CN1068092A - 生产以α-氧化铝为基质的烧结材料特别是磨料的方法 - Google Patents

生产以α-氧化铝为基质的烧结材料特别是磨料的方法 Download PDF

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CN1068092A
CN1068092A CN92104241A CN92104241A CN1068092A CN 1068092 A CN1068092 A CN 1068092A CN 92104241 A CN92104241 A CN 92104241A CN 92104241 A CN92104241 A CN 92104241A CN 1068092 A CN1068092 A CN 1068092A
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弗朗西斯科斯·范·迪琴
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Abstract

一种烧结材料，特别用作磨料，以α-氧化铝为基 质，从Al(OH)3或低温煅烧的氧化铝来生产。用 Bayer法中伴生的氢氧化铝作Al(OH)3原料。
此烧结材料特征在于典型粒径＜0.5μm，具高密 度、高硬度。

Description

本发明涉及用从氢氧化铝（水铝矿或三水铝矿）得到的氧化铝基或低温煅烧过的氧化铝来生产烧结材料，特别是磨粒的方法。
α-Al2O3（刚玉）由于它的高硬度多年来被用作磨料。生产适于研磨的刚玉的传统方法是在电弧炉中熔融氧化铝（矾土）或含氧化铝的原料（铝土矿），然后捣碎，筛选凝固的熔融物至希望的磨粒大小。由于它们的高熔点或高硬度，熔解和粉碎耗能都很高且设备处理及保养昂贵。
另外，这样所得到的磨粒的性能，特别是坚韧性在许多应用中也是不理想的。
故而目前已致力于在低于刚玉的熔点之下（约2050℃）加热含铝化合物得到刚玉磨料的尝试。需指出的是它不取决于烧结材料的密度和无孔洞，而是首先取决于烧结成材料的微结构所起的决定性作用。特别重要的是产生一不含单个粗晶杂质的、晶粒≤1μm的均匀细小结构。
高纯B hmits（氧化铝-单水化物，AlOOH）作初始原料（EP24099），用所谓的溶胶凝胶法来从公知的溶液达到上述目的，同时加入阻止粗晶形成的晶化核（“种”），通过上述过程使具有满意改进的快速完全晶化成为可能。因而低温下单个晶粒在时间和空间上均不致过度增长（EP-Anm，152768）。这样得到的产品尽管质量很高，但由于初始原料是从醇铝盐水解得到的，它本身已相当昂贵了，所以产品也比较贵。
用其它的方法几乎不能使碱金属，尤其是Na达到所必需的低含量。为了避免加热时形成β-氧化铝，低钠含量是很重要的。如产生粗晶形态，那会对研磨性能产生特别不利的影响。人们已尝试过用较少的高价B
Figure 921042418_IMG2
hmit得到有可比性质量的磨料，只需加入大量的（对铝的原子比率1：35～1：2）烧结助剂并保持一定的加热速度（DE-PS 3219607）。但此添加物会形成附加相，如在已提到的EP-PS 24099中描写的尖晶石，它本身是不希望有的，因为它会使磨粒软化。
本发明的目的是提供一种生产已提出的烧结的氧化铝磨料的方法，此方法用廉价原料作初始原料，过程简单，不需加入特殊的添加剂，产品具有良好研磨性能。
本发明的任务由权利要求书1的方法来解决。
人们惊奇地发现，如在Bayer法中出现的那样，本方法可通过适当的工艺步骤的结合从普通工业氢氧化铝（Al（OH）3，水铝矿，也被称作三水铝矿）来生产高密度和有硬度的、晶粒小于1μm的烧结α-氧化铝，例如甚至小于0.5μm。
从工业氢氧化铝生产α-氧化铝虽然是普遍已知的，（在大规模铝工业生产中它是一步法），但是这样得到的氧化铝通常所具有的性能是完全不适于一般的研磨目的的，因为它具有高孔隙率和低劣的烧结性能。
烧结在一很高的温度才开始，以致结合有强烈的晶体生长，最后形成产品虽然很紧密，但由于结构粗，力学性能是不理想的，与普遍刚玉比较无显著优点。
可以用相似的方法生产所谓的片状矾土，其特征为大（几百μm）片晶体。
这样的氧化铝适用于某些表面处理，比如抛光处理，抛光时仅较少材料受磨损（DD-PS76485）。
上述溶胶-凝胶法不适于普通氢氧化铝，因为其分散性较差并不发生胶凝化（对氢氧化铝的此性能参见如《Ullmann的化学工业百科全书》Al卷，557-594页，VCH出版公司mbH，Weinheim（1985）。
按本发明先把初始原料湿态研磨或脱水烧结，以便生产中产生的烧结物分成单个晶粒。
脱水烧结最好在一研磨机、一振动磨或一电动搅拌球磨机中进行，研磨体最好是全部或主要由氧化铝组成。液体量最好使悬浮液含10～40%的（重量）固体。
