CN101613201A - The method of synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps - Google Patents
The method of synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps Download PDFInfo
- Publication number
- CN101613201A CN101613201A CN200910031941A CN200910031941A CN101613201A CN 101613201 A CN101613201 A CN 101613201A CN 200910031941 A CN200910031941 A CN 200910031941A CN 200910031941 A CN200910031941 A CN 200910031941A CN 101613201 A CN101613201 A CN 101613201A
- Authority
- CN
- China
- Prior art keywords
- potassium
- powder
- hydro
- obtains
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 70
- 239000000919 ceramic Substances 0.000 title claims abstract description 39
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 19
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 84
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 57
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 41
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 18
- 239000011734 sodium Substances 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 13
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 12
- 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 description 12
- 238000003828 vacuum filtration Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000012856 packing Methods 0.000 claims description 10
- 238000012423 maintenance Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 6
- 239000010955 niobium Substances 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 229910052758 niobium Inorganic materials 0.000 abstract description 4
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 abstract description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001950 potassium oxide Inorganic materials 0.000 abstract description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract description 3
- 229910001948 sodium oxide Inorganic materials 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- 239000012071 phase Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- 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
- 230000018199 S phase Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of method of synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps, this method adopts two one-step hydrothermals, the first step obtains potassium niobate powder by oxide compound hydro-thermal reactions such as potassium hydroxide and Niobium Pentxoxides, adopts this powder and sodium hydroxide to carry out the final successfully potassium-sodium niobate powder of synthetic pure phase of the second step hydro-thermal reaction.Adopt that two one-step hydro-thermal synthesis method synthetic potassium-sodium niobate system lead-free piezoelectric ceramic powders provided by the invention have high-purity, ultra-fine, good fluidity, narrow diameter distribution, the particle agglomeration degree is light, crystal development is complete and the sintering activity advantages of higher, be convenient to sintered leadless free piezoelectric ceramics at a lower temperature, thereby avoid the volatilization of oxide compound such as potassium oxide and sodium oxide in the sintering process, finally realize the raising of potassium-sodium niobate system leadless piezoelectric ceramics piezoelectric property and mechanical property.
Description
One, technical field
The present invention relates to a kind of preparation method of piezoelectric ceramic powder, relate in particular to a kind of preparation method of lead-free piezoelectric ceramic powder.
Two, background technology
Piezoceramic material is an important functional material, is widely used in transverter, piezoelectric transformer, fields such as wave filter and ultrasonic motor.Piezoelectric ceramics occupies quite great proportion as important functional material in field of electronic materials.In recent years, piezoelectric ceramics was pressed about 15% speed increment at global annual sales.According to statistics, global piezoelectric ceramics product sales reached more than 3,000,000,000 dollars approximately in 2000.But, traditional piezoceramic material mainly is the lead base pottery, though it has piezoelectric property preferably, but plumbous all have very big harm to environment and human health, with the PZT piezoelectric ceramics is example, plumbous oxide accounts for more than 60% of its material content, in preparation, all can produce adverse influence to environment in use and the discarded aftertreatment.Calendar year 2001, European Parliament passed through the decree about " limiting objectionable impurities in electrical equipment and the electronics ", and implemented due to 2006.Wherein in the material that is limited to use, just comprise plumbiferous piezoelectric device.This shows that the forbidding that contains lead piezoelectric ceramics is an inexorable trend, thereby lead-free environmentally friendly lead-free piezoceramic material becomes the focus of research.
Present lead-free piezoceramic material mainly contains BaTiO
3Base, Bi
1/2Na
1/2TiO
3(BNT) base, niobate, bismuth laminated leadless piezoelectric ceramic etc.Na wherein
0.5K
0.5NbO
3(being called for short KNN) piezoceramic material belongs to perovskite structure, its Curie temperature is about 415 ℃, it under the room temperature oblique side's phase, be regarded as one of candidate material that substitutes conventional P ZT piezoelectric ceramics, domestic and international research in this respect rests on simple system more in a very long time, and the piezoelectric property of material is not high yet.In people's such as the Saito Y of institute of central authorities of Japanese Toyota research, obtained d
33At the niobate lead-free piezoelectric ceramics of 416pC/N, this has just caused people's attention again.But technology is too complicated, is difficult to be employed.Compare with the PZT piezoelectric ceramics, because potassium oxide and sodium oxide volatilize easily, the preparation technology of KNN is poor, and when normal atmospheric was depressed sintering, the density of pottery had only 90% of theoretical density, short texture, and performance is undesirable.
