CN1485299A - 用于机械加工化学反应性材料的烧结坯 - Google Patents

用于机械加工化学反应性材料的烧结坯 Download PDF

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CN1485299A
CN1485299A CNA031487963A CN03148796A CN1485299A CN 1485299 A CN1485299 A CN 1485299A CN A031487963 A CNA031487963 A CN A031487963A CN 03148796 A CN03148796 A CN 03148796A CN 1485299 A CN1485299 A CN 1485299A
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base
nitride
carbide
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CN100509700C (zh
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S・L・多勒
S·L·多勒
斯库尔洛克
R·D·斯库尔洛克
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Ge Super Abrasives
Diamond Innovations Inc
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General Electric Co
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Abstract

一种用于刀具的立方氮化硼(cBN)坯，它包含下列组分：约60－80体积％体均颗粒尺寸为约3－6μm的cBN和约40－20体积％陶瓷粘结剂相。陶瓷粘结剂包含下列组分：约20－60体积％一种或多种IVB或VIB族金属的碳化物、氮化物或硼化物和约40－80体积％一种或多种铝的碳化物、氮化物、硼化物或氧化物。该cBN坯还含有约3－15重量％钨。这种cBN坯特别适用于机械加工铁之类的化学反应性零件，尤其当这类零件是粉冶金属零件时。

Description

用于机械加工化学反应性材料的烧结坯
与本申请相关的交叉参考
本申请要求2002年6月26日提交的美国临时申请系列号60/391707的优先权。
技术领域
本发明涉及切削、铣削和车削刀具，更具体地说，涉及提高立方氮化硼(cBN)超磨刀具的材料切削操作性能。
背景技术
以高压高温(HP/HT)制造cBN的方法是本领域内公知的，如美国专利2,947,617所述。美国专利4,188,194曾描述过一种用热解六方氮化硼(HBN)在没有任何催化剂存在下制造烧结多晶cBN坯的方法。美国专利4,289,503公开了对这一直接转化法的改进，在其中，要在转化工艺前先除去HBN粉末表面的氧化硼。
一个烧结坯是一定质量以自粘方式或通过粘结剂介质或通过两者的组合方式粘结在一起的磨粒。复合材料坯是一种粘结到烧结金属碳化物之类基材上的坯。美国专利3,918,219提出，六方氮化硼(HBN)在与碳化物接触中催化转化成cBN，从而形成复合材料cBN坯。坯或复合材料坯能用于切削工具、钻头、整修工具和耐磨零件的坯。
多晶cBN坯常用来机械加工硬铁合金工件。刀具硬度和力学性能必须与刀具的反应性相平衡。高cBN含量的坯具有最高的硬度，但是，一般而言，它们对合金钢是反应性的。为保证应用性，常常加入非反应相以保护cBN免与含铁合金发生反应。
已有许多文献提出了从立方氮化硼(cBN)和过渡金属氮化物或碳化物制成高压高温烧结体用的各种组合物。
美国专利4,334,928描述的烧结体合20-80体积％cBN和一个粘结剂相，粘结剂相由周期表中IV和V族金属的碳化物、氮化物、碳-氮化物、硅化物或硼化物组成。也包括在粘结剂相中加入铝。加进混合物的Ti化合物优选具有化学计量，从而使通式Ti(X)z中的“z”值小于0.97，其中“X”是碳或氮或两者的组合。美国专利4,343,651描述了材料中含80-95体积％立方氮化硼的烧结体。
