivity meter is greater than 80W ⁇ m -1 ⁇ K -1 .
  • defoamer oleic acid, 0.5g
  • dispersant PEG, 0.5g
  • the prepared slurry was vacuumed to remove air bubbles for 12 hours, and the vacuum degree was -0.5kPa.
  • a cylindrical scraper was used to cast the above-mentioned slurry after debubbling, and the thickness of the cast film green body was precisely controlled at 0.4 ⁇ 0.04mm by controlling the height of the scraper.
  • the casting film green body was dried using a flowing hot N2 atmosphere with increasing temperature (flow rate of 100 L/min), the pressure of the N2 atmosphere was 0.1MPa, and the temperature of the hot N2 atmosphere with increasing temperature was 45 °C (8 min. ), 65°C (8 minutes) and 80°C (8 minutes) are composed of three stages: front, middle and back.
  • the green substrate was debonded at 700 °C for 2 h under a N2 atmosphere of 0.15 MPa.
  • the debonded substrate blanks were loaded into a high-purity BN crucible (purity > 99%) and then placed in a gas pressure sintering furnace. After sintering at 1900°C for 10h under a 5MPa N2 atmosphere, the furnace was cooled to room temperature.
  • the silicon nitride ceramic substrate prepared in Example 1 is shown in Fig. 1, the size is 114.4mm ⁇ 114.4mm, the size deviation is ⁇ 0.1mm, the thickness is 0.32 ⁇ 0.02mm, the flatness is 0.2mm, and the surface roughness is 0.4 ⁇ m.
  • the thermal conductivity of the material is 95W/(m ⁇ K) and the bending strength is 780MPa.
  • the substrate does not require subsequent mechanical processing, and can be directly used for the subsequent copper cladding process.
  • the microstructure of its section is shown in Figure 2, and the microstructure is uniform and dense.
  • Example 1 The raw material ratio, composition, and technological process refer to Example 1. Specific parameters such as slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering processes are shown in Table 1 in Figure 5. The prepared substrate The material properties are shown in Table 2 in Figure 6.
  • dispersant PEG, 0.3g
  • grinding ball silicon nitride ball, 120g
  • organic solvent absolute ethanol, 50g
  • the casting film green body was dried using a flowing hot N2 atmosphere with increasing temperature (flow rate of 50 L/min), the pressure of the N2 atmosphere was 0.2 MPa, and the temperature of the hot N2 atmosphere with increasing temperature was 45 °C (6 min. ), 65°C (6 minutes) and 80°C (6 minutes) are composed of front, middle and back sections.
  • Example 6 The raw material ratio, composition, and technological process refer to Example 6. Specific parameters such as slurry preparation, vacuum degassing, tape casting, green body shaping, debonding, nitriding treatment and sintering process are shown in Table 1. The sheet material properties are shown in Table 2.
  • Example 10 The preparation process of the silicon nitride ceramic substrate in Example 10 refers to Example 1, the difference is that: an automatic slicer is used to cut into square pieces of 200mm ⁇ 200mm, and cold isostatic pressing is performed at 100MPa for shaping.
  • Example 11 The preparation process of the silicon nitride ceramic substrate in Example 11 refers to Example 6, the difference is that: an automatic slicer is used to cut into square pieces of 200mm ⁇ 200mm, and cold isostatic pressing is performed at 100MPa for shaping.
  • the specific parameters of raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, debonding and sintering process are as shown in Table 1, and the process process refers to Example 1, the difference is that no china shaping pretreatment is performed.
  • the properties of the prepared substrate materials are shown in Table 2. Because the tape-casting substrate blank is not subjected to isostatic pressing pretreatment, the thickness uniformity and flatness of the prepared substrate are obviously reduced, and the thermal conductivity is also slightly reduced.
  • the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1.
  • the technological process refers to Example 1, except that high nitrogen gas is not used.
  • High temperature sintering was carried out under pressure, and only 0.1MPa N2 protective atmosphere was used.
  • the properties of the prepared substrate materials are shown in Table 2. Because the gas pressure sintering in a high nitrogen atmosphere is not used, the surface roughness of the prepared substrate is obviously increased, which cannot meet the requirements of the subsequent copper cladding process for the surface roughness of the substrate.