The synthetic methods such as solid-phase synthesis, hydrothermal method, sol-gel method that mainly contain of piezoelectric ceramic powder.Solid-phase synthesis is a kind of traditional powder synthetic method, and raw material is mixed pulverizing behind high temperature solid state reaction and obtains powder.This method has advantages such as cost is low, and technology is simple, but this method is difficult to make raw material to mix, and particle slightly disperses, and to potassium-sodium niobate series leadless piezoelectric ceramics, the powder of this method preparation is difficult to sintering.Therefore, adopt the synthetic potassium-sodium niobate system lead-free piezoelectric ceramic powder of wet chemical method such as hydrothermal method and sol-gel method more and more to come into one's own.
That the superfine powder of Hydrothermal Preparation has is high-purity, ultra-fine, good fluidity, narrow diameter distribution, the particle agglomeration degree is light, crystal development is complete and the sintering activity advantages of higher.Simultaneously, the Hydrothermal Preparation powder is once to finish in liquid phase, do not need the thermal treatment in later stage, thereby avoided growing up voluntarily and sneaking into impurity etc. easily owing to hard aggregation, crystal grain that the later stage sintering produces powder, therefore the Hydrothermal Preparation ceramic powder is to improving the ceramic post sintering activity, and reducing sintering temperature has very significance.Hydrothermal method has obtained in fields such as nano materials using widely in recent years, at present the synthetic potassium-sodium niobate powder preparing KNN series lead-free piezoelectric ceramic of hydrothermal method report very few, but (Takahashi H such as Takahashi, Numamoto Y, Tani J, et al.[J] .Jpn J Appl Phys, 2006,45 (1-3): L30-L32.).With hydrothermal method synthetic BT lead-free piezoelectric ceramic powder, obtained the ceramic of compact that density reaches theoretical density 98.3%, electromechanical coupling factor has reached 36%; (Karaki T, YanK, Adachi M, [J] .Applied Physics Express, 2008 (1): 111402.) such as Karaki.Adopt two-step sintering method to prepare the BT piezoelectric ceramics that piezoelectric constant is 460pC/N with the hydro-thermal powder, shown good piezoelectric property.Vousden (Vousden P, [J] .Acta Crystallogr, 1951,4:373-376.) at first with the synthetic NaNbO of hydrothermal method
3Powder, people such as Kinomura are with Na
8[Nb
6O
9] 13H
2O is a raw material, is that mineralizer has prepared NaNbO with NaOH
3(Kinomura N, Kumata N, Muto F, [J] .Mat Res Bull, 1984,19:299-304.), human hydrothermal methods such as Santos have been synthesized the NaNbO of single-phase rhombic system
3Powder, and reported the differential responses time, different mol ratio to the influence of product (Santos I, Loureiro L, Silva M, et al.[J] .Polyhedron, 2002,21:2009-2015.).Had in the recent period the investigator to begin to carry out the research of the synthetic pure phase KNN of hydro-thermal, and obtained preliminary progress (Zhang F, Han L, Bai S, et al.[J] .Jpn J Appl Phys, 2008.47 (9): 7685-7688.).But these preparation methods are single stage method.Because sodium ion radius (0.97
) less than potassium ion radius (1.33
), sodium ion is faster than potassium ion with the Niobium Pentxoxide speed of response under hydrothermal condition, when making the disposable hydro-thermal reaction of raw materials such as potassium hydroxide, sodium hydroxide and Niobium Pentxoxide, is easy to synthetic separately sodium columbate and potassium niobate, the powder that obtains mostly is two-phase coexistent, is not easy to obtain the K that has of pure phase
0.5Na
0.5NbO
3The ceramic powder of composition.
