CN110641091A - Lead-free piezoelectric ceramic fiber composite material and manufacturing process thereof - Google Patents
Lead-free piezoelectric ceramic fiber composite material and manufacturing process thereof Download PDFInfo
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Abstract
The invention provides a lead-free piezoelectric ceramic fiber composite material, which is formed by alternately arranging lead-free piezoelectric ceramic fibers and a high polymer material, wherein the lead-free piezoelectric ceramic fibers can be selected from potassium-sodium niobate (KNN) -based lead-free piezoelectric ceramics, bismuth-sodium titanate (BNT) -based lead-free piezoelectric ceramics and Barium Titanate (BT) -based lead-free piezoelectric ceramics; the high molecular polymer material can optionally comprise epoxy resin, polyimide and the like. Meanwhile, the invention provides a manufacturing process for preparing the lead-free piezoelectric ceramic fiber composite material.
Description
Technical Field
The invention belongs to the field of lead-free piezoelectric technology and fiber composite materials, and particularly relates to a lead-free piezoelectric ceramic fiber composite material and a manufacturing process thereof.
Background
The development of the field of intelligent materials and intelligent structures is changing day by day and gradually becomes an important technical means for monitoring, adjusting and driving key components and structures. The intelligent structure mostly adopts a structural form that functional devices are integrated with a base structure, and in order to be integrated with the structural base, new requirements on the geometric shapes and the sizes of functional elements in the intelligent structure are provided. Research on smart materials and structures has been a hot issue over the last decades. Although the variety of smart materials is wide, piezoelectric materials are considered as one of the most representative. The piezoelectric ceramic is an intelligent material capable of realizing mutual conversion of mechanical energy and electric energy, integrates sensing, driving and controlling functions, and has a very wide application prospect.
However, the piezoelectric ceramics have problems of large brittleness, difficulty in realizing a large-sized sheet structure, poor large deformation capability, and the like. The piezoelectric ceramics are made into fibers, can be made into various sizes and shapes, and can be compounded, woven and the like with other functional materials; the piezoelectric fiber composite material obtained not only keeps excellent piezoelectric property, but also has good flexibility and light weight, is suitable for being adhered to various working surfaces including curved surfaces, greatly expands the application range of the piezoelectric ceramic material and devices, and can be widely applied to the military and civil fusion fields of aviation, aerospace and the like.
In addition, in the prior art, lead zirconate titanate (PZT) materials are used for the piezoelectric elements. Lead is a toxic heavy metal which is extremely harmful to human bodies, and lead and compounds thereof can cause damage to a plurality of systems such as nerves, hematopoiesis, digestion, kidneys, cardiovascular system, endocrine system and the like after entering organisms. Lead-containing piezoelectric elements are often not effectively recycled after being discarded, and lead ions in the lead-containing piezoelectric elements enter soil and cause serious pollution to the ecological environment.
Disclosure of Invention
In view of the above, the present invention provides a lead-free piezoelectric ceramic fiber composite material, which is composed of a lead-free piezoelectric ceramic fiber and a high molecular polymer material, and a manufacturing process for preparing the lead-free piezoelectric ceramic fiber composite material.
In order to achieve the purpose, the invention is realized by the following technical scheme: a lead-free piezoelectric fiber composite material is formed by arranging lead-free piezoelectric ceramic fibers and a high polymer material alternately, wherein the lead-free piezoelectric ceramic fibers can be made of potassium-sodium niobate (KNN) -based lead-free piezoelectric ceramics, bismuth-sodium titanate (BNT) -based lead-free piezoelectric ceramics, Barium Titanate (BT) -based lead-free piezoelectric ceramics and the like; the high molecular polymer material can optionally comprise epoxy resin, polyimide and the like.
The molar content of the potassium sodium niobate and the doping modification material thereof in the potassium sodium niobate-based lead-free piezoelectric ceramic is 55-100%, wherein the mass fraction of niobium element is 40-70%. The molar content of sodium bismuth titanate and doped modified materials thereof in the sodium bismuth titanate-based lead-free piezoelectric ceramic is 55-100%, wherein the mass fraction of titanium element is 20-30%. The barium titanate-based lead-free piezoelectric ceramic contains 55-100% of barium titanate and doping modification materials thereof, wherein the mass fraction of barium is 50-75%.
