CN106082355A - A kind of Ca3co2o6the preparation method of powder - Google Patents
A kind of Ca3co2o6the preparation method of powder Download PDFInfo
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- CN106082355A CN106082355A CN201610342009.XA CN201610342009A CN106082355A CN 106082355 A CN106082355 A CN 106082355A CN 201610342009 A CN201610342009 A CN 201610342009A CN 106082355 A CN106082355 A CN 106082355A
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- calcium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/66—Cobaltates containing alkaline earth metals, e.g. SrCoO3
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention provides a kind of Ca3Co2O6The preparation method of powder, it concretely comprises the following steps: by Ca3Co2O6In stoichiometric proportion weigh calcium carbonate and cobalt oxide powder, will the two ground and mixed uniformly after, under the air atmosphere of 870~930 DEG C, sinter 3.5~4.5h.To solve Ca3Co2O6Manufacturing cycle length, reaction temperature high, need the auxiliary materials such as flux, and reaction raw materials mixing uniformity be limited, be easily caused non-stoichiometric, the heterogeneous and problem of irregular granule-morphology.The invention belongs to calcium cobalt base oxide preparation field.
Description
Technical field
The present invention relates to the preparation method of a kind of calcium cobalt base oxide, belong to calcium cobalt base oxide preparation field.
Background technology
In recent years, along with becoming increasingly conspicuous of environment and energy problem, people give pass greatly to thermo-electric converting material
Note. pyroelectric oxide Ca3Co2O6Owing to Heat stability is good, the features such as oxidation, avirulence, function admirable of not being afraid of become the heat of research
Point. at present, Ca3Co2O6Preparation use high temperature solid state reaction. utilize raw material to firstly generate intermediate product Ca3Co4O9, then in general
Between product Ca3Co4O9It is converted into Ca3Co2O6, such as: utilize calcium carbonate and cobalt sesquioxide in 1000 under the effect of flux
React about 12h about DEG C, generate intermediate product Ca3Co4O9, then by intermediate product Ca3Co4O9It is ground, after grinding
Ca3Co4O9It is converted into end product Ca after sintering 24h under the hot conditions of about 1200 DEG C3Co2O6.Current this method
Shortcoming is to need higher reaction temperature and longer heat treatment time, prepares finished powder at laboratory and typically needs a week
Left and right, preparation process needs the auxiliary materials such as flux, and reaction raw materials mixing uniformity is limited, especially intermediate product
Ca3Co4O9It is converted into Ca3Co2O6Process the highest to powder degree and uniformity requirement, be easily caused non-stoichiometric, non-all
Phase and irregular granule-morphology, therefore the performance of material and the controllability of reaction are the most undesirable.
Summary of the invention
It is an object of the invention to: a kind of Ca is provided3Co2O6The preparation method of powder, to solve Ca3Co2O6Preparation week
Phase length, reaction temperature are high, need the auxiliary materials such as flux, and reaction raw materials mixing uniformity is limited, is easily caused non-chemically
Metering is than, the heterogeneous and problem of irregular granule-morphology.
For solving the problems referred to above, intend using such a Ca3Co2O6The preparation method of powder, it concretely comprises the following steps: by 3:2
Mol ratio weigh calcium carbonate and cobalt oxide, will the two mixed grinding uniformly after, sinter under the air atmosphere of 870~930 DEG C
3.5~4.5h.
After uniform for the two mixed grinding, put in sintering furnace, make sintering furnace liter with the heating rate less than 10 DEG C/min
Temperature, until temperature rises to 870~930 DEG C, then Isothermal sinter.
Preferably 900 DEG C Isothermal sinter of sintering temperature, the preferred 4h of sintering time.
Compared with prior art, major advantage is that the method utilizes calcium carbonate and cobalt oxide at about 900 degree to the present invention
Under lower temperature, only need can directly prepare finished product Ca in about four hours3Co2O6Powder, it is not necessary to convert again after preparing intermediate product
For Ca3Co2O6, compare existing preparation method and enormously simplify the processing step of preparation, highly shortened manufacturing cycle, improve
Preparation efficiency, only needs time half a day can complete preparation;Preparation temperature is relatively low, and only needing about 900 degree can realize;Prepared
Cheng Wuxu adds other auxiliary materials, reduces preparation cost;And without intermediate product in preparation process, to reaction raw materials mixing all
Even degree and powder degree require slightly lower, are not easily caused non-stoichiometric, the asking of heterogeneous and irregular granule-morphology
Topic occurs, has highly important actual application and promotional value.
