CN112281222A - 一种静电纺丝法制备压电陶瓷粉的工艺 - Google Patents

一种静电纺丝法制备压电陶瓷粉的工艺 Download PDF

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CN112281222A
CN112281222A CN202011168276.2A CN202011168276A CN112281222A CN 112281222 A CN112281222 A CN 112281222A CN 202011168276 A CN202011168276 A CN 202011168276A CN 112281222 A CN112281222 A CN 112281222A
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piezoelectric ceramic
ceramic powder
electrostatic spinning
pvp
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段连威
彭大松
王晓东
李文文
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Chinese Sensor Technology (qingdao) Academy Of Science
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/62227—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/06—Washing or drying
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Fibers (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

本发明专利公布一种静电纺丝法制备压电陶瓷粉的方法，发明专利涉及一种多层压电陶瓷的制备工艺，该方法通过静电纺丝法，制备出颗粒直径在50~80nm纤维状压电陶瓷粉。依照此方法制备出的压电陶瓷粉烧结温度在550~600℃，可以极大降低压电陶瓷粉的烧结温度。

Description

一种静电纺丝法制备压电陶瓷粉的工艺
技术领域
本发明涉及压电陶瓷片的制备领域，尤其涉及压电陶瓷粉的制备。
背景技术
自压电效应发现以来，在各行业获得了广泛的应用，随着压电陶瓷技术的不断研究与应用，压电陶瓷材料已经成为电子、信息、医疗、航空航天等领域不可或缺的一部分。目前压电陶瓷粉制备多采用固相烧结法，固相法制备压电陶瓷工艺复杂，烧结温度高，且生产的压电陶瓷粉颗粒大。压电陶瓷粉颗粒的大小直接影响压电陶瓷器件性能，尤其在使用压电陶瓷粉制备陶瓷流延膜带工艺中，使用固相烧结法制备的压电陶瓷粉无法做出厚度小于20μm的流延膜带。
静电纺丝是利用高压静电将聚合物溶液拉伸细化,最终获得超细纤维的加工方法。
（一）解决的技术问题
本专利使用静电纺丝法制备压电陶瓷粉，工艺简单，烧结温度较低，压电陶瓷粉颗粒直径在50~80nm，为流延法制备20μm厚度以下膜带提供可能性。
（二）技术方案
为实现以上目的，本发明通过以下技术方案予以实现：一种静电纺丝法制备压电陶瓷粉的工艺，具体包括以下步骤：
步骤一、按组成比例称取压电陶瓷粉原料，加入到DMF中，在磁力搅拌器上搅拌溶解，搅拌温度为40~50℃，搅拌时间为2~3h；
步骤二、在搅拌好的溶液中加入PVP后在磁力搅拌器上搅拌溶解，搅拌时间为2~3h；
步骤三、将制备好的前驱体吸入注射器中，直流电压为15~20kV，纺丝速度为1m/μl，接收距离为20~30cm进行静电纺丝；
步骤四、将接收板上的压电陶瓷纤维收取后放入干燥箱中烘干，干燥温度为80~90℃，干燥时间为8~10h；
步骤五、将烘干后的压电陶瓷纤维放在烧结炉中，按既定烧结温度烧结。
优选的所述PVP的相对分子质量为1300000；
优选的所述加入PVP的量：DMF:PVP=1ml：(0.12-0.14)g；
（三）有益效果
本发明提供了一种静电纺丝法制备压电陶瓷粉的工艺，制备出了颗粒直径在50~80nm的压电陶瓷粉，制作工艺简单，降低压电陶瓷粉的烧结温度，并节省制作成本。
附图说明
图1为静电纺丝法示意图；
图2为本发明制备出的压电陶瓷粉的扫描电镜图。
其中图一中，1为推进器，2为注射器，3为高压直流电源，4为接收板。
具体实施方式
所描述的实施例仅是本发明一部分实施例，而不是全部实施例。基于本发明中实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得所有其他实施例，都属于本发明保护范围。
本发明实施例提供一种工艺方案：一种静电纺丝法制备压电陶瓷粉，具体包括以下步骤：
步骤一、按组成比例称取压电陶瓷粉原料，加入到DMF中，在磁力搅拌器上搅拌溶解，搅拌温度为40℃，搅拌时间为3h；
步骤二、在搅拌好的溶液中加入PVP，加入PVP的量：DMF:PVP=1ml：0.12g，在磁力搅拌器上搅拌溶解，搅拌时间为3h；
步骤三、将制备好的前驱体吸入注射器中，直流电压为18kV，纺丝速度为1m/μl，接收距离为20cm进行静电纺丝；
步骤四、将接收板上的压电陶瓷纤维收取后放入干燥箱中烘干，干燥温度为90℃，干燥时间为10h；
步骤五、将烘干后的压电陶瓷纤维放在烧结炉中，按既定烧结温度烧结，烧结温度为600℃。
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。

