CN107010948A - 一种压电陶瓷纤维的制备方法 - Google Patents

一种压电陶瓷纤维的制备方法 Download PDF

Info

Publication number
CN107010948A
CN107010948A CN201710266533.8A CN201710266533A CN107010948A CN 107010948 A CN107010948 A CN 107010948A CN 201710266533 A CN201710266533 A CN 201710266533A CN 107010948 A CN107010948 A CN 107010948A
Authority
CN
China
Prior art keywords
piezoelectric ceramic
ceramic fibers
preparation
parts
mixing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710266533.8A
Other languages
English (en)
Inventor
吴迪
薛洋
葛明月
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201710266533.8A priority Critical patent/CN107010948A/zh
Publication of CN107010948A publication Critical patent/CN107010948A/zh
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
    • C04B35/491—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates based on lead zirconates and lead titanates, e.g. PZT
    • 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
    • C04B35/62231—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining fibres based on oxide ceramics
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/6268—Thermal treatment of powders or mixtures thereof other than sintering characterised by the applied pressure or type of atmosphere, e.g. in vacuum, hydrogen or a specific oxygen pressure
    • 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
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62844—Coating fibres
    • C04B35/62847—Coating fibres with oxide ceramics
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/092—Forming composite materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N30/00—Piezoelectric or electrostrictive devices
    • H10N30/01—Manufacture or treatment
    • H10N30/09—Forming piezoelectric or electrostrictive materials
    • H10N30/093—Forming inorganic materials
    • H10N30/097—Forming inorganic materials by sintering
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3213—Strontium oxides or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
    • C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/522—Oxidic
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/54—Particle size related information
    • C04B2235/5463—Particle size distributions
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/606—Drying
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Fibers (AREA)

Abstract

本发明属于压电功能材料制备技术领域，具体涉及一种压电陶瓷纤维的制备方法。本发明首先以碳酸锂、钛酸四丁酯等为原料，进行混合加热并过滤，将滤液与柠檬酸溶液混合，经减压蒸馏，得纺丝液，再将纺丝液置于挤出装置中进行挤丝，得到凝胶纤维，接着将锆钛酸铅镧陶瓷粉碎后与粘结剂等混合搅拌，得陶瓷浆料，随后将其与凝胶纤维混合，并依次进行蒸汽处理和高温热解，即可得到压电陶瓷纤维。本发明制备的压电陶瓷纤维强度高，可以承受大的冲击，不易断裂，且也可用于弯曲的平面。

