CN106995313A - A kind of potassium-sodium niobate-based ceramic powder and preparation method thereof - Google Patents
A kind of potassium-sodium niobate-based ceramic powder and preparation method thereof Download PDFInfo
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- CN106995313A CN106995313A CN201710314700.1A CN201710314700A CN106995313A CN 106995313 A CN106995313 A CN 106995313A CN 201710314700 A CN201710314700 A CN 201710314700A CN 106995313 A CN106995313 A CN 106995313A
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- 239000000843 powder Substances 0.000 title claims abstract description 86
- 239000000919 ceramic Substances 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 27
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 60
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 52
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims abstract description 43
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 30
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 24
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000004939 coking Methods 0.000 claims abstract description 16
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 15
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 15
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 15
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 15
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 31
- 239000000126 substance Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 239000000084 colloidal system Substances 0.000 claims description 15
- 229910021645 metal ion Inorganic materials 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 229910010252 TiO3 Inorganic materials 0.000 claims description 14
- 238000005516 engineering process Methods 0.000 claims description 12
- 238000005253 cladding Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- 239000011858 nanopowder Substances 0.000 claims description 7
- 239000003643 water by type Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 9
- 239000007791 liquid phase Substances 0.000 abstract description 6
- 230000004523 agglutinating effect Effects 0.000 abstract description 5
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 5
- 230000002950 deficient Effects 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 235000015165 citric acid Nutrition 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 239000011259 mixed solution Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000003292 glue Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 244000131522 Citrus pyriformis Species 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 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 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005621 ferroelectricity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- -1 still Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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Abstract
The invention discloses a kind of potassium-sodium niobate-based ceramic powder, its main preparing raw material includes butyl titanate, citric acid, ethylene glycol, barium acetate, strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol.The colloidal sol that the present invention is prepared by polymer precursor, indissoluble powder suspension is coated, KNN based ceramic powder bodies are obtained by techniques such as coking, calcinings in the case of high-speed stirred.The problems such as solving liquid phase method and solid-phase method for preparing nano-sized micro-powder defective workmanship and not enough performance, and industrialization large-scale production can be realized.Meanwhile, the KNN based ceramic powder bodies of preparation have that component is homogeneous, crystallinity is high, average grain diameter is the excellent features such as 43 ~ 59nm.There are very big potentiality in terms of KNN base ceramic low-temp agglutinating properties are improved with electric property；There is huge application value and commercial promise in environmental protection, energy-conservation, the application of efficient leadless piezoelectric material material.
Description
Technical field
The present invention relates to piezoelectric ceramic powder and its preparation field, specially a kind of potassium-sodium niobate-based ceramic powder and its system
Preparation Method.
Background technology
Potassium sodium niobate piezoelectric ceramics（Referred to as KNN bases are ceramic）Material have higher Curie temperature and excellent dielectric,
Ferroelectricity and piezoelectric property etc., get more and more people's extensive concerning, and are considered as that the most potential leaded solid solution of substitution is made pottery in electronics
The material applied in porcelain component.However, when preparing KNN bases ceramics, generally existing causes system because sintering temperature is too high
Middle potassium, sodium element volatilization solute segregation and cause the defect in structure to increase, mechanical quality factor is low, dielectric properties reduction
Deng.
In order to improve the agglutinating property of KNN bases ceramics and improve electric property, typically by adding sintering aid and agglutinating property
Can good low temperature solid solution realize.But, in order to form dephasign not in KNN base ceramic structures and improve stable electrical properties
Property, generally require the high-quality powder for the nano-micrometre rank that component is homogeneous, crystal property is good, particle diameter distribution is narrow.
For the preparation of high-quality nano-micrometre powder, solid phase method is typically seldom used, is due to powder prepared by solid phase method
Body composition fluctuation is big, grain size is larger, particle diameter distribution is wide etc.；Although liquid phase method can prepare that particle diameter distribution is narrow, component is equal
One high-quality powder, still, liquid phase method mostly has that technological operation is more complicated, cost of equipment is higher, it is raw to be difficult to high-volume
The shortcomings of production.So, it would be highly desirable to optimize the preparation technology of the KNN based ceramic powder bodies of high-quality nano-micrometre rank, realize industrialization
Large-scale production, and finally realize the excellent KNN base ceramic materials of low temperature high-volume continuous production electric property.
