WO2022100249A1 - 一种高性能氮化铝陶瓷基板的浆料和制备方法 - Google Patents

一种高性能氮化铝陶瓷基板的浆料和制备方法 Download PDF

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WO2022100249A1
WO2022100249A1 PCT/CN2021/117499 CN2021117499W WO2022100249A1 WO 2022100249 A1 WO2022100249 A1 WO 2022100249A1 CN 2021117499 W CN2021117499 W CN 2021117499W WO 2022100249 A1 WO2022100249 A1 WO 2022100249A1
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aluminum nitride
slurry
ceramic substrate
nitride ceramic
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伍尚华
林坤吉
丁达飞
林立甫
黎业华
盛鹏飞
李建斌
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Guangdong University of Technology
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Definitions

  • the invention relates to the technical field of preparation of aluminum nitride ceramic substrates, in particular to a slurry of high-performance aluminum nitride ceramic substrates and a preparation method.
  • Aluminum nitride (A1N) is a covalent bond compound with a hexagonal wurtzite structure. It has high thermal conductivity, good high temperature insulation and dielectric properties, high material strength at high temperature, and thermal expansion coefficient that matches semiconductor silicon materials. A series of advantages such as non-toxicity have made it an ideal heat dissipation material for electronic packaging and high-performance ceramic substrate materials for assembling ultra-large-scale integrated circuits.
  • the main preparation method of aluminum nitride ceramic substrates is tape casting, and most of them are organic tape casting. Because aluminum nitride is easily hydrolyzed, it is difficult to control various variables in water-based tape casting. Realize large-scale, continuous production. However, organic tape casting adopts organic solvents with certain toxicity (benzene, toluene, xylene, acetone, butanone, etc.), which are flammable and cause great pollution to the environment and endanger human health.
  • the technical problem to be solved by the present invention is to reduce the pollution of the aluminum nitride ceramic substrate tape casting process, and to solve the problems that the current aluminum nitride ceramic substrate is soft and difficult to process.
  • the technical scheme adopted in the present invention is:
  • a slurry for a high-performance aluminum nitride ceramic substrate is composed of the following components in parts by mass: 100 parts of aluminum nitride powder, 1-8 parts of sintering aid, 0.1-4 parts of Sialon particles, 1- 6 parts of dispersant, 38-68 parts of solvent, 3-12 parts of binder and 3-10 parts of plasticizer;
  • the sintering aid is composed of the following components by mass: 0-8 parts of Y 2 O 3 , 0-5 parts of Sm 2 O 3 , 0-1 part of La 2 O 3 and 0.05-3 parts of metal aluminum powder;
  • the solvent is anhydrous ethanol, isopropanol and n-butanol. one or more.
  • the sintering aid is composed of the following components in parts by mass: 1-6 parts of Y 2 O 3 , 0-5 parts of Sm 2 O 3 , 0-1 parts of La 2 O 3 and 0.05-3 parts of La 2 O 3 metal aluminum powder.
  • the particle size of the metal aluminum powder is 2-3 ⁇ m.
  • the dispersant is one or more of triethyl phosphate, castor oil and glyceryl trioleate
  • the binder is polyvinyl butyral
  • the plasticizer is phthalic acid Butyl benzyl ester.
  • a preparation method of a high-performance aluminum nitride ceramic substrate comprising the following steps performed in sequence:
  • defoaming add 0.1-2 parts by mass of defoaming agent to the slurry, remove the foam under vacuum negative pressure for 10-50min, and then filter to obtain a casting slurry;
  • S3 Tape casting: transfer the casting slurry to a casting machine to form a blank strip, and then dry the blank strip and punch and cut it to form a blank;
  • the process of the vacuum debinding treatment is as follows: in the vacuum debinding furnace, the temperature is first heated from room temperature to 200-250° C., maintained for 0.5-2 hours, and then heated to 300-350° C. for 0.5-2 hours, and finally The temperature is raised to 500-650°C, and the temperature is kept for 1-5h; the process of the air debinding treatment is: in the air debinding furnace, the temperature is raised to 250-350°C, and the temperature is kept for 0.5-4h; the heating rate of the vacuum debinding treatment The temperature is 0.5-4°C/min, and the heating rate of the air debinding treatment is 0.5-4°C/min.
  • the green body is first cooled to room temperature.
  • isostatic pressing is as follows: under the conditions of a pressure of 90-200 MPa and a temperature of 25-100° C., isostatic pressing for 5-30 minutes.
