CN1799992A - 生产氮化硼的方法 - Google Patents

生产氮化硼的方法 Download PDF

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Publication number
CN1799992A
CN1799992A CNA2005101363840A CN200510136384A CN1799992A CN 1799992 A CN1799992 A CN 1799992A CN A2005101363840 A CNA2005101363840 A CN A2005101363840A CN 200510136384 A CN200510136384 A CN 200510136384A CN 1799992 A CN1799992 A CN 1799992A
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CN
China
Prior art keywords
lithium
compound
doping agent
boron nitride
nitrate
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Pending
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CNA2005101363840A
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English (en)
Inventor
D·W·小普尔茨
L·马尼恰
C·拉曼
A·穆鲁盖亚
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Momentive Performance Materials Inc
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General Electric Co
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Publication of CN1799992A publication Critical patent/CN1799992A/zh
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Abstract

一种生产高纯度和高导热系数氮化硼的方法，其中在掺杂剂的存在下，在至少1000℃使含氧硼化合物和含氮源反应至少一小时，并且其中掺杂剂形成蒸发温度低于该方法中最高加工温度的金属硼酸盐杂质。

Description

生产氮化硼的方法
相关申请的交叉引用
本申请要求2004年12月28日提交的U.S.60/639,714的优先权，该专利申请在此处全部引入作为参考。
技术领域
本发明通常涉及使用高纯度氮化硼产品的掺杂材料生产六角形氮化硼的方法。
背景技术
氮化硼是热稳定、高度耐火的材料，商业重要性在不断增加。通常，生产氮化硼的方法中使用硼酸作为反应组合物的硼来源。从硼酸生产氮化硼的建议方法公开于美国专利No.2,922,699；3,241,918；和3,261,667，以及英国专利No.874,166；874,165；和1,241,206中。日本专利公开No.06-040713公开了一种从硬硼酸钙石生产氮化硼的方法。
