CN1235567A - 涂层粉末形成的固结材料及其生产方法 - Google Patents
涂层粉末形成的固结材料及其生产方法 Download PDFInfo
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- CN1235567A CN1235567A CN97199239A CN97199239A CN1235567A CN 1235567 A CN1235567 A CN 1235567A CN 97199239 A CN97199239 A CN 97199239A CN 97199239 A CN97199239 A CN 97199239A CN 1235567 A CN1235567 A CN 1235567A
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Classifications
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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
- B22F3/02—Compacting only
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/18—Non-metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明涉及由几种涂层粉末形成的固结材料,在通过互相结合具有一定性能的粉末颗粒,形成一种模制品时,可以使粉末颗粒具有要求的排列方向,或可以以这样的预定的距离排列,以使固结材料达到所要求的性能。在粉末颗粒上有厚度0.01—20微米均匀涂膜,或者粘附各含有基体颗粒的粉末,在粉末颗粒上有多层涂膜,每层厚度均匀,为0.01—5微米,其中至少任何相邻的涂膜是不同类的,该粉末颗粒在涂膜处或通过粘合剂固结在一起,固结材料的特性归因于在其上有涂膜的粉末颗粒的特性,本发明也公开了一种由涂层粉末颗粒形成固结材料的方法。
Description
技术领域
本发明涉及涂层粉末的固结材料，该材料或者由固结其表面上有均匀厚度为0.01-20微米涂层薄膜的基体颗粒的粉末得到，或者由固结有两种或多种相似涂层薄膜的粉末得到，本发明还涉及生产粘结块的方法。换句话说，本发明涉及尤其是非线性材料的产品，例如像磁头和磁记录材料的磁性材料、电子零件、玻璃/陶瓷材料等，和这些材料的生产方法。
背景技术
人们已知一项技术，该技术包括用其他物质涂覆粉末表面，以改进该粉末的特性或赋予该粉末各种特性。为此，人们通常提出了各种方法。
在粉末中，常用金属粉末等，因为它们有各种应用。关于在金属粉末或金属氧化物粉末表面上形成一层金属涂层薄膜的方法，例如JP-A-3-271376提出了一种方法，在该方法中，通过用湿法使水溶性钴盐还原，在如钴金属、镍金属或铁金属之类的金属粉末表面上，或者在如铁氧体或氧化铬之类的金属氧化物粉末表面上生成钴金属涂层薄膜。但是，在工业上用厚而均匀的不同种类金属氧化物薄膜涂布金属或金属氧化物粉末表面，这通常是不可能的。
本发明人过去发明了一种通过将金属粉末或金属氧化物粉末分散在金属醇盐溶液中，使金属醇盐水解，而形成金属氧化物薄膜的方法，并申请了专利(JP-A-6-228604)。
本发明人通过在金属粉末表面或金属氧化物粉末表面交替地形成金属薄膜和金属氧化物薄膜，还研制出高功能性的粉末，并申请了专利(JP-A-7-90310)。例如，本发明人通过在如铁氧体或氧化铬之类的磁性材料粉末表面上形成一层金属氧化物的涂膜，并在涂膜上形成钴金属或银金属涂膜，在制备足够白的磁性粉末方面获得成功，还通过在具有令人满意的热导率的基体金属，例如银金属或铜金属的颗粒上形成金属氧化物薄膜，在制备具有令人满意的热导率的绝缘粉末方面也获得成功。此外，本发明人申请了一种方法的专利，该方法类似地包括在金属或金属化合物基体颗粒上形成多层金属氧化物薄膜，对包有多层金属氧化物薄膜的颗粒进行热处理，以得到具有更密实和更稳定的多层金属氧化物薄膜的粉末(JP-A-7-80832)。