  • the viscosity of the slurry is 7000-14500cps;
  • the Sialon ceramic ball contains at least 39wt% ⁇ Sialon phase;
  • the defoaming agent is composed of n-butanol and ethylene glycol in a mass ratio of 1:1 It is formed by mixing the proportions of 1 to 3; when casting, the height of the scraper is 0.3 to 0.9 mm, and the speed of the casting belt is 1 to 5 m/min.
  • the beneficial effects of the invention are as follows: the sialon particles are dispersed in the slurry system to play a toughening role; the multi-component sintering aids help to reduce the sintering temperature and promote the sintering compact; the metal aluminum powder can react with oxygen impurities, effectively improving the
  • the thermal conductivity is conducive to the formation of aluminum nitride in a nitrogen atmosphere, and further promotes sintering and densification.
  • non-toxic, low-toxic, low-cost solvents such as alcohols to replace toxic solvents such as benzene and ketones solves the problem that the preparation of aluminum nitride ceramics is unfriendly to humans and the environment.
  • the key idea of the present invention is to use rare earth metals, Group IIA metals or Group IIIA metals and their oxides, and metal aluminum powder as sintering aids, and use SiAlON ceramic balls as ball milling balls, and introduce them by ball milling.
  • Sialon particles are dispersed and toughened to prepare aluminum nitride ceramic substrates with high thermal conductivity and high flexural strength.
  • non-toxic, low-toxic and low-cost solvents such as alcohols are used to replace toxic solvents such as benzene and ketones to solve nitrogen problems.
  • the preparation of aluminide ceramics is not friendly to people and the environment. By isostatic pressing, the aluminum nitride cast blank is secondary molded to promote the densification of sintering.
  • a slurry for a high-performance aluminum nitride ceramic substrate is composed of the following components in parts by mass: 100 parts of aluminum nitride powder, 1-8 parts of sintering aid, 0.1-4 parts of Sialon particles, 1- 6 parts of dispersant, 38-68 parts of solvent, 3-12 parts of binder and 3-10 parts of plasticizer;
  • the sintering aid is composed of the following components by mass: 0-8 parts of Y 2 O 3 , 0-5 parts of Sm 2 O 3 , 0-1 part of La 2 O 3 and 0.05-3 parts of metal aluminum powder;
  • the solvent is anhydrous ethanol, isopropanol and n-butanol. one or more.
  • the sintering aid is composed of the following components by mass: 1-6 parts of Y 2 O 3 , 0-5 parts of Sm 2 O 3 , 0-1 parts of La 2 O 3 and 0.05-3 parts of La 2 O 3 metal aluminum powder.
  • the dispersant is one or more of triethyl phosphate, castor oil and glyceryl trioleate, the binder is polyvinyl butyral, and the plasticizer is butyl benzyl phthalate .
  • Sialon particles are dispersed in the slurry system and play a toughening role.
  • the toughening mechanisms such as crack deflection, crack bridging and residual stress, the mechanical properties of aluminum nitride ceramic substrates can be effectively improved; multiple sintering aids help reduce The sintering temperature promotes sintering and densification; 2-3 ⁇ m metal aluminum powder can react with oxygen impurities to effectively improve thermal conductivity, which is conducive to the formation of aluminum nitride under nitrogen atmosphere, and further promotes sintering and densification.
  • non-toxic, low-toxic, low-cost solvents such as alcohols to replace toxic solvents such as benzene, ketones, etc.
  • the dispersant disperses the powder in the slurry uniformly through steric hindrance.
  • a preparation method of a high-performance aluminum nitride ceramic substrate comprising the following steps performed in sequence:
  • S3 Tape casting: transfer the casting slurry to a casting machine to form a blank strip, and then dry the blank strip and punch and cut it to form a blank.
  • a preparation method of a high-performance aluminum nitride ceramic substrate comprising the following steps performed in sequence:
  • the sialon ceramic ball contains at least 39 wt % of the alpha sialon phase.
  • the Sialon particles introduced by ball milling are used as a dispersion and toughening system, which can effectively improve the mechanical properties of aluminum nitride ceramics and maintain high thermal conductivity.
  • the addition process is simple and low in cost.
  • Defoaming add 0.1-2 parts by mass of a defoaming agent to the slurry, and filter to obtain a casting slurry after vacuum negative pressure defoaming for 10-50 min;
  • the defoaming agent is composed of n-butanol, ethylene glycol according to The mass ratio of 1:1 is mixed to form;
  • S3 Tape casting: transfer the casting slurry to a casting machine, and cast a blank strip under the conditions of a blade height of 0.3-0.9 mm and a casting belt speed of 1-5 m/min to obtain a blank strip, and the blank strip is dried and punched , Cut to form a blank.