液体最好用水，但也可以用水量可与水混合的易蒸发的溶剂代替部分的水，如低级醇或酮。
这样所得到的悬浮液最好用酸调节pH值至小于5，如此可除去溶解的或吸附的二氧化碳，pH值最好调节在约2-4之间。
所用的合适的酸是硝酸、盐酸、柠檬酸、蚁酸、醋酸或草酸的一种，最好用盐酸。在此所需酸量取决于氢氧化铝的性能，尤其是它的比表面积。
也可以全部或部分地不用添加酸而用真空处理除去溶液中的气体。
在氢氧化铝悬浮液中放入适当的晶化核，最好是从α-氧化铝得到的。此核能用例如简单的方式，通过研磨α-氧化铝而制得，例如煅烧的矾土形式，粒径＜1μm。
此核用量最好为总量（以Al2O3计）的1～5%（重量），并彻底地混和，最好在脱湿烧结开始或进行时加入。除晶化核之外，在某些情况下还要加入助剂或添加剂，比如消泡剂，烧结助剂，核生长抑制剂等。按本发明方法，不需加入这些添加物。
这样所得到的悬浮液随即进行干燥。为避免形成气泡，干燥在沸点下温度适当进行。常压下干燥温度最好是约70℃。当悬浮液层厚为约10cm时，干燥可在此温度下进行2-3天。如用较高的压力，则由于沸点升高需提高干燥温度，缩短干燥时间。
干燥时由于液体含量减少，体积或层厚也相应减少，不产生重要的孔隙性问题。还可能使开口的孔隙率和≤0.05ml/g，平均孔径达到≤10mm（汞-渗入法测定）。
这样所得到的干燥烧结饼紧接着，也可能在破碎后，在与所希望的研磨粒化相适的粒度下进行烧结（烧结时测定烧失量）。
烧结温度在1100-1500℃是合适的，烧结持续时间取决于温度，例如1400℃下约2小时。
尽管从氢氧化铝转化成α-氧化铝的体积收缩很大（约30%线性），但通过本发明仍可不需附加的煅烧步骤而得到一稠密的烧结产品。
本发明方法所用的氢氧化铝可以是低温煅烧的氧化铝或氧化铝和氢氧化铝的混合物。
通过对干燥的悬浮液的热重力测量研究表明，低湿煅烧过的氧化铝还含有一些水，比如约8%（重量），并在本发明处理中通过水吸收再转化为氢氧化铝。由于低温煅烧的氧化铝是从氢氧化铝制得，并且它的使用性并无特别的优点，所以本发明优先考虑用氢氧化铝作初始原料。
本发明生产的烧结材料特点在于晶粒很细、高烧结密实度和高硬度，它的韧度在
Figure 921042418_IMG3
左右或更好些。它不仅适于磨料，这些性能还决定了它有其它的用途。
下面的实施例说明了本发明方法的实施。
实施例1.
在一磨碎机（0.6升）中，在100g脱盐水中的纯氢氧化铝（MartinalROL-104，Martinswerk有限公司产，D-W-5010 Bergheim）中加入1.5%（重量）（以氢氧化铝计）的α-氧化铝晶核与氧化铝磨粒（d＝1mm），一起研磨2小时，并脱水烧结。颗粒或烧结物大小在研磨前100%的颗粒都小于10μm，研磨后100%的颗粒小于1μm。此α-氧化铝晶核在磨碎机中被高温煅烧过的氧化铝磨成粒径＜0.5μm。通过在研磨前加入约20ml  37%的盐酸溶液pH值调节到2，悬浮液开始层厚为5cm，在70℃干燥2天。
干燥后的平均孔径达9.5nm（汞-孔率计测量），开口的孔隙率小于0.05ml/g。用热重力测量或差热分析表明干燥后的原料在350℃以下放出结合水，在1010℃此结晶转化为α-Al2O3。
在1400℃烧结2小时后得到一种原料，它的晶粒直径＜0.5μm，密度＞3.8g/ml（＞95%th.D.），维克斯氏硬度（500g重量）＞19GPa。
实施例2.
如实施例1描述的方法，但其中所用的70g氢氧化铝用低温煅烧的氧化铝（型号为HLS，Martinswerk的产品）（烧失量约5%（重量），Na2O约0.2%（重量），其它金属0.05%（重量），99%的颗粒＜1μm，比表面积200m2/g）代替。
与Al（OH）3组份相适应，由热重力测试得知，干燥了的材料在400℃下重量损失为35%。
在1400℃烧结2小时后，得到与实施例1相同性能的产品。
实施例3.
如实施例2所描述的方法，但用型号为Ax（（Martinswerk产品）烧失量约6%（重量），Na2O约0.2%（重量），其它金属0.06%（重量），颗粒大小分布：约25%＜106nm，约10%＜45μm，比表面积约175m/g）低温煅烧的氧化铝作初始原料。烧结后（1400℃，1小时）的钠含量达到0.11%（重量）。根据X射线衍射分析知烧结成的产物中不含β-Al2O3（察觉限度：约1%（重量））。
实施例4（对比实施例）
如实施例2描写的方法，但用胶体研磨机超声TurraxR，Janke和Kunkel）混和30分钟以取代研磨处理。在70℃干燥3天后，得到的烧结饼具有400nm的平均孔径和0.06ml/g的开孔率。通过1200℃（5小时）煅烧得到的物质具有0.11ml/g的开孔率。
与此相比，按实施例2在1200℃下煅烧5小时后，此物质仅有0.03ml/g的开孔率。