The invention adopts a tape casting-cutting method to prepare the lead-free piezoelectric ceramic fiber composite material, which comprises the following steps:
(1) powder synthesis: weighing raw materials according to a piezoelectric ceramic chemical formula of the lead-free piezoelectric ceramic fiber composite material to be prepared, ball-milling and mixing the weighed raw materials, drying, pre-sintering, ball-milling the pre-sintered powder again, drying, grinding and sieving to obtain the required piezoelectric ceramic powder;
(2) the preparation of the slurry comprises the steps of weighing piezoelectric ceramic powder, adding a mixed solvent and a dispersing agent into the ceramic powder, carrying out ball milling for 3 ~ 24h, adding a binder and a plasticizer, and carrying out secondary ball milling for 3 ~ 24h to obtain casting slurry;
(3) defoaming, namely placing the obtained casting slurry in a container and defoaming for 2 ~ 6 h;
(4) casting, namely adjusting a casting forming machine to be in a horizontal state, keeping the height of a first edge to be 5 ~ 20 mu m higher than that of a second edge, pouring prepared casting slurry into a knife edge groove of the casting forming machine, adjusting the movement rate of a rubber belt of the casting forming machine to be 0.2-2m/min, and drying to obtain a sheet with the required length;
(5) laminating: cutting the sheet obtained by casting according to the required size, laminating, pressing and molding to obtain a piezoelectric ceramic sheet with the thickness of 50-300 mu m;
(6) and (3) sintering: placing the obtained piezoelectric ceramic sheet in a corundum crucible, and sealing and sintering a gap of the corundum crucible;
(7) bonding, namely, stacking the sintered piezoelectric ceramic sheets, coating a high polymer material on the surface of each piezoelectric ceramic sheet to form a structure in which the piezoelectric ceramic sheets and the high polymer material are arranged alternately, and curing for 12 ~ 24 hours in a baking oven at 50 ~ 80 ℃ to obtain a multilayer piezoelectric ceramic composite;
(8) cutting: and cutting the cured multilayer piezoelectric ceramic composite according to the required size to obtain the piezoelectric ceramic fiber composite material.
The invention utilizes a tape casting method to prepare the piezoelectric ceramic sheets, after sintering, the surface of each piezoelectric ceramic sheet is coated with the high molecular polymer material, so that the piezoelectric ceramic sheets and the high molecular polymer material form a multilayer structure with alternately arranged piezoelectric ceramic sheets and high molecular polymer materials, and the piezoelectric ceramic fiber composite material is obtained by cutting. The piezoelectric ceramic fiber composite material can be used as a driver to be applied to the fields of structure control, vibration suppression, structure health monitoring and the like, and has wide application prospect. Meanwhile, the lead-free piezoelectric ceramic material is used as a raw material, compared with the existing lead-containing material, the lead-free piezoelectric ceramic has the characteristics of greenness, no toxicity, environmental protection and no pollution, and can effectively reduce the health and environmental problems caused by the use and abandonment of lead-containing elements.
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Detailed Description
Specific examples of the present invention will be described in further detail below.
Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is, what is meant is "including, but not limited to".
Example 1:
the composite material is formed by alternately arranging lead-free piezoelectric ceramic fibers and a high polymer material, wherein the lead-free piezoelectric ceramic fibers are made of potassium sodium niobate-based lead-free piezoelectric ceramics, and the high polymer material is epoxy resin. The molar content of potassium sodium niobate and doped modified materials thereof in the potassium sodium niobate-based lead-free piezoelectric ceramic is 90%, wherein the mass fraction of niobium element is 55%.
