CN111233476A - 一种无粘结剂多晶金刚石材料及其制备方法 - Google Patents
一种无粘结剂多晶金刚石材料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种无粘结剂多晶金刚石材料，制备原料包括50％～100％的金刚石微粉，0～50％的非金刚石碳粉；所述非金刚石碳包括石墨、无定型碳、碳纳米管、纳米洋葱碳、石墨烯、C60。上述无粘结剂多晶金刚石材料的制备方法，以50％～100％的金刚石微粉和0～50％的非金刚石碳粉为原料经高温高压烧结制备获得无粘结剂多晶金刚石材料成品。上述无粘结剂多晶金刚石材料非碳成分质量比低于1％，具有极高硬度、极高耐磨性及高热稳定性，应用于制作制备油气钻探的钻齿以及机械加工用刀具。
Description
技术领域
本发明涉及金刚石材料技术领域，具体涉及一种无粘结剂多晶金刚石材料及其制备方法。
背景技术
作为碳的一种形态(同素异形体)，金刚石是已知最硬的材料，已广泛应用在工业上。人工合成金刚石始于上世纪50年代，人们在静高压5GPa-7GPa(1GPa约为一万大气压)、温度为1300℃-1800℃且有触媒的作用下将石墨转变成金刚石，目前已在工业领域大规模生产，应用于除黑色金属以外的材料的研磨、抛光、钻、铣、切削加工，以及石油、天然气、采矿等的钻头钻齿的制作。
到目前为止，工业界已经可以使用相关技术(温度梯度法、晶种法、气相沉积法等)合成出厘米级大小的高纯度单晶金刚石。但是单晶金刚石由于各向异性，虽然硬度高，但性脆，容易沿解理面开裂，且价格昂贵，目前多用于首饰及高加工精度的超硬刀具制备。聚(多)晶金刚石烧结体(PCD，polycrystalline diamond，刀具用多晶金刚石复合片；PDC，polycrystalline diamond cutter，油气钻探用多晶金刚石复合片)虽然硬度不如单晶金刚石，但由于其宏观上地各向同性、较高的韧性及相对低的价格，在工业上的应用性价比优于单晶金刚石，成为了量大面广的人工合成材料。
然而，目前工业上使用的多晶金刚石(PCD/PDC)材料中含有非碳成分的粘结剂，如：钴等金属材料，或碳化硅、碳化硼、碳化钛等非金属材料，其非碳成分粘结剂质量百分比通常大于1％(一般为5％-20％)，致使其耐磨性、硬度及热稳定性等低于单晶金刚石。其主要原因在于：多晶金刚石(PCD/PDC)材料工作前端通常处于高温高应力状态，而材料中含有的非碳成分粘结剂，其热膨胀系数、弹性模量与金刚石差别大，导致粘结剂与金刚石晶粒间存在明显的体积变化差异，进而在晶粒结合处产生高的应力，使得材料内部出现裂纹，影响使用寿命；另外，金属粘结剂的存在，会导致金刚石的高温石墨化。
聚(多)晶金刚石复合钻齿(Polycrystalline Diamond Cutter,PDC)是油气、采矿、地质钻探的关键工作部件，一般由多晶金刚石层(1mm-5mm，即工作层)及WC硬质合金基体在高温(～1200℃-1800℃)高压(5-8万大气压，1GPa约为一万大气压)下烧结复合而成。在2000m以上深井钻探中，油气钻头大多采用PDC钻齿对岩石进行切(刮)削钻进，具有高效、节能、可提高安全性及降低成本的优点，但对PDC钻齿的性能要求严格，相关技术已成为油气地质钻探的核心技术之一。油气钻探用高性能PDC复合钻齿的研发制备是一项高技术含量的系统工程，其PDC复合钻齿的性能是直接影响钻探效率、成本、安全性的关键要素。
聚晶金刚石是人造超硬复合材料的一种，目前国内外有两种途径制备聚晶金刚石：其一是利用静高压法或者爆轰法生产微、纳米金刚石粉体，再通过高温高压和粘合剂(或触媒/催化剂)作用下聚合生成聚晶金刚石，粘结剂的加入主要是为了降低高温高压烧结的温度压力条件，这是目前国内外通用的生产方法；另一种是利用爆炸法(激波法)直接生成聚晶金刚石颗粒，但上述聚晶金刚石颗粒的尺寸通常在0.1mm以内，且含有大量杂质，无法用于制作油气钻探用的钻齿(尺寸通常大于5mm)。
