CN112661518A - 一种高导热氮化硅陶瓷绝缘板及其制备方法 - Google Patents

一种高导热氮化硅陶瓷绝缘板及其制备方法 Download PDF

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Publication number
CN112661518A
CN112661518A CN202011559771.6A CN202011559771A CN112661518A CN 112661518 A CN112661518 A CN 112661518A CN 202011559771 A CN202011559771 A CN 202011559771A CN 112661518 A CN112661518 A CN 112661518A
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silicon nitride
sintering aid
sintering
insulating plate
ceramic insulating
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CN202011559771.6A
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CN112661518B (zh
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张伟儒
梁盼盼
荆赫
孙峰
徐学敏
董廷霞
吕沛远
何霄
徐金梦
魏文钊
丁智杰
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Sinoma Advanced Nitride Ceramics Co Ltd
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Sinoma Advanced Nitride Ceramics Co Ltd
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Priority to PCT/CN2021/141240 priority patent/WO2022135571A1/zh
Priority to EP21909566.8A priority patent/EP4269372A1/en
Priority to JP2023538154A priority patent/JP2024500914A/ja
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Abstract

本发明提供了一种高导热氮化硅陶瓷绝缘板及其制备方法，属于陶瓷基板技术领域。本发明采用氧化镁作为第一烧结助剂，在烧结过程中氧化镁与原料氮化硅粉体反应生成液相，能够降低烧结温度，节约生产成本，同时还能提高氮化硅陶瓷绝缘板的致密度和抗弯强度；本发明以氧化铪作为第二烧结助剂，利用其与氧结合能力较强，在烧结过程中与原料氮化硅粉体中的杂质氧结合，消除晶格氧含量，提高氮化硅陶瓷绝缘板的热导率；本发明的第三烧结助剂在烧结过程中能够促进液相反应，与氮化硅粉体反应形成固溶体，减少晶界处的非晶相，在保证高热导率的同时提高产品抗弯强度。此外，本发明还解决了现有技术中难以制备超薄大尺寸基板的难题。

Description

一种高导热氮化硅陶瓷绝缘板及其制备方法
技术领域
本发明涉及陶瓷基板技术领域，尤其涉及高导热氮化硅陶瓷绝缘板及其制备方法。
背景技术
随着芯片特征尺寸不断缩小，集成度不断增大，芯片进入了超大规模集成电路时代。高集成度意味着器件承载功率变大，发热量增加，因此高集成电路存在着极大的散热问题，因此开发耐热并且具有高热导率的基板材料对集成电路的进一步发展有重要意义。目前常用的陶瓷基板材料是氧化铝(Al2O3)和氮化铝(AlN)，但这两种材料都存在一些缺点，氧化铝基板导热率太低(～20W/mk)，氮化铝基板导热率相对较高(～120W/mk)，但抗弯强度很差(～300MPa)，这两种材料都无法满足高集成电路散热和承载需求。
