CN101217180B - A preparation method for lead-free piezoelectricity thick film - Google Patents
A preparation method for lead-free piezoelectricity thick film Download PDFInfo
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- CN101217180B CN101217180B CN 200810046660 CN200810046660A CN101217180B CN 101217180 B CN101217180 B CN 101217180B CN 200810046660 CN200810046660 CN 200810046660 CN 200810046660 A CN200810046660 A CN 200810046660A CN 101217180 B CN101217180 B CN 101217180B
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Abstract
The invention discloses a silk screen printing preparation method of a lead-free piezoelectric thick-film, including: (1) the lead-free piezoelectric ceramic powder is prepared by adopting a solid phase method; (2) an adhesive is dissolved in terpineol according to the weight ratio of 3: 100 to 9: 100 so as to obtain an organic mixture; (3) the lead-free piezoelectric ceramic powder and the organic mixture are mixed according to the weight ratio of 15: 10 to 90: 10, a dispersant and a plasticizer are added for mixing, grinding and ball milling so as to obtain a paste which is ready to be printed; (4) the paste is printed on a substrate by adopting a silk screen printing technology, a thick-film blank with needed thickness is obtained by being placed flat, baking, preburning and repeated operation; (5) the blank is treated with sintering below 1050 to 1300 DEG C, and heat preservation is kept for 15 to 45 minutes. The invention has simple technology, environmental protection, high efficiency of film formation, good reproducibility, dense film formation and excellent electrical performances, the thickness can be controlled arbitrarily between 10 and 100Mum, various printing thick-film patterns can be obtained without a lithography technology; the invention is compatible with the MEMS technology and is applicable to the preparation of piezoelectric micro-motors, micro-fluid pumps, ultrasonic transducers and micro-actuators.
Description
Technical field
The invention belongs to functional ceramic thick film preparing technical field, specifically, it relates to a kind of silk screen printing preparation method of lead-free piezoelectric thick film.
Background technology
Piezoelectric thick is often referred to the piezoelectric film that thickness is 10～100 μ m; Compare with film; Its piezoelectricity, ferroelectric properties less receive influences such as interface, surface, and bigger thickness also can produce bigger actuating force, and has higher sensitivity and wideer operating frequency; Compare with the body material, the piezoelectric thick operating voltage low (＜5V), frequency of utilization is high, compatible with semiconductor technology.Therefore, piezoelectric thick is widely used in mini drive, piezoelectric micromotor motor, micro-fluid pump, ink jet-print head, ultrasonic transducer, hearing aids, sonar hydrophone and microelectromechanical systems (MEMS).
On the one hand, the device of using at present is through ceramic thinning technique the block ceramic attenuate to be obtained ceramic sheet mostly, then these ceramic sheets is assembled into device.Adopting now ceramic attenuate can reach minimal thickness is about 100 μ m, is subject in the process of grinding and polishing that thickness is thin excessively to be vulnerable to the extraneous application of force and to produce and break, and rate of finished products is about 5%, so the restriction that can't cross over 100 μ m downwards.And block ceramic becomes ceramic sheet will be passed through a series of cutting sanding and polishing process and want the labor time, complex procedures, and cost is high, and serious to waste of material.On the other hand; In the present Piezoelectric Film for Designing method, as sputtering method be with the piezoelectric ceramic bulk as target, utilize the sputter machine with the piezoelectric plated film on substrate; The pulse laser method also is as target with piezoceramic material; Utilize laser to make its moment become gaseous state and on substrate, deposit film forming, these two kinds of method deposition rates are low, and exist bigger stress to cause cracking easily; Sol-gal process is that the composition of piezoelectric is mixed into solution state with the mode of different compounds; Utilize the mode of sol evenning machine spin coating evenly to coat on the substrate again; And increase thickness with the stratiform accumulation mode, and reburning at last and form film, this mode individual layer maximum ga(u)ge that do not ftracture is about 300nm; If will make the piezoelectric thick that surpasses 10 μ m, the essential appreciable time of cost.And the number of plies too much also can cause cracking, so uncomfortable incompatible making thick film; Not only equipment and raw material are expensive for physical vapour deposition (PVD) and chemical vapour deposition (CVD) in addition, deficiency such as the big length consuming time of stress when equally also existing preparation thickness to surpass the piezoelectric film of 10 μ m.So must adopt new method to prepare the piezoelectric thick material between 10～100 μ m.
