CN1538908A - 高固含量六方晶氮化硼浆料、糊料、球形粒粉体,以及它们的制备与使用方法 - Google Patents

高固含量六方晶氮化硼浆料、糊料、球形粒粉体,以及它们的制备与使用方法 Download PDF

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CN1538908A
CN1538908A CNA028155955A CN02815595A CN1538908A CN 1538908 A CN1538908 A CN 1538908A CN A028155955 A CNA028155955 A CN A028155955A CN 02815595 A CN02815595 A CN 02815595A CN 1538908 A CN1538908 A CN 1538908A
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boron nitride
powder
hexagonal boron
slurry
spherical
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CN1307047C (zh
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V��K���ռ���
V·K·普加里
W·T·科林斯
Ŀ�
J·J·库茨克
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Saint Gobain Ceramics and Plastics Inc
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Saint Gobain Industrial Ceramics Inc
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Abstract

本发明涉及制备六方晶氮化硼及其浆料的方法。该方法涉及约0.5～5重量％的表面活性剂与约30重量％的六方晶氮化硼粉体在有利于形成六方晶氮化硼浆料条件下于介质内混合。本发明还涉及制备球形粒氮化硼粉体的方法，以及采用六方晶氮化硼浆料制备六方晶氮化硼糊料的方法。本发明另一方面涉及六方晶氮化硼糊料，它包含约60～80重量％的固体六方晶氮化硼。本发明还有一方面涉及球形氮化硼粉体，包含聚合物与球形六方晶氮化硼粉体的聚合物混合物，以及包含该聚合物混合物的体系。

Description

高固含量六方晶氮化硼浆料、糊料、球形粒粉体， 以及它们的制备与使用方法
本发明涉及制备六方晶(hexagonal)氮化硼浆料、糊料以及球形粒六方晶氮化硼粉体的方法。本发明还涉及制备得到的六方晶氮化硼浆料、糊料及球形粒六方晶氮化硼粉体，以及六立晶型氮化硼的球形粉体在聚合物混合体系和含热源与热阱的体系中的应用。
微电子器件，诸如集成电路片越变越小，功能也更强。当今发展趋势是生产出的集成片愈发高度集成化，在指定时间内能比原有芯片执行更多指令。这造成集成电路片内使用的电流增磊，结果，这些集成片比原有芯片产生更多的电阻热。为此，应对热的排放成了开发电子器件的主要问题。
通常，热源或诸如集成电路片的器件配备有热阱，以去除它们运行时产生的热。然而，热源或器件与热阱之间的接触热阻限止了热阱的散热效率。组装期间，通常涂覆一层热导膏，如硅烷，或涂一层热导有机蜡，以便在热源与热阱相对的匹配表面之间建一个低热阻通道。其它热导材料基于使用粘结剂，最好为树脂型粘结剂，如硅烷、热塑橡胶、尿烷、丙烯酸树脂或环氧树脂，至少有一种以上的热导填料分散于这些粘结剂中。
通常，这类填料为两大主要类别中之一：热导、电绝缘类，或热导、电导类填料。氧化铝、氧化镁、氧化锌、氮化铝以及氮化硼是最常被提及的热导、电绝缘类填料，用于热产品。氮化硼，且更具体地说是六方晶氮化硼(hBN)特别适用于那些具有优异热传导特性且又相对价廉的产品。
对于填料，要求其有高热导率(或尽可能的低热阻性)。为了使诸如hBN一类填料获得足够高的热导性，要求在粘结剂中采用高负载量的填料。然而，由于hBN呈片状颗粒结构，意欲获得高于20体积％固含量是件难事。
Shaffer等人的美国专利US Pat.No.5,898,009；6,048,511和欧洲专利EP 0939 066 A1公开了一种变通方法，以进一步提高hBN固体的负载量。它涉及到(a)经破碎后的hBN粉的冷压，(b)冷压块经破碎成更细小块，以及(c)细小块经过筛，得到符合粒度分布要求的团聚物。然而此团聚物呈非球形(棱形)，边缘短且参差不齐。由于如下原因，这类形状颗粒无法得到最佳固体负载量：(1)非球形团聚物颗粒之间润滑性不够，因而导致粘度提高；以及(2)非球形团聚物颗粒表面积较大，因而其表面吸附较多聚合物造成游离态聚合物，数量下降，反过来又提高了粘度。
因此，对于热导填充材料必须要求负载量高，以获得足够高的热导率，而并不提高其粘度。本发明的目的就是要克服这方面的缺陷。
本发明涉及制作六方晶氮化硼浆料的方法。本方法涉及0.5～5重量％的表面活性剂与30-50重量％的六方晶氮化硼粉体在有利于形成六方晶氮化硼浆料条件下于介质内混合。
本发明还涉及六方晶氮化硼浆料，所述浆料包含在介质中混合的约0.5～5wt％表面活性剂和约30～50wt％六方晶氮化硼粉体。
本发明还涉及制备球形粒氮化硼粉体的方法，它包括提供六方晶氮化硼浆料，在有利于形成球形粒氮化硼粉体(包括氮化硼片晶的球形团聚物)条件下进行喷雾干燥，以及对球形氮化硼粉体进行烧结。
本发明还涉及球形氮化硼粉体，它包括氮化硼片晶的球形团聚物。
本发明还涉及六方晶氮化硼糊料的制备方法。该方法涉及提供六方晶氮化硼浆料并在有利于形成高含60～80重量％固体六方晶氮化硼的六方晶氮化硼糊料条件下处理浆料。
本发明还涉及介质中高含60～80重量％固体六方晶氮化硼的六方晶氮化硼糊料。
本发明还涉及粉体相与聚合物形成的聚合物混合物。该粉体相包含六方晶氮化硼片晶的球形团聚物。粉体相均匀分布于聚合物内。
本发明还涉及包含热源、热阱，以及将热源与热阱相连的热导材料，其中热导材料含有包括六方晶氮化硼片晶球形团聚物的粉体相。
本发明的六方晶氮化硼浆料具有高固含量、低粘度特点。此外，该浆料可用于生产高产率的六方晶氮化硼粉体与糊料。本发明hBN球形团聚物有利于降低团聚物间的磨擦，因而在聚合物内允许更高的固含量，进而达到更高热导率。此外，球形hBN团聚物的表面积最小，因而降低了团聚物表面对聚合物的吸附量，从而有更多游离聚合物，可以改善流动性/降低粘度。而且，本发明球形hBN粉体中，球形团聚物中hBN片的分布是不规则的(与先前工艺中压制而成的团聚物中的有序片状晶相比)。因此，本发明填有球形hBN的聚合物应呈现更多的各向异性热导特性，在聚合物厚度方向上具有更高热导率。
附图简要说明
图1为氮化硼的结构示意图。许多这样的单元形成了氮化硼(BN)的片。
图2为固含量为50％且含各种表面活性剂的氮化硼浆料的流变特性。
本发明涉及六方晶氮化硼浆料的制备方法，该方法涉及约0.5～5重量％的表面活性剂与30-50重量％的六方晶氮化硼粉体在有利于形成六方晶氮化硼浆料条件下于介质内混合。
正如本发明采用的术语，浆料是指某种液体(即水介质或非水介质)与不可溶性物质的较稀混合液或悬浊液。
六方晶氮化硼，是呈化学惰性、光滑的陶瓷材料，具有片状六方晶结构(与石墨结构类似)(“hBN”)。参见图1，hBN的各向异性很容易得到清楚解释，hBN晶粒呈六面体。图1中的D所示为hBN晶粒的直径，并被示为方向a。氮化硼在平面a上为共价键，晶粒厚度示为Lc，并与晶粒直径成垂直角度，被示为方向c。氮化硼六面体靠相对较弱的范德瓦尔力堆聚而成(即沿方向c)。如果大于范德瓦尔力的剪切力施加于氮化硼六方体的晶面上，则较弱的范德瓦尔力消失，晶粒之间相对滑动性较好。hBN晶面相互间滑动性能相对较好是hBN高流动性的原因所在。
更令人称心的是，hBN是高度有序的六方晶结构的粉体。它的粉体晶粒参数(这里全文引用Hubacek在J.Cer.Soc.of Japan(日本陶瓷学会会刊)104：695-98(1996)上发表的题为Hypothetical Model of Turbostratic Layered BoronNitride(“湍流层氮化硼的假想模型”))至少为0.12(呈高度六方晶hBN的量化值)，且最佳大于0.15。hBN粉体的结晶度宜在0.20～0.55之间，最好在0.30～0.55之间。
通常，起始粉料由大体上呈湍流(无定形态)的氮化硼粉体原料经“高温处理”而制得(参见这里全文引用的Hagio等人在 J.Mat.Sci.Lett(材料科学通讯)16：795-798(1997)上发表的题为“Mierostructural Development withCrystallization of Hexagonal Boron Nitride”(“六方晶氮化硼结晶的微结构进展”))，而成为通常所述的“高纯六方晶氮化硼”。在较佳实施方式中，湍流态氮化硼细粉具有的结晶参数小于0.12，在氮气中于1400～2300℃下热处理长达0.5～12小时。通常这种热处理能制得结晶度更高的hBN的片状晶，因为小于1μm的湍流态细粉体片状晶的微晶在热处理期间变得更为有序晶化，晶粒长大(＞1μm)。
hBN起始原料颗粒的平均粒径较佳在2～20μm之间，更佳在2～12μm之间，最佳在4～12μm之间。这里采用的术语“粒径”或“直径”是指hBN片状颗粒在图1所示的D的尺寸。该尺寸通常采用如Leeds&NorthrupMicrotracX100(佛罗里达州Clearwater)扫描电子显微镜和激光散射技术测定。
另一实施方式中，hBN起始原料的含氧量在约0～1.0wt％之间，宜在约0～0.5重量％之间。hBN起始原料中的含氧量愈低，则制成的氮化硼的振实密度愈大。作为热处理用途的填料，高振实密度粉体具有许多优点：在于有较高热导率，在聚合物中有较高负载量，hBN片的团聚物结合力更牢(改善氮化硼聚合物复合材料金属粘接性能)，以及降低团聚物中孔隙率(孔隙率导致聚合物树脂或液体对团聚物的浸润性下降)。
本发明hBN浆料最好包含约40～50重量％的六方晶氮化硼粉体。
在另一实施方式中，hBN起始原料的表面积在约5～30m2/g，更佳在约7～20m2/g之间。
本发明的hBN浆料可以包含水介质或非水介质。合适的非水介质有：异丙醇、甲醇、以及乙醇。
本发明的六方晶氮化硼浆料为高固含量hBN浆料，在一个实施方式中，它含约30～50重量％六方晶氮化硼固体。在另一个实施方式中，它含约40～60重量％六方晶氮化硼固体。