In the planning outline of China 13, to further reaffirming with environmental protection, energy-conservation, efficient investigation of materials, study
The KNN based ceramic powder bodies for preparing high-quality nano-micrometre rank comply with the development in epoch, will also bring huge economy, society
Can benefit.
The content of the invention
In order to overcome prior art liquid phase method and solid-phase method for preparing nano-sized-micro-powder defective workmanship not enough with performance, this
Invention provides one kind using butyl titanate, citric acid, ethylene glycol, barium acetate, strontium nitrate, potassium nitrate, sodium nitrate and five oxygen
Change potassium-sodium niobate-based ceramic powder that two niobiums are prepared for primary raw material and preparation method thereof.
The object of the present invention is achieved like this：
A kind of potassium-sodium niobate-based ceramic powder, its main preparing raw material include butyl titanate, citric acid, ethylene glycol, barium acetate,
Strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol；
Described citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 3 ~ 5：1~2：14~16：18~21；
A kind of described potassium-sodium niobate-based ceramic powder, prepares colloidal sol by polymer-modified precursor process, indissoluble powder is hanged
Turbid liquid is coated in colloidal sol, and KNN base ceramic nano-powder bodies are made through techniques such as coking, calcinings；Analyzed by modern test technology
The structure and phase character of powder；
A kind of described potassium-sodium niobate-based ceramic powder, preparing the composition of the ceramic component can be represented by the chemical formula：(1−x)
K0.48Na0.52NbO3–xBa0.90Sr0.10TiO3, whereinx=0.05~0.20；
A kind of preparation method of described potassium-sodium niobate-based ceramic powder, is prepared, its concrete technology step using Sol-gel Coated method
It is as follows：
1）According to citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 3 ~ 5：1~2：14~16：18 ~ 21 mixing,
The solution A clarified for 1 ~ 2 hour is stirred at 40 ~ 50 DEG C；
2）According to metal ion molar ratio weighing barium acetate, strontium nitrate in chemical formula, dissolve in deionized water respectively, and according to
The order addition step 1 that strontium nitrate solution is added dropwise after barium acetate solution is first added dropwise）In the solution A of preparation, 55 ~ 65 DEG C are warming up to
Afterwards, the sol B stablized for 0.5 ~ 1 hour is stirred；
3）Dissolved in deionized water simultaneously according to the potassium nitrate and sodium nitrate of metal ion molar ratio weighing in chemical formula, and by
It is added dropwise to step 2）In the sol B of preparation, stir 0.5 ~ 1 hour, the colloidal sol C stablized；
4）Niobium pentaoxide powder according to metal ion molar ratio weighing in chemical formula is added in 40 ~ 50ml deionized waters,
Through ultrasonic disperse 20 ~ 30 minutes, obtained powder suspension is stirred vigorously；
5）By step 4）The suspension of preparation is added dropwise to stir speed (S.S.) for 600 ~ 800r/min steps 3）The solution C of preparation
In, stir 1 ~ 2 hour, the liquid of Sol-gel Coated is made；The liquid of Sol-gel Coated dries 1 ~ 2 hour in 100 ~ 120 DEG C of baking ovens
To cladding colloid D；
6）By step 5）The cladding colloid D of preparation coking 1.5 ~ 2 hours first in 300 ~ 400 DEG C of Muffle furnace, it is polished
Calcining obtains KNN based ceramic powder bodies for 2 ~ 3 hours in 850 ~ 950 DEG C of high temperature furnace.
Positive beneficial effect：The colloidal sol that the present invention is prepared by polymer precursor, by difficulty in the case of high-speed stirred
Molten powder suspension cladding, KNN based ceramic powder bodies are obtained by techniques such as coking, calcinings.Solve liquid phase method and solid phase legal system
The problems such as standby nano-micrometre powder defective workmanship and not enough performance, and industrialization large-scale production can be realized.Meanwhile, prepare
KNN based ceramic powder bodies have that component is homogeneous, crystallinity is high, average grain diameter is the excellent features such as 43 ~ 59nm.Improving KNN
There are very big potentiality in terms of base ceramic low-temp agglutinating property and electric property；In environmental protection, energy-conservation, efficient leadless piezoelectric material material
Application in have huge application value and commercial promise.
Brief description of the drawings
Fig. 1 is the x-ray diffraction pattern of the KNN base ceramic nano-powder bodies prepared in the present invention；
Fig. 2 is the cold field emission scanning electron microscope (SEM) photograph of the KNN base ceramic nano-powder bodies prepared in the present invention.
