CN103086719A - 聚集的氮化硼粉末 - Google Patents

聚集的氮化硼粉末 Download PDF

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CN103086719A
CN103086719A CN2013100256314A CN201310025631A CN103086719A CN 103086719 A CN103086719 A CN 103086719A CN 2013100256314 A CN2013100256314 A CN 2013100256314A CN 201310025631 A CN201310025631 A CN 201310025631A CN 103086719 A CN103086719 A CN 103086719A
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powder
boron nitride
aggregate
less
microns
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E·A·普鲁斯
T·M·克丽尔
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Saint Gobain Ceramics and Plastics Inc
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Saint Gobain Industrial Ceramics Inc
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Abstract

提供具有受控密度和断裂强度特征的新颖聚集氮化硼粉末。此外还提供该粉末的制备方法。一种方法要求提供包含氮化硼聚集体的原料粉末，并热处理该原料粉末形成热处理的聚集的氮化硼粉末。在一个实施方式中，原料粉末具有受控的晶体大小。在另一个实施方式中，原料粉末来自松散粉末源。

Description

聚集的氮化硼粉末
本发明是申请日为2004年8月19日，申请号为200480023782.5，发明名称为“聚集的氮化硼粉末”的专利申请的分案申请。
技术领域
本发明一般涉及制备聚集的氮化硼粉末的方法，该方法形成的粉末，含有这种粉末的部件。
背景技术
微电子器件如集成电路芯片变得越来越小且越来越高效。目前的趋势是在给定时间内制造在密度和功能方面比现有芯片不断增加的集成芯片。这导致功率消耗增加并产生更多热量，因此对热量的控制已经成为开发电子器件主要关注的问题。
通常，产热源或器件如集成电路芯片上配有散热器，除去操作期间产生的热量。然而，在热源或器件与散热器之间的接触热阻限制了散热器的有效除热能力。组装期间，一般施涂一层导热油脂，一般为硅脂或一层导热有机蜡，有助于在热源和散热器的相对接触面之间形成低热阻的路径。其它导热材料基于使用粘结剂，较好是树脂粘结剂，如有机硅、热塑性橡胶、氨基甲酸酯、丙烯酸类或环氧化物，导热材料中分散有一种或多种导热填料。
通常，这些填料为两大类中的一类：导热和电绝缘的填料，或导热和导电的填料。氧化铝、氧化镁、氧化锌、氮化铝和氮化硼是最常列举的用于热产品的导热和电绝缘的填料。氮化硼由于其优良的传热特性和相对价廉而特别有用。
然而，为了用目前所用的填料如氮化硼达到充分的导热性，粘结剂中需要加入大量的填料。例如参见美国专利No.5,898,009，No.6,048,511和欧洲专利No.EP0939066A1(都属于Shaffer等)，这些专利揭示另一种达到固体六边形氮化硼加入量接近45体积％的方法。
