CN102030531A - Method for preparing potassium sodium niobate nano powder - Google Patents
Method for preparing potassium sodium niobate nano powder Download PDFInfo
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- CN102030531A CN102030531A CN 201010619225 CN201010619225A CN102030531A CN 102030531 A CN102030531 A CN 102030531A CN 201010619225 CN201010619225 CN 201010619225 CN 201010619225 A CN201010619225 A CN 201010619225A CN 102030531 A CN102030531 A CN 102030531A
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- niobium
- sodium niobate
- oxalic acid
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- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000011858 nanopowder Substances 0.000 title claims abstract description 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 86
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000000843 powder Substances 0.000 claims abstract description 26
- WPCMRGJTLPITMF-UHFFFAOYSA-I niobium(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Nb+5] WPCMRGJTLPITMF-UHFFFAOYSA-I 0.000 claims abstract description 18
- 239000013067 intermediate product Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 4
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 27
- XNHGKSMNCCTMFO-UHFFFAOYSA-D niobium(5+);oxalate Chemical compound [Nb+5].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XNHGKSMNCCTMFO-UHFFFAOYSA-D 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 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 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052758 niobium Inorganic materials 0.000 abstract description 8
- 239000010955 niobium Substances 0.000 abstract description 8
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000008139 complexing agent Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract 2
- UYLYBEXRJGPQSH-UHFFFAOYSA-N sodium;oxido(dioxo)niobium Chemical compound [Na+].[O-][Nb](=O)=O UYLYBEXRJGPQSH-UHFFFAOYSA-N 0.000 abstract 2
- 238000003756 stirring Methods 0.000 abstract 2
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 15
- 239000000126 substance Substances 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- PNCDAXYMWHXGON-UHFFFAOYSA-N ethanol;niobium Chemical compound [Nb].CCO.CCO.CCO.CCO.CCO PNCDAXYMWHXGON-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 3
- 235000015320 potassium carbonate Nutrition 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical compound [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000484 niobium oxide Inorganic materials 0.000 description 2
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- -1 K wherein Chemical class 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- VVNXEADCOVSAER-UHFFFAOYSA-N lithium sodium Chemical compound [Li].[Na] VVNXEADCOVSAER-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing potassium sodium niobate nano powder, which is characterized in that niobium hydroxide with low cost is used as a niobium source and oxalate is used as a complexing agent. The method comprises the following steps of: (1) dissolving a certain quantity of oxalate into distilled water, then adding niobium hydroxide powder into an oxalate solution, and stirring till the niobium hydroxide powder is sufficiently dissolved to obtain a niobium-containing oxalate solution A, wherein the molar ratio of the niobium hydroxide to the niobium is 1:4 to 1:14; (2) dissolving the carbonate, the oxide or the hydroxide of Na and K into the solution A according to the composition proportion of Na0.5K0.5NbO3, adjusting the pH value to be 1-5 with ammonia, then adding ethylene glycol, and reacting by stirring to obtain a faint yellow solution B, wherein the molar ratio of the ethylene glycol to the oxalate is 1:1 to 5:1; (3) placing the solution B into a drying oven after reacting till being viscous, drying at 90-130 DEG C to obtain a solid C; (4) precalcining the solid C at the temperature of 300-400 DEG C to obtain an intermediate product D; and (5) calcining the intermediate product D at the temperature of 500-650 DEG C for 2-5h to obtain sodium niobate powder. The prepared sodium niobate powder has the advantages of high purity, uniform components, nano-level of powder grain size and large sintering activity.
Description
Technical field
The present invention relates to a kind ofly prepare the method for potassium-sodium niobate nano powder, belong to the preparation field of nano-powder in the function ceramics with chemical method.
Background technology
At present, Pb-based lanthanumdoped zirconate titanates (PZT) base ceramic material is still main commercial piezoelectric, but its leaded～65wt-% has than high toxicity, and is bigger to environment and human health risk.
Potassium-sodium niobate in the leadless piezoelectric material material (KNN) base pottery, piezoelectric property good (YasuyoshiSaito, et al.Nature, 2004,432:84-87), be expected to part and substitute the lead base piezoelectric.But alkali metals such as K wherein, Na volatilize easily, and the powder granule degree of conventional solid-state method preparation is bigger, and sintering activity is poor, and high sintering temperature has been aggravated the volatilization of elements such as K, Na, causes pottery to be difficult to densified sintering product.