Embodiment
With reference to specific embodiment, the present invention is described further：
Embodiment 1
A kind of potassium-sodium niobate-based ceramic powder, its main preparing raw material include butyl titanate, citric acid, ethylene glycol, barium acetate,
Strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol；Described citric acid：Butyl titanate：Ethylene glycol：Alcohol rubs
Your mass ratio is 4：1：15：20；A kind of described potassium-sodium niobate-based ceramic powder, is prepared molten by polymer-modified precursor process
Glue, indissoluble powder suspension is coated in colloidal sol, and KNN base ceramic nano-powder bodies are made through techniques such as coking, calcinings；By existing
The structure and phase character of powder are analyzed for measuring technology；A kind of described potassium-sodium niobate-based ceramic powder, prepare the ceramics into
The composition divided can be represented by the chemical formula： (1−x)K0.48Na0.52NbO3–xBa0.90Sr0.10TiO3, whereinx=0.05~0.20；
A kind of preparation method of described potassium-sodium niobate-based ceramic powder, is prepared, its concrete technology step using Sol-gel Coated method
It is as follows：
1）According to citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 4：1：15：20 mixing, are stirred at 40 DEG C
Mix the solution A clarified for 1 hour；
2）According to metal ion molar ratio weighing barium acetate, strontium nitrate in chemical formula, dissolve in deionized water respectively, and according to
The order addition step 1 that strontium nitrate solution is added dropwise after barium acetate solution is first added dropwise）In the solution A of preparation, it is warming up to after 55 DEG C, stirs
Mix the sol B stablized for 0.5 hour；
3）Dissolved in deionized water simultaneously according to the potassium nitrate and sodium nitrate of metal ion molar ratio weighing in chemical formula, and by
It is added dropwise to step 2）In the sol B of preparation, stir 0.5 hour, the colloidal sol C stablized；
4）Niobium pentaoxide powder according to metal ion molar ratio weighing in chemical formula is added in 40ml deionized waters, through super
Sound is scattered 20 ~ 30 minutes, is stirred vigorously obtained powder suspension；
5）By step 4）The suspension of preparation is added dropwise to stir speed (S.S.) for 600r/min steps 3）In the solution C of preparation, stir
Mix 1 ~ 2 hour, the liquid of Sol-gel Coated is made；The liquid of Sol-gel Coated dries in 100 DEG C of baking ovens obtains cladding colloid D for 1 hour；
6）By step 5）The cladding colloid D of preparation coking 1.5 hours first in 300 ~ 400 DEG C of Muffle furnace, it is polished
Calcining obtains KNN based ceramic powder bodies for 2 hours in 850 DEG C of high temperature furnace.
Embodiment 2
A kind of potassium-sodium niobate-based ceramic powder, its main preparing raw material include butyl titanate, citric acid, ethylene glycol, barium acetate,
Strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol；Described citric acid：Butyl titanate：Ethylene glycol：Alcohol rubs
Your mass ratio is 3：1：15：21；A kind of described potassium-sodium niobate-based ceramic powder, is prepared molten by polymer-modified precursor process
Glue, indissoluble powder suspension is coated in colloidal sol, and KNN base ceramic nano-powder bodies are made through techniques such as coking, calcinings；By existing
The structure and phase character of powder are analyzed for measuring technology；A kind of described potassium-sodium niobate-based ceramic powder, prepare the ceramics into
The composition divided can be represented by the chemical formula： (1−x)K0.48Na0.52NbO3–xBa0.90Sr0.10TiO3, whereinx=0.05~0.20；
A kind of preparation method of described potassium-sodium niobate-based ceramic powder, is prepared, its concrete technology step using Sol-gel Coated method
It is as follows：
1）According to citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 3：1：15：21 mixing, at 40 ~ 50 DEG C
It is lower to stir the solution A clarified for 1 ~ 2 hour；
2）According to metal ion molar ratio weighing barium acetate, strontium nitrate in chemical formula, dissolve in deionized water respectively, and according to
The order addition step 1 that strontium nitrate solution is added dropwise after barium acetate solution is first added dropwise）In the solution A of preparation, it is warming up to after 60 DEG C, stirs
Mix the sol B stablized for 0.8 hour；
3）Dissolved in deionized water simultaneously according to the potassium nitrate and sodium nitrate of metal ion molar ratio weighing in chemical formula, and by
It is added dropwise to step 2）In the sol B of preparation, stir 0.8 hour, the colloidal sol C stablized；
4）Niobium pentaoxide powder according to metal ion molar ratio weighing in chemical formula is added in 45ml deionized waters, through super
Sound is scattered 25 minutes, is stirred vigorously obtained powder suspension；
5）By step 4）The suspension of preparation is added dropwise to stir speed (S.S.) for 700r/min steps 3）In the solution C of preparation, stir
Mix 1.5 hours, the liquid of Sol-gel Coated is made；The liquid of Sol-gel Coated dries in 110 DEG C of baking ovens to be obtained coating colloid for 1.5 hours
D；
6）By step 5）Cladding colloid D coking 1.8 hours first in 350 DEG C of Muffle furnace of preparation, it is polished at 900 DEG C
High temperature furnace in calcining obtain within 2.5 hours KNN based ceramic powder bodies.