  • Pretreatment of the green body After the green body is stacked, firstly, under the conditions of a pressure of 90-200 MPa and a temperature of 25-100 °C, isostatic pressing is carried out for 5-30 minutes; In the glue furnace, the temperature is first raised from room temperature to 200-250°C, kept for 0.5-2h, then heated to 300-350°C, kept for 0.5-2h, and finally heated to 500-650°C, kept for 1-5h, and the heating rate is 0.5 ⁇ 4°C/min; cool the green body to room temperature, and then transfer it to the air debinding furnace for air debinding treatment: raise the temperature to 250-350°C, keep the temperature for 0.5 ⁇ 4h, and the heating rate is 0.5 ⁇ 4°C/min, and finally obtain The body to be sintered.
  • the green body has a higher density, which is conducive to the subsequent preparation of high-performance sintered bodies; the two-step debinding method is used to effectively avoid oxidation of the added metal aluminum powder, reduce the introduction of impurity oxygen, and segment
  • the heating method can better remove the remaining organic matter of the green body, effectively avoid the deformation and cracking of the green body, and improve the sintering quality of the aluminum nitride ceramic substrate.
  • Sialon ceramic balls were used as ball-milling balls, and Sialon particles were introduced by ball milling. During filtration, Sialon ceramic balls and a small amount of larger particles were removed. Due to the difference between the ball milling time and the ball milling speed, it is found that the filtered Sialon ceramic balls have a loss of 0.1-4 parts by mass, so in the present invention, 0.1-4 parts by mass of Sialon particles are introduced into the slurry by ball milling.
  • the Sialon ceramic ball contains at least 39 wt % of ⁇ -Sialon phase, and also includes ⁇ -phase Si 3 N 4 and a small amount of YAG phase.
  • test examples In order to further discuss the beneficial effects of the present invention, further description is made according to the following test examples, comparative examples and corresponding test results:
  • a preparation method of a high-performance aluminum nitride ceramic substrate comprising the following steps performed in sequence:
  • defoaming add 0.4 parts by mass of defoaming agent to the slurry, defoaming under the condition of vacuum-0.1MPa for 30min, and filter to obtain a casting slurry; after filtration, it is found that the loss of 0.3 parts by mass of Sialon ceramic balls;
  • the green body to be sintered is placed in a flowing nitrogen environment, and sintered at 1850° C. for 4 hours to obtain an aluminum nitride ceramic substrate.
  • a preparation method of an aluminum nitride ceramic substrate is different from that of Test Example 1 in that the ball mill uses zirconia balls instead of Sialon ceramic balls.
  • a preparation method of a high-performance aluminum nitride ceramic substrate the difference from Test Example 1 is that the sintering aid consists of 2.5 parts of Y 2 O 3 , 2.5 parts of La 2 O 3 and 0.3 parts of metal powder.
  • a commercially available aluminum nitride ceramic substrate was used as Comparative Example 2.
  • test examples 1-2 and comparative examples 1-2 are tested: the density of the sample is measured by the Archimedes drainage method; the bending strength of the sample is measured by the three-point bending test; the thermal conductivity of the sample is measured by the flash method .
  • the data is shown in Table 1:
  • the thermal conductivity of the aluminum nitride ceramic substrate prepared by the present invention is almost the same as that of the commercially available aluminum nitride substrate, while the bending strength is increased by nearly 30%, and the density is high and uniform. , which solves the difficult problems of the current aluminum nitride ceramic substrate being soft, difficult to process, and relatively polluting the environment.
  • Sialon ceramic balls are used as ball milling balls, and Sialon particles introduced by ball milling are used as a dispersion and toughening system, which effectively improves the mechanical properties of aluminum nitride ceramics and maintains high thermal conductivity. .
  • the process for adding Sialon particles is simple and low in cost.
  • the slurry and preparation method of a high-performance aluminum nitride ceramic substrate provided by the present invention have the following effects: (1)
  • the use of multi-component sintering aids and the addition of metal aluminum powder can greatly reduce impurity oxygen
  • the introduction of sintering temperature reduces the sintering temperature and promotes sintering densification, which is beneficial to improve the thermal conductivity and mechanical properties of aluminum nitride ceramics;
  • the Sialon particles introduced by ball milling are used as a dispersion toughening system, which can effectively improve the aluminum nitride ceramics.

