CN107522474A - 纳米晶烧结刚玉磨粒及其制备方法 - Google Patents

纳米晶烧结刚玉磨粒及其制备方法 Download PDF

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CN107522474A
CN107522474A CN201710731412.6A CN201710731412A CN107522474A CN 107522474 A CN107522474 A CN 107522474A CN 201710731412 A CN201710731412 A CN 201710731412A CN 107522474 A CN107522474 A CN 107522474A
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庞京涛
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Abstract

一种金属磨削用纳米晶烧结刚玉磨粒及制备方法，其原料组成重量百分比为：勃姆石(γ‑AlOOH)含量为91.5～97.0wt％；SiO2 0.1～0.5wt％；MnO、Fe2O3、MgO、Cr2O3中的一种或者几种的组合，含量为1.4～4.5wt％；稀土氧化物Eu2O3，La2O3，Y2O3中的一种或几种的组合，含量为1.5～3.5wt％；按照原料组成重量百分比加入各种原料混合均匀，再按照1:4的固液比加入1～2mol/L硝酸进行溶解形成溶胶，然后加入固液总重量0.5％的引晶剂和固液总重量0.3％的增塑剂，搅拌均匀静置形成凝胶后在烘箱中干燥6小时，然后通过成型工艺做成规整的形状将成型后产品在烧结炉中800℃进行初烧6‑8小时后，在1300～1400的回转炉中快速烧结3～8分钟，最终形成α‑Al2O3致密均匀的微晶结构。本发明具有很高的密度和硬度。能够解决常规磨粒在金属磨削过程中效率低、易烧伤等问题。

