CN101193695A - 生产超硬磨粒的方法 - Google Patents

生产超硬磨粒的方法 Download PDF

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CN101193695A
CN101193695A CNA2006800208200A CN200680020820A CN101193695A CN 101193695 A CN101193695 A CN 101193695A CN A2006800208200 A CNA2006800208200 A CN A2006800208200A CN 200680020820 A CN200680020820 A CN 200680020820A CN 101193695 A CN101193695 A CN 101193695A
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M·G·芒迪
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Element Six Production Pty Ltd
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Abstract

本发明涉及适合于在高压高温金刚石或立方氮化硼合成中使用的颗粒或材料的脱除粘合剂和/或纯化方法，该方法包括下述步骤：使颗粒或材料以连续的方式穿过具有控制氛围和温度的区域，该区域具有在该区域内大于约600℃的最大温度，其中在该区域内每一颗粒所度过的时间小于30分钟。

Description

生产超硬磨粒的方法
发明背景
本发明涉及生产超硬磨粒，尤其金刚石粒子的方法。
通过合成生产金刚石和立方氮化硼磨粒的方法是本领域众所周知的。可微调该方法生产具有特定特征的粒子。例如，可微调该方法生产诸如在粉碎之类应用中使用的发脆的金刚石粒子。或者，可微调该方法生产良好质量的坚固块状金刚石。这种金刚石典型地用于锯和粉碎应用中。
通过通常在金刚石溶剂存在下，将碳源，即金刚石的前体置于金刚石在其下晶体学稳定的升高的温度和压力条件下，合成金刚石。类似地，通过在用于立方氮化硼的溶剂/催化剂存在下，将六方氮化硼，即立方氮化硼的前体置于立方氮化硼在其下晶体学稳定的升高的温度和压力条件下，合成立方氮化硼粒子。
EP0737510公开了通过用非金刚石碳材料，金属粉末形式的催化剂/溶剂和有机粘合剂的至少一层涂布金刚石微粒，以使得它们至少部分彼此接触的方式压实涂布的粒子，将压实的结构置于合适的合成容器中，并将该压实的结构置于金刚石在其下晶体学稳定的温度和压力条件下，合成金刚石粒子的方法。
使用涂布的金刚石微粒形成颗粒以供合成较大的金刚石具有数个优点。可压实这种颗粒，以便得到微细的金刚石种子以规则阵列排列或者彼此至少隔开某一最小距离的压制品(compact)。使用这种压制品合成金刚石的潜力是与若种子金刚石在整个压制品中无规分布的情况相比，将得到较大量质量高的金刚石。
然而，在压实颗粒，形成在金刚石合成工艺中使用的固体压制品之前，需要从颗粒中除去粘合剂材料。这典型地通过在加热炉内，在选择的氛围和压力下，使颗粒置于升高的温度下来实现。所要求的温度取决于所使用的粘合剂材料。EP0737510教导了范围为300-600℃的范围，该专利还教导了加热炉内氛围应当为还原或者惰性氛围，以便最小化压制品内溶剂金属的氧化。所公开的实例是在400至600℃的温度下，经30至60分钟的时间段在颗粒上流过的氢气或氢气/氮气混合物的物流。它是间歇工艺，其中颗粒填充在加热炉内并保持静态，同时所选气体的加热气氛在其上流过，并将粘合剂去除工艺中的气体副产物泵送出加热炉。
在EP0737510中公开的粘合剂去除工艺的潜在缺点是，由于粘合剂的去除，颗粒显著弱化(weaken)，而粘合剂的目的是将各成分粘结在一起。在随后的处理和输送过程中，在其压实之前，这可能会增加颗粒破碎的可能性，其结果是会降低导致优异金刚石质量的有益的粒化效果。限制温度到小于600℃的另一缺点是，在升高的温度下需要度过相对长的时间，以便实现粘合剂的完全去除，这是因为去除速度倾向于随着温度增加而增加。这具有倾向于增加溶剂金属氧化程度的有害效果，其中在升高的温度下以及在该温度本身下，溶剂金属的氧化随着时间增加而增加。
间歇熔炼方法除去粘合剂的进一步的缺点是，粘合剂的去除速度可能不同，因此对于在加热炉内的不同部分处的颗粒来说，实际粘合剂的去除不同。若颗粒以相对厚的层填充在彼此顶部，则这一问题会恶化，这是因为在这一构造内，不同位置的颗粒可经历不同的温度、加热速度以及粘合剂燃烧速度和气体副产物去除速度。因此，在去除工艺之后一些颗粒或者仍然保留一些粘合剂材料，或者工艺时间比所需的要长，其结果是溶剂金属的氧化比必需的大。已知在这一阶段中粘合剂的不完全去除对在随后的合成工艺过程中生长的金刚石的质量和产率具有有害的影响。
发明概述
根据本发明，从多个颗粒中除去粘合剂材料的方法包括在足以从基本上所有颗粒中除去粘合剂材料的温度和时间下，使颗粒连续地穿过加热区，其中所述多个颗粒包括至少一个磨粒，磨粒的前体，磨粒/前体用溶剂/催化剂，和粘合剂材料。
实施方案的说明
本发明是制备用于金刚石合成的金刚石种子涂布的颗粒中使用的有机粘合剂材料的除去方法。特别地，本发明涉及适合于在高压高温金刚石或立方氮化硼合成中使用的颗粒或材料(下文称为颗粒)的脱除粘合剂(debinder)和/或纯化方法，该方法包括下述步骤：使颗粒以连续的方式穿过具有控制氛围和温度的区域，该区域具有在该区域内大于约600℃的最大温度，其中在该区域内每一颗粒所度过的时间小于30分钟。
优选地，颗粒以层，优选薄层形式填充在传送带体系上并以连续而不是间歇模式穿过具有控制的氛围和温度的区域，其中在该区域内的最大温度大于约600℃(热区)，并且其中在该热区内每一颗粒度过的时间小于30分钟。含氢气的气体物流(它典型地包括另一气体，如氮气和/或惰性气体)连续地穿过热区并在移动的颗粒上通过，从而带走去除工艺中的气体副产物。
