CN104051606A - Potassium niobate sodium-based multi-layer piezoelectric ceramic element and preparing method thereof - Google Patents
Potassium niobate sodium-based multi-layer piezoelectric ceramic element and preparing method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 110
- 239000011734 sodium Substances 0.000 title claims abstract description 46
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 25
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 25
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title claims description 11
- 238000000498 ball milling Methods 0.000 claims description 69
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 58
- 230000010287 polarization Effects 0.000 claims description 44
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 claims description 37
- 239000011230 binding agent Substances 0.000 claims description 36
- 239000000843 powder Substances 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 34
- 238000001354 calcination Methods 0.000 claims description 28
- 238000005245 sintering Methods 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- 238000002360 preparation method Methods 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 238000005266 casting Methods 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 21
- 238000007731 hot pressing Methods 0.000 claims description 21
- 239000002270 dispersing agent Substances 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 18
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 16
- 229910052700 potassium Inorganic materials 0.000 claims description 16
- 239000011591 potassium Substances 0.000 claims description 16
- 238000003475 lamination Methods 0.000 claims description 14
- 238000007639 printing Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 238000007766 curtain coating Methods 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- 229910052783 alkali metal Inorganic materials 0.000 claims description 8
- 150000001340 alkali metals Chemical class 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 7
- 238000007872 degassing Methods 0.000 claims description 7
- 239000007772 electrode material Substances 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 238000004806 packaging method and process Methods 0.000 claims description 7
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 claims description 7
- 229920003023 plastic Polymers 0.000 claims description 7
- 239000004033 plastic Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 230000008878 coupling Effects 0.000 abstract description 2
- 238000010168 coupling process Methods 0.000 abstract description 2
- 238000005859 coupling reaction Methods 0.000 abstract description 2
- 239000011812 mixed powder Substances 0.000 description 20
- 239000010955 niobium Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 6
- 229910052744 lithium Inorganic materials 0.000 description 6
- 229910052787 antimony Inorganic materials 0.000 description 5
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 5
- 238000009966 trimming Methods 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910000906 Bronze Inorganic materials 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 1
- QNZFKUWECYSYPS-UHFFFAOYSA-N lead zirconium Chemical compound [Zr].[Pb] QNZFKUWECYSYPS-UHFFFAOYSA-N 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a potassium niobate sodium-based multi-layer piezoelectric ceramic element. A chemometry general form of a formula of potassium niobate sodium-based leadless piezoelectric ceramics is that [(Na0.52K0.44)1-xLix] (Nb0.93-ySb0.07Tay)O3, wherein 0.02<=x<=0.06, 0.02<=y<=0.06, a piezoelectric constant ranges from 300 pC/N to 350 pC/N and even higher, a dielectric constant ranges from 1700 to 2000, and an electromechanical coupling coefficient ranges from 0.40 to 0.45.
Description
Technical field
The present invention relates to ceramic material technical field, relate in particular to a kind of lithium, antimony, the potassium-sodium niobate-based multilayer piezoelectric ceramic element of tantalum codope, the present invention also further relates to the preparation method of lithium, antimony, the potassium-sodium niobate-based multilayer piezoelectric ceramic element of tantalum codope.
Background technology
Multilayer piezoelectric ceramic element is a kind of important electric function ceramic element, than common individual layer piezo ceramic element, has driving voltage low, and piezoelectric strain is large, is easy to the advantage such as miniaturization, slimming.Multilayer piezoelectric ceramic element is widely used in piezoelectric transformer, piezoelectric actuator, piezoelectric speaker, the floating energy of piezoelectricity device, and multilayer ceramic capacitor, wherein piezoelectric actuator comprises automobile engine injection system, ultrasonic motor, linear ultrasonic motor, the high-precision pointed collar such as micro positioner territory, and multilayer device volume is little, consumption is large, so the research of multilayer piezoelectric ceramic has important scientific meaning and market value.But the raw material that at present multilayer piezoelectric ceramic is selected mostly are lead zirconate titanate system pottery, contain poisonous lead oxide more than 60wt%, produce, use and discarded process in very easily the health to human body and environment work the mischief.2006, European Union issues and implements RoHS instruction (about being limited in the instruction that uses some harmful components in electronic and electrical equipment), forbid in electronic product using the harmful components such as plumbous, the state such as Korean and Japanese of Sino-U.S. also issues or similar decree is issued in plan in succession subsequently.The world has started the substitution material of Study For Zirconium lead titanates series piezoelectric ceramic, the i.e. upsurge of leadless piezoelectric ceramics subsequently.Although lead zirconate titanate series piezoelectric ceramic is still enjoyed the prerogarive of mercy of this instruction now, European Union all can assess the technical merit of the alternative plumbous series piezoelectric ceramic of lead-free systems piezoelectric ceramic every year, once opportunity, maturation, will carry out the unleaded process of piezoelectric ceramic immediately.So having, the technology of preparing taking leadless piezoelectric ceramics as raw-material multilayer piezoelectric ceramic can predict urgent using value.