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Abstract

提供一种高性能氮化铝陶瓷基板的浆料和制备方法，浆料由以下质量份组分组成：100份的氮化铝粉体、1－8份的烧结助剂、0.1－4份的赛隆颗粒、1－6份的分散剂、38－68份的溶剂、3－12份的粘结剂和3－10份的增塑剂；烧结助剂由以下质量份组分组成：0－8份的Y 2O 3、0－5份的Sm 2O 3、0－1份的La 2O 3和0.05－3份的金属铝粉；溶剂为无水乙醇、异丙醇、正丁醇中的一种或几种。赛隆颗粒弥散在浆料体系中，起到增韧作用；多元的烧结助剂有助于降低烧结温度，促进烧结致密；金属铝粉可与氧杂质反应，有效提高热导率，在氮气氛围下有利于氮化铝的生成，进一步促进烧结致密化。应用醇类等无毒、低毒、低成本溶剂代替苯类、酮类等有毒溶剂，解决氮化铝陶瓷制备对人和环境不友好的问题。

Description

一种高性能氮化铝陶瓷基板的浆料和制备方法 技术领域
本发明涉及氮化铝陶瓷基板制备技术领域，尤其是指一种高性能氮化铝陶瓷基板的浆料和制备方法。
背景技术
随着大功率和超大规模集成电路的发展，集成电路和基板之间的散热要求越来越高，因此基板材料需要具有较高的热导率和电阻率。
氮化铝(A1N)是一种六方纤锌矿结构的共价键化合物，以热导率高、高温绝缘性和介电性能好、高温下材料强度大、热膨胀系数与半导体硅材料相匹配、无毒等一系列优点，成为了理想的电子封装散热材料以及组装超大规模集成电路的高性能陶瓷基板材料。
目前，氮化铝陶瓷基板的主要制备方法是流延成型，且绝大数为有机流延成型，因为氮化铝具有易水解性，在水基流延成型中各种变量难以把控，难以实现大规模、连续性生产。但有机流延成型采用的是具有一定毒性的有机溶剂(苯、甲苯、二甲苯、丙酮、丁酮等)，易燃且对环境的污染较大，危害人体健康。此外，目前大部分有关于氮化铝流延成型的研究都注重于提升氮化铝陶瓷的热导率，而对于其力学性能的研究比较少；在改善氮化铝陶瓷力学性能的同时，却忽略了对氮化铝陶瓷热导率的影响。
发明内容
本发明所要解决的技术问题是：降低氮化铝陶瓷基板流延成型工艺的污染问题，解决目前氮化铝陶瓷基板基板偏软、加工困难的问题。
为了解决上述技术问题，本发明采用的技术方案为：
一种高性能氮化铝陶瓷基板的浆料，由以下质量份组分组成：100份的氮化铝粉体、1-8份的烧结助剂、0.1-4份的赛隆颗粒、1-6份的分散剂、38-68份的溶剂、3-12份的粘结剂和3-10份的增塑剂；所述烧结助剂由以下质量份组分组成：0-8份的Y 2O 3、0-5份的Sm 2O 3、0-1份的La 2O 3和0.05-3份的金属铝粉；所述溶剂为无水乙醇、异丙醇、正丁醇中的一种或几种。
进一步地，所述烧结助剂由以下质量份组分组成：1-6份的Y 2O 3、0-5份的Sm 2O 3、0-1份的La 2O 3和0.05-3份的金属铝粉。
进一步地，所述烧结助剂中Y 2O 3、Sm 2O 3和金属铝粉按照Y 2O 3：Sm 2O 3：金属铝粉＝1：(0.1-0.5)：(0.1-0.5)的比例混合；所述金属铝粉的粒径为2-3μm。
进一步地，所述溶剂由无水乙醇与正丁醇按照无水乙醇：正丁醇＝1:1的比例混合形成，或由异丙醇与正丁醇按照异丙醇：正丁醇＝1:1的比例混合形成。
进一步地，所述分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的一种或几种，所述粘结剂为聚乙烯醇缩丁醛，增塑剂为邻苯二甲酸丁苄酯。
一种高性能氮化铝陶瓷基板的制备方法，包括依次执行的以下步骤：
S1：配制权利要求1至5任一所述的高性能氮化铝陶瓷基板的浆料：按照所需质量份将氮化铝粉体、烧结助剂、分散剂和溶剂加入到球磨罐中，按照氮化铝粉体：赛隆陶瓷球＝1:1-6的比例往球磨罐中加入赛隆陶瓷球，在球磨转速为250-500r/min的条件下，球磨6-20h后再加入粘结剂和增塑剂，继续球磨6-20h得到浆料；
