CN1389301A - 改进的研磨介质 - Google Patents

改进的研磨介质 Download PDF

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CN1389301A
CN1389301A CN02122067A CN02122067A CN1389301A CN 1389301 A CN1389301 A CN 1389301A CN 02122067 A CN02122067 A CN 02122067A CN 02122067 A CN02122067 A CN 02122067A CN 1389301 A CN1389301 A CN 1389301A
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S·P·西拉希
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Saint Gobain Ceramics and Plastics Inc
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Abstract

经溶胶-凝胶法制得的α-氧化铝研磨介质改进了在珠磨机中研磨氧化铝材料的应用。

Description

改进的研磨介质
发明的背景
本发明涉及在研磨机中粉碎固体材料,特别是陶瓷所用的研磨介质。这种研磨机包括那些用研磨介质和待粉碎的材料装填其中的旋转或滚动滚筒,通过介质和材料之间经常接触进行粉碎的研磨机。为了引用方便,下面将所有这种研磨机称为“珠磨机”(bead mills)。
市场上有若干种以这种普通原理进行操作的珠磨机。某些珠磨机垂直定位并可装有搅拌器,而另外一些珠磨机则沿滚筒轴水平方向定位。然而,所有的珠磨机都设计成在介质和材料之间产生经常性粉碎接触。
这种操作方式着重于介质,目前一般有四种不同种类的介质在商业上使用。然而,尽管在比常规大或比常规小的研磨机中可以使用较大和较小的介质,而且介质形状可以用非圆柱形,如球形,但每一种介质一般都是以约长1厘米、直径1厘米的短圆柱体的形式来供应。
选用介质的关键因素是用来制造它们的材料。如上所述,常用的四种不同材料是:钢、纯α-氧化铝、84%α-氧化铝和氧化锆,可以使用如氧化钇或一种其它已知的稳定添加剂以四方形的形式来稳定上述材料。每一种介质都有其特殊的用途,其中大部分由其性质来确定其最广泛的应用。然而,每一种介质也都有使其不适用于某些用途的问题。这种情况通常强烈地受下述因素的影响,即粉碎材料的所需用途和其对组合物杂质或对偏离粉碎产品所需粒度分布的敏感性。当然可以理解的是,使用研磨介质进行的粉碎不仅会导致所研磨的材料的断裂,而且会在某种程度上使介质本身断裂。这样,最终产物包含的某些碎片不仅来自粉碎材料,而且来自介质,这样就会产生问题。例如不能使用钢,因为其中的金属碎片会干扰粉末性质且不易于分离。氧化锆是非常韧性的,在摩擦时它不会有太多的损失,但它对研磨氧化铝通常不是很有效。研磨氧化铝通常用氧化铝介质,因为磨掉的材料与要研磨的材料基本相同。氧化铝介质是通过在高压和高温条件下烧结精细氧化铝粉末制得的。这种产物的孔隙率和理论密度基本上为零,它对粉碎氧化铝是非常有效的,因为它具有在化学组成上与要粉碎的材料相同的优点。然而,对于高纯度的氧化铝(93%+),若目标是制造微米大小或更细的氧化铝粉末,则介质在使用过程中的断裂会产生无法接受的大片断。另一方面,对于较低纯度的氧化铝,介质的断裂(只要发生)都会产生大小与所需最终产物相一致的微片。然而,这种介质包含相当量的二氧化硅,这在某些应用中可能是无法接受的污染物。
因此,非常需要适用于粉碎氧化铝的介质,该介质如果断裂,就会断裂成可接受的碎片,并且它基本上不含杂质。
发明的描述
本发明提供主要由经接种溶胶-凝胶法(seeded sol-gel process)制得的α-氧化铝组成的研磨介质。
经接种溶胶-凝胶法制得的氧化铝的特征在于其均一的晶体结构,其中晶体的平均直径不大于约2微米。平均直径是采用校正的截距法测量的,即沿抛光SEM显微照相横截面画对角线,将对角线的总长除以对角线贯穿的晶体的数目,再将结果乘以1.5,就得到晶体的实际平均直径。本发明较好的介质含有平均直径为1微米或更小(如从0.1微米直到1微米)的α-氧化铝晶体。
溶胶-凝胶法一般从勃姆石溶胶开始,然后用在加热到足够高的温度时能促进形成α-氧化铝的材料接种。合适的材料与α-氧化铝通常是同结构的,它们的晶格大小非常类似。显然,最常用的此种晶种材料当然是亚微米大小精细颗粒状的α-氧化铝本身。然后使含有均匀地分散在其中的晶种的溶胶凝胶化,干燥和煅烧,除去水分,制得α-氧化铝的中间前体形式,之后将其烧结成α-氧化铝。
在氧化铝中可以加入少量的改性陶瓷氧化物,即将其加到凝胶中,或者在中间体仍是多孔状态时用陶瓷氧化物前体渗透-氧化铝前体。这种改性陶瓷氧化物在最终氧化铝中的量可以多达5重量%,而不会破坏介质基本为α-氧化铝的特征。
将这种接种溶胶-凝胶氧化铝烧结到密度基本为理论值时,能制得Vickers硬度至少为20GPa,较好为21Gpa(在500g负载下测量)的α-氧化铝,所述烧结在至少约100℃或更高的转化温度下进行,但低于不存在晶种时的转化温度。由于更高的温度会促进晶体的生长,事实证明可以达到如此高的密度和硬度,而不损失细小、均匀的氧化铝微晶结构。
如上所述,介质的常规形状是圆柱形,这可以通过下述方法非常容易地达到,即将接种的溶胶-凝胶挤出,将挤出物切成大致上规定大小的颗粒,之后干燥并烧制成α-氧化铝的形式。
然而,值得注意的是,我们发现并不一定要采取这种方式来制造介质。尽管圆柱形介质是有效的,但球形或无规形状也是适用的。实际上,无规形状的颗粒与圆柱形颗粒是等效的或比圆柱形颗粒更为有效,尤其是当它们一开始就得到调理,即在研磨机中滚动除去一些边角后。
接种溶胶-凝胶氧化铝被非常广泛地用于制造磨砂(abrasive grits)。在制造这种磨砂的工业化方法中,将干的烧制的前体材料粉碎成无规的形状,然后将其烧结,转变成α-氧化铝。这会产生较宽范围的粒度,然后使用网目尺寸越来越细的筛子进行分类。将不能通过一个筛子但能留在下一个更细筛孔上的粒子表征为与留住它们的筛子相对应的粒度。我们发现大小为46粒度(grit)或更粗,例如36、24、20、16或14粒度的磨砂颗粒作为氧化铝研磨介质的性能非常好。然而,理论上细得多的粒度(如小至50粒度)的粒子可用于某些用途。
较好实施方案的描述
下述实施例说明了本发明研磨介质的效果,所述实施例显示,使用本发明介质能达到较高的粉碎效率。
实施例1
将购自Alcoa Company的商品α-氧化铝(15.8kg)用作待研磨的原料。将比表面积(用BET法测量)为6m2/gm(相应于平均粒度约为1微米)的这种氧化铝放在由Netzsch Inc.,Exton,PA以商品名“Labstar LMZ-10”销售的珠磨机中。这种研磨机有聚氨酯衬里,以免污染所得的粉末。将具有无规形状并由Saint-Gobain Ceramics and Plastics Inc.销售的46A粒度(0.27-0.8mm)的接种溶胶-凝胶氧化铝磨砂、“SG”磨料粒子(加入量占总体积的12%)用作研磨介质,加入去离子水(加入量占总体积的69.5%),使总加入量为40.82升,其中固体含量为30.5重量%。然后开始研磨。
不时加入更多的介质,以使介质的量保持恒定。在21小时的研磨过程中,总共仅需加入3.7kg,以使介质保持恒定的量。在研磨机上采用自动加料控制,以维持最大功率输入,但同时保持温度足够低,以避免损坏聚氨酯衬里。
仅在1200分钟后,就获得了表面积大于120m2/gm的α-氧化铝粉末。
相比之下,当将同样的氧化铝放在使用常规半英寸氧化铝介质的常规Sweco振动研磨机中进行研磨时,在约6天后还不能粉碎到这种程度。当加入75kg的氧化铝粉末时,产物是120kg的氧化铝粉末,这表明由于摩擦而损失了显著量的介质。这样,最终产物包含存在于约45kg介质和从加入的最初氧化铝粉末得到的粉碎产物中的所有杂质。
为了评价介质的脆性,在购自Netzsch Inc.的Labstar Trinex研磨机中处理90%上述所用相同介质物料,只加入水。操作持续2小时后,介质的重量损失仅为3.9%,这与按相同方式对常规研磨介质进行的测试相比是非常令人满意的。构成3.9%重量损失的颗粒的大小都是亚微米级,显然介质基本上没有发生粗断裂。
从上述结果可清楚看出,在珠磨机中使用接种溶胶-凝胶氧化铝介质能提供非常有效和有利的研磨方法。