Potassium-sodium niobate series piezoelectric ceramic, with good piezoelectric and dielectric properties and higher Curie temperature under its Unit Weight, is one of most important lead-free piezoceramic material system always.2004, the people such as Japanese scholars Saito realized the breakthrough of potassium/sodium niobtae piezoelectric piezoelectric property by lithium, antimony, tantalum codope and texturing, more than the optimum piezoelectric constant that wherein solid phase method codope obtains has reached 300pC/N first.Through further research and improving of Chinese scholars, lead free piezoelectric ceramics of potassium sodium niobate has become tool potentiality and has substituted one of material system of plumbous series piezoelectric ceramic.At present, the research of lead free piezoelectric ceramics of potassium sodium niobate sandwich type element and preparation are in the fast-developing stage, the present invention use there is lithium, the antimony of high dielectric, high tension performance, the potassium sodium niobate ceramic formula of tantalum codope, prepare multilayer leadless piezoelectric ceramics element by the preparation technology after improving, there is important production practices meaning.
CN101456733A discloses a kind of with general formula (Na
0.52k
0.44li
0.04) (Nb
0.80ta
0.20) O
3, the preparation method of the potassium niobate sodium base leadless piezoelectric ceramic thin sheet of expression, is made up of pretreatment of raw material, mixed material, pre-burning, slurrying, curtain coating, punching, binder removal, sintering, quilt silver, polarization process step.The present invention, compared with existing piezoelectric ceramic preparation method, has adopted slurrying, casting technique step, has been prepared into the admire potassium niobate sodium base leadless piezoelectric ceramic thin sheet of large, the thin crystalline substance of ore deposit structure, density and crystal grain homogeneous, good electrical property of pure calcium, and thickness is 0.12mm.The potassium niobate sodium base leadless piezoelectric ceramic thin sheet that adopts the inventive method to prepare, is prepared into leadless piezoelectric buzzer, non-environmental-pollution, and when driving voltage is 3V, acoustic pressure reaches maximum 86.06dB at 4.445kHz; When driving voltage is 6V, 9V, maximum sound pressure increases people to 91.91,95.22dB than respectively, shows the electroacoustic performance that piezoelectric buzzer has had, and reaches the application requirements as microphone device.It adopts the once technology of preparing of calcining, contain the alkali metals such as potassium, sodium, lithium due to lead free piezoelectric ceramics of potassium sodium niobate, volatile at the high temperature sintering 4-8 of 1150-1170 DEG C hour, once the technical scheme of calcining easily causes powder to become mutually inhomogeneous, powder real composition departs from the phenomenon of original formulation, it has the piezoelectric constant that piezoelectric constant is about 200-250pC/N, and the dielectric constant of 500-1100.In large-scale production practice, more easily occur and more serious, directly affected consistency and the yields of properties of product.
Summary of the invention
For this reason, to be solved by this invention is that existing potassium niobate sodium base leadless piezoelectric ceramic thin sheet exists alkali metal to be easy to volatilization problem in preparation process, cause the value of product real composition off-design, even produce the component zone with non-stoichiometric, generate tungsten bronze, the equal dephasign of Jiao Lvshi, reduce ceramic piezoelectric property, increase dielectric loss, and then cause properties of product to decline, the invention provides a kind of potassium-sodium niobate-based multilayer piezoelectric ceramic element, it has higher piezoelectric property for this reason.
The present invention also provides the preparation method of above-mentioned potassium-sodium niobate-based multilayer piezoelectric ceramic element further.