美国专利4,911,756描述了由一种含50-75体积％cBN和25-50体积％粘结剂相的烧结混合物制成的烧结体。该粘结剂相由20-50重量％Al或Al化合物、周期表中IV、V和VI族金属(包括Ti和W)的碳化物、氮化物、碳-氮化物、硅化物或硼化物组成，其中加入的Ti化合物规定为化学计量，从而使通式Ti(X)z中的z值在0.5-0.85范围内，其中“X”是碳或氮或两者的组合。
美国专利5,092,920描述了含45-60体积％平均颗粒尺寸等于或小于2μm的cBN和一个粘结剂相的烧结体，粘结剂相包含5-15重量％铝、2-20重量％钨，其余是以上提到的任何Ti化合物，其中Ti化合物的化学计量要使通式Ti(X)z中的z值在0.45-0.65范围内，其中“X”是碳或氮或两者的组合。
美国专利6,316,094描述了包含45-70体积％颗粒尺寸为2-6μm的cBN和一个二维连续粘结相的烧结体，粘结相包含至少一种下列化合物：IVB、VB或VIB族过渡金属(包括Ti和W)的碳化物、氮化物、碳-氮化合物或硼化物、铝的氮化物、硼化物或氧化物，铁、钴或镍的碳化物、氮化物、碳-氮化物或硼化物，及它们的固溶体。还规定粘结剂相的平均厚度要等于或小于1.5μm，标准偏差等于或小于0.9μm。
因此，尽管已经以上述方法实现了改进，但对于拟机械加工的各化学类合金材料，仍需要一种优化产品。这样就要在这类cBN机械加工产品成本中增加开发成本和生产线投资成本。申请人已经发现了一种用于改进机械加工性能的优化的烧结坯组合物，含有钨化合物和体均颗粒尺寸大于2μm的cBN颗粒。
发明内容
本发明的烧结坯由高压高温条件下烧结一种约60-80体积％体均颗粒尺寸为3-6μm的立方氮化硼(cBN)、约20-40体积％陶瓷粘结剂相以及约3-15重量％钨的混合物获得；其中粘结剂相的组成为：20-60体积％一种或多种周期表中IVB与VIB族金属的碳化物、氮化物或硼化物和约40-80体积％一种或多种铝的碳化物、氮化物、硼化物或氧化物。以碳化物或硼化物形式的其它铁族金属，也可作为工艺中引进的杂质存在。
本发明还涉及成形包含cBN坯的刀具，该cBN坯含一种组分如下的混合物：约60-80体积％体均颗粒尺寸为3-6μm的立方氮化硼(cBN)与约20-40体积％陶瓷粘结剂相和约3-15重量％钨。
附图简述
图1是示意本发明烧结cBN坯的一个实施方案中机械加工性能与W含量关系的曲线。
发明详述
新颖的cBN坯特别适用于成型刀具，例如用于工件机械加工的刀具。其中特别要提及的是在本发明的一个实施方案中本发明的cBN坯在机械加工化学反应性材料中的应用。
所谓“化学反应性材料”是指会与刀具材料发生化学反应的材料，例如在高温下与金刚石刀具发生反应的含铁工件。更重要的是，本发明的烧结cBN坯能机械加工粉冶金属零件，即由凝固或致密化形成工件或零件的粉末金属制成的零件，特别是用粉冶工艺从铁粉致密化形成的零件。
本发明的烧结cBN坯在机械加工化学反应性材料，例如，粉冶金属铁方面表现出优良的性能。特别是，本发明的cBN烧结坯擅长于机械加工粉冶金属零件(由金属粉末的凝固制成的零件)，例如目前在汽车工业中普遍的齿轮、阀座等。与本发明cBN烧结坯相关的量度是刀具的使用寿命，由机械加工金属的表面光洁度变成不合格之前所能完成的机械加工量确定。本发明的cBN烧结坯已经过试验并在一个实施方案中可以看到，其性能比商品坯的好2-1倍以上。
在制造本发明的烧结cBN坯时，原料粉末可研磨到所要求的颗粒尺寸并用多种技术混合，包括，例如超声混合、球磨混合、碾磨混合等。由所选混合技术产生的明显影响是加入了来自金属球的金属(例如来自于钨介质的钨)。混合物中可能加进无意加入的金属或其它介质，这一点可能是不希望的。或者也可用这种技术在原料混合物中引进所需的材料。例如，由于钨是最终原料混合物中所需的，因此可以选择用钨介质研磨以加入钨的技术来引进至少一部分钨量。