仍然需要改进的导热填料以及形成这种材料的方法。具体而言，需要能改进对最终产品性能的控制、经济和大量生产这种材料的方法。此外，仍然存在对改进的氮化硼粉末的需要，包括受控密度的粉末如低密度和中密度粉末，保持在应用中如半导体领域的加工和采用所需的足够强度。
除了使用氮化硼粉末作为导热性应用的填充材料外，本领域还需要制备具有在其它最终用途如降低摩擦的应用中采用所要求的目标性能的氮化硼粉末。在这方面，需要高度灵活的制造方法，这种方法采用有成本效益的技术，以高产率制造物理、热、电、机械和化学性质可以在宽范围变化的氮化硼粉末。
发明内容
根据本发明一个方面，一种聚集的氮化硼粉末具有断裂强度与摇实密度(tapdensity)的比值不小于约11MPa·cc/g的聚集体。
根据本发明另一个方面，聚集的氮化硼粉末具有断裂强度与包封密度(envelope density)的比值不小于6.5MPa·cc/g的聚集体。
根据本发明的一个方面，提供一种形成聚集的氮化硼粉末的方法，该方法使用了含氮化硼聚集体的原料粉末。这种原料粉末一般具有粒度不大于约5微米的细晶体。然后热处理该原料粉末，形成热处理的聚集的氮化硼粉末。
根据本发明另一个方面，提供一种微电子器件，该器件包括有效元件、基片、在有效元件和基片之间的热界面材料。有效元件通常产生热量，热界面材料包含断裂强度与包封密度比值不小于6.5MPa·cc/g的聚集体。
根据本发明另一个方面，提供一种印刷电路板，该电路板包含多个层，所述多个层包含至少一层含有断裂强度与包封密度的比值不小于6.5MPa·cc/g的聚集体的层。
根据本发明的另一个特征，提供一种复合结构的元件，该元件包含基体相和断裂强度与包封密度的比值不小于约6.5MPa·cc/g的聚集体。
根据本发明另一个方面，提供一种形成聚集的氮化硼粉末的方法，该方法中形成含聚集体的松散氮化硼粉末。然后，从该松散粉末中取出一部分的氮化硼聚集体，形成原料粉末，加热原料粉末形成聚集的氮化硼粉末。
根据本发明的另一个实施方式，提供一种形成聚集的氮化硼粉末的方法，该方法中形成含乱层氮化硼的氮化硼聚集体的原料粉末。然后对该原料粉末进行热处理，形成热处理的聚集的氮化硼粉末。
根据本发明的一个特征，聚集的氮化硼粉末进行热处理后可以进行机械搅拌操作，如破碎。这种方法能有效打破通常在热处理期间形成的聚集体间的弱键，使粒度分布类似或很接近于初始原料粉末的粒度分布。通常，至少25重量％的热处理氮化硼粉末在破碎后的粒度在原料粉末的初始粒度范围之内。
附图说明
本领域的技术人员参照下面附图能更好理解本发明，并且本发明的许多目的、特征和优点也将是显而易见的。
图1所示是按照本发明的一个实施方式形成聚集的氮化硼粉末的具体工艺流程的流程图。
图2所示是六边形氮化硼的理想晶体结构。
图3所示是用于表征本发明的实施方式的测试设备。
图4所示是按照本发明的一个实施方式的印刷电路板的截面图。
图5所示是一个微电子器件，包括通过用传热膜粘结在基片上的集成电路。
图6所示是结合了本发明一个实施方式外壳的手提电脑。
在不同附图中使用相同标记符号来表示类似或相同的部件。
具体实施方式
参见图1，所示为形成聚集的氮化硼粉末的一般工艺流程。该工艺流程从供给氮化硼压块或小球开始。通常，氮化硼压块或小球由氮化硼粉末压制为压块或小球形式形成。压块或小球的尺寸并不是特别重要，依据形成压块或小球的方法(如，滤饼，辊压紧(roll compact)、丸压制、等压压制)，其密度可以在宽范围变化。虽然本发明的实施方式利用了较小如几克数量级的压块或小球，但是也可以加工较大的如100千克数量级的压块。