S2：除泡：往浆料中加入0.1-2质量份的除泡剂，真空负压除泡10-50min后过滤得到流延浆料；
S3：流延成型：将流延浆料转至流延机上成型得到坯带，将坯带干燥后冲压、裁切形成坯体；
S4：坯体预处理：所述坯体层叠后，先经过等静压处理，然后依次进行真空排胶处理、空气排胶处理，最后得到待烧结坯体；
S5：将待烧结坯体置于流动氮气环境中，在1650-1850℃条件下烧结2-8h,得到氮化铝陶瓷基板。
进一步地，所述真空排胶处理的过程为：在真空排胶炉中，先从室温升温至200-250℃，保温0.5～2h，然后再升温至300-350℃，保温0.5～2h，最后升温至500～650℃，保温1～5h；所述空气排胶处理的过程为：在空气排胶炉中，升温至250-350℃，保温0.5～4h；所述真空排胶处理的升温速率为0.5～4℃/min，所述空气排胶处理的升温速率为0.5～4℃/min。
进一步地，将坯体从真空排胶炉中转至空气排胶炉前，先将坯体降温至室 温。
进一步地，所述等静压处理为：在压力为90～200MPa、温度为25～100℃的条件下，等静压压制5～30min。
进一步地，所述浆料的粘度为7000-14500cps；所述赛隆陶瓷球中包含至少39wt％的α赛隆相；所述除泡剂由正丁醇、乙二醇按照质量比1:1的比例混合形成；流延成型时，刮刀高度为0.3～0.9mm，流延带速为1～5m/min。
本发明的有益效果在于：赛隆颗粒弥散在浆料体系中，起到增韧作用；多元的烧结助剂有助于降低烧结温度，促进烧结致密；金属铝粉可与氧杂质反应，有效提高热导率，在氮气氛围下有利于氮化铝的生成，进一步促进烧结致密化。应用醇类等无毒、低毒、低成本溶剂代替苯类、酮类等有毒溶剂，解决氮化铝陶瓷制备对人和环境不友好的问题。
具体实施方式
本发明最关键的构思在于：采用稀土金属、IIA族金属或ⅢA族金属及其氧化物、金属铝粉为烧结助剂，并以赛隆(SiAlON)陶瓷球作为球磨球，通过球磨的方式引入赛隆颗粒弥散增韧，制备出高热导率、高抗弯强度的氮化铝陶瓷基板，同时应用醇类等无毒、低毒、低成本溶剂代替苯类、酮类等有毒溶剂，解决氮化铝陶瓷制备对人和环境不友好的问题。通过等静压的方式对氮化铝流延素坯进行二次成型，促进烧结的致密化。
为了进一步论述本发明构思的可行性，根据本发明的技术内容、构造特征、所实现目的及效果的具体实施方式详予说明。
实施例1
一种高性能氮化铝陶瓷基板的浆料，由以下质量份组分组成：100份的氮化铝粉体、1-8份的烧结助剂、0.1-4份的赛隆颗粒、1-6份的分散剂、38-68份的溶剂、3-12份的粘结剂和3-10份的增塑剂；所述烧结助剂由以下质量份组分组成：0-8份的Y 2O 3、0-5份的Sm 2O 3、0-1份的La 2O 3和0.05-3份的金属铝粉；所述溶剂为无水乙醇、异丙醇、正丁醇中的一种或几种。
优选地，所述烧结助剂由以下质量份组分组成：1-6份的Y 2O 3、0-5份的 Sm 2O 3、0-1份的La 2O 3和0.05-3份的金属铝粉。
更优选地，所述烧结助剂中Y 2O 3、Sm 2O 3和金属铝粉按照Y 2O 3：Sm 2O 3：金属铝粉＝1：(0.1-0.5)：(0.1-0.5)的比例混合；所述金属铝粉的粒径为2-3μm。
所述溶剂由无水乙醇与正丁醇按照无水乙醇：正丁醇＝1:1的比例混合形成，或由异丙醇与正丁醇按照异丙醇：正丁醇＝1:1的比例混合形成。
所述分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的一种或几种，所述粘结剂为聚乙烯醇缩丁醛，增塑剂为邻苯二甲酸丁苄酯。