本发明方法中合适的表面活性剂包括：聚羧酸(新泽西州Canbury罗地亚公司的Rhodaline 111MTM)，硅烷(迈阿密州Midland的陶氏化学公司的Z-6040SilaneTM)，以及有机金属化合物(如罗德岛Woonsocket的Cavedon化学公司的APGTM)。
本发明的hBN浆料还可以包含添加剂，诸如粘结剂和烧结添加剂。合适的粘结剂有聚乙二醇，聚乙烯醇，丙三醇和胶乳。当采用本发明的hBN浆料生产hBN粉体时，该浆料还可含有烧结添加剂，它包含，但不限于下列物质：氧化钇，CaO，MgO，CeB6，以及B。
本发明还涉及约0.5～5重量％表面活性剂和约30～50重量％六方晶氮化硼粉体在介质中混合而成的六方晶氮化硼浆料。
本发明hBN浆料固含量高，粘度低。特别地，在本发明hBN浆料中固含量可高达约30-50重量％。尽管不愿受理论束缚，可以认为由于hBN的片状晶和它的非浸润性，本发明表面活性剂用量在约0.5-5重量％就可获如此高固含量的浆料。与本领域其它工艺相比，使用约0.1-0.5重量％表面活性剂，氮化硼的固含量仅在约20-25重量％之间。
如下详述，本发明高固含量hBN浆料可用于制备高产率六方晶氮化硼粉体与糊料。
本发明另一方面涉及制备球形粒氮化硼的方法，它包括提供六方晶氮化硼浆料，在有利于形成球形粒氮化硼粉体(包括氮化硼片晶的球形团聚物)的条件下进行喷雾干燥，并对球形氮化硼粉体进行烧结。
本发明所用的团聚物是指氮化硼片晶粘结成的集合体。非团聚态氮化硼片晶仅含一个或多个晶粒。
在一个实施方式中，球型氮化硼晶粒团聚后的平均直径在约10-500μm之间。
在另一个实施方式中，大部分氮化硼团聚物的平均直径在约30-150μm之间。
按照本发明六方晶氮化硼浆料最好为高固含量六方晶氮化硼浆料。
喷雾干燥为本领域已知的技术，例如，在James S.Reed的“Introduction tothe Principles of Ceramic Processing”(《陶瓷工艺原理导论》)(由John Wiley父子公司于1988年出版)一书中有叙述，这里全文引用以供参考。
烧结最好在温度约1800℃下进行约1-4小时，较佳为2-3小时。较佳在约1800-2400℃下，更佳在约2000-2400℃下，最佳在2000-2100℃下进行。合适的烧结气氛为惰性气体、氮气、以及氩气。在其中一个实施方式中，在真空条件下进行烧结。在另一个实施方式中，在至少为一个大气压条件下进行烧结。
生产出的粉体的振实密度最好在0.4g/cc-0.7g/cc之间。
本发明的烧结步骤可改善热扩散率，从而提高生成后的氮化硼粉体的热导率，以及它的硬度与强度。尽管不愿受理论束缚，可以认为在烧结期间，氮化硼的各种颗粒相互渗透长大，形成交织的网络构型。烧结后粉体的交织性使得热扩散性与热导性提高。
在一种实施方式中，球形氮化硼粉体应在有效条件下分粒，以获得理想的团聚物颗粒分布。这里所用的团聚物颗粒分布是指按照团聚物特征直径，即团聚物所伸展的长度所定义的最小团聚物到最大团聚物之间所覆盖的团聚物大小的范围。分类的合适方法有：筛分法，空气分粒法，以及淘析法(参见“Chem.Eng.Handbook”(由Perry & Chilton编撰，McGraw-Hill于1973年出版的《化学工程手册》第五版)一书，这里全文引用以供参考。因为这种分类法已为本领域所知，这里仅作简单讨论。
筛分法是将各种不同粒径的固体颗粒物/团聚物的混合物通过筛网分离成两部分或更多部分。筛网使较小颗粒物/团聚物穿过网眼，而将较大颗粒物/团聚物挡在筛网上。该过程通过改变筛网网眼大小，对筛上物和筛下物可多次重复过筛，直至使颗粒物/团聚物筛分达到理想的粒径范围。
空气分粒器依靠空气牵引力与颗粒惯性使将细颗粒/团聚物从粗颗粒/团聚物中分离出来。所述颗粒惯性取决于颗粒/团聚物粒径。
淘析的一种设计为直立式重力型淘析仪，其中向上流经柱管的流体，将小于临界粒径的细小颗粒/团聚物携带而出。临界粒径取决于颗粒/团聚物在该流体中的沉降速率。
理想的团聚物尺寸或团聚物粒径分布(ASD)取决于球形氮化硼粉体的目标用途。例如，对于界面垫(其中聚合物为低弹力硅烷橡胶)，理想的ASD的最大粒径团聚物要小于界面垫的厚度。在包含球型氮化硼的聚合物的挠曲性比较重要的情况下。大于例如150μm的团聚物浓度减少，或全部去除，因为采用较小粒径团聚物可改善聚合物混合体系的挠曲性。此外，球形氮化硼的多种粒径分布范围可组合起来，以获得理想的挠曲性和热导性，因为较小粒径团聚物会填埋于较大粒径团聚物的晶隙内。
ASD较佳为30-125μm(更佳为74-125μm，最佳为74-105μm)，或为20-74μm(更佳为38-74μm，最佳为38-53μm)，或为10-38μm(更佳为20-38μm)之间。
本发明还涉及含有氮化硼片晶的球形团聚物的球形氮化硼粉体。
本发明的球形氮化硼粉体可用作热处理用途中的填料，例如用于如下所述的复合材料聚合物以及流体中。由于压实密度提高了，以及粉体能均匀填埋，球形氮化硼粉体也可用于热压。而且，球形氮化硼粉体也可用作将六方晶氮化硼转化成立方晶氮化硼的前驱体原料。在高纯六方晶氮化硼转化成立方晶氮化硼中，压实后的氮化硼在立方晶氮化硼相图的稳定区域内须经受极度高压与高温。氮化硼压片的密度对立方晶氮化硼转化工艺的经济成本是有特殊意义的。
本发明还涉及制备六方晶氮化硼糊料的方法，该方法涉及提供六方晶氮化硼浆料，以及在有利于形成高含60～80重量％固体六方晶氮化硼的六方晶氮化硼糊料条件下进行浆料的处理。
这里所用的糊料指的是半固体状制备物。
按照本发明，六方晶氮化硼浆料最好为高固含量六方晶氮化硼。
在一个实施方式中，处理方法包括将浆料灌入灰泥滑模板内，滑模会吸收浆料中水分，形成本发明的六方晶氮化硼糊料。已知模体孔隙率在约1-5μm时，六方晶氮化硼糊料的固含量可受浇铸时间长短的控制。
在另一个实施方式中，处理方法包括对浆料进行真空抽滤，直至要求的溶液量被从浆料中除去，形成本发明的六方晶氮化硼糊料。
本发明另一个实施例涉及在介质中含有约60-80重量％固体六方晶氮化硼的六方晶氮化硼糊料。
本发明hBN可以包含水溶液介质或非水溶液介质。合适的非水溶液介质为异丙醇、甲醇以及乙醇。
六方晶氮化硼糊料最好含有65-75重量％固体六方晶氮化硼。
本发明的六方晶氮化硼糊料可以用来形成不同形状的固体物，例如，通过挤出工艺。然后，这类固体物可用作诸如热处理应用中的填料。
本发明还涉及粉体相与聚合物形成的聚合物混合物。该粉体相包含六方晶氮化硼片晶的球形团聚物。粉体相均匀分布于聚合物内。
合适的聚合物体系包括可熔融处理的聚合物、聚酯、酚醛树脂、聚硅烷(如硅烷橡胶)、丙烯酸树脂、蜡类、热塑性聚合物、低分子量流体、以及环氧树脂模塑化合物。
在另一实施方式中，聚合物混合物包含约30-80重量％的球形氮化硼粉体。然而，聚合物混合物中球形氮化硼粉体的含量取决于所要求的混合物的挠曲性与热导率。例如，hBN的负载量较低，如30-50重量％，对于高挠曲性应用是理想的，但其热导率就偏低。因此，负载量达50-80重量％对于高热导率/低挠曲性应用是理想的。
生成的聚合物混合物的热导率取决于负载量、分散性以及其它因素。在一个实施方式中，聚合物混合物的热导率为约1-15W/mK。
由于本发明聚合物混合物中hBN团聚物呈球形，因此，团聚物之间摩擦减少了，因而可以达到更高负载量，进而具有更高热导率。
此外，球型hBN团聚物具有最小表面积，因而降低了团聚物表面对聚合物的吸附量，以便有更多游离聚合物，以改善流动性/降低粘度。
通常，聚合物中负载的hBN粉体采用压制工艺进行制备(参见全权授给Shaffer等人的美国专利US Pat.No.5,898,009；6,048,511和欧洲专利EP 0 939066 A1，这里全文引用参考)，其中生产的hBN粉体包含排列有序的hBN片的非球形团聚物。然而，本发明的球型hBN粉体中，hBN片颗粒分布是无序的(与压制后团聚物中的排列有序片相比)。因此，按照本发明填有球形hBN粉体的聚合物膜应呈现更多各向异性热导性和沿聚合物厚度方向的更高的热导率。
本发明的另一个实施例涉及包含热源、热阱，以及将热源与热阱体相连的热导材料，其中热导材料含有包括六方晶氮化硼片晶的球型团聚物粉体相。
这里所用的热阱指的是气态、液态或固态的物质，它能吸热，并从周围环境转移热量。
本发明的合适热源包括集成电路片、功率模块、变压器，以及其它电子器件。
按照本发明，合适的热阱包括翅片铝、铜、铍，以及金刚石。
这里所用的热导物质可以是复合物，聚合物或流体。在一个实施方式中，热导物质为合适的聚合物，例如，可熔融处理的聚合物，聚酯，酚醛树脂，聚硅烷(如硅烷橡胶)，丙烯酸树脂，蜡类，热塑性聚合物，低分子量流体，以及环氧树脂模塑化合物。
热导物质最好含有约30-80重量％的球形氮化硼粉体，它的热导率在1-15W/mK之间。
本发明优选实施方式
实施例1-高氮化硼固体负载量浆料的生产
含50重量％氮化硼固体浆料采用下表1列出的各组分混合而成。
表1含50重量％氮化硼固体浆料的各组份
    固体-50重量％     液体-50重量％
    XP1011氮化硼1    1400g     85％去离子水(pH9)       1700g
    HPP325氮化硼2    500g     10％异丙醇4             200g
    Y2O3 3            100g     5％111M5(表面活性剂)    100g
    任选4％丙三醇
1新泽西州Amherst的Saint-Gobain陶瓷与塑料制品公司
2新泽西州Amherst的Saint-Gobain陶瓷与塑料制品公司
3加州蒙的帕斯的钼公司
4马里兰州Ward Hill的Alfa Aesar公司
5新泽西州Cranbury的罗地亚公司的Rhodaline 111M
精确计量表1所列粉体与液体各组分用量。去离子水(DI)的酸度调节至pH为9～9.5之间，将表面活性剂加入到含有异丙醇的最终混料用的大桶内(纽约州Rochester的Nalgene Nunc有售)，体积约10L。采用空气推动浆叶式搅拌器(纽约州Rochester的Lightnin有售)搅拌表面活性剂/异丙醇溶液。将粉体慢慢加入表面活性剂/异丙醇溶液中，直至溶液无法再接受更多粉体时止。可以通过用稀薄的异丙醇涂在大部分氮化硼粉末上来进行，它要比去离子水更容易浸湿氮化硼表面。加入适量调节过pH值的去离子水，以维持浆料混合的粘度。还要求手拿刮刀搅和，将容器壁上粉体搅和进去。
为保证搅拌良好，还得通过高剪切机上下翻腾浆料(宾州Exton的Netzsch公司的Netzsch剪切机)。剪切时间长短决定了浆料的“混合度”和表面积。需要一台辅助冷却机(新罕布什尔州朴茨茅斯的Neslab仪器公司的冷却机)连至剪切机，使浆料温度降低，以减少异丙醇的蒸发。
