CN109231269A - A method of potassium-sodium niobate is prepared using wet chemistry method - Google Patents
A method of potassium-sodium niobate is prepared using wet chemistry method Download PDFInfo
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- CN109231269A CN109231269A CN201811033255.2A CN201811033255A CN109231269A CN 109231269 A CN109231269 A CN 109231269A CN 201811033255 A CN201811033255 A CN 201811033255A CN 109231269 A CN109231269 A CN 109231269A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
- C01G33/006—Compounds containing, besides niobium, two or more other elements, with the exception of oxygen or hydrogen
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Abstract
K is prepared using wet chemistry method the invention discloses a kind of0.5Na0.5NbO3Method, first by 30g Nb2O5It is dissolved in 120ml hydrofluoric acid, heating water bath is added dropwise ammonium hydroxide after cooling and obtains turbid solution, filters, and deionized water, stirring to supernatant liquor ph=7 is added, and lower layer forms precipitating；120g citric acid is weighed again, citric acid solution is made, and above-mentioned precipitating is dissolved in wherein, is formed niobic acid solution, it is spare；Again to raw material K2CO3And Na2CO3100 DEG C of baking processing respectively；The another citric acid 35g that weighs is made citric acid solution, then will treated 7.7991g K2CO3With 5.8310g Na2CO3It is dissolved in wherein, and this mixed solution is dissolved in spare niobic acid solution, obtain new mixed solution；It weighs ethylene glycol with ethylene glycol molar ratio according still further to aforementioned citric acid quality sum total for the ratio of 1:6 to be added in new mixed solution, heating water bath obtains gel, is Na after gel calcining0.5K0.5NbO3White powder is perovskite structure, complies fully with requirement.
Description
Technical field
The ceramic composition that the invention belongs to a kind of characterized by ingredient, in particular to it is a kind of to prepare niobium using wet chemistry method
The method of sour potassium sodium.
Background technique
(K0.5Na0.5)NbO3(being abbreviated as KNN) piezoceramic material belongs to perovskite structure, its piezoelectricity with higher
Constant and high Curie temperature (TC~420 DEG C), it is considered as that traditional Pb (Zr, Ti) O can be substituted3Etc. lead piezoelectric ceramics one
The unleaded perovskite ceramics material of kind.But Na and K have stronger volatility in high-temperature sintering process, therefore solid using tradition
Phase sintering method is difficult to prepare pure and high-densit KNN piezoceramic material, unsound ceramics electric property difference and
It is unstable.The application proposes a kind of method for preparing KNN using wet chemistry method.
Summary of the invention
The purpose of the present invention, be in order to overcome the prior art using conventional solid sintering process be difficult to prepare it is pure and high
Fine and close (K0.5Na0.5)NbO3The situation of piezoceramic material provides and a kind of prepares Curie temperature and piezoelectricity using wet chemistry method
Higher (the K of constant0.5Na0.5)NbO3Method.
The present invention is achieved by following technical solution.
It is a kind of to prepare K using wet chemistry method0.5Na0.5NbO3Method, have following steps:
(1) according to every 30g Nb2O5With the ratio of 120ml hydrofluoric acid, poured into plastic bottle after dissolution；
(2) liquid solution that step (1) is prepared is put into water-bath, heating water bath 20 hours；
(3) liquid solution after step (2) heating water bath is cooling in room temperature, after cooling, ammonium hydroxide is added dropwise, to no ammonia
Gas generates, it is ensured that ammonium hydroxide reacts completely with hydrofluoric acid, and the solution is turbid solution at this time；
(4) troubled liquor of step (3) is filtered, deionized water is added after suction filtration, stirred with glass bar to upper layer
Clear liquid ph=7, lower layer form precipitating；
(5) 120g citric acid is weighed, deionized water is completely dissolved in and forms citric acid solution；It is again that the precipitating of step (4) is molten
In the citric acid solution, stirring to form niobic acid solution to being completely dissolved；It is sealed, is kept spare with preservative film；
(6) to raw material K2CO3And Na2CO3100 DEG C of baking processing are carried out respectively；
(7) citric acid 35g is separately weighed, is completely dissolved in deionized water and forms citric acid solution；
(8) 7.7991g K is weighed2CO3With 5.8310g Na2CO3It is dissolved into the citric acid solution of step (7), stirring is extremely
It is completely dissolved；
(9) mixed solution of step (8) is dissolved in niobic acid solution in step (5), stirs, makes it completely dissolved, mixed
Close solution；
(10) it is calculated according to the citric acid quality sum total of step (5) and step (7) with ethylene glycol molar ratio for the ratio of 1:6
It weighs ethylene glycol to be added in the mixed solution of step (9), then heating water bath 8h, obtains gel；
(11) gel obtained by step (10) is calcined into 2h, forms white powder, as Na0.5K0.5NbO3Powder.
The water bath heating temperature of the step (2) and (10) is 85 DEG C.
The calcination temperature of the step (11) is 650 DEG C.
The present invention successfully provides a kind of method of wet-chemical for preparing potassium-sodium niobate powder, using this method preparation
Potassium-sodium niobate powder is tested using Rigaku company DMAX/RC type X-ray diffractometer, which is perovskite structure, is reached
Goal of the invention complies fully with requirement.
