CN103201234B - 多晶金刚石材料的制备方法 - Google Patents

多晶金刚石材料的制备方法 Download PDF

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CN103201234B
CN103201234B CN201180047527.4A CN201180047527A CN103201234B CN 103201234 B CN103201234 B CN 103201234B CN 201180047527 A CN201180047527 A CN 201180047527A CN 103201234 B CN103201234 B CN 103201234B
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diamond
crystal grain
salt
adamantine
diamond particles
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CN103201234A (zh
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喀吾施尼·奈都
杰弗里·约翰·戴维斯
约翰内斯·路德维克丝·迈伯勒
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Element Six Abrasives SA
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    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
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Abstract

一种制造多晶金刚石材料的方法，所述方法包括提供多个金刚石颗粒或晶粒，以具有非金属的金刚石催化剂材料的粘合剂材料涂覆所述金刚石颗粒或晶粒，巩固涂覆的金刚石颗粒或晶粒以形成生坯，并对所述生坯施加温度和压力，在其中金刚石是热力学稳定的，以烧结并形成多晶金刚石材料。

Description

多晶金刚石材料的制备方法
技术领域
本发明涉及制造多晶金刚石（PCD）材料的方法，及如此制造PCD材料。
背景技术
用于机器和其他工具的刀具嵌件可以包括一层结合到硬质合金基材的多晶金刚石（PCD）。PCD是超硬材料的例子，也称为超硬磨料，它具有基本上大于烧结碳化钨的硬度值。
包含PCD的组件可以被用于多种工具，例如切割、机加工、钻孔或降解硬的或磨蚀性的材料例如岩石、金属、陶瓷、复合和含木的材料。PCD包含大量基本上共生的金刚石晶粒，该金刚石晶粒形成骨架体并限定金刚石晶粒之间的间隙。PCD材料包含至少约80%体积比的金刚石，并且可在烧结助剂，也称为金刚石催化剂或溶剂/催化剂材料存在的情况下，通过使金刚石晶粒聚集体经受高于约5GPa的超高压力和至少约1200摄氏度的温度而制备。金刚石催化剂材料被理解为在金刚石比石墨热力学更稳定的压力和温度的条件下能够促进金刚石晶粒直接共生的材料。一些金刚石催化剂材料可在环境压力下，特别是在升高的温度下促进金刚石向石墨的转化。金刚石催化剂材料的实例为钴、铁、镍和包括这些中任意几种的特定合金。PCD可以形成在烧结钴碳化钨基材上，该基材可提供用于PCD的钴催化剂材料源。PCD材料中的间隙可以至少部分用催化剂材料进行填充。