  • the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1, and the technological process refers to Example 1, the difference is: no micro-positive Pressure debonding (debonding using vacuum conditions).
  • the properties of the prepared substrate materials are shown in Table 2. Due to the use of vacuum debonding, the escape rate of the gas generated by the decomposition of the organic matter during the debonding process is uncontrollable (too fast), and microcrack defects exist locally on the surface of the prepared substrate (see Figure 3).
  • the specific parameters such as raw material ratio and composition, slurry preparation, tape casting, green body shaping, debonding and sintering process are shown in Table 1, and the process refers to Example 1, except that vacuum degassing measures are not taken.
  • the properties of the prepared substrate materials are shown in Table 2. Because the vacuum degassing measure is not adopted, there are a small amount of air bubbles in the slurry, and there are small air bubble defects on the surface of the prepared substrate.
  • the specific parameters such as raw material ratio and composition, slurry preparation, vacuum degassing, tape casting, green body shaping, debonding and sintering process are as shown in Table 1.
  • the technological process refers to Example 1, the difference is that high purity is not used.
  • the BN crucible is used as a container for high-temperature sintering of silicon nitride substrate blanks, but is directly placed in the graphite crucible.
  • the properties of the prepared substrate materials are shown in Table 2. Because the high-purity BN crucible is not used, the graphite crucible is easy to contaminate the substrate, the surface uniformity of the prepared substrate is poor, and there are local color spot defects (see Figure 4).