在生产氮化硼的现有技术方法中，硼酸盐原料，其包含碱/碱土金属化合物-特别是钠和钙化合物-当用氨在1200℃或更高温度下吹扫时，形成氮化硼，加上需要附加洗涤/处理步骤以回收高纯度的氮化硼的副产物。一些副产物是多种形式的硼酸钙，其通过盐酸浸出从氮化硼除去。其它方法使用去离子水洗涤纯化氮化硼。美国专利No.3,415,625公开了在洗涤/处理步骤后高纯度氮化硼产物的连续或间歇法。
美国专利No.4,045,186公开了使用Li3N与小粒径氮化硼反应，随后从混合物中在大于1100℃的高温下，再结晶形成较大尺寸的结晶六角形氮化硼。中国专利公开No.CN1539729A公开了从三氟化硼醚和一氮化三锂用溶剂热合成法制备氮化硼的方法。德国专利公开No.DE4108367C1公开了一种制备主要为六角形结构的氮化硼的方法，该方法包括在20-230℃下，将一氮化三锂(无水二(2-6C)烷基醚中)的悬浮液和过量的三氟硼烷二(1-6C)烷基醚合物(优选二丁基醚合物)搅拌反应2-24小时。
除了洗涤要求，并且在洗涤步骤之前，现有技术方法通常需要两步方法生产氮化硼晶体。第一步是锻烧步骤，其中将反应物加热至高达1100℃的温度，形成“湍层”形式不完全反应的氮化硼。第二烧结步骤中，将湍层氮化硼加热至1500至2300℃温度，以控制最终氮化硼产物的结晶度和纯度。
本发明涉及制备高纯度和优良产率氮化硼的方法。另外，本发明方法中，将煅烧和烧结步骤合并成一个焙烧步骤，其中蒸发出金屑硼酸盐杂质，形成高纯度氮化硼晶体。最后，本发明涉及一种改进的方法，其中反应产物的洗涤/浸析对于高纯度氮化硼是任选的。
发明内容
本发明涉及生产高纯度和高导热系数多晶六角形氮化硼(hBN)化合物的方法，通过在掺杂剂的存在下，在至少1000℃的温度下，将含氧硼化合物和含氮源反应至少一小时，其中掺杂剂是含金属化合物，其形成蒸发温度低于最高加工温度的金属硼酸盐。
本发明进一步涉及在作为掺杂剂的硝酸锂存在下，生产六角形氮化硼化合物的方法。
最后，本发明涉及一种在作为掺杂剂的硝酸锂存在下，生产六角形氮化硼化合物的方法，其中加工温度为1000至2300℃。
具体实施方式
此处使用的估计语言可以用于修饰任何数量表示，所述数量表示可以改变，但不产生与其相关的基本功能改变。因此，用术语(一个或多个)，例如“约”和“基本上”修饰的值，有时可以不限于规定的精确值。
术语“加工温度”可以替代地使用术语“工艺温度”，其是指生产本发明hBN方法中设备/步骤中的温度。
术语“最高加工温度”或“最高工艺温度”是指生产本发明hBN方法中使用的步骤和/或设备中测量的最高工艺温度。
此处使用的氮化硼导热系数是指使用可商购的Hot Disk恒定热分析仪测量的样品导热系数，该样品由40体积％的hBN(大约60wt％)在Sylgard 184硅氧烷树脂和Sylgard 184固化剂(两者都可从Dow Coming Corp商购)中的混合物制备。说明性实例是10.0g的BN材料在6.24g的Sylgard 184硅氧烷树脂和062gSylgard 184固化剂中的混合物。混合后，固化该样品并制备样品垫板，测量导热系数。测试导热系数的Gage R&R数据表明结果精确度为+/-0.5W/mK以内。
用于本发明方法的原料。通常生产氮化硼的方法中，硼源和氮源用作原料，反应形成硼原子和氮原子共存的化合物。本发明涉及生产高纯度氮化硼的方法，其中在高温反应中，将掺杂剂与含氧硼化合物和有机含氮化合物的原料混合。反应期间从掺杂剂金属形成的金属硼酸盐蒸发，因此不需要浸析或洗净。
在本发明的一个实施方案中，含氧硼化合物选自硼酸、氧化硼、提供氧化硼的物质，例如三氧化二硼、二氧化二硼、三氧化四硼或五氧化四硼、和硼酸盐矿石，例如硬硼酸钙石、钠硼解石、白硼钙石、赛黄晶、硅钙硼石和其混合物。在本发明的一个实施方案中，含氧硼化合物包含50wt％硼酸和50wt％钠硼解石。在本发明的另一个实施方案中，使用硼酸作为含氧硼化合物。
