CN113582693A - 一种陶瓷雾化片材料及其制备方法 - Google Patents

一种陶瓷雾化片材料及其制备方法 Download PDF

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CN113582693A
CN113582693A CN202110889202.6A CN202110889202A CN113582693A CN 113582693 A CN113582693 A CN 113582693A CN 202110889202 A CN202110889202 A CN 202110889202A CN 113582693 A CN113582693 A CN 113582693A
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piezoelectric ceramic
conductive coating
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silicon dioxide
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CN113582693B (zh
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方豪杰
贺亦文
张晓云
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Hunan Meicheng Ceramic Technology Co ltd
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Abstract

本发明涉及陶瓷材料领域，具体为一种陶瓷雾化片材料及其制备方法，由压电陶瓷片体和导电涂层组成；所述压电陶瓷片体由以下化学结构式表示：xPb(Zr0.5Ti0.5)O3‑(1‑x)Pb(Ni0.5Nb0.5)O3‑αwt％CeO2‑βwt％Co2O3其中，x表示摩尔百分比，αwt％、βwt％分别表示CeO2、Co2O3占xPb(Zr0.5Ti0.5)O3‑yPb(Ni0.5Nb0.5)O3的质量百分数；x为0.65‑0.80，α为0.5‑1，β为0.1‑0.2；所述导电涂层为二氧化硅负载银导电涂层，本发明所制备的陶瓷雾化片材料不仅具有优良的力学和电学性能，而且使用寿命长，雾化效果好，有广阔的市场应用前景。