The preparation method comprises the following steps:
(1) powder synthesis: weighing raw materials according to a piezoelectric ceramic chemical formula of the lead-free piezoelectric ceramic fiber composite material to be prepared, ball-milling and mixing the weighed raw materials, drying, pre-sintering, ball-milling the pre-sintered powder again, drying, grinding and sieving to obtain the required piezoelectric ceramic powder;
(2) preparing slurry: weighing piezoelectric ceramic powder, adding a mixed solvent and a dispersing agent into the ceramic powder, and carrying out ball milling for 12 hours; adding a binder and a plasticizer, and carrying out secondary ball milling for 12 hours to obtain casting slurry;
(3) defoaming: placing the obtained casting slurry in a container and defoaming for 4 hours;
(4) casting: adjusting the tape casting forming machine to be in a horizontal state, and keeping the first knife edge 10 micrometers higher than the second knife edge; pouring the prepared casting slurry into a knife edge groove of a casting forming machine, adjusting the movement speed of an adhesive tape of the casting forming machine to be 0.5m/min, and drying to obtain a sheet with the required length;
(5) laminating: cutting the sheet obtained by casting according to the required size, laminating, pressing and molding to obtain a piezoelectric ceramic sheet with the thickness of 100 mu m;
(6) and (3) sintering: placing the obtained piezoelectric ceramic sheet in a corundum crucible, and sealing and sintering a gap of the corundum crucible;
(7) bonding: the sintered piezoelectric ceramic sheets are placed in a laminated manner, the surface of each piezoelectric ceramic sheet is coated with a high molecular polymer material to form a structure in which the piezoelectric ceramic sheets and the high molecular polymer material are arranged alternately, and the structure is cured in an oven at the temperature of 60 ℃ for 18 hours to obtain a multilayer piezoelectric ceramic composite;
(8) cutting: and cutting the cured multilayer piezoelectric ceramic composite according to the required size to obtain the piezoelectric ceramic fiber composite material.
Example 2:
the composite material is formed by alternately arranging lead-free piezoelectric ceramic fibers and a high polymer material, wherein the lead-free piezoelectric ceramic fibers are made of sodium bismuth titanate-based lead-free piezoelectric ceramics, and the high polymer material is polyimide. The molar content of sodium bismuth titanate and a doping modification material thereof in the sodium bismuth titanate-based lead-free piezoelectric ceramic is 85%, wherein the mass fraction of titanium element is 25%.
The preparation method comprises the following steps:
(1) powder synthesis: weighing raw materials according to a piezoelectric ceramic chemical formula of the lead-free piezoelectric ceramic fiber composite material to be prepared, ball-milling and mixing the weighed raw materials, drying, pre-sintering, ball-milling the pre-sintered powder again, drying, grinding and sieving to obtain the required piezoelectric ceramic powder;
(2) preparing slurry: weighing piezoelectric ceramic powder, adding a mixed solvent and a dispersing agent into the ceramic powder, and carrying out ball milling for 16 h; adding a binder and a plasticizer, and performing secondary ball milling for 20 hours to obtain casting slurry;
(3) defoaming: placing the obtained casting slurry in a container and defoaming for 6 h;
(4) casting: adjusting the tape casting forming machine to be in a horizontal state, and keeping the first knife edge to be 15 micrometers higher than the second knife edge; pouring the prepared casting slurry into a knife edge groove of a casting forming machine, adjusting the movement speed of an adhesive tape of the casting forming machine to be 0.5m/min, and drying to obtain a sheet with the required length;
(5) laminating: cutting the sheet obtained by tape casting according to the required size, laminating, pressing and forming to obtain a piezoelectric ceramic sheet with the thickness of 200 mu m;
(6) and (3) sintering: placing the obtained piezoelectric ceramic sheet in a corundum crucible, and sealing and sintering a gap of the corundum crucible;
(7) bonding: the sintered piezoelectric ceramic sheets are placed in a laminated manner, the surface of each piezoelectric ceramic sheet is coated with a high molecular polymer material to form a structure in which the piezoelectric ceramic sheets and the high molecular polymer material are arranged alternately, and the structure is cured in a 50 ℃ oven for 24 hours to obtain a multilayer piezoelectric ceramic compound;
(8) cutting: and cutting the cured multilayer piezoelectric ceramic composite according to the required size to obtain the piezoelectric ceramic fiber composite material.
