CN105502497A - Preparation method for ZnNb2O6 microwave dielectric ceramic powder - Google Patents
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- CN105502497A CN105502497A CN201510957668.XA CN201510957668A CN105502497A CN 105502497 A CN105502497 A CN 105502497A CN 201510957668 A CN201510957668 A CN 201510957668A CN 105502497 A CN105502497 A CN 105502497A
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- C01G33/00—Compounds of niobium
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/495—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/6261—Milling
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62625—Wet mixtures
- C04B35/6264—Mixing media, e.g. organic solvents
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/62605—Treating the starting powders individually or as mixtures
- C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
- C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
Abstract
The invention discloses a preparation method for ZnNb2O6 microwave dielectric ceramic powder. The preparation method comprises the steps of precursor preparation, a precipitation reaction, a hydrothermal reaction and pumping-filtration drying. Through the preparation method for the ZnNb2O6 microwave dielectric ceramic powder, the resultant temperature of the ZnNb2O6 microwave dielectric ceramic powder can be lowered, ultramicro ZnNb2O6 ceramic powder with excellent microcosmic properties can be obtained, and then the dielectric properties of microwave dielectric ceramic can be improved.
Description
Technical field
The present invention relates to a kind of preparation method, relate to a kind of ZnNb particularly
2o
6the preparation method of microwave dielectric ceramic powder.
Background technology
ZnNb
2o
6be a kind of important microwave dielectric material, it has excellent dielectric properties (ε
r=25, Q × f=83700GHz, τ
f=-56 × 10
-6/ DEG C), thus, be widely used in the various fields such as mobile communication, satellite television broadcasting communication, radar, NAVSTAR of frequency in 300MHz ~ 40GHz series.
ZnNb
2o
6the intrinsic sintering temperature of pottery is more than 1250 DEG C, and the too high meeting of conventional solid sintering temperature causes the volatilization of zinc element, and then is degrading the dielectric properties of pottery, meanwhile, for LTCC technology, and ZnNb
2o
6the higher sintering temperature of pottery can not meet burns with metal A g (961 DEG C), the Cu (1064 DEG C) compared with low melting point, altogether so reduce sintering temperature to seem extremely important.
At present, the method for the most frequently used reduction sintering temperature mainly contains: 1, mix appropriate low melting point oxide or low softening point glass to reduce sintering temperature; 2, wet chemical synthesis.But the mode that traditional solid phase method adds, can worsen the dielectric properties of pottery while reducing sintering temperature.This is because adopting traditional solid phase to add, is by mechanical process hybrid ceramic powder and sintering agent, it is uneven that this makes sintering agent mix, thus increase the consumption of sintering agent.
Moreover the dielectric properties of sintering agent are poor, so too much sintering agent can worsen the dielectric properties of pottery.Particularly, between the principal crystalline phase of (1) material and glassy phase, there is chemical reaction, produce second-phase, cause principal crystalline phase content to reduce, or have impurity phase to generate; (2) material internal exists because there being glassy phase, and its intrinsic loss is increased; (3) generation of lattice imperfection.Hydrothermal method in wet chemical method, can reduce sintering temperature to a certain extent, but to often powder production rate is lower, and it is serious to reunite, and then have impact on the performance of intelligent components and parts.Therefore for the preparation of high-end electronic element, searching can be synthesized the raw powder's production technology that particle diameter is little, narrow particle size distribution, purity are high and be seemed extremely important.
Therefore, for the problems referred to above, be necessary to propose further solution.
Summary of the invention
In view of this, the invention provides a kind of ZnNb
2o
6the preparation method of microwave dielectric ceramic powder, to overcome the deficiencies in the prior art.