Embodiment 3
A kind of potassium-sodium niobate-based ceramic powder, its main preparing raw material include butyl titanate, citric acid, ethylene glycol, barium acetate,
Strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol；Described citric acid：Butyl titanate：Ethylene glycol：Alcohol rubs
Your mass ratio is 4：2：15：19；A kind of described potassium-sodium niobate-based ceramic powder, is prepared molten by polymer-modified precursor process
Glue, indissoluble powder suspension is coated in colloidal sol, and KNN base ceramic nano-powder bodies are made through techniques such as coking, calcinings；By existing
The structure and phase character of powder are analyzed for measuring technology；A kind of described potassium-sodium niobate-based ceramic powder, prepare the ceramics into
The composition divided can be represented by the chemical formula： (1−x)K0.48Na0.52NbO3–xBa0.90Sr0.10TiO3, whereinx=0.05~0.20；
A kind of preparation method of described potassium-sodium niobate-based ceramic powder, is prepared, its concrete technology step using Sol-gel Coated method
It is as follows：
1）According to citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 4：2：15：19 mixing, are stirred at 50 DEG C
Mix the solution A clarified for 2 hours；
2）According to metal ion molar ratio weighing barium acetate, strontium nitrate in chemical formula, dissolve in deionized water respectively, and according to
The order addition step 1 that strontium nitrate solution is added dropwise after barium acetate solution is first added dropwise）In the solution A of preparation, it is warming up to after 65 DEG C, stirs
Mix the sol B stablized for 1 hour；
3）Dissolved in deionized water simultaneously according to the potassium nitrate and sodium nitrate of metal ion molar ratio weighing in chemical formula, and by
It is added dropwise to step 2）In the sol B of preparation, stir 1 hour, the colloidal sol C stablized；
4）Niobium pentaoxide powder according to metal ion molar ratio weighing in chemical formula is added in 50ml deionized waters, through super
Sound is scattered 30 minutes, is stirred vigorously obtained powder suspension；
5）By step 4）The suspension of preparation is added dropwise to stir speed (S.S.) for 800r/min steps 3）In the solution C of preparation, stir
Mix 2 hours, the liquid of Sol-gel Coated is made；The liquid of Sol-gel Coated dries in 120 DEG C of baking ovens obtains cladding colloid D for 2 hours；
6）By step 5）Cladding colloid D coking 2 hours first in 400 DEG C of Muffle furnace of preparation, it is polished at 950 DEG C
Calcining obtains KNN based ceramic powder bodies for 3 hours in high temperature furnace.
Embodiment 4
Prepare 0.95K0.48Na0.52NbO3–0.05Ba0.90Sr0.10TiO3Ceramic powder：Take 0.1702g butyl titanates and
0.4203g citric acids are dissolved in 0.4655g ethylene glycol with 0.6207g alcohol mixed solutions, stirring and obtaining at 45 DEG C for 1 hour
The solution A of clarification；0.1149g barium acetates and 0.0106g strontium nitrates are dissolved in deionized water respectively, then according to being first added dropwise
The order that strontium nitrate is added dropwise after barium acetate is added dropwise in above-mentioned solution A, is warming up to stirring after 60 DEG C and is obtained within 0.5 hour stabilization
Sol B；Weigh 0.4610g potassium nitrate and 0.4199g sodium nitrate dissolves in deionized water together, then drip mixed solution
It is added in above-mentioned sol B, stirs 0.5 hour, stable colloidal sol C is made；2.5252g niobium pentaoxide powders are taken to be added to 45ml
In deionized water, powder suspension is made in ultrasonic disperse after 30 minutes；Suspension is added dropwise to mixing speed for 750r/
In min above-mentioned colloidal sol C, stir 1.5 hours, the liquid of Sol-gel Coated is made, liquid dries 1.5 hours in 110 DEG C of baking ovens
To cladding colloid D；By colloid D in 350 DEG C of Muffle furnace coking 1.5 hours, calcine 2.5 in 900 DEG C of high temperature furnaces after grinding
Hour obtains 0.95K0.48Na0.52NbO3–0.05Ba0.90Sr0.10TiO3Ceramic powder.
