CN102272074B - 大型陶瓷部件及其制造方法 - Google Patents

大型陶瓷部件及其制造方法 Download PDF

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CN102272074B
CN102272074B CN200880130909.1A CN200880130909A CN102272074B CN 102272074 B CN102272074 B CN 102272074B CN 200880130909 A CN200880130909 A CN 200880130909A CN 102272074 B CN102272074 B CN 102272074B
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sintering
ceramic
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parts
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CN102272074A (zh
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沈志坚
赛义德·埃斯马艾尔扎德
卡塔琳娜·弗洛德斯特罗姆
夏洛特·维拉尔德
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Diamorph AB
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Abstract

本发明涉及适宜用作轴承中的滚动构件的氮化硅或塞隆的烧结的陶瓷部件和制造所述陶瓷部件的制造方法。所述陶瓷部件具有高密度和均匀的精细微结构，使得所述部件具有优异的机械性质。通过SPS制造烧结的陶瓷部件具有成本效益并且快速。

Description

大型陶瓷部件及其制造方法
技术领域
本发明涉及诸如滚动轴承构件等大型烧结陶瓷部件及其制造方法。
背景技术
在需要诸如高硬度、优异的高温行为、耐高热冲击性、低密度和高电绝缘能力等性质的应用中，使用烧结的陶瓷部件来代替金属部分。
一些应用极为需要例如其中滚动构件与环之间的接触部分要经受很高的局部应力的滚动轴承等部件。该接触部分也暴露于各种润滑、污染和温度条件。可靠的性能和长的使用寿命是至关重要的。所谓的混合轴承由陶瓷滚动构件和钢基环与钢、塑料或黄铜类保持架构成。混合轴承已经在某些操作情况下显示出了有利之处，所述条件例如有高旋转速度、缺乏润滑或润滑不良的情况、高固体污染情况和电流流过轴承的情况。高的相对密度、硬度、断裂韧度和强度的组合对于设计用于此类应用的陶瓷滚动构件而言看来是必需的。陶瓷材料的机械性质可能极好，但其通常受到诸如包含异物、孔隙、大的晶粒和裂纹等内部及表面缺陷的较大影响，这些特征将限制其可靠性。
滚动轴承由内环和外环及其之间的诸如球状体、圆柱形滚子、球形滚子、锥形滚子和杆状体(needle)等滚动构件构成。
用于制造陶瓷部件的原料是通过对液体中的组分进行研磨并随后对浆料进行干燥而制得的粉末。干燥可以通过例如喷雾干燥或冷冻干燥来进行。通常，用于轴承部件的粉末是氮化硅类物质。在氮化硅和塞隆(sialon，氮化硅类的材料，其中硅和氮由铝和氧取代)的情况中可以加入少量的稀土粉末以用于液相烧结。在传统方法中形成陶瓷部件时，往往使用有机添加剂作为粘合剂以用于通过干压或冷等静压而形成坯体。在最终的致密化之前需要通过煅烧陶瓷坯体除去有机添加剂。对于大型陶瓷部件来说，该方法要耗费很长的时间，并且对于大型坯体而言比小型或中等尺寸的部件更为困难。
