CN103880410A - Method of synthesizing ZnO-Cr2O3-Fe2O3-series humidity-sensitive ceramic sintered powder by molten-salt growth method - Google Patents

Method of synthesizing ZnO-Cr2O3-Fe2O3-series humidity-sensitive ceramic sintered powder by molten-salt growth method Download PDF

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CN103880410A
CN103880410A CN201410050251.0A CN201410050251A CN103880410A CN 103880410 A CN103880410 A CN 103880410A CN 201410050251 A CN201410050251 A CN 201410050251A CN 103880410 A CN103880410 A CN 103880410A
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CN103880410B (en
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王旭
佟志芳
廖春发
焦芸芬
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Jiangxi University of Science and Technology
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Abstract

The invention relates to a method of synthesizing ZnO-Cr2O3-Fe2O3-series humidity-sensitive ceramic sintered powder by a molten-salt growth method. The method comprises the following steps: (1) preparing materials; (2) pre-synthesizing (main parameters: a temperature of 700 DEG C-850 DEG C and synthesis time of 2hours-4hours); (3) final synthesizing (main parameters: a temperature of 900 DEG C-1000 DEG C and synthesis time of 1 hour-2hours; and (4) product separating and collecting. The method disclosed by the invention is low in cost for preparing materials, short in process flow, simple in equipment, free of emission of solids, liquid and gases, free of secondary pollution and capable of directly synthesizing the ZnO-Cr2O3-Fe2O3-series humidity-sensitive ceramic sintered powder by ZnO, Cr2O3 and Fe2O3 oxide powder with lower cost.