Example 3:
the composite material is formed by alternately arranging lead-free piezoelectric ceramic fibers and a high polymer material, wherein the lead-free piezoelectric ceramic fibers are barium titanate-based lead-free piezoelectric ceramics, and the high polymer material is epoxy resin. The molar content of barium titanate and doped modified materials in the barium titanate-based lead-free piezoelectric ceramic is 90%, wherein the mass fraction of barium is 60%.
The preparation method comprises the following steps:
(1) powder synthesis: weighing raw materials according to a piezoelectric ceramic chemical formula of the lead-free piezoelectric ceramic fiber composite material to be prepared, ball-milling and mixing the weighed raw materials, drying, pre-sintering, ball-milling the pre-sintered powder again, drying, grinding and sieving to obtain the required piezoelectric ceramic powder;
(2) preparing slurry: weighing piezoelectric ceramic powder, adding a mixed solvent and a dispersing agent into the ceramic powder, and performing ball milling for 6 hours; adding a binder and a plasticizer, and carrying out secondary ball milling for 12 hours to obtain casting slurry;
(3) defoaming: placing the obtained casting slurry in a container and defoaming for 4 hours;
(4) casting: adjusting the tape casting forming machine to be in a horizontal state, and keeping the first knife edge to be 5 microns higher than the second knife edge; pouring the prepared casting slurry into a knife edge groove of a casting forming machine, adjusting the movement speed of an adhesive tape of the casting forming machine to be 1m/min, and drying to obtain a sheet with the required length;
(5) laminating: cutting the sheet obtained by casting according to the required size, and laminating, pressing and molding to obtain a piezoelectric ceramic sheet with the thickness of 50 mu m;
(6) and (3) sintering: placing the obtained piezoelectric ceramic sheet in a corundum crucible, and sealing and sintering a gap of the corundum crucible;
(7) bonding: the sintered piezoelectric ceramic sheets are placed in a laminated manner, the surface of each piezoelectric ceramic sheet is coated with a high molecular polymer material to form a structure in which the piezoelectric ceramic sheets and the high molecular polymer material are arranged alternately, and the structure is cured in an oven at 70 ℃ for 12 hours to obtain a multilayer piezoelectric ceramic compound;
(8) cutting: and cutting the cured multilayer piezoelectric ceramic composite according to the required size to obtain the piezoelectric ceramic fiber composite material.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, and any modifications, equivalents or improvements that are within the spirit of the present invention are intended to be covered by the following claims.
Claims (7)
1. The lead-free piezoelectric fiber composite material is characterized by being formed by arranging lead-free piezoelectric ceramic fibers and high polymer materials at intervals.
2. The lead-free piezoelectric ceramic fiber according to claim 1, wherein the lead-free piezoelectric ceramic fiber is made of potassium-sodium niobate (KNN) -based lead-free piezoelectric ceramic, bismuth-sodium titanate (BNT) -based lead-free piezoelectric ceramic, Barium Titanate (BT) -based lead-free piezoelectric ceramic, or the like.
3. A high molecular weight polymer as claimed in claim 1, wherein the high molecular weight polymer material optionally comprises epoxy, polyimide, or the like.
4. The potassium-sodium niobate-based lead-free piezoelectric ceramic of claim 2, wherein the molar content of the potassium-sodium niobate and the doping modification material thereof in the potassium-sodium niobate-based lead-free piezoelectric ceramic is 55 to 100%, wherein the mass fraction of the niobium element is 40 to 70%.
5. The sodium bismuth titanate-based lead-free piezoelectric ceramic of claim 2, wherein the sodium bismuth titanate and the doping modification material thereof are contained in an amount of 55 to 100 mol%, and the mass fraction of titanium is 20 to 30 mass%.
6. The barium titanate-based lead-free piezoelectric ceramic according to claim 2, wherein the barium titanate-based lead-free piezoelectric ceramic has a molar content of barium titanate and a doping modification material thereof of 55 to 100%, wherein a mass fraction of barium element is 50 to 75%.