The present invention adopts following technical scheme:
A kind of potassium-sodium niobate-based multilayer piezoelectric ceramic element, the formula stoichiometry general formula of described potassium niobate sodium-based leadless piezoelectric ceramic original paper is:
[(Na
0.52K
0.44)
1-xLi
x](Nb
0.93-ySb
0.07Ta
y)O
3
Wherein 0.02≤x≤0.06,0.02≤y≤0.06.
The preparation method of above-mentioned potassium-sodium niobate-based multilayer piezoelectric ceramic element, comprises the steps
S1, preliminary treatment
By [(Na
0.52k
0.44)
1-xli
x] (Nb
0.93-ysb
0.07ta
y) O
3the footpath that must put in place after the dry ball milling of needed raw material is the slurry of 700-1300nm;
S2, calcining and ball mill grinding for the first time
Slurry prepared by step S1 is dried, and after pulverizing and sieving, is 800 DEG C-850 DEG C calcining 2-5h in temperature, and cooling, then taking absolute ethyl alcohol as dispersant, the slurry of footpath as 1500-2000nm must put in place after ball-milling medium ball milling taking zirconia ball;
S3, secondary clacining and ball mill grinding
Slurry prepared by step S2 is 800 DEG C-850 DEG C calcining 2-5h in temperature after drying and pulverizing and sieving, cooling, then taking absolute ethyl alcohol as dispersant, the slurry of the footpath 700-1300nm that must put in place after ball-milling medium ball milling taking zirconia ball, is potassium/sodium niobtae ceramic powder after drying;
S4, flow casting molding
According to potassium/sodium niobtae ceramic powder: binding agent: the ratio that the volume ratio of solvent is 1:0.25-0.35:0.35-0.5 joins in ball grinder, taking zirconia ball as ball-milling medium, slurry after ball milling is with leaving standstill after vacuum pump degasification deaeration 1-2h, and using casting machine casting film-forming thick is the film of 10-200 μ m;
S5, printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, ground floor is put new diaphragm after drying, and continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design; Multilayer Film plastic packaging after lamination, connects termination electrode after hot pressing, obtain final multi-layer ceramics green compact;
S6, binder removal, co-sintering and polarization
Ceramic green, with after aluminium oxide or load bearing board of zirconia clamping, is embedded in aluminium oxide ceramics powder, is placed in electric furnace, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h; Green compact after binder removal are sintering 2-4h at 1050-1100 DEG C, after cooling with stove, polarization.
Described step S1 is dried 8-12h by alkali metal raw material at 60-80 DEG C, and and Nb
2o
5, Ta
2o
5, Sb
2o
3after mixing, taking absolute ethyl alcohol as dispersant, carry out ball milling taking zirconia ball as ball-milling medium.
Described alkali metal raw material is Li
2cO
3, Na
2cO
3and K
2cO
3.
In described step S2 and step S3, slurry is crossed 60 mesh sieves.
Binding agent in described step S4 is polyvinyl butyral resin, and described solvent is a kind of in toluene or dimethylbenzene, absolute ethyl alcohol, isopropyl alcohol or several mixture wherein.
In described step S5, electrode material is selected silver palladium alloy, nickel or copper.
Hot pressing in described step S5 is to be 60-80 DEG C in temperature, and pressure is under 40-60MPa condition, to keep 10～30 minutes.
Ceramic green described in described step S6 supports to prevent to shrink inhomogeneous in temperature-rise period with load bearing board and is out of shape.
Polarization described in described step S6 is that the multi-layer ceramics sample that sintering is obtained adopts silicone oil oil bath polarization or air polarization.
The process conditions of described silicone oil oil bath polarization are: silicone oil oil bath temperature is 60-120 DEG C, and Polarization field strength is 2-3kV/mm, and the polarization time is 20-30 minute; The condition of described air polarization is: the temperature that polarizes in air is 60-120 DEG C, and Polarization field strength is 1-2kV/mm, and the polarization time is 20-30 minute.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) the formula stoichiometry general formula that potassium-sodium niobate-based multilayer piezoelectric ceramic element provided by the invention adopts is [(Na
0.52k
0.44)
1-xli
x] (Nb
0.93-ysb
0.07ta
y) O
3between a Composition Region with higher pressure electrical property, the potassium-sodium niobate-based multilayer piezoelectric ceramic element of lithium, antimony, tantalum codope niobium in this Composition Region has higher piezoelectric property, piezoelectric constant is that 300-350pC/N is even higher, dielectric constant is 1700-2000, and electromechanical coupling factor is 0.40-0.45.Due in traditional potassium-sodium niobate series piezoelectric ceramic preparation process when sintering alkali metal volatilization easily cause its true component deviation design component, proposition between this Composition Region can effectively ensure the performance of the piezoelectric ceramic of output, especially in large-scale production, has more advantage.