初始加工氮化硼压块或小球的目的是提供能按照本发明实施方式使用的原料粉末。原料粉末一般采用以下方法形成，首先在步骤10破碎氮化硼压块或小球。破碎压块的合适方法包括颚式破碎和辊破碎。压块或小球破碎成具有要求的聚集体粒度或直径的氮化硼聚集体。较好地，压块或小球被破碎成约10-1000微米的氮化硼聚集体。除了颚式破碎和/或辊破碎外，可以碾磨松散粉末，以形成更加小的颗粒，如由很细晶体如粒度小于10微米的晶体形成的颗粒。
一个实施方式中，采用颚式破碎、辊破碎和/或细碾磨的任意组合来破碎形成松散粉末后，在步骤16对该松散粉末进行分级，形成后面加工所需的原料粉末。大于目标粒度的粗聚集体可以再破碎和分级，直到这些聚集体在目标粒度分布之内。但是，更常用的是在步骤12压制松散粉末。压制通常以冷压或等压压制形式进行，在这一中间步骤形成新的大块(log)、压块或小球，它们具有要求的结晶度和B2O3含量性质。压制之后，新的大块、压块或小球在步骤14破碎。压制和破碎步骤12和14可以重复任意次，以改进所得的原料粉末的晶体大小、粒度、粒度分布以及B2O3的含量。
在步骤16分级的原料粉末以及松散粉末含有聚集体。本文中所用的聚集体是氮化硼晶体的集合，晶体结合在一起形成各个可识别的颗粒。虽然这样的聚集体通常由晶体形成，但是聚集体可以是部分或完全玻璃质的，如在有杂质或乱层氮化硼的情况。
根据本发明的一个实施方式，从粉末中除去非聚集的氮化硼颗粒(如，小片或晶体区)以及不在要求的原料粉末粒度分布之内的聚集体。这种非聚集的氮化硼颗粒粒度通常小于10微米。较好地，除去非聚集的氮化硼颗粒至小于约5％，更好小于约1％，如小于约0.1％。除去非聚集的颗粒的合适方法包括筛分、空气分级和淘析，(参见Chem.Eng.Handbook，Perry&Chilton，5th Ed.，McGraw-Hill(1973)，其全文内容被结合作为参考)。这类除去方法为本领域众所周知，本文只简单说明。
通常，通过筛分进行分级。筛分是通过筛面将不同粒度的固体颗粒/聚集体的混合物分离为两个或多个部分。筛面有开孔，小颗粒/聚集体通过开孔流出，而大颗粒/聚集体留在上面。对大粒度和小粒度的颗粒/聚集体流均可以按照需要多次重复这一过程，通过不同的筛孔，达到将颗粒/聚集体分级到要求的颗粒/聚集体粒度范围。
根据图1所示流程图的一个特征，破碎和分级之后，以及任选的压制和破碎操作步骤12和14之后，提供具有要求的性质的原料粉末。原料粉末由在具体预定的粒度范围内的聚集体形成，这些聚集体取自松散氮化硼聚集体粉末。在此，单独的聚集体是由细晶体(也称作晶体区)组成。这些晶体通过聚集体间的键合而结合在一起，通过SEM分析能分别识别。通常要求晶体的平均晶体大小不大于约5微米。更好地，晶体的平均晶体大小不大于约4微米，最好不大于约2微米。
虽然已经结合破碎氮化硼压块描述最初加工形成原料粉末，但应理解可以采用不同的加工方法来制备原料粉末，例如，在氮存在下硼氧化物的碳热还原，蜜胺化合物反应用作强还原氮化合物的来源，将硼氧化物还原为氮化硼和用氨直接渗氮。或者，如三氯化硼和氨的试剂在热解过程中反应形成高纯氮化硼。在强调纯度超过加工产量的情况，这种方法对形成高纯度氮化硼粉末特别有用。
虽然对原料粉末以及加工步骤的操作的说明都集中在供给很细晶体尺寸的原料粉末，但也注意到原料粉末可以是完全或部分乱层的。例如，一个实施方式中，乱层含量至少为10重量％，如至少20、30或40％的乱层。某些实施方式的乱层量占大部分。在这方面，这样的乱层氮化硼粉末的结晶指数通常小于0.12。对乱层氮化硼的性质和晶体结构的更详细说明可参见Hagio等，“六边形氮化硼晶体的微结构形成(Microstructural Development with Crystallization of Hexagonal BoronNitride)”J.Mat.Sci.Lett.16：795-798(1997)，其全文内容结合作为参考。
