CN103189330B - 氧化铝质烧结体、磨粒和砂轮 - Google Patents

氧化铝质烧结体、磨粒和砂轮 Download PDF

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CN103189330B
CN103189330B CN201180052635.0A CN201180052635A CN103189330B CN 103189330 B CN103189330 B CN 103189330B CN 201180052635 A CN201180052635 A CN 201180052635A CN 103189330 B CN103189330 B CN 103189330B
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aluminum oxide
powder
sintered compact
oxide sintered
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CN103189330A (zh
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富川伸一郎
宫泽宏和
家村武志
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Lishennoco Co ltd
Resonac Holdings Corp
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Showa Denko KK
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Abstract

本发明涉及一种氧化铝质烧结体和使用该氧化铝质烧结体而成的磨粒以及砂轮,所述氧化铝质烧结体是含有钛化合物和铁化合物的氧化铝质烧结体,其中,在氧化铝晶体的晶界存在FeTiAlO5晶体,该FeTiAlO5晶体的平均晶体尺寸为3.4~7.0μm。

Description

氧化铝质烧结体、磨粒和砂轮
技术领域
本发明涉及氧化铝质烧结体、使用该氧化铝质烧结体而成的磨粒和使用该磨粒而成的砂轮(磨石:grind stone)。
背景技术
氧化铝质烧结体发挥高硬度、高强度、高耐热性、高耐磨损性和高耐化学性等优异的特征,在各种产业领域被使用。特别是作为在钢铁产业中的强力磨削砂轮的原料(磨粒)被使用。
另外,作为构成以汽车为中心的运输用设备或产业用机械的部件的材料,较多地使用特殊合金。这些特殊合金与通常的SUS304等相比较硬,因此在市场上需求以往没有的「磨削比」高的强力磨削砂轮。在此,所谓「磨削比」是表示砂轮的性能的指标,由以下的式子表示。
磨削比=被磨削材料被磨削了的量(磨削量)/砂轮的磨损量
一般地,如果能用较少的砂轮磨削较多的被磨削材料则判断为性能良好,但砂轮的磨削比被该砂轮所使用的磨粒的「硬度」和「断裂韧性」影响。认为在「磨削比和硬度」以及「磨削比和断裂韧性」之间存在如下的关系。
(1)如果磨粒的硬度变高则磨削量增加,因此磨削比变大。
(2)如果断裂韧性变高则磨粒的磨损量变少,因此磨削比变大。
若考虑上述(1)和(2),则在磨削比的式子中的分子部分被磨削量影响,分母部分被磨损量影响。为了使砂轮的磨削比提高,硬度和断裂韧性都高是理想的。
在此,作为现有的强力磨削砂轮用的磨粒,已知使氧化铝质的微粉原料烧结了的磨粒(例如,参照专利文献1~3)和熔融氧化铝氧化锆磨粒(例如,参照专利文献4)、向高纯度微粒氧化铝粉末添加了氧化镁等的晶粒生长抑制剂的磨粒(例如,参照专利文献5)等。
