CN103708837A - Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process - Google Patents
Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process Download PDFInfo
- Publication number
- CN103708837A CN103708837A CN201310262118.7A CN201310262118A CN103708837A CN 103708837 A CN103708837 A CN 103708837A CN 201310262118 A CN201310262118 A CN 201310262118A CN 103708837 A CN103708837 A CN 103708837A
- Authority
- CN
- China
- Prior art keywords
- citric acid
- acid solution
- sol
- nano
- aqueous citric
- 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.)
- Pending
Links
Images
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention belongs to the technical field of electronic ceramic preparation and application, and particularly relates to a method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using a sol-gel method. The technical scheme comprises adopting a water-soluble sol-gel method to finely synthesize Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer precursor powder, and specifically comprises: 1) preparing a citric acid aqueous solution of Zn ions and Ba ions; 2) preparing a citric acid aqueous solution of Nb ions; and 3) synthesizing a Ba(Zn1/3Nb2/3)O3 ceramic nanometer precursor. According to the present invention, the low price oxide and the inorganic nitrate are adopted as the raw materials, use of the expensive metal alkoxide is avoided, and the synthesized powder has significant advantages of low synthesis temperature, uniform ceramic particles, good ceramic particle dispersity, pure phase, easy performing of fine doping modification of various elements, nano-scale powder (particle size of less than 100 nm), high specific surface energy, high activity and the like. In addition, the method has the following characteristics that: the subsequent low temperature sintering can be achieved, and the LTCC application requirements can be met.
Description
Technical field
The invention belongs to electronic ceramic preparation and applied technical field, relate in particular to a kind of meticulous synthetic Ba (Zn of wet chemical technology that utilizes
1/3nb
2/3) O
3media ceramic Nano-powder body method.
Background technology
In recent years, along with the fast development of micro-wave communication cause, the fields such as mobile communication, automobile telephone, telestar, military radar, global positioning system (GPS) and portable phone increase day by day to the demand of the microwave circuit of miniaturization, high performance and microwave device.This just requires to continually develop has the type material of high-performance more.The very high frequency of microwave signal, wavelength is extremely short, and information content is larger, has stronger directivity, penetrance and receptivity, and microwave equipment can realize the confidentiality of communication, is beneficial to the application of communication technical field and military field.The miniaturization, high stability and the cheap approach that realize microwave equipment are the integrated necessary of microwave circuit.And microwave dielectric material is the critical material of manufacturing these devices and meeting well performance requriements.
Have complex perovskite structure ceramic compound A (B '
1/3b "
2/3) O
3(A=Ba, Sr; B '=Mg, Zn, Co, Ni, Mn; B "=Nb and Ta) obtained paying close attention to comparatively widely.This ceramic compound of take can meet the requirement that specific inductivity is large, quality factor q is high and temperature coefficient of resonance frequency is low preferably as basic dielectric material, and the dielectric material can be used as on wave filter, resonator is applied in microwave frequency range.At present both at home and abroad research is more be A (B '
1/3b "
2/3) O
3series compound, but due to Ta
2o
5more expensive, require that purity is higher and system sintering temperature is too high (1500 ℃-1600 ℃), and limited its large-scale promotion application; And Nb
2o
5be a kind of compound of cheap wide material sources, utilize it to replace Ta
2o
5also can make under suitable condition the medium ceramic material of better performances.
Research both at home and abroad shows Ba (Zn
1/3nb
2/3) O
3(BZN) there is cubic perovskite structure, lattice parameter a=0.4094nm under room temperature, temperature coefficient of resonance frequency
τ f =+30 * 10
-6/ ℃,
ε r =41, Q=5400, as can be seen here, BZN is a kind of microwave dielectric ceramic materials that has very much development potentiality.About this architectural study, substantially take solid reaction process as main at present, solid phase synthesis and sintering temperature are higher, are unfavorable for following LTCC application demand.At present about this system Ba (Zn
1/3nb
2/3) O
3microwave-medium ceramics adopts wet chemical technology to carry out the meticulous synthetic report that always there is not yet both at home and abroad.