已经开发出了用于轴承零件的几个等级的陶瓷，并且可在市场上得到。而对于用于各种轴承应用的具有良好品质的大型陶瓷轴承部件仍有日益增长的需要。氮化硅和塞隆是质轻、坚硬且坚固的工程陶瓷。
现今，氮化硅和塞隆轴承部件主要通过热等静压(HIP)或气压烧结(GPS)来制造，这些方法是高烧结温度与高压相结合的方法。
制造用于轴承应用的具有良好品质的更大型陶瓷部件趋向于对压缩坯体提出挑战，烧结工艺导致产品昂贵。在烧结时使用更廉价的原料和更低的压力往往得到不充分的或至少劣化的机械性质，这使得用于严苛的轴承操作的可靠性和性能受到限制。
HIP工艺需要复杂的胶囊来包封待压缩的粉末，而且压缩周期缓慢且能耗很高。因此，利用HIP制造大型陶瓷部件的总生产周期对于每个批次均为几个小时。用于HIP制造部件的正常批次时间周期是约8小时且随着部件变大而时间延长，这使得较大部件的烧结极为耗时。
在气压烧结时，粉末首先在常规压力下压缩以封闭所有的表面孔隙，从而避免第二步中在压力升高时的气体渗透。烧结主要在具有高压的第二步中进行，并且冷却期间压力通常也保持在较高的水平。该方法是周期时间为几个小时的耗时耗能的方法。烧结部件的尺寸的增大导致时间和能量的消耗呈指数增长。
陶瓷轴承的许多发展特别是致力于小型陶瓷轴承部件，这些部件例如用于计算机硬盘驱动器或低振动运行极为重要的其他应用。通过传统方法难以烧结更大的陶瓷部件。非均匀结构和致密化的困难连同高成本、长生产周期和高能耗是主要问题。
电脉冲辅助固结(EPAC)包括基于用脉冲DC电流加热待烧结的材料的工艺。该技术的其他常用名称是火花等离子体烧结(SPS)、脉冲电流烧结(PECS)、场辅助烧结技术(FAST)、等离子体辅助烧结(PAS)和等离子体压力成型(P2C)。下面，在本文中将这些技术称为SPS。在SPS中，加热样品的同时施用单轴压力。通过对放置在石墨冲头之间的模具中的粉末施加电能脉冲而发生加热。该烧结方法允许在应用高加热速率和短停留时间的同时制得致密的材料。该技术应用高电流与低电压的组合。具有典型的几个毫秒的脉冲持续时间和0.5kA～30kA的电流的脉冲DC电流流过冲头、模具，并根据样品的电性质也流过该样品。电脉冲以脉冲包的形式产生，其中开启：关闭的比在1∶99～99∶1的范围内，通常为12∶2(12个脉冲开启，2个关闭)。压力在单轴方向上直接施加于冲头，其通常为5MPa～250MPa。
US5,622,905和US5,698,156描述了具有均匀的细晶粒的氮化硅类坯体。所用的氮化硅粉末应当由小于200nm的晶粒或具有无定形结构的晶粒构成。超细粉末通过化学气相沉积制备。用于氮化硅粉末的烧结温度为1200℃～1400℃或1400℃～1900℃，乃至更高的温度，只要总时间乘以温度为低于600000℃秒。SPS工艺可用于制造坯体。该方法的问题在于需要昂贵的处理，例如对初始粉末的化学气相沉积，以确保所得产物的细粒径。对于较大的部件也难以使用该方法，因为那将需要更长的停留时间，而这与极细的晶粒结构将是不相容的。
US 5,720,917描述了通过调整制造工艺以致能够使用纯度较低的氮化硅初始材料来制造更为廉价的高品质氮化硅产品的方法。氮化硅和烧结助剂可具有达5000ppm的金属杂质水平，并且能够在1300℃～1900℃的烧结温度进行处理，烧结温度与烧结时间的乘积为105℃秒～106℃秒。
US 6,844,282和US7,008,893描述了具有小于100nm的粒径且具有极低摩擦系数的氮化硅类烧结体。制造方法包括粉碎并混合氮化硅粉末、烧结助剂金属钛粉和石墨/碳粉至低于30nm的极小的粒径。粉块将在氮气氛围中在0.05MPa～1MPa的压力下烧结。
中国专利CN1793042提出了具有高刚性和高韧性的火花等离子体烧结的氮化硅。氮化硅包含稀土氧化物、氧化铝和氮化铝的添加剂。