Traditional piezoelectric system, wherein lead oxide (or lead orthoplumbate) accounts for about 70% of raw material gross mass.So high lead content brings very big infringement all can in preparation, use and in the discarded last handling process environment and human health.In recent years, in order to preserve our planet and the human existence space, prevent the pollution of environment, the friendly ferroelectric piezoelectric of research and development novel environmental has become one of focus material that world developed country endeavours to research and develop.Bismuth sodium titanate based, barium phthalate base and sodium niobate base piezoelectric are considered to the leadless piezoelectric system of potentialization, but present research almost rests in the research of body material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method for lead-free piezoelectricity thick film, adopt the piezoelectric thick of this method preparation to have environmental friendliness, very high density, higher piezoelectric modulus, be fit to be used for making piezoelectric microsensor and actuator.
Preparation method for lead-free piezoelectricity thick film provided by the invention, its step comprises:
(1) oxide or the salt of each metal in any chemical formula in the following formula (I) to (X) are pressed the stoichiometric proportion batch mixes in its formula, ball milling, oven dry is sieved; Precompressed, 800～950 ℃ of following pre-burnings, ball millings again; Oven dry is sieved, and obtains the leadless piezoelectric ceramics powder;
(2) select for use methylcellulose, ethyl cellulose or PVB as adhesive; Select for use terpinol as solvent; Is 3: 100～9: 100 batchings with adhesive and solvent by mass ratio, and adhesive is added in the solvent heating and stirs until dissolving fully, obtains organic mixture;
(3) above-mentioned leadless piezoelectric ceramics powder was mixed by mass ratio with organic mixture in 15: 10～90: 10, be milled into slurry;
(4) pour ball grinder into after above-mentioned slurry and plasticizer and dispersant are milled once more and carry out ball milling, promptly obtain thick film ink to be printed; Wherein, the mass ratio of slurry and plasticizer is 100: 0.5～100: 3, and the mass ratio of dispersant and slurry is 0.5: 100～4: 100, and plasticizer is polyethylene glycol or dibutyl phthalate, and dispersant is diethylene glycol monobutyl ether acetate or tributyl phosphate;
(5) slurry that step (4) is obtained is printed onto Pt/Al through 200～420 purpose silk-screen printing techniques
2O
3Or Pt/Ti/SiO
2On the substrate, set level through 5～15 minutes, 100～150 ℃ of bakings 5～15 minutes are down put into 500～600 ℃ of pre-burnings of rapid heat-treatment furnace again and are removed organic substance then;
(6) repeat above-mentioned steps (5), obtain the printing thick film biscuit of desired thickness;
(7) be that 2～9 ℃/min is heated to 1050～1300 ℃ of sintering with the thick film biscuit with heating rate, be incubated 15～45 minutes, obtain required lead-free piezoelectric thick film;
(1-x-y)Na
0.5Bi
0.5TiO
3-xBaTiO
3-y?K
0.5Bi
0.5TiO
3 (Ⅰ)
(1-x)Na
0.5Bi
0.5TiO
3-xBaTiO
3 (Ⅱ)
(1-x)Na
0.5K
0.5NbO
3-xBaTiO
3 (Ⅲ)
(1-x)Na
0.5Bi
0.5TiO
3-xLiNbO
3 (Ⅳ)
(1-x)BaTiO
3-xBaZrO
3 (Ⅴ)
(1-x)BaTiO
3-xKTaO
3 (Ⅵ)
(1-x)BaTiO
3-xBa
0.5NbO
3 (Ⅶ)
(1-x)NaNbO
3-xLiNbO
3 (Ⅷ)
(1-x)NaNbO
3-xK
0.5Bi
0.5TiO
3 (Ⅸ)
(1-x)Na
0.5K
0.5NbO
3-xLiNbO
3 (Ⅹ)
Wherein, 0＜x＜1,0＜x+y＜1.