研磨常在有乙醇、丙酮之类易除去且不会促进研磨中金属粉末发生不希望的氧化的溶剂存在下进行。这种研磨通常不会把粉末氧化到任何不希望的程度。研磨温度将是室温，时间可以在数小时范围内。按比例调节球磨设备的尺寸，能制造100g-2kg或更大量的共混混合物。
然后在低于溶剂闪点的温度下烘干共混混合物以除去溶剂(例如，异丙醇，丙酮)。然后将烘干的粉末在干态下稍加研磨，方法是将一定量适当尺寸的粉末置于含同样量WC或其它研磨介质粉末的瓶中，然后在瓶内翻滚。然后让粉末过筛到一定尺寸。共混材料的组成可以调整到各组分的相对含量保持在所需的范围内。
这时粉末已准备好用传统的HP/HT技术和本领域内熟知的设备，如以上所述的设备进行烧结。扼要地说，将粉末装进耐火金属(例如钽或铌)杯中。杯的大小限制最终烧结坯的尺寸。如本领域所知，在杯内装进一种支持材料(粉末或坯)以便与烧结cBN坯原位粘结在一起。适用的基体包括，例如，耐火金属(例如W)碳化物。压扁基体周边的杯材料密封该杯。
然后将此精制坯装进一个由压力传递与压力密封材料组成的高压盒，然后在高压(例如45-50千巴)和高温(约1400℃)下处理30-40分钟，以烧结该粉末混合物并将其钎焊进基体。从盒内取出烧结坯并进行机械加工，以除去杯材并使之达到所需尺寸。该精制坯的导电性足以用放电加工(EDM)法将其加工成适合于制造用来机械加工粉末金属铁和其它类似材料的刀具的形状和尺寸。所述烧结坯的尺寸与形状可通过改变部件尺寸而变化，而且其尺寸主要受用来促进烧结过程的高压/高温(HP/HT)设备的限制。该烧结好的cBN坯产品包含约60-80体积％颗粒平均尺寸约3-6μm的cBN，其余材料由均匀分散在cBN颗粒之间且含化学计量的碳化物、氮化物或硼化物的粘结剂相组成。
在本发明的一个实施方案中，粘结剂相含几个能用X-射线衍射技术鉴定的相，包括，例如，氮化铝、碳化钛、氮化钛、硼化钛、碳化钨、硼化钨和一种钨、硼和钴的化合物。这些相是在烧结期间由共混粉末组分反应而成的。
烧结cBN坯产品还包含约3-15重量％钨。钨含量较高时，cBN坯仍将表现出良好的机械加工性能，但可能在机械加工操作期间有碎裂的倾向。其原因是在高压/高温烧结操作期间形成了硼化钨(WB)相。WB相的形成会抑制二硼化钛(TiB2)相的形成，正如由最终产品的X-射线衍射所观察。
相信在本发明的一个实施方案中，在烧结期间会形成足够量的二硼化钛相，以提供最佳材料。因此较高钨含量带来一些害处，因为这会增加机械加工操作期间刀具材料碎裂的几率。在本发明的一个实施方案中，W含量范围为约3-8重量％。烧结cBN坯产品中的钨含量可以用X-射线衍射法测定。由硼化钨相(110)晶面产生的衍射峰强度可以与由二硼化钛相(100)晶面产生的衍射峰强度比较。二硼化钛峰与硼化钨峰的强度之比为约2∶1或更大。
然后可将烧结cBN坯成型为机械加工粉冶金属铁之类化学反应性材料的刀具。这类刀具的成形和所用的机械加工条件是本领域熟知且已应用于工业的。
虽然本发明已参考一个优选实施方案作了描述，但本领域的专业人员会理解，可以作许多变更，也可以用等同物取代而不会偏离本发明的范围。此外，还可以作许多修改以使特定情况或材料适应于本发明的原则而不偏离其基本范围。因此无意将本发明限制在以公开的具体实施方案作为实施本发明预期的最佳模式，而有意要使本发明包括所有落在所附权利要求范围内的实施方案。在本申请中所有的单位都用公制，所有的量和百分数都指重量，除非另有明确说明。同时所有引用的参考文献都明确包括于此供参考。
具体实施方式
实施例  在实施例中，标准化机械加工试验用铁粉冶零件(Z82，Keystone Powder Metal，St.Marys，PA 15857)进行。这种铁粉冶金属零件含不同量的Al、Cr、Co、Cu、Mn、Ni、Si和Ti。标准化试验步骤采用下列条件：
                      表1
材料    Z82P/M Exhaust洛氏B硬度＝82
工件速度    1000 SFM(300米/分钟)
进刀速度    0.004ipr(0.10mm/转)
吃刀深度    0.008英寸(0.20mm)
Vb Max    0.01英寸(0.25mm)