对于需要更大尺寸的部件的应用来说，对金属轴承的陶瓷替代品的需求不断增加。轴承用于诸如低重量、优异的机械性质和电绝缘等性质高度优先的应用。陶瓷轴承的一些性质也有利于更为环境友好的方案，例如较低的轴承重量可减少能耗。为了使用更大规模的陶瓷轴承，必须改善较大陶瓷轴承的品质，并且必须削减制造这些轴承的成本。
发明内容
本发明的一个目的是提供陶瓷部件，例如轴承用滚动构件，所述陶瓷部件具有均匀的微结构和最少的缺陷及良好的机械性质，并且可支持来自包括振动在内的滚动接触机械负载的高需求。
另一个目的是提供陶瓷部件，所述陶瓷部件的尺寸使其可被用作诸如大型压缩机和风力涡轮机中的轴承等大型轴承中的滚动构件。
本发明的另一个目的是用于制造大型高品质陶瓷部件的方法，尤其是具有成本效益的并且能够比目前用于制造大型陶瓷部件的制造方法更为快速地操作且具有更低能耗的方法。
这些目的通过具有小于1体积％孔隙率或小于0.2体积％的孔隙率的均匀的，完全或接近完全的致密结构的烧结的陶瓷部件而实现。余留在所述结构中的可能的孔将均匀分布，或仅是在所述部件的最核心处(部件直径的最大25％的区域上)被观察到，该结构实际上没有所谓的内裂(snowflake)。内裂是局部区域不完全致密化的标志，通过紫外光下的荧光渗透的折射而可视化。第二相的量将较低。第二陶瓷相的体积分数通常为低于0.2体积％，更常为低于0.06体积％。第二相可以是未反应的粉末，或是烧结过程中形成的副产物。
微结构可以是等轴的形式，或是嵌埋在非晶质晶界相中的伸长的晶粒的形式，晶粒和晶界相构成基体。伸长的晶粒应当优选为各向同性地分布在三维空间。晶粒可具有纳米级至微米级的尺寸。如果存在孔隙，则其具有的最大尺寸为10μm。
烧结的陶瓷部件可以由氮化硅、塞隆或其混合物制成。陶瓷粉末可包含最大量为10重量％的其他化合物的添加剂，例如氧化钇、其他稀土氧化物、氧化锆、氮化铝、氧化铝和/或用于二氧化硅和氮化硅的硅和铝的氮氧化物。
烧结陶瓷部件的制造包括制备不含有有机添加剂，或至少小于1重量％的有机添加剂的粉末混合物。粉末可通过传统的粉末制备技术如研磨来制备。制备不进行包封的烧结用粉末。火花等离子体烧结技术(SPS)用于制造陶瓷部件。SPS组合了快速加热、在所期望的烧结温度的短保持时间和高压以用于烧结陶瓷部件。该加工方法能够定制陶瓷部件的微结构。
为了制造在至少一个方向上具有超过30mm的尺寸的烧结的陶瓷部件，过程中使用的压力为5MPa～150MPa，优选为5MPa～70MPa。应用的加热速率为5℃分钟-1～600℃分钟-1，优选50℃分钟-1～200℃分钟-1。选择烧结温度和时间，从而发生表示密度超过99％的全部或近似全部的致密化。该过程可在烧结单元中在一步或几个步骤中发生，在所述步骤中一个步骤与另一个步骤的温度和压力可发生变化。可以进行包括几个步骤的过程，使第一步涉及将部件烧结至全部或近似全部的致密化，并使随后的步骤涉及在稍微更高的温度和更低的压力下的晶粒生长，从而获得所期望的微结构，例如三维针状结构。致密化步骤可以在1500℃～1600℃的温度和30MPa～150MPa的压力进行，在第二晶粒生长步骤中，温度为1600℃～1750℃，压力为低于30MPa。
制造在至少一个方向上具有超过30mm的尺寸的高品质烧结陶瓷部件的可能性使得能够生产例如轴承用滚动构件等对机械稳定性具有极高要求的部件。所用的材料与受控的烧结过程的组合具有许多有利之处，并且能够以短的整体加工时间制造高品质的陶瓷部件。极大缩短了加热部件的时间，并因此减少了整个过程的能耗。由于粉末制备的简单性、基本上无需有机添加剂的粉末的压制和不包封粉末进行烧结的可能性，减少了制造部件所需的装置的数量，并由此减少了对车间空间的需要。本发明能够以成本有效的方式制造高品质的烧结陶瓷。
尽管本发明能够制造大型陶瓷部件，不过其也适用于在至少一个方向上具有小至10mm的尺寸的较小部件。
附图说明
图1.根据以下实施例1制备的化学蚀刻的塞隆材料的扫描电子显微照片。