所有氮化硼粉体加完后，浆料的pH值经测定为8.5，加NaOH使pH调至9。此时的浆料稍为粘稠，但呈良好的剪切稀释度。
测量了浆料粘度对各种不同表面活性剂的剪切率的影响。如表1所示，表面活性剂用量为总固体量的5重量％。结果示于图2，其中Rhodaline111MTM(新泽西州Cranbury的罗地亚公司)被证明在降低粘度方面效果最佳。
随后，将浆料转移至密封容器内备用。
实施例2-烧结添加剂的混合
氮化硼粉体中添加烧结添加剂最好以浆料方式进行，这样有助于形成氮化硼与烧结助剂的均相混合物。如果湿法混合不可能或不现实，则可采用干法混合。
制备干法混料的技术取决于要求的样品量。如果样品量约少于25g，则采用研钵混合粉料。使用前粉料照此混合10分钟。
如果样品量较大，则用涂料搅拌机搅拌粉料。用涂料搅拌机时，在NalgeneNunc(纽约州Rochester)容器内，用直径为3/8”氮化硅磨球，帮助粉料的混合。磨球的用量约为Nalgene容器内粉体柱高的1/4。不同批量选用不同大小容器。涂料搅拌器先运行25分钟，然后开始混料。混料后，过筛取出磨球，收集粉料，再压制。如果压制有难度，则在混料时添加百分之几重量的低分子量聚乙烯醇作粘结剂。
实施例3-氮化硼浆料的喷雾干燥
实施例1中氮化硼浆料经喷雾干燥制得填模用氮化硼粉体。喷雾干燥也是制备均匀、多组份、无压烧结粉体体系的最为快速的方式。与其它陶瓷体系相比，尽管50重量％固体氮化硼浆料似乎负载量很高，但仍含有大量水分。为了在有限静置时间内赶尽所有水分，必须提高进口与出口端温度。伴随这些改变，浆料流速下降，原子化器的转速(rpm)增加。此外，如果准备用于干燥压制，则在喷雾干燥之前，在浆料中加入4重量％丙三醇。在喷雾干燥期间，持续搅拌浆料。
入口端温度设定为235℃，则出口端温度为85℃。浆料流速为60ml/min，且原子化器(迈阿密州底特律的Pentronix)设定为12,500rpm。这种设置通常产生球形氮化硼粉体，其粒径范围为-150μm/+30μm。该范围的低端常有变动，取决于集尘器挡板的设置。收集后粉体的含水率约为0.25-0.5％。
上面所勾画的浆料实施例要求在这些条件下于70分钟内通过喷雾干燥器。经筛分去除大颗粒后，粉体产率约为80％，其中包括容器壁以及旋风机上残留的材料。
上述所有条件仅适合本实施例中所用的喷雾干燥机。对于其他各系统，需稍作调整，这也在预料之中。较大的干燥机，颗粒粒度分布范围较宽，且产率也较高。
表2所示为氮化硼固体负载量(wt.％)对喷雾干燥后粉体性质的影响。
表2氮化硼固体负载量(wt.％)对喷雾干燥后粉体性质的影响
    粉料     固含量，(wt.％)   轻相密度LPD(g/cc)     振实密度(g/cc)     流动性(秒)     颗粒大小(mm)
    A     25   0.462     0.55     55.7     -150/+75
    B     25   0.492     0.586     57.4     -75
    C     25   无     0.541     -45
    D     50   0.533     0.62     54     -75
    E     50   0.574     0.652     43.2     -150
    XP     无   0.44     0.562     75.3     -105/+74
粉料B和D经筛分后粒度大小相同，说明随着负载量提高，产生的喷雾干燥粉体密度增加了。
实施例4-氮化硼类粘土糊料的滑模法生产
将实施例1的浆料倒入灰浆滑模板内。施压并在模板内定型12小时。由于模具很快灌满，浇注停止，没有更多水分从滑行中脱除。形成的材料为粘稠的糊状材料，固含量为76％。
实施例5-氮化硼类粘土糊料的真空抽滤法生产
将实施例1的浆料倒入装有滤纸的布氏漏斗，漏斗下端接有真空抽吸机。体系中的水分流入量杯内。收集到要求的水量后，停止真空抽滤。收集固含量为74％的氮化硼糊料样品，并密封在密封袋内备用。
尽管这里描述了最佳实施方式，但对那些与此相关领域里的技术人员而言，显然在不偏离本发明精神的前提下，可做出各种修改、添加和替换等，这些均可认为包含在下述权利要求所确定的本发明范围之内。

Claims (48)

1.制备六方晶氮化硼浆料的方法，它包括：
0.5-5重量％的表面活性剂与30-50重量％的六方晶氮化硼粉体在有利于形成六方晶氮化硼浆料的条件下于介质内混合。
2.如权利要求1所述的方法，其特征在于：六方晶氮化硼浆料含有约40-50重量％的六方晶氮化硼粉体。
3.如权利要求1所述的方法，其特征在于：表面活性剂选自下列物质：聚羧酸，硅烷，以及有机金属化合物。
4.如权利要求1所述的方法，其特征在于：六方晶氮化硼粉体的表面积在5-30m2/g。
5.如权利要求1所述的方法，其中介质为水溶液介质。
6.如权利要求1所述的方法，其中介质选自下列非水介质：异丙醇，甲醇，以及乙醇。
7.六方晶氮化硼浆料，包含：
约0.5-5重量％的表面活性剂和
在介质中30-50重量％的六方晶氮化硼粉体。
8.如权利要求7所述的浆料，其特征在于：该浆料包含约40-50重量％的六方晶氮化硼粉体。
9.如权利要求7所述的浆料，其特征在于：表面活性剂选自下列物质：聚羧酸，硅烷，有机金属化合物。
10.如权利要求7所述的浆料，其特征在于：六方晶氮化硼粉体的表面积在5-30m2/g。
11.如权利要求7所述的浆料，其中介质为水性介质。
12.如权利要求7所述的浆料，其中介质选自下列非水性介质：异丙醇，甲醇，乙醇。
13.制备球形氮化硼粉体的方法，它包括：
提供六方晶氮化硼浆料；在有利于形成球形粒氮化硼粉体包括氮化硼片晶的球形团聚物条件下进行喷雾干燥，对球形氮化硼粉体进行烧结。
14.如权利要求13所述的方法，其特征在于：该六方晶氮化硼浆料包含30-50重量％的六方晶氮化硼粉体。
15.如权利要求13所述的方法，其特征在于：氮化硼片晶的球形团聚物的平均直径在约10-500μm之间。
16.如权利要求15所述的方法，其特征在于：大部分氮化硼团聚物的平均直径在约30-150μm之间。
17.如权利要求13所述的方法，其特征在于：球形氮化硼粉体的振实密度在约0.4-0.7g/cc之间。
18.如权利要求13所述的方法，其特征在于：烧结温度在约1800-2400℃之间。
19.如权利要求13所述方法，它还包括：在有利于获得要求的团聚物粒度分级条件下对球形氮化硼粉体进行分粒。
20.如权利要求19所述的方法，其特征在于：采用下列分粒方法：筛分法，空气分级法，以及淘析法。
21.球形氮化硼粉体，它包含氮化硼片晶的球形团聚物。
22.如权利要求21所述的球形氮化硼粉体，其特征在于：氮化硼片晶的球形团聚物的平均直径约为10-500μm。
23.如权利要求22所述的球形氮化硼粉体，其特征在于：大部分氮化硼团聚物的平均直径约为30-150μm之间。
24.如权利要求21所述的球形氮化硼粉体，其特征在于：球形氮化硼粉体的约为0.4-0.7g/cc之间。
25.制备六方晶氮化硼糊料的方法，包括：
提供六方晶氮化硼浆料，
在有利于形成高含60～80重量％固体六方晶氮化硼的六方晶氮化硼糊料条件下对浆料进行处理。
26.如权利要求25所述的方法，其特征在于：六方晶氮化硼浆料含有约30-50重量％的六方晶氮化硼固体负载量。
27.如权利要求25所述的方法，其特征在于：所述处理方法包括将浆料倒入灰浆模内。
28.如权利要求25所述的方法，其特征在于：所述处理方法包括真空抽滤。
29.六方晶氮化硼糊料，它包含分散在介质中的约60-80重量％的固体六方晶氮化硼。
30.如权利要求29所述的六方晶氮化硼糊料，其中介质为水性介质。
31.如权利要求29所述的六方晶氮化硼糊料，其中介质选自下列非水性介质：异丙醇，甲醇，乙醇。
32.聚合物混合物，它包括一种聚合物，以及
包含六方晶氮化硼片晶的球形团聚物粉体相，其中粉体相均匀分布于聚合物内。
33.如权利要求32所述的聚合物混合物，其中氮化硼片晶的球形团聚物的平均直径约为10-500μm之间。
34.如权利要求33所述的聚合物混合物，其中大部分球形团聚物的平均直径约为30-150μm之间。
35.如权利要求32所述的聚合物混合物，其特征在于：粉体相的振实密度约为0.4-0.7g/cc之间。
36.如权利要求32所述的聚合物混合物，其特征在于：聚合物选自下列一组物质：可熔融处理的聚合物，聚酯，酚醛树脂，有机硅聚合物如硅橡胶，丙烯酸类树脂，蜡类，热塑性聚合物，低分子量流体，以及环氧树脂模塑化合物。
37.如权利要求32所述的聚合物混合物，其特征在于：该聚合物混合物包含约30-80重量％球形氮化硼粉体。
38.如权利要求32所述的聚合物混合物，其特征在于：该聚合物混合物的热导率约为1-15W/mK。
39.一种体系，包括：
热源；
热阱；以及
使热源与阱热阱相连的热导材料，其中热导材料包括含有六方晶氮化硼片晶球形团聚物的粉体相。
40.如权利要求39所述的体系，其特征在于：其中六方晶氮化硼球形团聚物的平均直径在10-500μm之间。
41.如权利要求40所述的体系，其特征在于：其中大部分球形团聚物的平均直径在30-150μm之间。
42.如权利要求39所述的体系，其特征在于：粉体相的振实密度在0.4-0.7g/cc之间。
43.如权利要求39所述的体系，其中热源为集成电路片，功率模块，或变压器。
44.如权利要求39所述的体系，其中热阱为翅片铝、铜、铍或金刚石。
45.如权利要求39所述的体系，其中热导材料为聚合物。
46.如权利要求45所述的体系，其特征在于：聚合物选自下列物质：可熔融处理的聚合物、聚酯、酚醛树脂，有机硅聚合物如硅橡胶、丙烯酸类树脂，蜡类，热塑性聚合物、低分子量流体，以及环氧树脂模塑化合物。
47.如权利要求39所述的体系，其中热导材料包含约30-80重量％球形氮化硼粉体。
48.如权利要求39所述的体系，其中热导材料的热导率约为1-15W/mK。
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102976294A (zh) * 2012-12-20 2013-03-20 沈阳大学 表面活性剂方式制备高结晶度球状六方氮化硼粉体的方法
CN104284860A (zh) * 2012-05-09 2015-01-14 Esk陶瓷有限两合公司 氮化硼团聚体、其制备方法及其用途
TWI474991B (zh) * 2010-08-19 2015-03-01 Earthgen Corp 製備球型氮化硼聚集體之漿料及其應用
CN105617934A (zh) * 2015-12-24 2016-06-01 富耐克超硬材料股份有限公司 六方氮化硼分散剂及分散方法