另外,曾提出了以氧化铝作为主材料并添加了TiO2的烧结材料(例如,参照专利文献6)。此外,作为具有高硬度和高断裂韧性的耐磨损性优异的氧化铝烧结体,曾提出了添加了可固溶于氧化铝晶体中的Ti、Mg、Fe等的金属化合物的氧化铝烧结体(例如,参照专利文献7)。
现有技术文献
专利文献1:日本特公昭39-4398号公报
专利文献2:日本特公昭39-27612号公报
专利文献3:日本特公昭39-27614号公报
专利文献4:日本特公昭39-16592号公报
专利文献5:日本特公昭52-14993号公报
专利文献6:日本特开平3-97661号公报
专利文献7:日本特开平11-157962号公报
发明内容
但是,专利文献1~5都是高硬度且低断裂韧性、或者低硬度且高断裂韧性的,对于高硬度且断裂韧性高的磨粒没有具体公开。专利文献6的烧结材料进行了对于硬度的评价,但对于断裂韧性毫无考虑。另外,专利文献7的氧化铝烧结体,仅公开了Ti和Mg的组合、以及Fe和Mg的组合,对于其他的组合没有具体公开。
本发明是在这样的状况下完成的,其目的是提供一种给予高硬度且断裂韧性优异的磨粒的氧化铝质烧结体、使用该氧化铝质烧结体而成的磨粒和使用该磨粒而成的砂轮。
本发明者们为了实现上述目的反复专心研究的结果发现:作为氧化铝质烧结体所含有的化合物,着眼于钛化合物(特别是钛氧化物)和铁化合物(特别是铁氧化物),由它们和氧化铝形成的FeTiAlO5粒子特别是在断裂韧性的提高上显示出优异的效果。本发明是基于该见解完成的。
即,本发明如下。
[1]一种氧化铝质烧结体,是含有钛化合物和铁化合物的氧化铝质烧结体,其中,在氧化铝晶体的晶界存在FeTiAlO5晶体,该FeTiAlO5晶体的平均晶体尺寸为3.4~7.0μm。
[2]根据上述[1]所述的氧化铝质烧结体,其中,将钛化合物换算成TiO2后的含量和将铁化合物换算成Fe2O3后的含量的合计量为5~13质量%。
[3]一种磨粒,由上述[1]或上述[2]所述的氧化铝质烧结体构成。
[4]一种砂轮,在作用面具有上述[3]所述的磨粒的层。
根据本发明,可以提供一种给予高硬度且断裂韧性优异的磨粒的氧化铝质烧结体、使用该氧化铝质烧结体而成的磨粒和使用该磨粒而成的砂轮。
附图说明
图1是说明对于本发明的氧化铝质烧结体的冲击的传播方式的作用说明图。
图2是对于本发明的氧化铝质烧结体的冲击试验前后的SEM照片,(A)表示冲击试验前的晶体组织的样子(热腐蚀处理过),(B)表示冲击试验后的裂纹扩展的样子(无热腐蚀处理)。
图3是说明对于仅由氧化铝构成的烧结体的冲击的传播方式的作用说明图。
图4是对于仅由氧化铝构成的烧结体的冲击试验前后的SEM照片,(A)表示冲击试验前的晶体组织的样子(热腐蚀处理过),(B)表示冲击试验后的裂纹扩展的样子(无热腐蚀处理)。
图5是表示实施例7的氧化铝质烧结体的组成分析(X射线衍射测定)结果的X射线衍射图。
具体实施方式
[氧化铝质烧结体]
在本发明的氧化铝质烧结体中,在由刚玉晶体构成的主结晶相的晶界,存在含有Ti、Fe和Al的复合金属氧化物的结晶相,具体地讲存在FeTiAlO5粒子。通过该FeTiAlO5粒子的存在,成为给予高硬度且断裂韧性优异的磨粒的氧化铝质烧结体。特别是通过FeTiAlO5粒子与刚玉相相比断裂韧性较高这一作用,可得到高硬度且断裂韧性优异的氧化铝质烧结体。由FeTiAlO5粒子构成的结晶相的存在和平均晶体尺寸可以采用后述的实施例中记载的方法来确认。
从高断裂韧性化的观点来看,含有Ti、Fe和Al的复合金属氧化物的结晶相(FeTiAlO5粒子)的平均晶体尺寸必须为3.4~7.0μm,优选为3.7~6.5μm。
当为3.4~7.0μm的范围以外时,抑制在破坏时产生的裂纹的行进的效果变小。相反地,通过使平均晶体尺寸在3.4~7.0μm的范围,可以良好地保持由该FeTiAlO5粒子带来的裂纹的偏向效果。