Description

Molten-salt growth method is synthesized ZnO-Cr 2o 3-Fe 2o 3it is humiceram agglomerated powder body method
Technical field
The present invention relates to molten-salt growth method synthesizing ceramic body technique, specifically the synthetic ZnO-Cr of a kind of molten-salt growth method 2o 3-Fe 2o 3it is humiceram agglomerated powder body method.
Background technology
ZnO-Cr 2o 3-Fe 2o 3based semiconductor composite oxides are current more common spinel type humicerams, should be very extensive as humidity sensor, and as fields such as household electrical appliances, automobile, medical treatment.And increasingly extensive application has proposed various requirement to such material, as stability, consistence, interchangeability is good, precision is high; Use wet district wide, sensitivity is suitable etc.For meeting these requirements, require to propose more effective synthetic method and preparation method.At present, be similar to ZnO-Cr 2o 3-Fe 2o 3the production process of composite oxides class modern functions Modern Ceramic Material and products thereof of system generally comprises the unit operations such as raw material processing and processing, batching and abrasive material batch mixing, moulding, sintering, product performance detection.Normally the powder raw materials such as the many oxide through processing are prepared burden by certain formula, therefore, the quality of the powder raw material needing in scientific research and plant produced composite oxides is most important.Current, the powder fineness that adopts mechanical processing method (as ball milling, vibration mill and comminution by gas stream etc.) to prepare in industrial production is limited.And superfine-material often adopts chemical process preparation, can make that material particular diameter is little, even, good fluidity, active large, formability and coking property better.Open up one have that the product purity that synthesis temperature is low, the reaction times is short, easy and simple to handle, synthetic is high, the feature such as the crystal formation of powder granule and pattern can be controlled, the preparation new way that meets the requirement of modern times " green " metallurgical technology has practical significance.
Fused salt synthesis method is a kind of inorganic materials synthetic method that RECENT DEVELOPMENTS is got up, and with other synthetic method comparison, operating process is simple, does not need other specific equipment.Main process is that oxide crystal is at high temperature dissolved in the melt of low melting point, then by slow cooling or other method, forms supersaturated solution, thus oxide crystal by being diffused in rearrangement in fused salt, forming core is separated out new oxide crystal mutually.First synthesized BaFe by molten-salt growth method from Arendt in 1973 12o 19and SrFe 12o 19since, the method has obtained research widely aspect synthesizing ceramic powder.In recent years, along with deepening continuously of research, the advantage of fused salt synthesis method shows gradually, and range of application is also more and more extensive, has prepared many oxide powder, as: ZnTiO 3, CaBi 2nb 2o 9, SrBi 2ta 2o 9deng.
Summary of the invention
The present invention seeks to for existing making ZnO-Cr 2o 3-Fe 2o 3be the weak point of humiceram precursor powder (sintering powder) technique, provide a kind of by ZnO, Cr 2o 3, Fe 2o 3the direct molten-salt growth method of oxide compound is synthesized ZnO-Cr 2o 3-Fe 2o 3it is humiceram agglomerated powder body method.
Technical solution of the present invention: a kind of molten-salt growth method is synthesized ZnO-Cr 2o 3-Fe 2o 3be humiceram agglomerated powder body method, comprise the following steps:
(1) proportioning starting material:
KCl, NaCl, the CaCl of crystal water will do not contained 2villaumite is the medium of building-up reactions, granularity 200-300 object ZnO, Cr 2o 3, Fe 2o 3oxide powder is primitive reaction material;
Ratio requirement:
Pre-synthesis system: ZnO, Cr 2o 3it is 20～40% that mixture accounts for pre-synthesis reaction system material molar content, wherein ZnO:Cr 2o 3mol ratio=1:1; All the other are KCl, NaCl, CaCl 2any two kinds of mixing salts in salt, blending ratio is mol ratio 1:1;
Whole synthetic system: Fe 2o 3account for ZnO, Cr 2o 3, Fe 2o 3the molar content of material total amount is 2～6% to add pre-synthesis system;
(2) pre-synthesis:
Abundant dewatered raw material, with ZnO, the Cr of above-mentioned content 2o 3kCl, the NaCl of mixed oxide and mol ratio 1:1, CaCl 2in salt, any two kinds of mixing salts fully mix, and pack reactor into, require to react 2-4h at 700～850 DEG C of temperature;
(3) synthetic eventually:
Add the Fe of above-mentioned content to the system of pre-synthesis 2o 3, at 900～1000 DEG C of reaction 1-2h of temperature;
(4) collection of product:
With after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.