As the prioritization scheme of technique scheme, in the step (1), for the first time added the absolute ethyl alcohol ball milling 3～5 hours during ball milling, added the absolute ethyl alcohol ball milling 6～9 hours during ball milling for the second time, be 100 mesh sieves when sieving for the first time, be 200 mesh sieves when sieving for the second time.
The present invention utilizes silk screen print method to prepare lead-free piezoelectric thick film, and particularly, the present invention has following technique effect:
1) technology is simple, does not need expensive equipment, and film forming efficiency is high, is suitable for producing favorable repeatability in enormous quantities;
2) solid concentration is high, and film forming is fine and close, and electrical property is excellent;
3) material system that is adopted is not leaded, can not pollute environment;
4) thickness of piezoelectric thick can arbitrarily be controlled in 10～100 μ m, has remedied the deficiency of this thickness functional material of conventional films and ceramics processing preparation;
5) can be very easy to obtain various printing thick film figures, need not the complicated photoetching process of program;
6) with semiconductor technology and MEMS technical compatibility, be particularly suitable for preparing piezoelectric micromotor motor, micro-fluid pump, ultrasonic transducer and microactrator.
Description of drawings
Fig. 1 is the surface (a) and cross section (b) the SEM figure of BNKT thick film behind 1100 ℃ of following sintering 0.5h;
Fig. 2 is a thick-film dielectric performance map under the different sintering temperatures;
Fig. 3 is thick film electric hysteresis loop figure.
Embodiment
The lead-free piezoelectric thick film material that the present invention is directed to is bismuth sodium titanate based, barium phthalate base and sodium niobate base, wherein bismuth sodium titanate based (1-x-y) Na that comprises
0.5Bi
0.5TiO
3-xBaTiO
3-yBi
0.5K
0.5TiO
3, (1-x) Na
0.5Bi
0.5TiO
3-xBaTiO
3, (1-x) Na
0.5Bi
0.5TiO
3-xK
0.5Bi
0.5TiO
3And (1-x) Na
0.5Bi
0.5TiO
3-xLiNbO
3Barium phthalate base comprises (1-x) BaTiO
3-xBaZrO
3, (1-x) BaTiO
3-xKTaO
3And (1-x) BaTiO
3-xBa
0.5NbO
3The sodium niobate base comprises (1-x) NaNbO
3-xLiNbO
3, (1-x) NaNbO
3-xK
0.5Bi
0.5TiO
3, (1-x) Na
0.5K
0.5NbO
3-xLiNbO
3And (1-x) Na
0.5K
0.5NbO
3-xBaTiO
3, 0＜x＜1,0＜x+y＜1.
Further illustrate substantive features of the present invention and marked improvement through eight embodiment below, but the present invention only limits to the described execution mode of said embodiment absolutely not.
With 8.48 gram sodium carbonate (Na
2CO
3), 2.76 gram potash (K
2CO
3), 46.6 gram bismuth oxide (Bi
2O
3) mix to add the absolute ethyl alcohol ball milling 4 hours, to pour square plate into and put into 90 ℃ of oven dry down of baking oven, 800 ℃ and 850 ℃ of each pre-burnings are 2 hours after the precompressed, and ball milling was dried 200 mesh sieves after 8 hours, promptly get about 140 gram (Na
0.82K
0.18)
0.5Bi
0.5TiO
3Piezoelectric ceramic powder; 0.5 gram ethyl cellulose joined in the 10 gram terpinols be stirred to dissolving fully under 55 ℃; Adding 35 gram piezoelectric ceramic powders mixing mills; And add 1 the gram diethylene glycol monobutyl ether acetate and 0.5 the gram dibutyl phthalate; Pour that mixing and ball milling promptly got thick film ink to be printed in 4 hours in the ball grinder into, using 320 mesh sieve printings is 20 * 15 * 0.5mm to having the Pt electrode size
3Alumina substrate on; Set level through 10 minutes; 120 ℃ were toasted 10 minutes down then; Put into 550 ℃ of pre-burnings of rapid heat-treatment furnace again and remove organic substance, repeat print after 8 layers with the thick film biscuit put into Muffle furnace carried out 1140 ℃ of sintered heat insulatings 30 minutes (heating rate be 5 ℃/min), promptly get the thick bismuth sodium titanate base leadless piezoelectricity thick film material of about 40 μ m.Thick film surface can be tested thick film properties through adopting sputter to prepare the Pt top electrode behind the sanding and polishing, and the dielectric constant under the 10KHz is 720, and dielectric loss is 2.8%, and remanent polarization is 27.3 μ C/cm
2, coercive field is 62.8KV/cm, vertically piezoelectric coefficient d
33Be 76pm/V.Bulk structure and performance such as Fig. 1, Fig. 2 and shown in Figure 3.
