CN111718186A - 颗粒尺寸可调的zta陶瓷微珠的制备方法 - Google Patents

颗粒尺寸可调的zta陶瓷微珠的制备方法 Download PDF

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CN111718186A
CN111718186A CN202010559053.2A CN202010559053A CN111718186A CN 111718186 A CN111718186 A CN 111718186A CN 202010559053 A CN202010559053 A CN 202010559053A CN 111718186 A CN111718186 A CN 111718186A
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zta ceramic
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吴事江
林杨
李拯
杨焕顺
张合军
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Shandong Ultraming Fine Ceramics Co ltd
Shandong Yilaisheng New Material Technology Co ltd
Zibo Xingao New Materials Research Institute Co ltd
Zibo Qimingxing New Material Co ltd
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Shandong Yilaisheng New Material Technology Co ltd
Zibo Xingao New Materials Research Institute Co ltd
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Abstract

本发明涉及陶瓷材料技术领域，具体涉及一种颗粒尺寸可调的ZTA陶瓷微珠的制备方法。所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，步骤如下：(1)将氧化铝粉、氧化锆、粘土、氧化镁、稀土氧化物混合得到陶瓷粉料，并加入陶瓷粉料总质量0.3‑2.0％的PVA；(2)将混合后的粉料放入球磨机中球磨制成料浆；(3)将料浆经离心喷塔雾化造粒，制成球形造粒粉；(4)将球形造粒粉进行除铁；(5)将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，得到ZTA陶瓷微珠。本发明的制备方法实现了工业规模化生产ZTA陶瓷微球，而且可以通过调整多种工艺条件控制球径大小，制备的ZTA陶瓷微珠球形度高。

