CN1243464A - 除去粘合剂的方法 - Google Patents

除去粘合剂的方法 Download PDF

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CN1243464A
CN1243464A CN98801795A CN98801795A CN1243464A CN 1243464 A CN1243464 A CN 1243464A CN 98801795 A CN98801795 A CN 98801795A CN 98801795 A CN98801795 A CN 98801795A CN 1243464 A CN1243464 A CN 1243464A
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CN1106898C (zh
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I·H·毕晓普
D·马什德
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Kyocera Avx Components Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052—Sintered electrodes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • B22F3/1025—Removal of binder or filler not by heating only

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  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Powder Metallurgy (AREA)
  • Lubricants (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract

本发明涉及一种从颗粒物质(如钽粉)压制成的多孔性制品中除去水不溶性粘合剂的方法。本发明提供了一种能从用于高纯度用途(如生产电容器)的压制品中除去基本上所有粘合剂的方法。该方法包括使压制品与能和所述粘合剂反应的试剂的水溶液接触,产生该粘合剂的水溶性衍生物,从而使所述粘合剂衍生物基本上溶解在所述溶液中。在一个特定的实例中,该衍生物由脂肪酸粘合剂水解产生。

Description

除去粘合剂的方法
本发明涉及通过压制由粘合剂/润滑剂粘合的颗粒物质制成制品的领域，具体地说是涉及一种生产高纯度烧结制品的部件时，在压制后烧结前除去粘合剂的方法。
在生产钽电容器时，阳极通常是这样制成的：使钽粉和少量粘合剂/润滑剂混合，将混合物压实并模塑成型成所需形状，然后真空加热使粘合剂升华、蒸馏或分解来除去粘合剂。在除去粘合剂后，对阳极进行烧结，使粉末熔结成整体制品。
在电子或其它高纯度用途中，粘合剂/润滑剂材料(后称“粘合剂”)的选择受到以下要求的限制：在真空加热过程后只能残留很少或不残留含碳残余物，且在除去粘合剂的过程中不能在阳极内加入氧。这些残余物的存在会使沉积在烧结钽产品上的阳极氧化膜劣化而改变电容器的电性能。目前采用的粘合剂包括樟脑、某些蜡和某些聚合物。
即使是使用这些粘合剂，阳极中也会不可避免地引入少量碳，因为难以完全除去粘合剂或其分解产物和残余物。而且，由于除去粘合剂时进行加热，而粘合剂本身中存在氧，所以阳极中还存在少量氧。
美国专利No.5,470,525的说明书公开了一种除去钽粉压制件中粘合剂的方法，该方法是将其浸在温热的洗涤剂水溶液中，然后用清水洗涤。然而，在前述说明书公开的方法中，浸的过程需要很长时间，通常要数小时。
本发明的一个目的是提供一种用于高纯度用途的除粘合剂方法，该方法比现有方法有所改进。
本发明提供了一种从多孔性制品中除去水不溶性粘合剂的方法，该制品由压制的颗粒物质压制而成，该方法包括使制品与能和所述粘合剂反应的试剂的水溶液接触，以产生该粘合剂的水溶性衍生物，从而使所述粘合剂衍生物基本上溶解在所述溶液中。
因此，本发明通过化学反应和可溶的反应产物的溶解作用来除去粘合剂。通过这种方式，无需现有技术中复杂的蒸馏或高温加热方法就能除去粘合剂，且除去的速度比已知的热浸方法快很多。
将制品浸在含有所述试剂的液体中就可实现上述的接触。通过这种方式，液体穿过制品中的通孔进入制品并与粘合剂接触。
本发明的一个方面是将制品浸在试剂的水溶液中来实现接触。
可对水溶液加热以有助于从制品中除去粘合剂。溶液温度宜高于粘合剂的熔点，从而使得粘合剂在制品浸在溶液中时液化。
粘合剂材料可能是高级脂肪酸。在这种情况下，改进方法可包括在碱性溶液中使其酸水解。这样就形成了脂肪酸的盐，该盐溶解在溶液中，从而实现了粘合剂的除去。
一种较佳的脂肪酸是硬脂酸。脂肪酸是廉价的、易获得的且非常有效的粘合剂/润滑剂。然而，由于在压制后很难完全除去粘合剂，它们的高碳含量使得残余物对某些高纯度用途特别有害，所以到目前为止它们在高纯度用途中的应用还受到限制。
在本发明的另一方面，粘合剂可能包含水不溶性粘合剂材料和水溶性粘合剂材料。这种水溶性材料可能是长链醇如聚乙二醇。一种较佳的组合是诸如硬脂酸的脂肪酸与聚乙二醇。在一些实例中，在高达5％重量的乙二醇中加入5％重量的脂肪酸。
聚乙二醇是一种很好的粘合剂，而脂肪酸则是一种很好的润滑剂。两种组分组合在一起形成了一种在由粉末压制成型时可提供良好加工性能的混合物。
水溶液可含有氢氧根离子，该离子通过加入可在水中电离的氢氧化物来导入。典型的例子是氢氧化钠、氢氧化钾、氢氧化铝等。
氢氧化物应加入充分比例以确保与粘合剂进行化学计量反应，同时应保持低的水溶液粘度，以便溶液有效地渗透入制品内。
在除去粘合剂的过程中，可以对液体进行搅拌或搅动。另外，制品本身在浸没时可以搅动，从而促进液体渗透入制品内。合适的搅拌装置是本领域技术人员所知的。
一旦该处理过程结束，就可通过在清水中洗涤制品来除去残留在制品中的所有粘合剂衍生物。清洗过程可以重复，以确保完全除去改性的粘合剂。当采用金属氢氧化物溶液时，洗涤过程的进展和效果可通过测定每次洗液的电导率来监控；溶液中残留的金属离子会提供相当高的电导率读数。
在洗涤后，可干燥制品，然后烧结成固结的产品。
制品可以是金属，例如铌、铝、钽和其它可作为阳极的金属。在一个实例中，制品包含钽粉。制品可以成型成电容器的阳极。这种制品的大小范围包括从约0.6毫米的立方体到直径为6毫米、长7毫米的圆柱体。
本发明在生产钽电容器中具有特别的用途(在该生产中是将钽粉烧结制成钽粉阳极然后插入电容器中)。在这些产品中，必须除去所有的粘合剂或粘合剂残余物，特别是限制在阳极表面形成含碳沉积物，以确保制成的电容器能正确可靠地运行。
下面通过一个实施例来描述实施本发明的方法。
使钽粉与少量(5％重量)硬脂酸(CH3-[CH2]16-COOH)粘合剂/润滑剂混合。然后将混合物压制成有一定形状的压制品，在本实施例中是固态电容器的阳极元件。
然后将制品浸在0.5％氢氧化钠水溶液中，将该溶液加热至80℃约30分钟以进行反应。在此期间，搅动制品确保溶液完全渗透入制品内，并且还确保未反应的溶液连续不断地进入制品，而反应产物则溶解到整体溶液中。
反应/溶解过程一旦结束，就从溶液中取出制品并在清水中洗涤，以除去残留在制品通孔中的所有硬脂酸盐。洗涤步骤可以重复，以确保洗涤完全。在每一步清洗后，用常规方法对清洗溶液取样，测定电导率用以表示钠离子的浓度。随着钠离子被洗去，洗液的电导率降低直至获得所需的清洁程度。
在本发明的另一个实例中，粘合剂包含硬脂酸与平均分子量为2000的聚乙二醇的混合物。硬脂酸和乙二醇的重量百分数分别为4％和0.5％(钽重量的百分数)。其余的过程变量基本上相同。
本发明方法所用化学物质的危害性相当低、价格低廉且容易弃置，对环境的影响很小。
本发明方法生产的钽阳极的碳含量很低，因为实际上含碳物质被完全除去。另外，由于本发明的除去粘合剂过程可能仅采用低温，因此在除去粘合剂过程中引入的氧量可以忽略。由于这个原因，最终成品的电性能得到显著改善。尤其是电容器的可靠性有所提高，减少了使用时的漏电现象。

