CN1126122C - 陶瓷电阻的制备方法及其使用 - Google Patents
陶瓷电阻的制备方法及其使用 Download PDFInfo
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Abstract
推荐一种陶瓷电阻，该陶瓷电阻是通过将至少一种硅有机聚合物及至少一种填充剂陶瓷化制成的。填充剂至少包含一种高熔点导电成分。填充剂占无溶剂聚合物-填充剂-混合物总体积的20-50%。通过填充剂所占比例的变化可对电阻率进行调整。该陶瓷电阻特别适用作白炽棒芯的热导体。
Description
本发明涉及陶瓷电阻的制备方法及其应用。
从EP-A 0 412 428 A1中已知建立在包含金属互化物、金属及金属氢化物填充剂的硅有机聚合物基础上的陶瓷。然而并不知道这种陶瓷在电路中用作电阻或导体的情况。
金属热导体的最高使用温度为1300℃，而陶瓷热导体的最高使用温度约为1800℃。现有技术下，只有具有很低或很高电阻率(如MoSi2：2×10-2欧姆厘米；SiC：5欧姆厘米)的陶瓷热导体可供使用。用常规的陶瓷材料几乎不可能得到其间的数值。即使将具有不同电阻率的陶瓷粉末相混合，烧结陶瓷的电阻也只能在很小的范围内变动，因为新的添加质会大大影响可烧结性。
本发明的任务是制成可在高温条件下使用的陶瓷电阻或热导体。本发明的另一个任务是以简单而可靠可再现的方式来调整电阻率。
发明的带有主要要求特征的陶瓷电阻可以解决这个问题，特别是在高温条件下的应用。发明的陶瓷电阻可以使用具有不同电学性质的各种填充剂粉末。可以最大限度地排除陶瓷的不利影响，因为热分解时的密实性在很大程度上取决于聚合物的热分解，而不取决于所用粉末的烧结性能。
试验表明，在遵从所要求的原材料物质成分条件下，在使用常用的塑料及陶瓷加工工艺进行造形时，保证预先给定的电阻率值在热分解后可在10-6至1011欧姆厘米间进行调整。特别是可在1200℃至1500℃的热分解温度区内制成持续稳定的电阻和导体。这时，理论密度可达到70％至98％。
通过其他要求中说明的特征与措施可以进一步加以改善。
如果在惰性气体、氮氢混合气或反应气体中热分解，可得到衰减小、尺寸准确、无裂缝及气孔少的电阻。氩(Ar)、氨(NH3)、氮(N2)及其混合气体最适合用作热分解气氛。
在惰性气体氩气氛中，化学反应只在填充物和聚合物之间进行，不会与气体发生反应。还原性氨气可以降低基体物质中碳含量，从而使其导电能力比在氩气氛条件下更低。在氮(N2)反应气氛中热分解时，填充物和/或基体物质会与热分解气体反应生成氮化物，并可同时改变复合物的导电能力。
为了通过铸造、挤压、热压和/或喷铸进行成形，用一种冷凝连接的，在室温条件下为固体的聚硅氧烷来制成这种电阻或导体被证明是有利的。
发明的陶瓷电阻如果使用二硅化钼与硅的混合物，通过按所需比例加进填充物可有利地显示出正的温度系数。二硅化钼与硅20∶20的电阻材料体积混合比特别适合于白炽元件，其对白炽棒形芯棒来说仅有几秒钟的加热时间。
除了导电的非金属、金属互化物或金属外，经过事先热分解的和/或硬化处理的金属有机聚合物也可很方便地用作填充剂。这样便有可能将各种基体物质的不同的电特性都充分地利用起来作为电阻或导体，同时可避免单一基体物质的缺点并增大了制造的可能性。
下面便借助于几个实例和有关附图来对本发明加以详细的说明：
图1所显示的是例1中二硅化钼占50％体积的复合体的组织情况。图2是发明的两种带正温度系数电阻的电阻率Rspez对温度的依赖关系。图3是发明的一种带负温度系数电阻的电阻率Rspez对温度的依赖关系。
图1显示的是发明的占50％体积、在1200℃氩气流中热分解的二硅化钼填充物的聚硅氧烷电阻的组织10。成分和制法均符合实例1。如图中比例尺所示，晶粒直径平均都在5微米以下。可见的灰色部分是晶粒30，可见的浅色部分是无定形的基体相20。
图2的示意图显示的是1200℃以下温度范围内的电阻。混合填充物占总体积的40％，二硅化钼与硅各占总体积的20％。电阻大约呈线性增加直到大约800℃为止，然后增长幅度变得平缓。填充物二硅化钼占体积的50％、但温度系数仍为正值的材料，其电阻率大大降低。因此可以期望，增加导体混合物的体积百分比可以降低电阻率。
图3显示的是类似于图2的示意图，但占体积50％的填充物是四氮化三硅(β-Si3N4)。随着温度的增高，电阻的导电能力增强，也即该电阻有了负温度系数。为调整到某个恒定的电阻区，也可以用产生电阻正温度系数的填充剂和产生电阻负温度系数的填充剂制成填充剂的混合物。