Summary of the invention
The object of the invention is the LTCC Technology application demand based on following LTCC (Low Temperature Co-fired Ceramic), overcome the shortcoming of traditional solid phase synthesis difficulty; A kind of meticulous synthetic Ba (Zn of sol-gel method that utilizes is provided
1/3nb
2/3) O
3media ceramic Nano-powder body method, adopts the meticulous synthetic Ba (Zn of sol-gel method
1/3nb
2/3) O
3ceramic powder, have that synthesis temperature is low, ceramic particle evenly mutually pure, the powder of (lower than 100nm), good dispersity, thing there is nano particle size and there is high-ratio surface energy, present the significant advantages such as greater activity, can realize follow-up low-temperature sintering, being expected to provides new candidate material for meeting LTCC application demand.
For solving the problems of the technologies described above, technical scheme of the present invention is:
1, utilize the meticulous synthesis of ternary Ba of water-soluble sol gel process (Zn
1/3nb
2/3) O
3media ceramic Nano-powder body method, is characterized in that: comprise the following steps:
(1) aqueous citric acid solution of preparation Zn and Ba ion;
(2) aqueous citric acid solution of preparation Nb;
(3) Ba (Zn
1/3nb
2/3) O
3synthesizing of microwave-medium ceramics nanometer presoma;
(a) Zn being prepared by step (1), (2) mixes with Ba aqueous citric acid solution, Nb aqueous citric acid solution, then adds polyoxyethylene glycol to carry out esterification, and the 4-6 that the molar weight that polyoxyethylene glycol adds is citric acid doubly; Heating
,stir, obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of being prepared by step (a) is placed in drying in oven, shrinks and forms xerogel;
(c) xerogel of step (b) is placed in to 850 ℃ of calcination processing of High Temperature Furnaces Heating Apparatus, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder;
2, the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: the aqueous citric acid solution of described step (1) preparation Zn and Ba ion comprises the following steps:
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, adjusting Ba/Zn/Nb element mole proportioning is 3/1+x/2, wherein x is: 0<x<0.05; First take zinc nitrate and nitrate of baryta, be dissolved in appropriate amount of deionized water, form colourless transparent solution;
(b) take citric acid, the mol ratio of citric acid be zinc nitrate and nitrate of baryta 4-6 doubly, add in above-mentioned solution, impel citric acid and Zn and Ba ion forming complex, make water white transparency Zn and Ba ion aqueous citric acid solution.
3, the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: the aqueous citric acid solution of described step (2) preparation Nb comprises the following steps:
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, takes niobium oxides, is placed in ceramic dielectic reactor, seals after adding hydrofluoric acid, then utilizes baking oven to carry out pyroprocessing 1-3 hour, and accelerate dissolution forms the HF acid solution of water white transparency Nb
;
(b), in the HF acid solution of above-mentioned Nb, adding ammoniacal liquor to adjust pH value is 8-10, impels Nb to complete precipitation with the form of niobium hydroxide;
(c) filter above-mentioned precipitation, repeatedly clean to be placed on for several times in lemon aqueous acid and carry out magnetic agitation, form the white citric acid suspension liquid that is uniformly dispersed, wherein adding citric acid molar weight is metal ion total amount 4-8 times;
(d) above-mentioned white citric acid suspension liquid is placed in to the sealing of ceramic dielectic autoclave, then utilize baking oven to carry out pyroprocessing 3-6 hour, impel and react, impel citric acid and Nb to carry out reacting forming complex dissolving, finally form the aqueous citric acid solution of water white transparency Nb.
4, the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 3
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: described step (a) and (d) in the temperature of baking oven pyroprocessing be 100-150 ℃.