在高温高压条件下烧结的聚(多)晶金刚石材料(PCD/PDC)通常含有粘结剂，影响材料的硬度、耐磨性以及热稳定性。而在高温高压下不用任何非碳添加剂或触媒而制备的多晶金刚石材料，被视为合成高性能、高纯多晶金刚石材料的有效方法。现有的无非碳添加剂或触媒的合成技术如：爆轰法、激光加热合成法、静高压瞬间高温法以及在静高压下直接加热法等，其所制备的多晶金刚石材料均因质量或尺寸达不到要求，亦或者价格过高，未能用于制作油气钻探用的钻齿以及机械加工用刀具。国外具有大尺寸高纯聚晶金刚石合成技术的只有日本爱媛大学及日本住友公司，采用高纯石墨作为初始材料，在基于两面顶压机(单轴加载压机)上合成，温度压力条件为10-20GPa、1500-3000℃，材料性能优越，金刚石晶粒尺寸在20nm左右，但价格昂贵，目前只用于刀具制作，未有用于制作油气钻探用的钻齿。公开发表的文献中，无粘结剂多晶金刚石材料的制作，均采用非金刚石碳作为初始材料，且未见应用于制作油气钻探用的钻齿。
发明内容
本发明所要解决的技术问题是：采用传统的静高压法，需要添加非碳添加剂或触媒，会影响材料的硬度、耐磨性以及热稳定性；而采用传统的无非碳添加剂或触媒合成的多晶金刚石的颗粒尺寸较小，不适用于制作油气钻探用的钻齿，本发明提供了解决上述问题的一种无粘结剂多晶金刚石材料及其制备方法。
本发明通过下述技术方案实现：
一种无粘结剂多晶金刚石材料，制备原料包括50％～100％的金刚石微粉，0～50％的非金刚石碳粉；所述非金刚石碳包括石墨、无定型碳、碳纳米管、纳米洋葱碳、石墨烯、C60。
进一步地，以金刚石微粉作为原料合成获得无粘结剂多晶金刚石材料。
进一步地，所述金刚石微粉或非金刚石碳粉的晶粒尺寸为0.001μm～500μm；进一步优选，所述金刚石微粉或非金刚石碳粉的晶粒尺寸为0.1μm～300μm。
进一步地，所述无粘结剂多晶金刚石材料中，非碳成分杂质的含量低于1％。
进一步地，所述无粘结剂多晶金刚石材料成品的颗粒度大于1mm；进一步优选，所述无粘结剂多晶金刚石材料成品的颗粒度大于5mm。
上述的一种无粘结剂多晶金刚石材料的制备方法，以50％～100％的金刚石微粉和0～50％的非金刚石碳粉为原料经高温高压烧结制备获得无粘结剂多晶金刚石材料成品。
进一步地，制备温度为1200℃～3000℃，制备压力为8GPa～30GPa。
进一步地，制备温度为1500℃～2500℃，制备压力为10GPa～18GPa。
进一步地，所述高温高压烧结操作是在基于六面顶压机的二级六-八型大腔体静高压装置中进行。
将上述一种无粘结剂多晶金刚石材料、以及采用上述制备方法获得的无粘结剂多晶金刚石材料，应用于制作制备油气钻探钻头的钻齿、机械加工用的切削刀具、以及钻孔钻头与拉丝模。
本发明具有如下的优点和有益效果：
本发明提供了一种无粘结剂多晶金刚石材料，尤其适用于直接用作油、气(石油、天然气、叶岩气等的钻探开采)钻探用钻头钻齿的多晶金刚石工作层材料，主要特点为：不含传统多晶金刚石(PCD/PDC)材料中的粘结剂，直接由金刚石晶粒(晶粒尺寸：0.001μm～500μm，可采用单一粒度或混合粒度)在高温高压下(1200℃～3000℃、8GPa～30GPa)烧结而成，其非碳成分质量比低于1％，具有极高硬度、极高耐磨性及高热稳定性。
附图说明
此处所说明的附图用来提供对本发明实施例的进一步理解，构成本申请的一部分，并不构成对本发明实施例的限定。在附图中：
图1为本发明的无粘接剂多晶金刚石材料实物图；