CN105947997A (zh) * 2011-11-29 2016-09-21 三菱化学株式会社 氮化硼凝聚粒子、含有该粒子的组合物、及具有包含该组合物的层的三维集成电路
CN107109011A (zh) * 2014-11-20 2017-08-29 杜邦三井氟化物株式会社 具有优异导热性的可熔融加工的含氟聚合物组合物、由该组合物制造的模制品及其制造方法
CN108101546A (zh) * 2017-09-13 2018-06-01 上海百图高新材料科技有限公司 一种球形六方氮化硼团聚体的制备方法
CN110430972A (zh) * 2017-02-10 2019-11-08 圣戈本陶瓷及塑料股份有限公司 具有受控氧化硼水平的氮化硼
CN112566868A (zh) * 2018-08-07 2021-03-26 水岛合金铁株式会社 六方晶氮化硼粉末
CN115520841A (zh) * 2022-08-30 2022-12-27 山东工业陶瓷研究设计院有限公司 一种球形氮化硼粉体及其原位合成制备方法

Families Citing this family (66)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7976941B2 (en) * 1999-08-31 2011-07-12 Momentive Performance Materials Inc. Boron nitride particles of spherical geometry and process for making thereof
US20070241303A1 (en) * 1999-08-31 2007-10-18 General Electric Company Thermally conductive composition and method for preparing the same
US6713088B2 (en) * 1999-08-31 2004-03-30 General Electric Company Low viscosity filler composition of boron nitride particles of spherical geometry and process
US7445797B2 (en) * 2005-03-14 2008-11-04 Momentive Performance Materials Inc. Enhanced boron nitride composition and polymer-based compositions made therewith
US6764975B1 (en) * 2000-11-28 2004-07-20 Saint-Gobain Ceramics & Plastics, Inc. Method for making high thermal diffusivity boron nitride powders
CN100398589C (zh) * 2001-04-30 2008-07-02 圣戈本陶瓷及塑料股份有限公司 聚合物加工用助剂和加工方法
US6645612B2 (en) 2001-08-07 2003-11-11 Saint-Gobain Ceramics & Plastics, Inc. High solids hBN slurry, hBN paste, spherical hBN powder, and methods of making and using them
US7494635B2 (en) 2003-08-21 2009-02-24 Saint-Gobain Ceramics & Plastics, Inc. Boron nitride agglomerated powder
WO2006023860A2 (en) * 2004-08-23 2006-03-02 General Electric Company Thermally conductive composition and method for preparing the same
DE102005020940A1 (de) * 2005-05-04 2006-11-09 Esk Ceramics Gmbh & Co. Kg Leicht dispergierbares BN-Granulat, Verfahren zu dessen Herstellung und dessen Verwendung
US7524560B2 (en) * 2005-08-19 2009-04-28 Momentive Performance Materials Inc. Enhanced boron nitride composition and compositions made therewith
CA2620851A1 (en) * 2005-08-26 2007-03-01 Cool Options, Inc. Thermally conductive thermoplastics for die-level packaging of microelectronics
JP2007137720A (ja) * 2005-11-18 2007-06-07 Teijin Ltd 窒化ホウ素ナノチューブ含有ポリマー分散液
JP4670100B2 (ja) * 2006-03-01 2011-04-13 独立行政法人物質・材料研究機構 窒化ホウ素ナノチューブの精製方法
US8206729B2 (en) * 2006-03-02 2012-06-26 Momentive Performance Materials Inc. Compositions for topical applications comprising boron nitride
JP2007230994A (ja) * 2006-03-02 2007-09-13 General Electric Co <Ge> 窒化ホウ素を含む局所塗布組成物
US8663665B2 (en) * 2006-03-02 2014-03-04 Momentive Performance Materials Inc. Anti-chafing compositions comprising boron nitride
CN101535176A (zh) * 2006-10-07 2009-09-16 迈图高新材料公司 混合的氮化硼组合物及其制备方法
US7527859B2 (en) * 2006-10-08 2009-05-05 Momentive Performance Materials Inc. Enhanced boron nitride composition and compositions made therewith
US8404768B2 (en) * 2007-01-10 2013-03-26 Momentive Performance Materials Inc. Thermal interface materials and methods for making thereof
JP2008179724A (ja) * 2007-01-25 2008-08-07 Nitto Denko Corp 半導体封止用エポキシ樹脂組成物およびそれを用いて得られた半導体装置
KR100908455B1 (ko) * 2008-10-14 2009-07-20 김태웅 비점착성 도료의 조성물 및 그 제조방법
JP5105372B2 (ja) * 2009-02-03 2012-12-26 独立行政法人物質・材料研究機構 窒化ホウ素球状ナノ粒子とその製造方法
KR20110012780A (ko) * 2009-07-31 2011-02-09 엘지디스플레이 주식회사 액정표시장치
US20110129673A1 (en) * 2009-12-01 2011-06-02 Henkel Corporation Silver-coated boron nitride particulate materials and formulations containing same
JP5340202B2 (ja) * 2010-02-23 2013-11-13 三菱電機株式会社 熱硬化性樹脂組成物、ｂステージ熱伝導性シート及びパワーモジュール
DE102010050900A1 (de) 2010-11-10 2012-05-10 Esk Ceramics Gmbh & Co. Kg Bornitrid-Agglomerate, Verfahren zu deren Herstellung und deren Verwendung
KR101970771B1 (ko) * 2011-08-31 2019-04-22 히타치가세이가부시끼가이샤 수지 조성물, 수지 시트, 금속박 구비 수지 시트, 수지 경화물 시트, 구조체, 및 동력용 또는 광원용 반도체 디바이스
CN105646847B (zh) * 2011-08-31 2018-01-16 日立化成株式会社 树脂组合物
CN105754293A (zh) * 2011-08-31 2016-07-13 日立化成株式会社 树脂组合物、树脂片、带金属箔的树脂片、树脂固化物片、结构体、以及半导体装置
JP2013056789A (ja) * 2011-09-07 2013-03-28 Mitsubishi Chemicals Corp 粉末状窒化ホウ素組成物、およびそれを含有する複合材組成物
US20150232336A1 (en) * 2011-10-11 2015-08-20 Ph Matter, Llc Method for producing bn-based nanoparticles and products therefrom
JP5987322B2 (ja) * 2012-01-17 2016-09-07 国立大学法人 香川大学 金属酸化物含有窒化ホウ素の製造方法
JP5189222B1 (ja) * 2012-07-18 2013-04-24 サンアロイ工業株式会社 低摩擦化能が付与された超硬合金及びその製造方法、並びに超硬工具
FR2999172A1 (fr) 2012-12-07 2014-06-13 Saint Gobain Ct Recherches Suspension de particules de nitrure de bore.
