CN109721370A - 氮化硅、陶瓷浆料及制备方法 - Google Patents
氮化硅、陶瓷浆料及制备方法 Download PDFInfo
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- CN109721370A CN109721370A CN201910164306.3A CN201910164306A CN109721370A CN 109721370 A CN109721370 A CN 109721370A CN 201910164306 A CN201910164306 A CN 201910164306A CN 109721370 A CN109721370 A CN 109721370A
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Abstract
氮化硅粉末及制备方法、含有该氮化硅粉末的陶瓷浆料及制备方法。氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.40‑0.85。陶瓷浆料包括该氮化硅粉末、烧结助剂和具有羟基、羧基、氨基、酯基、醛基、羰基等基团的有机组分。陶瓷浆料制备方法包括:(1)以控温活化燃烧合成法制备氮化硅初级粉末;(2)对氮化硅初级粉末进行粗筛,以硝酸、盐酸、硫酸的混合酸进行酸洗,然后水洗、抽滤并干燥;(3)将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂;(4)将步骤3所得粉末与流体混合后置于研磨机中研磨,过筛后得到产品。
Description
技术领域
本发明涉及氮化硅、氮化硅陶瓷浆料及其制备方法,特别涉及一种基板用氮化硅陶瓷浆料及制备方法,属于陶瓷材料领域。
背景技术
随着能源、空间技术、新能源动力与高铁地面交通等科学技术的高度发展,大功率电力电子器件需求量与日俱增。基板是电力电子器件集成电路的核心部件,在复杂、苛刻的使用条件下,影响基板稳定性的原因为极端热和机械应力的共同作用,而现有的基板材料难以兼备良好的抗热震性能和机械强度,所以迫切需求导热性能、机械性能优异的材料应用于基板制造领域。
氮化硅陶瓷具有低密度、低膨胀系数、高导热系数、高硬度、良好的热稳定性和化学稳定性、耐腐蚀、耐磨损等多种优异性能,非常适合于大功率电力电子器件功率模块的应用实况。高热导、高机械强度(抗弯强度和断裂韧性)的氮化硅基板能在严苛的工作环境下具有较高使用寿命及更高可靠性,使电子电力系统在运行过程中更加安全可靠。
发明内容
本发明的一个方面提供一种氮化硅粉末,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.40-0.85;优选的,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.50-0.80;进一步优选的,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.55-0.76。
根据本发明的一个方面,所述氮化硅粉末的粒径范围为0.4μm–20μm;优选为1μm–10μm;进一步优选为1.3μm–5μm。
根据本发明的一个方面,所述氮化硅粉末的比表面积为0.5m2/g-8.0m2/g;优选的,所述氮化硅粉末的比表面积为0.8m2/g-6.0m2/g;优选的,所述氮化硅粉末的比表面积为1.0m2/g-5.0m2/g;优选的,所述氮化硅粉末的比表面积为1.1m2/g-4.0m2/g。
根据本发明的一个方面,所述氮化硅粉末的α相含量>60wt%,优选>80wt%,更优选为85wt%-95wt%。
本发明的一个方面提供一种陶瓷浆料,其特征在于,所述陶瓷浆料包括如上所述的氮化硅粉末、烧结助剂和有机组分,其中,所述有机组分具有羟基、羧基、氨基、酯基、醛基、羰基等基团;优选的,所述有机组分具有羟基、羧基、氨基、酯基等基团;进一步优选的,所述有机组分具有羟基、羧基等基团。
根据本发明的一个方面,所述有机组分包括溶剂、分散剂、粘结剂和增塑剂;优选的,所述氮化硅粉末、所述烧结助剂、所述溶剂、所述分散剂、所述粘结剂和所述增塑剂的质量配比为100:(3-15):(20-70):(2-4):(5-20):(5-30)。
根据本发明的一个方面,所述烧结助剂选自氧化铝、氧化钇、氧化镁、氧化钙、镁硅氮中的一种或多种;优选的,所述溶剂选自乙醇、乙二醇、异丙醇、正丁醇、2-丁酮中的一种或多种;优选的,所述分散剂选自磷酸三乙酯、聚乙烯吡咯烷酮、聚丙烯酸氨、柠檬酸铵中的一种或多种;优选的,所述粘结剂选自聚乙二醇、聚乙烯醇缩丁醛、丙烯酸甲酯中的一种或多种;优选的,所述增塑剂选自邻苯二甲酸酯、聚乙二醇和甘油中的一种或多种。