5, the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: described step (3) Ba (Zn
1/3nb
2/3) O
3synthetic and the pottery preparation of microwave-medium ceramics nanometer presoma comprises the following steps:
(a) Zn being prepared by step (1), (2) mixes with Ba ion aqueous citric acid solution, Nb aqueous citric acid solution, then adds polyoxyethylene glycol to carry out esterification, and the molar weight that polyoxyethylene glycol adds is 4-6 times of Citric Acid Dosage total amount; By water-bath 60-90 ℃ of heating 8-20 hour, and constantly stir, guarantee evenly, to obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of step (3) (a) being prepared is placed in drying in oven, shrinks and forms xerogel;
(c) step (3) xerogel (b) is placed in to retort furnace in 850 ℃ of calcinings 1 hour, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder;
The invention has the beneficial effects as follows: the present invention adopts cheap nitrate of baryta and zinc nitrate, niobium oxides, as raw material, substitutes expensive metallorganics alkoxide, with mineral acid, carries out dissolution process; The metering of sol gel process process chemistry is more accurate than controlling, and technique is simple, reproducible; Based on collosol and gel principle, in conjunction with the advantage of hydro-thermal technique, realize the Ba (Zn of very low temperature synthesis of nano yardstick
1/3nb
2/3) O
3ceramic powder.The synthetic ceramic powder particle of this technology is tiny, even, and synthesis temperature is low, synthetic Ba (Zn
1/3nb
2/3) O
3media ceramic thing is stablized single mutually, disturbs accurate ion doping modification easy to implement without dephasign; Synthetic Ba (Zn
1/3nb
2/3) O
3dielectric ceramic powder is nanoscale, has high-specific surface area, high-ratio surface energy, active high, and relatively traditional liquid process easy-sintering is beneficial to energy-conservationly, and is expected to meet LTCC application demand.
Accompanying drawing explanation
Fig. 1 is that sol gel process of the present invention is prepared Ba (Zn
1/3nb
2/3) O
3ceramic nano presoma process flow sheet,
Fig. 2 is XRD typical consequence after 850 ℃ of calcinings of Ba-Zn-Nb gel of the present invention,
Fig. 3 is TEM typical case shape appearance figure after 850 ℃ of calcinings of xerogel of the present invention,
Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail.
Embodiment
embodiment 1
According to Fig. 1 sol gel process, prepare Ba (Zn
1/3nb
2/3) O
3ceramic nano precursor powder process flow sheet, has following steps:
(1) aqueous citric acid solution of preparation Zn, Ba ion
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, adjusting Ba/Zn/Nb element mole proportioning is 3/1+x/2, wherein x is: 0<x<0.05, this x=0.01; First precision balance takes Zn (NO
3)
2.6H
2totally 2.9749 grams of O, Ba (NO
3)
2totally 7.8405 grams, be dissolved in 200ml ionized water, magnetic agitation, forms colourless transparent solution;
(b) take 34.58 grams of citric acids, add in above-mentioned solution and stir, impel citric acid and Zn, Ba ion forming complex, make water white transparency Zn, Ba ion aqueous citric acid solution;
(2) aqueous citric acid solution of preparation Nb
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, takes respectively 5.316 grams of niobium oxides, is placed in ceramic dielectic reactor, seals after adding 50ml hydrofluoric acid, then utilizes baking oven to carry out 1 hour accelerate dissolution of 150 ℃ of hydrothermal treatment consists of high temperature, forms the HF acid solution of water white transparency Nb
;
(b), in the HF acid solution of above-mentioned Nb, adding ammoniacal liquor 100ml to adjust pH value is 10, impels Nb to complete precipitation with the form of niobium hydroxide;
(c) filter above-mentioned precipitation, repeatedly clean to be placed on for several times in lemon aqueous acid and carry out magnetic agitation, form the white citric acid suspension liquid that is uniformly dispersed, wherein adding citric acid molar weight is 46.11 grams;
(d) above-mentioned white citric acid suspension liquid is placed in to the sealing of ceramic dielectic autoclave, then utilize baking oven to carry out 150 ℃ of processing of high temperature and within 3 hours, impel reaction, impel citric acid and Nb to carry out reacting forming complex dissolving, finally form the mixing aqueous citric acid solution of water white transparency Nb;
(3) Ba (Zn
1/3nb
2/3) O
3synthesizing of media ceramic nanometer presoma
(a) Zn being prepared by step (1), (2), Ba aqueous citric acid solution, Nb aqueous citric acid solution mix, and then add polyoxyethylene glycol to carry out esterification, and polyoxyethylene glycol dosage is 100g; By 90 ℃ of heating of water-bath 10 hours, and constantly stir, guarantee evenly, to obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of step (3) (a) being prepared is placed in 150 ℃ of drying in oven, shrinks and forms xerogel;
(c) step (3) xerogel (b) is placed in to retort furnace in 850 ℃ of calcinings 1 hour, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder; See that Fig. 2 is XRD result after 850 ℃ of calcinings of Ba-Zn-Nb xerogel of the present invention.