Claims (9)

1.一种除去由颗粒物质压制成的多孔性制品中水不溶性粘合剂的方法，该方法包括使制品与能和所述粘合剂反应的试剂的水溶液接触，以产生该粘合剂的水溶性衍生物，从而使所述粘合剂衍生物基本上溶解在所述溶液中。
2.根据权利要求1所述的方法，其中衍生物通过水解来产生。
3.根据前述任一权利要求所述的方法，其中粘合剂包含酸性材料，溶液包含氢氧根离子。
4.根据前述任一权利要求所述的方法，其中粘合剂由脂肪酸组成。
5.根据前述任一权利要求所述的方法，其中粘合剂还进一步包含水溶性材料。
6.根据权利要求5所述的方法，其中亲水性材料是聚乙二醇。
7.根据前述任一权利要求所述的方法，其中颗粒物质由钽粉组成。
8.根据前述任一权利要求所述的方法，其中制品被成型为电容器的电极。
9.一种除去由颗粒物质的压制成多孔性制品中水不溶性粘合剂的方法，该方法基本上如前文所述。
CN98801795A 1997-01-13 1998-01-06 一种形成用于生产固态电容器的阳极体的方法 Expired - Fee Related CN1106898C (zh)

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GBGB9700566.4A GB9700566D0 (en) 1997-01-13 1997-01-13 Binder removal
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JP (1) JP4230541B2 (zh)
KR (1) KR100494140B1 (zh)
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AT (1) ATE223274T1 (zh)
AU (1) AU5490498A (zh)
DE (1) DE69807650T2 (zh)
GB (1) GB9700566D0 (zh)
IL (1) IL130892A (zh)
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WO (1) WO1998030348A1 (zh)

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