JP6076459B2 (ja) * 2013-03-01 2017-02-08 国立大学法人京都大学 セラミックス微粒子分散液の製造方法
CN105026312B (zh) * 2013-03-07 2018-03-20 电化株式会社 氮化硼粉末及含有该氮化硼粉末的树脂组合物
US9745499B2 (en) * 2013-09-06 2017-08-29 Korea Advanced Institute Of Science And Technology Hexagonal boron nitride nanosheet/ceramic nanocomposite powder and producing method of the same, and hexagonal boron nitride nanosheet/ceramic nanocomposite materials and producing method of the same
EP2860008A1 (de) 2013-10-14 2015-04-15 Esk Ceramics GmbH&Co. Kg Durch thermoplastische Verarbeitung von Polymer-Bornitrid-Compounds hergestellte Bauteile, Polymer-Bornitrid-Compounds zur Herstellung solcher Bauteile, Verfahren zur Herstellung solcher Bauteile sowie deren Verwendung
KR20160106579A (ko) * 2014-01-08 2016-09-12 제이엔씨 주식회사 열전도성 시트용 수지 조성물, 열전도성 시트, 수지 피막 금속 및 전자 기기
WO2015105145A1 (ja) * 2014-01-08 2015-07-16 電気化学工業株式会社 六方晶窒化ホウ素の製造方法、及び放熱シート
TWI687393B (zh) 2014-02-05 2020-03-11 日商三菱化學股份有限公司 氮化硼凝集粒子、氮化硼凝集粒子之製造方法、含有該氮化硼凝集粒子之樹脂組成物、成形體及片材
JP2015193504A (ja) * 2014-03-31 2015-11-05 ナガセケムテックス株式会社 窒化ホウ素粒子、樹脂組成物および熱伝導性シート
JP2017107888A (ja) * 2014-04-14 2017-06-15 三菱電機株式会社 熱伝導性シート用コンパウンドの製造方法、熱伝導性シート用コンパウンド及びパワーモジュール
JP6394115B2 (ja) * 2014-06-27 2018-09-26 三菱ケミカル株式会社 樹脂組成物、樹脂組成物からなる放熱シート、及び放熱シートを含むパワーデバイス装置
DE102014013375A1 (de) 2014-09-09 2016-03-10 Häusermann GmbH Leiterplatte mit thermischen Kontaktierungselementen
WO2016049109A2 (en) 2014-09-25 2016-03-31 Drexel University Physical forms of mxene materials exhibiting novel electrical and optical characteristics
CN104479291A (zh) * 2014-12-04 2015-04-01 中国科学院过程工程研究所 一种导热绝缘环氧树脂组合物、制备方法及其用途
FR3037579B1 (fr) * 2015-06-17 2017-06-16 Saint-Gobain Centre De Rech Et D'Etudes Europeen Poudre d'agregats a base de nitrure de bore
MX2017007385A (es) * 2015-12-14 2019-08-08 Arteco Nv Estabilizacion de nanoparticulas hexagonales de nitruro de boro.
EP3181627A1 (en) 2015-12-15 2017-06-21 3M Innovative Properties Company Thermally conductive pressure sensitive adhesive comprising anisotropic boron nitride agglomerates
DE102016005291B4 (de) 2016-04-29 2024-01-11 Ksg Austria Gmbh Verfahren zur Herstellung eines elektronischen Gerätes in der Form eines Spritzgußteils mit eingelegter Leiterplatte
WO2017205873A1 (en) 2016-05-27 2017-11-30 Saint-Gobain Ceramics & Plastics, Inc. Process for manufacturing boron nitride agglomerates
JP2019131410A (ja) * 2016-05-31 2019-08-08 デンカ株式会社 耐食性に優れたｂｎ焼結体
SG10201607550RA (en) * 2016-09-09 2018-04-27 3M Innovative Properties Co Thermal Interface Material
US11268004B2 (en) 2016-10-07 2022-03-08 Denka Company Limited Boron nitride aggregated grain
EP3661641A4 (en) 2017-08-01 2021-04-21 Drexel University MXEN SORPTION AGENT FOR THE REMOVAL OF SMALL MOLECULES FROM A DIALYSATE
CN110041080A (zh) * 2019-05-24 2019-07-23 丹东市化工研究所有限责任公司 一种制备类球状六方氮化硼团聚颗粒的方法
CN112029151B (zh) * 2020-09-09 2022-04-15 苏州巨峰电气绝缘系统股份有限公司 高导热微纳氮化硼粒子及其制备方法与应用
CN112225186B (zh) * 2020-10-21 2023-07-21 江西联锴科技有限公司 一种球形氮化硼的制备方法
CN113150476A (zh) * 2021-05-06 2021-07-23 浙江亿隆新材料有限公司 一种用于电子设备导热材料的制备方法
WO2023089452A1 (en) 2021-11-22 2023-05-25 3M Innovative Properties Company Spherical boron nitride particles having low surface roughness
CN114835092B (zh) * 2022-05-26 2023-05-16 南京工业大学 一种球形氮化硼导热材料及其制备方法
CN115232444A (zh) * 2022-09-02 2022-10-25 重庆大学 一种高导热球形氮化硼复合环氧树脂及其制备方法
CN115368758A (zh) * 2022-09-13 2022-11-22 安徽大学 一种非离子表面活性剂非共价改性氮化硼导热填料及基于其的导热复合材料
WO2024106404A1 (ja) * 2022-11-14 2024-05-23 デンカ株式会社 球状窒化ホウ素粉末、樹脂用充填剤、樹脂組成物及び球状窒化ホウ素粉末の製造方法

Family Cites Families (211)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB870084A (en) 1958-03-24 1961-06-14 United States Borax Chem Method of manufacturing boron nitride
US2991508A (en) 1959-09-23 1961-07-11 Du Pont Fabrication of thermoplastic resins
US3125547A (en) 1961-02-09 1964-03-17 Extrudable composition consisting of
US3351690A (en) 1962-04-18 1967-11-07 Gen Electric Heat treating pyrolytic graphite and boron nitride bodies with simultaneous application of multiaxial tension
CH494187A (de) 1966-03-09 1970-07-31 Lonza Werke Gmbh Verfahren zur Herstellung von Bornitrid
US3469941A (en) * 1967-09-05 1969-09-30 Green Refractories Ultrafine boron nitride and process of making same
US3617358A (en) * 1967-09-29 1971-11-02 Metco Inc Flame spray powder and process
US4097293A (en) 1969-04-30 1978-06-27 Tokyo Shibaura Electric Co., Ltd. Method for manufacturing heat-resistant reinforced composite materials
US3720740A (en) 1970-06-24 1973-03-13 Hitachi Ltd Low pressure sintering of boron nitride using low thermal expansion static sintering molds
CA1004073A (en) 1972-11-13 1977-01-25 Leroy A. Bartolomei Striped dichroic filter with butted stripes and dual lift-off method for making the same
JPS50854A (zh) 1973-05-01 1975-01-07
JPS521561B2 (zh) 1973-11-09 1977-01-17
US3954483A (en) 1974-01-08 1976-05-04 General Electric Company Dense polycrystalline silicon carbide
SU514796A1 (ru) 1974-07-05 1976-05-25 Ордена Трудового Красного Знамени Институт Проблем Материаловедения Ан Укр. Сср Спеченный материал на основе нитрида бора
US3981648A (en) 1974-10-23 1976-09-21 Sperry Rand Corporation Power transmission
