CN1078875C - 具有高疲劳寿命的氮化硅轴承球 - Google Patents

具有高疲劳寿命的氮化硅轴承球 Download PDF

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CN1078875C
CN1078875C CN95192160A CN95192160A CN1078875C CN 1078875 C CN1078875 C CN 1078875C CN 95192160 A CN95192160 A CN 95192160A CN 95192160 A CN95192160 A CN 95192160A CN 1078875 C CN1078875 C CN 1078875C
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silicon nitride
bearing ball
weight
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sintered silicon
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R·L·耶克利
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Saint Gobain Ceramics and Plastics Inc
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16C—SHAFTS; FLEXIBLE SHAFTS; ELEMENTS OR CRANKSHAFT MECHANISMS; ROTARY BODIES OTHER THAN GEARING ELEMENTS; BEARINGS
    • F16C33/00—Parts of bearings; Special methods for making bearings or parts thereof
    • F16C33/30—Parts of ball or roller bearings
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—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
    • C04B35/58—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • C04B35/593—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 borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride obtained by pressure sintering

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Ceramic Products (AREA)
  • Rolling Contact Bearings (AREA)

Abstract

公开了一种轴承球，它基本上含有；a)轴承球至少94重量%是氮化硅晶相，和b)主要由Mg，Al，Si和O构成的单一颗粒边界相，其中，颗粒边界相基本上由下列物质构成：轴承球的1-2重量%是Mg，以氧化镁状；轴承球的0.2-1.0重量%是Al；以氧化铝状：和轴承球的2-4重量%是Si，以氧化硅状；以及氧，并且用ASTM测试方法STP771，在6.9GPa接触应力下进行测试，其L10值至少为50百万应力周。