根据本发明的一个方面,所述陶瓷浆料杂质含量低于5wt%、固相体积分数为50%-75%、粘度小于0.2pa·s。
本发明的一个方面提供一种氮化硅粉末的制备方法,所述方法包括:
(1)以控温活化燃烧合成法制备氮化硅初级粉末;
(2)对所述氮化硅初级粉末进行粗筛,以硝酸、盐酸、硫酸的混合酸进行酸洗,然后水洗、抽滤并干燥;
(3)将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂;
(4)将步骤3所得粉末与流体混合后进行表面整形,过筛后得到含有氮化硅粉末的浆料,所述流体包括有机物;
(5)在无氧环境下热处理步骤3所得的所述含有氮化硅粉末的浆料,除去所述流体,密封包装,得到上所述的氮化硅粉末。
本发明一个方面提供一种氮化硅陶瓷浆料的制备方法,所述方法包括以下步骤:
(1)以控温活化燃烧合成法制备氮化硅初级粉末;
(2)对所述氮化硅初级粉末进行粗筛,以硝酸、盐酸、硫酸的混合酸进行酸洗,然后水洗、抽滤并干燥;
(3)将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂;
(4)将步骤3所得粉末与流体混合后进行表面整形,过筛后得到如上所述的陶瓷浆料,所述流体包括有机物。
其中,上述氮化硅粉末的制备方法和氮化硅陶瓷浆料的制备方法中,步骤(1)中控温活化燃烧合成法制备高纯α氮化硅粉体的粒度范围为0.4μm-20μm,α相含量>60wt%,杂质含量<10wt%,颗粒形貌一致性好,氮化硅粉体呈现等轴状形貌。得到的氮化硅粉体非常适合用于制备集成电路的基板。
上述所述步骤(1)例如可以包括:
(1.1)对原始粒度100-500目的硅粉原料进行球磨活化处理,以酒精或丙酮为介质,球磨处理12-36小时,将球磨后的浆料真空抽滤,在50-70℃温度下真空干燥,得到平均粒径约为0.5-1μm的高活性硅粉;
(1.2)以上述1.1活化处理的硅粉为原料,加入适量稀释剂,和添加剂,添加剂为NH4Cl、NH4F中一种或两种混合物,各组分的重量百分比如下:硅粉原料:20%-55wt%,氮化硅稀释剂:40%-70wt%,添加剂:5-10wt%,共混得到混合原料;
(1.3)将上述1.2所得混合原料在酒精或者丙酮介质中球磨10-20小时使其充分混合均匀,混合后的原料在50-70℃温度下真空干燥后,过50-200目筛,随后松装布料于石墨舟中;
(1.4)将1.3中的石墨舟放置在燃烧合成反应装置内,抽真空后,充入0.5-4.5MPa高纯氮气,引燃后发生燃烧合成反应;燃烧反应结束,经过充分冷却后,取出产物,从而制得α相含量大于60wt%的氮化硅粉体。
在上述氮化硅粉末的制备方法和氮化硅陶瓷浆料的制备方法中,步骤(2)中以150-900目的网筛对制备的氮化硅粉体进行粗筛并对其进行酸洗,以除去粉体表面氧化层以及含氧基团;所述的混合酸中硝酸、盐酸、硫酸的体积含量比例分别为10%-20%、60%-80%、10%-20%,各酸溶液质量分数分别小于68%、20%、70%,酸洗1-10小时,将酸洗后的粉体水洗1-5次,除去水溶性离子异物等水溶性物质,抽滤后采用压滤干燥、喷雾干燥或真空干燥的方法进行干燥。
在上述氮化硅粉末的制备方法和氮化硅陶瓷浆料的制备方法中,步骤(3)中对α氮化硅陶瓷粉体进行热处理以除去初始粉体中NH4Cl或NH4F添加剂;所述的加热装置为隧道窑或加热炉,热处理工艺为流动氮气气氛条件下在500-900℃下热处理1-8小时,升温速率5-10℃/min,其中氮气纯度为99.2%-99.999%,流速为2-5m/s。
在上述氮化硅粉末的制备方法和氮化硅陶瓷浆料的制备方法中,步骤(4)中将α氮化硅陶瓷粉体、烧结助剂、溶剂、分散剂、粘结剂、增塑剂混合,其质量配比为100:(3-15):(20-70):(2-4):(5-20):(5-30),并置于行星式球磨机、滚动式球磨机、砂磨机中研磨1-10小时,转速300-3000r/min,研磨介质为氮化硅磨球,过150-900目筛后制得到高纯α氮化硅陶瓷浆料;所述烧结助剂为氧化铝、氧化钇、氧化镁、氧化钙、镁硅氮中的一种或多种;所述溶剂优选乙醇、乙二醇、异丙醇、正丁醇、2-丁酮中的一种或多种;所述分散剂优选磷酸三乙酯、聚乙烯吡咯烷酮、聚丙烯酸氨、柠檬酸铵中的一种或多种;所述粘结剂优选聚乙二醇、聚乙烯醇缩丁醛、丙烯酸甲酯中的一种或多种;所述增塑剂优选邻苯二甲酸酯、聚乙二醇和甘油中的一种或多种。
在上述氮化硅粉末的制备方法和氮化硅陶瓷浆料的制备方法中,所述步骤(4)中的所述表面整形包括砂磨、搅拌磨、V型混合机混磨和/或滚筒磨,优选砂磨。