US4107276A (en) 1974-12-30 1978-08-15 Elektroschmelzwerk Kempten Gmbh Manufacture of hexagonal boron nitride
DE2629960C3 (de) 1976-07-02 1981-08-06 Moskovskij chimiko-technologičeskij institut imeni D.I. Mendeleeva, Moskva Verfahren zur Herstellung von Erzeugnissen auf der Basis von hexagonalem Bornitrid
US4188194A (en) 1976-10-29 1980-02-12 General Electric Company Direct conversion process for making cubic boron nitride from pyrolytic boron nitride
US4195002A (en) * 1978-07-27 1980-03-25 International Lead Zinc Research Organization, Inc. Water-dispersible coatings containing boron nitride for steel casting dies
JPS5856018B2 (ja) 1979-11-30 1983-12-13 日本油脂株式会社 切削工具用高密度相窒化硼素複合焼結体およびその製造方法
JPS6022676B2 (ja) 1980-02-23 1985-06-03 日本鋼管株式会社 窒化硅素・窒化硼素複合焼結体及びその製造方法
JPS5860679A (ja) 1981-10-02 1983-04-11 三菱マテリアル株式会社 切削および耐摩耗工具用高靭性窒化硼素基超高圧焼結材料
JPS5860680A (ja) 1981-10-07 1983-04-11 三菱マテリアル株式会社 切削および耐摩耗工具用高靭性窒化硼素基超高圧焼結材料
JPS5860680U (ja) 1981-10-16 1983-04-23 住友金属工業株式会社 クレ−ンにおける緩衝装置
JPS5860679U (ja) 1981-10-19 1983-04-23 株式会社佐々木商事 スライドビ−ム型天井走行クレ−ン
JPS5891005A (ja) 1981-11-25 1983-05-30 Toshiba Corp 窒化ケイ素粉末の製造方法
DE3201563A1 (de) 1982-01-20 1983-07-28 Elektroschmelzwerk Kempten GmbH, 8000 München Dichte formkoerper aus polykristallinem, hexagonalem bornitrid und verfahren zu ihrer herstellung durch isostatisches heisspressen
JPS5933388U (ja) 1982-08-27 1984-03-01 吉井　健 直接ピツクアツプ型骨導マイクロホン
JPS60110310U (ja) 1983-12-27 1985-07-26 マツダ株式会社 搬送高さ調整機能を有する搬送装置
JPS60195059A (ja) 1984-03-15 1985-10-03 株式会社トクヤマ 複合焼結体
CA1260671A (en) * 1984-06-07 1989-09-26 Takahisa Koshida High-purity powder of hexagonal boron nitride and a method for the preparation thereof
JPS61268763A (ja) 1984-11-26 1986-11-28 Shiseido Co Ltd 処理粉体の製造方法
JPS61132564A (ja) 1984-11-28 1986-06-20 川崎製鉄株式会社 窒化硼素常圧焼結体
US5332629A (en) 1985-01-11 1994-07-26 Sumitomo Electric Industries, Ltd. Boron nitride system including an hBN starting material with a catalyst and a sintered cNB body having a high heat conductivity based on the catalyst
JPH0337180Y2 (zh) 1985-02-08 1991-08-06
EP0212870B1 (en) 1985-07-29 1992-04-15 Shiseido Company Limited Silicone polymer-coated powder or particulate material
US4801445A (en) 1985-07-29 1989-01-31 Shiseido Company Ltd. Cosmetic compositions containing modified powder or particulate material
CA1306904C (en) 1985-10-09 1992-09-01 Tetsumi Suzuki Electrically conductive material and secondary battery using the electrically conductive material
JPS62123070A (ja) 1985-11-21 1987-06-04 株式会社香蘭社 窒化ボロン系焼結体の製造方法
JPH049745Y2 (zh) 1986-01-28 1992-03-11
US4997633A (en) * 1986-01-30 1991-03-05 Kawasaki Steel Corporation Water-soluble boron containing impurity reduced hexagonally crystalline boron nitride
JPS6340769Y2 (zh) 1986-04-03 1988-10-25
JPS636093A (ja) * 1986-06-27 1988-01-12 Shin Etsu Chem Co Ltd 窒化ほう素含有離型用または潤滑用組成物
JPS6340769A (ja) 1986-08-07 1988-02-22 昭和電工株式会社 高密度窒化硼素常圧焼結体の製造方法
JPS6345178A (ja) 1986-08-07 1988-02-26 株式会社　香蘭社 窒化ボロン焼結原料粉末
JPS6345104A (ja) * 1986-08-11 1988-02-26 Kawasaki Steel Corp スリツプキヤステイング用窒化硼素粉末及びその製造方法
JPH0753610B2 (ja) 1986-11-01 1995-06-07 株式会社香蘭社 窒化ボロン系焼結体の製造方法
US4849284A (en) 1987-02-17 1989-07-18 Rogers Corporation Electrical substrate material
JPH0617270B2 (ja) 1987-04-01 1994-03-09 工業技術院長 窒化硼素常圧焼結体
US5308044A (en) 1987-05-12 1994-05-03 Kabushiki Kaisha Kouransha Boron nitride ceramics and molten metal container provided with members made of the same ceramics
JP2590908B2 (ja) 1987-08-03 1997-03-19 松下電工株式会社 エポキシ樹脂成形材料
US4869954A (en) 1987-09-10 1989-09-26 Chomerics, Inc. Thermally conductive materials
US5001091A (en) 1987-11-02 1991-03-19 Norton Company Readily moldable or castable ceramic powders
JP2590964B2 (ja) 1987-11-11 1997-03-19 ミノルタ株式会社 画像形成方法
JPH01221454A (ja) 1988-02-29 1989-09-04 Shin Etsu Chem Co Ltd 押出成形用シリコーンゴム組成物
JP2821748B2 (ja) 1988-08-04 1998-11-05 株式会社香蘭社 耐溶損性に優れたｂｎ系常圧焼結セラミック
JPH0819328B2 (ja) 1988-08-22 1996-02-28 電気化学工業株式会社 シリコーンゴム成形品の製造方法
US4863881A (en) 1988-09-15 1989-09-05 California Institute Of Technology Shock consolidation of cubic boron nitride with whiskers of silicon compounds
JP2546709B2 (ja) 1988-09-29 1996-10-23 東芝タンガロイ株式会社 高強度立方晶窒化ホウ素含有焼結体
JPH02164433A (ja) 1988-12-19 1990-06-25 Denki Kagaku Kogyo Kk 多結晶型立方晶窒化ほう素粒子の製造方法
JPH069730B2 (ja) 1989-01-13 1994-02-09 花野商事株式会社 ダイカスト用粉末離型剤
US5011870A (en) 1989-02-08 1991-04-30 Dow Corning Corporation Thermally conductive organosiloxane compositions
US4971779A (en) 1989-02-17 1990-11-20 University Of New Mexico Process for the pyrolytic conversion of a polymeric precursor composition to boron nitride
CH677923A5 (zh) 1989-04-28 1991-07-15 Htm Ag
FR2646663B1 (fr) 1989-05-02 1991-12-27 Rhone Poulenc Chimie Nitrure de bore amorphe ou turbostratique a morphologie spherique et son procede de preparation
US5098609A (en) * 1989-11-03 1992-03-24 The Research Foundation Of State Univ. Of N.Y. Stable high solids, high thermal conductivity pastes
FR2655638A1 (fr) 1989-12-08 1991-06-14 Rhone Poulenc Chimie Nitrure de bore hexagonal monodisperse de haute purete vis-a-vis des metaux et de l'oxygene et son procede de preparation.