Containing KCl, NaCl, the CaCl of crystal water 2it is the 48h that dewaters at 300 DEG C of temperature in air that villaumite removes crystal water condition; Granularity 200-300 object ZnO, Cr 2o 3, Fe 2o 3oxide powder is dried 24h in air at 150 DEG C of temperature.
Major control condition and foundation:
1, reaction synthesis temperature will make the substance system of set proportioning fully melt and reach suitable activity, the volatilization of fused salt
Amount is 3-5%, and OK range is 700～1000 DEG C.
2, reaction generated time is wanted fully, and OK range is 1～4h.
Raw materials cost of the present invention and existing technique are lower by approximately 30%, and it is nearly 50% that technical process is shortened, and equipment is simple, can be with lower cost directly by ZnO, Cr 2o 3, Fe 2o 3oxide powder making ZnO-Cr 2o 3-Fe 2o 3be humiceram precursor powder, product granularity is little and even, and economical efficiency significantly improves.
Embodiment
Embodiment 1: be 200 object ZnO, Cr by granularity after KCl, NaCl after 300 DEG C of dehydration 48h in air and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=40:40:10:10 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 700 DEG C, constant temperature pre-synthesis reaction 2h; After 150 DEG C of dry 24h, granularity is 200 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=49:49:2 weighs, by the Fe weighing 2o 3powder add be warming up to 900 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 1h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 2um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
Embodiment 2: be 300 object ZnO, Cr by granularity after KCl, NaCl after 300 DEG C of dehydration 48h in air and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=30:30:20:20 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 850 DEG C, constant temperature pre-synthesis reaction 4h; After 150 DEG C of dry 24h, granularity is 300 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=47:47:6 weighs, by the Fe weighing 2o 3powder add be warming up to 1000 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 2h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 5um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
Embodiment 3: by the CaCl after 300 DEG C of dehydration 48h in air 2, granularity is 200 object ZnO, Cr after NaCl and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=40:40:10:10 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 700 DEG C, constant temperature pre-synthesis reaction 2h; After 150 DEG C of dry 24h, granularity is 200 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=49:49:2 weighs, by the Fe weighing 2o 3powder add be warming up to 900 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 1h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 2um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
Embodiment 4: by the CaCl after 300 DEG C of dehydration 48h in air 2, granularity is 300 object ZnO, Cr after NaCl and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=30:30:20:20 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 850 DEG C, constant temperature pre-synthesis reaction 4h; After 150 DEG C of dry 24h, granularity is 300 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=47:47:6 weighs, by the Fe weighing 2o 3powder add be warming up to 1000 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 2h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 5um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
Embodiment 5: by the CaCl after 300 DEG C of dehydration 48h in air 2, granularity is 200 object ZnO, Cr after KCl and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=40:40:10:10 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 700 DEG C, constant temperature pre-synthesis reaction 2h; After 150 DEG C of dry 24h, granularity is 200 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=49:49:2 weighs, by the Fe weighing 2o 3powder add be warming up to 900 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 1h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 2um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
Embodiment 6: by the CaCl after 300 DEG C of dehydration 48h in air 2, granularity is 300 object ZnO, Cr after KCl and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=30:30:20:20 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 850 DEG C, constant temperature pre-synthesis reaction 4h; After 150 DEG C of dry 24h, granularity is 300 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=47:47:6 weighs, by the Fe weighing 2o 3powder add be warming up to 1000 DEG C after pre-synthesis system after constant temperature carry out whole building-up reactions 2h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.Fused salt volatilization quality is 5%, and the recovery rate of powder is 96%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 5um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.