(2) the invention provides a kind of solid phase method preparation method of improved potassium/sodium niobtae ceramic powder.By secondary clacining ball milling, can effectively improve powder and become phase ratio, improve the uniformity that powder distributes, obtain high activity, even, tiny potassium/sodium niobtae ceramic powder, be greatly conducive to the steps such as follow-up forming and sintering.This is improved one's methods higher efficiency and better effect in the production of potassium/sodium niobtae ceramic powder in enormous quantities.
(3) the invention provides a kind of potassium/sodium niobtae multilayer piezoelectric ceramic element and be prepared into the manufacture method of burning till altogether type from powder, be applicable to design and the manufacture of the unleaded multilayer piezoelectric ceramic element of the multi-purpose different-thickness number of plies.
(4) potassium-sodium niobate-based multilayer piezoelectric ceramic element of the present invention has adopted component S b, this component can significantly reduce orthogonal phase-Tetragonal phase transition temperature of potassium-sodium niobate-based pottery, the enhancing mechanism that promotes many crystal transitions, improves ceramic dielectric constant, remanent polarization and piezoelectric constant.
(5) sintering temperature adopting in the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element in the present invention is 1050-1100 DEG C, with prior art CN101456733A adopt 1150-1170 DEG C compared with, temperature reduces at least 50 DEG C, and sintering time was reduced to 2-4 hour by 4-8 hour, can effectively reduce the volatilization of alkali metal.
Brief description of the drawings
For content of the present invention is more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is according to the Laser particle-size distribution figure of the final powder of lead free piezoelectric ceramics of potassium sodium niobate of embodiments of the invention 4;
Fig. 2 is according to the stereoscan photograph of the section polishing of the potassium/sodium niobtae multi-layer ceramic component of embodiments of the invention 4;
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, embodiments of the present invention are described in further detail.
The present invention can implement in many different forms, and should not be understood to be limited to embodiment set forth herein.On the contrary, provide these embodiment, making the disclosure will be thorough and complete, and design of the present invention fully will be conveyed to those skilled in the art, and the present invention will only be limited by claim.
Embodiment 1
In the present embodiment, the formula stoichiometry general formula of potassium-sodium niobate-based multilayer piezoelectric ceramic element is:
(Na
0.52K
0.44Li
0.04)(Nb
0.91Sb
0.07Ta
0.02)O
3
The preparation method of above-mentioned potassium-sodium niobate-based multilayer piezoelectric ceramic element comprises the steps:
(1) raw material is prepared and batching
Li
2cO
3, Na
2cO
3, K
2cO
3these alkali carbonates easily water suction make moist, must be for subsequent use at 60 DEG C of oven dry 12h before use.According to the stoichiometric proportion of formula general formula, first take: Li
2cO
3, Na
2cO
3, K
2cO
3; Then take Nb
2o
5, Ta
2o
5, Sb
2o
3.
(2) ball mill mixing
It is dispersant that the raw material preparing is added to absolute ethyl alcohol, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 4h (producer's model of planetary ball mill ball milling please be provided).
(3) calcining and ball mill grinding for the first time
The slurry obtaining after ball mill mixing obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, 800 DEG C of calcining 5h, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 8h.
(4) secondary clacining and ball mill grinding
First ball mill grinding disposed slurry obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, again calcines 5h for 800 DEG C, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 8h.The slurry that ball milling obtains is final potassium/sodium niobtae ceramic powder after drying.
(5) flow casting molding
According to ceramic powder: binding agent: the ratio that the ratio of solvent is 1:0.25:0.35 joins in ball grinder, wherein, binding agent is PVB (polyvinyl butyral resin), solvent is toluene.Taking zirconia ball as ball-milling medium, planetary ball mill ball milling 36h.Slurry after ball milling, with leaving standstill after vacuum pump degasification deaeration 2h, uses casting machine curtain coating, regulates line speed according to the specification of casting machine, bake out temperature etc., and controlling as required thickness is 200 μ m.