Description

一种压电陶瓷纤维的制备方法
技术领域
本发明属于压电功能材料制备技术领域，具体涉及一种压电陶瓷纤维的制备方法。
背景技术
所谓压电效应有两种，即正压电效应及逆压电效应。当压电体受到电场作用时，电偶极矩会被拉长，压电体会沿电场方向伸长，即将电能转换为机械能。反之，对压电体施加压力，体内的电偶极矩会随材质的压缩而变短，此时压电体内为抵抗这种趋势，将产生电压以保持原状态。因此，压电材料具有机械能与电能之间来回转换的特性。故压电材料广泛地使用于运动感应器、致动器、转换器、微定位器、振动检测以及超音波产生器等用途。传统压电材料多为块材型式，其质地坚硬易碎，机电转换输出受到限制，而局限了压电材料的发展运用。若能将压电材料纤维化，借由纤维化后的高长宽比，以提高其形变能力而大幅增加其压电特性、灵敏度与机电耦合系数，尤其纤维化后的压电材料再结合高弹性树脂材料形成的压电复材可大幅提升其压电性与机械性能，进一步拓展压电材料的运用领域。
利用挤压成型法制造压电陶瓷纤维。该方法将压电陶瓷粉末与粘结剂及交联剂水溶液均匀混合，以形成聚合物胶体。接着，将聚合物胶体借由挤型机挤压成型以形成陶瓷纤维生胚。然后，进行干燥及烧结步骤，即形成压电陶瓷纤维。虽然该方法工艺简单、成本低廉且不会造成环境污染，但是得到的压电陶瓷纤维强度低，无法承受大的冲击，也不能应用于弯曲的平面，因此限制了压电陶瓷纤维的广泛应用。
发明内容
本发明所要解决的技术问题：针对传统的压电陶瓷纤维强度低，无法承受大的冲击，也不能应用于弯曲的平面，因此限制了压电陶瓷纤维的广泛应用的问题，提供了一种压电陶瓷纤维的制备方法。
为解决上述技术问题，本发明采用的技术方案是：
（1）按重量份数计，分别选取5～10份碳酸锂、20～30份钛酸四丁酯、3～5份异丙醇锆、3～5份醋酸溶液、10～20份无水乙醇和50～70份乙二醇单甲醚混合，混合后加入三口烧瓶中，放入油浴锅中，加热反应得反应物；
（2）按质量比1:3将反应物和弱酸溶液混合，在室温下搅拌混合后移入减压浓
缩罐中，减压浓缩后得纺丝液；
（3）将纺丝液移入挤出装置中，将挤出装置升温至100～102℃后通过80～90μm
的微孔，控制挤出速度进行挤出成丝，收集挤出的丝并冷却至室温，即可得到凝胶纤维，备用；
（4）称取锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎，过筛得陶瓷粉末，将陶瓷
粉末加入水中，搅拌混合后再依次加入锆钛酸铅镧陶瓷质量4～6%粘结剂和锆钛酸铅镧陶瓷质量3～5%非离子表面活性剂，并加入分散机中搅拌混合后得陶瓷浆料；
（5）按质量比1:3将步骤（3）备用的凝胶纤维和陶瓷浆料混合，得混合料后放
入蒸汽炉中进行蒸汽处理，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中干燥得干燥物，将干燥物放入马弗炉中，逐步升温至200～300℃、500～600℃和850～950℃，依次在不同温度下保温热解，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
优选的，所述步骤（1）中废弃轮胎颗粒粒径为0.08～0.15mm。
优选的，步骤（2）中所述的弱酸溶液为质量分数3%柠檬酸溶液、质量分数5%苹果酸溶液、质量分数4%醋酸溶液、质量分数5%琥珀酸溶液中的一种或多种。
优选的，步骤（2）中所述的减压浓缩温度为40～50℃，减压浓缩压力为0.05～0.07MPa，减压浓缩时间为1～2h。
优选的，步骤（3）中所述的挤出速度为0.3～0.5m/s。
优选的，步骤（4）
中所述的陶瓷粉末过500～520目筛。
优选的，步骤（4）中所述的粘结剂为羧甲基纤维素、聚偏氟乙烯、聚乙烯吡咯烷酮中的一种或多种。
优选的，步骤（4）中所述的非离子表面活性剂为椰子油脂肪酸单乙醇酰胺、辛基酚聚氧乙烯醚、蔗糖脂肪酸酯中的一种或多种。
优选的，步骤（5）中所述的蒸汽处理温度为80～90℃，蒸汽处理时间为20～22h，所述的保温热解时间为1～2h。
本发明与其他方法相比，有益技术效果是：
（1）本发明将碳酸锂、钛酸四丁酯和异丙醇锆与醋酸等混合后，钛酸四丁酯会进行水解得到的二氧化钛溶胶，并且异丙醇锆在无水乙醇和醋酸条件下水解成氧化锆，并与二氧化钛溶胶结合后与弱酸溶液混合，混合后浓缩，得纺丝液，对纺丝液挤压成丝，在挤出过程中实现微米级单晶纤维的定向排列，成为压电陶瓷纤维中的增强型凝胶纤维，并且经过弱酸处理后，可以增强凝胶与陶瓷浆料之间的结合力；