embodiment 2
According to Fig. 1 sol gel process, prepare Ba (Zn
1/3nb
2/3) O
3ceramic nano precursor powder process flow sheet, has following steps:
(1) aqueous citric acid solution of preparation Zn, Ba ion
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, adjusting Ba/Zn/Nb element mole proportioning is 3/1+x/2, wherein x is: 0<x<0.05, this x=0.04; First precision balance takes Zn (NO
3)
2.6H
2totally 5.9498 grams of O, Ba (NO
3)
2totally 15.681 grams, be dissolved in 200ml ionized water, magnetic agitation, forms colourless transparent solution;
(b) take 38.428 grams of citric acids, add in above-mentioned solution and stir, impel citric acid and Zn, Ba ion forming complex, make water white transparency Zn, Ba ion aqueous citric acid solution;
(2) aqueous citric acid solution of preparation Nb
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, takes respectively 2.987 grams of niobium oxides, is placed in ceramic dielectic reactor, seals after adding 90ml hydrofluoric acid, then utilizes baking oven to carry out 3 hours accelerate dissolution of 100 ℃ of hydrothermal treatment consists of high temperature, forms the HF acid solution of water white transparency Nb
;
(b), in the HF acid solution of above-mentioned Nb, adding ammoniacal liquor 180ml to adjust pH value is 8, impels Nb to complete precipitation with the form of niobium hydroxide;
(c) filter above-mentioned precipitation, repeatedly clean to be placed on for several times in lemon aqueous acid and carry out magnetic agitation, form the white citric acid suspension liquid that is uniformly dispersed, wherein adding citric acid molar weight is 57.642 grams;
(d) above-mentioned white citric acid suspension liquid is placed in to the sealing of ceramic dielectic autoclave, then utilizing baking oven to carry out 100 ℃ of high temperature processes to impel for 6 hours and reacts, impel citric acid and Nb to carry out reacting forming complex dissolving, finally form the aqueous citric acid solution of water white transparency Nb;
(3) Ba (Zn
1/3nb
2/3) O
3synthesizing of media ceramic nanometer presoma
(a) Zn being prepared by step (1), (2), Ba aqueous citric acid solution, Nb aqueous citric acid solution mix, and then add polyoxyethylene glycol to carry out esterification, and polyoxyethylene glycol dosage is 60g; By 60 ℃ of heating of water-bath 15 hours, and constantly stir, guarantee evenly, to obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of step (3) (a) being prepared is placed in 100 ℃ of drying in oven, shrinks and forms xerogel;
(c) step (3) xerogel (b) is placed in to retort furnace in 850 ℃ of calcinings 1 hour, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder; Fig. 2 is XRD result after 850 ℃ of calcinings of Ba-Zn-Nb xerogel of the present invention, and Fig. 3 is TEM shape appearance figure under 850 ℃ of calcining temperatures.