Description

颗粒尺寸可调的ZTA陶瓷微珠的制备方法
技术领域
本发明涉及陶瓷材料技术领域，具体涉及一种颗粒尺寸可调的ZTA陶瓷微珠的制备方法。
背景技术
自1975年氧化锆相变增韧发表以来，人们围绕着ZrO2的相变特性进行了大量研究，并将这一相变特性引入应用广泛的Al2O3陶瓷制备中。随着材料增韧技术的发展、制备工艺的优化和改善、烧结方式的多样化，ZTA复合陶瓷的研究受到了研究人员们的广泛关注。Nik Akmar Rejab等人制备了CeO2和MgO做为添加剂的ZTA陶瓷，发现裂纹在扩展过程中会发生桥联和偏转，ZTA的断裂韧性得到提高(Inter.J.of Refr.Metals and Hard Mater,2013,41:522)。杨东亮等人发现，在ZTA陶瓷中引入适量的高岭土可促进ZTA陶瓷的烧结，细化晶粒，提高了综合性能(山东陶瓷，2001，24(4)：3)，ZTA复相陶瓷具有高强度、高韧性、优良的耐腐蚀性以及生物相容性等特性，在先进核能材料、陶瓷刀具、耐磨衬板、生物医用等领域都得到了广泛应用。
在新材料制备过程经常需要利用纳米原材料制备复合材料，为了使更微小粒径的陶瓷材料分散在纳米技术原材料中，对平均粒径小于100μm(甚至更小)的陶瓷微珠需求急速提高(例如参照日本特许第2707528号公报)。另外，在超细研磨或纳米研磨设备中也需要0.1mm或0.2mm的微珠(例如广东某家公司生产的HKZN-98WD型卧式纳米全陶瓷砂磨机)。但这些微珠很难通过传统的滚制成型或压制成型工艺制备；滴定法生产效率低，熔喷法耗能又高。
索进平等利用陶瓷粉料、粘结剂和有机溶剂混合球磨后形成悬浮液浆料，然后通过微滴喷射的形式把料浆喷入油性成型介质中，利用两不相溶液体产生的界面张力作用形成小球。这种方法生产效率低，很难满足工业化大生产，且形成的凝胶球需要洗涤和排胶，工艺上负责，生产成本也就相对更高(专利CN2018112914863，一种陶瓷微球制备方法及其装置)。
邓湘凌采用加热粘结剂制得液态粘结剂，然后把陶瓷主料与液态粘结剂混合，再用针管向聚乙烯醇里滴所述陶瓷材料，利用表面张力的原理凝固成球形。这种方法应该属于实验室方案，很难批量化生产以及控制球径大小(专利CN201910252350X，陶瓷微珠制作方法)。
日本专利2011101579412利用大于等于2微米小于等于100微米的氢氧化铝粉末至火焰中煅烧形成球形氧化铝。专利CN2019110495785中采用氧化锆料浆喷入含有交联剂的油性介质中，使氧化锆浆料液滴中的粘结剂与交联剂反应固化形成氧化锆微球。专利CN2018107328212中使用ZrO(NO3)2.XH2O、六次甲基四胺、尿素、炭黑等混合形成胶液，然后将胶液逐滴分散到硅油中，在硅油中固化得到凝胶微球，洗涤后烘干煅烧。上述这些制备微球的工艺大部分都是利用滴定法，但是这种工艺很难适应规模化生产，而且工艺过程相对复杂，控制难度较大。
发明内容
本发明的目的在于提供一种颗粒尺寸可调的ZTA陶瓷微珠的制备方法，实现了工业规模化生产ZTA陶瓷微球，而且可以通过调整多种工艺条件控制球径大小，制备的ZTA陶瓷微珠球形度高。
本发明所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，步骤如下：
(1)配料：将氧化铝粉、氧化锆、粘土、氧化镁、稀土氧化物混合得到陶瓷粉料，并加入陶瓷粉料总质量0.3-2.0％的PVA；
(2)球磨：将步骤(1)中混合后的粉料放入球磨机中球磨10-20h，制成固含量为30-65％的料浆；
(3)雾化造粒：将料浆经离心喷塔雾化造粒，制成球形造粒粉；
(4)除铁：将球形造粒粉进行除铁；
(5)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，得到ZTA陶瓷微珠。
步骤(1)中，以重量份数计，陶瓷粉料配比为：
Figure BDA0002545621500000021
PVA的聚合度为500-2400，醇解度86-99％。
氧化铝粉为α-Al2O3，中位粒径为0.3-2.0μm，Na2O含量小于0.1wt％。
稀土氧化物为氧化镧、氧化铈、氧化钕中的一种或多种。
步骤(1)中，氧化锆粉混合前单独球磨3-10h，打开其软团聚或硬团聚。
步骤(2)中，料浆流动性为10-25S，中位粒径为0.5-1.5μm。
步骤(3)中，料浆进入离心喷塔前需要进行除铁。
步骤(3)中，离心喷塔的进口温度为270-320℃，出口温度为75-110℃，雾化器转速为8000-16000r/min，料浆流速为1-3L/min。
步骤(5)中，匣钵装载量为匣钵高度的1/3-1/2，煅烧温度1500-1560℃，保温时间150-350min，推车速度为25-40min/板。
本发明可通过控制料浆粘度、雾化转速、喷塔负压等多种方式控制球径大小，料浆粘度越高形成的雾滴尺寸越大，得到的ZTA球尺寸也更大；雾化器转速越高，料浆撕裂形成的雾滴就越小，得到的ZTA微珠尺寸也就越小；塔内负压的形成是靠引风机的抽力形成，抽力越大，负压越大，那一些小颗粒可以通过风机的作用把小颗粒抽离出来，剩下的颗粒也就相对更匀更大。
与现有技术相比，本发明具有以下有益效果：
(1)本发明利用离心喷塔雾化原理制备出小粒径微珠，离心得到的造粒粉含水率很低(小于0.8％)，不需要通过干燥，直接煅烧即可制得ZTA陶瓷微珠，工艺过程简便，生产设备简单，且生产过程运动部件很少，基本不需要维修，减少了设备投入和维修成本；
(2)本发明与现有大部分微球制备方法相比(滴定法、熔融喷吹法、溶胶凝胶法等)工艺过程简短，可控性较强，而且可以通过控制料浆粘度、雾化转速、料浆浓度、喷塔负压等多种方式控制球径大小，制备的ZTA陶瓷微珠球形度高。
附图说明
图1是本发明实施例1所得ZTA陶瓷微珠的图片；
图2是本发明实施例1-5所得不同大小ZTA陶瓷微珠的累积分布图。
具体实施方式
实施例1
(1)配料：将氧化铝粉76份、氧化锆21份、粘土2份、氧化镁0.5份、稀土氧化物0.5份等物料按照设定比例配好备用，并同时往上述粉料中加入0.6份牌号为21-99的PVA；
(2)球磨：将按比例称取好的粉料放入球磨机中球磨15h，制成固含量为65％的料浆，流动性为10-25S，中位粒径为0.5-1.5μm；
(3)雾化造粒：将料浆先经除铁器除铁，再进入离心喷塔雾化造粒，离心喷塔进口温度285℃，出口温度85℃，料浆流速1.5L/min，雾化器转速8000r/min，制成球形造粒粉，并进一步除铁；
(4)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，烧成温度1560℃，保温150min，得到ZTA陶瓷微珠。
实施例1制备的ZTA陶瓷微珠的外观与微观形貌如图1所示，其颗粒形貌为球形，且颗粒大小均匀。
实施例2
(1)配料：将氧化铝粉80份、氧化锆18份、粘土1份、氧化镁0.3份、稀土氧化物0.7份等物料按照设定比例配好备用，并同时往上述粉料中加入1.5份牌号为17-88的PVA；
(2)球磨：将按比例称取好的粉料放入球磨机中球磨18h，制成固含量为45％的料浆，流动性为10-25S，中位粒径为0.5-1.5μm；
(3)雾化造粒：将料浆先经除铁器除铁，再进入离心喷塔雾化造粒，离心喷塔进口温度310℃，出口温度75℃，料浆流速2L/min，雾化器转速12000r/min，制成球形造粒粉，并进一步除铁；
(4)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，烧成温度1530℃，保温200min，得到ZTA陶瓷微珠。
实施例3
(1)配料：将氧化铝粉72.5份、氧化锆25份、粘土1.0份、氧化镁0.5份、稀土氧化物1.0份等物料按照设定比例配好备用，并同时往上述粉料中加入1.0份牌号为17-99的PVA
(2)球磨：将按比例称取好的粉料放入球磨机中球磨15h，制成固含量为40％的料浆，流动性为10-25S，中位粒径为0.5-1.5μm；
(3)雾化造粒：将料浆先经除铁器除铁，再进入离心喷塔雾化造粒，离心喷塔进口温度300℃，出口温度90℃，料浆流速2.5L/min，雾化器转速14000r/min，制成球形造粒粉，并进一步除铁；
(4)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，烧成温度1540℃，保温250min，得到ZTA陶瓷微珠。
实施例4
(1)配料：将氧化铝粉66份、氧化锆30份、粘土2.5份、氧化镁0.5份、稀土氧化物1.0份等物料按照设定比例配好备用，并同时往上述粉料中加入0.4份牌号为24-99的PVA；
(2)球磨：将按比例称取好的粉料放入球磨机中球磨10h，制成固含量为55％的料浆，流动性为10-25S，中位粒径为0.5-1.5μm；
(3)雾化造粒：将料浆先经除铁器除铁，再进入离心喷塔雾化造粒，离心喷塔进口温度295℃，出口温度85℃，料浆流速2L/min，雾化器转速15000r/min，制成球形造粒粉，并进一步除铁；
(4)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，烧成温度1540℃，保温250min，得到ZTA陶瓷微珠。
实施例5
(1)配料：将氧化铝粉75份、氧化锆21份、粘土2.0份、氧化镁0.5份、稀土氧化物1.5份等物料按照设定比例配好备用，并同时往上述粉料中加入2.0份牌号为05-99的PVA；
(2)球磨：将按比例称取好的粉料放入球磨机中球磨20h，制成固含量为35％的料浆，流动性为10-25S，中位粒径为0.5-1.5μm；
(3)雾化造粒：将料浆先经除铁器除铁，再进入离心喷塔雾化造粒，离心喷塔进口温度320℃，出口温度110℃，料浆流速3L/min，雾化器转速16000r/min，制成球形造粒粉，并进一步除铁；
(4)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，烧成温度1500℃，保温350min，得到ZTA陶瓷微珠。
实施例1-5制备的ZTA陶瓷微珠的性能指标如表1所示。
表1实施例1-5制备的ZTA陶瓷微珠的性能指标
项目 实施例1 实施例2 实施例3 实施例4 实施例5
Na<sub>2</sub>O含量，％ 0.06 0.08 0.06 0.05 0.06
密度，g/cm<sup>3</sup> 4.28 4.26 4.30 4.35 4.25
平均粒径D50，μm 130.03 96.54 69.49 52.86 41.58
颗粒形貌 球形 球形 球形 球形 球形