如上所述，本发明人通过在金属粉末或金属化合物粉末(基体颗粒)表面形成一种或多种金属或金属氧化物薄膜，以赋予它一种特性，该特性不是起核心作用的金属或金属化合物基体颗粒所具有的特性，努力研制一种高功能的金属或金属化合物粉末。
但是，人们想以低成本得到一种比较高功能的金属或金属化合物粉末，并提供一种技术，该技术可用于由除金属或金属化合物之外的材料，例如有机材料制成的各种各样的粉末，并且该技术能够在有机基体颗粒等表面上形成两种或多种金属或金属氧化物薄膜。
另一方面，通过包括粉末固结和模压的方法，或通过包括重叠薄片并固结和模压薄片的方法，由粉末或薄片等生产出许多产品，特别是非线性材料，例如磁头、磁记录材料等之类的磁性物质的产品、如边界层电容器等之类电子零件的产品，和如高韧性玻璃材料、偏转滤光器等之类的玻璃/陶瓷材料的产品。
生产这些产品的这样一些方法包括一种技术，在该技术中，向原料粉末加入一种杂质，并进行固结热处理，在原料粉末与固结材料(介质等)之间的边界分离出加入的杂质，以赋予被固结的材料非线性特性，或把分离的物质用作使粉末颗粒互相固结的介质。该技术的一个实例是采用一种技术生产的变阻器边界电容器，在该技术中，使如钛酸钡之类的铁电体材料粉末固结并将其插在由金属导体制成的电极之间，其操作期间，绝缘杂质与铁电体粉末分开，以改进绝缘性。
在玻璃材料和光学材料中，例如在MgO-Al2O3-SiO2玻璃方面有一种技术，该技术是在熔化玻璃注模之前将TiO2加入和分散到熔化玻璃中，使用TiO2作为晶核使熔融物进行结晶，得到高韧性玻璃材料。另一种技术包括将银分散在光学玻璃中，使银呈胶态，并用胶体银作为晶核使玻璃结晶，从而得到非线性光学材料。
采用重叠、固结和模压薄片的方法生产产品的实例包括录音和复制用磁头，这种磁头是采用将坡莫合金薄片重叠，再用粘合剂固结这些薄片生产的。至于其他磁性材料，将多晶铁氧体与绝缘体固结在一起所得到的材料用作录音磁带和计算机磁带的数字头，而铁硅铝磁合金用于具有高矫顽力的磁带。
用上述磁性材料等生产磁头和磁心时，固结具有预定颗粒直径的磁性材料，以得到最大能量产品，从而改进磁性。但是，进行固结而不改变颗粒直径是困难的，磁性材料由于其中晶体生长而不可避免地增加颗粒的直径。
此外，在上述高韧性玻璃材料的生产中，例如，使加入的添加剂均匀地分散到具有高粘度的熔融玻璃中几乎是不可能的。
如上所述，生产具有高价值的特色产品，例如具有非线性特性的产品，需要高水平的技术，例如一种技术是，让作为核心的薄片或针形基体颗粒以等距排列，以便按一定的方向取向，并固结这些薄片或颗粒，同时保持这种状态，一种技术是通过颗粒之间的薄膜使排列的颗粒结合起来，以及一种技术是将颗粒与高粘度液体均匀混合，以得到均匀的分散体。仅用传统的已知技术常常难以生产出这些产品。
本发明的一个目的是消除这些问题，并提供能以低成本稳定地生产具有高价值的特色产品的技术。
具体地，例如，其目的是提供一种技术，其中例如为了改进磁头的磁性，均匀固结具有能得到最大能量产品的这样一种颗粒直径的磁性颗粒，而不会造成晶体生长，提供一项技术，其中通过采用导体作为核心颗粒(称作基体颗粒)，在这些颗粒上形成厚度均匀的铁电体材料层，并在其上形成导体层，从而生产出质量水平更稳定的高容量电容器，这些电容器在构造上与BL电容器相似。
发明内容
本发明人曾注意，采用上述有关具有一层或多层涂膜粉末的技术可能会解决上述问题，并进行了研究，结果得到了本发明。
换句话说，本发明通过以下方法成功地解决了上述问题。
(1)一种由几种涂层粉末形成的固结材料，每种基体颗粒上都有0.01-20微米厚度均匀的涂膜，其中涂层粉末在其涂膜处或通过粘合剂而互相粘附。
(2)根据上述(1)的由涂层粉末形成的固结材料，其中涂层粉末各含有基体颗粒，在每种基体颗粒上有0.01-20微米厚度均匀的涂膜，基体颗粒包括玻璃、金属或金属氧化物，涂膜是金属膜或金属氧化物膜。