Chemical method is having many advantages aspect the preparation nano-powder: chemical composition ratio easy to control; Can reach the uniform mixing of molecular level; Sintering temperature is low and can effectively control diameter of particle etc. by regulating sintering temperature.The key that chemical method prepares KNN based ceramic powder body is choosing of niobium source.The ethanol niobium often is selected as the niobium source of chemical method because of its good solubility in organism.(Anirban?Chowdhury，et?al.JNanopart?Res，2010：209-215)。But the ethanol niobium costs an arm and a leg, and very easily hydrolysis, and operating environment is required height, is unfavorable for large-scale production.S.A.O ' the Callaghan of Cambridge University etc. has prepared Na with the ammonium niobium oxalate for the niobium source
0.5K
0.5NbO
3Powder (S.A.O ' Callaghan and K.M.Knowles.MaterialsScience and Technology, 2009,25 (11): 1302-1306).Though ammonium niobium oxalate is low than ethanol niobium price, but still is difficult to obtain, and the diameter of particle that makes is bigger, median size reaches 200nm.The superfine people of the king of Beijing University of Technology is the niobium source with the niobium oxides, and citric acid is that complexing agent has prepared the little lithium sodium kalium niobate powder of grain size (king is superfine.The chemistry journal.2009,67 (3): 203-207), though cost is lower, preparation process is cumbersome, need make the reaction of niobium oxides and potassium hydroxide obtain water-soluble potassium niobate earlier.Therefore how prepare subject matter that potassium-sodium niobate nano-powder will solve and be with the cheap raw material that is easy to get, simply technology obtains the little and uniform powder of particle diameter.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing potassium-sodium niobate nano-powder.By choosing suitable starting material, significantly reduce cost, simplify production technique.This method also is applicable to other niobate materials of preparation.
The method for preparing potassium-sodium niobate nano-powder comprises following sequential steps:
Step 1: contain the preparation of niobium oxalate solution.A certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added in the oxalic acid solution, 70～95 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully; Wherein, niobium hydroxide and oxalic acid mol ratio are 1: 4～1: 14 (especially 1: 8-1: 10);
Step 2: carbonate, oxide compound or the oxyhydroxide of sodium, potassium are pressed Na
0.5K
0.5NbO
3The chemical formula proportioning be dissolved in step 1 preparation contain niobium oxalate solution A, transfer pH value to 1～5 with ammoniacal liquor; Add ethylene glycol then in solution A, ethylene glycol is 1: 1～5: 1 (especially 2: 1～3: 1) by the mol ratio with oxalic acid, make its under 70～95 ℃ of agitation conditions, react yellow solution B;
Step 3: treat that solution B is reacted to thickness and put into loft drier, 90～130 ℃ of dry solid C;
Step 4: pre-burning: solid C processing under 300～400 ℃ was got intermediate product D in 2 hours;
Step 5: calcining: intermediate product D calcining under 500～650 ℃ was got the potassium-sodium niobate powder in 2～5 hours.
Characteristics of the present invention be by adopt niobium hydroxide cheap and easy to get to do the niobium source, oxalic acid is made complexing agent, has significantly reduced cost, has simplified production technique.Utilize method provided by the invention can synthesize high-purity, the uniform potassium-sodium niobate powder of composition, the granule-morphology of prepared powder is similar to cube, particle median size 60-80nm, sintering activity is big, and sintering obtains fine and close leadless piezoelectric ceramics at a lower temperature.
Description of drawings
Fig. 1 is embodiment 1 a potassium-sodium niobate nano-powder X ray diffracting spectrum.
Fig. 2 is embodiment 1 a potassium-sodium niobate nano-powder transmission electron microscope photo.
Embodiment
Below by the elaboration of specific embodiment, further specify substantive distinguishing features of the present invention and obvious improvement, but the present invention only is confined to embodiment by no means.
Embodiment 1
In the present embodiment, potassium-sodium niobate nano-powder adopts the sol-gel method preparation, and concrete processing step is as follows:
A) contain the preparation of niobium oxalate solution.A certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added oxalic acid solution, the mol ratio of niobium hydroxide and oxalic acid is 1: 8, and 80 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully.