这一种的PCD材料经历一个众所周知的问题，然而，是金刚石催化剂材料的残余存在，特别是金属的金刚石催化剂材料，例如在空隙中的钴，镍或铁，高温下PCD材料的性能可能产生的一个不利的影响。在应用中，PCD材料可能受热和热降解，这主要是由于在金属的催化剂材料的存在下，可以催化的金刚石的石墨化，由于金属的催化剂材料和金刚石的微观结构之间的热膨胀相差大，也可能导致在PCD材料的应力。
解决此问题的一种方法是移除，通常是通过从PCD材料过滤催化剂材料，所述催化剂材料也指在本领域中作为催化剂/溶剂。
专利号为3,745,623和4,636,253的美国专利教导了在过滤过程中加热的酸混合物的使用，其中分别使用了HF，HCl，HNO3和HNO3和HF的混合物。
专利号为4,288,248和4,224,380的美国专利描述了通过单独在含有HNO3-HF（硝酸和氢氟酸）的热介质或结合含有HCl-HNO3（盐酸和硝酸）的第二热的介质过滤PCD表面以去除催化剂/溶剂。
专利公布号为2007/0169419的美国专利申请描述了一种从PCD表面过滤部分或所有的催化剂/溶剂的方法，所述方法通过屏蔽部分PCD表面使其不被过滤，和在腐蚀溶液中浸渍屏蔽的PCD表面以溶解催化剂/溶剂在水和王水中。通过使用声波能量加速过滤过程，所述声波能量搅拌PCD表面和腐蚀性溶液之间的界面，加速的催化剂/溶剂的溶解速率。
专利号为4,572,722的美国专利公开了在过滤过程之前或期间，通过激光切割或火花发射在PCD表面形成孔以加速过滤过程。然后，使用传统的酸过滤技术，电解过滤和锌液的提取过滤PCD表面。
解决这个问题的另一种方法是使用一个非金属的金刚石催化剂材料，所述金刚石催化剂材料产生一个更热稳定的PCD材料。
JP2795738（B2）描述了在压力为6-12GPa和温度为1700-2500°C下，烧结金刚石粉末和金属碳酸盐的混合物，以得到在烧结金刚石层中的，由0.1-15％体积比的非金属的粘合剂组成的烧结的多晶材料。
JP4114966描述了使用加入的碳粉末和碱土碳酸盐作为烧结助剂金刚石粉末，为了提高非金属系统的烧结性。
JP2003226578也发表了较差的烧结性的问题，它描述了草酸二水合物在碳酸酯类非金属溶剂/催化剂体系作为烧结助剂的使用。
JP2002187775描述了加入其他有机化合物来实现烧结的基于碳酸酯的非金属的PCD，和类似地加入JP6009271中描述的金属碳化物。
发明内容
从第一个方面看，提供了一种用于制造多晶金刚石材料的方法，该方法包括：提供多个金刚石颗粒或晶粒，用包括一个非金属的金刚石催化剂材料的粘合剂材料涂覆的金刚石颗粒或晶粒，巩固涂覆的金刚石颗粒或晶粒形成生坯，并对所述生坯施加温度和压力，在其中金刚石是热力学稳定的，以烧结并形成多晶金刚石材料。
在一些实施例中，金刚石颗粒或晶粒悬浮在液体介质中，用于金刚石的非金属催化剂材料在液体介质中原位沉淀在相应的金刚石颗粒或晶粒的表面上，以涂覆金刚石颗粒或晶粒。
在一些实施例中，用于金刚石的非金属催化剂材料是沉淀的盐，它包括第一的碱或碱土金属的盐的溶液的反应产物，并第二的阴离子的盐的溶液，与第一的盐的碱土或碱土金属能够形成不溶性的盐。
在一些实施例中，当沉淀用于金刚石的非金属催化剂材料，包含第一和第二的盐的溶液同时引入到金刚石悬浮液，从而涂覆金刚石颗粒或晶粒。
在一些实施例中，在涂覆之前的金刚石颗粒或晶粒具有平均颗粒或晶粒尺寸为约10纳米至约50微米。