(3)一种由几种涂层粉末形成的粘合在一起的涂层粉末，每种涂层粉末均有一种基体颗粒，该基体颗粒上有多层厚度均匀的涂膜，每层膜的厚度为0.01-5微米，在涂膜中至少任何相邻的涂膜是不同种类的，其中涂层粉末在最外面的涂膜处或通过粘合剂而互相粘附。
(4)根据上述(3)的由涂层粉末形成的固结材料，其中涂层粉末各含有一种基体颗粒，在基体颗粒上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻的涂膜是不同类的，其中基体颗粒包括玻璃、金属或金属氧化物，涂膜是各金属薄膜或金属氧化物薄膜。
(5)根据上述(1)-(4)中之一的由涂层粉末形成的固结材料，其中基体颗粒包括磁性材料。
(6)根据上述(5)的由涂层粉末的固结材料，其中至少一层涂膜含有介电材料。
(7)一种由互相固结的几种涂层粉末形成固结材料的生产方法，该方法包括在涂膜处粘附各含有一种基体颗粒的粉末，该颗粒上有一层厚度0.01-20微米的均匀涂膜，或者粘附各含有一种基体颗粒的粉末，该颗粒上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻涂膜是不同类的。
(8)一种由互相固结的几种涂层粉末形成固结材料的生产方法，该方法包括通过粘合剂粘附各含有一种基体颗粒的粉末，该颗粒上有一层厚度0.01-20微米的均匀涂膜，或者粘附各含有一种基体颗粒的粉末，该粉末上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻涂膜是不同类的。
用于本发明的由几种涂层粉末形成固结材料的粉末核心的基体颗粒在其材料、颗粒直径和颗粒形状方面并不受到特别限制。其材料可以是任何有机物和无机物材料，其颗粒直径也没有受到特别限制，只要它的平均颗粒直径不大于6毫米。此外，其形状可以是球状或椭圆状，或可以是如用星状表示的那些形状。在某些情况中，基体颗粒可以是多孔颗粒。
在本发明中优选使用的基体颗粒如下。其材料优选地是有机聚合物、硅氧烷树脂、玻璃、金属或金属氧化物，特别优选地是玻璃、金属或金属氧化物。其颗粒直径是平均颗粒直径为100微米或100微米以下。此外，其形状近似球形或椭圆形，其表面优选地是光滑的，因为均匀涂膜容易得到。
在本发明中，可用各种技术涂布由例如有机聚合物、硅氧烷树脂、玻璃、金属或金属氧化物制成的基体颗粒的表面。例如，一种优选的技术包括将基体颗粒分散到无水醇中，在充分搅拌的同时向其加入金属醇盐，其金属醇盐相应于在颗粒表面形成涂膜的该金属氧化物，向上述均匀混合物中逐渐加入醇/水混合物，使醇盐水解，在被处理的基体颗粒表面上形成一层金属氧化物溶胶，并将溶胶转化成凝胶。在单层涂膜的情况下，通过干燥沉积在被处理的基体颗粒表面上的醇盐凝胶，得到涂层粉末。优选地，这种技术使用的干燥方法是真空干燥。
在生产有多层涂膜的涂层粉末时，将用金属醇盐得到的凝胶涂敷的粉末分散在无水醇中，重复上述操作程序，其中，在充分搅拌的同时，加入用于进行表面处理的金属醇盐，向均匀混合物中逐渐加入醇/水混合物，以水解醇盐，并在用要求量的金属氧化物凝胶层如此包裹基体颗粒之后，干燥粉末，从而得到所要求的涂层粉末。
如铁金属粉末、镍金属粉末、铝金属粉末、聚苯乙烯珠、聚甲基丙烯酸酯珠、淀粉珠、乙酰基纤维素珠之类的粉末等，在强酸水溶液中经受表面变性作用，即使其浓度较低时也如此，例如通过引起反玻璃化作用，这种表面变性作用可以影响最终产品的性质。因此，在使用这样一种物质作为粉末核心的情况下，使用如硫酸钛、氯化钛、硫酸铝等之类的金属盐，作为在粉末表面形成涂膜的原料是不合要求的。
但是，即使当使用表面易于受到化学侵蚀的基体颗粒作为核心时，在基体颗粒表面预先形成耐化学作用的涂膜，就能够使用如硫酸钛、氯化钛、硫酸铝等之类的腐蚀性金属盐用作涂覆核心物质表面的原料。因而，能够扩宽表面涂覆方法的范围。