Claims (11)

1、一种生产以α-氧化铝为基质的烧结材料的方法，它包括从α-氧化铝前体和可能采用的普遍添加物生产悬浮液，干燥此悬浮液并烧结，其特征在于，用氢氧化铝(Al(OH)3)或一种低温煅烧的氧化铝作为α-氧化铝前体，进行研磨和脱水烧结处理而形成悬浮液。
2、如权利要求1所述的方法，其特征在于，所述的研磨和烧结处理在一研磨机、振动磨或电动搅拌球磨中进行。
3、如权利要求2所述的方法，其特征在于所述的研磨机振动磨或电动搅拌球磨用主要是由α-氧化铝组成的磨粒进行工作。
4、如权利要求1至3中之一项或多项权利要求所述的方法，其特征在于，为阻止烧结时核生长，在悬浮液中加入来源于α-氧化铝的晶化核。
5、如权利要求1～4的一项或多项权利要求所述的方法，其特征在于，此悬浮液通过加入一种酸将pH值调节至小于5。
6、如权利要求5所述的方法，其特征在于，所采用的酸是硝酸、盐酸、醋酸、柠檬酸、蚁酸或草酸中的一种。
7、如权利要求1～6的一项或多项权利要求所述的方法，其特征在于，为除去溶解和/或吸附的气体，对悬浮液进行真空处理。
8、如权利要求1～7的一项或多项权利要求所述的方法，其特征在于，在1100～1500℃的温度下进行烧结。
9、如权利要求1～8的一项或多项权利要求所述的方法，其特征在于，用按Bayer方法生产矾土时伴生的氢氧化铝作为氢氧化铝原料。
10、以α-氧化铝为基质的烧结材料，也可添加其他的氧化物、碳化物、氮化物、硅化物或金属，可从按权利要求1所述的方法得到。
11、用如权利要求10所述的烧结材料作磨粒。
CN92104241A 1991-06-21 1992-05-29 生产以α-氧化铝为基质的烧结材料特别是磨料的方法 Pending CN1068092A (zh)

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