在一些实施例中，提供不同平均颗粒或晶粒尺寸的金刚石颗粒或晶粒的多峰混合物。
在一些实施例中，多晶金刚石材料的金刚石含量是至少约80％，至少约88％，至少约90％，至少约92％或甚至至少约96％的多晶金刚石材料的体积。在一个实施例中，多晶金刚石材料的金刚石含量最多约98％的多晶金刚石材料的体积。
在一些实施方案中，非金属催化剂材料的含量是至多约10％体积比，至多约8％体积比，或甚至至多约4％体积比的PCD材料。
在一个实施例中，该方法包括在用于金刚石的非金属催化剂材料的存在下，对生坯施加压力和温度，使金刚石比石墨热力学更稳定。在一个实施例中，压力是至少约6.8GPa和温度是至少约2000摄氏度。
从进一步的方面看，提供大量金刚石颗粒或晶粒，其涂覆在用于金刚石的非金属催化剂材料。
在一些实施例中，用于金刚石的非金属催化剂材料从碳酸盐的碱或碱土金属中的组选择出。
在一些实施例中，用于金刚石的非金属催化剂材料是选自碳酸钙，碳酸镁，碳酸钡，碳酸锶，碳酸钠，以及它们的混合物组成的组中。
在一个实施例中，用于金刚石的非金属催化剂材料是碳酸钙和碳酸镁的组合。
在一些实施例中，相应的金刚石颗粒或晶粒的涂层的厚度是从约5纳米至约5微米。
在一些实施例中，相应的涂覆的金刚石颗粒或晶粒包括从约1％至约50％体积比，或从约5％至约15％体积比的用于金刚石的非金属催化剂材料。
在一些实施例中，各自的金刚石颗粒或晶粒的表面覆盖率为从约5％至约100％。
从另一个方面来看，提供了一种根据上述方法形成的包括多晶金刚石材料磨损元件。
附图说明
现在将通过示例的方式参考附图详细描述非限制性实施方式，附图中：
图1是一个多晶金刚石材料的实施例的样品的XRD分析;
图2是在250倍放大倍数的SEM显微照片的一个多晶金刚石材料的实施例的横截面;
图3是在5,000倍放大倍数的SEM显微照片的一个多晶金刚石材料的实施例的横截面;
图4是在2,500倍放大倍数的SEM显微照片的一个多晶金刚石材料的实施例的横截面.
具体实施方式
如本文所用，“多晶金刚石”（PCD）材料包括大量金刚石晶粒，其中的主要部分是直接彼此结合的，并在其中金刚石的含量是至少材料的约80％体积比。在PCD材料的一个实施例中，金刚石晶粒之间的间隙可以是至少部分地用一种粘合剂材料填充，所述粘合剂材料包括一个用于金刚石的非金属催化剂。
如本文所用，“用于金刚石的非金属催化剂材料”是一种能够涂覆金刚石颗粒或晶粒的表面上的材料，并且在金刚石比石墨热力学更稳定的温度和压力的条件下，能够催化多晶金刚石颗粒或晶粒共生。
如本文所用，“间隙”或“间隙性区域”是PCD材料的金刚石晶粒的之间的区域。
大量的晶粒的多峰尺寸分布被理解为具有一个以上的单峰的尺寸分布的晶粒，每一个峰对应于一个相应的“模式”。多峰的多晶体通常通过提供一个以上的多个晶粒的源而形成，每个源包括具有基本上不同的平均尺寸的晶粒，并与从源得来的晶粒或颗粒混合在一起。混合晶粒的尺寸分布的测量通常显示对应于不同的模式的不同的峰。当颗粒烧结在一起，以形成多晶体，由于晶粒彼此压实并发生断裂，所述晶粒进一步改变尺寸分布从而减少整体的晶粒的尺寸。然而，在烧结制品的图像分析，晶粒的多峰通常仍是明显。
如本文所用，生坯是要烧结的或已部分烧结的物，但尚未完全的烧结以形成最终产品。一般情况下，它可能是自己支撑的，并且可以具有预期完成的一般形式。
如本文所用，超硬磨损元件是包括超硬材料的元件，用于磨损的应用，如降解，钻孔，切割或机械加工包括硬盘或研磨材料的工件或体。