Embodiment 2
Make about 140 gram (Na by embodiment 1
0.82K
0.18)
0.5Bi
0.5TiO
3Piezoelectric ceramic powder; 0.5 gram ethyl cellulose joined in the 10 gram terpinols be stirred to dissolving fully under 55 ℃; Adding 35 gram piezoelectric ceramic powders mixing mills; And add 0.5 gram dibutyl phthalate and make plasticizer, pour that mixing and ball milling promptly got thick film ink to be printed in 4 hours in the ball grinder into, print to Pt/Ti/SiO with 320 mesh sieves
2On the substrate; Set level through 10 minutes; 120 ℃ were toasted 10 minutes down then; Put into 550 ℃ of pre-burnings of rapid heat-treatment furnace again and remove organic substance, repeat print after 8 layers with the thick film biscuit put into Muffle furnace carried out 1140 ℃ of sintered heat insulatings 30 minutes (heating rate be 5 ℃/min), promptly get the thick bismuth sodium titanate base leadless piezoelectricity thick film material of about 40 μ m.Thick film surface can be tested thick film properties through adopting sputter to prepare the Pt top electrode behind the sanding and polishing, and the dielectric constant under the 10KHz is 680, and dielectric loss is 4.6%, and remanent polarization is 22.4 μ C/cm
2, coercive field is 59.7KV/cm, vertically piezoelectric coefficient d
33Be 66pm/V.
Embodiment 3
65.67 gram brium carbonates, 76.70 gram titanium dioxide were mixed adding absolute ethyl alcohol ball milling 2 hours with 1.025 gram zirconium dioxides; Pour square plate into and put into 90 ℃ of oven dry down of baking oven; 850 ℃ of following pre-burnings 4 hours, ball milling was dried 200 mesh sieves after 7 hours after the precompressed, promptly got about 100 gram BaTi
0.975Zr
0.025O
3Piezoelectric ceramic powder prepares the thick film biscuit by embodiment 1 method, put into Muffle furnace carried out 1300 ℃ of sintered heat insulatings 30 minutes (heating rate be 5 ℃/min) promptly get the thick barium titanate-based lead-free piezoelectric thick material of about 40 μ m.Thick film surface can be tested thick film properties through adopting sputter to prepare the Pt top electrode behind the sanding and polishing, and the dielectric constant under the 10KHz is 816, and dielectric loss is 3.7%, and remanent polarization is 14.8 μ C/cm
2, coercive field is 46.6KV/cm, vertically piezoelectric coefficient d
33Be 58pm/V.
Embodiment 4
Restrain sodium carbonate, 32.43 gram potash, 62.51 gram niobium pentaoxides, 2.22 gram lithium carbonates and 13.26 gram tantalum pentoxides with 24.91 and mixed adding absolute ethyl alcohol ball milling 4 hours; Pour square plate into and put into 90 ℃ of oven dry down of baking oven; After the precompressed 900 ℃ of following pre-burnings 4 hours; Ball milling was dried 120 mesh sieves after 4 hours, promptly get about 150 gram 0.94Na
0.5K
0.5NbO
3-0.06LiTaO
3Piezoelectric ceramic powder prepares the thick film biscuit by embodiment 1 method, put into Muffle furnace carried out 1100 ℃ of sintered heat insulatings 30 minutes (heating rate be 5 ℃/min) promptly get thick sodium niobate base high-curie temperature (420 ℃) lead-free piezoelectric thick film of about 40 μ m.Thick film surface can be tested thick film properties through adopting sputter to prepare the Pt top electrode behind the sanding and polishing, and the dielectric constant under the 10KHz is 642, and dielectric loss is 3.3%, and remanent polarization is 11.7 μ C/cm
2, coercive field is 42.3KV/cm, vertically piezoelectric coefficient d
33Be 49pm/V.