embodiment 3
(1) aqueous citric acid solution of preparation Zn, Ba ion
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, adjusting Ba/Zn/Nb element mole proportioning is 3/1+x/2, wherein x is: 0<x<0.05, this x=0.03; First precision balance takes Zn (NO
3)
2.6H
2totally 8.9247 grams of O, Ba (NO
3)
2totally 23.5215 grams, be dissolved in 200ml ionized water, magnetic agitation, forms colourless transparent solution;
(b) take 96.07 grams of citric acids, add in above-mentioned solution and stir, impel citric acid and Zn ion forming complex, make water white transparency Zn ion aqueous citric acid solution;
(2) aqueous citric acid solution of preparation Nb
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, takes respectively 4.4805 grams of niobium oxides, is placed in ceramic dielectic reactor, seals after adding 80ml hydrofluoric acid, then utilizes baking oven to carry out 2 hours accelerate dissolution of 130 ℃ of hydrothermal treatment consists of high temperature, forms the HF acid solution of water white transparency Nb
;
(b), in the HF acid solution of above-mentioned Nb, adding ammoniacal liquor 190ml to adjust pH value is 9, impels Nb to complete precipitation with the form of niobium hydroxide;
(c) filter above-mentioned precipitation, repeatedly clean to be placed on for several times in lemon aqueous acid and carry out magnetic agitation, form the white citric acid suspension liquid that is uniformly dispersed, wherein adding citric acid molar weight is 115 grams;
(d) above-mentioned white citric acid suspension liquid is placed in to the sealing of ceramic dielectic autoclave, then utilize baking oven to carry out 130 ℃ of processing of high temperature and within 4 hours, impel generation hydro-thermal reaction, impel citric acid and Nb to carry out reacting forming complex dissolving, finally form the mixing aqueous citric acid solution of water white transparency Nb;
(3) Ba (Zn
1/3nb
2/3) O
3synthesizing of media ceramic nanometer presoma
(a) Zn being prepared by step (1), (2), Ba aqueous citric acid solution, Nb aqueous citric acid solution mix, and then add polyoxyethylene glycol to carry out esterification, and polyoxyethylene glycol dosage is 150g; By 80 ℃ of heating of water-bath 12 hours, and constantly stir, guarantee evenly, to obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of step (3) (a) being prepared is placed in 120 ℃ of drying in oven, shrinks and forms xerogel;
(c) step (3) xerogel (b) is placed in to retort furnace in 850 ℃ of calcinings 1 hour, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder; Fig. 2 is XRD result after 850 ℃ of calcinings of Ba-Zn-Nb xerogel of the present invention, and Fig. 3 is TEM shape appearance figure under 850 ℃ of calcining temperatures.
Claims (6)
1. utilize the meticulous synthesis of ternary Ba of water-soluble sol gel process (Zn
1/3nb
2/3) O
3media ceramic Nano-powder body method, is characterized in that: comprise the following steps:
(1) aqueous citric acid solution of preparation Zn and Ba ion;
(2) aqueous citric acid solution of preparation Nb;
(3) Ba (Zn
1/3nb
2/3) O
3synthesizing of microwave-medium ceramics nanometer presoma;
(a) Zn being prepared by step (1), (2) mixes with Ba aqueous citric acid solution, Nb aqueous citric acid solution, then adds polyoxyethylene glycol to carry out esterification, and the 4-6 that the molar weight that polyoxyethylene glycol adds is citric acid doubly; Heating
,stir, obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of being prepared by step (a) is placed in drying in oven, shrinks and forms xerogel;
(c) xerogel of step (b) is placed in to 850 ℃ of calcination processing of High Temperature Furnaces Heating Apparatus, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder.
2. the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: the aqueous citric acid solution of described step (1) preparation Zn and Ba ion comprises the following steps:
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, adjusting Ba/Zn/Nb element mole proportioning is 3/1+x/2, wherein x is: 0<x<0.05; First take zinc nitrate and nitrate of baryta, be dissolved in appropriate amount of deionized water, form colourless transparent solution;
(b) take citric acid, the mol ratio of citric acid be zinc nitrate and nitrate of baryta 4-6 doubly, add in above-mentioned solution, impel citric acid and Zn and Ba ion forming complex, make water white transparency Zn and Ba ion aqueous citric acid solution.