0.95K0.48Na0.52NbO3–0.05Ba0.90Sr0.10TiO3Ceramic powder has high crystallinity；Average particle diameter size
For 43nm.
Embodiment 5
0.90K0.48Na0.52NbO3–0.10Ba0.90Sr0.10TiO3Ceramic powder：Take 0.3404g butyl titanates and 0.8406g lemons
Lemon acid is dissolved in 0.9310g ethylene glycol and 1.2414g alcohol mixed solutions, at 45 DEG C stirring clarified within 1 hour it is molten
Liquid A；0.2298g barium acetates and 0.0212g strontium nitrates are dissolved in deionized water respectively, then according to first be added dropwise barium acetate after
The order that strontium nitrate is added dropwise is added dropwise in above-mentioned solution A, is warming up to the sol B that stirring is stablized for 0.5 hour after 60 DEG C；
Weigh 0.4367g potassium nitrate and 0.3978g sodium nitrate dissolves in deionized water together, be then added drop-wise to mixed solution above-mentioned
In sol B, stir 0.5 hour, stable colloidal sol C is made；2.3923g niobium pentaoxide powders are taken to be added to 42ml deionized waters
In, powder suspension is made in ultrasonic disperse after 27 minutes；It is the above-mentioned of 750r/min that suspension is added dropwise into mixing speed
In colloidal sol C, stir 1.5 hours, the liquid of Sol-gel Coated is made, liquid dries in 110 DEG C of baking ovens to be obtained coating colloid for 1.5 hours
D；By colloid D in 350 DEG C of Muffle furnaces coking 1.5 hours, calcine and obtain in 900 DEG C of high temperature furnaces after grinding for 2.5 hours
0.90K0.48Na0.52NbO3–0.10Ba0.90Sr0.10TiO3Ceramic powder.
0.90K0.48Na0.52NbO3–0.10Ba0.90Sr0.10TiO3Ceramic powder has high crystallinity；Average particle diameter size
For 52nm.
Embodiment 6
0.85K0.48Na0.52NbO3–0.15Ba0.90Sr0.10TiO3Ceramic powder：Take 0.5106g butyl titanates and 1.2609g lemons
Lemon acid is dissolved in 1.3965g ethylene glycol and 1.8621g alcohol mixed solutions, at 45 DEG C stirring clarified within 1 hour it is molten
Liquid A；0.3447g barium acetates and 0.0318g strontium nitrates are dissolved in deionized water respectively, then according to first be added dropwise barium acetate after
The order that strontium nitrate is added dropwise is added dropwise in above-mentioned solution A, is warming up to the sol B that stirring is stablized for 0.5 hour after 60 DEG C；
Weigh 0.4125g potassium nitrate and 0.3757g sodium nitrate dissolves in deionized water together, be then added drop-wise to mixed solution above-mentioned
In sol B, stir 0.5 hour, stable colloidal sol C is made；2.2594g niobium pentaoxide powders are taken to be added to 40ml deionization
In water, powder suspension is made in ultrasonic disperse after 25 minutes；It is the upper of 750r/min that suspension is added dropwise into mixing speed
State in colloidal sol C, stir 1.5 hours, the liquid of Sol-gel Coated is made, liquid dries in 110 DEG C of baking ovens to be obtained coating glue for 1.5 hours
Body D；By colloid D in 350 DEG C of Muffle furnace coking 1.5 hours, calcine and obtain in 900 DEG C of high temperature furnaces after grinding for 2.5 hours
0.85K0.48Na0.52NbO3–0.15Ba0.90Sr0.10TiO3Ceramic powder.