下文中凡未谈到热分解时保护气的，均按用保护气体氩的实例实施。实例1：
往烧杯内放入23.1克加成聚合的甲基-苯基-乙烯-氢-聚硅氧烷(Wacker硅酮-浸渍树脂H62C)，并将其在50毫升丙酮中溶解。在该溶液中借助磁性搅拌器将126.9克的二硅化钼粉末(H.C.Starck二硅化钼，B等级，粒度d50＝3.0微米，98％＜10微米)搅匀。这对无溶剂的聚合物-填充物-混合物来说，相当于50％体积的填充度。将该悬浮液浇到HostaphanTM胶片上，在50℃的通风干燥柜内将丙酮蒸发掉。也可加入甲苯、己烷、链烃或芳烃等其他溶剂。我们可以得到一种能用手分成一份一份的可塑性物质。将该物质压入模型，在10兆帕的压力及200℃温度下硬化30分钟以上。将如此得到的成形体放在流动的氩气(5升/小时)中按下面表1所给的温度实施热分解：表1
| 加热/冷却速度(℃/分钟) | 结束温度(℃) | 持续时间(分钟) |
| 5 | 450 | 120 |
| 5 | 1200 | 240 |
| 2.5 | 20 |
正如图1所表明那样，该材料大部分由二硅化钼组成。二硅化钼被镶嵌在一种无定形的Si-Ox-Cy基体之中。有少量的二硅化钼与聚合物中的碳反应生成SiC或MoC2，其密度为4.1克/立方厘米，开口孔隙度为14.3％。利用四点技术用BursterDigomat的2302型微欧姆计测量棒形试样的矩形横截面，室温条件下的电阻率Rspcz为2.2×10-4欧姆厘米。材料的四点力学弯曲强度为115兆帕。实例2：
如例1所述，但填充剂二硅化钼粉末被二硅化铬(CrSi2)粉末所代替(H.C.Starck硅化铬，＜10微米，粒度d50＝3.7微米)，体积百分比为40％。热分解后被嵌入无定形基体中的填充剂绝大部分还是二硅化铬。此外也有晶体相CrSi，SiC和SiO2(Cristobalit)存在。热分解后的材料密度为3.5克/立方厘米，开口孔隙度为3.3％。室温电阻率为3.0×10-3欧姆厘米。弯曲强度为120兆帕。实例3：
方法如例1，区别是用50％体积的硅粉末来代替二硅化钼粉末。(H.C.StarckSiMP，B10，粒度d50＝4.4微米)。硅填充剂几乎不变化，只生成很少量的SiC。该材料密度为2.1克/立方厘米，开口孔隙度为3.3％。室温电阻率为1.0×102欧姆厘米。弯曲强度为70兆帕。实例4：
如例1所述，但在28.5克的硅氧烷树脂内要加进由19.5克硅粉末和52.0克二硅化钼粉末组成的混合粉末。这相当于硅占20％体积(H.C.Starck SiMP，B10)和二硅化钼占20％体积(H.C.Starck硅化钼，B级)的填充剂含量。热分解后的材料密度为3.2克/立方厘米，开口孔隙度为0.3％。室温电阻率为1.6×10-3欧姆厘米。弯曲强度为120兆帕。实例5：
如例1所述，但42.2克的硅氧烷被溶于100克的丙酮中。在该溶液中弥散有49.8克的碳化硅(Kempten电化学熔融厂，F600灰色碳化硅粉末，90％＜22微米，平均粒度12微米)和57.9克的二硅化钼。这对无溶剂的聚合物-填充剂-混合物来说，相当于40％体积的填充剂，其中二硅化钼占总体积的15％，碳化硅占总体积的25％。电阻率Rspez为2×10欧姆厘米。实例6：
如例1所述，但有80.1克的硅氧烷被溶于150克的丙酮中。在该溶液中散有42.5克的碳化硅和27.4克的二硅化钼。这对无溶剂的聚合物-填充剂-混合物来说相当于20％体积的填充剂，其中二硅化铝占总体积的5％，碳化硅占总体积的15％。电阻率Rspez为3×108欧姆厘米。实例7：
材料制法如例1，但代替二硅化钼粉末的是要加进50％体积的石墨粉末(Aldrich 28，286-3，粒度1至2微米)。热分解后物体的密度为1.9克/立方厘米，开口孔隙度为8.9％。室温电阻率为1.6×10-2欧姆厘米。实例8：
如例1所述，但要加进四氮化三硅粉末(H.C.Starck四氮化三硅，S1，粒度d50＝0.9微米)作为填充剂。填充度为体积的50％。这样就制成了一种高电阻材料，其室温电阻率为3.6×1010欧姆厘米。该数值是用两点技术用HP 4339A型太拉欧姆计测定的。密度为2.1克/立方厘米，开口孔隙度为27.4％。用AlN和BN重复实例6。实例9：
陶瓷材料的制法如例1所述，但要加进30％体积的三氧化二铝粉末作(Alcoa XA1000，粒度d50＝0.5微米)为填充剂。这种热分解陶瓷的室温电阻率为3.5×104欧姆厘米。密度为2.8克/立方厘米，开口孔隙度为2.8％。实例10：