Accompanying drawing explanation
Fig. 1 is gained Ca3Co2O6The XRD figure spectrum of compound;
Fig. 2 is gained Ca3Co2O6The SEM pattern of compound.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, the present invention will be made the most detailed below
Describe,
Embodiment 1:
Preparation Ca3Co2O6Powder: weigh calcium carbonate and cobalt oxide by the mol ratio of 3:2, puts the two in mortar and grinds all
After even, put in sintering furnace, with the heating rate less than 10 DEG C/min be heated to about 800 DEG C and at this temperature insulation 4 little
Time, i.e. obtain Ca3Co2O6Dusty material, obtained Ca3Co2O6The XRD figure spectrum of compound and SEM pattern refer to Fig. 1 and Fig. 2.
Embodiment 2:
Preparation Ca3Co2O6Powder: weigh calcium carbonate and cobalt oxide by the mol ratio of 3:2, puts the two in mortar and grinds all
After even, put in sintering furnace, be heated to 910 DEG C with the heating rate less than 10 DEG C/min and burn under the air atmosphere of 910 DEG C
Knot 3.8h, obtains Ca3Co2O6Powder.
Embodiment 3:
Preparation Ca3Co2O6Powder: weigh calcium carbonate and cobalt oxide by the mol ratio of 3:2, puts the two in mortar and grinds all
After even, put in sintering furnace, be heated to 920 DEG C with the heating rate less than 10 DEG C/min and burn under the air atmosphere of 920 DEG C
Knot 3.6h, obtains Ca3Co2O6Powder.
Embodiment 4:
Preparation Ca3Co2O6Powder: weigh calcium carbonate and cobalt oxide by the mol ratio of 3:2, puts the two in mortar and grinds all
After even, put in sintering furnace, be heated to 880 DEG C with the heating rate less than 10 DEG C/min and burn under the air atmosphere of 880 DEG C
Knot 4.2h, obtains Ca3Co2O6Powder.
Embodiment 5:
Preparation Ca3Co2O6Powder: weigh calcium carbonate and cobalt oxide by the mol ratio of 3:2, puts the two in mortar and grinds all
After even, put in sintering furnace, be heated to 890 DEG C with the heating rate less than 10 DEG C/min and burn under the air atmosphere of 890 DEG C
Knot 4.4h, obtains Ca3Co2O6Powder.
Claims (4)
1. a Ca3Co2O6The preparation method of powder, it is characterised in that concretely comprise the following steps: weigh calcium carbonate by the mol ratio of 3:2
And cobalt oxide, after uniform for the two mixed grinding, under the air atmosphere of 870~930 DEG C, sinter 3.5~4.5h.
A kind of Ca3Co2O6The preparation method of powder, it is characterised in that: by equal for the two mixed grinding
After even, put in sintering furnace, make sintering furnace heat up with the heating rate less than 10 DEG C/min, until temperature rises to 870~930
DEG C, then Isothermal sinter.
A kind of Ca3Co2O6The preparation method of powder, it is characterised in that: sintering temperature is 900 DEG C.
A kind of Ca3Co2O6The preparation method of powder, it is characterised in that: sintering time is 4h.
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CN201610342009.XA CN106082355A (en) | 2016-05-23 | 2016-05-23 | A kind of Ca3co2o6the preparation method of powder |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1389430A (en) * | 2002-06-21 | 2003-01-08 | 清华大学 | Calcium cobaltate-based oxide thermoelectric material and its prepn. |
CN1621354A (en) * | 2004-11-05 | 2005-06-01 | 北京工业大学 | Preparation method of Ca3Co2O6 based oxide thermoelectric material |
CN101157482A (en) * | 2007-09-19 | 2008-04-09 | 哈尔滨工业大学 | Modified Ca-Co-O system doped transition metal composite oxides and preparation method thereof |
-
2016
- 2016-05-23 CN CN201610342009.XA patent/CN106082355A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1389430A (en) * | 2002-06-21 | 2003-01-08 | 清华大学 | Calcium cobaltate-based oxide thermoelectric material and its prepn. |
CN1621354A (en) * | 2004-11-05 | 2005-06-01 | 北京工业大学 | Preparation method of Ca3Co2O6 based oxide thermoelectric material |
CN101157482A (en) * | 2007-09-19 | 2008-04-09 | 哈尔滨工业大学 | Modified Ca-Co-O system doped transition metal composite oxides and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
路清梅等: "Ca3Co2O6 块体的放电等离子烧结及热电性能研究", 《稀有金属》 * |
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Application publication date: 20161109 |
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