Three, summary of the invention
1, technical problem: the technical problem to be solved in the present invention provides a kind of method for preparing lead-free piezoelectric ceramic powder, this method adopts two one-step hydrothermals, the first step obtains potassium niobate powder by oxide compound hydro-thermal reactions such as potassium hydroxide and Niobium Pentxoxides, adopts this powder and sodium hydroxide to carry out the final successfully potassium-sodium niobate powder of synthetic pure phase of the second step hydro-thermal reaction.
2, technical scheme:
In order to solve above-mentioned technical problem, the method for the synthetic lead-free piezoelectric ceramic powder of two step hydro-thermals of the present invention comprises the following steps:
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 0.5M～2M, the concentration of sodium hydroxide solution is 0.5M～2M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 20%～80%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 5～1: 30; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 5～60 minutes;
Step 4: with the described polytetrafluoroethyllining lining of the step 2 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃～300 ℃, and the time is 4～36 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 60 ℃～100 ℃ dry down potassium niobate powders that obtained good dispersity in 24～48 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 20%～80%;
Step 7: take by weighing rapid five potassium niobate powders that obtain and pour in the mixing solutions of step 6, stirred 5～60 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 4～5: 1;
Step 8: with the polytetrafluoroethyllining lining of the step 6 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃～300 ℃, and the time is 4～36 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 24～48 hours at 60 ℃～100 ℃, obtained the potassium-sodium niobate K of good dispersity
xNa
(1-x)NbO
3Powder, wherein 0.1≤x≤0.9.
The potassium niobate powder that above-mentioned steps six obtains by step 5 to step 9 makes dispersiveness potassium-sodium niobate powder preferably.
3, beneficial effect
Adopt that two one-step hydro-thermal synthesis method synthetic potassium-sodium niobate system lead-free piezoelectric ceramic powders provided by the invention have high-purity, ultra-fine, good fluidity, narrow diameter distribution, the particle agglomeration degree is light, crystal development is complete and the sintering activity advantages of higher, be convenient to sintered leadless free piezoelectric ceramics at a lower temperature, thereby avoid the volatilization of oxide compound such as potassium oxide and sodium oxide in the sintering process, finally realize the raising of potassium-sodium niobate system leadless piezoelectric ceramics piezoelectric property and mechanical property.As shown in Figure 2, particle is cube bulk of rule as can be seen, and crystal grain is grown complete, and the reunion degree is light.
Four, description of drawings
Fig. 1 is the structural representation of stainless steel hydrothermal reaction kettle among the present invention;
Fig. 2 is the present invention's two one-step hydro-thermal synthesis method synthetic potassium-sodium niobate system lead-free piezoelectric ceramic powder SEM synoptic diagram, and its molecular formula is K
0.24Na
0.76NbO
3
Five, embodiment
The synthetic K of embodiment one: two step hydro-thermal
0.1Na
0.9NbO
3Lead-free piezoelectric ceramic powder;
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 2M, the concentration of sodium hydroxide solution is 2M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 50%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 5; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 60 minutes;
Step 4: with pack into as shown in Figure 1 stainless steel hydrothermal reaction kettle 1 of the described polytetrafluoroethyllining lining 11 of step 2, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃, and the time is 24 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 60 ℃ of dry down potassium niobate powders that obtained good dispersity in 24 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 50%, to realize the auxiliary hydrothermal synthesis reaction of Virahol;
Step 7: take by weighing the potassium niobate powder that step 5 obtains and pour in the mixing solutions of step 6, stirred 30 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 4;
Step 8: with pack into as shown in Figure 1 stainless steel hydrothermal reaction kettle of the polytetrafluoroethyllining lining of step 6, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃, and the time is 24 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 24 hours at 60 ℃, obtained the potassium-sodium niobate K of good dispersity
0.1Na
0.9NbO
3Powder.