Description

一种陶瓷雾化片材料及其制备方法
技术领域
本发明涉及陶瓷材料领域，具体涉及一种陶瓷雾化片材料及其制备方法。
背景技术
压电陶瓷是一种特殊功能陶瓷材料，能够实现机械能和电能的相互转换，属于无机非金属材料。压电陶瓷广泛应用于雾化器、传感器、换能器等多种器件的制作，其应用领域涉及医疗、电子、精密控制等各个方面。压电陶瓷驱动的雾化器近年来发展迅速，特别是在雾化加湿器和医疗雾化吸入治疗方面应用广泛。此种雾化器利用压电陶瓷逆效应，通过电能转化为机械能，迫使液体通过微米级小孔形成喷雾，与其他种类的雾化器相比，压电陶瓷雾化器产生的雾滴直径小且均匀，工作时噪声小、功率小、效率高，且对药物的药性和活性几乎无影响。
作为电介质材料之一，压电陶瓷本身是不导电的，作为雾化片使用前需要为压电陶瓷的两面被覆上电极，目前一般是丝网刷银浆作为电极，但是在压电陶瓷表面的导电银层附着力较差，在长时间工作后易脱落，既影响雾化效果，雾化片的使用寿命也不高。
发明内容
发明目的：针对现有技术的缺陷或改进需求，本发明提供了一种陶瓷雾化片材料及其制备方法。
本发明所采用的技术方案如下：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
所述压电陶瓷片体由以下化学结构式表示：
xPb(Zr0.5Ti0.5)O3-(1-x)Pb(Ni0.5Nb0.5)O3-αwt％CeO2-βwt％Co2O3
其中，x表示摩尔百分比，αwt％、βwt％分别表示CeO2、Co2O3占xPb(Zr0.5Ti0.5)O3-yPb(Ni0.5Nb0.5)O3的质量百分数；
x为0.65-0.80，α为0.5-1，β为0.1-0.2；
所述导电涂层为二氧化硅负载银导电涂层。
进一步的，所述二氧化硅负载银导电涂层位于压电陶瓷片体的相对面。
进一步的，所述二氧化硅负载银导电涂层的厚度为250-600μm。
进一步的，x为0.80，α为0.5，β为0.2。
进一步的，所述二氧化硅负载银导电涂层由以下原料制备而成：
二氧化硅负载银颗粒、乙醇、松油醇、乙基纤维素、氢化蓖麻油、硅烷偶联剂、聚二甲基硅氧烷、CBS微晶玻璃粉。
进一步的，所述二氧化硅负载银导电涂层由以下重量份数的原料制备而成：
二氧化硅负载银颗粒5-10份、乙醇20-30份、松油醇40-50份、乙基纤维素1-3份、氢化蓖麻油0.1-1份、硅烷偶联剂0.1-1份、聚二甲基硅氧烷0.1-1份、CBS微晶玻璃粉10-20份。
进一步的，所述二氧化硅负载银颗粒的制备方法如下：
S1：搅拌下将硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用；
S2：将二氧化硅空心微球加入水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出；
S3：将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于50-60℃下保温10-20min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
S1：将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨5-10h后烘干，900-950℃预烧2-3h后，恢复室温后二次球磨5-10h，烘干，造粒、制片后，升温至500-550℃保温排胶1-2h后再升温至1250-1300℃烧结2-3h，得到压电陶瓷片体；
S2：将压电陶瓷片体用混酸蚀刻后水洗至中性，烘干；
S3：在压电陶瓷片体的相对面涂覆二氧化硅负载银导电涂层，升温至750-850℃烘制10-30min即可。
进一步的，所述混酸由氢氟酸和浓硝酸组成。
进一步的，蚀刻时间为90-100s。
本发明的有益效果：
本发明提供了一种陶瓷雾化片材料，压电陶瓷片体和导电涂层具有很高的结合强度，导电涂层不易脱落，雾化效果好，雾化片的使用寿命高，使用二氧化硅负载银颗粒一方面增加了压电陶瓷片体与导电涂层接触面的粗糙度提高了附着力，另一方面采用二氧化硅空心微球，其稳定性好、比表而积大，可以避免在烧银时熔融收缩导致的漏瓷现象，使导电涂层连续性好，均匀程度高，玻璃粉作为电极粘结相，一方面必须保证压电陶瓷片体和导电涂层有较好的粘结力，另一方面还须保证不侵蚀、污染压电陶瓷片体，避免压电性能遭到破坏，发明人通过不断测试选择了CBS微晶玻璃粉，本发明所制备的陶瓷雾化片材料不仅具有优良的力学和电学性能，而且使用寿命长，雾化效果好，有广阔的市场应用前景。
附图说明
图1为本发明实施例1制备陶瓷雾化片材料的SEM图，可以观察到表面的导电涂层连续性好，均匀程度高。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
压电陶瓷片体由以下化学结构式表示：
0.5Pb(Zr0.5Ti0.5)O3-0.5Pb(Ni0.5Nb0.5)O3-0.5wt％CeO2-0.2wt％Co2O3
导电涂层为厚度为250μm的二氧化硅负载银导电涂层，且位于压电陶瓷片体的相对面，互不接触，由以下重量份数的原料制备而成：
二氧化硅负载银颗粒10份、乙醇20份、松油醇40份、乙基纤维素3份、氢化蓖麻油0.1份、硅烷偶联剂0.1份、聚二甲基硅氧烷0.2份、CBS微晶玻璃粉10份。
其中，二氧化硅负载银颗粒的制备方法如下：
搅拌下将物质的量浓度为0.1mol/L的硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用，将二氧化硅空心微球加入5倍于其的水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出，将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于50℃下保温20min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
按照化学结构式称取Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨10h后烘干，900℃预烧2h后，恢复室温后二次球磨10h，烘干，与聚乙烯醇混合造粒、制片后，升温至550℃保温排胶1h后再升温至1250℃烧结3h，得到压电陶瓷片体，将压电陶瓷片体用15wt％氢氟酸和浓硝酸按体积比1:1组成的混酸蚀刻90s后水洗至中性，烘干，在压电陶瓷片体的上下相对面涂覆二氧化硅负载银导电涂层，涂覆过程中注意不要使上下面的导电涂层接触以防发生短路，升温至850℃烘制20min即可。
实施例2：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
压电陶瓷片体由以下化学结构式表示：
0.5Pb(Zr0.5Ti0.5)O3-0.5Pb(Ni0.5Nb0.5)O3-0.5wt％CeO2-0.2wt％Co2O3
导电涂层为厚度为250μm的二氧化硅负载银导电涂层，且位于压电陶瓷片体的相对面，互不接触，由以下重量份数的原料制备而成：
二氧化硅负载银颗粒5份、乙醇20份、松油醇40份、乙基纤维素1份、氢化蓖麻油0.1份、硅烷偶联剂0.1份、聚二甲基硅氧烷0.1份、CBS微晶玻璃粉10份。
其中，二氧化硅负载银颗粒的制备方法如下：
搅拌下将物质的量浓度为0.1mol/L的硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用，将二氧化硅空心微球加入5倍于其的水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出，将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于50℃下保温10min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