通常，原料粉末、压块、大块或小球(在此都称作致密体)的密度约为0.3-2.0g/cc。在这方面，通过从压块、大块或小球切下并称重已知每一面尺寸的立方体，来测量原料粉末致密体的密度。另一种表征原料粉末的方法是测定用于进一步加工的最初摇实密度。根据本发明的几个实施方式，最初摇实密度在约0.2-1.0g/cc范围内。
再参见压制步骤12，如本领域所理解的，通常采用等压进行压制。处理时压力通常超过5,000psi。更典型的大于10,000psi，优选大于15,000psi，甚至20,000psi。二次破碎步骤14和随后分级步骤16之后，通常存在在要求的原料粉末粒度范围之外的颗粒。例如，大于目标粒度分布的粗聚集体可以再破碎并分级，直到粒度在目标范围内，而小于最小聚集体粒度的小聚集体和非聚集的颗粒从原料粉末中排除。在后一种情况，排除的粉末可以循环，通常是将循环的粉末再次进行压制步骤12，随后进行破碎步骤14，如图1所示。这样循环的粉末一般与引入的依照破碎步骤10形成的初始粉末混合。或者，通过单轴压制(压成丸或压片)的辊压紧或压块进行压制步骤12。如前面所述，施加足够的压力来获得要求密度的固结体。或者，采用湿法形成致密体，从而喷雾干燥或过滤氮化硼的浆液形成致密体。
虽然聚集的原料粉末的粒度范围很大程度上依据对最终粉末产品要求的最终性质来变化，但原料粉末的粒度通常在约20-1,000微米范围，通常约为40-500微米。为严格控制最终产品的粒度，通常加工到在前述宽范围内的窄粒度范围。本文中，粒度范围通常由上述筛分方法所决定。在这方面，注意到筛分并不是一种理想的方法，因此存在一定比例的不合需要的粒度的颗粒，最典型的是在底部筛上的产物中的细颗粒，从而使粒度范围移向略小于列举的范围。
如图1所示，分级后，原料粉末在步骤18进行烧结操作。在此，对粉末形式，而不是任何松散形式如块、小球或大块的氮化硼聚集体进行烧结。在烧结操作中，通常聚集体通过弱的聚集体间的键结合在一起(颈缩)。因此，一般要求对热处理或烧结后的粉末在步骤20进行破碎操作。如上面结合步骤10所述的，步骤20的破碎操作可采用各种方法进行，包括颚式破碎和粗辊破碎，虽然在步骤20通常不进行碾磨，以保持尽可能接近初始原料粉末的最初粒度(聚集体)范围。
通常，步骤18的烧结操作在能促进晶体生长和非晶相(乱层)晶体的温度下进行，以形成通常六边形晶体结构的热处理产物。在这方面，烧结温度通常高于至少约1,400℃，如在约1,600-2,400℃范围。烧结温度范围为1,800-2,300℃，具体在约1,850-1,900℃范围。通常，烧结时的环境是惰性的，以减小或防止与氮化硼粉末的不希望有的反应。在这方面，一般对烧结炉抽真空，如在低于约1个大气压的压力。烧结环境中存在的气体通常是惰性气体，如氩气或氮气(N2)。根据炉子设计和加热速率，通常热处理制备进行约0.25-12小时。
由于烧结操作的结果，原料粉末的密度通常会下降，这与其它类型的陶瓷材料的烧结操作不同。对“烧结”期间密度下降的一种解释是通过非致密化扩散过程如同气相传送在相邻颗粒之间形成颈缩。(参见Modern Ceramic Engineering，D.W.Richerson，Chapter7，1982)。通常可观察到密度下降至少约0.1g/cc，如至少0.2g/cc。热处理粉末的特定例子的摇实密度在步骤20破碎和步骤22分级后在约0.2-1.0g/cc量级。在这方面，分级步骤22可采用对结合分级步骤16所述的任一种方法进行。
根据本发明的一个实施方式，分级步骤22显示至少25重量％的热处理后聚集的氮化硼粉末(破碎后)在原料粉末的初始粒度范围之内。通常，热处理的氮化硼粉末(破碎后)的平均粒度至少为20微米，粒度范围约为40-500微米。在这方面，一般要求最终粉末产物的粒度分布接近最初原料粉末的粒度分布。这一特征能比本领域目前加工技术如依赖小球、块、大块或压块形式的氮化硼热处理的方法有效提高最终热处理后破碎并分级的聚集的氮化硼粉末的产率。