术语薄层是指包括小于20mm深的颗粒层，更优选小于10mm深，更优选小于9mm深，更优选小于8mm深，更优选小于7mm深，更优选小于6mm深，最优选小于5mm深。
优选地，热区的温度大于700℃，更优选大于750℃，更优选大于800℃，更优选大于850℃，最优选大于900℃。优选地，最小温度是颗粒内包含的粘合剂的热解温度。
优选地，热区的温度小于1300℃，更优选小于1190℃，更优选小于1180℃，更优选小于1170℃，更优选小于1160℃，最优选小于1150℃。
优选地，在热区内每一颗粒度过的时间小于10分钟，更优选小于9分钟，更优选小于8分钟，更优选小于7分钟，更优选小于6分钟，最优选小于5分钟。
可利用这一方法很好地控制颗粒穿过热区的速度、气体物流在热区内的流动速度和因此气体副产物的去除速度，以及热区的温度和尺寸。因此，可非常好地控制粘合剂的去除工艺，因为这样可在颗粒内均匀地除去粘合剂。
优选地，穿过热区的气体物流的速度和颗粒的通过速度存在净差(net difference)。要理解，气体物流和颗粒可在相同的方向上行进(在不同的速度下)，但在本发明的优选实施方案中，气体物流与颗粒穿过的方向相反。
本发明方法的重要特征是如此布局以便每一颗粒经历基本上相同的温度和气体环境条件。其结果是，粘合剂的去除反应，反应产物的去除和通过该方法引起的颗粒的任何变化对于每一颗粒来说基本上相同。这进而得到每一颗粒的化学和物理状态的再现与优化的理想结果，因为它涉及使用颗粒的压制品制备优异质量的合成金刚石。
本发明的优点是，所有颗粒相同地在粘合剂去除工艺中进行处理，因为在相同的时间段内它们全部暴露于同样的温度和大气条件下。因此所有颗粒经历相同的粘合剂去除速度和程度。因此，一旦优化加热炉内条件，则所有颗粒具有得到相同优异质量金刚石晶体的潜力。此外，由于暴露于升高的温度下的时间少于现有技术，因此此处所使用的较高温度的结果是，颗粒内溶剂金属的氧化潜力下降。
使用高于600℃的温度的另一优点是，颗粒内在溶剂金属粉末之间的粘结程度更大，这是因为这种粘结程度倾向于随着温度增加而增加。因此，在粘合剂去除工艺之后，颗粒倾向于更加坚固，因此更加结实，并且在处理和运输过程中颗粒破碎的程度下降。在压实工艺之前和压实工艺之中颗粒更大可能地保持其结构完整性的事实意味着对于金刚石的合成来说，使用压实颗粒的优势更加可能充分地实现。
与间歇熔炼方法相反，在使用该颗粒随后生产的金刚石质量方面，本发明方法的有益程度令人惊奇地大。
根据本发明方法处理的颗粒各自含有超硬磨粒，和优选仅仅一种这样的粒子。该颗粒还含有用于磨粒的溶剂/催化剂或这种溶剂/催化剂的前体和超硬磨粒的前体。该颗粒是任何合适形状或尺寸的各种组分的粘着物料，且可通过诸如粒化、造粒或喷涂之类的方法生产。
该颗粒还含有粘合剂，所述粘合剂可以是有机或无机粘合剂，优选有机粘合剂。这种粘合剂的实例是纤维素醚，有机聚合物和类似物。根据本发明的方法，在颗粒置于高温/高压生长条件下之前除去这种粘合剂。
磨粒通常是金刚石或立方氮化硼粒子。本发明方法在生产金刚石粒子中具有特殊的应用。颗粒内的粒子通常是微细的，例如尺寸小于100微米。
可以以层形式或者以每一颗粒的混合物形式提供溶剂/催化剂或其前体和用于磨粒的前体，其中优选后者。这些组分在颗粒内通常为粉末形式。
用于金刚石和立方氮化硼的溶剂/催化剂是本领域众所周知的。金刚石溶剂/催化剂的特别合适的实例是过渡金属，例如钴、铁、镍或含有一种或更多种这些金属的合金。也可使用溶剂/催化剂的前体。金刚石溶剂/催化剂前体的实例是诸如氧化镍、氧化钴或氧化铁之类的氧化物，或将还原或热解为氧化物的化合物，例如诸如铁、钴或镍之类金属的碳酸盐和草酸盐。当使用前体时，优选颗粒进行热处理，还原前体为金属，之后使颗粒进行高温/高压烧结。用于还原的热处理根据颗粒性质、其内容物和前体的性质而变化。溶剂/催化剂的前体还原为特别微细粒度的金属，以便在超硬磨粒周围提供层中各组分的微细和均匀的混合物。
用于金刚石的前体是非金刚石碳，例如石墨或无定形碳。用于立方氮化硼的前体是六方氮化硼。
颗粒置于其下的升高的温度和压力生长条件是本领域众所周知的。典型的压力范围为3-8GPa和典型地温度范围为1000-2100℃。
从高温/高压装置的反应区中取出处理过的材料。使用本领域已知的回收步骤回收该材料。
参考下述非限定性实施例描述本发明。
实施例1：
在不锈钢盘上热处理适合于金刚石合成的含石墨、铁和镍粉末的颗粒，所述不锈钢盘穿过具有控制的还原氛围的输送式加热炉，以除去粘合剂并纯化颗粒。所使用的条件是每盘1 kg颗粒(该盘的面积为800cm2)，维持含85％N2、15％H2的控制氛围和各自600 1/120 1/分钟的实际流速(足以避免在加热炉入口和出口处空气进入)，加热炉的顶部温度为1050℃，和在顶部温度下颗粒的时间为4分钟30秒。
紧跟着在热处理之后分析颗粒。
所有的测量结果用百分数表示。
    元素     批料A(1.1mm颗粒)     批料阶段B(1.6mm颗粒)
    Al     0.0003     0.0007
    Ca     0.0010     0.0007
    Co     0.0002     0.0001
    Cr     0.0010     0.0010
    Cu     0.0011     0.0010
    Mg     0.0001     0.0001
    Mn     0.0009     0.0006
    Mo     0.0005     0.0005
    N     0.0051     0.0063
    Na     0.0011     0.0056
    O     0.0090     0.0094
    P     0.0177     0.0022
    S     0     0.0004
    Si     0.0056     0.0061
    V     0.0005     0.0005
实施例2：
与以上一样采用100％的H氛围。获得类似的分析结果。
实施例3：
与以上一样在900℃下。微量元素化学类似，但发现O的浓度较高为0.0120％。
实施例3：
与以上一样在1130℃下。微量元素化学类似，但发现O的浓度较低为0.0085％。