赛隆颗粒弥散在浆料体系中，起到增韧作用，通过裂纹偏转、裂纹桥接以及残余应力等增韧机制，有效提高氮化铝陶瓷基板的力学性能；多元的烧结助剂有助于降低烧结温度，促进烧结致密；2-3μm的金属铝粉可与氧杂质反应，有效提高热导率，在氮气氛围下有利于氮化铝的生成，进一步促进烧结致密化。应用醇类等无毒、低毒、低成本溶剂代替苯类、酮类等有毒溶剂，解决氮化铝陶瓷制备对人和环境不友好的问题；此外，醇类溶剂的溶解特性好，挥发速率稳定，对坯体影响小。分散剂通过空间位阻作用使浆料中的粉体分散均匀。
实施例2
一种高性能氮化铝陶瓷基板的制备方法，包括依次执行的以下步骤：
S1：配制上述所述的高性能氮化铝陶瓷基板的浆料：按照所需质量份将氮化铝粉体、烧结助剂、分散剂和溶剂加入到球磨罐中，按照氮化铝粉体：赛隆陶瓷球＝1:1-6的比例往球磨罐中加入赛隆陶瓷球，在球磨转速为250-500r/min的条件下，球磨6-20h后再加入粘结剂和增塑剂，继续球磨6-20h得到浆料。
S2：除泡：往浆料中加入0.1-2质量份的除泡剂，真空负压除泡10-50min后过滤得到流延浆料。
S3：流延成型：将流延浆料转至流延机上成型得到坯带，将坯带干燥后冲压、裁切形成坯体。
S4：坯体预处理：所述坯体层叠后，先经过等静压处理，然后依次进行真空排胶处理、空气排胶处理，最后得到待烧结坯体。
S5：将待烧结坯体置于流动氮气环境中，在1650-1850℃条件下烧结2-8h, 得到氮化铝陶瓷基板。
实施例3
一种高性能氮化铝陶瓷基板的制备方法，包括依次执行的以下步骤：
S1：配制上述所述的高性能氮化铝陶瓷基板的浆料：按照所需质量份将氮化铝粉体、烧结助剂、分散剂和溶剂加入到球磨罐中，按照氮化铝粉体：赛隆陶瓷球＝1:1-6的比例往球磨罐中加入赛隆陶瓷球，在球磨转速为250-500r/min的条件下，球磨6-20h后再加入粘结剂和增塑剂，继续球磨6-20h得到浆料，所述浆料的粘度控制在7000-14500cps即可。
所述赛隆陶瓷球中包含至少39wt％的α赛隆相。通过球磨方式引入的赛隆颗粒作为弥散增韧体系，有效提高氮化铝陶瓷的力学性能，并保持高热导率，该添加工艺简单、成本低。
S2：除泡：往浆料中加入0.1-2质量份的除泡剂，真空负压除泡10-50min后过滤得到流延浆料；所述除泡剂由正丁醇、乙二醇按照质量比1:1的比例混合形成；
S3：流延成型：将流延浆料转至流延机上，在刮刀高度为0.3～0.9mm、流延带速为1～5m/min条件下流延成型得到坯带，将坯带干燥后冲压、裁切形成坯体。
S4：坯体预处理：所述坯体层叠后，先在压力为90～200MPa、温度为25～100℃的条件下，等静压压制5～30min；然后进行真空排胶处理：在真空排胶炉中，先从室温升温至200-250℃，保温0.5～2h，然后再升温至300-350℃，保温0.5～2h，最后升温至500～650℃，保温1～5h，升温速率为0.5～4℃/min；将坯体降温至室温，然后转入空气排胶炉进行空气排胶处理：升温至250-350℃，保温0.5～4h，升温速率为0.5～4℃/min，最后得到待烧结坯体。
通过等静压处理使坯体致密度更高，有利于后续制备高性能的烧结体；采用两步排胶法，有效避免加入的金属铝粉被氧化，减少杂质氧的引入量，且分段式升温方式能更好的排除坯体剩余的有机物，有效避免坯体变形、开裂，提高氮化铝陶瓷基板的烧结质量。
S5：将待烧结坯体置于流动氮气环境中，在1650-1850℃条件下烧结2-8h,得到氮化铝陶瓷基板。
实施例2-3中，以赛隆陶瓷球作为球磨球，通过球磨的方式引入赛隆颗粒，在过滤时，将赛隆陶瓷球以及少量粒径较大颗粒除掉。由于球磨时间与球磨转速的不同，发现过滤后的赛隆陶瓷球有0.1-4质量份的损耗，故本发明中通过球磨的方式往浆料中引入0.1-4质量份的赛隆颗粒。所述赛隆陶瓷球中包含至少39wt％的α赛隆相，还包含β相Si 3N 4及少量YAG相。
为进一步论述本发明的有益效果，根据以下试验例、对比例以及相应的测试结果作进一步说明：