热处理的聚集的氮化硼粉末通常是六边形晶体结构。六边形氮化硼是一种惰性光滑的(lubricious)陶瓷材料，具有片状(platey)六边形晶体结构(类似于石墨的结构)(“h-BN”)。参见图2能容易地说明h-BN的众所周知的各向异性的特性，图2显示六边形的h-BN颗粒。h-BN颗粒小片的直径是如图2中所示的D，并称作a-方向。BN共价结合在在a-方向平面。颗粒厚度尺寸是所示的Lc，它垂直于直径，并称作c-方向。堆叠的BN六边形(即在c-方向)通过范德华力(相对较小)结合在一起。
最终热处理的破碎和分级的聚集氮化硼粉末具有六边形的晶体结构，从高度有序的六边形晶体结构到混乱的六边形结构。这种粉末的结晶指数通常约为0.12和更高。(参见Hubacek，“乱层的层状氮化硼的假设模型(Hypothetical Model ofTurbostratic Layered Boron Nitride”J.Cer.Soc.of Japan，104：695-98(1996)，其全部内容结合作为参考)。
此外，烧结操作能有效挥发杂质和表面氧化物致污物。得到的产物在破碎前是弱聚集的聚集体的“饼”，容易破碎到类似于原料粉末最初粒度分布的粒度分布。
注意到虽然如图1所示在步骤12和16之间，和步骤20和22之间有循环步骤，但在图1所示的基本流程的各个处理步骤之间可以采用循环步骤。
最终聚集的氮化硼产物通常有特别是相对于其包封密度(实际聚集体的密度)和/或粉末摇实密度(粉末的堆积密度(bulk density))的较高的断裂强度，。例如，一个实施方式的断裂强度与摇实密度的比值不小于约11MPa·cc/g，如不小于约12MPa·cc/g，13MPa·cc/g，甚至14MPa·cc/g。按照包封密度，这样的比值通常不小于6.5MPa·cc/g，如不小于6.7MPa·cc/g，或不小于6.9MPa·cc/g。
关于粉末粒度特性，粉末具有在约20-500微米范围的平均聚集体粒度，如约40-200微米。在这方面，某些实施方式有至少60％的粉末在约40-200微米的粒度分布范围内，或有至少80％的粉末在40-150微米范围内。
根据本发明的实施方式，形成具有上面特征的粉末。然而，其它实施方式在各种应用中使用这些粉末。例如，再参见图4，提供一种印刷电路板200，它包含多个层206-218形成的叠层204。如图所示，其中相反的主表面之一包含多个焊接凸起，用来与其它电子元件电连接。虽然并未示出，印刷电路板的相反的主表面可以有电轨迹沿该轨迹发送电信号。按照图4所示的实施方式，206-218中任何一层或多层可包含上面所述的聚集体。通常，加入足够比例的聚集体，使聚集体形成互连的网络并一般相互接触用于有效传热。聚集体的这种互连网络在此指一种渗流的结构，一般能形成骨架结构，该结构延伸通过并嵌埋在基体相中。通常，这种基体相由聚合物包括有机聚合物形成。某些实施方式中，为了加工方便，要求使用热塑性聚合物。根据本发明的实施方式，含有聚集体的层有利地提高了要求电子应用的印刷电路板的传热。
再参见图5，所示为本发明的另一个实施方式，包括微电子器件。在这一特定实施方式中，微电子器件300包括包封态的半导体管芯302，即固定在下面基片304的倒装片(flip-chip)，该芯片用于和其它微电子器件电连接。微电子器件300包括传热膜310，它包含在基体相通常是聚合物如树脂中的如上所述的聚集体。如上面结合印刷电路板的说明，聚集体形成互连的网络或渗流结构，用来提高集成电路302和下面基片304之间的传热。如本领域一般理解的，集成电路和基片之间的电互连可通过加入结合到半导体管芯上各个焊接点，通过焊接材料回流结合到基片接触件上的焊接凸起306来实现。