Claims (4)

1. the synthetic ZnO-Cr of molten-salt growth method 2o 3-Fe 2o 3be humiceram agglomerated powder body method, it is characterized in that comprising the following steps:
(1) proportioning starting material:
KCl, NaCl, the CaCl of crystal water will do not contained 2villaumite is the medium of building-up reactions, granularity 200-300 object ZnO, Cr 2o 3, Fe 2o 3oxide powder is primitive reaction material;
Ratio requirement:
Pre-synthesis system: ZnO, Cr 2o 3it is 20～40% that mixture accounts for pre-synthesis reaction system material molar content, wherein ZnO:Cr 2o 3mol ratio=1:1; All the other are KCl, NaCl, CaCl 2any two kinds of mixing salts in salt, blending ratio is mol ratio 1:1;
Whole synthetic system: Fe 2o 3account for ZnO, Cr 2o 3, Fe 2o 3the molar content of material total amount is 2～6% to add pre-synthesis system;
(2) pre-synthesis:
Abundant dewatered raw material, with ZnO, the Cr of above-mentioned content 2o 3kCl, the NaCl of mixed oxide and mol ratio 1:1, CaCl 2in salt, any two kinds of mixing salts fully mix, and pack reactor into, require to react 2-4h at 700～850 DEG C of temperature;
(3) synthetic eventually:
Add the Fe of above-mentioned content to the system of pre-synthesis 2o 3, at 900～1000 DEG C of reaction 1-2h of temperature;
(4) collection of product:
With after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product.
2. a kind of molten-salt growth method is synthesized ZnO-Cr according to claim 1 2o 3-Fe 2o 3be humiceram agglomerated powder body method, it is characterized in that: containing KCl, NaCl, the CaCl of crystal water 2it is the 48h that dewaters at 300 DEG C of temperature in air that villaumite removes crystal water condition; Granularity 200-300 object ZnO, Cr 2o 3, Fe 2o 3oxide powder is dried 24h in air at 150 DEG C of temperature.
3. a kind of molten-salt growth method is synthesized ZnO-Cr according to claim 1 2o 3-Fe 2o 3be humiceram agglomerated powder body method, it is characterized in that: pre-synthesis reaction synthesis temperature will make the substance system of set proportioning fully melt and reach suitable activity, and the volatile quantity of fused salt is 3-5%, and OK range is 700～850 DEG C; Whole building-up reactions synthesis temperature will make reactant reach suitable activity, and OK range is 900～1000 DEG C.
4. a kind of molten-salt growth method is synthesized ZnO-Cr according to claim 1 2o 3-Fe 2o 3be humiceram agglomerated powder body method, it is characterized in that: Best Applying Condition: be 200 object ZnO, Cr by granularity after KCl, NaCl after 300 DEG C of dehydration 48h in air and 150 DEG C of dry 24h 2o 3kCl:NaCl:ZnO:Cr in molar ratio 2o 3=40:40:10:10 weighs and fully mixes, and mixing salt is put into corundum crucible; Energising is heated to 700 DEG C, constant temperature pre-synthesis reaction 2h; After 150 DEG C of dry 24h, granularity is 200 order Fe 2o 3powder is by pre-synthesis reaction ZnO, Cr 2o 3the amount of powder is with mol ratio ZnO:Cr 2o 3: Fe 2o 3=49:49:2 weighs, by the Fe weighing 2o 3powder add with synthetic system after be warming up to 900 DEG C after constant temperature carry out whole building-up reactions 1h; After system air cooling with after distilled water cleaning reaction thing, its insoluble solid particle drying and obtain end product; Fused salt volatilization quality is 3%, and the recovery rate of powder is 95%, and by material phase analysis, product is mainly ZnO-Zn (Fe, Cr) 2o 4, mean particle size is 2um, meets ZnO-Cr 2o 3-Fe 2o 3it is the requirement of humiceram sintering powder.
CN201410050251.0A 2014-02-14 2014-02-14 Method of synthesizing ZnO-Cr2O3-Fe2O3-series humidity-sensitive ceramic sintered powder by molten-salt growth method Expired - Fee Related CN103880410B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108585795A (en) * 2018-07-11 2018-09-28 中国科学院新疆理化技术研究所 A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material
CN109161227A (en) * 2018-08-23 2019-01-08 佛山市三水区康立泰无机合成材料有限公司 A kind of preparation method of the reddish brown colorant of ceramic ink jet
WO2022148145A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic and preparation method therefor, and atomization core
WO2022148144A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic, atomization core and preparation method therefor
WO2022148146A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic and preparation method therefor, and atomization core

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1789203A (en) * 2005-12-27 2006-06-21 武汉理工大学 Method for synthesizing multi-element, inorganic compound ceramic uniformed powder

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1789203A (en) * 2005-12-27 2006-06-21 武汉理工大学 Method for synthesizing multi-element, inorganic compound ceramic uniformed powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
苏海林等: "熔盐法生长ZnO单晶颗粒的微结构与形貌研究", 《合肥工业大学学报（自然科学版）》 *
韩娟等: "ZnO导电陶瓷的制备及电性能研究", 《青岛科技大学学报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108585795A (en) * 2018-07-11 2018-09-28 中国科学院新疆理化技术研究所 A kind of method that molten salt process prepares negative temperature coefficient thermal-sensitive ceramic material
CN108585795B (en) * 2018-07-11 2021-02-05 中国科学院新疆理化技术研究所 Method for preparing negative temperature coefficient thermal sensitive ceramic material by salt melting method
CN109161227A (en) * 2018-08-23 2019-01-08 佛山市三水区康立泰无机合成材料有限公司 A kind of preparation method of the reddish brown colorant of ceramic ink jet
WO2022148145A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic and preparation method therefor, and atomization core
WO2022148144A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic, atomization core and preparation method therefor
WO2022148146A1 (en) * 2021-01-08 2022-07-14 惠州市新泓威科技有限公司 Humidity-sensitive porous ceramic and preparation method therefor, and atomization core

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