(6) printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, electrode material can be selected silver palladium alloy.Ground floor is put new diaphragm after drying, and uses dry press pressing, continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design.After Multilayer Film plastic packaging after lamination, use the static pressure such as hot water to carry out hot pressing, temperature is 80 DEG C, and pressure is under 40MPa, to keep 10 minutes.Multilayer Film after hot pressing carries out last cutting trimming angle according to design, connects termination electrode, obtains final multi-layer ceramics green compact.
(7) binder removal and co-sintering
Ceramic green is supported to prevent to shrink inhomogeneous in temperature-rise period and is out of shape with load bearing board, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h.Green compact after binder removal are sintering 2h at 1050-1100 DEG C, after cooling with stove.
(8) polarization
The multi-layer ceramics sample that sintering obtains can adopt silicone oil oil bath polarization: silicone oil oil bath temperature is 60 DEG C, and Polarization field strength is 3kV/mm, and the polarization time is 30 minutes.
Embodiment 2
In the present embodiment, the formula stoichiometry general formula of potassium-sodium niobate-based multilayer piezoelectric ceramic element is:
(Na
0.52K
0.44Li
0.04)(Nb
0.87Sb
0.07Ta
0.06)O
3
(1) raw material is prepared and batching
Li
2cO
3, Na
2cO
3, K
2cO
3these alkali carbonates easily water suction make moist, must be for subsequent use at 80 DEG C of oven dry 8h before use.According to the stoichiometric proportion of formula general formula, first take: Li
2cO
3, Na
2cO
3, K
2cO
3; Then take Nb
2o
5, Ta
2o
5, Sb
2o
3.
(2) ball mill mixing
It is dispersant that the raw material preparing is added to absolute ethyl alcohol, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 4h or with common tank mill formula ball mill ball milling 24h.
(3) calcining and ball mill grinding for the first time
The slurry obtaining after ball mill mixing obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, 850 DEG C of calcining 2h, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 4h.
(4) secondary clacining and ball mill grinding
First ball mill grinding disposed slurry obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, again calcines 2h for 850 DEG C, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 24h.The slurry that ball milling obtains is final potassium/sodium niobtae ceramic powder after drying.
(5) flow casting molding
According to ceramic powder: binding agent: the ratio that the ratio of solvent is 1:0.35:0.5 joins in ball grinder, wherein, binding agent is PVB (polyvinyl butyral resin), solvent is dimethylbenzene.Taking zirconia ball as ball-milling medium, planetary ball mill ball milling 16h.Slurry after ball milling, with leaving standstill after vacuum pump degasification deaeration 1h, uses casting machine curtain coating, regulates line speed according to the specification of casting machine, bake out temperature etc., and controlling as required thickness is 10 μ m.
(6) printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, electrode material can be selected silver palladium alloy, nickel, copper etc.Ground floor is put new diaphragm after drying, and uses dry press pressing, continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design.After Multilayer Film plastic packaging after lamination, use the static pressure such as hot water to carry out hot pressing, temperature is 60 DEG C, and pressure is under 60MPa, to keep 30 minutes.Multilayer Film after hot pressing carries out last cutting trimming angle according to design, connects termination electrode, obtains final multi-layer ceramics green compact.
(7) binder removal and co-sintering
Ceramic green is supported to prevent to shrink inhomogeneous in temperature-rise period and is out of shape with load bearing board, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h.Green compact after binder removal are sintering 3h at 1050-1100 DEG C, after cooling with stove.
(8) polarization
The multi-layer ceramics sample that sintering obtains can adopt two kinds of modes of air polarization: the temperature that polarizes in air is 60 DEG C, and Polarization field strength is 1kV/mm, and the polarization time is 20 minutes.
Embodiment 3
In the present embodiment, the formula stoichiometry general formula of potassium-sodium niobate-based multilayer piezoelectric ceramic element is:
(Na
0.52K
0.44Li
0.04)(Nb
0.90Sb
0.07Ta
0.03)O
3
(1) raw material is prepared and batching
Li
2cO
3, Na
2cO
3, K
2cO
3these alkali carbonates easily water suction make moist, must be for subsequent use at 70 DEG C of oven dry 10h before use.According to the stoichiometric proportion of formula general formula, first take: Li
2cO
3, Na
2cO
3, K
2cO
3; Then take Nb
2o
5, Ta
2o
5, Sb
2o
3.