图2.紫外光下的塞隆样品的显微照片，显示出：a)具有许多大范围的所谓内裂的局部区域微缺陷的不良样品。b)不具有(或具有隔离的、极小的)内裂的可接受的样品。
图3.本发明的样品与现有技术的样品的微结构的比较。
图4.Si3N4样品的显微照片。
具体实施方式
轴承用陶瓷滚动构件尤其是大尺寸构件，例如具有30mm～60mm的直径乃至更大的尺寸的构件，可由氮化硅、塞隆(氮化硅类的材料，其中硅和氮由铝和氧取代)、其混合物制成。此外，诸如钇氧化物(三氧化二钇)、其他稀土氧化物、锆氧化物(氧化锆)、氮化铝和铝氧化物(氧化铝)等添加剂的最大含量可以为达到10重量％。
进行粉末混合过程而不使用有机添加剂，或使用最大为1重量％的有机添加剂。与使用有机粘合剂的传统方法相比，本发明的方法包括不含有来自有机添加剂的残余物的更纯的最终产物，以及更为环境友好的过程(不排放二氧化碳)。低含量有机添加剂或完全不含有机添加剂将防止致密化期间的碳的形成以及在陶瓷部件内的可能的包封。烧结材料的晶粒可包含一个单一晶相，或者是不同晶相的混合物，而且在基体中存在非晶质晶界相。
为了减少延长加热对部件的影响，使用火花等离子体烧结(SPS)技术，该技术组合了快速加热、在所期望的烧结温度的短保持时间和高压以用于烧结陶瓷部件。
该过程中所用的压力为5MPa～150MPa，优选为5MPa～70MPa。应用的加热速率为5℃分钟-1～600℃分钟-1，优选30℃分钟-1～150℃分钟-1。选择烧结温度和时间，从而发生全部或近似全部的致密化(＞理论密度的99％)。该步骤可通过获取具有部件的尺寸和组成的所期望的组合的样品而进行验证。致密化过程可在烧结单元中在一个步骤或几个步骤中发生，在所述步骤中可以改变温度和压力。在第一温度和第一压力下的第一步使得坯体进行致密化，具有第二、更高的温度和第二、更低的压力的第二步允许用于氮化硅和塞隆类材料的受控的晶粒生长。
SPS处理方法提供了对所制得的材料的微结构进行定制的能力。使用传统的烧结工艺，例如热压或HIP，致密化伴随着晶粒生长和液相反应。由于采用SPS的快速致密化，晶粒生长可以与致密化相分离。通过SPS的快速改变温度和压力的可能性使得可以控制晶粒的生长。对于塞隆和氮化硅，烧结温度影响晶粒的结晶度，由此影响晶粒的形态。通常对于氮化硅和塞隆来说，温度越高β相越多，因而伸长的晶粒越多，此外粒径随温度而增大。采用SPS，等轴的晶粒结构和具有伸长的晶粒的自增强材料(类似于晶须增强型材料)二者均可通过受控的晶粒生长而形成。经历受控晶粒生长的伸长的β相晶粒对于改善塞隆和氮化硅材料的断裂韧性是极为理想的。
对于直径大于30mm的部件，滚动构件也显示出高硬度和高压痕断裂韧度的优异组合。具有60mm直径的滚动构件在总计小于2小时的时间制得，直径约20mm的更小的构件可以在30分钟内制得。此外，获得了完全致密的或近似完全致密的材料(密度为理论密度的至少99％)，不存在或仅有极低含量的所谓内裂(由于局部微缺陷导致的紫外光下荧光渗透的折射)，并具有细粒结构。本发明显示，可以制得大于20mm或30mm～60mm乃至更大的大尺寸的高品质陶瓷部件。传统上利用HIP或GPS制造大型部件由于加热过程缓慢所致更为耗时，并在获得完全致密材料以及均匀微结构方面会发生问题。
用于烧结的陶瓷部件的塞隆和氮化硅材料优选具有高β相含量，β相通常超过50重量％。β相含量由烧结参数控制。在对测试样品进行评估后选择适宜的烧结温度。β相晶粒伸长并能够形成坚固的三维网状结构。在图1的扫描电子显微照片中可看到作为浅灰色区域的伸长的β晶粒的存在。
对于氮化硅和塞隆材料及其混合物，烧结在1300℃～1750℃发生。用于氮化硅和塞隆的烧结温度在制造过程的至少一个步骤中为1500℃～1750℃，优选为1600℃～1750℃。
通常，在所期望的温度下的保持时间对于15mm直径的部件为5分钟，对于60mm直径的部件为达到40分钟～60分钟。对于更大的部件和在多样品模具中制造的样品则可应用更长的保持时间。