Embodiment 5
Prepare about 140 gram (Na with embodiment 1 method
0.82K
0.18)
0.5Bi
0.5TiO
3Piezoelectric ceramic powder; 0.5 gram ethyl cellulose joined in the 10 gram terpinols be stirred to dissolving fully under 55 ℃; Adding 20 gram piezoelectric ceramic powders mixing mills; And add 0.5 gram diethylene glycol monobutyl ether acetate and 0.5 gram dibutyl phthalate, and pour that mixing and ball milling promptly get thick film ink to be printed in 4 hours in the ball grinder into, all the other carry out the printing heat processing with embodiment 1.Making the dielectric constant of the thick BNKT thick film of about 40 μ m under 10KHz is 467, and dielectric loss is 7.4%, and remanent polarization is 11.2 μ C/cm
2, coercive field is 76.5KV/cm.
Embodiment 6
Prepare about 140 gram (Na with embodiment 1 method
0.82K
0.18)
0.5Bi
0.5TiO
3Piezoelectric ceramic powder; 0.7 gram ethyl cellulose joined in the 10 gram terpinols be stirred to dissolving fully under 55 ℃; Adding 35 gram piezoelectric ceramic powders mixing mills; And add 2 gram diethylene glycol monobutyl ether acetates and 1 gram dibutyl phthalate, pour that mixing and ball milling promptly got thick film ink to be printed in 4 hours in the ball grinder into.All the other carry out printing heat with embodiment 1 and handle.Making the dielectric constant of the thick BNKT thick film of about 40 μ m under 10KHz is 683, and dielectric loss is 3.4%, and remanent polarization is 23.7 μ C/cm
2, coercive field is 63.8KV/cm.
Embodiment 7
By embodiment 1 make answer slurry after; Repeat print after 4 layers with the thick film biscuit put into Muffle furnace carried out 1140 ℃ of sintered heat insulatings 30 minutes (heating rate be 5 ℃/min); Making the dielectric constant of the thick BNKT thick film of about 20 μ m under 10KHz is 365; Dielectric loss is 8.3%, and remanent polarization is 9.8 μ C/cm
2, coercive field is 89.5KV/cm.
By embodiment 1 make answer slurry after; Repeat print after 12 layers with the thick film biscuit put into Muffle furnace carried out 1050 ℃ of sintered heat insulatings 90 minutes (heating rate be 5 ℃/min); The dielectric constant that makes under the thick BNKT thick film of the about 60 μ m 10KHz is 786; Dielectric loss is 3.2%, and remanent polarization is 21.6 μ C/cm
2, coercive field is 59.8KV/cm.