(2) ball mill mixing
It is dispersant that the raw material preparing is added to absolute ethyl alcohol, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 4h.
(3) calcining and ball mill grinding for the first time
The slurry obtaining after ball mill mixing obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, 830 DEG C of calcining 3h, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 6h.
(4) secondary clacining and ball mill grinding
First ball mill grinding disposed slurry obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, again calcines 4h for 830 DEG C, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, and planetary ball mill ball milling 4h.The slurry that ball milling obtains is final potassium/sodium niobtae ceramic powder after drying.
(5) flow casting molding
According to ceramic powder: binding agent: the ratio that the ratio of solvent is 1:0.3:0.34 joins in ball grinder, wherein, binding agent is PVB (polyvinyl butyral resin), solvent is absolute ethyl alcohol.Taking zirconia ball as ball-milling medium, planetary ball mill ball milling 20h.Slurry after ball milling, with leaving standstill after vacuum pump degasification deaeration 1.5h, uses casting machine curtain coating, regulates line speed according to the specification of casting machine, bake out temperature etc., and controlling as required thickness is 50 μ m.
(6) printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, electrode material can be selected silver palladium alloy, nickel, copper etc.Ground floor is put new diaphragm after drying, and uses dry press pressing, continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design.After Multilayer Film plastic packaging after lamination, use the static pressure such as hot water to carry out hot pressing, temperature is 70 DEG C, and pressure is under 50MPa, to keep 15 minutes.Multilayer Film after hot pressing carries out last cutting trimming angle according to design, connects termination electrode, obtains final multi-layer ceramics green compact.
(7) binder removal and co-sintering
Ceramic green is supported to prevent to shrink inhomogeneous in temperature-rise period and is out of shape with load bearing board, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h.Green compact after binder removal are sintering 3h at 1050-1100 DEG C, after cooling with stove.
(8) polarization
The multi-layer ceramics sample that sintering obtains can adopt two kinds of modes of air polarization: the temperature that polarizes in air is 80 DEG C, and Polarization field strength is 1.5kV/mm, and the polarization time is 25 minutes.
Embodiment 4
In the present embodiment, the formula stoichiometry general formula of potassium-sodium niobate-based multilayer piezoelectric ceramic element is:
(Na
0.52K
0.44Li
0.04)(Nb
0.89Sb
0.07Ta
0.04)O
3
(1) raw material is prepared and batching
Li
2cO
3, Na
2cO
3, K
2cO
3these alkali carbonates easily water suction make moist, must be for subsequent use at 65 DEG C of oven dry 11h before use.According to the stoichiometric proportion of formula general formula, first take: Li
2cO
3, Na
2cO
3, K
2cO
3; Then take Nb
2o
5, Ta
2o
5, Sb
2o
3.
(2) ball mill mixing
It is dispersant that the raw material preparing is added to absolute ethyl alcohol, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 24h.
(3) calcining and ball mill grinding for the first time
The slurry obtaining after ball mill mixing obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, 840 DEG C of calcining 4h, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 24h.
(4) secondary clacining and ball mill grinding
First ball mill grinding disposed slurry obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, again calcines 3h for 810 DEG C, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 48h.The slurry that ball milling obtains is final potassium/sodium niobtae ceramic powder after drying.
(5) flow casting molding
According to ceramic powder: binding agent: the ratio that the ratio of solvent is 1:0.28:0.45 joins in ball grinder, wherein, binding agent is PVB (polyvinyl butyral resin), solvent is isopropyl alcohol.Taking zirconia ball as ball-milling medium, planetary ball mill ball milling 30h.Slurry after ball milling, with leaving standstill after vacuum pump degasification deaeration 1-2h, uses casting machine curtain coating, regulates line speed according to the specification of casting machine, bake out temperature etc., and controlling as required thickness is 100 μ m.
(6) printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, electrode material can be selected silver palladium alloy, nickel, copper etc.Ground floor is put new diaphragm after drying, and uses dry press pressing, continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design.After Multilayer Film plastic packaging after lamination, use the static pressure such as hot water to carry out hot pressing, temperature is 75 DEG C, and pressure is under 55MPa, to keep 20 minutes.Multilayer Film after hot pressing carries out last cutting trimming angle according to design, connects termination electrode, obtains final multi-layer ceramics green compact.