使用上述方法得到的氮化硅陶瓷浆料,杂质含量低于5wt%、固相体积分数为50-75%、粘度小于0.2pa·s,氮化硅粉末中α相含量大于60wt%,适合流延成型,且制备方法简单。由上述描述可知,本文得到的氮化硅陶瓷浆料同时具备固相体积分数高(50-75%)和粘度低(小于0.2pa·s)这两个优点。一般来说,陶瓷浆料的固相体积分数越高,其粘度也会越高,因为固体成分增加以及增加后的团聚等削弱了浆料的流动性。氮化硅陶瓷基板普遍地采用流延成型制造,而流延成型要求浆料同时具备固含量高和粘度低这两个特性,以制备得到高品质的氮化硅陶瓷基板。在本发明提出以前,如何能够得到同时具备高固相体积分数和低粘度两种特性的氮化硅陶瓷浆料,这一技术问题长久地困扰着这一领域研发人员。
在本发明以前,研究人员尝试了各种方式,包括传统的机械制浆法、化学制浆法、有机溶剂制浆法等,想要获得同时具备高的固相体积分数和低粘度的氮化硅陶瓷浆料,但结果都不尽人意。这一领域研发人员几乎形成了这样的根深蒂固的认知,即认为高固相含量和低粘度是一对不可调和的矛盾,要获得同时具备高固相含量和低粘度两种特性的氮化硅陶瓷浆料,几乎是不可能完成的任务。
本发明提供的如上所述的氮化硅粉体很好的解决了上面的技术问题。不受任何理论和现有经验的束缚,本发明的发明人在研究中出人意料地发现,造成较高固相含量的陶瓷浆料的高粘度的主要原因之一是:陶瓷浆料中使用的氮化硅粉体颗粒具有较小的粒径和较大的比表面积,具有大的比表面积的氮化硅粉体与空气等氧化性环境接触,在粉体表面形成过多的羟基或其他含氧基团,静电能量增加,粉体颗粒在静电力和氢键等作用力下发生团聚,阻碍了粉体间的流动性和润滑性,从而无法获得同时具备高的固相含量和低粘度的氮化硅陶瓷浆料。
在出人意料地发现并且深刻地认识了上述技术问题的基础上,本发明的发明人提供了如上所述的新型氮化硅粉体,其具有高的未氧化氮化硅表面面积:全部氮化硅表面面积的比例,从而大大改善了氮化硅粉体在陶瓷浆料中的分散性、降低了陶瓷浆料的粘度、提高了氮化硅的固相含量,非常适合流延成型制造集成电路基板。对于该新型氮化硅粉体,本发明的发明人设计了如下简单、巧妙、高效的方案:先将氮化硅粉体与有机组分预混,利用设备对该有机-无机混合物进行表面整形,充分破碎其中的氮化硅粉体、将氮化硅粉体内部物质暴露出来形成新的表面。本发明的发明人发现,由于在上述表面整形过程中,氮化硅粉体被有机组分包裹,从而与空气隔绝,那么被表面整形(例如,研磨、破碎)而新露出的氮化硅表面不会被空气中的氧气氧化,表面不易形成含氧官能团固相含量。通过上述简单但有效的方式,本发明的发明人解决了前述的长久困扰这一领域研发人员的问题:成功地提供了一种同时具备高的固相含量和低粘度的氮化硅陶瓷浆料。本发明实施例提供的陶瓷浆料,固相含量(体积分数)可达50-75%,而同时其粘度还能够小于0.2pa·s。
另外,在上述预混、研磨之前,本发明的发明人还通过对氮化硅粉末进行酸洗,以除去粉体表面氧化层以及含氧基团;酸洗后进行水洗,以除去水溶性离子异物;水洗之后再进行热处理,通过所述热处理除去初始粉体中NH4Cl或NH4F添加剂。在预混、研磨之前的上述酸洗、水洗、热处理等工艺更进一步地提高了氮化硅粉体的纯度、改善了其表面性质,更加适合制造性能优异的陶瓷浆料。
正是由于采用了上述表面整形、酸洗、水洗、热处理等手段,大大改善了氮化硅陶瓷浆料的综合性能,使得本文的氮化硅陶瓷浆料适合于采用更多种方法制备。例如可以采用适合大规模工业生产的燃烧合成法来制备氮化硅粉体,再利用该氮化硅粉体进一步制备陶瓷浆料。燃烧合成法是一种利用燃烧反应放出的热量来制备材料的方法,其利用外部提供的瞬间能量,诱发高放热化学反应体系产生局部化学反应,形成自维持的反应燃烧波,进而在燃烧波蔓延前进的过程中使得原料发生反应转化为产物。采用燃烧合成法制备氮化硅粉体相比于其他制备方法具有成本低、节能、高效、工艺简单、产物纯度高、适合大规模生产等诸多优点。然而,在本发明提出以前,将燃烧合成法制备的氮化硅粉体制成陶瓷浆料,其性能难以满足集成电路基板的制备要求。也就是说,采用燃烧合成法制备氮化硅粉体,再利用该氮化硅粉体制造得到氮化硅陶瓷浆料,同样有前述的困扰:难以获得同时具备高固相含量和低粘度的陶瓷浆料。但用燃烧合成法制备得到氮化硅初级粉末,再对这一氮化硅初级粉末进行本文上述的表面整形、酸洗、水洗、热处理等处理,能够得到适合于流延成型的高品质的陶瓷浆料,固相体积分数可达50-75%,而同时其粘度还能够小于0.2pa·s。本发明的发明人提出的解决方案使得燃烧合成法可以被用来生产氮化硅粉体、并进一步基于该氮化硅粉体大量工业化生产适合于流延成型的高品质氮化硅陶瓷浆料,这一贡献不但具有技术上的开拓性意义,同时在商业上也能创造很大的价值。
在本文的叙述中,为了清楚、简明的目的,将上述被表面整形而新露出的氮化硅表面称为“未氧化氮化硅表面”。可以理解,“未氧化氮化硅表面”的面积与“全部氮化硅表面”的面积之比值,将能够反映氮化硅粉体在上述研磨过程中新生的、从而是未被空气中的氧气氧化的表面占全部表面之比例。由于“表面积”之比与“比表面积”之比相同,而“比表面积”通过科学手段测定更加方便,因此本文的实施例中将采用“比表面积”之比来确定“表面积”之比。