Description

具有高疲劳寿命的氮化硅轴承球
新颖结构的陶瓷材料因其优异的性能质量而引起了工业界的注意。这些性能，如优异的高温强度、高刚性、耐热冲击和耐氧化性，为它们在多种应用中的潜在用途奠定了基础。
美国专利No.4,935,388(Lucek)指出，陶瓷材料的可靠性与其空间同质性相关，而这种同质性以材料展现的光学异常程度为特征。Lucek特别指出，当材料具有空间同质性时，氮化硅的可靠性会大大提高，例如大于约70微米就没有光学异常现象。Lucek提出，上述光学异常预示了许多种不同质的现象，其中包括(但并不限于)多孔区域、被铁等材料污染的区域和具有微小裂缝的区域。Lucek公开的氮化硅陶瓷含有约1重量％氧化镁作为烧结助剂，其滚动接触疲劳寿命(roll contact fatigue life，简称“RCF寿命”)用L10值表示时，(用ASTM测试方法STP 771进行测试，6.9GPa接触应力)至少为4百万个应力周。尽管该RCF寿命是已知最高中的一个，但是商业上仍需要RCF寿命进一步提高的碳化硅材料。
因此，本发明的目的是提高一种具有优异RCF寿命的氮化硅材料。
发明概述
根据本发明，提供了一种轴承球，它基本上含有：
a)至少约94重量％的晶相氮化硅，和
b)主要由Mg，Al，Si和O构成的单一颗粒边界相。
并且用ASTM测试方法STP 771，在6.9GPa接触应力下进行测试时，其L10值至少为50百万应力周。较佳地，其L10值至少为60百万周。更佳地，其L10值至少为70百万周。
在优选例子中，颗粒边界相基本上由下列物质构成：1-2重量％Mg，以氧化镁状；0.21.0重量％Al，以氧化铝状；和2-4重量％Si，以氧化硅状；以及氧。更佳地，颗粒边界相的Mg组份为轴承的1.0-1.6重量％，以氧化镁状；颗粒边界相的Al组份为0.3-0.6重量％，以氧化铝状；颗粒边界相的Si组份为2.0-3.0重量％，以氧化硅状。在特别优选的例子中，轴承用ASTM测试方法STP771，6.9GPa接触应力下进行测试，其L1O值为50-80百万应力周。
此外，在优选例中，本发明轴承球的挠曲强度至少为950MPa。
发明详细描述
出乎意料地发现，向基本由氮化硅和约1重量％氧化镁构成的坯体(greenbody)添加约0.20-1.0重量％的氧化铝，获得了RCF寿命非常高的陶瓷。
为了不受某一具体理论的束缚，据信，在Lucek的常规氮化硅陶瓷的烧结过程中，氧化镁烧结助剂和3重量％氧化硅(以杂质形式存在于氮化硅粉末中)在平衡时形成至少两种不可混和的液相，从而在烧结体内形成至少两种颗粒边界相。这种非均一的颗粒边界相可能降低了陶瓷的强度、刚性和RCF寿命。根据相图，在本发明中添加氧化铝据信可在平衡时生成单一的MgO-SiO2-Al2O3相。因此能获得更好的均匀性和更高的性能。
本发明的氮化硅陶瓷可用常规材料和常规的加工方法制造。在优选例子中，陶瓷是用氮化硅粉末或其初始粉末制造的。如果陶瓷是用氮化硅粉末制造的，那么可以使用任何一种常规的氮化硅粉末。典型地，氮化硅占本发明陶瓷的至少约94重量％，更佳为约97-98.5重量％。
在本发明的优选例子中，氧化镁和氧化铝被用作烧结助剂。氧化镁的添加量为烧结陶瓷的约1.0-2.0重量％，较佳为约1.0-1.6重量％。最佳地，使用约1重量％，纯度大于99％，平均颗粒大小小于1微米的氧化镁。类似地，氧化铝的添加量为烧结陶瓷的约0.20-1.0重量％，较佳为约0.4-0.6重量％。最佳地，使用约0.47重量％，纯度大于99％，平均颗粒大小小于1微米的氧化镁。
氧化硅可以杂质形式存在于原料氮化硅粉末中。最后，硅以氧化硅状态存在于烧结陶瓷的颗粒边界相中，含量约为陶瓷的2-4重量％，较佳为2-3重量％。
氮化硅和烧结助剂粉末可用任何已知的混合方法进行混合，其中包括(但并不限于)球磨或碾磨法。在本发明的优选例中，优选振磨法(vibratory milling)。
如果形成坯体，那么可用本领域中任何典型方法进行。这些方法包括粉浆浇注、压模、冷冻铸模、和冷等静压。在本发明的优选例中，本发明的粉末是用冷等静加压法。
本发明的烧结周期可包括任何常规的烧结方法，包括无压烧结、气体压力烧结、热模压和使用玻璃的热等静压法(“玻璃密封热等静压法”)。在本发明的优选例中，使用美国专利No.4,446,100和4,339,271中所述的玻璃密封热等静压法。更优选的是在非常高的填充效率时(即各部件相互接触)使用美国专利No.4,446,100和4,339,271的例子。
实施例I
将具有下列性能的氮化硅粉末用作该实施例的粉末：大于约90重量％αSi3N4，小于约2.0重量％总氧，小于0.1重量％钙，约0.03重量％铁，约0.05重量％铝和约5-9平方米/克的表面积。
将约98重量份数的这种粉末与约1.33重量份数的试剂级的碳酸镁和约0.47重量份数氧化铝和异丙醇混合，形成含45％固体的浆料。浆料在振动式研磨机中与氮化硅研磨介质一起同时进行共混和研磨。最终的表面积为约10-14平方米/克。得到的浆料通过20微米的筛网和磁性分离器。浆料通过横向过滤被浓缩至含65％固体。接着，向浆料中加入占粉末约1.25重量％的PVP(聚乙烯吡咯烷酮)。接着，浆料在防爆喷射干燥器中干燥。干燥的粉末再通过30目的nalgene筛网。所有上述操作都是在一个1000级的用于氮化硅加工的清洁室中进行的。干燥的结块粉末在30ksi下用冷等静压法压成圆柱体并磨成直径约0.52英寸、长约3.8英寸的小棒。粉末压缩物在600℃下燃烧以去除PVP。样品被密封在玻璃介质中，在约1790℃，30,000psi压力下热等静压约1小时。
实施例II和III
基本上相同地重复上述过程，除了生产3/4英寸的球体和3×4×50毫米的曲率棒。
测量形成的陶瓷的硬度。10千克负荷时产生了维氏金刚石棱锥硬度缺口。平均硬度为约15.2GPa。作为比较，Norton Company(Worcester，MA)生产的含1重量％氧化镁的氮化硅轴承材料的硬度为约15-15.6GPa。
断裂刚性是通过测量在内径的拉力表面上带有维氏缺口(10千克负荷)的3×4×50毫米的4点弯曲样品在十字头速度约为0.5毫米/分钟时的断裂情况加以确定的，根据P.Chant ikul等人在“a Critical Evaluation of IndentationTechniques for Measuring Fracture ToughnessII：Strength Menthods”，J.Am.Ceram.Soc.64(9)，pp.539-544(1981)中所述的程序进行。本发明陶瓷的平均刚性为约5.6MPa M1/2。作为对比，NBD-200的断裂刚性为约5-5.8MPa M1/2。
还测量了本发明陶瓷的4点挠曲强度。选择3×4×50毫米的B型样品在外径40毫米、内径20毫米的测试夹具(ASTM C1161-90)进行测试。测得的平均挠曲强度为约950MPa。作为对比，NBD-200的挠曲强度为约700-850MPa。
还用ASCERA拉伸强度测试程序分析拉伸强度。该程序可参见Brit.Ceram.Trans J.，89，21-23，1990。本发明的拉伸强度为约475MPa。作为对比，NBD-200的拉伸强度为约400 MPa。
还测试了在实施例II中制备的棒的滚动接触疲劳(RCF)寿命，具体地用ASTM-STP771中所述的加速轴承测试程序。该测试程序中施加的接触压力比常规遇到的压力为大，从而加速测试材料的疲劳损伤。该测试对许多测试样品的数据进行统计分析，结果一般用变量Lx表示，它表示在给定应力水平下导致X百分比的被测试样品损伤的应力周期的数目。在对本发明进行RCF测试时，装入3个用AISI52100不锈钢制成的从动球(slave ball)碰撞本发明的氮化硅棒，施加约6.9GPa的平均接触应力。棒用电动机以约3600rpm的速度进行旋转。从动球和棒两者都通过滴加器以每分钟滴加约8滴润滑油的速度而得以润滑。测试在棒上产生了约0.1英寸宽的外周疲劳裂纹。本发明的氮化硅表现出通常的断裂模式和均匀的磨损。在24根用于RCF测试的本发明的棒中，第一根断裂的棒在约5400万周时发生断裂。如果假设维泊尔斜率为0.74(即假设本发明的断裂机制与NBD-200相同。)，那么本发明的L10达到8000万周左右。作为对比，NBD-200的L10寿命为400万周。
以实施例I-III为代表性例子的本发明的机械性能总结于表1，表中还列出了作为对比的氮化硅陶瓷NBD-200。
                      表1
       性能     实施例I-III     NBD-200
L10 RCF寿命(周)     80,000,000     4,000,000
拉伸强度(MPa)     475     400
挠曲强度(MPa)     950     ＜850
断裂刚性(MPa m1/2)     5.6     ＜5.8
硬度(GPa)     15.2     ＜15.6
本发明的氮化硅可用于多种常规的陶瓷应用场合，其中包括(但并不限于)：轴承球、滚动轴承、平面滑动轴承和其它结构或磨损件。