US5064589A (en) * 1989-12-29 1991-11-12 Showa Denko K.K. Method for producing high density hexagonal boron nitride sintered article
US5120688A (en) 1990-05-29 1992-06-09 The Morgan Crucible Company Plc Pressureless sintered silicon nitride-boron nitride composite
US5116589A (en) 1990-06-18 1992-05-26 The United States Of America As Represented By The United States Department Of Energy High density hexagonal boron nitride prepared by hot isostatic pressing in refractory metal containers
US5118496A (en) 1990-10-02 1992-06-02 Morris Herstein Coated cosmetic materials and method of coating cosmetic materials
JPH04164805A (ja) * 1990-10-30 1992-06-10 Kawasaki Steel Corp 高純度六方晶窒化硼素粉末の製造方法
JP3012316B2 (ja) 1990-11-29 2000-02-21 タスコジャパン株式会社 放射温度計
JP2981002B2 (ja) 1991-04-23 1999-11-22 松下電工株式会社 窒化アルミニウム粉末
US5194480A (en) * 1991-05-24 1993-03-16 W. R. Grace & Co.-Conn. Thermally conductive elastomer
EP0519644B1 (en) 1991-06-17 1996-12-11 General Electric Company Silicon carbide composite with metal nitride coated fiber reinforcement
US5285108A (en) 1991-06-21 1994-02-08 Compaq Computer Corporation Cooling system for integrated circuits
US5194071A (en) 1991-07-25 1993-03-16 General Electric Company Inc. Cubic boron nitride abrasive and process for preparing same
US5273558A (en) 1991-08-30 1993-12-28 Minnesota Mining And Manufacturing Company Abrasive composition and articles incorporating same
US5213868A (en) 1991-08-13 1993-05-25 Chomerics, Inc. Thermally conductive interface materials and methods of using the same
JP2925402B2 (ja) 1991-09-11 1999-07-28 三菱電機株式会社 高熱伝導性低収縮湿式不飽和ポリエステル系樹脂組成物を成形してなる筐体を有する回路遮断器
US5229339A (en) 1991-11-12 1993-07-20 Norton Company Pressure casting ceramic slurries
US5234712A (en) 1992-06-08 1993-08-10 The Dow Chemical Company Method of making moisture resistant aluminum nitride powder and powder produced thereby
ATE146509T1 (de) 1992-07-23 1997-01-15 Silberline Ltd Metallpulverpigment
GB9222548D0 (en) 1992-10-27 1992-12-09 Foseco Int Metallurgical pouring vessels
US5320989A (en) * 1992-12-07 1994-06-14 Orpac, Inc. Boron nitride-containing bodies and method of making the same
US5985228A (en) 1992-12-22 1999-11-16 General Electric Company Method for controlling the particle size distribution in the production of multicrystalline cubic boron nitride
US5312571A (en) 1993-01-07 1994-05-17 Norton Company Shaped bodies and the production thereof
JPH06219714A (ja) * 1993-01-29 1994-08-09 Shin Etsu Chem Co Ltd 窒化ホウ素の水系スラリー
JPH06321638A (ja) * 1993-05-11 1994-11-22 Nippon Cement Co Ltd 窒化ホウ素系複合セラミックスの鋳込み成形用泥漿の調製方法
US5457075A (en) 1993-05-11 1995-10-10 Hitachi Metals, Ltd. Sintered ceramic composite and molten metal contact member produced therefrom
DE69328687D1 (de) 1993-07-06 2000-06-21 Toshiba Kawasaki Kk Wärmeleitende platte
US5510174A (en) 1993-07-14 1996-04-23 Chomerics, Inc. Thermally conductive materials containing titanium diboride filler
JP2922096B2 (ja) * 1993-07-30 1999-07-19 川崎製鉄株式会社 六方晶窒化硼素粉末の製造方法
US5536485A (en) 1993-08-12 1996-07-16 Agency Of Industrial Science & Technology Diamond sinter, high-pressure phase boron nitride sinter, and processes for producing those sinters
US5571760A (en) 1993-08-27 1996-11-05 Saint-Gobain/Norton Industrial Ceramics Corporation Silicon nitride having a high tensile strength
JP3177361B2 (ja) 1993-11-17 2001-06-18 松下電器産業株式会社 光送信装置
JPH07157369A (ja) * 1993-12-10 1995-06-20 Hitachi Ltd セラミックス造粒粉
US5409868A (en) 1993-12-23 1995-04-25 Electrofuel Manufacturing Co. Ceramic articles made of compositions containing borides and nitrides
JPH07204492A (ja) * 1994-01-18 1995-08-08 Shin Etsu Chem Co Ltd 窒化ホウ素含有水系分散体
US5545473A (en) 1994-02-14 1996-08-13 W. L. Gore & Associates, Inc. Thermally conductive interface
US5591034A (en) 1994-02-14 1997-01-07 W. L. Gore & Associates, Inc. Thermally conductive adhesive interface
IT1269816B (it) 1994-05-23 1997-04-15 Ausimont Spa Composizioni solide espandibili a base di perfluoropolimeri e processoper la loro preparazione
US5528462A (en) 1994-06-29 1996-06-18 Pendse; Rajendra D. Direct chip connection using demountable flip chip package
US6249703B1 (en) 1994-07-08 2001-06-19 Medtronic, Inc. Handheld patient programmer for implantable human tissue stimulator
JP3460099B2 (ja) 1994-08-19 2003-10-27 株式会社三谷バルブ エアゾ−ル容器用バルブ
FR2725129B1 (fr) 1994-09-30 1997-06-13 Oreal Composition cosmetique anhydre resistante a l'eau
US5759481A (en) 1994-10-18 1998-06-02 Saint-Gobain/Norton Industrial Ceramics Corp. Silicon nitride having a high tensile strength
JPH08127793A (ja) * 1994-10-31 1996-05-21 Mitsui Toatsu Chem Inc 潤滑剤用窒化ホウ素スラリー
US5601874A (en) 1994-12-08 1997-02-11 The Dow Chemical Company Method of making moisture resistant aluminum nitride powder and powder produced thereby
SE514574C2 (sv) * 1994-12-12 2001-03-12 Sandvik Ab Bindefasfria korrosionsbeständiga hårdmetaller för tribologiska tillämpningar
JPH08183906A (ja) * 1994-12-28 1996-07-16 Shin Etsu Chem Co Ltd 窒化ほう素懸濁液
US5770819A (en) 1995-02-13 1998-06-23 Raychem Corporation Insulated wire or cable having foamed fluoropolymer insulation
US5567353A (en) * 1995-04-13 1996-10-22 Rohm And Haas Company Method for dispersing ceramic material in an aqueous medium
US5614319A (en) 1995-05-04 1997-03-25 Commscope, Inc. Insulating composition, insulated plenum cable and methods for making same
WO1996035651A1 (en) 1995-05-10 1996-11-14 Saint-Gobain Industrial Ceramics, Inc. High solids silicon nitride slurries
DE19620942A1 (de) 1995-06-05 1996-12-12 Gen Electric Effizientes Verfahren zum Hydrophobieren von anorganischem Pulver
US5688449A (en) 1995-10-02 1997-11-18 Nitech Corporation Method of forming and extruding an additive-coated resin composition
US5962122A (en) 1995-11-28 1999-10-05 Hoechst Celanese Corporation Liquid crystalline polymer composites having high dielectric constant
JPH09151324A (ja) 1995-11-30 1997-06-10 Fuji Kobunshi Kogyo Kk 難燃性・高熱伝導性シリコーンゴム組成物
JP3461651B2 (ja) 1996-01-24 2003-10-27 電気化学工業株式会社 六方晶窒化ほう素粉末及びその用途
US5681883A (en) * 1996-03-05 1997-10-28 Advanced Ceramics Corporation Enhanced boron nitride composition and polymer based high thermal conductivity molding compound
US5898009A (en) 1996-03-19 1999-04-27 Advanced Ceramics Corporation High density agglomerated boron nitride particles
US5688457A (en) 1996-04-10 1997-11-18 E. I. Du Pont De Nemours And Company High speed extrusion
US5610203A (en) 1996-04-10 1997-03-11 E. I. Du Pont De Nemours And Company Foamable fluoropolymer composition
US5726502A (en) 1996-04-26 1998-03-10 Motorola, Inc. Bumped semiconductor device with alignment features and method for making the same
US5950066A (en) 1996-06-14 1999-09-07 The Bergquist Company Semisolid thermal interface with low flow resistance
US5738936A (en) 1996-06-27 1998-04-14 W. L. Gore & Associates, Inc. Thermally conductive polytetrafluoroethylene article
JPH1015937A (ja) 1996-07-08 1998-01-20 Matsuno Kikai Seisakusho:Kk 穿孔装置
KR100323941B1 (ko) * 1996-08-06 2002-02-16 오츠카 유지로 질화붕소 및 그의 제조방법
JP3142800B2 (ja) 1996-08-09 2001-03-07 信越化学工業株式会社 熱伝導性シリコーン組成物、熱伝導性材料及び熱伝導性シリコーングリース
JP3611930B2 (ja) 1996-08-15 2005-01-19 蛇の目ミシン工業株式会社 ヒートシンク製造装置及びその製造法
TW398163B (en) * 1996-10-09 2000-07-11 Matsushita Electric Ind Co Ltd The plate for heat transfer substrate and manufacturing method thereof, the heat-transfer substrate using such plate and manufacturing method thereof
US5783308A (en) 1996-10-25 1998-07-21 Quaker State Corporation Ceramic reinforced fluoropolymer
JP3215364B2 (ja) 1996-11-18 2001-10-02 松下電器産業株式会社 半導体装置
US5781412A (en) * 1996-11-22 1998-07-14 Parker-Hannifin Corporation Conductive cooling of a heat-generating electronic component using a cured-in-place, thermally-conductive interlayer having a filler of controlled particle size
JPH10194711A (ja) 1997-01-13 1998-07-28 Shin Etsu Chem Co Ltd 高充填性窒化ホウ素粉末及びその製造方法
JP3714502B2 (ja) 1997-01-24 2005-11-09 三井化学株式会社 高熱伝導性樹脂組成物
JP2001503471A (ja) 1997-02-07 2001-03-13 ロックタイト コーポレーション 伝導性樹脂組成物