在本文中,“表面整形”是指,将氮化硅粉体与有机组分预混的情况下,利用设备对该有机-无机混合物进行机械处理例如研磨、破碎,充分破碎其中的氮化硅粉体、将氮化硅粉体内部物质暴露出来形成新的表面,同时在这一过程中,氮化硅粉体的上述新的表面与上述有机组分发生物理的、化学的作用,最终形成同时具备高的固相含量和低粘度的陶瓷浆料。所述表面整形例如包括砂磨、搅拌磨、V型混合机混磨和/或滚筒磨,优选砂磨。优选砂磨的原因在于,砂磨能够有效地破碎氮化硅粉体,并且能够得到表面形貌规整、粒径均一的细粉,以及提升粉体与有机组份的混合效果。但本文中的“表面整形”不限于上述限定的方式,只要能够有效破碎氮化硅粉体并且获得具有优良的微观形貌的氮化硅细粉的处理手段,就能够达到上述“表面整形”的目的。由上述内容可知,本文所述“表面整形”不但增加了氮化硅粉体未被氧化的表面,而且还改善了氮化硅粉体的微观形貌,使其更加适合于制备高性能的陶瓷浆料。特别的,为能够至少从一个方面定量地界定本文所述“表面整形”,经过“表面整形”后,氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.40-0.85,上述范围优选为0.50-0.80;进一步优选为0.55-0.76。
本发明的技术方案与已有技术相比较具有如下突出优点:
(1).本发明实施例提供的氮化硅粉末具有高比例的未氧化表面,氮化硅粉体呈现等轴状的规整形貌,氮化硅粉末之间不容易发生团聚,适合用于进一步制备高品质的氮化硅陶瓷浆料。
(2).以控温活化燃烧合成法制备氮化硅粉体,实现了较低温度下的燃烧合成,大幅度减少了合成产物在高温区间的停留时间,避免了高温煅烧引起的大面积硬团聚,制备了纯度高、α相含量高、颗粒形态一致性好的基板用氮化硅粉体。
(3).通过酸洗、水洗、热处理等工艺极大提高了基板用氮化硅陶瓷浆料初始粉体的纯度。酸洗工艺除去粉体表面氧化层以及含氧基团;水洗工艺除去水溶性离子异物;热处理除去初始粉体中NH4Cl或NH4F添加剂。
(4).采用研磨机将氮化硅陶瓷粉体、溶剂以及添加剂研磨共混制备基板用氮化硅陶瓷浆料,过程中氮化硅粉体被有机组分包裹,从而与空气隔绝,研磨细化的氮化硅的新鲜表面不易形成含氧官能团,阻碍了氮化硅粉体的团聚现象,极大地提高了氮化硅陶瓷浆料的分散均匀性和稳定性。
(5).制得的基板用氮化硅陶瓷浆料α相含量高、纯度高、粘度低、固相含量高、适合流延成型,并且制备方法简单,适合产业化生产。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例的附图作简单地介绍,显然,下面描述中的附图仅仅涉及本发明的一些实施例,而非对本发明的限制。
图1是实施例3中控温活化燃烧合成氮化硅粉体微观形貌图;
图2是实施例3中控温活化燃烧合成氮化硅粉体的XRD分析图谱。
具体实施方式
下文将结合具体实施例对本发明的氮化硅、氮化硅陶瓷浆料做更进一步的说明。应当理解,下列实施例仅为示例性地说明和解释本发明,而不应被解释为对本发明保护范围的限制。凡基于本发明上述内容所实现的技术均涵盖在本发明旨在保护的范围内。
实施例1
在1MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为3μm,α相含量为85%,杂质含量为2%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗3小时,接着水洗3次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在600℃下热处理5小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。测试所得氮化硅粉体的比表面积为S1=0.625m2/g。
接着,按质量配比为100:50:3:15:20称取α氮化硅陶瓷粉体、溶剂、分散剂、粘结剂、增塑剂(以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为800r/min的砂磨机中用氮化硅磨球研磨2小时。取少量试样,采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,测试其比表面积为S2=2.180m2/g。S2-S1/S2=0.713。不难理解,研磨后新增加的氮化硅表面(即S2-S1)由于始终被溶剂、分散剂等组分包裹,与外界空气隔绝,是未被氧化的表面,即本文发明内容部分所定义的“未氧化氮化硅表面”。