按照化学结构式称取Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨5h后烘干，900℃预烧2h后，恢复室温后二次球磨5h，烘干，与聚乙烯醇混合造粒、制片后，升温至500℃保温排胶1h后再升温至1250℃烧结2h，得到压电陶瓷片体，将压电陶瓷片体用15wt％氢氟酸和浓硝酸按体积比1:1组成的混酸蚀刻90s后水洗至中性，烘干，在压电陶瓷片体的上下相对面涂覆二氧化硅负载银导电涂层，涂覆过程中注意不要使上下面的导电涂层接触以防发生短路，升温至800℃烘制10min即可。
实施例3：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
压电陶瓷片体由以下化学结构式表示：
0.5Pb(Zr0.5Ti0.5)O3-0.5Pb(Ni0.5Nb0.5)O3-0.5wt％CeO2-0.2wt％Co2O3
导电涂层为厚度为400μm的二氧化硅负载银导电涂层，且位于压电陶瓷片体的相对面，互不接触，由以下重量份数的原料制备而成：
二氧化硅负载银颗粒10份、乙醇30份、松油醇50份、乙基纤维素3份、氢化蓖麻油1份、硅烷偶联剂1份、聚二甲基硅氧烷1份、CBS微晶玻璃粉20份。
其中，二氧化硅负载银颗粒的制备方法如下：
搅拌下将物质的量浓度为0.1mol/L的硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用，将二氧化硅空心微球加入10倍于其的水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出，将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于60℃下保温20min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
按照化学结构式称取Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨10h后烘干，950℃预烧3h后，恢复室温后二次球磨10h，烘干，与聚乙烯醇混合造粒、制片后，升温至550℃保温排胶2h后再升温至1300℃烧结3h，得到压电陶瓷片体，将压电陶瓷片体用15wt％氢氟酸和浓硝酸按体积比1:1组成的混酸蚀刻100s后水洗至中性，烘干，在压电陶瓷片体的上下相对面涂覆二氧化硅负载银导电涂层，涂覆过程中注意不要使上下面的导电涂层接触以防发生短路，升温至850℃烘制30min即可。
实施例4：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
压电陶瓷片体由以下化学结构式表示：
0.5Pb(Zr0.5Ti0.5)O3-0.5Pb(Ni0.5Nb0.5)O3-0.5wt％CeO2-0.2wt％Co2O3
导电涂层为厚度为500μm的二氧化硅负载银导电涂层，且位于压电陶瓷片体的相对面，互不接触，由以下重量份数的原料制备而成：
二氧化硅负载银颗粒5份、乙醇30份、松油醇40份、乙基纤维素3份、氢化蓖麻油0.1份、硅烷偶联剂0.1份、聚二甲基硅氧烷0.1份、CBS微晶玻璃粉20份。
其中，二氧化硅负载银颗粒的制备方法如下：
搅拌下将物质的量浓度为0.1mol/L的硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用，将二氧化硅空心微球加入5倍于其的水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出，将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于60℃下保温10min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
按照化学结构式称取Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨10h后烘干，900℃预烧3h后，恢复室温后二次球磨5h，烘干，与聚乙烯醇混合造粒、制片后，升温至550℃保温排胶1h后再升温至1300℃烧结2h，得到压电陶瓷片体，将压电陶瓷片体用15wt％氢氟酸和浓硝酸按体积比1:1组成的混酸蚀刻100s后水洗至中性，烘干，在压电陶瓷片体的上下相对面涂覆二氧化硅负载银导电涂层，涂覆过程中注意不要使上下面的导电涂层接触以防发生短路，升温至800℃烘制30min即可。
实施例5：
一种陶瓷雾化片材料，由压电陶瓷片体和导电涂层组成；
压电陶瓷片体由以下化学结构式表示：
0.5Pb(Zr0.5Ti0.5)O3-0.5Pb(Ni0.5Nb0.5)O3-0.5wt％CeO2-0.2wt％Co2O3
导电涂层为厚度为250μm的二氧化硅负载银导电涂层，且位于压电陶瓷片体的相对面，互不接触，由以下重量份数的原料制备而成：
二氧化硅负载银颗粒10份、乙醇20份、松油醇50份、乙基纤维素1份、氢化蓖麻油1份、硅烷偶联剂0.1份、聚二甲基硅氧烷1份、CBS微晶玻璃粉10份。
其中，二氧化硅负载银颗粒的制备方法如下：
搅拌下将物质的量浓度为0.1mol/L的硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用，将二氧化硅空心微球加入10倍于其的水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出，将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于50℃下保温20min，取出水洗再烘干即可。
上述陶瓷雾化片材料的制备方法如下：
按照化学结构式称取Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨5h后烘干，950℃预烧2h后，恢复室温后二次球磨10h，烘干，与聚乙烯醇混合造粒、制片后，升温至500℃保温排胶2h后再升温至1250℃烧结3h，得到压电陶瓷片体，将压电陶瓷片体用15wt％氢氟酸和浓硝酸按体积比1:1组成的混酸蚀刻90s后水洗至中性，烘干，在压电陶瓷片体的上下相对面涂覆二氧化硅负载银导电涂层，涂覆过程中注意不要使上下面的导电涂层接触以防发生短路，升温至800℃烘制10min即可。
对比例1
对比例1与实施例1完全相同，区别在于，用银粉代替二氧化硅负载银颗粒。
对比例2
对比例2与实施例1完全相同，区别在于，不加入CBS微晶玻璃粉。
性能测试：
将本发明实施例1-5、对比例1-2所制备的陶瓷雾化片材料分别记为样品1-7，参考标准SJ/T143-1996“被银陶瓷零件”中试验方法对样品1-7中压电陶瓷片体和导电涂层之间的拉脱强度进行测试，测试结果如下表1所示：
表1：
Figure BDA0003195250880000081
Figure BDA0003195250880000091
对样品1-5极化后进行性能测试，测试结果如下表2所示：
表2
Figure BDA0003195250880000092
由上表1和表2可知，本发明所制备的陶瓷雾化片材料具有优良的力学和电学性能，使用寿命长，雾化效果好，有广阔的市场应用前景。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。