试验例1
一种高性能氮化铝陶瓷基板的制备方法，包括依次执行的以下步骤：
S1：配制浆料：以质量份计算，将100份的氮化铝粉体、1份的Y 2O 3、4份的Sm 2O 3、0.3份的2-3μm的金属铝粉、3份的磷酸三乙酯和44份的溶剂加入到球磨罐中，所述溶剂由异丙醇与正丁醇按照异丙醇：正丁醇＝1:1的比例混合形成，往球磨罐中加入150份的赛隆陶瓷球，以350r/min的转速球磨6h后再加入5份的聚乙烯醇缩丁醛和5份的邻苯二甲酸丁苄酯，继续球磨6h得到浆料；
S2：除泡：往浆料中加入0.4质量份的除泡剂，真空-0.1MPa条件下除泡30min，过滤得到流延浆料；过滤后发现赛隆陶瓷球损耗0.3质量份；
S3：流延成型：将流延浆料转至流延机上，在刮刀高度为0.35mm、流延带速为1.2m/min条件下流延成型得到坯带，将坯带干燥后冲压、裁切形成50*50mm 2的坯体；
S4：坯体预处理：所述坯体层叠后，先在压力为200MPa、温度为30℃的条件下，等静压压制5min，得到3*50*50mm 3的坯体；然后进行真空排胶处理：在真空排胶炉中，先以0.5℃/min速率从室温升温至200℃，保温1h，然后继续以0.5℃/min速率升温至350℃，保温1h，最后以1℃/min速率升温至550℃，保温1h；将坯体降温至室温，然后转入空气排胶炉进行空气排胶处理：以1℃/min速率升温至320℃，保温3h，得到待烧结坯体；
S5：将待烧结坯体置于流动氮气环境中，在1850℃条件下烧结4h,得到氮化铝陶瓷基板。
对比例1
一种氮化铝陶瓷基板的制备方法，与试验例1的差别在于，球磨所采用的是氧化锆球，而非赛隆陶瓷球。
试验例2
一种高性能氮化铝陶瓷基板的制备方法，与试验例1的差别在于，所述烧结助剂由2.5份的Y 2O 3、2.5份的La 2O 3以及0.3份的金属粉组成。
对比例2
以市面上买到的氮化铝陶瓷基板作为对比例2。
对上述试验例1-2以及对比例1-2进行测试：利用阿基米德排水法测试样品的密度；利用三点弯曲试验测得样品的弯曲强度；利用闪光法测得样品的热导率。数据如表1所示：
表1不同氮化铝陶瓷基板的性能结果
  试验例1 对比例1 试验例2 对比例2
热导率，W/(mK) 175 172 173 180
抗弯强度，MPa 504 471 489 357
密度，g/cm 3 3.37 3.37 3.33 3.33
从表1中的数据可以看出，本发明制备的氮化铝陶瓷基板与市面所售氮化铝基板相比，热导率相差无几，而弯曲强度提升了将近30％，致密度高且均匀，解决了目前氮化铝陶瓷基板偏软、加工困难、环境污染较大等难问题。本发明制备的氮化铝陶瓷基板时，以赛隆陶瓷球作为球磨球，通过球磨的方式引入的赛隆颗粒作为弥散增韧体系，有效提高氮化铝陶瓷的力学性能，并保持高热导率。该添加赛隆颗粒的工艺简单、成本低。
综上所述，本发明提供的一种高性能氮化铝陶瓷基板的浆料和制备方法，具有以下效果：(1)利用多元烧结助剂，配合金属铝粉的加入，大幅度降低杂质氧的引入，降低烧结温度，促进烧结致密化，有利于提高氮化铝陶瓷的热导 率和力学性能；(2)通过球磨方式引入的赛隆颗粒作为弥散增韧体系，有效提高氮化铝陶瓷的力学性能，并保持高热导率，该添加工艺简单、成本低；(3)选用醇类等无毒或低毒溶剂代替苯类、酮类等有毒溶剂，溶解特性好，挥发速率稳定，对坯体影响小；(3)通过等静压处理使坯体致密度更高，有利于后续制备高性能的烧结体；(4)采用两步排胶法(真空排胶和空气排胶)，有效避免加入的金属铝粉被氧化，减少杂质氧的引入量，且分段式升温方式能更好的排除坯体剩余的有机物，有效避免坯体变形、开裂，提高氮化铝陶瓷基板的烧结质量。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (10)