3. the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: the aqueous citric acid solution of described step (2) preparation Nb comprises the following steps:
(a) according to Ba (Zn
1/3nb
2/3) O
3the stoichiometric ratio of pottery thing phase, takes niobium oxides, is placed in ceramic dielectic reactor, seals after adding hydrofluoric acid, then utilizes baking oven to carry out pyroprocessing 1-3 hour, and accelerate dissolution forms the HF acid solution of water white transparency Nb
;
(b), in the HF acid solution of above-mentioned Nb, adding ammoniacal liquor to adjust pH value is 8-10, impels Nb to complete precipitation with the form of niobium hydroxide;
(c) filter above-mentioned precipitation, repeatedly clean to be placed on for several times in lemon aqueous acid and carry out magnetic agitation, form the white citric acid suspension liquid that is uniformly dispersed, wherein adding citric acid molar weight is metal ion total amount 4-8 times;
(d) above-mentioned white citric acid suspension liquid is placed in to the sealing of ceramic dielectic autoclave, then utilize baking oven to carry out pyroprocessing 3-6 hour, impel and react, impel citric acid and Nb to carry out reacting forming complex dissolving, finally form the aqueous citric acid solution of water white transparency Nb.
4. the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 3
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: described step (a) and (d) in the temperature of baking oven pyroprocessing be 100-150 ℃.
5. the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 1
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: described step (3) Ba (Zn
1/3nb
2/3) O
3synthetic and the pottery preparation of microwave-medium ceramics nanometer presoma comprises the following steps:
(a) Zn being prepared by step (1), (2) mixes with Ba ion aqueous citric acid solution, Nb aqueous citric acid solution, then adds polyoxyethylene glycol to carry out esterification, and the molar weight that polyoxyethylene glycol adds is 4-6 times of Citric Acid Dosage total amount; By water-bath 60-90 ℃ of heating 8-20 hour, and constantly stir, guarantee evenly, to obtain Ba-Zn-Nb precursor sol;
(b) the Ba-Zn-Nb precursor solution of step (3) (a) being prepared is placed in drying in oven, shrinks and forms xerogel;
(c) step (3) xerogel (b) is placed in to retort furnace in 850 ℃ of calcinings 1 hour, can obtains evengranular nano level Ba (Zn
1/3nb
2/3) O
3powder.
6. the meticulous synthesis of nano Ba of the sol-gel method (Zn that utilizes according to claim 5
1/3nb
2/3) O
3media ceramic precursor powder method, is characterized in that: the temperature of the baking oven hyperthermia drying in described step (b) is 60-90 ℃, and the calcining temperature in step (c) is 850 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310262118.7A CN103708837A (en) | 2013-06-27 | 2013-06-27 | Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310262118.7A CN103708837A (en) | 2013-06-27 | 2013-06-27 | Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103708837A true CN103708837A (en) | 2014-04-09 |
Family
ID=50402231
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310262118.7A Pending CN103708837A (en) | 2013-06-27 | 2013-06-27 | Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103708837A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609861A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for fine synthesis of Ba(Zn1/3Nb2/3)O3 dielectric ceramic nano-powder through utilizing water-soluble sol-gel method |
| CN104986800A (en) * | 2015-07-14 | 2015-10-21 | 宜春金洋新材料股份有限公司 | Method for preparing niobium hydroxide precipitate by taking fluoroniobate as raw material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775141A (en) * | 2012-08-16 | 2012-11-14 | 济南大学 | Method for finely synthesizing ternary ZnO-Nb2O5-TiO2 microwave dielectric ceramics by wet chemical process |
-
2013