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Abstract

本发明涉及一种高热导、净尺寸氮化硅陶瓷基片的制备方法,包括:(1)将氮化硅粉和硅粉中至少一种作为原始粉体、烧结助剂、分散剂、消泡剂、粘结剂和增塑剂在保护气氛中混合后,再经真空脱气,得到混合浆料;(2)在氮气气氛中进行流延成型和干燥,得到第一素坯;(3)将所得第一素坯进行整形预处理,得到第二素坯;(4)将所得第二素坯在微正压的氮气气氛中、500~900℃下进行脱粘,得到第三素坯;(5)将所得第三素坯置于氮气气氛中、1800~2000℃下进行气压烧结,得到所述高热导、净尺寸氮化硅陶瓷基片。

Description

一种高热导、净尺寸氮化硅陶瓷基片的制备方法 技术领域
本发明涉及一种高热导、净尺寸氮化硅陶瓷基片的制备方法,属于陶瓷材料制备领域。
背景技术
近年来,半导体器件沿着大功率化、高频化、集成化的方向迅猛发展。半导体器件工作产生的热量是引起半导体器件失效的关键因素,而绝缘基板的导热性是影响整体半导体器件散热的关键。此外,如在电动汽车、高铁等领域,半导体器件使用过程中往往要面临颠簸、震动等复杂的力学环境,这对所用材料的力学可靠性提出了严苛的要求。
高导热氮化硅(Si 3N 4)陶瓷具有优异的力学和热学性能,优良的力学性能和良好的高导热潜质使氮化硅陶瓷有望弥补现有氧化铝、氮化铝等基板材料的不足,在高端半导体器件、特别是大功率半导体器件应用方面极具市场前景。
目前,商业应用对氮化硅陶瓷基片的厚度要求集中在0.2~0.8mm左右,对于如此薄的样品,成型难度非常大。因此,基片的成型是实现其批量化及后续应用的核心技术。目前陶瓷基片的成型方法主要有流延成型、干压成型、轧膜成型等。其中,干压成型的基片因粉体流动的不均匀性和机械加压的工艺特性,往往存在难以直接制备出厚度0.5mm以下的陶瓷基片、厚度不能精确控制和厚度不均匀等难题,因此需要后续机械加工。轧膜成型工艺复杂,需要反复轧膜以消除工艺本身局限性带来的厚度不均匀和因原料结团带来的疙瘩料,导致制备的基片容易出现起泡和表面的凹凸不平,同样需要机械加工才能满足后续的覆铜工艺要求。相比之下,流延成型工艺的生产效率高、成本低,可实现全自动化,便于连续批量化生产,是陶瓷基片成型最有发展前景和潜力的工艺技术,但同样存在制备的流延膜容易起泡、开裂、变形、厚度不均匀等现象,导致成品率低下、平面度低、厚度不均匀、需要后续机械加工等难题。而陶瓷基片具有高平面度、厚度均匀、表面光滑等特性是其后续覆铜的工艺要求。
发明内容
为此,本发明提供了一种高热导、净尺寸氮化硅陶瓷基片的制备方法,包括:
(1)将选自氮化硅粉和硅粉中至少一种的原始粉体、烧结助剂、分散剂、消泡剂、粘结剂和增塑剂在保护气氛中混合后,再经真空脱气,得到混合浆料;所述真空脱气的真空度为-0.1~-10kPa,时间为6~24小时;
(2)在氮气气氛中进行流延成型和干燥,得到第一素坯;所述干燥为采用温度递增 的流动热N 2气氛进行干燥;
(3)将所得第一素坯进行整形预处理,得到第二素坯,所述整形预处理为采用冷等静压的方式处理第一素坯;
(4)将所得第二素坯在微正压的氮气气氛中、500~900℃下进行脱粘,得到第三素坯,所述微正压的氮气气氛的气氛压力为0.12~0.2MPa;所述脱粘的时间为1~3小时;
(5)将所得第三素坯置于氮气气氛中、1800~2000℃下进行气压烧结,得到所述高热导、净尺寸氮化硅陶瓷基片;所述气压烧结所用坩埚为高纯BN坩埚或表面附着有高纯BN隔离层的石墨坩埚。
在本公开中,通过流延成型制备工艺过程中的浆料制备、真空脱气、流延成型、素坯干燥、素坯整形、脱粘和烧结工艺的设计与调控,解决流延基片易起泡、开裂、变形、厚度不均匀等难题,实现高热导氮化硅陶瓷基片的净尺寸成型。具体包括:通过流延浆料制备过程中在保护气氛下充分球磨混料、并结合低真空长时间脱气处理,达到减少或消除浆料中的气泡、减少浆料中团聚的目的。通过流延成型过程中圆筒形刮刀及其高度的精密控制、以及温度递增的连续热N 2气氛对流延膜素坯干燥处理措施,实现高质量、无缺陷流延膜的制备及其厚度均匀性的精确控制。通过球磨混料和流延成型过程中的N 2保护气氛等措施,抑制氮化硅粉体原料的二次氧化,保证所制备氮化硅陶瓷基片具有高热导率特性。