图2为X射线衍射比对图谱；图中A表示目前工业上所用多晶金刚石材料(含钴)；B表示本发明无粘结剂多晶金刚石材料(实施例1制备)；C表示初始金刚石微粉；
图3为扫描电镜图；其中图(a)表示商用多晶金刚石材料，黑色颗粒为金刚石，白色区域为金属(Co)粘结剂；图(b)为本发明无粘结剂多晶金刚石材料(实施例1制备)，只含有金刚石；
图4为商用多晶金刚石材料的高温原位X射线图谱；
图5为本发明无粘结剂多晶金刚石材料的高温原位X射线图谱；
图6为耐磨性比对试验结果；图(a)表示本发明无粘结剂多晶金刚石材料(实施例1制备)的刃口磨损光学照片；图(b)表示商用多晶金刚石材料的刃口磨损光学照片。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明白，下面结合实施例和附图，对本发明作进一步的详细说明，本发明的示意性实施方式及其说明仅用于解释本发明，并不作为对本发明的限定。
实施例1
本实施例提供了一种无粘结剂多晶金刚石材料，通过以下方法制备获得：以100％的金刚石微粉为原料经高温高压烧结制备获得无粘结剂多晶金刚石材料成品。
金刚石微粉的晶粒尺寸为：5μm；
烧结温度为：2300℃；
烧结压力为：16GPa；
高温高压烧结操作是在基于六面顶压机的二级六-八型大腔体静高压装置中进行。
最终获得的无粘结剂多晶金刚石材料中，非碳成分杂质的含量为0.03％(低于1％)。无粘结剂多晶金刚石材料成品的颗粒度为10mm。
实施例2-14
实施例2-14分别提供无粘结剂多晶金刚石材料，均基于实施例1的技术方案获取无粘接剂多晶金刚石材料，各参数因素参见表1所示。最终获得的无粘结剂多晶金刚石材料中，非碳成分杂质的含量均低于1％。
一、性能测试条件：
高温原位烧结方法及条件：原材料经过混合、高温真空除杂、预压成型、组装后，进行高温高压烧结处理，然后再通过去除包裹、表面研磨抛光、激光切割等工序，即可得到成品多晶金刚石材料。
1、耐磨性试验方法及条件：本发明制备的无粘结剂多晶金刚石材料及商用多晶金刚石材料均加工成相同尺寸的圆柱体(直径为10mm，高5mm)，固定在数控车床的刀柄上，对花岗岩圆棒进行车削。车削参数为：线速度50-200m/min；切深0.1-0.5mm；进给0.1-0.5mm/r。切削相同里程(如：2000min)后，在光学显微镜下对刃口的磨损程度进行拍照、测量，比较计算磨耗比。
2、高温原位X射线衍射分析方法及条件：将待测样品置于高温X射线衍射仪样品平台上，在空气中于设定温度下进行X射线衍射谱采集，以观测样品在高温下的氧化、相变情况。
3、维氏硬度测量方法及条件：样品表面抛光成镜面，在维氏硬度计上进行硬度测量，采用金刚石单晶压头，加载力为5-50N，加载时间为15s，硬度值可在设备上直接读出，或者根据加载力及压头在样品表面的压痕面积计算得出。
二、性能测试结果：
(一)、针对实施例1制备的无粘结剂多晶金刚石材料性能表征结果如下：
1、如图3所示，为扫描电镜图；其中图(a)表示商用多晶金刚石材料，黑色颗粒为金刚石，白色区域为金属(Co)粘结剂；图(b)为本发明无粘结剂多晶金刚石材料(实施例1制备)，只含有金刚石；
2、如图4和5所示，图4所示的商用PDC/PCD材料在800℃左右即开始氧化，图5所示的本发明制备的无粘结剂多晶金刚石材料可稳定保持到1200℃。
3、如图6所示，为耐磨性对比试验，图(a)所示的本发明制备的无粘结剂多晶金刚石材料及图(b)所示的商用PCD/PDC材料在切削花岗岩(同一测试条件)后的刃口磨损照片。数据表明：本发明制备的无粘结剂多晶金刚石材料的耐磨性为商用PCD/PDC材料的3倍以上。
(二)实施例1-实施例14制备的无粘结剂多晶金刚石材料性能比较如下：