Claims (3)

1.一种静电纺丝法制备压电陶瓷粉的方法，其特征在于：所述制备工艺包括如下步骤：
步骤一、按组成比例称取压电陶瓷粉原料，加入到DMF中，在磁力搅拌器上搅拌溶解，搅拌温度为40~50℃，搅拌时间为2~3h；
步骤二、在搅拌好的溶液中加入PVP，在磁力搅拌器上搅拌溶解，搅拌时间为2~3h；
步骤三、将制备好的前驱体吸入注射器中，直流电压为15~20kV，纺丝速度为1m/μl，接收距离为20~30cm进行静电纺丝；
步骤四、将接收板上的压电陶瓷纤维收取后放入干燥箱中烘干，干燥温度为80~90℃，干燥时间为8~10h；
步骤五、将烘干后的压电陶瓷纤维放在烧结炉中，按既定烧结温度烧结。
2.根据权利要求1静电纺丝法制备压电陶瓷粉，其特征在于：所用PVP的相对分子质量为1300000。
3.据权利要求1静电纺丝法制备压电陶瓷粉，其特征在于：加入PVP的量：DMF:PVP=1ml：(0.12-0.14)g。
CN202011168276.2A 2020-10-28 2020-10-28 一种静电纺丝法制备压电陶瓷粉的工艺 Pending CN112281222A (zh)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102976752A (zh) * 2012-12-05 2013-03-20 景德镇陶瓷学院 一种铌酸钾钠基织构化压电陶瓷水基流延浆料及其陶瓷膜片的制备方法
CN108411406A (zh) * 2018-03-30 2018-08-17 西安理工大学 一种压电光催化复合纤维的制备方法
CN108442038A (zh) * 2018-01-16 2018-08-24 北京科技大学 一种具有高输出的柔性压电纤维薄膜及其制备方法
CN109097864A (zh) * 2018-06-12 2018-12-28 西安理工大学 一种多孔压电阻尼复合材料的制备方法
CN109997238A (zh) * 2016-10-12 2019-07-09 Ntn株式会社 压电元件及其制造方法
CN111621158A (zh) * 2019-12-23 2020-09-04 江苏集萃先进高分子材料研究所有限公司 一种用于选择性激光烧结3d打印的压电硅橡胶材料及其制备方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102976752A (zh) * 2012-12-05 2013-03-20 景德镇陶瓷学院 一种铌酸钾钠基织构化压电陶瓷水基流延浆料及其陶瓷膜片的制备方法
CN109997238A (zh) * 2016-10-12 2019-07-09 Ntn株式会社 压电元件及其制造方法
CN108442038A (zh) * 2018-01-16 2018-08-24 北京科技大学 一种具有高输出的柔性压电纤维薄膜及其制备方法
CN108411406A (zh) * 2018-03-30 2018-08-17 西安理工大学 一种压电光催化复合纤维的制备方法
CN109097864A (zh) * 2018-06-12 2018-12-28 西安理工大学 一种多孔压电阻尼复合材料的制备方法
CN111621158A (zh) * 2019-12-23 2020-09-04 江苏集萃先进高分子材料研究所有限公司 一种用于选择性激光烧结3d打印的压电硅橡胶材料及其制备方法

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