通过等静压整形预处理工艺,进一步提高所制备流延膜的致密度、厚度均匀性和平整度。采取微正压脱粘工艺,通过精密控制脱粘过程中有机物分解所产生气体的逸出速率,阻止素坯脱粘过程中的开裂、表面起皮和气泡的产生,避免基片素坯产生表面缺陷。通过烧结过程中高氮气压力烧结,控制烧结过程中基片素坯的形变,抑制氮化硅的分解,进而精密调节氮化硅基片的表面粗糙度。通过上述工艺技术的共同作用,最终实现高热导、高平面度、高厚度均匀性、表面粗糙度可控、表面质量均匀一致的高性能氮化硅陶瓷基片的净尺寸制备,不需后续机械加工便可直接用于后续覆铜工艺。
较佳的,步骤(1)中,所述烧结助剂为稀土氧化物和碱土金属氧化物,加入量为氮化硅粉、硅粉氮化形成的氮化硅、和烧结助剂的总质量的4.0~5.0wt%。优选地,所述稀土氧化物含有Y 2O 3,所述碱土金属氧化物含有MgO。较佳的,步骤(1)中,所述分散剂选自聚乙二醇(PEG)、磷酸三乙酯(TEP)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%。较佳的,步骤(1)中,所述消泡剂可为油酸,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%。较佳的,步骤(1)中,所述粘结剂可为聚乙烯醇缩丁醛(PVB),加入量为氮化硅粉、硅粉 完全氮化形成的氮化硅和烧结助剂总质量的5~9wt%。较佳的,步骤(1)中,所述增塑剂选自邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、聚乙二醇(PEG)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的2~6wt%。
较佳的,步骤(1)中,所述保护气氛为氮气气氛或惰性气氛,保护气氛的压力为0.1MPa。较佳的,步骤(1)中,所述混合的方式为球磨混合,所述球磨混合的转速为30~100转/分钟,总时间为6~24小时;所述真空脱气的真空度为-0.1~-10kPa,时间为6~24小时。又,较佳的,步骤(1)中,先将氮化硅粉和硅粉中至少一种、烧结助剂、分散剂和消泡剂球磨混合3~12小时后,再加入粘结剂和增塑剂继续球磨混合3~12小时,得到所述混合浆料。
较佳的,步骤(2)中,当流延成型时,所述氮气气氛的压力为0.1~0.2MPa。较佳的,步骤(2)中,当进行干燥时,所述氮气气氛为流动的氮气,压力为0.1~0.2MPa,温度为40~85℃,干燥的总时间为15~60分钟;优选地,采用至少两个阶段的方式进行干燥,且后一个阶段的氮气温度>前一个阶段的氮气温度;更优选,阶段数为3个,包括:第一阶段的温度为40~60℃、干燥时间为5~20分钟,第二阶段的温度范围为55~70℃、干燥时间为5~20分钟,第三阶段的温度范围为65~85℃、干燥时间为5~20分钟,且第一阶段的温度<第二阶段的温度<第三阶段的温度。
较佳的,步骤(3)中,所述整形预处理为采用冷等静压的方式处理第一素坯;所述冷等静压的压力为40~200MPa,时间为2~10分钟。较佳的,步骤(4)中,所述微正压的氮气气氛的气氛压力为0.1~0.2MPa;所述脱粘的时间为1~3小时。
较佳的,当原始粉体中含有硅粉时,硅粉的质量不低于原始粉体质量的75%,其中原始粉体质量为氮化硅粉体和硅粉完全氮化之后所生成氮化硅的质量总和;优选地,在气压烧结之前,将第三素坯进行氮化处理,所述氮化处理的参数包括:氮气气氛为氢气含量不高于5vol%的氢气/氮气混合气氛,气体的压力为0.1~0.2MPa,氮化处理温度为1350~1450℃,氮化处理时间为3~6小时。
较佳的,步骤(5)中,所述气压烧结中氮气气氛的压力为0.5~10MPa;所述气压烧结的保温时间为4~12小时。又,较佳的,所述气压烧结所用坩埚得高纯BN坩埚或表面附着有高纯BN隔离层的石墨坩埚。其中高纯BN坩埚的纯度>99%。高纯BN隔离层的纯度>99%。
再一方面,本发明提供了一种根据上述制备方法制备的高热导、净尺寸氮化硅陶瓷基片,所述高热导、净尺寸氮化硅陶瓷基片厚度为0.2~1.0mm,厚度均匀性为±0.04mm, 平面度为0~0.002mm/mm,表面粗糙度为0.3~0.8μm;所述氮化硅陶瓷基片的热导率大于80W·m -1·K -1。当基片的平面度、厚度均匀性及其表面粗糙度分别控制在0.002mm/mm、±0.04mm以及0.3~0.8μm范围时,就可以不需机械加工、直接用于后续覆铜工艺。