根据本发明的另一个特征，提供的复合结构部件包括基体相和如上面所述的聚集体。该复合结构部件可以采取各种结构形式，在特定实施方式中，形成微电子器件如硬盘驱动器的集成部件。在这种硬盘驱动器特定情况，部件可以是传动装置臂(actuator arm)。
或者，结构部件可提供计算机外壳，如图6所示。图6所示是一个笔记本电脑400，有两个半壳402和404的外壳。外壳部分402一般构成结构支撑以及计算机LCD屏的背面，而外壳部分404封闭并保护手提电脑400的敏感的微电子部件，并包括底表面406。宜用复合材料形成该外壳，根据本发明实施方式，该复合材料包括基体相和聚集体。基体相可以是一种结构合理的聚合物材料，如热塑性聚合物。虽然图6显示手提电脑，应理解该外壳可构造成适合于台式计算机，以及用于服务器和其它计算器件。
此外，在各种用于微电子器件的壳体或箱体中，结构部件可以是电话外壳形式，构成电话听筒如移动电话的外结构表面。
下面并不是合适复合结构部件的详尽清单，并且对各种应用(包括微电子应用)能提供无数的几何构形。例如，结构部件可以采取加热管形式，如US6,585,039中概述的，复合加热器，如6,300,607和6,124,579中所述，制动衬块结构，如5,984,055所述，或各种过电压部件，如US6,251,513所述。
下面实施例提及的筛分参数是基于抗拉筛布(tensile bolting cloth)(TBC)标准，除非另外指出。为方便说明，下面表1列出对TBC筛目大小、U.S.Sieve、微米和密耳之间的换算。
表1
Figure BDA00002766806000091
实施例
实施例1
以20ksi等压压制，将约50磅由粒度不大于约5微米的细晶体组成的原料氮化硼粉末固结。形成的材料然后用颚式破碎机，然后用辊型破碎机进行破碎。将形成的粉末进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于150微米，细聚集体为小于40微米。用配有120和200TBC(抗拉筛布)筛的筛分机进行筛分。得到8磅60％大于74微米的材料。该材料在约1900℃热处理12小时，产生高纯度氮化硼饼。用颚式破碎机，然后用辊型破碎机对该饼进行破碎。形成的粉末然后进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于150微米，细聚集体为小于150微米。粒度大于150微米的聚集体再次破碎，直到它们在目标聚集体粒度范围之内，即对本实施例为小于150微米。筛分后得到2磅95％在150微米和74微米之间的材料，其摇实密度约为0.50g/cc。选择直径为125微米的颗粒的强度为8.2MPa。
实施例2.
约50磅由粒度不大于约5微米的细晶体组成的原料氮化硼粉末用颚式破碎机，然后用辊型破碎机进行破碎。将形成的粉末进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于150微米，细聚集体为小于40微米。用配有120和200TBC(抗拉筛布)筛的筛分机进行筛分。得到5磅60％大于74微米的材料。该材料在约1900℃热处理12小时，产生高纯度氮化硼饼。用颚式破碎机，然后用辊型破碎机对该饼进行破碎。形成的粉末然后进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于150微米，细聚集体为小于150微米。粒度大于150微米的聚集体再次破碎，直到它们在目标聚集体粒度范围之内，即对本实施例为小于150微米。筛分后得到2磅95％在150微米和74微米之间的材料，其摇实密度约为0.35g/cc。选择直径为125微米的颗粒的强度为4.5MPa。
实施例3.