在JP-A-6-228604和JP-A-7-90310中描述了一种在本发明的核心物质表面沉积金属氧化物膜的可使用方法。在基体颗粒上沉积金属氢氧化物膜或金属氧化物膜时使用这种方法的情况下，可在基体颗粒表面上形成涂膜，而不用担心颗粒表面变性。这种称为溶胶-凝胶法的方法能够生成组成精细均匀的氧化物。将这种方法应用于粉末，可得到一层均匀厚实的薄膜。选择一种金属醇盐，它是一种与所要求的金属氧化物相对应的金属醇盐，如锌、铝、镉、钛、锆、钽、硅等。
另一种在本发明核心物质(基体颗粒)表面金属氧化物膜的方法是，在基体颗粒表面涂覆金属氢氧化物或金属氧化物膜。例如，这种方法使用一种金属盐，例如硫酸钛、硫酸铝等作为原料，该方法还包括把核心物质浸在金属盐水溶液中，用苛性碱、氨、尿素等水溶液中和该系统，以便使生成的金属氢氧化物或金属氧化物沉积在基体颗粒上。在使用这种方法时应该注意，因为取决于中和方法和加热方法，会有基体颗粒表面变性的情况出现。
但是，由于上述方法能够使用金属盐用作涂布颗粒表面的原料，因此上述方法是一种沉积金属氢氧化物膜或金属氧化物膜的简单方法，并且相当便宜。因而，可广泛选择生产方法。
金属盐的实例包括金属酸性盐。
可用作本发明金属盐的金属实例包括铁、镍、铬、钛、锌、铝、镉、锆和硅，还包括钙、镁和钡。这些金属盐的实例包括硫酸盐、硝酸盐、盐酸盐、草酸盐、碳酸盐和羧酸盐。上述金属的螯合物也包括在内。根据要赋予粉末表面的性质和要使用的生产方法选择本发明使用的合适种类的金属盐。
除了以上方法，还可用许多传统的方法在粉末表面形成涂膜，如涂层法、沉积法、溅射、真空镀膜、电沉积、阳极化等。可用于固结在其上已采用根据本发明的上述方法形成了涂膜的粉末的方法包括，在粉末表面涂一种粘合剂，模压其粉末，并使模压物经过压制和热处理。
将带有涂膜的粉末模压成产品所使用的粘合剂实例包括基于乙烯基聚合物、橡胶、缩合树脂等的有机聚合物粘合剂，和基于玻璃、陶瓷等的无机聚合物粘合剂。有机聚合物不仅能以在水中或在有机溶剂中的溶液型有机聚合物粘合剂使用，而且还能以如环氧粘合剂和苯酚甲醛粘合剂之类的缩合型有机聚合物粘合剂使用。如玻璃或陶瓷基料无机聚合物粘合剂之类的无机聚合物粘合剂能以粉料使用，其使用方式是将粘合剂粉末与本发明粉末均匀混合，并采用如热等静压工艺(HIP)之类的热处理方法模压粉末混合物，以得到煅烧材料。
在本发明中，除了由无机物构成的颗粒之外，用作本发明多层涂层粉末核心的基体颗粒还可以是由有机物构成的颗粒。组成本发明基体颗粒的无机物实例包括金属，如铁、镍、铬、钛、铝等；金属合金，例如铁-镍、铁-钴合金等；铁-镍合金氮化物；铁-镍-钴合金氮化物；金属氧化物，如铁、镍、铬、钛、铝、硅、钙、镁、钡等的氧化物，和这些金属的复合氧化物；粘土；和玻璃。
可用作构成基体颗粒的特别优选物质是磁性金属如铁、镍等，或磁性金属合金，如铁-镍合金、铁-钴合金等，或者是磁性金属氧化物，如氧化铁、氧化铬等。
当具有各种电性质的物质，如铁酸钡、Mn-Zn铁酸盐、Ni-Zn铁酸盐、Cu-Zn铁酸盐、坡莫合金、铁硅铝磁合金、波明德、高导磁铁铝合金、磁性Sm-Co-Fe合金及其氮化物，磁性Nd-B合金等作为那种物质使用时，那么由它们可得到具有基于这些物质的性质的粘合块。
当玻璃或陶瓷用作那种物质时，那么可得到能有效利用这些物质粉末的粘合块。
在本发明中，根据本发明的基体颗粒可以由有机物组成。构成本发明有机基体颗粒的有机物实例包括天然和合成的聚合物。合成的聚合物实例包括聚苯乙烯、聚乙烯、聚丙烯、聚丙烯酸酯、聚甲基丙烯酸酯，和组成这些聚合物的任何一种单体与其他一种或多种单体的共聚物。天然聚合物实例包括淀粉、琼脂糖、纤维素和明胶。除了这些物质，还可使用的物质是半合成聚合物，如乙酰基纤维素、羟乙基纤维素等。尽管由这种有机聚合物构成的基体颗粒可呈不规则形状，但优选地是由悬浮聚合方法或晶种聚合法或由溶液分散法等形成的球形颗粒。
根据本发明，采用任何上述方法，都可将金属氢氧化物薄膜、金属氧化物薄膜、铁电体薄膜、粘性薄膜等以给定的厚度，沉积在基体颗粒表面，通过这种方法将一定的性质赋予该颗粒，并且得到具有单层涂膜或者复合涂膜的粉末。通过粉末颗粒上的涂膜本身使粉末颗粒彼此结合在一起，从而使该粉末模压成粘合在一起的模制件。要不然，以相同的距离以一定的方向排列具有单层涂膜或具有复合涂膜的粉末颗粒，使用如树脂等之类的任何一种上述粘合剂，以下述的任何一种操作方法处理这些粉末颗粒，同时保持这一状态，以得到固结的模制件。通过压力下的热处理，如HIP等，将该粉末模压成煅烧材料也是可能的。因而，可赋予具有涂膜的粉末一种新的效能。