试验测量(3副刀具平均值)    机械加工等同零件的数目(EPM)
对比实施例1  用一个商品cBN坯(BZN 6000，90体积％cBN，10体积％陶瓷和金属相，GE Superabrasives，Worthington，OH)进行标准化机械加工试验。该材料以130 EPM试验。该商品的cBN含量超过了确定为适用于本发明cBN烧结坯的含量。
对比实施例2  用一个商品cBN坯(BZN 8200，65体积％cBN，33体积％化学计量TiNx(其中x＜0.97)和2体积％AIN，GESuperabrasives，Worthington，OH)进行标准化加工试验。该材料以120EPM试验。应注意TiN中N的化学计量含量＜1。
实施例3  将平均颗粒尺寸小于约2.5μm的铝化钛(TiAl3)粉、平均颗料尺寸小于3μm的碳化钛(TiC)粉与平均颗粒尺寸约4-5μm的cBN粉共混成组成如下的混合物：约77重量％cBN、15重量％TiAl3和8重量％TiC。用传统的WC研磨介质(直径0.25μm)并以异丙醇(IPA)为研磨液球磨该混合物4小时。该研磨操作把最终粉末混合物中的WC含量提高到约5重量％。
在低于醇的闪点的温度下烘干该共混物以除去醇。在干态下稍稍研磨该干燥粉末，方法是将一定量的粉末置于适当尺寸的塑料瓶内，瓶中装有重量与粉末重量相等的WC研磨介质，然后在瓶内翻滚30分钟。接着让该粉末过20目筛。将该加工好的粉末混合物装进耐火金属杯并盖上碳化钨基体。然后将该杯组件装进一个由压力传递与压力密封材料组成的高压盒，并使之在高压(40-50千巴)和高温(1400℃)下处理30-40分钟，以烧结该粉末混合物并钎焊到碳化钨基体上。
在该实施例中，烧结粉末中有约75体积％颗粒平均尺寸约4-5μm的cBN颗粒，其余材料为均匀分散在cBN颗料间的粘结剂相。粘结剂相含几个相，据X-射线衍射鉴定，包括氮化铝、碳化钛、氮化钛、硼化钛、碳化钨和一种钨、硼和钴的化合物。这些相在烧结工艺期间由共混粉末组分反应而成。根据加进烧结混合物的粉末重量％和由XRD观察到的反应产物，烧结坯中的粘结剂相含约60体积％铝化合物(主要是氮化物与硼化物)和约40体积％的钛化合物(主要是碳化物与硼化物)。
机械加工该烧结坯以除去杯材料并达到所要求的尺寸(厚3.2mm、直径59mm)。该精加工坯的电导性足以使它能用放电加工(EDM)法切削成适合于制造用来机械加工粉冶金属铁和其它类似材料的刀具的形状与尺寸。该类cBN烧结坯用标准化机械加工试验法进行试验，结果如下。
                                                   表2
  次数     组成(重量)        研磨   cBN(μm)   EPM(平均)
   TiN   TiC   TiAl3    WC   类型   溶剂
    6     0   8.16   14.72   1.97   球磨   丙酮   4.5   278.7
    15     0   8.16   14.72   1.97   球磨   IPA   4.5   274.3
该结果表明本发明的烧结cBN坯具有优良性能，而且溶剂类型对烧结cBN坯的机械加工性能无重要影响。
实施例4  按实施例1中所述的方法制造另一个颗粒尺寸不同的，即cBN颗料尺寸为3.0μm的cBN烧结坯，并用标准化机械加工试验法进行试验。记录的结果如下。
                                    表3
次数                 组成(重量)     研磨类型   cBN(μm)   EPM(平均)
  TiN   TiC   TiAl3     WC
  1    0   8.16   14.72     1.97     球磨   3.0   248.8
这些结果表明仅减小cBN的颗粒尺寸就使其性能从276.5EPM(实施例3)降到248.8EPM。
实施例5  用TiN代替TiC的配方，按实施例1中所述的方法制造另一个cBN烧结坯，并用标准化机械加工试验法进行试验，结果如下。
                              表4