本发明的方法的一个实施方式包括：(i)将粉末材料或预成型坯体插入包括模具和冲头的导电石墨室中；(ii)对石墨室的两个导电冲头施加单轴压力，由此对材料施加压力；(iii)使用通过冲头和导电模具的脉冲电能加热材料。烧结工序包括高加热速率(陡斜的加热斜率)和在所期望的烧结温度的短保持时间。样品的冷却可以程序化进行，或者电流被切断时样品将自动冷却。
烧结的陶瓷部件被切割并通过传统方法抛光之后对其进行分析。
对于氮化硅和塞隆类材料，维氏硬度Hv10为1550kgmm-2～2200kgmm-2，通常为1600kg mm-2～2000kg mm-2，断裂压痕韧度为4.5MPa·m1/2～10.0MPa·m1/2，通常为5.0MPa·m1/2～8.0MPa·m1/2，4-点抗弯强度为600～1000，通常为810MPa。部件不存在所谓的内裂。
图2a和图2b显示了内裂在紫外光下是如何可视化的。图2a显示的不良样品在结构中具有许多大范围的所谓内裂的微缺陷区域。在图2b中，显示出不具有内裂或仅具有隔离的极小的内裂的可接受的微结构。
此外，孔隙率为低于1％，通常为小于体积的0.02％。孔隙应具有最大为10μm的尺寸，如果存在孔隙，则其应当均匀分布或者仅在部件的最核心处的部件直径的最大25％的区域上被观察到。
在图3a～图3d中显示了与传统的塞隆和氮化硅样品比较的本发明的样品的孔隙率和均匀性的一个实例。图3a示出了来自实施例1的抛光样品。显微照片显示，样品基本上不存在孔隙，并且未显示许多的第二相。其他的传统制得的氮化硅材料可显示出分布在氮化硅基体中的各种程度的第二相。图3b示出均匀分布在氮化硅基体中的相当大量的较粗尺寸的浅色相和深色相。图3c显示了微结构，其中浅色的第二陶瓷相仍然极细，但具有极为致密的分布(高体积分数)，而深色的陶瓷相形成了较粗尺寸的聚簇。图3d显示了微结构，其中浅色相和深色相二者均具有较粗尺寸的聚簇分布。第二相的较粗尺寸和聚簇分布在氮化硅基体中是不均匀的，这会影响强度、局部硬度和裂纹扩展。
滚动构件可以是滚子、球状体、锥形体和杆状体的形式。典型尺寸是：滚动构件的直径为10mm～65mm，非球形部件的长度为6mm～70mm。
实施例
实施例1
通过混合91重量％Si3N4(d50＜0.5μm)、5重量％Y2O3(d50＜0.9μm)和4重量％SiAl6O2N6(d50＜2.50μm)来制造粉末。将粉末混在液体介质中并进行冻干。将粉末插入石墨模具室中，并通过两个冲头来使室封闭。粉末在SPS单元中烧结，温度最初自动升至600℃。随后，应用100℃分钟-1的加热速率。样品首先在1550℃致密化3分钟，之后在1730℃的第二温度处理5分钟。用聚焦于烧结模具表面的光学高温计测定温度。烧结在真空下发生。压力在第一致密化步骤中保持为50MPa，然后在第二温度处理步骤中降至5MPa。
形成的塞隆部件具有的维氏硬度Hv10为约1800kg mm-2，断裂韧度K1c为6.4MPa·m1/2～6.8MPa·m1/2。检测了断裂压痕韧度的各向异性，其在与压力方向平行的方向和垂直的方向间小于5％，最弱的方向仍然显示出高于6MPa·m1/2的最小断裂压痕韧度。由双轴强度测试评估4-点抗弯强度为约810MPa，威布尔参数(Weibullparameter)为约9。在对抛光样品放大倍数达200倍的光学显微镜下，微结构显示出没有可见的孔隙，有限的第二相或没有第二相，并且没有内裂。
烧结部件由X-射线粉末衍射测定为由80重量％的β-塞隆和20重量％的α-塞隆的混合物构成。不使用添加剂SiAl6O2N6，可以使用Si3N4、AlN和Al2O3的组合，并且不使用Si3N4与添加剂的组合，可以使用塞隆粉末以用于相同的目的。
实施例2