Description

纳米晶烧结刚玉磨粒及其制备方法
技术领域
本发明涉及一种纳米晶烧结刚玉磨粒，用于金属磨削领域，尤其涉及的是高精度磨削用纳米晶烧结刚玉磨粒及其制备方法。
背景技术
1981年美国3M公司工业磨料部推出了一种牌号为"Cubitron"的陶瓷刚玉磨料。其韧性是普通刚玉的2倍以上。磨削性能优于大多数普通磨料。八十年代中期，诺顿公司开发出了一种SG(商标名)磨料，它也是一种陶瓷刚玉磨料，性能与Cubitron磨料相似，其实，这两种磨料都是采用一种俗称为溶胶-凝胶(Sol-gel,简称SG)工艺的化学陶瓷工艺制造的。其工艺过程是：配制勃姆石(γ-AlOOH)的水溶胶体，经凝胶化后。干燥固化，再破碎成颗粒，最后烧结成磨料。
另外，由于烧结刚玉磨料颗粒是由大量亚微米级的A12O3晶体烧结而成，在磨削时能不断破裂并暴露出新的切削，因此其自锐性特别好。其磨削性能明显优于普通刚玉，主要表现为耐磨、自锐性好、磨除率高、磨削比大等优点。主要用于难磨削材料的高效磨削。它通过一种溶胶凝胶工艺使生产出的每颗磨粒中含有成千上万个微小结晶。每颗陶瓷磨粒的微观结构，使它能自锐，持续地露出新的、锋利的切削刃。因而微米级烧结刚玉磨料非常致密、粗糙、坚固、锋利。它磨削时产生一个与刀具后角相似的锋利的切削刃，因此其切削温度较低，它比普通氧化铝对难磨削材料的烧伤或金相损害更少，并且可在低负荷下长时间保持锋利，总停机时间较少，寿命更长。因而该磨料的砂带和砂盘能在难磨削材料，如航空和航天合金以及锻钢上进行快速切削。这种独特的能力提高了产量，降低了劳动成本。
由于上述磨料的晶粒尺寸仅到微米级，磨粒的自锐性还有改善的空间，并且凝胶干燥后破碎过程中有20％以上的细粉损耗，会造成粉尘污染及浪费。因此，现有技术存在不足，需要改进。
发明内容
针对上述现有技术的不足，本发明提供一种纳米晶烧结刚玉磨粒及其制备方法，将晶粒的尺寸降低至纳米级，改善磨料的硬度和自锐性。并且增加成型工艺直接将凝胶成型至需要的形状，避免破碎过程中的浪费和污染。
本发明采用如下技术方案：
一种纳米晶烧结刚玉磨粒，其特点在于，原料组成的重量百分比为：
勃姆石(γ-AlOOH) 含量91.5～97.0wt％；
SiO2 含量0.1～0.5wt％；
MnO、Fe2O3、MgO、Cr2O3中的一种或者几种的组合， 含量1.4～4.5wt％；
Eu2O3，La2O3，Y2O3中的一种或几种的组合， 含量1.5～3.5wt％。
优选的，MnO、Fe2O3、MgO、Cr2O3的重量百分比为：MnO:Fe2O3:MgO:Cr2O3＝1：1：1：2。
优选的，Eu2O3，La2O3，Y2O3的重量百分比为：Eu2O3:La2O3:Y2O3＝1：2：1。
上述纳米晶烧结刚玉磨粒的制备方法，包括下列步骤：
1)选定所述的原料组成重量百分比并称量各原料，混合均匀，再按照1:4的固液比加入1-2mol/L硝酸进行溶解形成溶胶，然后加入溶胶总重量的0.4～0.6％的引晶剂，加入溶胶总重量0.3～0.5％的增塑剂，然后搅拌均匀，静置30-40分钟形成凝胶；
2)将所述的凝胶在烘箱中干燥6-8小时；
3)将干燥后的凝胶通过成型工艺做成规整的形状的刚玉磨粒毛坯；
4)将所述的刚玉磨粒毛坯在烧结炉中650-800℃初烧6～8小时，然后在1300～1400℃的回转炉中快速烧结3～8分钟，形成烧结刚玉磨粒。
所述的引晶剂是指为改善凝胶速度加入的30-60纳米的α-Al2O3，制造方法为：将200纳米的α-Al2O3湿法球磨72小时，使其粒径达到30～60纳米。比表面积大于160m2/g。
所述的增塑剂为羟丙基甲基纤维素醚(100000粘度)，钠含量低于0.1％。
所述的成型工艺包括：
条状烧结刚玉磨粒的成型工艺是将干燥好的凝胶放入圆形截面的条形模具或三角截面的条形模具中，通过挤面条机挤压成长条型，相应地得到圆柱型烧结刚玉磨粒毛坯或三棱柱状的烧结刚玉磨粒毛坯；
片状烧结刚玉磨粒的成型工艺是将干燥好的凝胶放入三角形片状模腔或六角型片状模腔中，再通过压机压制成三角形片状刚玉磨粒毛坯或六角形片状刚玉磨粒毛坯。
该磨料的物理性能是密度大于3.80g/mm3,硬度HV大于1800kg/mm2。
烧结后的磨粒α-Al2O3作为主晶相；SiO2含量0.1～0.5％，SiO2的加入主要是在高温下与α-Al2O3形成莫来石相，增加整个微晶结构的高温下的强度；MnO、Fe2O3、MgO、Cr2O3中的一种或者几种的组合，含量1.4-4.5wt％，MnO等氧化物的加入主要是与α-Al2O3形成固溶体，存在于晶界上，抑制α-Al2O3的晶粒长大。稀土氧化物Eu2O3，La2O3，Y2O3中的一种或几种的组合，含量1.5～3.5wt％，稀土氧化物的加入是作为大颗粒存在于α-Al2O3的晶界上，防止晶粒的异常长大及抑制晶界缺陷的扩展，增加产品的韧性，微观晶相结构如图1所示。烧结后的磨粒的微观结构为片状晶粒和条状晶粒混合存在，晶粒的大小为300～600纳米，纳米级的晶粒增加了磨粒的硬度，并且晶粒在磨削过程中不断脱落，保持磨削刃口的锋利，并且带走磨削的热量，不产生烧伤。片状晶粒和条状晶粒的间隔存在给磨料提供了额外的韧性，使其在磨削过程中能承受更大的冲击了，从而能够保持长的磨削寿命。