Claims (10)

1.一种陶瓷雾化片材料，其特征在于，由压电陶瓷片体和导电涂层组成；
所述压电陶瓷片体由以下化学结构式表示：
xPb(Zr0.5Ti0.5)O3-(1-x)Pb(Ni0.5Nb0.5)O3-αwt％CeO2-βwt％Co2O3
其中，x表示摩尔百分比，αwt％、βwt％分别表示CeO2、Co2O3占xPb(Zr0.5Ti0.5)O3-yPb(Ni0.5Nb0.5)O3的质量百分数；
x为0.65-0.80，α为0.5-1，β为0.1-0.2；
所述导电涂层为二氧化硅负载银导电涂层。
2.如权利要求1所述的陶瓷雾化片材料，其特征在于，所述二氧化硅负载银导电涂层位于压电陶瓷片体的相对面。
3.如权利要求1所述的陶瓷雾化片材料，其特征在于，所述二氧化硅负载银导电涂层的厚度为250-600μm。
4.如权利要求1所述的陶瓷雾化片材料，其特征在于，x为0.80，α为0.5，β为0.2。
5.如权利要求1所述的陶瓷雾化片材料，其特征在于，所述二氧化硅负载银导电涂层由以下原料制备而成：
二氧化硅负载银颗粒、乙醇、松油醇、乙基纤维素、氢化蓖麻油、硅烷偶联剂、聚二甲基硅氧烷、CBS微晶玻璃粉。
6.如权利要求5所述的陶瓷雾化片材料，其特征在于，所述二氧化硅负载银导电涂层由以下重量份数的原料制备而成：
二氧化硅负载银颗粒5-10份、乙醇20-30份、松油醇40-50份、乙基纤维素1-3份、氢化蓖麻油0.1-1份、硅烷偶联剂0.1-1份、聚二甲基硅氧烷0.1-1份、CBS微晶玻璃粉10-20份。
7.如权利要求5所述的陶瓷雾化片材料，其特征在于，所述二氧化硅负载银颗粒的制备方法如下：
S1：搅拌下将硝酸银溶液加入到氨水中，直至体系由浑浊变澄清，得到溶液A待用；
S2：将二氧化硅空心微球加入水中，搅拌下将乙二醛、三乙醇胺加入，搅拌均匀后，将其滤出；
S3：将溶液A均匀喷洒至上述二氧化硅空心微球表面，再于50-60℃下保温10-20min，取出水洗再烘干即可。
8.如权利要求1-7任一项所述的陶瓷雾化片材料的制备方法，其特征在于，具体如下：
S1：将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、CeO2、Co2O3混合球磨5-10h后烘干，900-950℃预烧2-3h后，恢复室温后二次球磨5-10h，烘干，造粒、制片后，升温至500-550℃保温排胶1-2h后再升温至1250-1300℃烧结2-3h，得到压电陶瓷片体；
S2：将压电陶瓷片体用混酸蚀刻后水洗至中性，烘干；
S3：在压电陶瓷片体的相对面涂覆二氧化硅负载银导电涂层，升温至750-850℃烘制10-30min即可。
9.如权利要求8所述的陶瓷雾化片材料的制备方法，其特征在于，所述混酸由氢氟酸和浓硝酸组成。
10.如权利要求8所述的陶瓷雾化片材料的制备方法，其特征在于，蚀刻时间为90-100s。
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