  1. 一种高性能氮化铝陶瓷基板的浆料，其特征在于，由以下质量份组分组成：100份的氮化铝粉体、1－8份的烧结助剂、0.1－4份的赛隆颗粒、1－6份的分散剂、38－68份的溶剂、3－12份的粘结剂和3－10份的增塑剂；所述烧结助剂由以下质量份组分组成：0－8份的Y 2O 3、0－5份的Sm 2O 3、0－1份的La 2O 3和0.05－3份的金属铝粉；所述溶剂为无水乙醇、异丙醇、正丁醇中的一种或几种。
  2. 如权利要求1所述的高性能氮化铝陶瓷基板的浆料，其特征在于，所述烧结助剂由以下质量份组分组成：1－6份的Y 2O 3、0－5份的Sm 2O 3、0－1份的La 2O 3和0.05－3份的金属铝粉。
  3. 如权利要求2所述的高性能氮化铝陶瓷基板的浆料，其特征在于，所述烧结助剂中Y 2O 3、Sm 2O 3和金属铝粉按照Y 2O 3：Sm 2O 3：金属铝粉＝1：(0.1－0.5)：(0.1－0.5)的比例混合；所述金属铝粉的粒径为2－3μm。
  4. 如权利要求1至3任一所述的高性能氮化铝陶瓷基板的浆料，其特征在于，所述溶剂由无水乙醇与正丁醇按照无水乙醇：正丁醇＝1：1的比例混合形成，或由异丙醇与正丁醇按照异丙醇：正丁醇＝1：1的比例混合形成。
  5. 如权利要求4所述的高性能氮化铝陶瓷基板的浆料，其特征在于，所述分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的一种或几种，所述粘结剂为聚乙烯醇缩丁醛，增塑剂为邻苯二甲酸丁苄酯。
  6. 一种高性能氮化铝陶瓷基板的制备方法，其特征在于，包括依次执行的以下步骤：
    S1：配制权利要求1至5任一所述的高性能氮化铝陶瓷基板的浆料：按照所需质量份将氮化铝粉体、烧结助剂、分散剂和溶剂加入到球磨罐中，按照氮化铝粉体：赛隆陶瓷球＝1：1－6的比例往球磨罐中加入赛隆陶瓷球，在球磨转速为250－500r/min的条件下，球磨6－20h后再加入粘结剂和增塑剂，继续球磨6－20h得到浆料；
    S2：除泡：往浆料中加入0.1－2质量份的除泡剂，真空负压除泡10－50min后过滤得到流延浆料；
    S3：流延成型：将流延浆料转至流延机上成型得到坯带，将坯带干燥后冲 压、裁切形成坯体；
    S4：坯体预处理：所述坯体层叠后，先经过等静压处理，然后依次进行真空排胶处理、空气排胶处理，最后得到待烧结坯体；
    S5：将待烧结坯体置于流动氮气环境中，在1650－1850℃条件下烧结2－8h，得到氮化铝陶瓷基板。
  7. 如权利要求6所述的高性能氮化铝陶瓷基板的制备方法，其特征在于，所述真空排胶处理的过程为：在真空排胶炉中，先从室温升温至200－250℃，保温0.5～2h，然后再升温至300－350℃，保温0.5～2h，最后升温至500～650℃，保温1～5h；所述空气排胶处理的过程为：在空气排胶炉中，升温至250－350℃，保温0.5～4h；所述真空排胶处理的升温速率为0.5～4℃/min，所述空气排胶处理的升温速率为0.5～4℃/min。
  8. 如权利要求7所述的高性能氮化铝陶瓷基板的制备方法，其特征在于，将坯体从真空排胶炉中转至空气排胶炉前，先将坯体降温至室温。
  9. 如权利要求6至8任一所述的高性能氮化铝陶瓷基板的制备方法，其特征在于，所述等静压处理为：在压力为90～200MPa、温度为25～100℃的条件下，等静压压制5～30min。
  10. 如权利要求9所述的高性能氮化铝陶瓷基板的制备方法，其特征在于，所述浆料的粘度为7000－14500cps；所述赛隆陶瓷球中包含至少39wt％的α赛隆相；所述除泡剂由正丁醇、乙二醇按照质量比1：1的比例混合形成；流延成型时，刮刀高度为0.3～0.9mm，流延带速为1～5m/min。
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