0.85K0.48Na0.52NbO3–0.15Ba0.90Sr0.10TiO3Ceramic powder has high crystallinity；Average particle diameter size
For 59nm.
The colloidal sol that the present invention is prepared by polymer precursor, by indissoluble powder suspension bag in the case of high-speed stirred
Cover, KNN based ceramic powder bodies are obtained by techniques such as coking, calcinings.Solve liquid phase method and solid-phase method for preparing nano-sized-micro-powder
The problems such as defective workmanship and not enough performance, and industrialization large-scale production can be realized.Meanwhile, the KNN based ceramic powder bodies of preparation
With component is homogeneous, crystallinity is high, average grain diameter is the excellent features such as 43 ~ 59nm.Improving KNN base ceramic low-temp agglutinating properties
With having very big potentiality in terms of electric property；Have in environmental protection, energy-conservation, the application of efficient leadless piezoelectric material material huge
Application value and commercial promise.
Above example is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the knowledge that the field those of ordinary skill possesses, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., it all should cover within the scope of claimed technical scheme of the invention.
Claims (5)
1. a kind of potassium-sodium niobate-based ceramic powder, it is characterised in that：Its main preparing raw material include butyl titanate, citric acid,
Ethylene glycol, barium acetate, strontium nitrate, potassium nitrate, sodium nitrate, niobium pentaoxide and alcohol.
2. a kind of potassium-sodium niobate-based ceramic powder according to claim 1, it is characterised in that：Described citric acid：Metatitanic acid
Four butyl esters：Ethylene glycol：The molal weight ratio of alcohol is 3 ~ 5：1~2：14~16：18~21.
3. described in a kind of potassium-sodium niobate-based ceramic powder, colloidal sol is prepared by polymer-modified precursor process, by indissoluble powder
Suspension is coated in colloidal sol, and KNN base ceramic nano-powder bodies are made through techniques such as coking, calcinings；Pass through modern test technology point
Analyse the structure and phase character of powder.
4. a kind of potassium-sodium niobate-based ceramic powder according to claim 1, it is characterised in that：Prepare the group of the ceramic component
Into can be represented by the chemical formula：(1−x)K0.48Na0.52NbO3–xBa0.90Sr0.10TiO3, whereinx=0.05~0.20。
5. a kind of preparation method of potassium-sodium niobate-based ceramic powder as described in claim 1-3 Arbitrary Terms, it is characterised in that：Adopt
Prepared with Sol-gel Coated method, its concrete technology step is as follows：
1）According to citric acid：Butyl titanate：Ethylene glycol：The molal weight ratio of alcohol is 3 ~ 5：1~2：14~16：18 ~ 21 mixing,
The solution A clarified for 1 ~ 2 hour is stirred at 40 ~ 50 DEG C；
2）According to metal ion molar ratio weighing barium acetate, strontium nitrate in chemical formula, dissolve in deionized water respectively, and press
Step 1 is added according to the order that dropwise addition strontium nitrate solution after barium acetate solution is first added dropwise）In the solution A of preparation, 55 ~ 65 DEG C are warming up to
Afterwards, the sol B stablized for 0.5 ~ 1 hour is stirred；
3）Dissolved in deionized water simultaneously according to the potassium nitrate and sodium nitrate of metal ion molar ratio weighing in chemical formula, and by
It is added dropwise to step 2）In the sol B of preparation, stir 0.5 ~ 1 hour, the colloidal sol C stablized；
4）Niobium pentaoxide powder according to metal ion molar ratio weighing in chemical formula is added in 40 ~ 50ml deionized waters,
Through ultrasonic disperse 20 ~ 30 minutes, obtained powder suspension is stirred vigorously；
5）By step 4）The suspension of preparation is added dropwise to stir speed (S.S.) for 600 ~ 800r/min steps 3）The solution C of preparation
In, stir 1 ~ 2 hour, the liquid of Sol-gel Coated is made;
The liquid of Sol-gel Coated dries in 100 ~ 120 DEG C of baking ovens obtains cladding colloid D for 1 ~ 2 hour；
6）By step 5）The cladding colloid D of preparation coking 1.5 ~ 2 hours first in 300 ~ 400 DEG C of Muffle furnace, it is polished
Calcining obtains KNN based ceramic powder bodies for 2 ~ 3 hours in 850 ~ 950 DEG C of high temperature furnace.
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