在此,对于推测可得到如上述那样的效果的机理进行说明。
首先,在仅由氧化铝构成的烧结体的情况下,如图3所示,裂纹的扩展方式沿氧化铝粒子12的晶界向箭头Y方向行进。并且,根据冲击的大小,如图4(B)的SEM照片所示,沿晶界直线地产生龟裂。再者,图4是后述的比较例1涉及的烧结体的SEM照片,图4(A)表示施加冲击前的晶体组织的样子,图4(B)表示施加冲击后的裂纹扩展的样子。
另一方面,通过含有钛化合物和铁化合物,如图1所示,断裂韧性值高的复合金属氧化物的结晶相(例如FeTiAlO5粒子10)在氧化铝粒子12的晶界生成。通过该FeTiAlO5粒子10存在于氧化铝粒子12的晶界,即使在施加了冲击时产生的裂纹行进,裂纹也以该粒子10为起点沿箭头X方向以迂回的方式偏向,因此冲击力不是一个方向而是被分散、缓和。因此认为作为整体断裂韧性值变高。
这从图2所示的表示冲击试验的结果的SEM照片可以知道。即,当以如图2(A)的SEM照片那样在氧化铝粒子的晶界存在FeTiAlO5粒子的状态施加冲击时,如图2(B)那样裂纹以FeTiAlO5粒子为起点以对其进行迂回的方式行进。
再者,图2是后述的实施例3涉及的烧结体的SEM照片,该图中,位于在氧化铝粒子的晶界的三重点位置的灰色部分(颜色淡的部分)相当于FeTiAlO5粒子。
优选:本发明的氧化铝质烧结体含有钛化合物和铁化合物,将钛化合物按TiO2换算后的含量(以下,有时称为「TiO2换算含量」)、将铁化合物按Fe2O3换算后的含量(以下,有时称为「Fe2O3换算含量」)和氧化铝的含量的3种成分合计量为98质量%以上。
另外,TiO2换算含量和Fe2O3换算含量的两种成分合计量优选为5~13质量%,更优选为7~10质量%。
此外,在本发明的氧化铝质烧结体中,为了得到高硬度且高断裂韧性的烧结体,TiO2换算含量和Fe2O3换算含量的质量比(TiO2:Fe2O3)优选为0.85:1.15~1.15:0.85,更优选为0.90:1.10~1.10:0.90,进一步优选为0.95:1.05~1.05:0.95。
在此,关于TiO2换算含量和Fe2O3换算含量的两种成分合计量和硬度的关系,存在合计量越多则硬度就越低这样的关系,但如果两种成分合计量在本发明的范围,则作为硬度的指标的平均维氏硬度变为例如16GPa以上,具有在实用上也优异的硬度。
另一方面,关于两种成分合计量和断裂韧性的关系,没有如上述硬度那样的关系,但本发明者们发现:两种成分合计量在特定的范围中时,断裂韧性显著变高。即,如果两种成分合计量在本发明的范围,则断裂韧性值变为例如3.0MPa·m1/2以上。
另外,如在后述的氧化铝质烧结体的制造方法中说明的那样,从制造成本的观点来看,作为含有Ti和Fe的原料,优选使用钛铁矿(Ilmenite;钛精矿;FeTiO3)。
另外,为了得到具有更高断裂韧性的烧结体,优选:本发明的氧化铝质烧结体含有作为TiO2、Fe2O3和Al2O3以外的金属化合物的硅化合物和/或钙化合物。
将硅化合物按SiO2换算后的含量(以下,有时称为「SiO2换算含量」)和将钙化合物按CaO换算后的含量(以下,有时称为「CaO换算含量」)的合计量优选为2质量%以下,更优选为0.5~2质量%。
认为硅化合物和钙化合物作为晶粒生长剂起作用,通过它们按氧化物换算存在2质量%以下,使氧化铝的刚玉晶体的形状和尺寸不均一,来产生裂纹的偏向。也就是说,认为通过特定量的钛化合物和铁化合物、以及特定量的硅化合物和钙化合物的存在,各自的作用组合,效率良好地产生裂纹的偏向,可得到更高的断裂韧性化的效果。
在此,氧化铝的含量、TiO2换算含量、Fe2O3换算含量、SiO2换算含量、CaO换算含量、其他的金属化合物的金属氧化物换算含量,可以采用荧光X射线元素分析法求得。具体地讲,如以下那样求出。