以20ksi等压压制，将约100磅由粒度不大于约5微米的细晶体组成的原料氮化硼粉末固结。形成的材料然后用颚式破碎机，然后用辊型破碎机进行破碎。将形成的粉末进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于200微米，细聚集体为小于40微米。粒度大于200微米的聚集体再次破碎，直到它们在目标聚集体粒度范围之内，即对本实施例为小于200微米。通过空气分级，从较大聚集体分离出在破碎期间产生的通常小于10微米的细聚集体和细晶体。用配有88和120TBC(抗拉筛布)筛的筛分机(Kason Corporation，Millburn，N.J.)对产生的181磅粗产物进行筛分，得到3磅60％大于150微米的材料。该材料在约1900℃热处理12小时，产生高纯度氮化硼饼。用颚式破碎机，然后用辊型破碎机对该饼进行破碎。形成的粉末然后进行筛分，分离成细和粗的聚集体。对本实施例，粗聚集体为大于200微米，细聚集体为小于200微米。筛分后得到2磅95％在200微米和74微米之间的材料，其摇实密度约为0.50g/cc。选择直径为150微米的颗粒的强度为7.5MPa。
按照上面的工艺流程，制备另外的样品作为实施例5-7的样品，这些样品的摇实密度列于下面表2。此外，制备比较例1、2和3的样品用来比较测试。比较例样品的制备方式类似于上面实施例1-3，明显不同的之处是比较例中对大块或压块形式的材料进行热处理，而不是如本发明实施方式所述的对聚集的粉末形式进行热处理。所有样品都进行聚集体强度测试，具体是使用图3所示的测试设备。该设备由小的加载机构100和移动台阶110组成。该台阶在x、y和z方向移动，并用步进电动机(Newport PM500Precision Motion Controller)控制。z-向运动设定为2微米/秒。使用4.9N(500g)测力传感室102，将样品放在高抛光的平行SiC平台104和106上。该台阶的运动通过LabView控制。以20个数据点/秒的取样速度获取数据，产生0.1微米和0.01N的分辨率。
通过手工从样品批料中拾取类似粒度的聚集体，得到测试的样品，测试单一聚集体的断裂强度。假设不规则形状是处于球体和立方体之间，计算每个聚集体的有效拉伸强度，得到
σe＝1.37(P/a2)
式中，P是断裂负荷，a是聚集体直径(粒度)。
按照ASTM B527-70测定摇实密度。
包封密度用Hg孔隙仪，通过在40Kpsi压力下渗透液体Hg进行测定。包封密度代表样品聚集体的平均密度，与摇实密度不同，后者是堆积密度的测定值。
表2
Figure BDA00002766806000111
根据前述，提供相对高强度的受控密度的粉末，特别是提供适用于导热应用的高强度低密度和中密度的粉末。此外，这种粉末一般具有各向同性的热和结构性能。此外，本发明的实施方式还提供了形成聚集的氮化硼粉末的加工方法。这种方法是高度灵活，能有效提高产率，因此是有成本效益的。虽然按照本发明实施方式的粉末特别适用于导热应用，如在半导体领域，但是这种加工方法是灵活的，能形成用于其它应用的氮化硼粉末。

Claims (13)

1.一种经烧结的聚集的氮化硼粉末，包含断裂强度与摇实密度的比值不小于约11MPa·cc/g的经烧结的聚集体。
2.如权利要求1所述的粉末，其特征在于，所述比值不小于约12MPa·cc/g。
3.如权利要求1所述的粉末，其特征在于，所述比值不小于约13MPa·cc/g。
4.如权利要求1所述的粉末，其特征在于，所述比值不小于约14MPa·cc/g。
5.如权利要求1所述的粉末，其特征在于，所述粉末的平均聚集体粒度在约20-1000微米范围。
6.如权利要求1所述的粉末，其特征在于，所述粉末的平均聚集体粒度在约40-500微米范围。
7.如权利要求1所述的粉末，其特征在于，所述粉末的平均聚集体粒度在约40-200微米范围。
8.如权利要求1所述的粉末，其特征在于，所述粉末的平均聚集体粒度在约20-90微米范围。
9.如权利要求1所述的粉末，其特征在于，至少60重量％的所述粉末的粒度分布在约40-200微米范围。
10.如权利要求1所述的粉末，其特征在于，至少80重量％的所述粉末的粒度分布在约40-150微米范围。
11.如权利要求1所述的粉末，其中所述粉末包含断裂强度与包封密度的比值不小于约6.5MPa·cc/g的聚集体。
12.如权利要求11所述的粉末，其特征在于，所述比值不小于约6.7MPa·cc/g。
13.如权利要求11所述的粉末，其特征在于，所述比值不小于约6.9MPa·cc/g。
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