（2）本发明利用锆钛酸铅镧陶瓷为压电陶瓷的原料，与粘结剂和非离子表面活性剂混合后得陶瓷浆料，可通过粘结剂和非离子表面活性剂的双重作用下可以降低陶瓷浆料的表面张力，可使凝胶纤维和陶瓷浆料混合后达到良好润湿的目的；
（3）本发明通过蒸汽处理，可使凝胶纤维表面覆有陶瓷浆料，通过蒸汽处理，陶瓷浆料进行膨胀和剥分，陶瓷浆料片晶之间有一定空隙，使陶瓷浆料和凝胶纤维间相互叠加组装，从而达到高强度压电陶瓷纤维的目的，本发明制备的压电陶瓷纤维拉伸强度达到26.55MPa以上，可以承受大的冲击，不易断裂；
（4）本发明制备的压电陶瓷纤维可用于弯曲的平面，弹性模量达到7.12×103～8.19×103MPa，饱和场强达到11～15kV/mm、剩余极化强度达到41.4～43.2μC/cm2，矫顽场达到1.10～1.30kV/mm。
具体实施方式
按重量份数计，分别选取5～10份碳酸锂、20～30份钛酸四丁酯、3～5份异丙醇锆、3～5份质量分数36%醋酸溶液、10～20份无水乙醇和50～70份乙二醇单甲醚混合，混合后加入三口烧瓶中，将三口烧瓶放入油浴锅中，加热至140～150℃，以500～700r/min转速进行搅拌反应1～2h后得反应物，按质量比1:3将反应物和弱酸溶液混合，在室温下搅拌混合3～4h后移入减压浓缩罐中，在温度为40～50℃、压力为0.05～0.07MPa下减压浓缩1～2h，浓缩后得纺丝液；将纺丝液移入挤出装置中，将挤出装置升温至100～102℃后通过80～90μm的微孔进行挤出成丝，挤出的速度为0.3～0.5m/s，收集挤出的丝并冷却至室温，即可得到凝胶纤维，再称取100～150g锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎后过500～520目筛得陶瓷粉末，将陶瓷粉末加入200～300g水中，搅拌混合10～15min后再依次加入锆钛酸铅镧陶瓷质量4～6%粘结剂和锆钛酸铅镧陶瓷质量3～5%非离子表面活性剂，并加入分散机中以1000～1200r/min转速搅拌混合20～30min后得陶瓷浆料；按质量比1:3将凝胶纤维和陶瓷浆料混合，得混合料后放入蒸汽炉中，在80～90℃下蒸汽处理20～22h，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中，在60～80℃下干燥8～10h后得干燥物，将干燥物放入马弗炉中，以5～7℃/min速率逐步升温至200～300℃、500～600℃和850～950℃，依次在不同温度下保温热解1～2h，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
所述的弱酸溶液为质量分数3%柠檬酸溶液、质量分数5%苹果酸溶液、质量分数4%醋酸溶液、质量分数5%琥珀酸溶液中的一种或多种。
所述的粘结剂为羧甲基纤维素、聚偏氟乙烯、聚乙烯吡咯烷酮中的一种或多种。所述的非离子表面活性剂为椰子油脂肪酸单乙醇酰胺、辛基酚聚氧乙烯醚、蔗糖脂肪酸酯中的一种或多种。
经检测，本发明制备的高强度压电陶瓷纤维拉伸强度达到26.55MPa以上，弹性模量达到7.12×103～8.19×103MPa，饱和场强达到11～15kV/mm、剩余极化强度达到41.4～43.2μC/cm2，矫顽场达到1.10～1.30kV/mm。
实例1
按重量份数计，分别选取10份碳酸锂、30份钛酸四丁酯、5份异丙醇锆、5份质量分数36%醋酸溶液、20份无水乙醇和70份乙二醇单甲醚混合，混合后加入三口烧瓶中，将三口烧瓶放入油浴锅中，加热至150℃，以700r/min转速进行搅拌反应2h后得反应物，按质量比1:3将反应物和质量分数3%柠檬酸溶液混合，在室温下搅拌混合4h后移入减压浓缩罐中，在温度为50℃、压力为0.07MPa下减压浓缩2h，浓缩后得纺丝液；将纺丝液移入挤出装置中，将挤出装置升温至102℃后通过90μm的微孔进行挤出成丝，挤出的速度为0.5m/s，收集挤出的丝并冷却至室温，即可得到凝胶纤维，再称取150g锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎后过520目筛得陶瓷粉末，将陶瓷粉末加入300g水中，搅拌混合15min后再依次加入锆钛酸铅镧陶瓷质量6%羧甲基纤维素和锆钛酸铅镧陶瓷质量5%椰子油脂肪酸单乙醇酰胺，并加入分散机中以1200r/min转速搅拌混合30min后得陶瓷浆料；按质量比1:3将凝胶纤维和陶瓷浆料混合，得混合料后放入蒸汽炉中，在90℃下蒸汽处理22h，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中，在80℃下干燥10h后得干燥物，将干燥物放入马弗炉中，以7℃/min速率逐步升温至300℃、600℃和950℃，依次在不同温度下保温热解2h，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