氮化硅陶瓷由于其高强、高韧、高温性能、较高的理论热导率等一系列优异性能，引起广泛的关注，是理想的基板材料。但是，氮化硅陶瓷存在高温下易分解(1870℃左右)，生产成本高，抗弯强度和热导率无法兼具等问题。
发明内容
本发明的目的在于提供一种高导热氮化硅陶瓷绝缘板及其制备方法，本发明的氮化硅陶瓷绝缘板兼具高抗弯强度和高热导率，且具有较低的烧结温度。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种高导热氮化硅陶瓷绝缘板，包括以下重量百分比的制备原料：氮化硅粉86～96％、第一烧结助剂1～5％、第二烧结助剂2.5～8％和第三烧结助剂0.5～1％；
所述第一烧结助剂为氧化镁；
所述第二烧结助剂为氧化铪；
第三烧结助剂为氧化硼、氧化铁、氧化钙和氧化钛中的一种或多种。
优选的，所述氮化硅粉的D50＜1μm，α相含量大于90％，比表面积＜15m2/g，氧含量＜1wt.％，Fe＜0.0005wt.％，Al＜0.001wt.％，Ca＜0.0001wt.％。
优选的，所述第一烧结助剂、第二烧结助剂和第三烧结助剂的D50独立地小于＜1μm。
本发明提供了上述方案所述高导热氮化硅陶瓷绝缘板的制备方法，包括以下步骤：
将氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂、溶剂和粘结剂混合，得到混合浆料；
将所述混合浆料进行造粒，得到造粒粉；
将所述造粒粉进行压制成型，得到陶瓷素坯；
将所述陶瓷素坯进行冷等静压，得到致密素坯；
将所述致密素坯依次进行排胶和烧结，冷却后得到高导热氮化硅陶瓷绝缘板；
所述烧结的温度为1800～1950℃，所述冷却的速率在30℃/min以下。
优选的，所述混合为：将所述氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂和溶剂进行第一搅拌磨，得到中间浆料；向所述中间浆料中加入粘结剂进行第二搅拌磨，得到混合浆料。
优选的，所述溶剂包括乙醇，所述乙醇的用量以满足中间浆料的固含量为40～70％为准；所述粘结剂包括聚乙烯醇缩丁醛酯，所述粘结剂的用量为所述中间浆料的3～5wt.％。
优选的，所述压制成型的压力为10～15T，保压时间为15～20s。
优选的，所述冷等静压的压力为300～350MPa，保压时间为20min。
优选的，所述排胶的温度为400～600℃，保温时间为6～12h。
优选的，所述烧结的保温时间为12～24h。
本发明提供了一种高导热氮化硅陶瓷绝缘板，包括以下重量百分比的制备原料：氮化硅粉86～96％、第一烧结助剂1～5％、第二烧结助剂2.5～8％和第三烧结助剂0.5～1％；所述第一烧结助剂为氧化镁；所述第二烧结助剂为氧化铪；第三烧结助剂为氧化硼、氧化铁、氧化钙和氧化钛中的一种或多种。
本发明采用氧化镁作为第一烧结助剂，在烧结过程中氧化镁与原料氮化硅粉体反应生成液相，降低烧结温度，节约生产成本，同时还能提高氮化硅陶瓷绝缘板的致密度和抗弯强度；本发明以氧化铪作为第二烧结助剂，利用其与氧结合能力较强，在烧结过程中与原料氮化硅粉体中的杂质氧结合，消除晶格氧含量，提高氮化硅陶瓷绝缘板的热导率；本发明的第三烧结助剂在烧结过程中能够促进液相反应，与氮化硅粉体反应形成固溶体，减少晶界处的非晶相，在保证高热导率的同时提高产品抗弯强度。
此外，本发明相对于现有技术还能制备超薄大尺寸陶瓷基板并节省生产成本。现有技术制备的大尺寸陶瓷基板往往是对较厚的基板进行研磨加工，浪费很多原料，或者通过激光切割的方式切出薄板，生产成本较高，无法直接压制出较薄的基板，这是由于大尺寸的基板太薄在烧结过程中会出现弯曲开裂。现有技术中为了防止弯曲开裂，就要提高陶瓷基板的抗弯强度，但抗弯强度一旦提高就要牺牲热导率，所以导致热导率和抗弯强度均较高的超薄大尺寸基板难以获得。而本发明采用上述配方可以兼顾高热导率和抗弯强度，抗弯强度的提高，使得在烧结过程中不会发生开裂和弯曲，从而解决了现有技术中难以通过直接压制制备超薄大尺寸基板的难题。本发明制备的高导热氮化硅陶瓷绝缘板，尺寸高达190*138mm*0.25mm。
本发明还提供了上述方案所述高导热氮化硅陶瓷绝缘板的制备方法，通过控制烧结的温度和冷却的速率，有利于氮化硅陶瓷晶粒充分生长，减少晶界，进而提高热导率。
实施例的结果表明，本发明制备的高导热氮化硅陶瓷绝缘板抗弯强度≥600MPa，热导率≥100MPa·m-1/2，介电常数为7～9。
具体实施方式