次数              组成(重量) 研磨类型 cBN(μm)   EPM(平均)
  TiN   TiC   TiAl3     WC
17     4     0     19     0 碾磨  4.5   234.9
这些结果表明仅用TiN取代TiC就使性能下降。
实施例6  按实施例1中所述的方法制造另一个cBN烧结坯并用标准化机械加工试验法进行试验，TiN在烧结期间转化为TiC，如X-射线衍射分析测定，结果如下。
                                  表5
次数                      组成(重量) 研磨类型 cBN(μm) EPM(平均)*
    TiN     TiC   TiAl3   WC
 23     9.43     0   12.65   1.97 碾磨  45 269.9
再次表明，性能因烧结cBN坯中存在TiC而得已提高。
实施例7  按实施例1中所述的方法制造另一个cBN烧结坯并用标准化机械加工试验法进行试验，与实施例6的差别在于使用了碾磨而非球磨。记录结果如下。
                                    表6
次数                  组成(重量) 研磨类型 cBN(μm)   EPM(平均)*
  TiN   TiC   TiAl3   WC
  9   0   8.16   14.72   1.97 碾磨 4.5   250.7
与实施例3相比，性能的下降(278.7EPM对250.7EPM)可归因于以下事实：与球磨相比，采用碾磨会造成配方中加入的WC量较少。也证明配方中存在WC的重要性。
实施例8  用TiN、TiC、TiAl3从前述实施例中所列的组分配制另一个烧结cBN坯。改变W(以WC供料)的量以确定W对机械加工性能的影响，对于尺寸为3-6μm的cBN颗粒，记录结果如下，同时也示于图1。
                表7
    ％W  EPM(平均)
    1.31     234.9
    3.4     268.9
    3.6     250.7
    3.76     262.2
    5.28     278.7
    6.04     274.3
    10.4     252.0
    11.1     269.9
    12.44     246.4
    13.56     258.8
    16.72     256.2
    17.86     247.7
这些数据表明机械加工性能(用机械加工粉冶金属，PM，铁零件测定)在5重量％W时最高，以及对于含约3-15重量％W的烧结cBN坯，可获得合格的机械加工性能。
实施例9  WC含量不同的其它cBN烧结坯，按实施例1所述的方法制造并用更严格的标准化机械加工试验法(工件的洛氏B硬度＝95)进行试验。分别用ICP(电感耦合等离子体)和XRD(X-射线衍射)法分析这些粉末共混样品和烧结坯中的W含量。烧结坯中W的相对含量用[101]TiB2峰对[110]WB峰的XRD强度之比确定，这些数据示于表8。
                         表8
坯名   [101]TiB2峰相对XRD强度   [110]WB峰相对XRD强度 ICP％W   WB/TiB2XRD强度比
  A   49％   6％   6.5％   0.12
  B   46％   10％   6.5％   0.22
  C   51％   0％   5.0％   0.00
  D   47％   0％   5.0％   0.00
  E   48％   0％   5.0％   0.00
  F   47％   6％   4.0％   0.12
  G   50％   0％   4.0％   0.00
  H   50％   4％   4.2％   0.08
  I   49％   0％   4.0％   0.00
  J   46％   5％   4.4％   0.10
  K   39％   32％   10.7％   0.81