- 2013-06-27 CN CN201310262118.7A patent/CN103708837A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775141A (en) * | 2012-08-16 | 2012-11-14 | 济南大学 | Method for finely synthesizing ternary ZnO-Nb2O5-TiO2 microwave dielectric ceramics by wet chemical process |
Non-Patent Citations (1)
| Title |
|---|
| DUYGU SERT ER AL.: "Production of nanoscale Ba(Zn1/3Nb2/3)O3 microwave dielectric ceramics by polymerized complex method", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104609861A (en) * | 2015-01-25 | 2015-05-13 | 济南唯博新材料有限公司 | Method for fine synthesis of Ba(Zn1/3Nb2/3)O3 dielectric ceramic nano-powder through utilizing water-soluble sol-gel method |
| CN104986800A (en) * | 2015-07-14 | 2015-10-21 | 宜春金洋新材料股份有限公司 | Method for preparing niobium hydroxide precipitate by taking fluoroniobate as raw material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102775141B (en) | Method for finely synthesizing ternary ZnO-Nb2O5-TiO2 microwave dielectric ceramics by wet chemical process | |
| CN103708834A (en) | New method for finely preparing ixiolite structure MgTiNb2O8 microwave dielectric ceramic by using chemical process | |
| AU2006201026B2 (en) | An improved process for the manufacture of strontium doped lanthanum manganite (LSM) ceramic powder suitable for solid oxide fuel cell (SOFC) applications | |
| CN103214235A (en) | Preparation method of microwave dielectric ceramic material | |
| CN103708838A (en) | New method for preparing monoclinic structure ZnZrNb2O8 microwave dielectric ceramic through low temperature sintering | |
| CN101774812B (en) | Method for preparing magnesium tantalate microwave ceramic powder by sol-gel technique | |
| CN104609466A (en) | Method for finely synthesizing ilmenite-structured ZnTiO3 nano powder by using water-soluble sol-gel process | |
| CN100551872C (en) | A kind of method for preparing composite high dielectric constant microwave medium ceramic | |
| CN103708537A (en) | Method for finely synthesizing ilmenite structure ZnTiO3 nanometer powder by using water-soluble sol-gel process | |
| CN108807986A (en) | A kind of preparation method of mineral yellow micro-nano structure crystal | |
| CN105731396B (en) | A kind of carbon containing item chain nano tellurium nickel and its preparation, application | |
| CN104529428A (en) | Manganese cerium doped nickel zinc ferrite nano wave absorbing powder and preparation method thereof | |
| CN101266859A (en) | Method for quick sintering of micro-crystal ferrite magnetic core part | |
| CN105693243A (en) | Preparation method of dielectric constant high-performance microwave dielectric ceramic | |
| CN103864425B (en) | Preparation method of microwave dielectric ceramic material | |
| CN103708837A (en) | Method for finely synthesizing Ba(Zn1/3Nb2/3)O3 dielectric ceramic nanometer powder by using water-soluble sol-gel process | |
| CN101428856A (en) | Process for producing silver tantalate niobate nano-powder | |
| CN104609861A (en) | Method for fine synthesis of Ba(Zn1/3Nb2/3)O3 dielectric ceramic nano-powder through utilizing water-soluble sol-gel method | |
| CN103951424A (en) | Method for low-temperature fine synthesis of MgZrNb2O8 dielectric ceramic nano-powder having wolframite structure by wet chemical technology | |
| CN108558401B (en) | Preparation of Bi by sol-gel method2/3Cu2Ta2Ti2O12Method for producing ceramic powder | |
| CN114044540B (en) | A-site and B-site co-doped perovskite type electromagnetic wave-absorbing material and preparation method thereof | |
| CN107903072B (en) | Method for preparing strontium barium niobate nano powder by two-step coprecipitation method | |
| Mane et al. | Solution Methods for Metal Oxide Nanostructures | |
| CN104119075A (en) | Novel method for lowering sintering temperature of corundum-type Mg4Ta2O9 microwave dielectric ceramic by doping H3BO3 | |
| CN103951426B (en) | Dielectric ceramic K 6nb 10.8o 30the preparation method of powder and sintered body thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C05 | Deemed withdrawal (patent law before 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140409 |