首先,为了进行测定,进行元素的组成已知的标准氧化物试样的湿式分析。以得到的湿式分析值作为基准值,制成在测定时需要的校准线。样品的定量分析,以该制成的校准线为基础进行。作为测定设备,可以使用Panalytical公司制的「PW2400型」。另外,测定优选在管球为铑管球、特性X射线为Kα射线的条件下实施。管电压和管电流优选在每个元素不同的条件下进行测定。将管电压和管电流的条件的一例示于下述表1。
再者,在本说明书中,求各金属氧化物换算含量时的成为分母的总体量,为将氧化铝质烧结体所含有的全部的金属元素换算成氧化物来合计的量。
表1每种金属氧化物的管电压和管电流值
元素 管电压[kV] 管电流[mA]
Al 24 120
Fe 60 48
Ti 40 72
Si 24 120
Ca 40 72
[氧化铝质烧结体的制造方法]
接着,对于已经叙述的本发明的氧化铝质烧结体的制造方法进行说明。(原料)
在本发明的氧化铝质烧结体的制造方法中,作为原料使用氧化铝、钛化合物、铁化合物。根据需要还使用硅化合物和/或钙化合物。它们也可以是含有两种以上的复合氧化物。
作为这些原料的形态,可举出粉末、金属粉末、浆液、水溶液等,在本发明中,从操作时的处理的容易度等的观点来看,优选使用粉末原料。在使用粉末原料的情况下,为了得到均质的混合粉末,氧化铝粉末、钛化合物粉末、铁化合物粉末、硅化合物粉末和钙化合物粉末的累积质量50%直径(d50)优选分别为3μm以下,更优选为1μm以下。
在此,各种粉末的累积质量50%直径(d50)可以采用激光衍射法测定。
氧化铝粉末是用于在得到的氧化铝质烧结体中形成由刚玉晶体构成的主结晶相的原料,因此优选为高纯度的粉末,优选使用例如由拜耳法形成的氧化铝等。
作为钛化合物粉末和铁化合物粉末,可以分别是高纯度的TiO2粉末和高纯度的Fe2O3粉末,也可以是钛、铁、氧化铝的全部或者它们之中的两种形成了复合氧化物的粉末。作为复合氧化物,可举出钛铁矿(FeTiO3)粉末、钛酸铝粉末、FeTiAlO5粉末等。钛铁矿粉末比高纯度的TiO2粉末和高纯度的Fe2O3粉末便宜,因此可以抑制磨粒的制造成本。因此,优选使用钛铁矿粉末。
在此,钛铁矿也称为ilmenite,是天然产的铁和钛的氧化矿物,作为组成由FeTiO3表示。作为产地,为澳大利亚、挪威、俄罗斯乌拉尔地区、印度、加拿大、美国、马来西亚等,化学组成因产地而不同。也有FeTiO3的Fe2+的一部分被Mg2+置换了的矿物。
将构成钛铁矿(澳大利亚昆士兰产)的成分之中的氧化铝成分、和铁化合物、钛化合物、硅化合物以及钙化合物按氧化物换算后的情况的各自的化学组成示于下述表2。
表2钛铁矿中的氧化铝和按氧化物换算的情况的各成分的含量(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0.43 46.93 49.10 0.35 0.02
在使用钛铁矿粉末的情况下,钛铁矿粉末相对于氧化铝粉末的质量混合比(钛铁矿粉末/氧化铝粉末)优选为0.05:0.95~0.16:0.84,更优选为0.08:0.92~0.12:0.88。通过将质量混合比设为0.05:0.95~0.16:0.84,可以使TiO2换算含量和Fe2O3换算含量的两种成分合计量为5~13质量%。
另外,在使用硅化合物和/或钙化合物的情况下,将硅化合物按SiO2换算后的含量和将钙化合物按CaO换算后的含量的合计设为2质量%以下,优选为0.5~2质量%。通过使用这些化合物可以使断裂韧性值更加提高。
作为硅化合物粉末、钙化合物粉末,可以分别是高纯度的SiO2粉末和高纯度的CaO粉末、碳酸钙粉末等,也可以是二氧化硅、氧化钙、氧化铝的全部或者它们之中的两种形成了复合氧化物的粉末。作为复合氧化物,可举出莫来石(mullite)、沸石、膨润土、钙铝黄长石(gehlenite)、钙长石(anorthite)等的粉末。
(混合物的调制)