具体地，因为固结的模制件能够由两种或多种组分构成，其中涂膜具有特性并能进行调整以具有不变的质量水平，又因为具有涂膜的粉末颗粒能以一定的距离以一定的方向排列并联结成固结的模制件，同时保持该状态，因此本发明产生了出色的效果。
下面将举出本发明的具体实施方案，以进一步解释本发明。
(1)一个实施例，其中通过调整涂膜的厚度和以相同的距离排列颗粒来得到具有高价值的产品。
具有颗粒直径0.3微米的Mn-Zn铁氧体用作起核心作用的基体颗粒。在基体颗粒的表面上形成厚度为0.01微米的二氧化硅层涂膜。这种具有起绝缘膜作用的二氧化硅涂膜的Mn-Zn铁氧体，例如装进模子中，使颗粒以一定的方向排列。在模子中的粉末用环氧粘合剂固结，同时保持这一状态，通过这一方法可以生产出在高频率时具有极低涡流损耗的录音/复制用磁头。
(2)在导体的基体颗粒与涂膜之间插入具有严格相等厚度的铁电体薄膜，形成本发明的复合颗粒。用绝缘涂层材料模压和固结该复合颗粒，同时使单个颗粒的最外面的导电涂膜保持互相电联结状态，因此这些颗粒可以具有相同的电势。因而，可以生产出高容量电容器(BL电容器)。
(3)在由如硫化镉(CdS)等之类的半导体或由金、银等之类的导体制成的基体颗粒的表面涂上硼硅酸盐玻璃，形成涂膜。通过煅烧使该涂层粉末固结，通过这样一种方法生产具有光学各向异性的玻璃。
(4)即使当由有机聚合物制成的薄膜在颗粒上作为涂膜沉积时，能够采用根据本发明的技术生产出具有高价值的固结模制品。
实施本发明的最佳方式
将以实施例的方式描述通过上述微粒电容器和其他电容器的固结/模压，生产高容量电容器的方法，以能够更清楚地理解本发明。但是，不应该说明本发明将受到以下实施例的限制。
实施例1(BL电容器)
100克平均颗粒直径5微米的钛酸钡颗粒分散到预先将2000克乙醇与80克乙醇锌混合而成的溶液中。之后，在1小时内滴加预先制备的400克乙醇和80克去离子水到分散体中，使氧化锌沉积，从而形成氧化锌涂膜。得到的氧化锌薄膜厚度为0.2微米。从液体中分离出颗粒上有氧化锌涂膜的钛酸钡粉末，并干燥。
采用HIP方法，在空气中在1200℃煅烧该粉末3小时，得到已煅烧的物质。
测量该煅烧物质的电容。结果，E1KHz是11000。
对比实施例1(BL电容器)
不经过任何预处理的100克如实施例1中使用的相同钛酸钡颗粒(平均颗粒直径5微米)采用HIP方法在空气中在1200℃煅烧3小时，得到煅烧物质。
测量该煅烧物质的电容。结果，E1KHz是1800。
与对比实施例1相比，在煅烧钛酸钡颗粒时，在实施例1的颗粒上预先形成的具有高电阻的氧化物薄膜使颗粒边界彼此隔开，从而可以提高相对介电常数。
实施例2(高介电常数电容器)
第一层，钛酸钡层：
往由2000克乙醇与86克异丙醇钡和70克乙醇钛预先混合制备的溶液中加入100克平均颗粒直径为5微米的银金属颗粒。在该溶液保持在55℃时，在1小时内往该溶液滴加由140克去离子水与400克乙醇混合而成的溶液。加入之后，得到的混合物反应6小时。
反应后，这些颗粒在650℃氮气氛中加热3小时，得到涂有钛酸钡的银粉末B1。
第二层：银层：
将100克上述方法制备得到的涂有钛酸钡银粉末B1分散到1200毫升预先制备的银溶液中。在搅拌的同时，往该溶液中加入1200毫升预先制备的还原性溶液。通过还原1小时使银金属沉积，得到涂有银、涂有钛酸钡的银粉末B2。
上面使用的银溶液是一种采用如下方法制备的液体：将3.5克硝酸银溶解在60克去离子水中，往该溶液加入4克氨水(29％)，向其加入由氢氧化钠溶解于60克水所制备的水溶液，接着再加入5克氨水(29％)，然后充分搅拌所得到的混合物。
还原性溶液是一种采用如下方法制备的溶液：将葡萄糖和酒石酸溶解于1升水中，煮沸得到的溶液，冷却该溶液，然后加入79.3克乙醇。
第三层，钛酸钡层：