最后,按照α氮化硅陶瓷粉体:烧结助剂的质量配比100:10加入烧结助剂,所述烧结助剂为氧化铝和镁硅氮,混合后置于转速为800r/min的砂磨机中用氮化硅磨球研磨1小时。过600目筛后制得到高纯α氮化硅陶瓷浆料CX1。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为3wt%、固相体积分数为50.5%、粘度0.125pa·s。
实施例2
在3MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为5μm,α相含量为90%,杂质含量为1.6%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗5小时,接着水洗5次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在700℃下热处理4小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。测试所得氮化硅粉体的比表面积为S1=0.375m2/g。
接着,按质量配比为100:40:3:10:15称取α氮化硅陶瓷粉体、溶剂、分散剂、粘结剂、增塑剂(以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为1000r/min的砂磨机中用氮化硅磨球研磨3小时。取少量试样,采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,测试其比表面积为S2=1.562m2/g。S2-S1/S2=0.760。
最后,按照α氮化硅陶瓷粉体:烧结助剂的质量配比100:10加入烧结助剂,所述烧结助剂为氧化铝和氧化镁,混合后置于转速为1000r/min的砂磨机中用氮化硅磨球研磨1小时。过600目筛后制得到高纯α氮化硅陶瓷浆料CX2。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为1wt%、固相体积分数为57%、粘度0.14pa·s。
实施例3
在0.6MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为1.5μm,α相含量为93%,杂质含量为1.3%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗5小时,接着水洗5次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在800℃下热处理6小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。测试所得氮化硅粉体的比表面积为S1=1.250m2/g。
接着,按质量配比为100:30:2:8:10称取α氮化硅陶瓷粉体、溶剂、分散剂、粘结剂、增塑剂(以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为1500r/min的砂磨机中用氮化硅磨球研磨4小时。取少量试样,采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,测试其比表面积为S2=2.880m2/g。S2-S1/S2=0.566。
最后,按照α氮化硅陶瓷粉体:烧结助剂的质量配比100:5加入烧结助剂,所述烧结助剂为氧化钇和氧化镁,混合后置于转速为1500r/min的砂磨机中用氮化硅磨球研磨1小时。过600目筛后制得到高纯α氮化硅陶瓷浆料CX3。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为0.9wt%、固相体积分数为64.5%、粘度0.165pa·s。
对上述获得的氮化硅粉体的粒度采用扫描电镜进行表征,结果如图1所示。从图1可知,本实施例所获得的氮化硅粉体呈现等轴状形貌,颗粒直径大部分小于2μm,部分颗粒直径小于1μm。对上述获得的氮化硅粉体的相组成与含量采用X射线衍射表征分析,结果如图2所示。由图2可知,本实施例获得的氮化硅绝大部分都是α相的氮化硅,β相的氮化硅所占比例小于7wt%。
实施例4
在0.5MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为1.3μm,α相含量为95%,杂质含量为1.1%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗5小时,接着水洗5次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在900℃下热处理5小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。测试所得氮化硅粉体的比表面积为S1=1.442m2/g。