Claims (3)

1.一种在珠磨机中研磨α-氧化铝粉末的方法,它包括使用经接种溶胶-凝胶法制得的α-氧化铝作为研磨介质颗粒。
2.如权利要求1所述的方法,其中研磨介质是主要由平均直径小于1微米的α-氧化铝晶体组成的氧化铝颗粒。
3.如权利要求1所述的方法,其中研磨介质是无规形状的α-氧化铝颗粒。
CNB021220670A 2001-06-01 2002-05-31 改进的研磨介质 Expired - Lifetime CN1143735C (zh)

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* Cited by examiner, † Cited by third party
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CN101992044A (zh) * 2010-11-25 2011-03-30 张家港西一新型汽车配件有限公司 涂料生产线上的投料装置
CN104465362A (zh) * 2008-03-05 2015-03-25 卡伯特微电子公司 使用水溶性氧化剂的碳化硅抛光方法
CN111180719A (zh) * 2020-01-07 2020-05-19 马鞍山科达普锐能源科技有限公司 一种三级研磨制备纳米硅的方法

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CN111180719A (zh) * 2020-01-07 2020-05-19 马鞍山科达普锐能源科技有限公司 一种三级研磨制备纳米硅的方法

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CN1143735C (zh) 2004-03-31
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FR2825297B1 (fr) 2004-09-17
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SE0201583L (sv) 2002-12-02
US20020179755A1 (en) 2002-12-05
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SE523504C2 (sv) 2004-04-27
DE10221650A1 (de) 2002-12-12

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