在本发明的一个实施方案中，含氮化合物包含有机伯、仲和叔胺，例如二苯胺、双氰胺、亚乙基胺、六亚甲基胺、三聚氰胺、脲和其混合物。在一个实施方案中，使用三聚氰胺作为含氮化合物。
与原料混合的掺杂剂选自其形成的金属硼酸盐的蒸发温度低于最高加工温度的化合物。这种含金属化合物的实例包括钡化合物，例如氧化钡；铯化合物例如氧化铯；钾化合物例如氢氧化钾；锶化合物例如氧化锶；铷化合物例如氧化铷；和锂化合物例如氧化锂、硝酸锂、乙酰丙酮化锂、环戊二烯(cyclopentadienide)锂、酞菁二锂、二锂盐、乙酸锂、乙酰丙酮化锂、氨基化锂、双(三甲基甲硅烷基)氨基化锂、四氢硼酸锂、碳酸锂、二甲基氨基化锂、氢化锂、氢氧化锂、偏硼酸锂、钼酸锂、铌酸锂、高氯酸锂、过氧化锂、四硼酸锂、氢硼化锂、三乙基氢硼酸锂和草酸锂；和其混合物。
在一个实施方案中，使用硝酸锂作为起始混合物的掺杂材料，形成在低于最高加工温度1800℃的温度蒸发的硼酸盐化合物，使得从氮化硼反应产物除去杂质的最终洗涤/浸析步骤成为任选的步骤。
在一个实施方案中，原料包含30至55wt％硼酸、40至50wt％三聚氰胺、和1至5wt％含锂掺杂材料。在另一个实施方案中，原料包含52.5wt％硼酸、44.5wt％三聚氰胺和3wt％硝酸锂。
方法步骤：本发明生产hBN的方法可以间歇法或连续法进行，包括下列方法步骤。
混合/共混。初始步骤中，将包括掺杂剂的原料混合，或在合适的设备例如混合器中以干燥状态共混在一起。
任选的预加热/干燥步骤：在本发明的一个实施方案中，混合供混步骤后，在约100至400℃将原料干燥0.5至15小时，以赶走反应物中任何水分，并在原料中产生孔隙，形成小块、大块或颗粒形式的材料聚集体。
在一个实施方案中，在150至250℃的温度下进行干燥。干燥操作可以在空气、或氮气或氨气气氛中进行。干燥时间取决于干燥温度，此外还取决于干燥步骤是否在静态气氛或循环空气或气体中进行。在一个实施方案中，干燥时间为在静态环境中在200℃4小时至在150℃15小时。另一个实施方案中，原料在250℃下干燥3小时。
在一个实施方案中，反应物和掺杂剂包含在容器/胶囊中，并置于高达1000℃的高温炉(推杆炉或旋转式烘干炉)中高达2小时。在该预热步骤中，通过逆流氮气引导逸出气体朝向炉入口，控制气体的逸出。
任选的粉碎前体：在一个实施方案中，混合供混步骤后或干燥步骤后，使用常规设备例如辊碾磨机、十字型碾磨机、滚动磨盘等，将起始原料粉碎或破碎成为可以随后压实的小块。在一个实施方案中，将粉碎材料破碎成为每个重量为10mg至10g的块。在另一个实施方案中，该材料破碎成为每个重量约0.2g的块。
任选在粉碎步骤后，当硼源是碱或碱土金属硼酸盐化合物例如钠硼解石时，将粉碎材料与二氧化硅混合。钠硼解石中的钙与二氧化硅反应，产生硅酸钙，限制否则可能生成的3CaO.B2O3的形成，因而在最终反应中产生高产率的BN。在一个实施方案中，二氧化硅相对于钠硼解石的总量保持在SiO2/CaO的摩尔比率小于0.5。在第二实施方案中，摩尔比率保持在小于1.0的比率。
任选的预加热和压实(“造粒”)步骤：在一个实施方案中，在混合/共混步骤后，干燥/粉碎混合前体，并使用本领域已知的方法尤其是例如制片、压块、挤出、造粒和压缩，进行压实。该步骤中，将粉碎的混合物压实成为每个重量0.1g至200g的颗粒。在一个实施方案中，颗粒具有～10g的平均重量。在第二实施方案中，将粉碎的混合物压实成为平均重量约2g的颗粒。