接着,按质量配比为100:20:2:6:8称取α氮化硅陶瓷粉体、溶剂、分散剂、粘结剂、增塑剂(以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为2000r/min的砂磨机中用氮化硅磨球研磨5小时。取少量试样,采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,测试其比表面积为S2=3.233m2/g。S2-S1/S2=0.553。
最后,按照α氮化硅陶瓷粉体:烧结助剂的质量配比100:4加入烧结助剂,所述烧结助剂为氧化铝和氧化镁,混合后置于转速为2000r/min的砂磨机中用氮化硅磨球研磨1小时。过600目筛后制得到高纯α氮化硅陶瓷浆料CX4。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为0.86wt%、固相体积分数为72.5%、粘度0.180pa·s。
实施例5
在1MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为3μm,α相含量为85%,杂质含量为2%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗3小时,接着水洗3次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在600℃下热处理5小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。
接着,按质量配比为100:10:50:3:15:20称取α氮化硅陶瓷粉体、烧结助剂、溶剂、分散剂、粘结剂、增塑剂(以氧化铝与镁硅氮作为烧结助剂、以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为800r/min的砂磨机中用氮化硅磨球研磨3小时。
最后,过600目筛后制得到高纯α氮化硅陶瓷浆料CX5。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为3wt%、固相体积分数为50.3%、粘度0.130pa·s。
本实施例的内容与实施例1基本相同,区别在于,实施例1中增加了氮化硅粉体在研磨前后比表面积S1、S2的步骤。需要说明的是,增加氮化硅粉体在研磨前后比表面积S1、S2的步骤仅为了探索本发明技术方案获得良好技术效果的原因。在实际生产过程中,完全可以略去这一步骤,像本实施例这样,直接将氮化硅陶瓷粉体与形成陶瓷浆料必不可少的试剂混合、研磨,得到最终的陶瓷浆料产品。
实施例6
在1MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为3μm,α相含量为85%,杂质含量为2%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗3小时,接着水洗3次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在600℃下热处理5小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。
接着,按质量配比为100:85称取α氮化硅陶瓷粉体、溶剂(以乙醇作为溶剂)进行混合,并置于转速为800r/min的砂磨机中用氮化硅磨球研磨3小时。在无氧环境中(例如,充入氮气的手套箱中),采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,进行无氧包装(例如,包装袋中充入氮气)或者真空密封包装。在无氧环境下,取上述真空密封包装内的氮化硅粉体,按质量配比为100:10:50:3:15:20称取α氮化硅陶瓷粉体、烧结助剂、溶剂、分散剂、粘结剂、增塑剂(以氧化铝与镁硅氮作为烧结助剂、以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合,并置于转速为800r/min的砂磨机中用氮化硅磨球研磨3小时。
最后,过600目筛后制得到高纯α氮化硅陶瓷浆料CX6。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为3wt%、固相体积分数为51.1%、粘度0.126pa·s。
基于本实施例可以理解,本文的氮化硅粉末可真空无氧密封包装,单独销售。用户可以根据具体需求,在无氧环境下自行配制成陶瓷浆料。对于陶瓷浆料的组分、各组分之间的配比,用户可以灵活选择、确定。这样给用户留下较大的自由度。
对比实施例1未进行表面整形(简单混合)