较佳的,所述氮化硅陶瓷基片的尺寸至少为90mm×90mm,优选为(114~140)mm×(114~190)mm。
有益效果:
本发明的显著特征在于,所制备的氮化硅陶瓷基片可实现烧结尺寸和表面质量的精密控制,不需后续加工便可以直接使用,具有制备工艺简单、经济实用的特点。本发明的另一个显著特征在于,通过控制制备工艺过程中的氧化和杂质引入,实现氮化硅陶瓷基片的高热导性能。
附图说明
图1为实施例1制备的氮化硅陶瓷基片。
图2为实施例1制备的氮化硅陶瓷基片的微观结构。
图3为对比例3制备的氮化硅陶瓷基片。
图4为对比例5制备的氮化硅陶瓷基片。
图5中表1为本发明制备的氮化硅陶瓷基片的工艺参数。
图6中表2为本发明制备的氮化硅陶瓷基片的性能参数。
具体实施方式
以下通过下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。
在本公开中,通过流延成型制备工艺过程中浆料制备、真空脱气、流延成型、素坯干燥、素坯整形、脱粘和烧结工艺的设计与调控,解决了氮化硅陶瓷基片的易起泡、开裂、变形、厚度不均匀等难题,实现厚度均匀、无表面气孔与色斑、不需后续机械加工、可以直接用于后续覆铜工艺的氮化硅陶瓷基片的制备。以下示例性地说明高热导、净尺寸氮化硅陶瓷基片的制备方法。
无团聚、无气泡浆料的制备。将氮化硅粉和硅粉中至少一种、烧结助剂、分散剂、消泡剂、粘结剂和增塑剂在保护气氛(例如N 2气氛,压力可为0.1MPa)下的球磨混料后,再进行真空脱气,制备出无团聚、无气泡的混合浆料。球磨过程中,采用氮化硅陶瓷研磨球。其中烧结助剂可为稀土氧化物和碱土金属氧化物。所述稀土氧化物至少含有Y 2O 3,所述碱土金属氧化物至少含有MgO。所述稀土氧化物和碱土金属氧化物之间的摩尔比可为 (1.0~1.4):(2.5~2.9)。其中当含有硅粉时,所述硅粉含量可为75~100wt%。对制备的浆料进行抽真空除气泡处理,真空度可为-0.1~-10kPa,脱气时间可为6~24h。
厚度均匀、表面无气泡的流延膜素坯制备。在N 2气氛(0.1~0.2MPa)下流延成型。在流动热N 2气氛(流速可为10~1000升/分钟)下进行干燥,实现厚度均匀、表面无气泡的流延膜素坯的制备。作为一个示例,在N 2气氛下采用圆筒形刮刀流延成型,并通过控制刮刀高度实现对流延膜素坯厚度的调节。采用温度递增的流动热N 2气氛对流延膜素坯进行干燥,热N 2气氛的温度范围可为40~85℃,气氛压力可为0.1~0.2MPa。例如,通过温度阶段数为2个,包括:第一阶段的温度可为40~65℃、干燥时间为15~30分钟,第二阶段的温度范围可为60~85℃、干燥时间为15~30分钟,且第一阶段的温度<第二阶段的温度。例如,通过温度阶段数为3个,包括:第一阶段的温度可为40~60℃、干燥时间可为5~20分钟,第二阶段的温度范围可为55~70℃、干燥时间可为5~20分钟,第三阶段的温度范围可为65~85℃、干燥时间可为5~20分钟,且第一阶段的温度<第二阶段的温度<第三阶段的温度。
流延膜素坯的整形预处理。在一定压力(40~200MPa)条件下,对切割后的流延膜素坯(基片素坯)进行冷等静压整形预处理,保证流延膜的厚度均匀性和平整度。其中,整形预处理的时间可为2~10分钟。
基片素坯的脱粘。在微正压、一定温度条件下对基片素坯进行热处理。作为一个示例,通过通入N 2气氛产生微正压,气氛压力可为0.1~0.2MPa,处理温度为500~900℃,处理时间为1~3h。
基片素坯的氮化。当原始粉体中含有硅粉时,硅粉的质量不低于原始粉体质量的75%,其中原始粉体质量为氮化硅粉体和硅粉完全氮化之后所生成氮化硅的质量总和。而且,当原始粉体中含有硅粉时,在氢气含量不高于5vol%的氢气/氮气混合气氛、一定温度条件下对基片素坯进行氮化处理。作为一个示例,在氢气含量不高于5vol%的氢气/氮气混合气氛,气氛压力可为0.1~0.2MPa,氮化处理温度可为1350~1450℃,氮化处理时间可为3~6小时。