在一个实施方案中，压实/造粒步骤在一个挤出步骤中进行，其中将包含掺杂剂和任选二氧化硅的原料与粘合剂送入双螺杆挤出机或类似设备，其中粘合剂为例如聚乙烯醇；聚氧乙烯基非离子型表面活性剂；聚羧酸盐例如丙烯酸、甲基丙烯酸、衣康酸、别失水苹果酸(boletic acid)和马来酸；聚噁唑啉例如聚(2-乙基-2-噁唑啉)；硬脂酸；N，N′-亚乙基双硬脂酰胺；失水山梨糖醇化合物例如单硬脂酸失水山梨糖醇酯等。然后从挤出机引出时干燥该材料并造粒。
在连续过程中，引出的颗粒可以直接送入下一步骤的反应容器中，或在另一个实施方案中，在送入反应容器之前经过200℃的加热炉进行附加干燥加工，其中在反应容器中形成本发明高纯度的氮化硼。
结合的锻烧和热处理步骤：在下一步骤中，在反应室中，在含氮气氛下焙烧颗粒，其中将反应室从室温以每小时20至1200℃的速度加热到1200至2300℃的高温。然后保持加工温度约1至30小时，其中以足够支持非氧化环境的速度保持氮气吹洗。
在一个实施方案中，颗粒保持在氨气中，同时焙烧至1200至1600℃2至12小时。在第二实施方案中，在1400℃焙烧颗粒约4小时。在第三实施方案中，从室温以500℃每小时的速度，将颗粒焙烧至1800℃。然后将温度保持在1800℃5小时，其中保持氮气吹洗。
在另一个实施方案中，使用例如等离子体射流加热炉，在超过2000℃的加工温度下进行反应，以获得高反应速度。在另一个实施方案中，含氮气氛是氨气和惰性气体的混合物。
如上所述步骤可以以间歇法进行，从而将松散颗粒引入反应室进行焙烧。在另一个实施方案中，将该步骤作为连续过程的一部分进行，其中将颗粒连续送入反应容器。在连续过程的一个实施方案中，用强迫进料机构使反应容器穿过加热炉组件，其中随着将每个容器引入加热炉组件，每个在前容器经过加热炉移动一个容器长度。
应该注意到在本发明方法中，在单个步骤中，在升高的加工温度焙烧包含反应物和掺杂剂的颗粒，形成BN晶体，这与其中需要两步方法的现有技术方法相反。
此处单个结合锻烧和热处理的步骤(与现有技术的两个步骤相反)的最终产物是具有至少99％高纯度氮化硼的高结晶度产物。在一个实施方案中，BN产物具有至少99.5％的纯度。
此处使用的高结晶度BN产物是指均匀、平滑触感的产物，它具有至少90％氮化硼纯度，并且通常超过99％纯度。结晶度涉及摩擦期间“触摸”的平滑度，与较差结晶材料的粗糙、白垩触感相反(如在现有技术的2步方法的第一步骤后得到的材料，其中在高达1100℃的锻烧步骤中形成湍层氮化硼)。
任选的研磨步骤：最后，任选地将焙烧颗粒的反应产物冷却至通过喷射研磨进行研磨之前的温度，其中将其研磨成为尺寸为0.1至60微米的片晶形式的高纯度氮化硼产物。在一个实施方案中，将反应产物研磨成为平均粒径为1至5微米的粉末。尺寸是标称的，因为各个颗粒不具有该尺寸，而是松散粘合超细、亚微米微晶的团聚体具有该尺寸。
在本发明的另一个实施方案中，粉碎并筛选氮化硼粉末，以产生40目至325目的烧结体，该材料可以用于热应用。
应注意到本发明反应产物比现有技术无掺杂方法的氮化硼明显更纯。如之前说明的，估计在相对低的温度蒸发出金属硼酸盐杂质，得到高纯度氮化硼产物。
其它任选的后处理步骤：如所说明的，本发明方法的氮化硼产物具有高纯度，从而不需要酸洗/浸析。然而，在本发明的一个实施方案中，作为特别纯度氮化硼产物的任选步骤，任选对产物进行洗涤处理。在一个实施方案中，用溶剂例如甲醇或1％的硝酸水溶液洗涤最终的BN产物，以产生细小的、白色、高纯度结晶氮化硼粉末。
在本发明的另一个实施方案中，进一步在非氧化气体气氛例如氮气、氨气或氩气中，在1700至2100℃下热处理或烧结本发明的BN产物。该处理导致结晶发展，产生具有改善的结晶度和纯度，并且导热系数至少为0.3W/mK的BN产物。在本发明的一个实施方案中，BN粉末具有3至15W/mK的导热系数。