经检测，本实例制备的高强度压电陶瓷纤维拉伸强度达到27.68MPa，弹性模量达到7.12×103MPa，饱和场强达到11kV/mm、剩余极化强度达到41.4μC/cm2，矫顽场达到1.10kV/mm。
实例2
按重量份数计，分别选取5份碳酸锂、20份钛酸四丁酯、3份异丙醇锆、3份质量分数36%醋酸溶液、10份无水乙醇和50份乙二醇单甲醚混合，混合后加入三口烧瓶中，将三口烧瓶放入油浴锅中，加热至140℃，以500r/min转速进行搅拌反应1h后得反应物，按质量比1:3将反应物和质量分数5%苹果酸溶液混合，在室温下搅拌混合3h后移入减压浓缩罐中，在温度为40℃、压力为0.05MPa下减压浓缩1h，浓缩后得纺丝液；将纺丝液移入挤出装置中，将挤出装置升温至100℃后通过80μm的微孔进行挤出成丝，挤出的速度为0.3m/s，收集挤出的丝并冷却至室温，即可得到凝胶纤维，再称取100g锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎后过500目筛得陶瓷粉末，将陶瓷粉末加入200g水中，搅拌混合10min后再依次加入锆钛酸铅镧陶瓷质量4%聚偏氟乙烯和锆钛酸铅镧陶瓷质量3%辛基酚聚氧乙烯醚，并加入分散机中以1000r/min转速搅拌混合20min后得陶瓷浆料；按质量比1:3将凝胶纤维和陶瓷浆料混合，得混合料后放入蒸汽炉中，在80℃下蒸汽处理20h，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中，在60℃下干燥8h后得干燥物，将干燥物放入马弗炉中，以5℃/min速率逐步升温至200℃、500℃和850℃，依次在不同温度下保温热解1h，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
经检测，本实例制备的高强度压电陶瓷纤维拉伸强度达到28.26MPa，弹性模量达到8.01×103MPa，饱和场强达到13kV/mm、剩余极化强度达到42.8μC/cm2，矫顽场达到1.20kV/mm。
实例3
按重量份数计，分别选取7份碳酸锂、25份钛酸四丁酯、4份异丙醇锆、4份质量分数36%醋酸溶液、15份无水乙醇和60份乙二醇单甲醚混合，混合后加入三口烧瓶中，将三口烧瓶放入油浴锅中，加热至145℃，以600r/min转速进行搅拌反应1h后得反应物，按质量比1:3将反应物和质量分数5%琥珀酸溶液混合，在室温下搅拌混合3h后移入减压浓缩罐中，在温度为45℃、压力为0.06MPa下减压浓缩1h，浓缩后得纺丝液；将纺丝液移入挤出装置中，将挤出装置升温至101℃后通过85μm的微孔进行挤出成丝，挤出的速度为0.4m/s，收集挤出的丝并冷却至室温，即可得到凝胶纤维，再称取130g锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎后过510目筛得陶瓷粉末，将陶瓷粉末加入250g水中，搅拌混合12min后再依次加入锆钛酸铅镧陶瓷质量5%聚乙烯吡咯烷酮和锆钛酸铅镧陶瓷质量4%椰子油脂肪酸单乙醇酰胺，并加入分散机中以1100r/min转速搅拌混合25min后得陶瓷浆料；按质量比1:3将凝胶纤维和陶瓷浆料混合，得混合料后放入蒸汽炉中，在85℃下蒸汽处理21h，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中，在70℃下干燥9h后得干燥物，将干燥物放入马弗炉中，以6℃/min速率逐步升温至250℃、550℃和900℃，依次在不同温度下保温热解1h，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
经检测，本实例制备的高强度压电陶瓷纤维拉伸强度达到28.65MPa，弹性模量达到8.19×103MPa，饱和场强达到15kV/mm、剩余极化强度达到43.2μC/cm2，矫顽场达到1.30kV/mm。