在制造本发明的氧化铝质烧结体的方法中,调制原料的混合物的方法没有特别限制,例如可以优选地采用下述的方法。
首先,在含有聚乙烯醇的水性介质中,将采用拜耳法得到的氧化铝粉末、钛铁矿粉末(或者TiO2粉末和Fe2O3粉末)分别加入规定量。其后,使用例如超声波分散机、行星球磨机、球磨机、砂磨机等的使用了介质的分散机、アルティマイザー(商品名)、ナノマイザー(商品名)等的无介质分散机等得到均质的浆液。接着,将该浆液干燥处理后粉碎,调制累积质量50%直径(d50)为3μm以下、优选为1μm以下的混合物(粉末)。
(混合物的烧结)
烧结如上述那样调制的原料的混合物的成型体(成形体),得到相对密度为95%以上、优选为97%以上的本发明的氧化铝质烧结体。通过使相对密度为95%以上,可以抑制起因于烧结体中的气孔和空隙的烧结体硬度和断裂韧性的降低。再者,相对密度可以将采用阿基米德法测定的烧结体积密度除以真密度来求得。
另外,在烧结时,通过公知的成型(成形)手段,例如模具压制、冷等静压、浇铸成型、注射成型、挤出成型等来成型为任意的形状,接着采用公知的烧结法,例如热压法、常压烧成法、气体加压烧成法、微波加热烧成法等各种的烧结方法来烧结该成型体。
这样得到的本发明的氧化铝质烧结体为高硬度且具有优异的断裂韧性,适合作为例如磨削材料、切削材料、研磨材料等的磨削·切削·研磨等的工具、以及钢铁产业中的强力磨削用砂轮的磨粒。
[磨粒]
本发明的磨粒由本发明的氧化铝质烧结体构成。本发明的氧化铝质烧结体,通过依次实施粉碎处理、混炼处理、成型(成形)处理、干燥处理、烧结处理来得到。
[砂轮]
本发明的砂轮是在作用面具有本发明的磨粒的层的砂轮。
作为本发明的砂轮中的磨粒向作用面的固定方法,可举出树脂结合剂、陶瓷(vitrified)结合剂、金属结合剂、电沉积等。
另外,作为基体金属的材质,可举出钢、不锈钢合金、铝合金等。
树脂结合剂,锋利度良好,但耐久性低。陶瓷结合剂,锋利度良好,耐磨损性也良好,但磨粒产生内部应力,磨粒容易开裂、缺损。电沉积,形状的自由度大,锋利度也良好。
鉴于以上情况,在砂轮中,可根据其用途选择磨粒的固定方法。
具体地讲,例如在树脂结合剂砂轮的情况下,采用混合酚树脂、聚酰亚胺树脂等的粘合剂的粉末和磨粒,或者对磨粒涂覆粘合剂,填充到模具进行压制成型的方法,或者混合环氧树脂、不饱和聚酯树脂等的液态的结合剂和磨粒,流入模具中使其固化的方法,得到在基体金属的作用面固定磨粒层而成的本发明的砂轮。
对于本发明的砂轮的形状没有特别限制,根据砂轮的用途从平形、杯形等的形状适当选择即可。
实施例
接着,通过实施例更加详细地说明本发明,但本发明丝毫不被这些例子限定。
再者,在各例中的各种特性按照以下所示的方法求得。
(1)原料粉末的累积质量50%直径(d50)测定
原料粉末的累积质量50%直径(d50)通过激光衍射法(日机装(株)制、マイクロトラックHRA)测定。
(2)氧化铝质烧结体的平均维氏硬度测定
作为装置使用(株)アカシ制、机种名「MVK-VL、Hardness Tester」,测定条件设为载荷0.98N、压头的压入时间为10秒,以15点的测定值的平均值作为平均维氏硬度。如果平均维氏硬度为16GPa以上则在实用上没有问题。
(3)氧化铝质烧结体的平均断裂韧性值
作为装置使用松泽精机株式会社制、机种名「DVK-1」,测定条件设为最大载荷9.81N、压头的压入速度为50μm/秒、压头的压入时间为15秒,以15点的平均值作为平均断裂韧性值。计算式如下。另外,如果平均断裂韧性值为3.0MPa·m1/2以上则在实用上没有问题。
KIC=0.026*E1/2*P1/2*a/c3/2
KIC:断裂韧性值(MPa·m1/2
E:杨氏模量(Pa)
P:最大载荷(N)
a:压痕尺寸(m)
c:裂纹的尺寸(m)