7. A manufacturing process for preparing the lead-free piezoelectric ceramic fiber composite material is characterized by comprising the following steps:
(1) powder synthesis: weighing raw materials according to a piezoelectric ceramic chemical formula of the lead-free piezoelectric ceramic fiber composite material to be prepared, ball-milling and mixing the weighed raw materials, drying, pre-sintering, ball-milling the pre-sintered powder again, drying, grinding and sieving to obtain the required piezoelectric ceramic powder;
(2) the preparation of the slurry comprises the steps of weighing piezoelectric ceramic powder, adding a mixed solvent and a dispersing agent into the ceramic powder, carrying out ball milling for 3 ~ 24h, adding a binder and a plasticizer, and carrying out secondary ball milling for 3 ~ 24h to obtain casting slurry;
(3) defoaming, namely placing the obtained casting slurry in a container and defoaming for 2 ~ 6 h;
(4) casting, namely adjusting a casting forming machine to be in a horizontal state, keeping the height of a first edge to be 5 ~ 20 mu m higher than that of a second edge, pouring prepared casting slurry into a knife edge groove of the casting forming machine, adjusting the movement rate of a rubber belt of the casting forming machine to be 0.2-2m/min, and drying to obtain a sheet with the required length;
(5) laminating: cutting the sheet obtained by casting according to the required size, laminating, pressing and molding to obtain a piezoelectric ceramic sheet with the thickness of 50-300 mu m;
(6) and (3) sintering: placing the obtained piezoelectric ceramic sheet in a corundum crucible, and sealing and sintering a gap of the corundum crucible;
(7) bonding, namely, stacking the sintered piezoelectric ceramic sheets, coating a high polymer material on the surface of each piezoelectric ceramic sheet to form a structure in which the piezoelectric ceramic sheets and the high polymer material are arranged alternately, and curing for 12 ~ 24 hours in a baking oven at 50 ~ 80 ℃ to obtain a multilayer piezoelectric ceramic composite;
(8) cutting: and cutting the cured multilayer piezoelectric ceramic composite according to the required size to obtain the piezoelectric ceramic fiber composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111151434A (en) * | 2020-02-29 | 2020-05-15 | 桐乡清锋科技有限公司 | Low-frequency leadless piezoelectric atomization element |
| CN111185339A (en) * | 2020-02-29 | 2020-05-22 | 桐乡清锋科技有限公司 | Megahertz leadless piezoelectric atomization element |
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| CN102024901A (en) * | 2010-10-21 | 2011-04-20 | 南京航空航天大学 | Piezoelectric ceramic fiber composite material and preparation method thereof |
| CN104821372A (en) * | 2015-05-20 | 2015-08-05 | 中南大学 | Shearing-type piezoelectric composite material |
| CN105405964A (en) * | 2015-12-10 | 2016-03-16 | 武汉理工大学 | Method for preparing piezoelectric fiber composite structural layer |
| CN107565012A (en) * | 2017-08-30 | 2018-01-09 | 湖北工程学院 | The preparation method and piezoelectric fibre composite material of piezoelectric fibre composite material |
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| CN102024901A (en) * | 2010-10-21 | 2011-04-20 | 南京航空航天大学 | Piezoelectric ceramic fiber composite material and preparation method thereof |
| CN104821372A (en) * | 2015-05-20 | 2015-08-05 | 中南大学 | Shearing-type piezoelectric composite material |
| CN105405964A (en) * | 2015-12-10 | 2016-03-16 | 武汉理工大学 | Method for preparing piezoelectric fiber composite structural layer |
| CN107565012A (en) * | 2017-08-30 | 2018-01-09 | 湖北工程学院 | The preparation method and piezoelectric fibre composite material of piezoelectric fibre composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111151434A (en) * | 2020-02-29 | 2020-05-15 | 桐乡清锋科技有限公司 | Low-frequency leadless piezoelectric atomization element |
| CN111185339A (en) * | 2020-02-29 | 2020-05-22 | 桐乡清锋科技有限公司 | Megahertz leadless piezoelectric atomization element |
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