本发明提供了一种高导热氮化硅陶瓷绝缘板，包括以下重量百分比的制备原料：氮化硅粉86～96％、第一烧结助剂1～5％、第二烧结助剂2.5～8％和第三烧结助剂0.5～1％；
所述第一烧结助剂为氧化镁；
所述第二烧结助剂为氧化铪；
第三烧结助剂为氧化硼、氧化铁、氧化钙和氧化钛中的一种或多种。
在本发明中，未经特殊说明，所用原料均为本领域熟知的市售商品。
以重量百分比计，本发明提供的高导热氮化硅陶瓷绝缘板包括氮化硅粉86～96％，优选为87～95％。在本发明中，所述氮化硅粉的D50优选＜1μm，α相含量优选大于90％，比表面积优选＜15m2/g，氧含量优选＜1wt.％，Fe含量优选＜0.0005wt.％，Al含量优选＜0.001wt.％，Ca含量优选＜0.0001wt.％。
以重量百分比计，本发明提供的高导热氮化硅陶瓷绝缘板包括第一烧结助剂1～5％，更优选为2～4％。在本发明中，所述第一烧结助剂为氧化镁，所述氧化镁的D50优选＜1μm。在本发明中，所述氧化镁在烧结过程中与原料氮化硅粉体反应生成液相，降低烧结温度，节约生产成本，同时还能提高氮化硅陶瓷绝缘板的致密度和抗弯强度。
以重量百分比计，本发明提供的高导热氮化硅陶瓷绝缘板包括第二烧结助剂2.5～8％，优选为4～6％。在本发明中，所述第二烧结助剂为氧化铪，所述第二烧结助剂的D50优选＜1μm。本发明利用硼化铪与氧结合能力较强的特点，在烧结过程中硼化铪与原料氮化硅粉体中的杂质氧结合，能够消除晶格氧含量，提高氮化硅陶瓷绝缘板的热导率。当硼化铪的用量超出上述范围后，不利于氮化硅的烧结，会降低陶瓷绝缘板的热导率。
以重量百分比计，本发明提供的高导热氮化硅陶瓷绝缘板包括第三烧结助剂0.5～1％，优选为0.6～0.8％。在本发明中，所述第三烧结助剂为氧化硼、氧化铁、氧化钙和氧化钛中的一种或多种，更优选为其中的一种。当所述第三烧结助剂为上述物质中的多种时，本发明对各助剂的配比没有特殊要求，任意配比均可。本发明的第三烧结助剂在烧结过程中能够促进液相反应，与氮化硅粉体反应形成固溶体，减少晶界处的非晶相，在保证高热导率的同时提高产品抗弯强度。当所述第三烧结助剂的用量超出上述范围后，不利于烧结过程的进行，会降低陶瓷绝缘板的热导率。
本发明提供了上述方案所述高导热氮化硅陶瓷绝缘板的制备方法，包括以下步骤：
将氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂、溶剂和粘结剂混合，得到混合浆料；
将所述混合浆料进行造粒，得到造粒粉；
将所述造粒粉进行压制成型，得到陶瓷素坯；
将所述陶瓷素坯进行冷等静压，得到致密素坯；
将所述致密素坯依次进行排胶和烧结，冷却后得到高导热氮化硅陶瓷绝缘板；
所述烧结的温度为1800～1950℃，所述冷却的速率在30℃/min以下。
本发明将氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂、溶剂和粘结剂混合，得到混合浆料。
在本发明中，所述混合优选为：将所述氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂和溶剂进行第一搅拌磨，得到中间浆料；向所述中间浆料中加入粘结剂进行第二搅拌磨，得到混合浆料。
在本发明中，所述溶剂优选包括乙醇。所述乙醇的用量优选以满足中间浆料的固含量为40～70％为准，更优选为45～65％，进一步优选为50～60％。
在本发明中，所述粘结剂优选包括聚乙烯醇缩丁醛酯，所述粘结剂的用量优选为所述中间浆料的3～5wt.％，更优选为4wt.％。本发明利用粘结剂使得原料团聚，从而有利于后面的造粒。
在本发明中，所述第一搅拌磨和第二搅拌磨优选采用氮化硅球为研磨介质，球料比优选为1:1。
在本发明中，所述第一搅拌磨的时间优选为24～36h，第二搅拌磨的时间优选为24～48h。所述第一搅拌磨和第二搅拌磨的转速独立地优选为25～35转/分钟，更优选为30转/分钟。
得到混合浆料后，本发明将所述混合浆料进行造粒，得到造粒粉。
在本发明中，所述造粒的方式优选为喷雾造粒。在本发明中，所述喷雾造粒的条件优选包括：供料泵压力为0.6～0.8MPa，进口温度为150～180℃，出口温度为50～70℃，旋风压差为0.8～1KPa。作为进一步优选的方案，所述喷雾造粒的条件为：供料泵压力为0.65～0.75MPa，进口温度为160～170℃，出口温度为55～65℃，旋风压差为0.85～0.95KPa。