如例1所述，但要加进70％体积的铁粉末(Hoganas ASC 100，粒度d50＝60微米)作为填充剂。热分解后材料密度为6.1克/立方厘米，开口孔隙度为13.8％。该材料的室温电阻率为2.0×10-5欧姆厘米。实例11：
成形物体的制法如例10，但代替纯铁粉的是铁粉末与二氧化锆粉末组成的混合物。填充剂铁(Hoganas ASC 100)的含量为复合材料总体积的20％，填充剂二氧化锆(Magnesium Electron Ltd.二氧化锆SC 30 R，粒度d50＝14.5微米)的含量为复合材料总体积的20％。热分解后材料的室温电阻率为2.2×10-3欧姆厘米。用ThO2、CeO、CeO2或ZrO2与HfO2的混合物重复实施例11。实例12：
如例3所述，但使用的是室温条件下呈固体的、冷凝交联的聚硅氧烷(Chemiewerk Nunchritz NH 2400)作聚合物。在溶剂挥发后得到的不是一种塑性物质，而是一种粗颗粒粒料。这种粒料要通过磨研进行再加工。磨好的粒料用与例3不同的方法通过喷铸注入到模型内，接着按例1所述进行热分解。实例13：
按例6制作材料，但不再使用聚硅氧烷，而改用聚硅氮烷(Hoechst VT 50)作聚合物，并用50％体积的四氮化三硅粉末作填充剂。不再添加丙酮，因为聚硅氮烷已经溶在THF之中。热分解需在流动的氮气中进行。与例1-12不同之处是这里的无定形基体由Si1.0N1.3C1.6组成。热分解后材料的密度为1.8克/立方厘米，开口孔隙度为24.0％。例1-14中使用的粉末粒度有变化是为了更好地适应复合材料的用途。实例14：陶瓷白炽元件
根据例1-12中所描述的方法中的任何一法制成一U形体。成形可用热压法。
通过钎焊连接U形体的两腿触点。材料的成分可以这样选择：在向物体诸触点处加上规定电压时截面最小处应白炽化，并达到可点燃气体或混合气所需之温度。实例15：耐高温传导线路
根据例1-12中所描述的方法制成一聚合物—填充剂—混合物。待溶剂蒸发后通过刮动或丝网印刷将混合物结构化地印到还未热分解的、填充的硅有机基质上。填充的聚合物层在200℃的干燥柜内被硬化。接着涂层和基质在800-1400℃时一起被热分解。我们便在基质上得到了一种耐高温的传导线路，其电阻的大小可通过改变填充剂的成分来调整。实例16：耐高温的电路
如例13所述，但涂层的结构是由带有局部不同成分的聚合物-填充剂-混合物组成的。这样所产生的电阻也有所不同。我们得到了一种耐高温的电路。聚合物-填充剂-混合物的成分在基质平面上和在与其垂直的方向上都可以变化。在第二种情况下，电路是建立在多层技术上的。
Claims (12)
1.一种制备用作电路中的电阻或导体的陶瓷电阻(10)的方法，通过将至少一种包埋于至少一种硅有机聚合物基质(20)中的填充剂(30)陶瓷化而制备，其特征在于所用的填充剂是选自MoSi2、CrSi2、Si、SiC、石墨、Si3N4、Al2O3、Fe和混有ZrO2、ThO2、CeO或ZrO2与HfO2的混合物的Fe中的至少一种导电成分或非导电成分，填充剂在无溶剂聚合物/填充剂混合物中的比例为20-70体积％，通过填充剂种类和比例的变化改变陶瓷化材料的电阻率。
2.根据权利要求1的方法，其特征在于向导电成分中添加另外一种不导电和/或半导电的成分。
3.根据权利要求1或2的方法，其特征在于导电成分是MoSi2，它在无溶剂聚合物/填充剂混合物中的体积含量为5-50％。
4.根据权利要求3的方法，其特征在于向MoSi2中加入的另外一个成分是Si。
5.根据权利要求4的方法，其特征在于所选的MoSi2∶Si的混合比例使得在0～900℃之间的温度范围内可获得电阻率一温度的线性依赖关系。
6.根据权利要求4的方法，其特征在于填充剂混合物占总体积的40％，并且所使用的MoSi2和Si的体积比为1∶1。
7.根据权利要求3的方法，其特征在于加入MoSi2中的另外一个成分是SiC。
8.根据权利要求7的方法，其特征在于对总体积而言，MoSi2∶SiC的体积混合比是5％∶15％至15％∶25％。
9.根据权利要求1的方法，其特征在于所使用的陶瓷或金属粉末形式的填充剂的粒度为0.01至100微米。
10.根据权利要求1的方法，其特征在于所使用的有机硅聚合物为聚硅烷、聚碳硅烷、聚硅氮烷或聚硅氧烷。
11.制备用作加热元件的陶瓷电阻(10)的方法，通过陶瓷化至少一种包埋于至少一种有机硅聚合物基质(20)中的填充剂(30)而制备，其特征在于所使用的填充剂是选自MoSi2、CrSi2、Si、SiC、石墨、Si3N4、Al2O3、Fe和混有ZrO2、ThO2、CeO或ZrO2与HfO2的混合物的Fe中的至少一种导电成分或非导电成分，填充剂在无溶剂聚合物/填充剂混合物中的比例为20-70体积％，通过填充剂种类和比例的变化可改变陶瓷化材料的电阻率。