(7) binder removal and co-sintering
Ceramic green is supported to prevent to shrink inhomogeneous in temperature-rise period and is out of shape with load bearing board, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h.Green compact after binder removal are sintering 2h at 1050-1100 DEG C, after cooling with stove.
(8) polarization
The multi-layer ceramics sample that sintering obtains can adopt silicone oil oil bath polarization: silicone oil oil bath temperature is 100 DEG C, and Polarization field strength is 2.5kV/mm, and the polarization time is 28 minutes.
Embodiment 5
In the present embodiment, the formula stoichiometry general formula of potassium-sodium niobate-based multilayer piezoelectric ceramic element is:
(Na
0.52K
0.44Li
0.04)(Nb
0.88Sb
0.07Ta
0.05)O
3
Wherein step (1) raw material is prepared and batching, and step (2) ball mill mixing is with step (1) and the step (2) of embodiment 1;
(3) calcining and ball mill grinding for the first time
The slurry obtaining after ball mill mixing obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, 835 DEG C of calcining 4h, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 48h.
(4) secondary clacining and ball mill grinding
First ball mill grinding disposed slurry obtains mixed powder after drying, and mixed powder pulverizes and sieves, and after 60 mesh standard sieves, puts into the alumina crucible of adding a cover, and in air, again calcines 4.5h for 845 DEG C, cooling with stove.The powder obtaining after calcining is taking absolute ethyl alcohol as dispersant, taking zirconia ball as ball-milling medium, with common tank mill formula ball mill ball milling 35h.The slurry that ball milling obtains is final potassium/sodium niobtae ceramic powder after drying.
(5) flow casting molding
According to ceramic powder: binding agent: the ratio that the ratio of solvent is 1:0.32:0.42 joins in ball grinder, wherein, binding agent is PVB (polyvinyl butyral resin), solvent is toluene.Taking zirconia ball as ball-milling medium, planetary ball mill ball milling 35h.Slurry after ball milling, with leaving standstill after vacuum pump degasification deaeration 1.5h, uses casting machine curtain coating, regulates line speed according to the specification of casting machine, bake out temperature etc., and controlling as required thickness is 150 μ m.
(6) printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, electrode material can be selected silver palladium alloy, nickel, copper etc.Ground floor is put new diaphragm after drying, and uses dry press pressing, continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design.After Multilayer Film plastic packaging after lamination, use the static pressure such as hot water to carry out hot pressing, temperature is 75 DEG C, and pressure is under 55MPa, to keep 25 minutes.Multilayer Film after hot pressing carries out last cutting trimming angle according to design, connects termination electrode, obtains final multi-layer ceramics green compact.
(7) binder removal and co-sintering
Ceramic green is supported to prevent to shrink inhomogeneous in temperature-rise period and is out of shape with load bearing board, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h.Green compact after binder removal are sintering 2.5h (2) at 1050-1100 DEG C, after cooling with stove.
(8) polarization
The multi-layer ceramics sample that sintering obtains can adopt silicone oil oil bath polarization: silicone oil oil bath temperature is 110 DEG C, and Polarization field strength is 2kV/mm, and the polarization time is 26 minutes.
The potassium-sodium niobate-based multilayer piezoelectric ceramic element function test chart that table 1 embodiment 1-6 prepares
| Powder granule size (nm) | Dielectric constant | Individual layer piezoelectric constant (pC/N) |
| Embodiment 1719 | 1737 | 272 |
| Embodiment 3771 | 1766 | 318 |
| Embodiment 41300 | 1910 | 334 |
Certainly, above-described embodiment is only for example is clearly described, and the not restriction to execution mode.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all execution modes.And the apparent variation of being extended out thus or variation are still among protection scope of the present invention.
Claims (11)
1. a potassium-sodium niobate-based multilayer piezoelectric ceramic element, is characterized in that, the formula stoichiometry general formula of described potassium niobate sodium-based leadless piezoelectric ceramic original paper is:
[(Na
0.52K
0.44)
1-xLi
x](Nb
0.93-ySb
0.07Ta
y)O
3
Wherein 0.02≤x≤0.06,0.02≤y≤0.06.