The synthetic K of embodiment two: two steps hydro-thermal
0.9Na
0.1NbO
3Lead-free piezoelectric ceramic powder;
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 1M, the concentration of sodium hydroxide solution is 1M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 80%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 30; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 30 minutes;
Step 4: with the described polytetrafluoroethyllining lining of the step 2 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 300 ℃, and the time is 36 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 100 ℃ of dry down potassium niobate powders that obtained good dispersity in 48 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 80%;
Step 7: take by weighing rapid five potassium niobate powders that obtain and pour in the mixing solutions of step 6, stirred 60 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 1;
Step 8: with the polytetrafluoroethyllining lining of the step 6 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 300 ℃, and the time is 36 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 48 hours at 100 ℃, obtained the potassium-sodium niobate K of good dispersity
0.9Na
0.1NbO
3Powder.
The synthetic K of embodiment three: two steps hydro-thermal
0.5Na
0.5NbO
3Lead-free piezoelectric ceramic powder;
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 2M, the concentration of sodium hydroxide solution is 2M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 80%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 20; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 60 minutes;
Step 4: with the described polytetrafluoroethyllining lining of the step 2 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 200 ℃, and the time is 24 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 80 ℃ of dry down potassium niobate powders that obtained good dispersity in 48 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 80%;
Step 7: take by weighing rapid five potassium niobate powders that obtain and pour in the mixing solutions of step 6, stirred 30 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 3;
Step 8: with the polytetrafluoroethyllining lining of the step 6 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 200 ℃, and the time is 6 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 48 hours at 80 ℃, obtained the potassium-sodium niobate K of good dispersity
0.5Na
0.5NbO
3Powder.
The synthetic K of embodiment four: two steps hydro-thermal
0.24Na
0.76NbO
3Lead-free piezoelectric ceramic powder;
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 2M, the concentration of sodium hydroxide solution is 2M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 80%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 25; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 60 minutes;
Step 4: with the described polytetrafluoroethyllining lining of the step 2 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 200 ℃, and the time is 24 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 80 ℃ of dry down potassium niobate powders that obtained good dispersity in 48 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 80%;
Step 7: take by weighing rapid five potassium niobate powders that obtain and pour in the mixing solutions of step 6, stirred 30 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 2;
Step 8: with the polytetrafluoroethyllining lining of the step 6 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 200 ℃, and the time is 6 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 48 hours at 80 ℃, obtained the potassium-sodium niobate K of good dispersity
0.24Na
0.76NbO
3Powder.
As shown in Figure 2, the molecular formula of present embodiment preparation is K as can be seen
0.24Na
0.76NbO
3Piezoelectric ceramic powder be the rule cube bulk, crystal development is complete, the reunion degree is light.
Claims (1)
1, a kind of method of synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps is characterized in that, comprises the following steps:
Step 1: preparation potassium hydroxide and sodium hydroxide solution, the concentration of potassium hydroxide solution is 0.5M～2M, the concentration of sodium hydroxide solution is 0.5M～2M;