12.根据权利要求11的方法，其特征在于所述的加热元件用作陶瓷白炽元件。
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| ITTO20040161A1 (it) * | 2004-03-11 | 2004-06-11 | Sergio Ceschini | Procedimento per la realizzazione di resistori ceramici, e relativi resistori ceramici |
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| CN102244376B (zh) * | 2010-05-13 | 2014-05-07 | 宜兴市丁山电瓷避雷器材厂 | 一种碳化硅灭磁电阻及其制备方法 |
| TWI440616B (zh) * | 2012-02-07 | 2014-06-11 | Polytronics Technology Corp | 過電流保護元件 |
| RU2559802C2 (ru) * | 2013-10-02 | 2015-08-10 | Акционерное общество "Научно-исследовательский институт конструкционных материалов на основе графита "НИИграфит" | Резистивный композиционный корунд-углеродный материал |
| CN106587954B (zh) * | 2016-12-27 | 2019-09-03 | 中国西电电气股份有限公司 | 一种陶瓷碳电阻及其制备方法 |
| DE102020117987A1 (de) | 2020-07-08 | 2022-01-13 | Polymerge Gmbh | Infrarotstrahlungs-Emitter, Schweißanlage, insbesondere Kunststoffschweißanlage, mit einem solchen Infrarotstrahlungs-Emitter, sowie Schweißverfahren mit einem solchen Infrarotstrahlungs-Emitter |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3027332A (en) * | 1953-06-10 | 1962-03-27 | Kanthal Ab | Heat resisting materials and methods for their manufacture |
| NL7511173A (nl) * | 1975-09-23 | 1977-03-25 | Philips Nv | Zelfregelend verwarmingselement. |
| US4545914A (en) * | 1984-08-31 | 1985-10-08 | Dow Corning Corporation | Conductive elastomers from electrically conductive fibers in silicone emulsion |
| US4666628A (en) * | 1984-12-20 | 1987-05-19 | Mitsubishi Denki Kabushiki Kaisha | Moisture sensitive material and process for its production |
| US4634756A (en) * | 1985-11-25 | 1987-01-06 | Xerox Corporation | Electrical resistor |
| DE3855544T2 (de) * | 1987-04-10 | 1997-03-27 | Hitachi Ltd | Keramische Verbundwerkstoff und Verfahren zur Herstellung desselben |