在1MPa氮气压力下,采用控温活化燃烧合成法制备了粒度为3μm,α相含量为85%,杂质含量为2%,颗粒形貌一致的高纯α氮化硅粉体。以600目的网筛该氮化硅粉体进行粗筛,并置于硝酸、盐酸、硫酸(体积含量比例分别为20%、60%、20%,酸溶液质量分数分别40%、15%、58%)组成的混合酸进行酸洗3小时,接着水洗3次,抽滤后采用真空干燥的方法进行干燥。之后,将氮化硅粉体置于加热炉中热处理,具体工艺为流动氮气气氛条件下在600℃下热处理5小时,升温速率8℃/min,其中氮气纯度为99.999%,流速为3m/s。测试所得氮化硅粉体的比表面积为S1=0.625m2/g。
接着,按质量配比为100:50:3:15:20称取α氮化硅陶瓷粉体、溶剂、分散剂、粘结剂、增塑剂(以乙醇作为溶剂、以磷酸三乙酯与聚乙烯吡咯烷酮作为分散剂、以聚乙烯醇缩丁醛为粘结剂、以聚乙二醇和甘油作为增塑剂)进行混合。取少量试样,采用燃烧或者蒸馏分离等方法,去除溶剂、分散剂、粘结剂和增塑剂,得到氮化硅粉体,测试其比表面积为S2=0.625m2/g。S2-S1/S2=0。
最后,按照α氮化硅陶瓷粉体:烧结助剂的质量配比100:10加入烧结助剂,所述烧结助剂为氧化铝和镁硅氮,充分混合。过600目筛后制得到氮化硅陶瓷浆料CX1’。对氮化硅陶瓷浆料进行表征分析的结果为杂质含量为2.8wt%、固相体积分数为43.6%、粘度0.974pa·s。
本对比例1的内容与实施例1基本相同,区别在于,对比例1中未采用砂磨机进行研磨,也就是说未进行表面整形。将实施例1的结果与对比例1的结果对比可知,对比例1的固相体积分数低于实施例1,而粘度显著高于实施例1。
表1:基板用高纯α氮化硅陶瓷浆料产品性能表
Claims (10)
1.一种氮化硅粉末,其特征在于,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.40-0.85;优选的,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.50-0.80;进一步优选的,所述氮化硅粉末的未氧化氮化硅表面面积:全部氮化硅表面面积为0.55-0.76。
2.根据权利要求1所述的氮化硅粉末,其特征在于,所述氮化硅粉末的粒径范围为0.4μm–20μm;优选为1μm–10μm;进一步优选为1.3μm–5μm;
优选的,所述氮化硅粉末的比表面积为0.5m2/g-8.0m2/g;优选的,所述氮化硅粉末的比表面积为0.8m2/g-6.0m2/g;优选的,所述氮化硅粉末的比表面积为1.0m2/g-5.0m2/g;优选的,所述氮化硅粉末的比表面积为1.1m2/g-4.0m2/g;
优选的,所述氮化硅粉末的α相含量>60wt%,优选>80wt%,更优选为85wt%-95wt%。
3.一种陶瓷浆料,其特征在于,所述陶瓷浆料包括如权利要求1或2所述的氮化硅粉末、烧结助剂和有机组分,其中,所述有机组分具有选自羟基、羧基、氨基、酯基、醛基、羰基的基团中的至少一种;优选的,所述有机组分具有选自羟基、羧基、氨基、酯基的基团中的一种;进一步优选的,所述有机组分具有羟基、羧基的基团中的至少一种。
4.根据权利要求3所述的陶瓷浆料,其特征在于,所述有机组分包括溶剂、分散剂、粘结剂和增塑剂;优选的,所述氮化硅粉末、所述烧结助剂、所述溶剂、所述分散剂、所述粘结剂和所述增塑剂的质量配比为100:(3-15):(20-70):(2-4):(5-20):(5-30);
优选的,所述烧结助剂选自氧化铝、氧化钇、氧化镁、氧化钙、镁硅氮中的一种或多种;优选的,所述溶剂选自乙醇、乙二醇、异丙醇、正丁醇、2-丁酮中的一种或多种;优选的,所述分散剂选自磷酸三乙酯、聚乙烯吡咯烷酮、聚丙烯酸氨、柠檬酸铵中的一种或多种;优选的,所述粘结剂选自聚乙二醇、聚乙烯醇缩丁醛、丙烯酸甲酯中的一种或多种;优选的,所述增塑剂选自邻苯二甲酸酯、聚乙二醇和甘油中的一种或多种;
优选的,所述陶瓷浆料杂质含量低于5wt%、固相体积分数为50%-75%、粘度小于0.2pa·s。
5.如权利要求1或2所述的氮化硅粉末的制备方法,其特征在于,所述方法包括:
(1)以控温活化燃烧合成法制备氮化硅初级粉末;
(2)对所述氮化硅初级粉末进行粗筛,以硝酸、盐酸、硫酸的混合酸进行酸洗,然后水洗、抽滤并干燥;
(3)将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂;
(4)将步骤3所得粉末与流体混合后进行表面整形,过筛后得到含有氮化硅粉末的浆料,所述流体包括有机物;
(5)在无氧环境下热处理步骤3所得的所述含有氮化硅粉末的浆料,除去所述流体,密封包装,得到所述氮化硅粉末。
6.如权利要求5所述的方法,其特征在于,所述步骤(1)得到的所述氮化硅初级粉末的粒度范围为0.1μm–20μm,优选为1μm–10μm;进一步优选为1.3μm–5μm;α相含量>60wt%,优选>80wt%,更优选为85wt%-95wt%;杂质含量<10%;优选的,所述氮化硅初级粉末的颗粒均为等轴状形貌;优选的,所述步骤(4)中的所述表面整形包括砂磨、搅拌磨、V型混合机混磨和/或滚筒磨,优选砂磨;