本发明的技术效果如下：
本发明解决了常规磨粒磨削效率低，磨粒易老化的问题。本发明以氧化铝微粉为主要原料，添加MnO、Fe2O3、MgO、Cr2O3中的一种或者几种的组合,稀土氧化物Eu2O3，La2O3，Y2O3中的一种或几种的组合，通过烧结的方法制成的磨粒。添加的氧化物的作用是降低氧化铝的烧结温度,抑制晶粒的长大。烧结后形成α-Al2O3致密均匀的纳米晶结构。产品具有很高的密度和硬度。能够解决常规微晶烧结刚玉磨粒削效率低，易老化等性能问题以及粉尘污染和损耗等其他方面问题。
附图说明
图1为本发明磨粒晶相结构图；1，条状α-Al2O3晶粒，2，片状α-Al2O3晶粒
图2为圆柱型磨粒图，其中a为示意图，b为实物图；
图3为三棱柱型磨粒图，其中a为示意图，b为实物图；
图4为三角型磨粒图，其中a为示意图，b为实物图；
图5为六角型磨粒图，其中a为示意图，b为实物图。
具体实施方式
以下结合具体实施例和附图，对本发明进行详细说明。
实施例1配方试验及产品的物理特性
烧结刚玉磨粒，勃姆石(γ-AlOOH)含量91.5～97.0wt％；SiO2 0.1～0.5wt％；MnO、Fe2O3、MgO、Cr2O3中的一种或者几种的组合，含量1.4～4.5wt％；稀土氧化物Eu2O3，La2O3，Y2O3中的一种或几种的组合，含量1.5～3.5wt％；上述的原料按照配比混合均匀，再按照1:4的固液比加入2mol/L硝酸进行溶解形成溶胶，然后加入固液总重量0.4～0.6％的引晶剂，加入固液总重量0.3～0.5％的增塑剂，然后搅拌均匀，静置30分钟形成凝胶。
所述的烧结刚玉磨粒的形状有条状和片状两类，其中条状是圆柱型(图2)、三棱柱型(图3)与陶瓷结合剂混合后模压成砂轮，主要应用于齿轮成型磨。圆柱型的优点是强度高，与树脂结合剂的接触面积大，结合力高，不容易脱落。三棱柱型本省带有棱边。在磨削过程中与被磨工件接触面积小，磨粒会层层剥落，自锐性好，磨削效率高。
片状的磨粒主要包含三角形片状，和六角形片状，主要应用于金属切割及打磨领域的树脂切割片及打磨片。由于磨粒本身比较薄，易于做成较薄的切割片/打磨片。并且三角型磨粒或者六角型磨粒的棱边、尖角会显著的提升切削效率。
以下是片状磨粒的特征描述：
所述的三角型烧结刚玉磨粒，横截面为等边三角形，其特征为厚度是边长的1/10到1/2。所述的六角型烧结刚玉磨粒，横截面为六角形，其特征为厚度为边长的1/10到1/2。
根据上述配方进行如下表1所示的具体实验：
表1
将勃姆石、SiO2粉末、MnO等氧化物粉末、Eu2O3等稀土氧化物粉末按照上表配方称量，然后再高速混料机中混合30分钟。将混合好的粉料投入搅拌罐，并且按上表配方加入硝酸，搅拌30分钟至变成半透明液体。然后投入引晶剂和增塑剂，再搅拌30分钟。将搅拌好的物料倒入干燥盘，静置30分钟凝固成果冻状。然后放入烘箱在120℃干燥6小时，自然冷却至室温。将干燥好的物料放入挤面条机或者压机，匹配不同形状的模具，挤压出不同形状的素坯。将素坯静置12小时，然后进入烧结炉在800℃烧结6小时即可得到需要的磨粒。用硬度计和密度计测量烧结后磨粒的密度和硬度，结果如上表所示。
磨粒齿轮磨削试验：
将实施例1配方的做成条状颗粒磨粒用陶瓷结合剂制作成φ350mm厚度40mm砂轮，进行磨削试验。试验条件：砂轮线速度40m/s，半精磨。试验结果如下表2所示：
从表1可以看出本发明的磨削效率均比较好。
片状磨粒的金属切割试验：
将实施例1中生产的三角型磨粒和六角形磨粒加入树脂结合剂和玻纤增强网片，制作成φ101.6厚度1.0切割片，进行切割试验。切割线速度80m/s,试验素材Φ16#45钢棒。
表3
从表3可以看出本发明中磨粒的切割效率和寿命均比较好。
片状磨粒的金属打磨试验：
将实施例1中生产的三角型磨粒和六角形磨粒加入树脂结合剂和玻纤增强网片，制作成φ115厚度3.0打磨片，进行金属打磨试验。试验素材#45钢，打磨机功率720W，转速11000RPM，打磨素材#45钢，打磨时间10分钟。
表4
从表4可以看出本发明中磨粒的磨削效率比较好。
实施例2配方边界试验验证
将勃姆石、SiO2粉末、MnO等氧化物粉末、Eu2O3等稀土氧化物粉末按照表5配方称量，然后再高速混料机中混合30分钟。将混合好的粉料投入搅拌罐，并且按上表配方加入1mol/L硝酸，搅拌40分钟至变成半透明液体。然后投入引晶剂和增塑剂，再搅拌25分钟。将搅拌好的物料倒入干燥盘，静置40分钟凝固成果冻状。然后放入烘箱在120℃干燥8小时，自然冷却至室温。将干燥好的物料放入挤面条机或者压机，匹配不同形状的模具，挤压出不同形状的素坯。将素坯静置10小时，然后进入烧结炉在650℃烧结8小时即可得到需要的磨粒。用硬度计和密度计测量烧结后磨粒的密度和硬度.试验表明配方在边界条件下也能达到合理的物理性能。
表5
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。

Claims (7)

1.一种纳米晶烧结刚玉磨粒，其特征在于，原料组成的重量百分比为：
2.根据权利要求1所述一种纳米晶烧结刚玉磨粒，其特征在于，MnO、Fe2O3、MgO、Cr2O3的重量百分比为：MnO:Fe2O3:MgO:Cr2O3＝1：1：1：2。
3.根据权利要求1所述一种纳米晶烧结刚玉磨粒，其特征于，Eu2O3，La2O3，Y2O3的重量百分比为：Eu2O3:La2O3:Y2O3＝1：2：1。
4.根据权利要求1所述的纳米晶烧结刚玉磨粒的方法，其特征在于该方法包括下列步骤：
1)按照权利要求1，选定所述的原料组成重量百分比并称量各原料，混合均匀，再按照1:4的固液比加入1～2mol/L硝酸进行溶解形成溶胶，然后加入溶胶总重量的0.4～0.6％的引晶剂和加入溶胶总重量0.3～0.5％的增塑剂，并搅拌均匀，静置30～40分钟形成凝胶；
2)将所述的凝胶在烘箱中干燥6-8小时；
3)将干燥后的凝胶通过成型工艺做成规整的形状的刚玉磨粒毛坯；
4)将所述的刚玉磨粒毛坯在烧结炉中650-800℃初烧6～8小时，然后在1300～1400℃的回转炉中快速烧结3～8分钟，形成烧结刚玉磨粒。
5.根据权利要求2中所述的制备方法，其特征在于，所述的引晶剂是指为改善凝胶速度加入的30～60纳米的α-Al2O3，制造方法为：将200纳米的α-Al2O3湿法球磨72小时，使其粒径达到30～60纳米。比表面积大于160m2/g。
6.根据权利要求2中所述的制备方法，其特征在于，所述的增塑剂为羟丙基甲基纤维素醚，100000粘度，钠含量低于0.1％。
7.根据权利要求2中所述的制备方法，其特征在于，所述的成型工艺包括：
条状烧结刚玉磨粒的成型工艺是将干燥好的凝胶放入圆形截面的条形模具或三角截面的条形模具中，通过挤面条机挤压成长条型，相应地得到圆柱型烧结刚玉磨粒毛坯或三棱柱状烧结刚玉磨粒毛坯；
片状烧结刚玉磨粒的成型工艺是将干燥好的凝胶放入三角形片状模腔或六角型片状模腔中，再通过压机压制成三角形片状刚玉磨粒毛坯或六角形片状烧结刚玉磨粒毛坯。
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CN113045296A (zh) * 2021-03-26 2021-06-29 福清蓝金新材料科技有限公司 一种陶瓷磨粒压印法成形的方法
CN113045296B (zh) * 2021-03-26 2022-08-09 福清蓝金新材料科技有限公司 一种陶瓷磨粒压印法成形的方法
CN113881348A (zh) * 2021-11-04 2022-01-04 青岛福禄泰科表面材料科技有限公司 一种复合氧化铝抛光液及其制备方法和应用
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CN114316901A (zh) * 2022-01-20 2022-04-12 苏州远东砂轮有限公司 规则形状立体聚合磨料颗粒及其制备方法与应用
CN116768608A (zh) * 2023-07-13 2023-09-19 郑州蚂蚁特材有限公司 一种半脆刚玉及其制备方法

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