Claims (9)

1.一种压电陶瓷纤维的制备方法，其特征在于具体制备步骤为：
（1）按重量份数计，分别选取5～10份碳酸锂、20～30份钛酸四丁酯、3～5份异丙醇锆、3～5份醋酸溶液、10～20份无水乙醇和50～70份乙二醇单甲醚混合，混合后加入三口烧瓶中，放入油浴锅中，加热反应得反应物；
（2）按质量比1:3将反应物和弱酸溶液混合，在室温下搅拌混合后移入减压浓
缩罐中，减压浓缩后得纺丝液；
（3）将纺丝液移入挤出装置中，将挤出装置升温至100～102℃后通过80～90μm
的微孔，控制挤出速度进行挤出成丝，收集挤出的丝并冷却至室温，即可得到凝胶纤维，备用；
（4）称取锆钛酸铅镧陶瓷，加入气流粉碎机中粉碎，过筛得陶瓷粉末，将陶瓷
粉末加入水中，搅拌混合后再依次加入锆钛酸铅镧陶瓷质量4～6%粘结剂和锆钛酸铅镧陶瓷质量3～5%非离子表面活性剂，并加入分散机中搅拌混合后得陶瓷浆料；
（5）按质量比1:3将步骤（3）备用的凝胶纤维和陶瓷浆料混合，得混合料后放
入蒸汽炉中进行蒸汽处理，取出蒸汽处理后的凝胶纤维，并放入真空干燥箱中干燥得干燥物，将干燥物放入马弗炉中，逐步升温至200～300℃、500～600℃和850～950℃，依次在不同温度下保温热解，热解后冷却至室温，得热解物，即可得到压电陶瓷纤维。
2.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（1）
中所述的醋酸溶液为质量分数30～35%醋酸溶液，所述的加热反应温度为140～150℃，加热时间为1～2h。
3.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（2）
中所述的弱酸溶液为质量分数3%柠檬酸溶液、质量分数5%苹果酸溶液、质量分数4%醋酸溶液、质量分数5%琥珀酸溶液中的一种或多种。
4.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（2）
中所述的减压浓缩温度为40～50℃，减压浓缩压力为0.05～0.07MPa，减压浓缩时间为1～2h。
5.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（3）
中所述的挤出速度为0.3～0.5m/s。
6.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（4）
中所述的陶瓷粉末过500～520目筛。
7.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（4）
中所述的粘结剂为羧甲基纤维素、聚偏氟乙烯、聚乙烯吡咯烷酮中的一种或多种。
8.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（4）
中所述的非离子表面活性剂为椰子油脂肪酸单乙醇酰胺、辛基酚聚氧乙烯醚、蔗糖脂肪酸酯中的一种或多种。
9.根据权利要求1所述的一种压电陶瓷纤维的制备方法，其特征在于：步骤（5）
中所述的蒸汽处理温度为80～90℃，蒸汽处理时间为20～22h，所述的保温热解时间为1～2h。
CN201710266533.8A 2017-04-21 2017-04-21 一种压电陶瓷纤维的制备方法 Pending CN107010948A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710266533.8A CN107010948A (zh) 2017-04-21 2017-04-21 一种压电陶瓷纤维的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710266533.8A CN107010948A (zh) 2017-04-21 2017-04-21 一种压电陶瓷纤维的制备方法

Publications (1)

Publication Number Publication Date
CN107010948A true CN107010948A (zh) 2017-08-04

Family

ID=59448472

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710266533.8A Pending CN107010948A (zh) 2017-04-21 2017-04-21 一种压电陶瓷纤维的制备方法

Country Status (1)