本发明生产的BN粉末的应用：本发明高纯度氮化硼粉末可以用作热控制应用的填料，例如在复合材料、聚合物、润滑脂和流体中的填料。此外氮化硼粉末可以用于热压应用，或作为转化六角形氮化硼至立方氮化硼中的前体原材料。在另一个实施方案中，该材料用于生产六角形氮化硼糊剂。如此处使用的糊剂为半固体制剂。该方法包括提供氮化硼浆液，和在能有效产生包含约60wt％至约80wt％固体六角形氮化硼的糊剂的条件下，处理该浆液。
在热控制应用例如导热性片材中，本发明氮化硼用作基体中的填料，其中该基体包含至少一种树脂，选自热塑性树脂例如聚乙烯、聚丙烯、聚苯乙烯、聚对二甲苯、聚醋酸乙烯酯、聚丙烯酸酯、聚甲基丙烯酸甲酯、聚氯乙烯、聚偏氯乙烯、氟基塑料、聚乙烯醚、聚乙烯酮、聚醚、聚碳酸酯、热塑性聚酯、聚酰胺、二烯基塑料、聚氨酯基塑料、聚硅氧烷和无机塑料；和热固性树脂例如酚树脂、呋喃树脂、二甲苯/甲醛树脂、酮/甲醛树脂、脲醛树脂、三聚氰胺树脂、苯胺树脂、醇酸树脂、不饱和聚酯树脂和环氧树脂。
在热控制应用的一个实施方案中，本发明氮化硼用作基体的填料，该基体包含高达60wt％的复合材料，其选自聚硅氧烷、环氧树脂、丙烯酸类树脂、氯乙烯、聚氨酯和其混合物，导热系数为至少0.50W/m.K。
在热控制应用中，发现掺杂剂帮助增加氮化硼产物的导热系数。在实施方案中，其中LiNO3用作生产本发明hBN的掺杂剂或种子(seed)材料，使用本发明BN的样品的导热系数比使用现有技术无掺杂方法生产的BN的样品的导热系数高得多。
实施例1-4：生产四个包含重量比为23∶27的三聚氰胺和硼酸的样品。实施例1仅包括三聚氰胺和硼酸；实施例2包含附加量的1.5wt％硝酸锂；实施例3具有3.0wt％硝酸锂；和实施例4具有5.0wt％硝酸锂。全部样品在275℃干燥一整夜。然后将该干燥材料压成圆柱形颗粒，并在氮气中焙烧，以500℃每小时的速度从室温至1800℃，并保持3小时。将四个实施例制备的颗粒称重，并用球磨机研磨用于分析。生产样品垫板并测量导热系数。
在以下表中给出导热系数(“TC”)结果和从实施例计算的总产率。
表
  实施例1   实施例2   实施例3   实施例4
  掺杂剂％   0.0％   1.5％   3.0％   5.0％
  TC(W/mK)   1.8   1.5   7.2   7.1
  产率(％)   19.3   20.0   19.9   18.2
根据本发明方法制备的氮化硼产物显示出比现有技术产物更高的导热系数，即，具有至少1.5W/mK的导热系数。在某种程度上，导热系数可以用作氮化硼(BN)物质纯度的指标。如果BN产物包含杂质例如硼酸盐化合物或氧，将影响导热。
该书面说明书使用实施例公开本发明，包括最佳方式，此外使得任何本领域熟练技术人员能够生产并使用本发明。本发明可取得专利权的范围由权利要求限定，并可以包括本领域熟练技术人员进行的其它实施例。其它实施例在权利要求范围内，如果它们具有与权利要求字面上语言相同的结构成分，或如果它们包括与权利要求语言无实质差异的等价结构成分。
本文参考的全部引用文献此处清楚地引入作为参考。

Claims (26)

1、一种生产六角形氮化硼化合物的方法，其包括：
在用作掺杂剂的一种或更多种化合物的存在下，在至少1000℃的加工温度下，将含氧硼化合物与含氮源反应至少一小时，以形成六角形氮化硼化合物，
其中掺杂剂是金属化合物，其形成蒸发温度低于加工温度的金属硼酸盐。
2、权利要求1的方法，其中六角形氮化硼化合物显示出至少1.5W/mK的导热系数。
3、权利要求1的方法，其中六角形氮化硼化合物显示出至少3W/mK的导热系数。