To achieve these goals, of the present inventionly a kind of ZnNb is provided
2o
6the preparation method of microwave dielectric ceramic powder, it comprises the steps:
S1. measure than taking Nb by mol
2o
5powder and Zn (SO
4)
27H
2o powder, is mixed with solution respectively, by the solution mixing be mixed with, obtains the mixing solutions of zinc, niobium;
S2. to the mixed solution and dripping ammoniacal liquor in step S1, stir, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping;
S3. by the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration, leave standstill and obtain coagulating sedimentation thing;
S4. in the coagulating sedimentation thing will obtained in step S3, drip ionic liquid, add a small amount of dispersion agent, under sealed high pressure condition, constant temperature 24-72h, is cooled to room temperature simultaneously;
S5., after being left standstill by the mixture finally obtained in step S4, by aftertreatment, ZnNb of the present invention is obtained
2o
6microwave dielectric ceramic powder.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described step S1 specifically comprises:
Amount is than taking Nb by mol
2o
5powder, by the Nb taken
2o
5powder joins in HF solution, and under water bath with thermostatic control condition, magnetic agitation is clarified to solution, for subsequent use;
Amount is than taking Zn (SO by mol
4)
27H
2o powder, the Zn (SO will taken with distilled water
4)
27H
2it is 0.25 ~ 1mol/L that O powder is diluted to concentration, after magnetic agitation 0.5h, for subsequent use;
Be mixed with two kinds of solution are slowly mixed, and by ultrasonic oscillation 20min, the zinc obtained, the mixing solutions of niobium.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described step S2 specifically comprises:
To the ammoniacal liquor of the mixed solution and dripping 0.25mol/L in step S1, and magnetic agitation, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described step S3 specifically comprises:
By the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration 0.5h, leave standstill 4h, obtain coagulating sedimentation thing.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described step S4 specifically comprises:
The coagulating sedimentation thing obtained in step S3 is placed in autoclave, in coagulating sedimentation thing, drips ionic liquid, add a small amount of dispersion agent simultaneously;
The tight autoclave of sealing is placed in constant temperature oven, takes out after constant temperature 24-72h, be cooled to room temperature.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, after dripping ionic liquid, the mixing solutions in autoclave accounts for 80% of autoclave volume.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, the dripping quantity of described ionic liquid is 30% of coagulating sedimentation thing integral molar quantity, described dispersion agent is polyoxyethylene glycol, and its concentration is 0.1mol/L, and the addition of described dispersion agent is 3% of coagulating sedimentation thing integral molar quantity.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described step S5 specifically comprises:
After the mixture finally obtained in step S4 is left standstill 6h, suction filtration, after the powder washing after suction filtration, put into air dry oven, under 80-100 DEG C of condition, dry 12h, dried powder are after grinding, fragmentation, obtain ZnNb of the present invention
2o
6microwave dielectric ceramic powder.
As ZnNb of the present invention
2o
6the improvement of the preparation method of microwave dielectric ceramic powder, described washing comprises: repeatedly washed by the powder after suction filtration and wash with ethanol.
Compared with prior art, the invention has the beneficial effects as follows: ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder can not only reduce ZnNb
2o
6the synthesis temperature of microwave dielectric ceramic powder, and the ultra micro ZnNb that can also obtain micro-property excellence
2o
6ceramic powder, and then the dielectric properties that can improve microwave-medium ceramics.
Particularly, ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder possesses following beneficial effect:
(1) the present invention adopts Liquid preparation methods, Liquid preparation methods be based upon atom, molecule size on carry out, whole reaction process Ar ion mixing is even, reaction potential energy needed for reaction reduces, so target powder can be synthesized at a lower temperature, and diameter of particle is smaller, uniform ingredients, grain growing is perfect.May be used for the preparation of multiple microwave dielectric ceramic powder;
(2) the present invention by adding nontoxic ionic liquid in mixing solutions, and then can improve the production rate of target powder, and the powder dispersity that the presoma after ultrasonic vibration is prepared after hydro-thermal reaction is good, even grain size;
(3) ionic liquid is applied in Liquid preparation methods as catalysts by the present invention, not only can overcome the shortcoming of conventional solid method high temperature sintering, can also prepare that particle diameter is little, thing is mutually pure, uniform particle sizes, micro-nano crystal grain that reunion is few, carry out nano functional device for next step and carry out powder preparation work in early stage.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 ZnNb of the present invention
2o
6the method flow schematic diagram of preparation method one embodiment of microwave dielectric ceramic powder.
Embodiment
Be described in detail to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
As shown in Figure 1, ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder can not only reduce ZnNb
2o
6the synthesis temperature of microwave dielectric ceramic powder, and the ultra micro ZnNb that can also obtain micro-property excellence
2o
6ceramic powder, and then the dielectric properties that can improve microwave-medium ceramics.
The principle of preparation method of the present invention is: by hydro-thermal reaction method, adds the ionic liquid with katalysis in reaction soln, and then promotes the combination of metal ion, reduces chemical reaction potential energy, makes it can synthesize target powder at a lower temperature; Meanwhile, the presoma powder of reaction, by shaking under Ultrasonic Conditions, can be conducive to zinc, niobium ion mixes, effectively can provide the productivity of thing phase, reduces the reunion situation of powder.
ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder comprises: the preparation of S1. presoma; S2, S3 precipitin reaction; S4. hydro-thermal reaction; S5. suction filtration is dry.