往由2000克乙醇与86克异丙醇钡和70克乙醇钛预先混合制备的溶液中加入100克上述制备的涂有银、涂有钛酸钡的银粉末B2。将该溶液保持在55℃，在1小时内往该溶液滴加由140克去离子水与400克乙醇混合制成的溶液。加入之后，得到的混合物反应6小时。
反应后，这些颗粒在650℃氮气氛中加热3小时，得到涂有钛酸钡的、涂有银的银粉末B3。
第四层，银层：
将100克上述方法制备得到的涂有银的、涂有钛酸钡的银粉末B3分散到1200毫升预先制备的银溶液中。在搅拌的同时，往该溶液加入1200毫升预先制备的还原性溶液。通过还原1小时沉积银金属，得到涂有银的、涂有钛酸钡的银粉末B4。
第五层，钛酸钡层：
往由2000克乙醇与86克异丙醇钡和70克乙醇钛预先混合制成的溶液中加入100克上述方法制备得到的涂有银、涂有钛酸钡的银粉末B4。将该溶液保持在55℃，在1小时内往该溶液滴加由140克去离子水与400克乙醇混合制成的溶液。加入之后，得到的混合物反应6小时。
反应后，这些颗粒在650℃氮气氛中加热3小时，得到涂有钛酸钡的、涂有银的银粉末B5。
性能试验：
测试在涂膜形成的各阶段的粉末性能，以确定其性能差异。
涂有钛酸钡的银粉末B1、涂有银的、涂有钛酸钡的银粉末B3和涂有银的、涂有钛酸钡的银粉末B5，这些粉末中的每一种粉末都采用HIP方法在1200℃空气中煅烧3小时，得到煅烧物质。
得到的煅烧物质的电容E1KHz列于表1中。
如表1所示，当导体银用作基体颗粒，钛酸钡用作电介质时，那么随银薄膜数量增加电容也增加。
表1
在涂膜粉末的煅烧物质中薄膜数与相对介电常数之间的关系
| 涂膜种类 | 涂膜的层组成 | 电容E1KHz |
| B1 | 有一层钛酸钡膜的银粉末 | 1,100 |
| B3 | 有两层钛酸钡膜和一层银膜的银粉末 | 5,600 |
| B5 | 有三层钛酸钡膜和两层银膜的银粉末 | 17,100 |
实施例3(高韧性材料)
将100克钛金属基体颗粒(平均颗粒直径3微米)分散到异丙醇中。往该溶液加入50克异丙醇铝，接着加入由20克氨水与30克水混合而成的溶液。得到的混合物反应5小时。反应之后，用足量的乙醇洗涤这些颗粒。在固液分离后，所回收的颗粒在90℃真空干燥器中干燥8小时，得到涂有氧化铝的钛粉末3A。
再用具有相同组成的溶液涂布所得到的涂有氧化铝的钛粉末3A，然后干燥。这种干燥的粉末在650℃氮气氛下在旋转管式炉中加热2小时，得到涂有氧化铝的钛粉末3B。所得到粉末的平均颗粒直径为5微米。
将100克氧化锆基体颗粒(平均颗粒直径3微米)分散到异丙醇中。往该溶液加入50克异丙醇铝，接着加入由20克氨水与35克水混合制成的溶液。得到的混合物反应5小时。反应之后，用足量乙醇洗涤这些颗粒。在固液分离后，所回收的颗粒在90℃真空干燥器中干燥8小时，得到涂有氧化铝的氧化锆基体颗粒3C。
再使用具有相同组成的溶液涂布所得到的涂有氧化铝的氧化锆粉末3C，然后干燥。这种干燥的粉末在氮气氛下在650℃旋转管式炉中加热2小时，得到涂有氧化铝的氧化锆粉末3D。所得到粉末的平均颗粒直径为5微米。
用V形搅拌器将由制得的粉末3B和3D组成的粉末与氧化铝粉末(平均颗粒直径5微米)彼此混合均匀。这种均匀粉末可采用HIP方法在1350℃煅烧8小时，得到煅烧物质。所得到煅烧物质的断裂韧性为9.9(MN*m-3/2)。
对比实施例2
对实施例3中使用的氧化铝基体颗粒(平均颗粒直径5微米)采用HIP方法在1350℃煅烧8小时。所得到煅烧物质的断裂韧性为4.4(MN*m-3/2)，它比煅烧上面所述混合粉末的断裂韧性的一半还低。
如上所示，通过形成含有均匀沉积的多组分的煅烧物质，可以得到增加的断裂韧性。
工业可应用性
根据本发明，具有一定厚度的一层或多层功能性涂层沉积在基体颗粒表面，将一定的性能赋予这些颗粒，并得到具有单层涂膜或复合涂膜的粉末。当通过颗粒之间存在的薄膜使粉末颗粒相互结合而模压这种粉末时，或当具有单层涂膜或复合涂膜的粉末颗粒以相同距离以一定方向排列并固结和模压，同时保持这一状态时，能够稳定地生产出具有一定功能的高价值产品。