喷雾干燥后，本发明优选还包括过100目筛，取筛下物作为造粒粉。本发明利用喷雾造粒的方式有利于得到流动性好、适合压制成型的造粒粉。在本发明中，所述造粒粉性能满足：松装密度为0.8～1g/m3，流时为55.68～58.07s。
得到造粒粉后，本发明将所述造粒粉进行压制成型，得到陶瓷素坯。本发明优选将造粒粉通入干粉压机模具中，然后采用压头压制成型。在本发明中，所述压制成型的压力优选为10～15T，更优选为11～14T，保压时间优选为15～20s，更优选为16～18s。本发明对所述干粉压机模具的尺寸没有特殊要求，根据目标陶瓷绝缘板的尺寸确定。在本发明中，当目标陶瓷绝缘板的尺寸为190*138mm*0.25mm时，所述干粉压机模具的尺寸为272*198mm。所述干粉压机模具的高度优选大于0.5mm。
本发明采用压制成型，可以获得大尺寸的陶瓷素坯，配合氮化硅陶瓷绝缘板的配方，使获得大尺寸的高导热氮化硅陶瓷绝缘板成为可能。
得到陶瓷素坯后，本发明将所述陶瓷素坯进行冷等静压，得到致密素坯。
本发明优选将陶瓷素坯放入真空袋，在真空袋中放入钢板作为衬底，然后抽真空放入冷等静压机腔体内进行冷等静压。在本发明中，所述抽真空的真空度优选为-0.1MPa。所述钢板的尺寸优选与所述陶瓷素坯的尺寸相同。
本发明采用钢板作为衬底可以防止陶瓷素坯在冷等静压过程中发生变形和断裂。
在本发明中，所述冷等静压的压力优选为300～350MPa，更优选为310～340MPa；保压时间优选为20min。本发明将冷等静压的条件控制在上述范围，可以增加陶瓷素坯的致密性，有助于后续烧结成型。
得到致密素坯后，本发明将所述致密素坯依次进行排胶和烧结，冷却后得到高导热氮化硅陶瓷绝缘板。
本发明优选将所述致密素坯层叠放入坩埚中，在层叠致密素坯的最上面放置石墨板，然后放入多功能气压烧结炉中进行排胶和烧结。
在本发明中，所述石墨板的重量优选为致密素坯质量的1～2倍，更优选为1.2～1.8倍。本发明放置石墨板可以防止致密素坯在排胶和烧结过程中发生开裂和变形。
在本发明中，所述排胶的温度优选为400～600℃，更优选为450～550℃；保温时间优选为6～12h，更优选为8～10h。本发明升温至排胶的温度的升温速率优选不超过10℃/min。当升温速率大于10℃/min后，致密素坯容易发生开裂。
在本发明中，所述排胶优选在空气氛围下进行。本发明所述排胶过程中，致密素坯中的有机物被排出。
完成所述排胶后，本发明直接在排胶温度的基础上升温至烧结的温度，进行烧结。
在本发明中，所述升温至烧结的温度的升温速率优选不超过10℃/min。当升温速率大于10℃/min后，坯料容易发生开裂。
在本发明中，所述烧结的温度为1800～1950℃，优选为1850～1900℃；保温时间优选为6～12h，更优选为6～10h。本发明优选在空气氛围下进行烧结。本发明在所述烧结过程的初始阶段，由于第一烧结助剂和第三烧结助剂与氮化硅粉体表面的SixOy发生反应，反应产物熔点较低，形成液相，随着反应进行，液相流动，填充颗粒之间的孔洞，进而促进材料烧结致密，提高产品抗弯强度，以上过程伴随着α相氮化硅向β相氮化硅的转变，进而提高热导率。
完成所述烧结后，本发明将烧结后产物进行冷却，所述冷却的速率在30℃/min以下，优选为10～30℃/min。本发明将冷却速度控制在上述范围，有利于氮化硅陶瓷晶粒充分生长，减少晶界，进而提高热导率。
冷却后，本发明优选还包括将所得陶瓷毛坯进行后加工，得到高导热氮化硅陶瓷绝缘板。本发明对所述后加工的方式没有特殊要求，采用本领域熟知的后加工方式，能够保证高导热氮化硅陶瓷绝缘板在厚度和表面粗糙度方面达到精度要求即可，具体的可以为但不局限于研磨。在本发明中，所述高导热氮化硅陶瓷绝缘板的粗糙度优选＜5μm。
下面结合实施例对本发明提供的高导热氮化硅陶瓷绝缘板及其制备方法进行详细的说明，但是不能把它们理解为对本发明保护范围的限定。
以下实施例所用氮化硅粉的D50＜1μm，α相含量大于90％，比表面积＜15m2/g，氧含量＜1wt.％，Fe＜0.0005wt.％，Al＜0.001wt.％，Ca＜0.0001wt.％；所用氧化镁、氧化铪、氧化硼、氧化铁、氧化钙和氧化钛的D50均＜1μm。
实施例1～13及比较例1～5