基片素坯的烧结。在高压N 2气氛条件下进行气压烧结。作为一个示例,基片素坯的烧结,置于BN坩埚中、在高压N 2气氛条件下进行气压烧结,其中N 2气氛压力优选为0.5~10MPa,在此范围内更有利于提高材料的力学/热学/电学性能、降低基片表面的粗糙度。烧结温度可为1800~2000℃,保温时间可为4~12小时。
综上所述,本发明中高热导、净尺寸氮化硅陶瓷基片的制备过程全部是在氮气气氛 中进行。采用千分尺测试所得氮化硅陶瓷基片的厚度均匀性为±0.04mm。采用轮廓仪测试所得氮化硅陶瓷基片的平面度可为0~0.002mm/mm。采用轮廓仪测试所得氮化硅陶瓷基片的表面粗糙度可为0.3~0.8μm。采用激光导热仪测试所得氮化硅陶瓷基片的所述氮化硅陶瓷基片的热导率大于80W·m -1·K -1
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
实施例1
首先,将起始陶瓷粉体(氮化硅95g)、烧结助剂(5g,Y 2O 3:MgO=1.2:2.5,摩尔比)、消泡剂(油酸,0.5g)、分散剂(PEG,0.5g)、研磨球(氮化硅球,200g)、有机溶剂(无水乙醇,80g)置入密封的尼龙材质球磨罐中,抽真空后通入N 2气氛保护,在100rpm下球磨混料4h;在上述浆料中进一步加入粘结剂(PVB,7g)和增塑剂(DBP,4g),继续在N 2气氛保护下球磨8h后得到分散均匀、无团聚的浆料。其次,对制备的浆料进行抽真空除气泡处理12h,真空度为-0.5kPa。随后,在N 2保护气氛下采用圆筒形刮刀对上述除气泡后的浆料进行流延成型,通过控制刮刀高度使流延膜素坯厚度精确控制在0.4±0.04mm。采用流动的温度递增的热N 2气氛(流速为100升/分钟)对流延膜素坯进行干燥,N 2气氛压力为0.1MPa,温度递增的热N 2气氛包括温度分别为45℃(8分钟)、65℃(8分钟)和80℃(8分钟)等前、中、后三段组成。采用自动切片机切割成143.0mm×143.0mm的方片,并在100MPa下冷等静压整形处理5分钟。将整形后基片素坯在0.15MPa的N 2气氛下700℃保温2h脱粘。将脱粘后的基片素坯装入高纯度BN坩埚(纯度>99%)后再放入气压烧结炉中,在5MPa的N 2气氛下1900℃保温10h烧结后,随炉冷却至室温。
本实施例1中制备的氮化硅陶瓷基片见图1,尺寸为114.4mm×114.4mm,尺寸偏差为±0.1mm,厚度为0.32±0.02mm,平面度为0.2mm,表面粗糙度为0.4μm。材料的热导率为95W/(m·K),弯曲强度为780MPa。该基片无需后续机械加工,可以直接用于后续的覆铜工艺。其断面微观结构见图2,微观结构均匀、致密。
实施例2-5
原料配比与组成、工艺过程参照实施例1,浆料制备、真空脱气、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照图5中表1所示,所制备基片材料特性如图6中表2所示。
实施例6
首先,将起始陶瓷粉体(氮化硅3g、硅粉55g)、烧结助剂(4.5g,Y 2O 3:MgO=1.1:2.9,摩尔比)、消泡剂(油酸,0.3g)、分散剂(PEG,0.3g)、研磨球(氮化硅球,120g)、有机溶剂(无水乙醇,50g)置入密封的尼龙材质球磨罐中,抽真空后通入N 2气氛保护,在100rpm下球磨混料4h;在上述浆料中进一步加入粘结剂(PVB,5g)和增塑剂(DBP,3g),继续在N 2气氛保护下球磨8h后得到分散均匀、无团聚的浆料。其次,对制备的浆料进行抽真空除气泡处理12h,真空度为-0.5kPa。随后,在N 2保护气氛下采用圆筒形刮刀对上述除气泡后的浆料进行流延成型,通过控制刮刀高度使流延膜素坯厚度精确控制在0.5±0.05mm。采用流动的温度递增的热N 2气氛(流速为50升/分钟)对流延膜素坯进行干燥,N 2气氛压力为0.2MPa,温度递增的热N 2气氛包括温度分别为45℃(6分钟)、65℃(6分钟)和80℃(6分钟)等前、中、后三段组成。采用自动切片机切割成142.6mm×194.4mm的方片,并在150MPa下冷等静压整形处理3分钟。将整形后基片素坯在0.15MPa的N 2气氛下700℃保温2h脱粘。将脱粘后基片素坯在0.2MPa N 2(含有5%H 2)气氛下1450℃氮化处理6h。将氮化处理后的基片素坯装入高纯度BN坩埚(纯度>99%)后再放入气压烧结炉中,在5MPa的N 2气氛下1900℃保温10h烧结后,随炉冷却至室温。所制备基片材料特性如表2所示。