US5926371A (en) 1997-04-25 1999-07-20 Advanced Micro Devices, Inc. Heat transfer apparatus which accommodates elevational disparity across an upper surface of a surface-mounted semiconductor device
US5907474A (en) 1997-04-25 1999-05-25 Advanced Micro Devices, Inc. Low-profile heat transfer apparatus for a surface-mounted semiconductor device employing a ball grid array (BGA) device package
JP3714506B2 (ja) 1997-06-17 2005-11-09 三井化学株式会社 優れた耐水性を有する高熱伝導性樹脂組成物
JP3654743B2 (ja) 1997-07-01 2005-06-02 電気化学工業株式会社 放熱スペーサー
JPH1122971A (ja) 1997-07-04 1999-01-26 Maruichi:Kk 火口兼注入口を有するガスライター
JPH1119564A (ja) 1997-07-07 1999-01-26 Hirano Tecseed Co Ltd 塗工装置
JPH1131066A (ja) 1997-07-10 1999-02-02 Nec Eng Ltd バッファ制御システム
JPH1131065A (ja) 1997-07-11 1999-02-02 Ricoh Co Ltd 画像表示装置
JPH1131062A (ja) 1997-07-14 1999-02-02 Mitsubishi Electric Corp 文書情報処理システム、アイコン作成方法及びアイコン作成用ツールを記録した媒体
JPH1133982A (ja) 1997-07-18 1999-02-09 Yokohama Rubber Co Ltd:The 軟質材料切削装置
BR9815894A (pt) 1997-07-28 2001-01-16 Green Clouds Ltd Dispositivo ultrasÈnico de atomização com circuito de circulação lìquida
JPH1145965A (ja) * 1997-07-28 1999-02-16 Kyocera Corp 伝熱性化合物およびこれを用いた半導体装置
JPH1160215A (ja) * 1997-08-04 1999-03-02 Shin Etsu Chem Co Ltd 高充填性窒化ホウ素粉末造粒物及びその製造方法並びに等方性窒化ホウ素成形体の製造方法
JPH1160216A (ja) * 1997-08-04 1999-03-02 Shin Etsu Chem Co Ltd 熱伝導性窒化ホウ素フィラー及び絶縁放熱シート
JP3195277B2 (ja) 1997-08-06 2001-08-06 信越化学工業株式会社 熱伝導性シリコーン組成物
US6124579A (en) 1997-10-06 2000-09-26 Watlow Electric Manufacturing Molded polymer composite heater
US5945217A (en) 1997-10-14 1999-08-31 Gore Enterprise Holdings, Inc. Thermally conductive polytrafluoroethylene article
JPH11116213A (ja) 1997-10-15 1999-04-27 Toshiba Ceramics Co Ltd シラノール基含有ポリオルガノシロキサン被膜でコーティングされた窒化アルミニウム粉末およびその製造方法
JPH11134944A (ja) 1997-10-28 1999-05-21 Fujikura Ltd 高熱伝導性絶縁材料及び超電導ケーブル
US6251513B1 (en) 1997-11-08 2001-06-26 Littlefuse, Inc. Polymer composites for overvoltage protection
US5984055A (en) 1997-11-21 1999-11-16 Northrop Grumman Corporation Integrated fiber reinforced ceramic matrix composite brake pad and back plate
US5898217A (en) 1998-01-05 1999-04-27 Motorola, Inc. Semiconductor device including a substrate having clustered interconnects
JP3290127B2 (ja) 1998-01-27 2002-06-10 松下電工株式会社 熱伝導性シリコーンゴム組成物及びこの熱伝導性シリコーンゴム組成物によりなる放熱シート
US6168859B1 (en) 1998-01-29 2001-01-02 The Dow Chemical Company Filler powder comprising a partially coated alumina powder and process to make the filler powder
EP0939066B1 (en) 1998-02-16 2002-08-07 Advanced Ceramics Corporation Method for forming high density boron nitride and high density agglomerated boron nitride particles
JP4155473B2 (ja) 1998-02-27 2008-09-24 モーメンティブ・パフォーマンス・マテリアルズ・インク 高密度窒化ホウ素および高密度凝集窒化ホウ素粒子の製造法
JPH11269302A (ja) * 1998-03-23 1999-10-05 Nishimura Togyo Kk 樹脂製品の熱伝導性向上用充填剤及びその製造方法
US5908796A (en) 1998-05-01 1999-06-01 Saint-Gobain Industrial Ceramics, Inc. Dense silicon nitride ceramic having fine grained titanium carbide
US6512023B1 (en) 1998-06-18 2003-01-28 Closure Medical Corporation Stabilized monomer adhesive compositions
JP3948834B2 (ja) 1998-07-16 2007-07-25 電気化学工業株式会社 樹脂添加用窒化硼素とそれを用いた樹脂組成物、放熱部品
JP3942280B2 (ja) * 1998-08-17 2007-07-11 電気化学工業株式会社 六方晶窒化ほう素焼結体の製造方法
US6136758A (en) 1998-08-17 2000-10-24 Shin-Etsu Chemical Co., Ltd. Aluminum nitride powder and thermally conductive grease composition using the same
US6162849A (en) * 1999-01-11 2000-12-19 Ferro Corporation Thermally conductive thermoplastic
JP3525792B2 (ja) * 1999-03-31 2004-05-10 日本碍子株式会社 液滴吐出装置
SE519860C2 (sv) * 1999-04-07 2003-04-15 Sandvik Ab Sätt att tillverka ett skär bestående av en PcBN-kropp och en hårdmetall- eller cermet-substrat
SE519862C2 (sv) * 1999-04-07 2003-04-15 Sandvik Ab Sätt att tillverka ett skär bestående av en PcBN-kropp och en hårdmetall- eller cermet-kropp
US6348179B1 (en) * 1999-05-19 2002-02-19 University Of New Mexico Spherical boron nitride process, system and product of manufacture
JP2001010867A (ja) * 1999-06-21 2001-01-16 Murata Mfg Co Ltd セラミック原料造粒粉末の製造方法
US6158894A (en) 1999-07-28 2000-12-12 Saint-Gobain Ceramics & Plastics, Inc. All ceramic bearing
US6713088B2 (en) * 1999-08-31 2004-03-30 General Electric Company Low viscosity filler composition of boron nitride particles of spherical geometry and process
US7976941B2 (en) 1999-08-31 2011-07-12 Momentive Performance Materials Inc. Boron nitride particles of spherical geometry and process for making thereof
US7445797B2 (en) 2005-03-14 2008-11-04 Momentive Performance Materials Inc. Enhanced boron nitride composition and polymer-based compositions made therewith
US20060121068A1 (en) 1999-08-31 2006-06-08 General Electric Company Boron nitride particles of spherical geometry and process for making thereof
JP4528397B2 (ja) 1999-12-17 2010-08-18 ポリマテック株式会社 接着方法および電子部品
CA2311178A1 (en) 1999-12-22 2001-06-22 Evgueni E. Rozenbaoum Extrusion aid combination
US6585039B2 (en) 2000-02-01 2003-07-01 Cool Options, Inc. Composite overmolded heat pipe construction
US6660241B2 (en) 2000-05-01 2003-12-09 Saint-Gobain Ceramics & Plastics, Inc. Highly delaminated hexagonal boron nitride powders, process for making, and uses thereof
US6794435B2 (en) 2000-05-18 2004-09-21 Saint Gobain Ceramics & Plastics, Inc. Agglomerated hexagonal boron nitride powders, method of making, and uses thereof
EP1160212A1 (en) 2000-05-31 2001-12-05 Asahi Glass Co., Ltd. Hollow glass microspheres and method for producing the same
JP2002080617A (ja) 2000-09-06 2002-03-19 Polymatech Co Ltd 熱伝導性シート
JP2002097372A (ja) 2000-09-20 2002-04-02 Polymatech Co Ltd 熱伝導性高分子組成物及び熱伝導性成形体
US6764975B1 (en) 2000-11-28 2004-07-20 Saint-Gobain Ceramics & Plastics, Inc. Method for making high thermal diffusivity boron nitride powders
JP2002198619A (ja) 2000-12-25 2002-07-12 Matsushita Electric Ind Co Ltd 回路基板
US6824753B2 (en) 2001-04-24 2004-11-30 Science & Technology Corporation @Unm Organoboron route and process for preparation of boron nitride
CN100398589C (zh) 2001-04-30 2008-07-02 圣戈本陶瓷及塑料股份有限公司 聚合物加工用助剂和加工方法
US6652822B2 (en) 2001-05-17 2003-11-25 The Regents Of The University Of California Spherical boron nitride particles and method for preparing them
US6645612B2 (en) 2001-08-07 2003-11-11 Saint-Gobain Ceramics & Plastics, Inc. High solids hBN slurry, hBN paste, spherical hBN powder, and methods of making and using them
JP2003060134A (ja) 2001-08-17 2003-02-28 Polymatech Co Ltd 熱伝導性シート
KR100493021B1 (ko) 2002-07-10 2005-06-07 삼성전자주식회사 반도체 메모리 장치 및 그의 제조방법
JP2005036016A (ja) 2002-10-18 2005-02-10 Advanced Ceramics Corp 球形形態の窒化ホウ素粒子の低粘性充填剤組成物及びその製造方法
JP4164805B2 (ja) 2003-06-17 2008-10-15 マツダ株式会社 走行支援システム及び車載端末器
US7494635B2 (en) 2003-08-21 2009-02-24 Saint-Gobain Ceramics & Plastics, Inc. Boron nitride agglomerated powder
DE102004017436A1 (de) 2004-04-08 2005-10-27 Bayer Materialscience Ag Verfahren zur kontinuierlichen Herstellung einer wässrigen Polyurethandispersion
WO2006023860A2 (en) 2004-08-23 2006-03-02 General Electric Company Thermally conductive composition and method for preparing the same
JP5000853B2 (ja) 2005-03-24 2012-08-15 パナソニック株式会社 燃料電池用セパレータ材料の製造方法と燃料電池用セパレータ並びに燃料電池
US20060228542A1 (en) 2005-04-08 2006-10-12 Saint-Gobain Performance Plastics Corporation Thermal interface material having spheroidal particulate filler
DE102005020940A1 (de) 2005-05-04 2006-11-09 Esk Ceramics Gmbh & Co. Kg Leicht dispergierbares BN-Granulat, Verfahren zu dessen Herstellung und dessen Verwendung
JP4321506B2 (ja) 2005-09-08 2009-08-26 オムロン株式会社 光電センサの製造方法
US7557054B2 (en) 2006-02-27 2009-07-07 Kyocera Corporation Boron carbide sintered body and protective member
US20070205706A1 (en) 2006-03-01 2007-09-06 General Electric Company Optical Substrate Comprising Boron Nitride Particles
US7527859B2 (en) 2006-10-08 2009-05-05 Momentive Performance Materials Inc. Enhanced boron nitride composition and compositions made therewith
JP3177361U (ja) 2012-04-26 2012-08-02 株式会社ブロッコリー カードゲーム具

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