表1实施例1～实施例14制备的无粘结剂多晶金刚石材料性能测试结果
表1给出了制备参数对无粘结剂金刚石性能影响的一些典型数据，由表1数据可知(规律)：
1、原料晶粒尺寸对金刚石尺寸及性能的影响：原料的晶粒尺寸在0.001μm～500μm范围内，制备获得的无粘结剂多晶金刚石表现出优于常规多晶金刚石的耐磨性、高温稳定性及维氏硬度；但是，原料晶粒尺寸过大或过小，所制备的无粘结剂多晶金刚石材料中的金刚石含量转化率反而降低、性能反而减弱，且烧结后体积收缩过大，本发明提供的原料的晶粒尺寸存在优选范围0.5μm～300μm。
2、烧结温度和压力对金刚石尺寸及性能的影响：烧结温度过高或者烧结压力过低，会导致初始材料中的金刚石部分石墨化；烧结温度过低或者烧结压力过低，会导致初始材料中的非金刚石碳不能完全转化为金刚石；烧结压力过高，会导致样品变形量与残余应力大，在样品中产生裂纹。本发明提供的优选制备温度为1500℃～2500℃，制备压力为10GPa～18GPa。
以上所述的具体实施方式，对本发明的目的、技术方案和有益效果进行了进一步详细说明，所应理解的是，以上所述仅为本发明的具体实施方式而已，并不用于限定本发明的保护范围，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种无粘结剂多晶金刚石材料，其特征在于，制备原料包括50％～100％的金刚石微粉，0～50％的非金刚石碳粉；所述非金刚石碳包括石墨、无定型碳、碳纳米管、纳米洋葱碳、石墨烯、C60。
2.根据权利要求1所述的一种无粘结剂多晶金刚石材料，其特征在于，以金刚石微粉作为原料合成获得无粘结剂多晶金刚石材料。
3.根据权利要求1所述的一种无粘结剂多晶金刚石材料，其特征在于，所述金刚石微粉或非金刚石碳粉的晶粒尺寸为0.001μm～500μm。
4.根据权利要求1所述的一种无粘结剂多晶金刚石材料，其特征在于，所述无粘结剂多晶金刚石材料中，非碳成分杂质的含量低于1％。
5.根据权利要求1所述的一种无粘结剂多晶金刚石材料，其特征在于，所述无粘结剂多晶金刚石材料成品的颗粒度大于1mm。
6.权利要求1至5任一项所述的一种无粘结剂多晶金刚石材料的制备方法，其特征在于，以50％～100％的金刚石微粉和0～50％的非金刚石碳粉为原料经高温高压烧结制备获得无粘结剂多晶金刚石材料成品。
7.根据权利要求6所述的一种无粘结剂多晶金刚石材料的制备方法，其特征在于，制备温度为1200℃～3000℃，制备压力为8GPa～30GPa。
8.根据权利要求7所述的一种无粘结剂多晶金刚石材料的制备方法，其特征在于，制备温度为1500℃～2500℃，制备压力为10GPa～18GPa。
9.根据权利要求6所述的一种无粘结剂多晶金刚石材料的制备方法，其特征在于，所述高温高压烧结操作是在基于六面顶压机的二级六-八型大腔体静高压装置中进行。
10.权利要求1至5任一项所述的一种无粘结剂多晶金刚石材料、以及权利要求6至9任一项所述的制备方法获得的无粘结剂多晶金刚石材料，应用于制作制备油气钻探钻头的钻齿、机械加工用的切削刀具、以及钻孔钻头与拉丝模。
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| CN112158835A (zh) * | 2020-09-23 | 2021-01-01 | 吉林大学 | 一种具有超强硬度的碳材料的合成方法 |
| CN117088366A (zh) * | 2023-07-20 | 2023-11-21 | 郑州大学 | 厘米级超韧超导电超硬碳复合材料的制备方法 |
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