实施例7-9
原料配比与组成、工艺过程参照实施例6,浆料制备、真空脱气、流延成型、素坯整形、脱粘、氮化处理和烧结工艺等具体参数按照表1所示,所制备基片材料特性如表2所示。
实施例10
本实施例10中氮化硅陶瓷基片的制备过程参照实施例1,区别在于:采用自动切片机切割成200mm×200mm的方片,并在100MPa下冷等静压整形。
实施例11
本实施例11中氮化硅陶瓷基片的制备过程参照实施例6,区别在于:采用自动切片机切割成200mm×200mm的方片,并在100MPa下冷等静压整形。
对比例1
原料配比与组成、浆料制备、真空脱气、流延成型、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:未进行素坯整形预处理。所制备基片材料特性如表2所示。因未对流延成型基片素坯进行等静压整形预处理,所制备基片的厚度均匀性和平面度明显降低,热导率也有些微降低。
对比例2
原料配比与组成、浆料制备、真空脱气、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:未采用高氮气压力进行高温烧结,仅采用0.1MPa的N 2保护气氛。所制备基片材料特性如表2所示。因未采用高氮气气氛的气压烧结,所制备基片的表面粗糙度明显增大,不能满足后续覆铜工艺对基片表面粗糙度的要求。
对比例3
原料配比与组成、浆料制备、真空脱气、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:未采用微正压脱粘(采用真空条件脱粘)。所制备基片材料特性如表2所示。因采用真空脱粘,有机物在脱粘过程中分解产生气体的逸出速度不可控(过快),所制备基片表面局部存在微裂纹缺陷(见图3)。
对比例4
原料配比与组成、浆料制备、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:未采取真空脱气措施。所制备基片材料特性如表2所示。因未采用真空脱气措施,浆料中存在少量气泡,所制备基片表面局部存在小气泡缺陷。
对比例5
原料配比与组成、浆料制备、真空脱气、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:未采用高纯度BN坩埚作为氮化硅基片素坯高温烧结用容器,而是直接置于石墨坩埚中。所制备基片材料特性如表2所示。因未采用高纯度BN坩埚,石墨坩埚容易污染基片,所制备基片表面均匀性较差,存在局部色斑缺陷(见图4)。
对比例6
原料配比与组成、浆料制备、真空脱气、流延成型、素坯整形、脱粘和烧结工艺等具体参数按照表1所示,工艺过程参照实施例1,区别在于:在浆料球磨过程中采用空气气氛。因为未采用氮气气氛保护,氮化硅粉体原料在球磨过程中产生了一定程度的氧化,导致所制备氮化硅陶瓷基片的热导率偏低。

Claims (15)

  1. 一种高热导、净尺寸氮化硅陶瓷基片的制备方法,其特征在于,包括:
    (1)将选自氮化硅粉和硅粉中至少一种的原始粉体、烧结助剂、分散剂、消泡剂、粘结剂和增塑剂在保护气氛中混合后,再经真空脱气,得到混合浆料;所述真空脱气的真空度为-0.1~-10kPa,时间为6~24小时;
    (2)在氮气气氛中进行流延成型和干燥,得到第一素坯;所述干燥为采用温度递增的流动热N 2气氛进行干燥;
    (3)将所得第一素坯进行整形预处理,得到第二素坯,所述整形预处理为采用冷等静压的方式处理第一素坯;
    (4)将所得第二素坯在微正压的氮气气氛中、500~900℃下进行脱粘,得到第三素坯,所述微正压的氮气气氛的气氛压力为0.12~0.2MPa;所述脱粘的时间为1~3小时;
    (5)将所得第三素坯置于氮气气氛中、1800~2000℃下进行气压烧结,得到所述高热导、净尺寸氮化硅陶瓷基片;所述气压烧结所用坩埚为高纯BN坩埚或表面附着有高纯BN隔离层的石墨坩埚。
  2. 根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述烧结助剂为稀土氧化物和碱土金属氧化物,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂的总质量的4.0~5.0wt%;