Claims (2)
1. preparation method for lead-free piezoelectricity thick film, its step comprises:
(1) oxide or the salt of each metal in any chemical formula in the following formula (I) to (X) are pressed the stoichiometric proportion batch mixes in its formula, ball milling, oven dry is sieved; Precompressed, 800～950 ℃ of following pre-burnings, ball millings again; Oven dry is sieved, and obtains the leadless piezoelectric ceramics powder;
(2) select for use methylcellulose, ethyl cellulose or PVB as adhesive; Select for use terpinol as solvent; Is 3: 100～9: 100 batchings with adhesive and solvent by mass ratio, and adhesive is added in the solvent heating and stirs until dissolving fully, obtains organic mixture;
(3) above-mentioned leadless piezoelectric ceramics powder was mixed by mass ratio with organic mixture in 15: 10～90: 10, be milled into slurry;
(4) after milling once more, pour above-mentioned slurry and plasticizer and dispersant into ball grinder and carry out ball milling, promptly obtain thick film ink to be printed; Wherein, the mass ratio of slurry and plasticizer is 100: 0.5～100: 3, and the mass ratio of dispersant and slurry is 0.5: 100～4: 100, and plasticizer is polyethylene glycol or dibutyl phthalate, and dispersant is diethylene glycol monobutyl ether acetate or tributyl phosphate;
(5) slurry that step (4) is obtained is printed onto Pt/Al through 200～420 purpose silk-screen printing techniques
2O
3Or Pt/Ti/SiO
2On the substrate, set level through 5～15 minutes, 100～150 ℃ of bakings 5～15 minutes are down put into 500～600 ℃ of pre-burnings of rapid heat-treatment furnace again and are removed organic substance then;
(6) repeat above-mentioned steps (5), obtain the printing thick film biscuit of desired thickness;
(7) be that 2～9 ℃/min is heated to 1050～1300 ℃ of sintering with the thick film biscuit with heating rate, be incubated 15～45 minutes, obtain required lead-free piezoelectric thick film;
(1-x-y)Na
0.5Bi
0.5TiO
3-xBaTiO
3-yK
0.5Bi
0.5TiO
3 (Ⅰ)
(1-x)Na
0.5Bi
0.5TiO
3-xBaTiO
3 (Ⅱ)
(1-x)Na
0.5K
0.5NbO
3-xBaTiO
3 (Ⅲ)
(1-x)Na
0.5Bi
0.5TiO
3-xLiNbO
3 (Ⅳ)
(1-x)BaTiO
3-xBaZrO
3 (Ⅴ)
(1-x)BaTiO
3-xKTaO
3 (Ⅵ)
(1-x)BaTiO
3-xBa
0.5NbO
3 (Ⅶ)
(1-x)NaNbO
3-xLiNbO
3 (Ⅷ)
(1-x)NaNbO
3-xK
0.5Bi
0.5TiO
3 (Ⅸ)
(1-x)Na
0.5K
0.5NbO
3-xLiNbO
3 (Ⅹ)
Wherein, 0＜x＜1,0＜x+y＜1.
2. preparation method according to claim 1; It is characterized in that: in the step (1), for the first time added the absolute ethyl alcohol ball milling 3～5 hours during ball milling, added the absolute ethyl alcohol ball milling 6～9 hours during ball milling for the second time; When sieving for the first time is 100 mesh sieves, is 200 mesh sieves when sieving for the second time.
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| CN101859869B (en) * | 2010-05-18 | 2011-09-14 | 四川大学 | High d33 lead-free piezoelectric ceramics-polymer-salt piezoelectric composite material and preparation method thereof |
| CN103360060B (en) * | 2013-07-19 | 2014-11-19 | 景德镇陶瓷学院 | Sodium bismuth titanate based textured piezoelectric ceramic water-based tape casting slurry and preparation method of ceramic membrane thereof |
| CN103922730B (en) * | 2014-02-27 | 2015-08-19 | 天津大学 | The preparation method of the multilayer ceramic capacitor medium of wide operating temperature range |
| CN103896581B (en) * | 2014-02-27 | 2015-08-19 | 天津大学 | The preparation method of the multilayer ceramic capacitor medium of wide operating temperature range |
| CN104129987B (en) * | 2014-07-22 | 2016-04-06 | 桂林电子科技大学 | A kind of high-temp leadless nanometer piezoelectric ceramics and preparation method thereof |
| CN107032789A (en) * | 2017-03-24 | 2017-08-11 | 合肥羿振电力设备有限公司 | A kind of high tension performance ceramic material and preparation method thereof |
| CN108511246A (en) * | 2018-05-28 | 2018-09-07 | 北京梦之墨科技有限公司 | A kind of thin film switch and preparation facilities and method using screen printing mode preparation |
| CN113264766A (en) * | 2021-06-07 | 2021-08-17 | 西安交通大学 | Lead-free piezoelectric film material and preparation method thereof |
| CN114751735B (en) * | 2022-03-03 | 2023-04-18 | 常州大学 | Dielectric medium energy storage ceramic powder, preparation method and application thereof in ceramic membrane |
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| JP2003095737A (en) * | 2001-09-17 | 2003-04-03 | National Institute Of Advanced Industrial & Technology | Piezoelectric ceramic composition |
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