通过混合91重量％Si3N4(d50＜0.5μm)、5重量％Y2O3(d50＜0.9μm)和4重量％SiAl6O2N6(d50＜2.50μm)来制造粉末。将粉末混在液体介质中并进行冻干。将159g粉末插入直径为34mm的石墨模具室中，并通过两个冲头来使室封闭。粉末在SPS单元中以30℃分钟-1的加热速率进行烧结。样品在1650℃致密化30分钟。用聚焦于烧结模具表面的光学高温计测定温度。烧结在真空下发生。压力保持在40MPa。
形成的塞隆部件具有的维氏硬度Hv10为约1700kg mm-2，断裂韧度K1c为约6.7MPa·m1/2。检测了断裂压痕韧度的各向异性，其在与压力方向平行的方向和垂直的方向间小于11％，最弱的方向仍然显示出高于5.7MPa·m1/2的最小断裂压痕韧度。在对抛光样品放大倍数达200倍的光学显微镜下，微结构显示出没有可见的孔隙，有限的第二相或没有第二相，并且没有内裂。仅在部件的最核心中有很小的5mm直径区域显示出尺寸至多为10μm的几个孔隙，局部的孔隙体积分数最大为0.2％，更常为低于0.06体积％。
圆柱形部件的最终尺寸为Φ34x54mm。
实施例3
通过混合91重量％Si3N4(d50＜0.5μm)、5重量％Y2O3(d50＜0.9μm)和4重量％SiAl6O2N6(d50＜2.50μm)来制造粉末。将粉末混在液体介质中并进行冻干。将粉末在SPS单元中以30℃分钟-1的加热速率进行烧结。样品在1600℃致密化30分钟。用聚焦于烧结模具表面的光学高温计测定温度。烧结在真空下发生。压力保持在40MPa。
形成的塞隆部件具有的维氏硬度Hv10为约1700kgmm-2，断裂韧度K1c为约7MPa·m1/2。检测了断裂压痕韧度的各向异性，其在与压力方向平行的方向和垂直的方向间小于11％，最弱的方向仍然显示出高于5.7MPa·m1/2的最小断裂压痕韧度。在对抛光样品放大倍数达200倍的光学显微镜下，微结构显示出没有可见的孔隙，有限的第二相或没有第二相，并且没有内裂。仅在部件的最核心中有很小的7mm直径区域显示出尺寸至多为10μm的几个孔隙，局部的孔隙体积分数最大为0.2％，更常为低于0.06体积％。
圆柱形部件的最终尺寸为Φ42x67mm。
实施例4
通过混合90重量％Si3N4(d50＜0.5μm)、5重量％Y2O3和5重量％的Al2O3来制造粉末。通过标准技术，即用球磨研磨液体介质中的混合物并进行冻干，制备粉末。粉末在SPS单元中在1500℃致密化3分钟。得到的部件由Si3N4构成。3分钟后部件已被视为完全致密化。图4是该样品的透射电子显微照片，显示没有孔隙。

Claims (5)

1.一种陶瓷部件作为轴承用陶瓷滚动构件的应用，所述部件通过电脉冲辅助固结(SPS)工艺烧结，在至少一个方向上具有超过30mm的尺寸，并且包含氮化硅、塞隆或其混合物以及至多10重量%的稀土氧化物、氮化铝、氧化铝和/或硅和铝的氮氧化物作为添加剂，其中，所述部件具有均匀的微结构和为理论密度的至少99%的密度，最大孔体积为1体积%，或最大为0.2体积%，并且第二陶瓷相体积分数不超过0.2体积%，其中第二陶瓷相是未反应的粉末或烧结过程中形成的副产物，并且其中，所述滚动构件的维氏硬度HV10为1550kg mm-2～2200kg mm-2，断裂压痕韧度为5.0MPa·m1/2～8.0MPa·m1/2，4-点抗弯强度为600MPa～1000MPa。
2.如权利要求1所述的应用，其特征在于，可能的余留在所述结构中的孔隙将均匀分布，或仅是在所述滚动构件的最核心处、在所述滚动构件直径的最大25%的区域上被观察到。
3.如权利要求1或2所述的应用，其特征在于，所述滚动构件具有超过50重量%的β相含量。
4.如权利要求3所述的应用，其特征在于，所述均匀的微结构包括形成三维网络的伸长的β晶粒。
5.如权利要求1所述的应用，其特征在于，所述第二陶瓷相体积分数不超过0.06体积%。
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