4、权利要求1的方法，其中六角形氮化硼化合物显示出至少5W/mK的导热系数。
5、权利要求1的方法，其中在掺杂剂的存在下，在1000至2300℃的加工温度下使含氧硼化合物与含氮源反应。
6、权利要求5的方法，其中加工温度至少是1500℃。
7、权利要求6的方法，其中加工温度至少是1800℃。
8、权利要求5的方法，其中在掺杂剂的存在下，在1000至2300℃的加工温度下，使含氧硼化合物与含氮源反应高达72小时的时间。
9、权利要求8的方法，其中该反应进行高达30小时的时间。
10、权利要求9的方法，其中该反应进行高达12小时的时间。
11、权利要求10的方法，其中该反应进行高达6小时的时间。
12、权利要求1的方法，其中掺杂剂选自钡化合物、铯化合物、钾化合物、锶化合物、铷化合物、硝酸锂、氧化锂、乙酰丙酮化锂、环戊二烯锂、酞菁二锂、二锂盐、乙酸锂、乙酰丙酮化锂、氨基化锂、双(三甲基甲硅烷基)氨基化锂、四氢硼酸锂、碳酸锂、二甲基氨基化锂、氢化锂、氢氧化锂、偏硼酸锂、钼酸锂、铌酸锂、高氯酸锂、过氧化锂、四硼酸锂、氢硼化锂、三乙基氢硼酸锂、草酸锂和其混合物。
13、权利要求12的方法，其中掺杂剂选自氧化钡、硝酸钡、氧化铯、硝酸铯、氢氧化钾、氧化锶、硝酸锶、氧化铷、氮化铷、硝酸锂、氧化锂、乙酰丙酮化锂、环戊二烯锂、酞菁二锂、二锂盐、乙酸锂、乙酰丙酮化锂、氨基化锂、双(三甲基甲硅烷基)氨基化锂、四氢硼酸锂、碳酸锂、二甲基氨基化锂、氢化锂、氢氧化锂、偏硼酸锂、钼酸锂、铌酸锂、高氯酸锂、过氧化锂、四硼酸锂、氢硼化锂、三乙基氢硼酸锂、草酸锂和其混合物。
14、权利要求12的方法，其中掺杂剂的存在量是含氧硼化合物和含氮源总重量的至少1wt％。
15、权利要求12的方法，其中掺杂剂选自氧化钡、氧化铯、氢氧化钾、氧化锶、氧化铷、硝酸锂和其混合物。
16、权利要求13的方法，其中掺杂剂是硝酸锂，并且其中掺杂剂的存在量是含氧硼化合物和含氮源总重量的至少1wt％。
17、权利要求16的方法，其中掺杂剂是硝酸锂，并且其中掺杂剂的存在量是含氧硼化合物和含氮源总重量的至少2wt％。
18、权利要求13的方法，其中掺杂剂选自硝酸锂、氧化锂、乙酰丙酮化锂、环戊二烯锂、酞菁二锂、二锂盐、乙酸锂、乙酰丙酮化锂、氨基化锂、双(三甲基甲硅烷基)氨基化锂、四氢硼酸锂、碳酸锂、二甲基氨基化锂、氢化锂、氢氧化锂、偏硼酸锂、钼酸锂、铌酸锂、高氯酸锂、过氧化锂、四硼酸锂、氢硼化锂、三乙基氢硼酸锂、草酸锂和其混合物。
19、权利要求18的方法，其中掺杂剂选自硝酸锂、氧化锂、碳酸锂、氢化锂、氢氧化锂、偏硼酸锂、过氧化锂、四硼酸锂、氢硼化锂和其混合物。
20、权利要求19的方法，其中掺杂剂是硝酸锂。
21、权利要求1的方法，其中所述方法是连续法。
22、用权利要求1的方法生产的六角形氮化硼化合物。
23、一种制品，包含用权利要求1的方法生产的六角形氮化硼化合物。
24、一种生产六角形氮化硼化合物的方法，该方法包括步骤：
a)形成含氧硼化合物、含氮源和掺杂剂的混合物，掺杂剂存在量为含氧硼化合物和含氮源总重量的至少1wt％；
b)在至少200℃温度下将混合物加热至少0.5小时，以干燥除去混合物中的任何水分；
c)使混合物经历至少1200℃的加工温度至少一小时，以形成六角形氮化硼化合物；
其中掺杂剂是金属化合物，其形成蒸发温度低于加工温度的金属硼酸盐。
25、权利要求24的方法，其中形成的产物具有至少99％的氮化硼纯度。
26、权利要求24生产六角形氮化硼化合物的方法，基本上由步骤a)和c)组成。
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