Specific embodiment
Below by specific embodiment, the invention will be further described, and raw materials used in example is the commercially available pure examination of analysis
Agent, specific embodiment are as follows.
(1) 30g Nb is weighed2O5, 120ml hydrofluoric acid dissolution, which is measured, with plastic cylinder pours into plastic bottle；
(2) by step (1) prepare solution be put into water-bath, 85 DEG C heating water bath 20 hours；
(3) solution after step (2) heating water bath is cooling in room temperature, after cooling, ammonium hydroxide is added dropwise with rubber head dropper, wait not have
There is ammonia gas generation, it is ensured that ammonium hydroxide reacts completely with hydrofluoric acid, and the solution is turbid solution at this time；
(4) troubled liquor of step (3) is filtered, deionized water is added after suction filtration, stirred with glass bar to upper layer
Clear liquid ph=7, lower layer form precipitating；
(5) 120g citric acid is weighed, deionized water is dissolved in and forms citric acid solution, then step (4) precipitating is dissolved in lemon
In acid solution, stirring to form niobic acid solution to being completely dissolved.It is sealed, is kept spare with preservative film；
(6) to raw material K2CO3And Na2CO3100 DEG C of baking processing are carried out respectively；
(7) citric acid 35g is separately weighed, is dissolved in deionized water and forms citric acid solution；
(8) 7.7991g K is weighed2CO3With 5.8310g Na2CO3It is dissolved into the citric acid solution in step (7), stirs
To being completely dissolved；
(9) mixed solution of step (8) is dissolved in niobic acid solution in step (5), stirs, makes it completely dissolved, mixed
Close solution；
(10) it is calculated according to step (5) step and the citric acid quality of rapid (7) sum total with ethylene glycol molar ratio for the ratio of 1:6
Weigh ethylene glycol 270ml (step (5) step and the citric acid quality of rapid (7) sum total are 155g, and the ethylene glycol after calculating is 300g,
Being scaled liquid volume is 270ml) it is added in the mixed solution in step (9), 85 DEG C of heating water bath 8h obtain gel；
(11) gained gel in step (10) is formed into white powder in 650 DEG C of calcining 2h, K is made0.5Na0.5NbO3Powder
End.
The present invention is not limited to the above embodiment, and the variation of some details is possible, but therefore this does not violate this hair
Bright scope and spirit.
Claims (3)
1. a kind of prepare K using wet chemistry method0.5Na0.5NbO3Method, have following steps:
(1) according to every 30g Nb2O5With the ratio of 120ml hydrofluoric acid, poured into plastic bottle after dissolution；
(2) liquid solution that step (1) is prepared is put into water-bath, heating water bath 20 hours；
(3) liquid solution after step (2) heating water bath is cooling in room temperature, after cooling, ammonium hydroxide is added dropwise, to no ammonia gas
It generates, it is ensured that ammonium hydroxide reacts completely with hydrofluoric acid, and the solution is turbid solution at this time；
(4) troubled liquor of step (3) is filtered, deionized water is added after suction filtration, stirred with glass bar to supernatant liquor
Ph=7, lower layer form precipitating；
(5) 120g citric acid is weighed, deionized water is dissolved in and forms citric acid solution；The precipitating of step (4) is dissolved in citric acid again
In solution, stirring to form niobic acid solution to being completely dissolved；It is sealed, is kept spare with preservative film；
(6) to raw material K2CO3And Na2CO3100 DEG C of baking processing are carried out respectively；
(7) citric acid 35g is separately weighed, is dissolved in deionized water and forms citric acid solution；
(8) 7.7991g K is weighed2CO3With 5.8310g Na2CO3It is dissolved into the citric acid solution of step (7), stirs to complete
Dissolution；
(9) mixed solution of step (8) is dissolved in niobic acid solution in step (5), stirs, makes it completely dissolved, obtain mixing molten
Liquid；
(10) it is weighed according to step (5) and the citric acid quality sum total of step (7) with ethylene glycol molar ratio for the ratio calculating of 1:6
Ethylene glycol is added in the mixed solution of step (9), then heating water bath 8h, obtains gel；
(11) gel obtained by step (10) is calcined into 2h, forms white powder, as Na0.5K0.5NbO3Powder.
2. a kind of utilization wet chemistry method according to claim 1 prepares Na0.5K0.5NbO3Method, which is characterized in that it is described
The water bath heating temperature of step (2) and (10) is 85 DEG C.
3. a kind of utilization wet chemistry method according to claim 1 prepares Na0.5K0.5NbO3Method, which is characterized in that it is described
The calcination temperature of step (11) is 650 DEG C.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249307A (en) * | 2011-05-06 | 2011-11-23 | 天津大学 | Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film |
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2018
- 2018-09-05 CN CN201811033255.2A patent/CN109231269A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249307A (en) * | 2011-05-06 | 2011-11-23 | 天津大学 | Preparation method of Bi1.5MgNb1.5O7 (BMN) dielectric film |
Non-Patent Citations (1)
| Title |
|---|
| 李菊梅等: ""聚合物前驱体法制备铌酸钾钠纳米粉体"", 《陶瓷学报》 * |
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Application publication date: 20190118 |