2. a preparation method for potassium-sodium niobate-based multilayer piezoelectric ceramic element described in claim 1, is characterized in that, comprises the steps:
S1, preliminary treatment
By [(Na
0.52k
0.44)
1-xli
x] (Nb
0.93-ysb
0.07ta
y) O
3the footpath that must put in place after the dry ball milling of needed raw material is the slurry of 700-1300nm;
S2, calcining and ball mill grinding for the first time
Slurry prepared by step S1 is dried, and after pulverizing and sieving, is 800 DEG C-850 DEG C calcining 2-5h in temperature, and cooling, then taking absolute ethyl alcohol as dispersant, the slurry of footpath as 1500-2000nm must put in place after ball-milling medium ball milling taking zirconia ball;
S3, secondary clacining and ball mill grinding
Slurry prepared by step S2 is 800 DEG C-850 DEG C calcining 2-5h in temperature after drying and pulverizing and sieving, cooling, then taking absolute ethyl alcohol as dispersant, the slurry of the footpath 700-1300nm that must put in place after ball-milling medium ball milling taking zirconia ball, is potassium/sodium niobtae ceramic powder after drying;
S4, flow casting molding
According to potassium/sodium niobtae ceramic powder: binding agent: the ratio that the volume ratio of solvent is 1:0.25-0.35:0.35-0.5 joins in ball grinder, taking zirconia ball as ball-milling medium, slurry after ball milling is with leaving standstill after vacuum pump degasification deaeration 1-2h, and using casting machine casting film-forming thick is the film of 10-200 μ m;
S5, printing, lamination, hot pressing and cutting
The diaphragm that curtain coating the obtains pattern that prints electrode as required, ground floor is put new diaphragm after drying, and continues to print electrode after pressing, and so circulating printing is stacked to the number of plies of design; Multilayer Film plastic packaging after lamination, connects termination electrode after hot pressing, obtain final multi-layer ceramics green compact;
S6, binder removal, co-sintering and polarization
Ceramic green, with after aluminium oxide or load bearing board of zirconia clamping, is embedded in aluminium oxide ceramics powder, is placed in electric furnace, slow intensification binder removal between 200-500 DEG C, programming rate is 10-12 DEG C/h; Green compact after binder removal are sintering 2-4h at 1050-1100 DEG C, after cooling with stove, polarization.
3. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 2, is characterized in that,
Described step S1 is dried 8-12h by alkali metal raw material at 60-80 DEG C, and and Nb
2o
5, Ta
2o
5, Sb
2o
3after mixing, taking absolute ethyl alcohol as dispersant, carry out ball milling taking zirconia ball as ball-milling medium.
4. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 3, is characterized in that,
Described alkali metal raw material is Li
2cO
3, Na
2cO
3and K
2cO
3.
5. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 2, is characterized in that, in described step S2 and step S3, slurry is crossed 60 mesh sieves.
6. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 2, is characterized in that,
Binding agent in described step S4 is polyvinyl butyral resin, and described solvent is a kind of in toluene or dimethylbenzene, absolute ethyl alcohol, isopropyl alcohol or several mixture wherein.
7. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 2, is characterized in that,
In described step S5, electrode material is selected silver palladium alloy, nickel or copper.
8. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 7, is characterized in that,
Hot pressing in described step S5 is to be 60-80 DEG C in temperature, and pressure is under 40-60MPa condition, to keep 10～30 minutes.
9. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 2, is characterized in that,
Ceramic green described in described step S6 supports to prevent to shrink inhomogeneous in temperature-rise period with load bearing board and is out of shape.
10. the preparation method of potassium-sodium niobate-based multilayer piezoelectric ceramic element according to claim 9, is characterized in that,
Polarization described in described step S6 is that the multi-layer ceramics sample that sintering is obtained adopts silicone oil oil bath polarization or air polarization.
The preparation method of 11. potassium-sodium niobate-based multilayer piezoelectric ceramic elements according to claim 10, is characterized in that,
The process conditions of described silicone oil oil bath polarization are: silicone oil oil bath temperature is 60-120 DEG C, and Polarization field strength is 2-3kV/mm, and the polarization time is 20-30 minute; The condition of described air polarization is: the temperature that polarizes in air is 60-120 DEG C, and Polarization field strength is 1-2kV/mm, and the polarization time is 20-30 minute.
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