在一些实施例中，制造多晶金刚石材料的方法包括用于金刚石的非金属催化剂材料的粘合剂材料涂覆多个金刚石颗粒或晶粒。涂覆的金刚石颗粒或晶粒被巩固并入生坯，然后对生坯施加温度和压力，其中金刚石是比石墨热力学更稳定的，以烧结和形成多晶金刚石材料。
在一个实施例中，非金属性粘合剂材料在溶胶-凝胶过程中与金刚石颗粒或晶粒结合。在剧烈搅拌下，金刚石粉末悬浮在液体中，以形成金刚石悬浮液。虽然可以使用任何适当的液体介质，该液体可以是，例如，水。选择所需的碱或碱土金属成为第一的盐，使得其在溶剂中是可溶的，但与选定的金刚石悬浮液中的阴离子形成一种不溶性的盐。选择所需阴离子成为第二的盐，使得其在溶剂中是可溶的，但阴离子与第一的盐的碱或碱土金属形成不溶性的盐。
随着逐滴加入含溶液的两个盐到金刚石悬浮液，使得由第一盐的碱或碱土金属和第二盐的阴离子组成的不溶的沉淀物形成在相应的金刚石颗粒或晶粒的表面上。
在逐滴加入期间，含有悬浮的金刚石颗粒或晶粒的液体被搅拌。这种搅拌可以通过的加热搅拌器和磁力搅拌器，或由一个顶部搅拌器，或通过超声波处理，或任何其它能够有效地分散液体中的金刚石颗粒的合适的方法完成。
金刚石粉末与沉淀的盐可以从悬浮液中除去，并在适合用于除去可能存在的任何残留的悬浮介质或溶剂的温度干燥。干燥温度通常是50-100℃。金刚石与沉淀的盐可能在干燥过程中固定，或被搅拌，抛出或在增加效率或干燥速率的方式移动。
沉淀之前，金刚石颗粒可以具有范围从10纳米至50微米的平均尺寸。它们可能具有的表面的功能群包括羟基，羰基，羧酸，醛，酮或任何其它表面的功能群，其中含有一个或多个氧，碳，氢，氮和硼。
在金刚石颗粒的表面上形成的沉淀的盐可以是圆形的小球，扁平的圆顶，诸如晶须或纤维的细长的形状，或平面或不规则形状。沉淀的盐可以覆盖部分或完全的金刚石颗粒，提供了足够薄的涂层，以允许在选择的烧结条件下发生金刚石共生。沉淀的盐可以具有单位至少一个维度上是从2纳米至1微米的平均颗粒尺寸。
可以从碱或碱土金属的组的碳酸盐选择沉淀的盐。例子是碳酸钙，碳酸镁，碳酸钡，碳酸锶，碳酸钠，或它们的混合物。沉淀的盐可以是碳酸钙和碳酸镁的混合物，其可以同时或依次沉积。用于金刚石的非金属催化剂材料的其它实例为本领域的技术人员在现有技术中所理解，包括硫酸盐，氢氧化物，氧化物，磷酸盐和硅酸盐。
在一个合适的容器中，金刚石颗粒与沉淀的盐被合并以形成生坯，并放置在高压高温冲压。为了一起烧结金刚石颗粒，通常施加压力为6.8-7.7GPa或更大，温度为2000-2200℃或更高。
在烧结体中，金刚石晶粒显示共生，并且可以具有从10纳米至50微米的平均晶粒尺寸的范围。
在烧结体中，非金属的粘合剂包括平均颗粒尺寸范围从2纳米到5微米的晶粒。
实施例
参考下面非限制性实施例，对实施方案进行更详细的描述。
实施例1
平均颗粒尺寸为4微米的100克的金刚石粉末被称量加入到一个5升的烧杯中，并加入2升的去离子水，并用磁力搅拌器搅拌。一种超声波探头插入烧杯中，超声水-金刚石悬浮液15分钟，以确保完全分散的金刚石粉末。然后除去探头，但搅拌是继续的。在一个1升的玻璃烧杯中，以200毫升的去离子水形成5.5克无水氯化镁溶液，并转移到一个滴液漏斗中。在一个1升的玻璃烧杯中，另一种以200毫升的去离子水形成5.7克无水碳酸铵，并转移到另一个滴液漏斗。所述的滴液漏斗位于玻璃烧杯的上方，并在约45分钟的时段逐滴加入所述两种溶液到悬浮的金刚石。计算在最终涂覆的金刚石粉末中的溶液的浓度和量，得到一个大概5％容量的碳酸镁的值。继续搅拌约10分钟。涂覆碳酸镁沉淀物的金刚石被滤出，并用冷的去离子水洗涤，最后用乙醇洗涤，并于40℃的烘箱中干燥一个晚上。SEM分析显示碳酸镁的沉淀物在金刚石颗粒的表面上。所述沉淀物是直径约30至300纳米的典型扁平的圆顶状物。X射线衍射分析证实所述沉淀物是MgCO3.3H2O，如附图1中所示。