| JPH01287169A (ja) * | 1988-04-01 | 1989-11-17 | Toshiba Silicone Co Ltd | 導電性シリコーンゴム組成物 |
| JP2808296B2 (ja) * | 1989-02-28 | 1998-10-08 | 東芝シリコーン株式会社 | プライマー組成物 |
| JPH02261835A (ja) * | 1989-03-31 | 1990-10-24 | Shin Etsu Chem Co Ltd | 発泡性シリコーンゴム組成物 |
| DE3926077A1 (de) * | 1989-08-07 | 1991-02-14 | Peter Prof Dr Greil | Keramische verbundkoerper und verfahren zu ihrer herstellung |
| US5332701A (en) * | 1990-12-14 | 1994-07-26 | Massachusetts Institute Of Technology | Ceramic synthesis by pyrolysis of metal-containing polymer and metal |
| JPH0539442A (ja) * | 1991-08-02 | 1993-02-19 | Genji Naemura | 導電性発熱流動体 |
| US5482656A (en) * | 1993-03-04 | 1996-01-09 | Kabushiki Kaisha Toshiba | Non-linear optical devices employing a polysilane composition and a polysilane composition therefor |
| JP2713093B2 (ja) * | 1993-04-13 | 1998-02-16 | 信越化学工業株式会社 | 導電性シリコーンゴム組成物 |
| US5549851A (en) * | 1994-01-25 | 1996-08-27 | Shin-Etsu Chemical Co., Ltd. | Conductive polymer composition |
-
1995
- 1995-10-19 DE DE59505670T patent/DE59505670D1/de not_active Expired - Lifetime
- 1995-10-19 EP EP95934616A patent/EP0787349B1/de not_active Expired - Lifetime
- 1995-10-19 CN CN95195763A patent/CN1126122C/zh not_active Expired - Fee Related
- 1995-10-19 JP JP51350596A patent/JP3927599B2/ja not_active Expired - Fee Related
- 1995-10-19 WO PCT/DE1995/001452 patent/WO1996013044A1/de active IP Right Grant
- 1995-10-19 ES ES95934616T patent/ES2131335T3/es not_active Expired - Lifetime
-
1998
- 1998-08-10 US US09/131,866 patent/US5961888A/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP3927599B2 (ja) | 2007-06-13 |
| EP0787349B1 (de) | 1999-04-14 |
| EP0787349A1 (de) | 1997-08-06 |
| ES2131335T3 (es) | 1999-07-16 |
| CN1161756A (zh) | 1997-10-08 |
| US5961888A (en) | 1999-10-05 |
| JPH10507591A (ja) | 1998-07-21 |
| DE59505670D1 (de) | 1999-05-20 |
| WO1996013044A1 (de) | 1996-05-02 |
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