  L   39％   33％   10.3％   0.85
  M   39％   34％   10.5％   0.89
  N   50％   30％   10.6％   0.61
  O   38％   32％   9.0％   0.85
  P   34％   35％   8.8％   1.04
  Q   36％   20％   8.7％   0.55
可以看到这些样品可分为两组：W含量＜8重量％和XRD强度之比WB/TiB2＜0.4(样品A-J)的为一组；W含量＞8重量％和XRD强度比WB/TiB2＞0.4(样品K-Q)的为另一组。当由这两组制成的刀具经受更严格的标准PM机械加工试验时，由XRD强度之比WB/TiB2＞0.4(样品K-Q)的一组制成的刀具在13次试验中有13次都因突然碎裂而失败，而XRD强度之比WB/TiB2＜0.4的一组在25次试验中仅失败17次。
这些数据表明当W含量低于约8重量％和XRD强度比WB/TiB2＜0.4时，在机械加工较硬的工件时，烧结坯碎裂的倾向有所减少。

Claims (18)

1.一种用于切削工具的烧结立方氮化硼(cBN)坯，它包含：
(a)约60-80体积％体均颗粒尺寸为约3-6μm的cBN；
(b)约40-20体积％陶瓷粘结剂相，其中有
(i)约20-60体积％一种或多种IVB或VI B族金属的碳化物、氮化物或硼化物；
(ii)约40-80体积％一种或多种铝的碳化物、氮化物、硼化物或氧化物；
(c)约3-15重量％钨。
2.权利要求1的烧结cBN坯，其中陶瓷粘结剂相(b)(i)主要是碳化钛。
3.权利要求1的烧结cBN坯，其中钨含量约为3-8重量％。
4.权利要求1的烧结cBN坯，其中所述陶瓷粘结剂相包括TiB2，TiB2可用XRD检测到。
5.权利要求4的烧结cBN坯，它含有WB，其中TiB2[101]峰与WB[110]峰的XRD强度之比小于约0.4。
6.制造用于刀具的烧结立方氮化硼(cBN)坯的方法，该方法包含使下述混合物经受高压和高温(HP/HT)条件：
(a)约60-80体积％体均颗粒尺寸为约3-6μm的cBN；
(b)约40-20体积％陶瓷粘结剂相，其中有
(i)约20-60体积％一种或多种IVB或VIB族金属的碳化物、氮化物或硼化物；
(ii)约40-80体积％一种或多种铝的碳化物、氮化物、硼化物或氧化物；
(c)约3-15重量％钨。
7.权利要求6的方法，其中所述HP/HT条件包括在约45-50千巴压力和约1400℃温度下处理约30-40分钟。
8.权利要求6的方法，其中，所述陶瓷粘结剂相(b)(i)主要是碳化钛。
9.权利要求6的方法，其中钨含量为约3-8重量％。
10.权利要求6的方法，其中所述陶瓷粘结剂相包括TiB2，TiB2可用XRD检测到。
11.权利要求10的方法，它含WB，其中TiB2[101]峰与WB[110]峰的XRD强度之比小于约0.4。
12.机械加工化学反应性材料的方法，它包含下列步骤：
让所述材料接触一个烧结立方氮化硼(cBN)坯，以除去至少一部分所述材料，所述cBN坯包含：
(a)约60-80体积％体均颗粒尺寸为约3-6μm的cBN；
(b)约40-20体积％陶瓷粘结剂相，其中有
(i)约20-60体积％一种或多种IVB或VIB族金属的碳化物、氮化物或硼化物；
(ii)约40-80体积％一种或多种铝的碳化物、氮化物、硼化物或氧化物；
(c)约3-15重量％钨。
13.权利要求12的方法，其中所述化学反应性材料包含一种含铁工件。
14.权利要求12的方法，其中陶瓷粘结剂相(b)(i)主要是碳化钛。
15.权利要求12的方法，其中钨含量为约3-8重量％。
16.权利要求12的方法，其中所述陶瓷粘结剂相包括TiB2，TiB2可用XRD检测到。
17.权利要求16的方法，它包含WB，其中TiB2[101]峰与WB[110]峰的XRD强度之比小于约0.4。
18.一种包含权利要求1的cBN坯的制品，其形式为切削工具、钻头或整形工具。
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