具体地，在使用由磁性材料制成的基体颗粒的情况下，不仅得到磁头、磁核等，而且得到具有出色性能的高容量电容器。在使用由玻璃制成的基体颗粒的情况下，通过使用具有特定折光率的材料，形成具有特定厚度的涂膜，可以得到以一定角度发出偏振光的偏振滤光片等。
Claims (8)
1、一种由几种涂层粉末形成的固结物质，每种涂层粉末均包含具有厚度的0.01-20微米的均匀涂膜的基体颗粒，其中涂层粉末在涂膜处或由粘合剂而互相粘附。
2、根据权利要求1所述的由涂层粉末形成的固结物质，其中各涂层粉末均含有基体颗粒，该基体颗粒上有厚度0.01-20微米的均匀涂膜，基体颗粒包括玻璃、金属或金属氧化物，涂膜是金属薄膜或金属氧化物薄膜。
3、一种由几种涂层粉末粘合在一起的涂层粉末，每种涂层粉末均包含基体颗粒，该基体颗粒上有每层厚度均匀，为0.01-5微米的多层涂膜，其中至少任何相邻的涂膜是不同类的，其中该涂层粉末在最外层涂膜处或由粘合剂将其互相粘附。
4、根据权利要求3所述的由涂层粉末形成的固结物质，其中各涂层粉末均含有基体颗粒，该基体颗粒上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻的涂膜是不同类的，其中基体颗粒包括玻璃、金属或金属氧化物，涂膜是金属薄膜或金属氧化物薄膜。
5、根据权利要求1-4中任一权利要求所述的由涂层粉末形成的固结物质，其中基体颗粒包括磁性材料。
6、根据权利要求5所述的由涂层粉末形成的固结物质，其中至少一层涂膜包括介电材料。
7、一种由互相固结的几种涂层粉末形成固结材料的生产方法，该方法包括在涂膜处粘附各含有一种基体颗粒的粉末，该颗粒上有厚度0.01-20微米均匀涂膜，或者粘附各含有一种基体颗粒的粉末，该颗粒上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻的涂膜是不同类的。
8、一种由互相固结的几种涂层粉末形成固结材料的生产方法，该方法包括通过粘合剂粘附各含有一种基体颗粒的粉末，该颗粒上有厚度0.01-20微米均匀涂膜，或粘附各含有一种基体颗粒的粉末，在颗粒上有多层涂膜，每层厚度均匀，为0.01-5微米，其中至少任何相邻的涂膜是不同类的。
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|---|---|---|---|
| JP22871396A JP3742153B2 (ja) | 1996-08-29 | 1996-08-29 | 被覆粉体固結物およびその製造方法 |
| JP228713/96 | 1996-08-29 |
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| CN1235567A true CN1235567A (zh) | 1999-11-17 |
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| EP (1) | EP0950455A4 (zh) |
| JP (1) | JP3742153B2 (zh) |
| KR (1) | KR100470818B1 (zh) |
| CN (1) | CN1235567A (zh) |
| AU (1) | AU736896B2 (zh) |
| CA (1) | CA2264620A1 (zh) |
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| CN1771569B (zh) * | 2003-02-05 | 2010-05-26 | 加拿大易姆芬公司 | 用于ac应用的高性能磁性复合材料及其生产方法 |
| CN110382440A (zh) * | 2016-11-07 | 2019-10-25 | 科罗拉多大学董事会 | 改进技术级陶瓷的性能 |
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1997