Country Link
CN (1) CN107010948A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109323783A (zh) * 2018-09-07 2019-02-12 成都新柯力化工科技有限公司 一种用于智能控制的可伸缩性电子皮肤及制备方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1524792A (zh) * 2003-02-28 2004-09-01 新加坡纳米材料科技有限公司 一种制备各种晶态钙钛矿类化合物粉体的方法
CN101214454A (zh) * 2007-12-28 2008-07-09 上海第二工业大学 一种具有双孔分布的大孔氧化铝的制备方法
CN102603306A (zh) * 2012-03-22 2012-07-25 厦门大学 一种压电陶瓷纤维的压力挤出成型方法
US20130285510A1 (en) * 2012-04-26 2013-10-31 Betacer Inc. Method for fabricating piezoelectric composite material and piezoelectric power generating device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1524792A (zh) * 2003-02-28 2004-09-01 新加坡纳米材料科技有限公司 一种制备各种晶态钙钛矿类化合物粉体的方法
CN101214454A (zh) * 2007-12-28 2008-07-09 上海第二工业大学 一种具有双孔分布的大孔氧化铝的制备方法
CN102603306A (zh) * 2012-03-22 2012-07-25 厦门大学 一种压电陶瓷纤维的压力挤出成型方法
US20130285510A1 (en) * 2012-04-26 2013-10-31 Betacer Inc. Method for fabricating piezoelectric composite material and piezoelectric power generating device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
陈照峰: "《无机非金属材料学（第2版）》", 29 February 2016, 西北工业大学出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109323783A (zh) * 2018-09-07 2019-02-12 成都新柯力化工科技有限公司 一种用于智能控制的可伸缩性电子皮肤及制备方法

Similar Documents

Publication Publication Date Title
CN108442038A (zh) 一种具有高输出的柔性压电纤维薄膜及其制备方法
CN102700203B (zh) 一种具有压电阻尼的碳纤维复合材料层合板的制备方法
CN111218841A (zh) 一种纳米芳纶纸基材料及其制备方法和应用
CN109265879B (zh) 一种高定向排布核壳结构纤维聚偏氟乙烯基复合介质及其制备方法
CN109734413A (zh) 一种改性二氧化硅粉体/二氧化硅纳米纤维复合气凝胶材料及其制备方法
CN101144253B (zh) 一种耐高温绝缘连续片材及其制作方法
CN106436016B (zh) 一种石墨烯纤维阻燃导电无纺布及其制备方法
CN103572640A (zh) 一种用对位芳纶沉析纤维制备对位芳纶纸的方法
CN111423698B (zh) 高填充量六方氮化硼纳米片/纤维/聚合物块状复合材料及制备方法
WO2019061273A1 (zh) 一种过滤用棉秆皮纤维与壳聚糖复合非织布的制备方法
CN107010948A (zh) 一种压电陶瓷纤维的制备方法
CN113233466B (zh) 一种3D超弹电纺碳纳米纤维/MXene复合气凝胶及其协同组装制备方法
CN102953288A (zh) 一种对位芳纶浆粕增强聚酰亚胺纤维纸的制备方法
CN109097864A (zh) 一种多孔压电阻尼复合材料的制备方法
CN111622016A (zh) 一种含中空多孔二氧化硅微球的耐压隔热纸及其制备方法
CN201735259U (zh) 一种空气净化用非织造粘合纤维层结构
CN102786307A (zh) 压电陶瓷纤维的制法
CN101639151A (zh) 复合保温云母板及其制作方法
CN105672026B (zh) 一种高性能芳纶绝缘纸及其制备方法与应用
CN111009425A (zh) 一种低噪抗击穿超级电容器
CN110219095A (zh) 一种石墨烯纤维阻燃导电无纺布及其制备方法
WO2020211412A1 (zh) 一种空气热交换器及其制备方法和应用
CN112092412B (zh) 一种纳米二氧化钛/硫掺杂改性纤维体复合材料的制备方法
CN114702305B (zh) 一种可杀菌自清洁的射频美容仪用透明陶瓷及其制备方法
CN112011174B (zh) 一种纳米二氧化硅/氮掺杂改性纤维体复合材料的制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20170804