Particularly, ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder comprises the steps:
S1. measure than taking Nb by mol
2o
5powder and Zn (SO
4)
27H
2o powder, is mixed with solution respectively, by the solution mixing be mixed with, obtains the mixing solutions of zinc, niobium.
This step is for realizing the preparation of described presoma.Wherein, this step specifically comprises:
S11. measure than taking Nb by mol
2o
5powder, by the Nb taken
2o
5powder joins in HF solution, and under water bath with thermostatic control condition, magnetic agitation is clarified to solution, for subsequent use;
S12. measure than taking Zn (SO by mol
4)
27H
2o powder, the Zn (SO will taken with distilled water
4)
27H
2it is 0.25 ~ 1mol/L that O powder is diluted to concentration, after magnetic agitation 0.5h, for subsequent use;
S13. be mixed with two kinds of solution are slowly mixed, and by ultrasonic oscillation 20min, the zinc obtained, the mixing solutions of niobium.
S2. to the mixed solution and dripping ammoniacal liquor in step S1, stir, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping.
S3. by the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration, leave standstill and obtain coagulating sedimentation thing.
Step S2, S3 are used for realizing described precipitin reaction.Wherein, described step S2 specifically comprises:
To the ammoniacal liquor of the mixed solution and dripping 0.25mol/L in step S1, and magnetic agitation, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping.The judgement of described pH value, measures by pH acidometer.
Described step S3 specifically comprises:
By the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration 0.5h, leave standstill 4h, obtain coagulating sedimentation thing.
S4. in the coagulating sedimentation thing will obtained in step S3, drip ionic liquid, add a small amount of dispersion agent, under sealed high pressure condition, constant temperature 24-72h, is cooled to room temperature simultaneously.
This step is used for realizing described hydro-thermal reaction.Wherein, described step S4 specifically comprises:
S41. the coagulating sedimentation thing obtained in step S3 is placed in autoclave, in coagulating sedimentation thing, drips ionic liquid, add a small amount of dispersion agent simultaneously;
S42. the tight autoclave of sealing is placed in constant temperature oven, takes out after constant temperature 24-72h, be cooled to room temperature.
In above-mentioned steps, the dripping quantity of described ionic liquid is 30% of coagulating sedimentation thing integral molar quantity, and described dispersion agent is polyoxyethylene glycol, and its concentration is 0.1mol/L, and the addition of described dispersion agent is 3% of coagulating sedimentation thing integral molar quantity.In addition, after dripping ionic liquid, the mixing solutions in autoclave accounts for 80% of autoclave volume.
S5., after being left standstill by the mixture finally obtained in step S4, by aftertreatment, ZnNb of the present invention is obtained
2o
6microwave dielectric ceramic powder.
It is dry that this step is used for realizing described suction filtration.Wherein, described step S5 specifically comprises:
After the mixture finally obtained in step S4 is left standstill 6h, suction filtration, after the powder washing after suction filtration, put into air dry oven, under 80-100 DEG C of condition, dry 12h, dried powder are after grinding, fragmentation, obtain ZnNb of the present invention
2o
6microwave dielectric ceramic powder.
In above-mentioned steps, described washing comprises: repeatedly washed by the powder after suction filtration and wash with ethanol.
In sum, ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder can not only reduce ZnNb
2o
6the synthesis temperature of microwave dielectric ceramic powder, and the ultra micro ZnNb that can also obtain micro-property excellence
2o
6ceramic powder, and then the dielectric properties that can improve microwave-medium ceramics.
Particularly, ZnNb of the present invention
2o
6the preparation method of microwave dielectric ceramic powder possesses following beneficial effect:
(1) the present invention adopts Liquid preparation methods, Liquid preparation methods be based upon atom, molecule size on carry out, whole reaction process Ar ion mixing is even, reaction potential energy needed for reaction reduces, so target powder can be synthesized at a lower temperature, and diameter of particle is smaller, uniform ingredients, grain growing is perfect.May be used for the preparation of multiple microwave dielectric ceramic powder;
(2) the present invention by adding nontoxic ionic liquid in mixing solutions, and then can improve the production rate of target powder, and the powder dispersity that the presoma after ultrasonic vibration is prepared after hydro-thermal reaction is good, even grain size;
(3) ionic liquid is applied in Liquid preparation methods as catalysts by the present invention, not only can overcome the shortcoming of conventional solid method high temperature sintering, can also prepare that particle diameter is little, thing is mutually pure, uniform particle sizes, micro-nano crystal grain that reunion is few, carry out nano functional device for next step and carry out powder preparation work in early stage.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (9)
1. a ZnNb
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described preparation method comprises the steps:
S1. measure than taking Nb by mol
2o
5powder and Zn (SO
4)
27H
2o powder, is mixed with solution respectively, by the solution mixing be mixed with, obtains the mixing solutions of zinc, niobium;
S2. to the mixed solution and dripping ammoniacal liquor in step S1, stir, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping;
S3. by the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration, leave standstill and obtain coagulating sedimentation thing;
S4. in the coagulating sedimentation thing will obtained in step S3, drip ionic liquid, add a small amount of dispersion agent, under sealed high pressure condition, constant temperature 24-72h, is cooled to room temperature simultaneously;
S5., after being left standstill by the mixture finally obtained in step S4, by aftertreatment, ZnNb of the present invention is obtained
2o
6microwave dielectric ceramic powder.