Claims (16)

1.适合于在高压高温金刚石或立方氮化硼合成中使用的颗粒或材料的脱除粘合剂和/或纯化方法，该方法包括下述步骤：使颗粒或材料以连续的方式穿过具有控制氛围和温度的区域，该区域具有在该区域内大于约600℃的最大温度，其中在该区域内每一颗粒所度过的时间小于30分钟。
2.权利要求1的方法，其中含氢气的气体物流连续地穿过该区域并在颗粒或材料上穿过。
3.权利要求2的方法，其中气体物流进一步包括另一气体，如氮气和/或惰性气体。
4.权利要求2和3中任何一项的方法，其中气体物流带走脱除粘合剂和/或纯化工艺中的气体副产物。
5.前述权利要求中任何一项的方法，其中颗粒或材料以薄层形式堆积在穿过该区域的盘内。
6.前述权利要求中任何一项的方法，其中该区域具有大于700℃的温度。
7.前述权利要求中任何一项的方法，其中该区域具有小于1300℃的温度。
8.前述权利要求中任何一项的方法，其中在热区内每一颗粒所度过的时间小于30分钟。
9.前述权利要求中任何一项的方法，其中颗粒或材料穿过该区域的速度、气体物流在该区域内的流动速度、气体副产物的去除、该区域的温度和尺寸是可控的。
10.前述权利要求中任何一项的方法，其中穿过该区域的气体物流的速度和穿过该区域的颗粒或材料的速度存在净差。
11.权利要求10的方法，其中气体物流与颗粒的穿过方向相反。
12.前述权利要求中任何一项的方法，其中每一颗粒经历基本上相同的温度和气体环境条件。
13.前述权利要求中任何一项的方法，其中区域的温度使得发生颗粒或材料的部分烧结。
14.进行过权利要求1-13中任何一项的方法的颗粒。
15.基本上如前所述或例举的本发明的方法。
16.基本上如前所述或例举的本发明的颗粒。
CNA2006800208200A 2005-05-04 2006-05-04 生产超硬磨粒的方法 Pending CN101193695A (zh)

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