Step 2: adopt the potassium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, and the maintenance compactedness is 20%～80%;
Step 3: take by weighing niobium pentaoxide powder, with potassium hydroxide mol ratio in the step 1 be 1: 5～1: 30; And the niobium pentaoxide powder that takes by weighing is poured in the mixing solutions of step 2, stirred 5～60 minutes;
Step 4: with the described polytetrafluoroethyllining lining of the step 2 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃～300 ℃, and the time is 4～36 hours, obtains throw out;
Step 5: the throw out that step 4 obtains is extremely neutral with the deionized water vacuum filtration, and the filter cake that obtains is at 60 ℃～100 ℃ dry down potassium niobate powders that obtained good dispersity in 24～48 hours;
Step 6: adopt the sodium hydroxide solution of step 1 and the mixing solutions that Virahol configuration volume ratio is 2: 3, pour in the polytetrafluoroethyllining lining, keeping compactedness is 20%～80%;
Step 7: take by weighing rapid five potassium niobate powders that obtain and pour in the mixing solutions of step 6, stirred 30 minutes 5～60 minutes, the mol ratio of sodium hydroxide and potassium niobate is 5: 4～5: 1;
Step 8: with the polytetrafluoroethyllining lining of the step 6 stainless steel hydrothermal reaction kettle of packing into, put into baking oven and carry out hydro-thermal reaction, temperature is 160 ℃～300 ℃, and the time is 4～36 hours, obtains throw out;
Step 9: the throw out that step 8 obtains is extremely neutral with the deionized water vacuum filtration; The filter cake that obtains descended dry 24～48 hours at 60 ℃～100 ℃, obtained the potassium-sodium niobate K of good dispersity
xNa
(1-x)NbO
3Powder, wherein 0.1＜x≤0.9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100319410A CN101613201B (en) | 2009-06-25 | 2009-06-25 | Method for synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100319410A CN101613201B (en) | 2009-06-25 | 2009-06-25 | Method for synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101613201A true CN101613201A (en) | 2009-12-30 |
| CN101613201B CN101613201B (en) | 2011-11-30 |
Family
ID=41493110
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100319410A Active CN101613201B (en) | 2009-06-25 | 2009-06-25 | Method for synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101613201B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060545A (en) * | 2010-11-29 | 2011-05-18 | 南京航空航天大学 | Preparation method of spherical microporous niobate molecular sieve fiber |
| KR101381130B1 (en) | 2007-08-29 | 2014-04-04 | 알까뗄 루슨트 | Multi-user precoding and scheduling method and base station for implementing the method |
| CN104098334A (en) * | 2014-07-14 | 2014-10-15 | 陕西科技大学 | Method for synthetizing leadless piezoelectric ceramic K0.65Na0.35NbO3 powder adopting two-step hydrothermal method |
| CN104119077A (en) * | 2014-07-25 | 2014-10-29 | 陕西科技大学 | One-step method for synthesizing leadless piezoelectric K0.1Na0.9NbO3 powder by hydrothermal process |
| CN104119078A (en) * | 2014-07-25 | 2014-10-29 | 陕西科技大学 | Method for preparing KNN (K, Na, Nb) series low-loss leadless piezoelectric ceramic |
| CN110041073A (en) * | 2019-05-31 | 2019-07-23 | 河南科技大学 | A kind of preparation method of potassium sodium niobate ceramic |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321901C (en) * | 2006-03-03 | 2007-06-20 | 北京工业大学 | Coprecipitation process of preparing relation base niobate ferroelectric powder |
| CN100575305C (en) * | 2007-10-19 | 2009-12-30 | 北京工业大学 | The colloidal sols gelatin synthesizing method of leadless piezoelectric ceramic lithium sodium kalium niobate nano-powder |
| CN101186338B (en) * | 2007-12-04 | 2010-06-09 | 北京科技大学 | Hydro-thermal synthesis method for tantalum adulterated potassium sodium niobate leadless piezoelectric ceramic powder |
-
2009
- 2009-06-25 CN CN2009100319410A patent/CN101613201B/en active Active
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101381130B1 (en) | 2007-08-29 | 2014-04-04 | 알까뗄 루슨트 | Multi-user precoding and scheduling method and base station for implementing the method |
| CN102060545A (en) * | 2010-11-29 | 2011-05-18 | 南京航空航天大学 | Preparation method of spherical microporous niobate molecular sieve fiber |
| CN102060545B (en) * | 2010-11-29 | 2012-12-26 | 南京航空航天大学 | Preparation method of spherical microporous niobate molecular sieve fiber |