B) yellow soda ash and salt of wormwood are pressed Na
0.5K
0.5NbO
3The chemical formula proportioning be dissolved in solution A, transfer pH value to 2.5 back to add ethylene glycol with ammoniacal liquor, making the mol ratio of ethylene glycol and oxalic acid is 2: 1, make its under 80 ℃ of agitation conditions, react yellow solution B;
C) treating that solution B is reacted to thickness puts into loft drier, 95 ℃ of dry solid C;
D) pre-burning: solid C processing under 350 ℃ was got intermediate product D in 2 hours;
E) calcining: intermediate product D calcining under 500 ℃ was got the potassium-sodium niobate powder in 2 hours.
X-ray diffraction (XRD) analysis revealed, the potassium-sodium niobate powder of method for preparing is pure perovskite structure, crystalline quality good (as Fig. 1); Shown in Fig. 2 transmission electron microscope photo, the potassium-sodium niobate nano-powder granule-morphology that makes is similar to cube, and median size is about 70nm.
Embodiment 2
In the present embodiment, potassium-sodium niobate nano-powder adopts the sol-gel method preparation, and concrete processing step is as follows:
A) contain the preparation of niobium oxalate solution.A certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added oxalic acid solution, the mol ratio of niobium hydroxide and oxalic acid is 1: 8, and 90 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully.
B) yellow soda ash, salt of wormwood are pressed Na
0.5K
0.5NbO
3The chemical formula proportioning be dissolved in solution A, transfer pH value to 4 back to add ethylene glycol with ammoniacal liquor, the mol ratio of ethylene glycol and oxalic acid is 2: 1, make its under 90 ℃ of agitation conditions, react yellow solution B;
C) treating that solution B is reacted to thickness puts into loft drier, 115 ℃ of dry white solid C;
D) pre-burning: xerogel C processing under 400 ℃ was got intermediate product D in 2 hours;
E) calcining: intermediate product D calcining under 600 ℃ was got the potassium-sodium niobate powder in 2 hours.
All the other are with embodiment 1
Embodiment 3
In this example, potassium-sodium niobate nano-powder adopts novel sol-gel method preparation, and concrete processing step is as follows:
A) contain the preparation of niobium oxalate solution.A certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added oxalic acid solution, the mol ratio of niobium hydroxide and oxalic acid is 1: 10, and 80 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully.
B) yellow soda ash, salt of wormwood are pressed Na
0.5K
0.5NbO
3The chemical formula proportioning be dissolved in solution A, transfer pH value to 2.5 back to add ethylene glycol with ammoniacal liquor, the mol ratio of ethylene glycol and oxalic acid is 3: 1, make its under 80 ℃ of agitation conditions, react yellow solution B;
C) treating that solution B is reacted to thickness puts into loft drier, 115 ℃ of dryings 24 hours white solid C;
D) pre-burning: xerogel C processing under 350 ℃ was got intermediate product D in 2 hours;
E) calcining: intermediate product D calcining under 500 ℃ was got the potassium-sodium niobate powder in 2 hours.
Embodiment 4
In this example, potassium-sodium niobate nano-powder adopts novel sol-gel method preparation, and concrete processing step is as follows:
A) contain the preparation of niobium oxalate solution.A certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added in the oxalic acid solution, the mol ratio of niobium hydroxide and oxalic acid is 1: 8, and 80 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully.
B) sodium oxide, potassium oxide are pressed Na
0.5K
0.5NbO
3Composition proportion be dissolved in solution A, transfer pH value to 3 back to add ethylene glycol with ammoniacal liquor, making the mol ratio of ethylene glycol and oxalic acid is 2: 1, make its under 80 ℃ of agitation conditions, react yellow solution B;
C) treating that sol B is reacted to thickness puts into loft drier, 115 ℃ of dry white xerogel C;
D) pre-burning: xerogel C processing under 350 ℃ was got intermediate product D in 2 hours;
E) calcining: intermediate product D calcining under 600 ℃ was got the potassium-sodium niobate powder in 4 hours.Prepared morphology microstructure such as embodiment 1, median size is 80nm.