Claims (6)

1.一种烧结氮化硅轴承球，它基本上含有：
a)轴承球至少94重量％是氮化硅晶相，和
b)主要由Mg，Al，Si和O构成的单一颗粒边界相，其中，颗粒边界相基本上由下列物质构成：轴承球的1-2重量％是Mg，以氧化镁状；轴承球的0.2-1.O重量％是Al，以氧化铝状；和轴承球的2-4重量％是Si，以氧化硅状；以及氧，
用ASTM测试方法STP 771，在6.9GPa接触应力下进行测试，其L10值至少为50百万应力周。
2.如权利要求1所述的烧结氮化硅轴承球，颗粒边界相的Al组份为轴承球的0.3-0.6重量％，以氧化铝状。
3.如权利要求1所述的烧结氮化硅轴承球，颗粒边界相的Si组份为轴承球的2.0-3.0重量％，以氧化硅状。
4.如权利要求1所述的烧结氮化硅轴承球，其Ll0值至少为60百万周。
5.如权利要求1所述的烧结氮化硅轴承球，其L10值至少为70百万周。
6.如权利要求1所述的烧结氮化硅轴承球，其挠曲强度至少为950MPa。
CN95192160A 1994-03-22 1995-03-17 具有高疲劳寿命的氮化硅轴承球 Expired - Fee Related CN1078875C (zh)

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US08/215,834 US5508241A (en) 1994-03-22 1994-03-22 Silicon nitride bearing ball having a high rolling contact fatigue life
US08/215,834 1994-03-22

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