| CN104098334A (en) * | 2014-07-14 | 2014-10-15 | 陕西科技大学 | Method for synthetizing leadless piezoelectric ceramic K0.65Na0.35NbO3 powder adopting two-step hydrothermal method |
| CN104098334B (en) * | 2014-07-14 | 2016-08-24 | 陕西科技大学 | A kind of two one-step hydrothermal synthesis leadless piezo-electric ceramic Ks0.65na0.35nbO3the method of powder body |
| CN104119077A (en) * | 2014-07-25 | 2014-10-29 | 陕西科技大学 | One-step method for synthesizing leadless piezoelectric K0.1Na0.9NbO3 powder by hydrothermal process |
| CN104119078A (en) * | 2014-07-25 | 2014-10-29 | 陕西科技大学 | Method for preparing KNN (K, Na, Nb) series low-loss leadless piezoelectric ceramic |
| CN104119077B (en) * | 2014-07-25 | 2016-04-06 | 陕西科技大学 | A kind of hydrothermal method one-step synthesis leadless piezoelectric K 0.1na 0.9nbO 3the method of powder |
| CN104119078B (en) * | 2014-07-25 | 2016-08-24 | 陕西科技大学 | A kind of KNN system low-loss leadless piezoelectric ceramics preparation method |
| CN110041073A (en) * | 2019-05-31 | 2019-07-23 | 河南科技大学 | A kind of preparation method of potassium sodium niobate ceramic |
| CN110041073B (en) * | 2019-05-31 | 2021-11-23 | 河南科技大学 | Preparation method of potassium-sodium niobate ceramic |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101613201B (en) | 2011-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101613201B (en) | Method for synthesizing potassium-sodium niobate leadless piezoelectric ceramic powder by two hydro-thermal steps | |
| CN102311266B (en) | Preparation method of (K05Na05) NbO3 (KNN) lead-free piezoelectric ceramic material | |
| CN100386291C (en) | Lead free piezoelectric ceramics of potassium sodium niobate and preparation thereof | |
| CN101186338B (en) | Hydro-thermal synthesis method for tantalum adulterated potassium sodium niobate leadless piezoelectric ceramic powder | |
| CN101619494A (en) | Method for preparing perovskite structure lead titanate monocrystal nano rod | |
| CN101913853A (en) | Method for preparing bismuth titanate-barium titanate powder by hydrothermal method | |
| CN101891473B (en) | Method for preparing potassium-sodium niobate lead-free piezoelectric ceramics | |
| CN103553605B (en) | KNN-BF leadless piezoelectric ceramic and preparation method thereof | |
| CN101182203A (en) | Barium titanate based piezoelectric ceramic materials as well as preparation method and uses thereof | |
| CN103866386A (en) | Preparation method of novel ternary piezoelectric crystal monophase material | |
| CN101880160A (en) | Method for preparing CaCu3Ti4O12 powder | |
| Li et al. | Low-temperature hydro/solvothermal synthesis of Ta-modified K0. 5Na0. 5NbO3 powders and piezoelectric properties of corresponding ceramics | |
| CN105198417A (en) | Preparation method of zirconic acid sodium bismuthide lithium cerium doped potassium-sodium niobate based ceramic material | |
| CN102923766B (en) | Preparation method of lead-titanate ceramic single-crystal nanosheet | |
| CN112479708A (en) | Lead-free piezoelectric ceramic for medical ultrasonic transducer and preparation method and application thereof | |
| CN101786880B (en) | Sodium potassium niobate-potassium lithium niobate piezoelectric ceramics and preparation method thereof | |
| CN105541327A (en) | Preparation method of potassium sodium niobate-based piezoelectric ceramic | |
| CN101585704B (en) | Leadless piezoelectric ceramics material and method for preparing same | |
| CN105254295B (en) | A kind of preparation method of neodymium-doped titanium acid barium nano-ceramic powder | |
| CN101172857A (en) | Method for producing nano-micrometre double-scale crystal grain composite PZT piezoelectric ceramic | |
| CN110372372A (en) | The preparation method of the bismuth-sodium titanate base lead-free piezoelectric ceramic of low-dielectric loss under high temperature | |
| CN104211395A (en) | Leadless piezoelectric ceramic material applicable to energy collecting device and preparation method thereof | |
| CN101798227A (en) | Solid phase synthetic method of niobate-titanate nano-powder | |
| CN102259909B (en) | Preparation method of lead carbonate combustion catalyst for solid propellant | |
| CN101333005A (en) | Method for low-temperature preparing K0.5Na0.5NbO3 super fines |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |