CN112608145A - 一种无铅压电陶瓷材料的制备方法 - Google Patents
一种无铅压电陶瓷材料的制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 39
- 239000002002 slurry Substances 0.000 claims abstract description 36
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000005469 granulation Methods 0.000 claims abstract description 22
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000000853 adhesive Substances 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 229920003023 plastic Polymers 0.000 claims abstract description 9
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 5
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
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- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 4
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 4
- 238000007723 die pressing method Methods 0.000 claims description 4
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- 239000011656 manganese carbonate Substances 0.000 claims description 4
- 229940093474 manganese carbonate Drugs 0.000 claims description 4
- 235000006748 manganese carbonate Nutrition 0.000 claims description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 4
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims description 4
- 239000012778 molding material Substances 0.000 claims description 4
- 229910000484 niobium oxide Inorganic materials 0.000 claims description 4
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
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- 238000007873 sieving Methods 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
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- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 abstract description 3
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Abstract
本发明提供一种无铅压电陶瓷材料的制备方法，包括以下步骤：（1）配料：按如下重量百分比的原料选料配比：碳酸钡BaCO3：67~68%、钛白粉TiO2：29~30%、稀土：3~3.1%；（2）混料：使用球磨机加入去离子水将各种原材料磨成粒径为1～3um的一次浆料；（3）烘干；（4）破碎；（5）预烧；（6）二次球磨；（7）离心造粒：在所述二次浆料中加入粘合剂并配以搅拌，将搅拌后的二次浆料送入喷雾塔内并控制其温度，进行喷雾造粒；（8）成型；（9）排塑；（10）烧结。通过本发明，以解决现有技术存在的压电陶瓷材料中含有铅金属，重金属污染的问题。
Description
技术领域
本发明涉及压电陶瓷材料技术领域，具体地说涉及一种无铅压电陶瓷材料的制备方法。
背景技术
现有换能器（超声波振子）所用的压电陶瓷材料中大量含有铅成分。在生产的过程中，对工人呼吸系统极其有害，对环境的破坏，废料污染釉导致重金属污染、烧制过程中铅粉挥发对空气的污染。而现有生产出来的低铅含量的压电陶瓷材料的居里温度低，Kt值低，无法用在大功率清洗换能器上。
发明内容
本发明提供一种无铅压电陶瓷材料的制备方法，以解决现有技术存在的压电陶瓷材料中含有铅金属，重金属污染的问题。
为解决上述技术问题，本发明提供一种无铅压电陶瓷材料的制备方法，包括以下步骤：
（1）配料：按如下重量百分比的原料选料配比：碳酸钡BaCO3：67~68%、钛白粉TiO2：29~30%、稀土：3~3.1%；
（2）混料：使用球磨机加入去离子水将各种原材料磨成粒径为1～3um的一次浆料；
（3）烘干：将所述一次浆料放入恒温循环烘箱内，将水分蒸发成料块；
（4）破碎：将烘干后的料块进行破碎，并且能过20目筛；
（5）预烧：将料块进行预烧，预烧温度为1250℃，预烧时间为3～5h；
（6）二次球磨：使用球磨机将预烧后的料块加入去离子水磨成粒径为1～3um的料浆，将所述料浆置于砂磨机内磨成粒径为0.5～8um的二次浆料；
（7）离心造粒：在所述二次浆料中加入粘合剂并配以搅拌，将搅拌后的二次浆料送入喷雾塔内并控制其温度，进行喷雾造粒；
（8）成型：将喷雾造粒获得的粉体使用模压工艺成型；
（9）排塑：将成型后的材料加热至600～800°C，并保持10-30min；
（10）烧结：将排塑处理后的成型材料送至烧结炉中烧结，烧结温度为1320~1350℃，烧结时间为2～2.5h。
优选地，所述配料中稀土包括氧化铌、氧化铋、碳酸锰、碳酸钠。
优选地，所述离心造粒中加入的粘合剂的重量为原料重量的6.5％。
优选地，所述离心造粒中喷雾塔进口温度控制在250～300°C，出口温度控制在100°C～120°C。
优选地，所述粘合剂的配方为：聚乙烯醇15％、甘油7％、酒精3％、蒸馏水75％。
本发明带来的有益效果：与现有技术相比，本发明制备的压电陶瓷材料具有良好的稳定性和机械强度，满足大功率清洗换能器的材料特性要求，Kt＞0.4，居里温度高；同时制备原料中不含有铅的成分，减少了重金属污染，减少了对生产工人呼吸系统的伤害。
附图说明
图1是根据本发明实施例的无铅压电陶瓷粉料化学合成后结晶断裂状态的SEM图。
图2是普通压电陶瓷材料制作出的元器件的特性数据图。
图3是根据本发明实施例的无铅压电陶瓷材料制作出的元器件的特性数据图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚，以下结合附图及具体实施例，对本发明作进一步地详细说明。
实施例一：
一种无铅压电陶瓷材料的制备方法，包括以下步骤：
（1）配料：按如下重量百分比的原料选料配比：碳酸钡BaCO3：67%、钛白粉TiO2：30%、稀土：3%；
（2）混料：使用球磨机加入去离子水将各种原材料磨成粒径为1um的一次浆料；
（3）烘干：将所述一次浆料放入恒温循环烘箱内，将水分蒸发成料块；
（4）破碎：将烘干后的料块进行破碎，并且能过20目筛；
（5）预烧：将料块进行预烧，预烧温度为1250℃，预烧时间为5h；
（6）二次球磨：使用球磨机将预烧后的料块加入去离子水磨成粒径为1um的料浆，将所述料浆置于砂磨机内磨成粒径为0.5um的二次浆料；
（7）离心造粒：在所述二次浆料中加入粘合剂并配以搅拌，将搅拌后的二次浆料送入喷雾塔内并控制其温度，进行喷雾造粒；
（8）成型：将喷雾造粒获得的粉体使用模压工艺成型；
（9）排塑：将成型后的材料加热至600°C，并保持10min；
（10）烧结：将排塑处理后的成型材料送至烧结炉中烧结，烧结温度为1320℃，烧结时间为2h。
所述配料中稀土包括氧化铌、氧化铋、碳酸锰、碳酸钠。
所述离心造粒中加入的粘合剂的重量为原料重量的6.5％。
所述离心造粒中喷雾塔进口温度控制在250°C，出口温度控制在100°C。
所述粘合剂的配方为：聚乙烯醇15％、甘油7％、酒精3％、蒸馏水75％。
实施例二：
一种无铅压电陶瓷材料的制备方法，包括以下步骤：
（1）配料：按如下重量百分比的原料选料配比：碳酸钡BaCO3：67.9%、钛白粉TiO2：29%、稀土：3.1%；
（2）混料：使用球磨机加入去离子水将各种原材料磨成粒径为3um的一次浆料；
（3）烘干：将所述一次浆料放入恒温循环烘箱内，将水分蒸发成料块；
（4）破碎：将烘干后的料块进行破碎，并且能过20目筛；
（5）预烧：将料块进行预烧，预烧温度为1250℃，预烧时间为5h；
（6）二次球磨：使用球磨机将预烧后的料块加入去离子水磨成粒径为3um的料浆，将所述料浆置于砂磨机内磨成粒径为8um的二次浆料；
（7）离心造粒：在所述二次浆料中加入粘合剂并配以搅拌，将搅拌后的二次浆料送入喷雾塔内并控制其温度，进行喷雾造粒；
（8）成型：将喷雾造粒获得的粉体使用模压工艺成型；
（9）排塑：将成型后的材料加热至800°C，并保持30min；
（10）烧结：将排塑处理后的成型材料送至烧结炉中烧结，烧结温度为1350℃，烧结时间为2.5h。
所述配料中稀土包括氧化铌、氧化铋、碳酸锰、碳酸钠。
所述离心造粒中加入的粘合剂的重量为原料重量的6.5％。
所述离心造粒中喷雾塔进口温度控制在300°C，出口温度控制在120°C。
所述粘合剂的配方为：聚乙烯醇15％、甘油7％、酒精3％、蒸馏水75％。
最后，采用上述无铅压电陶瓷材料，根据需要生产的产品尺寸要求生产元器件。
实验方法：分别设置对照组与实验组，对照组采用传统工艺生产的压电陶瓷材料制造的元器件，实验组采用本发明实施例二方法生产的无铅压电陶瓷材料制造的元器件，每组设置10个小组，测试收集每个小组元器件的Kt值、居里温度等。
实验结果：从对照组与实验组的对比可以看出，实验组每个小组的Kt值均大于0.4，对照组的Kt值小于0.4，实验组的居里温度相对对照组提高了40％，压电陶瓷材料的性能得到了提高。
综上所述，本发明制备的压电陶瓷材料具有良好的稳定性和机械强度，满足大功率清洗换能器的材料特性要求，Kt＞0.4，居里温度高；同时制备原料中不含有铅的成分，减少了重金属污染，减少了对生产工人呼吸系统的伤害。
以上所述仅为本发明的实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的权利要求范围之内。
Claims (5)
1.一种无铅压电陶瓷材料的制备方法，其特征在于：包括以下步骤：
（1）配料：按如下重量百分比的原料选料配比：碳酸钡BaCO3：67~68%、钛白粉TiO2：29~30%、稀土：3~3.1%；
（2）混料：使用球磨机加入去离子水将各种原材料磨成粒径为1～3um的一次浆料；
（3）烘干：将所述一次浆料放入恒温循环烘箱内，将水分蒸发成料块；
（4）破碎：将烘干后的料块进行破碎，并且能过20目筛；
（5）预烧：将料块进行预烧，预烧温度为1250℃，预烧时间为3～5h；
（6）二次球磨：使用球磨机将预烧后的料块加入去离子水磨成粒径为1～3um的料浆，将所述料浆置于砂磨机内磨成粒径为0.5～8um的二次浆料；
（7）离心造粒：在所述二次浆料中加入粘合剂并配以搅拌，将搅拌后的二次浆料送入喷雾塔内并控制其温度，进行喷雾造粒；
（8）成型：将喷雾造粒获得的粉体使用模压工艺成型；
（9）排塑：将成型后的材料加热至600～800°C，并保持10-30min；
（10）烧结：将排塑处理后的成型材料送至烧结炉中烧结，烧结温度为1320~1350℃，烧结时间为2～2.5h。
2.如权利要求1所述的无铅压电陶瓷材料的制备方法，其特征在于，所述配料中稀土包括氧化铌、氧化铋、碳酸锰、碳酸钠。
3.如权利要求1所述的无铅压电陶瓷材料的制备方法，其特征在于，所述离心造粒中加入的粘合剂的重量为原料重量的6.5％。
4.如权利要求1所述的无铅压电陶瓷材料的制备方法，其特征在于，所述离心造粒中喷雾塔进口温度控制在250～300°C，出口温度控制在100°C～120°C。
5.如权利要求3所述的无铅压电陶瓷材料的制备方法，其特征在于，所述粘合剂的配方为：聚乙烯醇15％、甘油7％、酒精3％、蒸馏水75％。
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