再者,在本发明中,上述杨氏模量E使用了氧化铝的值(3.9×1011Pa)。
(4)氧化铝质烧结体的各结晶相的平均晶体尺寸的测定
作为装置使用日本电子(株)制、机种名「JSM-6510V」,拍摄SEM照片。从得到的SEM照片测定了各结晶相的平均晶体尺寸。平均晶体尺寸通过直径法测定各晶体(50个)的在相同方向上的最大长度,算出平均值来求得。
(5)氧化铝质烧结体的含有Ti、Fe和Al的金属氧化物结晶相的组成分析
作为装置使用Panalytical公司制、机种名「X’pert PRO」,在特性X射线:CuKα射线、管电压40kV、管电流40mA的条件下,进行了上述金属氧化物结晶相的组成分析。
(6)相对密度
相对密度是通过采用阿基米德法测定的各烧结体的体积密度除以真密度而求得的。
此时,假定添加的铁化合物和钛化合物全部反应变为FeTiAlO5,在此基础上,将氧化铝的真密度设为3.98、FeTiAlO5的真密度设为4.28,以可生成的FeTiAlO5的比例和其余量的氧化铝的比例为基础算出真密度。
如上述那样,作为烧结体的原料的形态,可举出粉末、金属粉末、浆液、水溶液等。在本实施例中,考虑到从操作时的处理的容易度等的观点来看优选使用粉末的原料,使用了粉末原料。在此,将作为原料使用的氧化铝粉末、钛铁矿粉末、氧化硅(二氧化硅)粉末、碳酸钙粉末、氧化铁粉末和氧化钛粉末的化学组成(氧化铝的含量、TiO2换算含量、Fe2O3换算含量、SiO2换算含量、CaO换算含量)示于下述表3~8。
表3氧化铝粉末中的氧化铝、和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
99.36 0.02 <0.01 0.01 <0.01
上述氧化铝粉末是昭和电工(株)制「AL-160SG-3」,其累积质量50%直径(d50)为0.6μm。
表4钛铁矿(FeTiO3)粉末中的氧化铝和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0.43 46.93 49.10 0.35 0.02
上述钛铁矿粉末是澳大利亚产,将澳大利亚的CRL(ConsolidatedRutile Limited)公司制的钛铁矿粉碎成累积质量50%直径(d50)为0.75μm进行利用。
表5氧化硅粉末中的氧化铝和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0 0 0 99.91 0
上述氧化硅粉末是日本アエロジル(株)制的AEROSIL200,其累积质量50%直径(d50)为约12nm。
表6碳酸钙粉末中的氧化铝和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0 0 0 0 99.5
上述碳酸钙粉末是和光纯药工业(株)制的碳酸钙(特级),其累积质量50%直径(d50)为2.3μm。配合时按CaO换算来添加。
表7氧化铁(Fe2O3)粉末中的氧化铝和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0.019 96.66 0.017 2.38 0.006
上述氧化铁粉末是利根产业(株)制的氧化铁红SR-570,其累积质量50%直径(d50)为0.5μm。
表8氧化钛(TiO2)粉末中的氧化铝和按氧化物换算的情况的各成分的化学组成(质量%)
Al2O3 Fe2O3 TiO2 SiO2 CaO
0.057 0 99.22 0 0.0011
上述氧化钛粉末是昭和タイタニウム(株)制「スーパータイタニア(注册商标)G系列」,其累积质量50%直径(d50)为0.6μm。
(实施例1~11和比较例1~7)
将累积质量50%直径(d50)为0.6μm的上述氧化铝粉末和累积质量50%直径(d50)为0.75μm的上述钛铁矿粉末以所形成的氧化铝质烧结体中的TiO2和Fe2O3的各含量成为表9-1和表9-2所示的值的方式混合,得到了各种混合物。