将干燥的金刚石的碳酸镁粉末放置在金属杯并放置在高压高温冲压，并施加压力为约7.7GPA，温度为约2100℃约1分钟。提取和抛光已烧结的PCD，并通过SEM查验。观察到某些共生的金刚石晶粒。
实施例2
按照如在实施例1的同样的步骤，不同的是烧结温度提高到约2250℃。抛光的样品的SEM分析显示比在实施例1中有更多共生，如附图2至4中所示。
实施例3
按照如在实施例1的同样的步骤，不同的是烧结温度提高到约2200℃。抛光的样品的SEM分析显示比在实施例1中有更多共生。
实施例4
按照如在实施例1的同样的步骤，不同的是烧结温度提高到约2200℃，并停留时间增加至3分钟。抛光的样品的SEM分析显示比在实施例1中有更多共生。
实施例1至4中的四个样品的性质进行了测定并于表1中报告。
表1
样品的热重分析证实样品相对有金属粘合剂的PCD有改进的热稳定性。有Co-WC粘合剂的PCD的氧化的发端测定为750℃，而当前发明的PCD样品的氧化的发端，使用非金属粘合剂，是在约970℃。
在磨损性能测试中，相比基于Co-WC的PCD，钻岩石显示非金属的PCD有24-85％的磨损性能的改善。

Claims (9)

1.一种制造多晶金刚石材料的方法，所述方法包括提供多个金刚石颗粒或晶粒，以包含用于金刚石的非金属催化剂材料的粘合剂材料涂覆所述金刚石颗粒或晶粒，巩固涂覆的金刚石颗粒或晶粒以形成生坯，并对所述生坯施加温度和压力，在其中金刚石是热力学稳定的，以烧结并形成多晶金刚石材料；
其中所述金刚石颗粒或晶粒悬浮在液体介质中，所述用于金刚石的非金属催化剂材料在液体介质中原位沉淀在相应的金刚石颗粒或晶粒的表面上，以涂覆金刚石颗粒或晶粒；及
其中所述用于金刚石的非金属催化剂材料是沉淀的盐，所述沉淀的盐包括第一的碱或碱土金属的盐的溶液的反应产物，并第二的阴离子的盐的溶液，其与第一的盐的碱土或碱土金属能够形成不溶性的盐。
2.如权利要求1所述的方法，其中当所述用于金刚石的非金属催化剂材料沉淀，包含第一和第二的盐的溶液同时引入到金刚石悬浮液，从而涂覆金刚石颗粒或晶粒。
3.如权利要求1所述的方法，其中在涂覆之前的金刚石颗粒或晶粒具有平均颗粒或晶粒尺寸为10纳米至50微米。
4.如权利要求1所述的方法，其中所述多晶金刚石材料的金刚石含量是至少80％和最多98％的多晶金刚石材料的体积。
5.如权利要求1所述的方法，其中所述用于金刚石的非金属催化剂材料是选自由碱或碱土金属的碳酸盐组成的组中的沉淀的盐。
6.如权利要求5所述的方法，其中所述用于金刚石的非金属催化剂材料是选自由碳酸钙，碳酸镁，碳酸钡，碳酸锶，碳酸钠，以及它们的混合物组成的组中。
7.如权利要求1所述的方法，其中所述多晶金刚石材料包括至多10％体积的用于金刚石的非金属催化剂材料。
8.如权利要求1所述的方法，其中所述方法包括在用于金刚石的非金属催化剂材料的存在下，对生坯施加温度和压力，其中金刚石是比石墨热力学更稳定的。
9.如权利要求8所述的方法，其中所述压力是至少6.8GPa和温度是至少2000摄氏度。
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