- 1997-08-20 KR KR10-1999-7001339A patent/KR100470818B1/ko not_active IP Right Cessation
- 1997-08-20 CN CN97199239A patent/CN1235567A/zh active Pending
- 1997-08-20 EA EA199900240A patent/EA003173B1/ru not_active IP Right Cessation
- 1997-08-20 AU AU38672/97A patent/AU736896B2/en not_active Ceased
- 1997-08-20 CA CA002264620A patent/CA2264620A1/en not_active Abandoned
- 1997-08-20 US US09/254,005 patent/US6863979B2/en not_active Expired - Fee Related
- 1997-08-20 WO PCT/JP1997/002895 patent/WO1998008638A1/ja not_active Application Discontinuation
- 1997-08-20 EP EP97935840A patent/EP0950455A4/en not_active Ceased
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1999
- 1999-02-26 NO NO990946A patent/NO990946L/no not_active Application Discontinuation
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2004
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1771569B (zh) * | 2003-02-05 | 2010-05-26 | 加拿大易姆芬公司 | 用于ac应用的高性能磁性复合材料及其生产方法 |
| CN110382440A (zh) * | 2016-11-07 | 2019-10-25 | 科罗拉多大学董事会 | 改进技术级陶瓷的性能 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO1998008638A1 (fr) | 1998-03-05 |
| EP0950455A1 (en) | 1999-10-20 |
| EA003173B1 (ru) | 2003-02-27 |
| NO990946D0 (no) | 1999-02-26 |
| US20030129388A1 (en) | 2003-07-10 |
| US6863979B2 (en) | 2005-03-08 |
| AU3867297A (en) | 1998-03-19 |
| US20050003192A1 (en) | 2005-01-06 |
| NO990946L (no) | 1999-04-28 |
| CA2264620A1 (en) | 1998-03-05 |
| EA199900240A1 (ru) | 1999-10-28 |
| JPH1068002A (ja) | 1998-03-10 |
| EP0950455A4 (en) | 2004-04-07 |
| AU736896B2 (en) | 2001-08-02 |
| KR20000035790A (ko) | 2000-06-26 |
| KR100470818B1 (ko) | 2005-03-07 |
| JP3742153B2 (ja) | 2006-02-01 |
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