向该各种混合物分别加入含有5质量%聚乙烯醇的水溶液300g、和纯水600g,通过球磨机进行粉碎、混合处理(实施例1~5和比较例1~6为4小时、其他为8小时),调制了混合物浓度约为25质量%的均质的各种浆液。
接着,将该各种浆液分别在120℃干燥处理24小时后,利用乳钵进行破碎处理,得到了累积质量50%直径(d50)为300μm以下的各种粉碎品。将该各种粉碎品分别在100MPa的压力下进行模具成型后,再在150MPa的压力下实施等静压处理,制作了各种成型体。
其后,利用电炉(大气气氛)将该各种成型体烧成4小时,使得相对密度达到95%以上,由此得到了各种的氧化铝质烧结体。对它们进行已述那样的试验(评价)。将结果示于下述表9-1和表9-2。
另外,图2表示对于实施例3的氧化铝质烧结体的冲击试验前后的SEM照片,图4表示对于比较例1的氧化铝质烧结体的的冲击试验前后的SEM照片。再者,这些图中,(A)表示冲击试验前的晶体组织的样子,(B)表示冲击试验后的裂纹扩展的样子。
(实施例12、13和比较例8、9)
将累积质量50%直径(d50)为0.6μm的上述氧化铝粉末和累积质量50%直径(d50)为0.5μm的氧化铁粉末以及累积质量50%直径(d50)为0.6μm的氧化钛粉末以所形成的氧化铝质烧结体中的TiO2和Fe2O3的各含量成为表9-1和表9-2所示的值的方式混合,得到了各种混合物。
向该各种混合物分别加入含有5质量%聚乙烯醇的水溶液300g、和纯水600g,通过球磨机进行粉碎、混合处理(处理时间:4小时),调制了混合物浓度约为25质量%的均质的各种浆液。
接着,将该各种浆液分别在120℃干燥处理24小时后,利用乳钵进行破碎处理,得到了累积质量50%直径(d50)为300μm以下的各种粉碎品。将该各种粉碎品分别在100MPa的压力下进行模具成型后,再在150MPa的压力下实施等静压处理,制作了各种成型体。
接着,利用电炉(大气气氛)将该各种成型体烧成4小时,使得相对密度达到95%以上,由此得到了各种的氧化铝质烧结体。对它们进行前面所述那样的试验(评价)。将结果示于下述表9-1和表9-2。
通过X射线衍射测定确认了:在实施例1~13和比较例3~9的氧化铝质烧结体中,存在于由刚玉晶体构成的主结晶相的晶界的含有Ti、Fe和Al的金属氧化物结晶相,是由FeTiAlO5构成的结晶相。
再者,图5表示实施例7的氧化铝质烧结体的X射线衍射测定的结果。
X射线衍射测定的数据分析,使用PANalytical公司制的分析软件「X’Pert High Score Plus」进行。
在该分析软件中,FeAlTiO5的结构,是以在1982年Tiedemann等发表的文献为基础来确定晶体结构。
对照由此得到的图和实验样品的结果,判断为峰是起因于FeAlTiO5的峰。
附图标记说明
10:FeAlTiO5粒子
12:氧化铝粒子
X:表示裂纹的行进方向的箭头
Y:表示裂纹的行进方向的箭头

Claims (3)

1.一种氧化铝质烧结体,是含有钛化合物和铁化合物的氧化铝质烧结体,其中,
在氧化铝晶体的晶界存在FeTiAlO5晶体,该FeTiAlO5晶体的平均晶体尺寸为3.4~7.0μm,
将钛化合物换算成TiO2后的含量和将铁化合物换算成Fe2O3后的含量的合计量为5~13质量%,
所述将钛化合物换算成TiO2后的含量和所述将铁化合物换算成Fe2O3后的含量的质量比为0.85:1.15~1.15:0.85。
2.一种磨粒,由权利要求1所述的氧化铝质烧结体构成。
3.一种砂轮,在作用面具有权利要求2所述的磨粒的层。
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