    所述分散剂选自聚乙二醇(PEG)、磷酸三乙酯(TEP)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%;
    所述消泡剂为油酸,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的0.2~1.0wt%;
    所述粘结剂为聚乙烯醇缩丁醛(PVB),加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的5~9wt%;
    所述增塑剂选自邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)和聚乙二醇(PEG)中的至少一种,加入量为氮化硅粉、硅粉完全氮化形成的氮化硅和烧结助剂总质量的2~6wt%。
  3. 根据权利要求2所述的制备方法,其特征在于,所述稀土氧化物含有Y 2O 3,所述碱土金属氧化物含有MgO。
  4. 根据权利要求1或2所述的制备方法,其特征在于,步骤(1)中,所述保护气氛为氮气气氛或惰性气氛,保护气氛的压力为0.1MPa;所述混合的方式为球磨混合,所述球磨混合的转速为30~100转/分钟,总时间为6~24小时。
  5. 根据权利要求4所述的制备方法,其特征在于,先将氮化硅粉和硅粉中至少一种、烧结助剂、分散剂和消泡剂球磨混合3~12小时后,再加入粘结剂和增塑剂继续球磨混合3~12小时,得到所述混合浆料。
  6. 根据权利要求1所述的制备方法,其特征在于,步骤(2)中,当流延成型时,所述氮气气氛的压力为0.1~0.2MPa;
    当进行干燥时,所述氮气气氛为流动的氮气,压力为0.1~0.2MPa,温度为40~85℃,干燥的总时间为15~60分钟。
  7. 根据权利要求6所述的制备方法,其特征在于,采用至少两个阶段的方式进行干燥,且后一个阶段的氮气温度>前一个阶段的氮气温度。
  8. 根据权利要求7所述的制备方法,其特征在于,阶段数为3个,包括:第一阶段的温度为40~60℃、干燥时间为5~20分钟,第二阶段的温度范围为55~70℃、干燥时间为5~20分钟,第三阶段的温度范围为65~85℃、干燥时间为5~20分钟,且第一阶段的温度<第二阶段的温度<第三阶段的温度。
  9. 根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述冷等静压的压力为40~200MPa,时间为2~10分钟。
  10. 根据权利要求1所述的制备方法,其特征在于,当原始粉体中含有硅粉时,硅粉的质量不低于原始粉体质量的75%,其中原始粉体质量为氮化硅粉体和硅粉完全氮化之后所生成氮化硅的质量总和。
  11. 根据权利要求10所述的制备方法,其特征在于,在气压烧结之前,将第三素坯进行氮化处理,所述氮化处理的参数包括:氮气气氛为氢气含量不高于5vol%的氢气/氮气混合气氛,气体的压力为0.1~0.2MPa,氮化处理温度为1350~1450℃,氮化处理时间为3~6小时。
  12. 根据权利要求1所述的制备方法,其特征在于,步骤(5)中,所述气压烧结中氮气气氛的压力为0.5~10MPa;所述气压烧结的保温时间为4~12小时。
  13. 一种根据权利要求1-12中任一项所述的制备方法制备的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述高热导、净尺寸氮化硅陶瓷基片厚度为0.2~1.0mm,厚度均匀性为±0.04mm,平面度为0~0.002mm/mm,表面粗糙度为0.3~0.8μm;所述氮化硅陶瓷基片的热导率大于80W·m -1·K -1
  14. 根据权利要求13所述的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述氮化硅陶瓷基片的尺寸至少为90mm×90mm。
  15. 根据权利要求14所述的高热导、净尺寸氮化硅陶瓷基片,其特征在于,所述氮化硅陶瓷基片的尺寸至少为(114~140)mm×(114~190)mm。
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