Claims (4)
1. method for preparing potassium-sodium niobate nano-powder is characterized in that may further comprise the steps:
1. a certain amount of oxalic acid is dissolved in distilled water, then the niobium hydroxide powder is added in the oxalic acid solution, 70～95 ℃ are stirred to and dissolve to such an extent that contain niobium oxalate solution A fully; Wherein, niobium hydroxide and oxalic acid mol ratio are 1: 4～1: 14;
2. carbonate, oxide compound or the oxyhydroxide of sodium, potassium are pressed Na
0.5K
0.5NbO
3Composition proportion be dissolved in solution A, transfer pH value to 1～5 with ammoniacal liquor; In solution A, add ethylene glycol, ethylene glycol by with oxalic acid be 1: 1～5: 1 in molar ratio, and under 70～95 ℃ of agitation conditions, react yellow solution B;
3. treat that solution B is reacted to thickness and put into loft drier, 90～130 ℃ of dry solid C;
4. pre-burning: 3. step is made solid C 300～400 ℃ of following pre-burnings, obtain intermediate product D;
5. calcining: intermediate product D is calcined acquisition potassium-sodium niobate powder down at 500～650 ℃.
2. by the described method of claim 1, it is characterized in that:
A) mol ratio of 1. described niobium hydroxide of step and oxalic acid is 1: 8-1: 10;
B) mol ratio of 2. described ethylene glycol of step and oxalic acid is 2: 1-3: 1;
C) the 4. described pre-burning time of step is 2 hours;
D) the 5. described calcination time of step is 2-5 hour.
3. by claim 1 or 2 described methods, it is characterized in that the granule-morphology of the potassium-sodium niobate powder for preparing is approximate cube.
4. by the described method of claim 3, it is characterized in that the potassium-sodium niobate particle median size for preparing is 60-80nm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583538A (en) * | 2012-02-28 | 2012-07-18 | 齐齐哈尔大学 | Sol-gel method for preparation of nanometer potassium sodium niobate rod |
| CN104085922A (en) * | 2014-07-14 | 2014-10-08 | 湖北大学 | Preparation method of high-purity cubic phase sodium niobate nano powder |
| WO2023013288A1 (en) * | 2021-08-04 | 2023-02-09 | 三井金属鉱業株式会社 | Niobate-dispersed aqueous solution, and method for producing same |
| CN116102065A (en) * | 2023-02-20 | 2023-05-12 | 河北东同光电科技有限公司 | Preparation method of high-purity niobium pentoxide superfine powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538067A (en) * | 2009-04-27 | 2009-09-23 | 桂林工学院 | Method for chemically synthesizing potassium sodium niobate nano-powder |
| CN101550511A (en) * | 2009-05-21 | 2009-10-07 | 桂林理工大学 | Potassium sodium niobate-silver particulate composite with ultra-high dielectric coefficient and preparation method thereof |
| CN101921112A (en) * | 2010-07-06 | 2010-12-22 | 齐齐哈尔大学 | Sol-gel method for preparing potassium-sodium niobate nano-powder |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101538067A (en) * | 2009-04-27 | 2009-09-23 | 桂林工学院 | Method for chemically synthesizing potassium sodium niobate nano-powder |
| CN101550511A (en) * | 2009-05-21 | 2009-10-07 | 桂林理工大学 | Potassium sodium niobate-silver particulate composite with ultra-high dielectric coefficient and preparation method thereof |
| CN101921112A (en) * | 2010-07-06 | 2010-12-22 | 齐齐哈尔大学 | Sol-gel method for preparing potassium-sodium niobate nano-powder |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583538A (en) * | 2012-02-28 | 2012-07-18 | 齐齐哈尔大学 | Sol-gel method for preparation of nanometer potassium sodium niobate rod |
| CN102583538B (en) * | 2012-02-28 | 2016-07-20 | 齐齐哈尔大学 | A kind of sol-gel process preparing potassium-sodium niobate nanometer rods |
| CN104085922A (en) * | 2014-07-14 | 2014-10-08 | 湖北大学 | Preparation method of high-purity cubic phase sodium niobate nano powder |
| CN104085922B (en) * | 2014-07-14 | 2015-12-02 | 湖北大学 | A kind of preparation method of high-purity Emission in Cubic sodium niobate nanometer powder |
| WO2023013288A1 (en) * | 2021-08-04 | 2023-02-09 | 三井金属鉱業株式会社 | Niobate-dispersed aqueous solution, and method for producing same |
| CN116102065A (en) * | 2023-02-20 | 2023-05-12 | 河北东同光电科技有限公司 | Preparation method of high-purity niobium pentoxide superfine powder |
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