Claims (10)

1.一种颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤如下：
(1)配料：将氧化铝粉、氧化锆、粘土、氧化镁、稀土氧化物混合得到陶瓷粉料，并加入陶瓷粉料总质量0.3-2.0％的PVA；
(2)球磨：将步骤(1)中混合后的粉料放入球磨机中球磨，制成料浆；
(3)雾化造粒：将料浆经离心喷塔雾化造粒，制成球形造粒粉；
(4)除铁：将球形造粒粉进行除铁；
(5)烧成：将除铁后的球形造粒粉装入高温匣钵放入推板窑中进行煅烧，得到ZTA陶瓷微珠。
2.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(1)中，以重量份数计，陶瓷粉料配比为：
Figure FDA0002545621490000011
3.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：PVA的聚合度为500-2400，醇解度86-99％。
4.根据权利要求1或2所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：氧化铝粉为α-Al2O3，中位粒径为0.3-2.0μm，Na2O含量小于0.1wt％。
5.根据权利要求1或2所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：稀土氧化物为氧化镧、氧化铈、氧化钕中的一种或多种。
6.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(1)中，氧化锆粉混合前单独球磨3-10h。
7.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(2)中，料浆流动性为10-25S，中位粒径为0.5-1.5μm，固含量为30-65％。
8.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(3)中，料浆进入离心喷塔前需要进行除铁。
9.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(3)中，离心喷塔的进口温度为270-320℃，出口温度为75-110℃，雾化器转速为8000-16000r/min，料浆流速为1-3L/min。
10.根据权利要求1所述的颗粒尺寸可调的ZTA陶瓷微珠的制备方法，其特征在于：步骤(5)中，匣钵装载量为匣钵高度的1/3-1/2，煅烧温度1500-1560℃，保温时间150-350min，推车速度为25-40min/板。
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