按表1所示原料配比和种类，将氮化硅粉和烧结助剂加入到搅拌磨中，以酒精为溶剂介质，氮化硅球为研磨介质(球料比为1:1)，研磨30h，得到中间浆料(固相含量60％)；再向所述中间浆料中加入4wt.％聚乙烯醇缩丁醛酯(PVB)研磨48h，得到混合浆料。将所述混合浆料通过喷雾造粒工艺(供料泵压力为0.7MPa，进口温度为170℃，出口温度为60℃，旋风压差为0.9KPa)，过100目筛，制备出适合压制成型的造粒粉(松装密度为0.8～1g/m3，流时为55.68～58.07s)。将所述造粒粉通入干粉压机模具，进行压制成型，干粉压机模具尺寸为272*198mm*0.8mm，压制压力为10T，保压时间20s，得到陶瓷素坯。将所述陶瓷素坯和钢板放入真空袋抽真空后进行冷等静压，等静压压力为300MPa，保压20min，得到致密素坯。将所述致密素坯叠层放置在坩埚上，在最上放置石墨板，然后放入多功能气压烧结炉中，先以10℃/min升温至600℃保温12h进行排胶，然后继续升温至烧结温度保温24h，烧结完成后冷却，冷却速度控制在30℃/min以下，得到陶瓷毛坯。通过研磨工艺对陶瓷毛坯进行加工，最终得到尺寸为190*138mm*0.25mm，粗糙度＜5μm的高导热氮化硅陶瓷绝缘板，具体的烧结温度和冷却速率以及性能指标见表1。
表1实施例1～13及比较例1～5的反应条件和性能
Figure BDA0002860109430000081
Figure BDA0002860109430000091
由表1的结果可知，本发明制备的高导热氮化硅陶瓷绝缘板抗弯强度≥600MPa，热导率≥100MPa·m-1/2。比较例1相比本发明的实施例，由于冷却速度太大，导致产品的导热率不高；比较例2由于烧结温度太低，导致产品导热率较低；比较例3由于第二烧结助剂氧化铪含量太高，不利于产品烧结，导致产品热导率很低；比较例4由于第三烧结助剂氧化钙含量太高，且冷却速度较大，产品三点弯曲强度很高，但热导率太低；比较例5由于第三烧结助剂氧化钙含量太高，导致产品热导率很低。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (10)

1.一种高导热氮化硅陶瓷绝缘板，其特征在于，包括以下重量百分比的制备原料：氮化硅粉86～96％、第一烧结助剂1～5％、第二烧结助剂2.5～8％和第三烧结助剂0.5～1％；
所述第一烧结助剂为氧化镁；
所述第二烧结助剂为氧化铪；
第三烧结助剂为氧化硼、氧化铁、氧化钙和氧化钛中的一种或多种。
2.根据权利要求1所述的高导热氮化硅陶瓷绝缘板，其特征在于，所述氮化硅粉的D50＜1μm，α相含量大于90％，比表面积＜15m2/g，氧含量＜1wt.％，Fe＜0.0005wt.％，Al＜0.001wt.％，Ca＜0.0001wt.％。
3.根据权利要求1所述的高导热氮化硅陶瓷绝缘板，其特征在于，所述第一烧结助剂、第二烧结助剂和第三烧结助剂的D50独立地小于＜1μm。
4.权利要求1～3任一项所述高导热氮化硅陶瓷绝缘板的制备方法，包括以下步骤：
将氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂、溶剂和粘结剂混合，得到混合浆料；
将所述混合浆料进行造粒，得到造粒粉；
将所述造粒粉进行压制成型，得到陶瓷素坯；
将所述陶瓷素坯进行冷等静压，得到致密素坯；
将所述致密素坯依次进行排胶和烧结，冷却后得到高导热氮化硅陶瓷绝缘板；
所述烧结的温度为1800～1950℃，所述冷却的速率在30℃/min以下。
5.根据权利要求4所述的制备方法，其特征在于，所述混合为：将所述氮化硅粉、第一烧结助剂、第二烧结助剂、第三烧结助剂和溶剂进行第一搅拌磨，得到中间浆料；向所述中间浆料中加入粘结剂进行第二搅拌磨，得到混合浆料。
6.根据权利要求5所述的制备方法，其特征在于，所述溶剂包括乙醇，所述乙醇的用量以满足中间浆料的固含量为40～70％为准；所述粘结剂包括聚乙烯醇缩丁醛酯，所述粘结剂的用量为所述中间浆料的3～5wt.％。
7.根据权利要求4所述的制备方法，其特征在于，所述压制成型的压力为10～15T，保压时间为15～20s。
8.根据权利要求4所述的制备方法，其特征在于，所述冷等静压的压力为300～350MPa，保压时间为20min。
9.根据权利要求4所述的制备方法，其特征在于，所述排胶的温度为400～600℃，保温时间为6～12h。
10.根据权利要求4所述的制备方法，其特征在于，所述烧结的保温时间为12～24h。
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