2. ZnNb according to claim 1
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described step S1 specifically comprises:
Amount is than taking Nb by mol
2o
5powder, by the Nb taken
2o
5powder joins in HF solution, and under water bath with thermostatic control condition, magnetic agitation is clarified to solution, for subsequent use;
Amount is than taking Zn (SO by mol
4)
27H
2o powder, the Zn (SO will taken with distilled water
4)
27H
2it is 0.25 ~ 1mol/L that O powder is diluted to concentration, after magnetic agitation 0.5h, for subsequent use;
Be mixed with two kinds of solution are slowly mixed, and by ultrasonic oscillation 20min, the zinc obtained, the mixing solutions of niobium.
3. ZnNb according to claim 1
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described step S2 specifically comprises:
To the ammoniacal liquor of the mixed solution and dripping 0.25mol/L in step S1, and magnetic agitation, until adularescent Precipitation, continue to stir, drip, when mixing solutions pH value is 8 ~ 10, stop dripping.
4. ZnNb according to claim 1
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described step S3 specifically comprises:
By the mixing solutions with precipitation that obtains in step S2 under ul-trasonic irradiation, after ultrasonic vibration 0.5h, leave standstill 4h, obtain coagulating sedimentation thing.
5. ZnNb according to claim 1
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described step S4 specifically comprises:
The coagulating sedimentation thing obtained in step S3 is placed in autoclave, in coagulating sedimentation thing, drips ionic liquid, add a small amount of dispersion agent simultaneously;
The tight autoclave of sealing is placed in constant temperature oven, takes out after constant temperature 24-72h, be cooled to room temperature.
6. ZnNb according to claim 5
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, after dripping ionic liquid, the mixing solutions in autoclave accounts for 80% of autoclave volume.
7. ZnNb according to claim 5
2o
6the preparation method of microwave dielectric ceramic powder, it is characterized in that, the dripping quantity of described ionic liquid is 30% of coagulating sedimentation thing integral molar quantity, and described dispersion agent is polyoxyethylene glycol, its concentration is 0.1mol/L, and the addition of described dispersion agent is 3% of coagulating sedimentation thing integral molar quantity.
8. ZnNb according to claim 1
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described step S5 specifically comprises:
After the mixture finally obtained in step S4 is left standstill 6h, suction filtration, after the powder washing after suction filtration, put into air dry oven, under 80-100 DEG C of condition, dry 12h, dried powder are after grinding, fragmentation, obtain ZnNb of the present invention
2o
6microwave dielectric ceramic powder.
9. ZnNb according to claim 8
2o
6the preparation method of microwave dielectric ceramic powder, is characterized in that, described washing comprises: repeatedly washed by the powder after suction filtration and wash with ethanol.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924168A (en) * | 2016-05-09 | 2016-09-07 | 中科院微电子研究所昆山分所 | Preparation method of TiO2-doped ZnNb2O6 ceramic target material |
| CN106198867A (en) * | 2016-07-04 | 2016-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of ZnNb2o6the synthetic method of gas sensitive |
| CN112979312A (en) * | 2021-04-30 | 2021-06-18 | 昆明理工大学 | AB2O6Niobate ceramic and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105924168A (en) * | 2016-05-09 | 2016-09-07 | 中科院微电子研究所昆山分所 | Preparation method of TiO2-doped ZnNb2O6 ceramic target material |
| CN106198867A (en) * | 2016-07-04 | 2016-12-07 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of ZnNb2o6the synthetic method of gas sensitive |
| CN112979312A (en) * | 2021-04-30 | 2021-06-18 | 昆明理工大学 | AB2O6Niobate ceramic and preparation method thereof |
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