优选的,所述步骤(1)控温活化燃烧合成法制备氮化硅初级粉末过程中,氮气压力为0.5MPa-8MPa,优选0.6MPa-3MPa;
优选的,所述步骤(2)包括:以150-900目的网筛对所述氮化硅初级粉末进行粗筛,并以硝酸、盐酸、硫酸的混合酸进行酸洗,以除去所述氮化硅初级粉末表面氧化层以及含氧基团;所述的混合酸中所述硝酸、所述盐酸、所述硫酸的体积含量比例分别为10%-20%、60%-80%、10%-20%,质量分数分别小于68%、小于20%、小于70%,酸洗1-10小时,将酸洗后的粉末水洗1-5次,除去水溶性物质,抽滤后采用压滤干燥、喷雾干燥或真空干燥的方法进行干燥;
优选的,所述步骤(3)包括:将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂,所述添加剂包括NH4Cl和/或NH4F;所述加热装置包括隧道窑或加热炉;所述热处理包括:为流动氮气气氛条件下,在500℃-900℃下热处理1-8小时,升温速率5℃/min-10℃/min,其中氮气纯度为99.2wt%-99.999wt%,流速为2m/s-5m/s;
优选的,所述步骤(4)中所述有机物选自磷酸三乙酯、聚乙烯吡咯烷酮、聚丙烯酸氨、柠檬酸铵中的一种或多种。
7.如权利要求3或4所述的陶瓷浆料的制备方法,其特征在于,所述方法包括:
(1)以控温活化燃烧合成法制备氮化硅初级粉末;
(2)对所述氮化硅初级粉末进行粗筛,以硝酸、盐酸、硫酸的混合酸进行酸洗,然后水洗、抽滤并干燥;
(3)将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂;
(4)将步骤3所得粉末与流体混合后进行表面整形,过筛后得到如权利要求5-7任一项所述的陶瓷浆料,所述流体包括有机物。
8.如权利要求7所述的方法,其特征在于,所述步骤(1)得到的所述氮化硅初级粉末的粒度范围为0.1μm–20μm,优选为1μm–10μm;进一步优选为1.3μm–5μm;α相含量>60wt%,优选>80wt%,更优选为85wt%-95wt%;杂质含量<10%;优选的,所述氮化硅初级粉末的颗粒均为等轴状形貌;优选的,所述步骤(4)中的所述表面整形包括砂磨、搅拌磨、V型混合机混磨和/或滚筒磨,优选砂磨;
优选的,所述步骤(1)控温活化燃烧合成法制备氮化硅初级粉末过程中,氮气压力为0.5MPa-8MPa,优选0.6MPa-3MPa;
优选的,所述步骤(2)包括:以150-900目的网筛对所述氮化硅初级粉末进行粗筛,并以硝酸、盐酸、硫酸的混合酸进行酸洗,以除去所述氮化硅初级粉末表面氧化层以及含氧基团;所述的混合酸中所述硝酸、所述盐酸、所述硫酸的体积含量比例分别为10%-20%、60%-80%、10%-20%,质量分数分别小于68%、小于20%、小于70%,酸洗1-10小时,将酸洗后的粉末水洗1-5次,除去水溶性物质,抽滤后采用压滤干燥、喷雾干燥或真空干燥的方法进行干燥;
优选的,所述步骤(3)包括:将步骤2所得粉末置于加热装置中,在流动氮气气氛条件下热处理除去添加剂,所述添加剂包括NH4Cl和/或NH4F;所述加热装置包括隧道窑或加热炉;所述热处理包括:为流动氮气气氛条件下,在500℃-900℃下热处理1-8小时,升温速率5℃/min-10℃/min,其中氮气纯度为99.2wt%-99.999wt%,流速为2m/s-5m/s;
优选的,所述步骤(4)的所述流体包括烧结助剂、溶剂、分散剂、粘结剂和增塑剂,将步骤3所得粉末、所述烧结助剂、所述溶剂、所述分散剂、所述粘结剂、所述增塑剂混合,其质量配比为100:(3-15):(20-70):(2-4):(5-20):(5-30);
优选的,所述烧结助剂选自氧化铝、氧化钇、氧化镁、氧化钙、镁硅氮中的一种或多种;优选的,所述溶剂选自乙醇、乙二醇、异丙醇、正丁醇、2-丁酮中的一种或多种;优选的,所述分散剂选自磷酸三乙酯、聚乙烯吡咯烷酮、聚丙烯酸氨、柠檬酸铵中的一种或多种;优选的,所述粘结剂选自聚乙二醇、聚乙烯醇缩丁醛、丙烯酸甲酯中的一种或多种;优选的,所述增塑剂选自邻苯二甲酸酯、聚乙二醇和甘油中的一种或多种;
优选的,所述步骤(4)包括:将步骤3所得粉末、所述烧结助剂、所述溶剂、所述分散剂、所述粘结剂、所述增塑剂混合后置于砂磨机中研磨1-10小时,转速300-3000r/min,研磨介质为氮化硅磨球,过150-900目筛后制得到所述陶瓷浆料。
9.一种氮化硅烧结体,将包括权利要求1或2所述的氮化硅粉末的陶瓷浆料或者权利要求3或4所述的陶瓷浆料烧结而得到。
10.一种电路基板,使用如权利要求9所述的氮化硅烧结体。
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