CN106395764A - Preparation method of quaternary layered compound - Google Patents
Preparation method of quaternary layered compound Download PDFInfo
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- CN106395764A CN106395764A CN201610750756.7A CN201610750756A CN106395764A CN 106395764 A CN106395764 A CN 106395764A CN 201610750756 A CN201610750756 A CN 201610750756A CN 106395764 A CN106395764 A CN 106395764A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to a preparation method of a quaternary layered compound. The technical problems of complexness and high device requirements of present preparation methods of the quaternary layered compound are solved in the invention. The method comprises the following steps: grinding a composite molten salt, grinding raw materials, preparing a reaction solution, and carrying out a post-treatment process. The method can be widely used in the field of preparation of the quaternary layered compound.
Description
Technical field
The present invention relates to lithium ion battery electrode material preparation field and in particular to a kind of preparation side of quaternary lamellar compound
Method.
Background technology
After the industrial revolution, global economy and science and technology have obtained fast development, but always with very while development
Many problems.On the one hand, the excessive exploitation of resource causes the drastically minimizing of traditional energy.On the other hand, industrial production produces
Waste, waste liquid, waste gas etc. can not process in time and cause serious environmental pollution.Therefore, active demand is developed one kind and can be reduced
The burning of fossil fuel and the new technology recycling low grade heat energy such as industrial waste heat, vehicle exhaust etc..And thermoelectric power generation skill
Art research and development make used heat be converted into electric energy be possibly realized and can be expected to replace fossil fuel come to alleviate global climate become
Warm problem.The lamellar compound bismuth copper selenolite that a kind of in recent years intrinsic low-heat is led shows good thermoelectricity capability, causes people
Great interest.
Quaternary lamellar compound, such as BiCuSeO, LaCuSeO etc. are typical ZrSiCuAs crystalline structures, and it is typically by carrying
The conductive layer of supplied for electronic transport channel and as the layer structure material alternately piled up layer by layer as phon scattering region insulation
Material.Because it has low thermal conductivity, can be used as the extremely promising thermoelectric material of one kind.And stem-winding be above-mentioned quaternary
Lamellar compound can make ZT value have very big raising by other elements of adulterating.
But traditional synthetic method such as solid-phase synthesis, PLD method, higher to equipment requirement, technological process is typically more multiple
Miscellaneous, it is difficult to carry out industrialized production.
Content of the invention
The present invention is exactly to solve existing quaternary lamellar compound preparation method complexity, the technology higher to equipment requirement
Problem, provides a kind of production technology to simplify, can reduce the preparation method of the quaternary lamellar compound of production cost.
The present invention comprises the steps：(1) grind composite molten salt：Under room temperature, by two kinds of composite molten salt with mol ratio
For (0.2～1)：1 ratio weighs total amount and is 5～20 grams, is poured into grinding 10～30min in mortar, is allowed to be sufficiently mixed；
(2) grind raw material：By ln compound, selenium powder, cuprous oxide according to (1～3)：(2～5)：(1～3) mol ratio is weighed, former
Material total amount is (0.05～0.2) with the mass ratio of composite molten salt total amount：1, after grinding uniformly, composite molten salt is poured into enter again
Row grinds, and makes powder homogeneous；(3) configure reaction solution：Weigh reducing agent, pour in water heating kettle, add water to be allowed to percent mass
Specific concentration is 5%～20%, fully dissolves, more ground material in step (2) is poured in water heating kettle stirs, by hydro-thermal
Kettle is put in autoclave, then puts into water heating kettle in baking oven；Reaction condition：Oven temperature is 150～250 DEG C, the reaction time
For 24～72h, the volume of water is 25～100mL, the material quality concentration that in the aqueous solution, step (2) is ground is 0.02～
0.05g/mL；(4) last handling process：Take out autoclave and allow it be cooled to room temperature, deionized water and absolute ethyl alcohol are clear respectively
Wash for several times, be finally placed in 50～80 DEG C of drying box drying the sample obtaining synthesizing using collecting product by the way of centrifugation.
Preferably, the system of composite molten salt is LiCl-KCl, NaCl-KCl, MgCl2-KCl、Li2SO4-K2SO4、
AlCl3One or more of-NaCl or NaSCN-KSCN.
Preferably, the ln compound in step (2) is bismuth oxide, bismuth chloride, bismuth nitrate, bismuth citrate, lanthanum nitrate, chlorination
One or more of lanthanum, cerium chloride or cerous nitrate.
Preferably, the reducing agent in step (3) be one of polyethylene glycol, polyvinylpyrrolidone or hydrazine hydrate or
Several.
The quaternary lamellar compound of the present invention makes electrode as follows, and carries out electrochemical property test：
Quaternary lamellar compound is sufficiently mixed all by mortar grinder mode with conductive black Super-P (10wt%)
Even, sequentially add the 1-METHYLPYRROLIDONE of Kynoar (10wt%) and 20 times of Kynoar quality, be sufficiently stirred for
Uniformly become pasty state.Using nickel foam as collector, the above-mentioned material mixing is evenly coated in foam nickel surface, will make
Pole piece 100 DEG C be vacuum dried 12 hours, then dried pole piece is carried out battery assembling in glove box, is wherein electrolysed
Liquid is 1MLiPF6, solvent is 1 for volume ratio：In 1 ethylene carbonate and dimethyl carbonate, battery size is 2025.Electrochemistry
Method of testing is in 0.005～3V voltage range, 200mA h g-1It is circulated test under constant current conditions.
The present invention has the advantage that：
(1) prepare the quaternary lamellar compound of pure phase using composite molten salt method, gather has the pattern of comparison rule simultaneously,
Preparation is simple, controllability is strong, products collection efficiency more than 90%, and utilize under relatively low temperature conditionss water heating kettle and
Baking oven just can complete synthesis so that production cost reduces it is easy to be applicable, and opens the new think of of preparation quaternary lamellar compound
Road.
(2) the invention enables lithium ion battery negative material has more selections, there is provided be applied to thermoelectric material
The thinking of lithium ion battery.The layer structure of quaternary lamellar compound is provided for conductive layer and active mass layer, and this makes
Material has more preferable electric conductivity, and conductive layer can serve as buffering area, and the volumetric expansion to electrode material also has certain suppression
Make and use, stratified material has more preferable ion transportation, and above-mentioned makes a little it have more preferable electrode material simultaneously
Application prospect.
Brief description
Fig. 1 is the XRD of the BiCuSeO of the embodiment of the present invention 1 preparation.
Fig. 2 is the BiCuSeO nanometer sheet SEM figure of the embodiment of the present invention 1 preparation.
Fig. 3 is charge and discharge cycles curve under 200mA/g constant current for the BiCuSeO preparing in inventive embodiments 1.
Specific embodiment
With the preparation method of the present invention, the quaternary lamellar compound prepared by the present invention is retouched further below in conjunction with the accompanying drawings
State：
Embodiment 1
Under room temperature, with mol ratio as LiCl：The ratio of KCl=0.2 weighs the complex salt that total amount is 5 grams, is poured into and grinds
Grind 10min in alms bowl, be allowed to be sufficiently mixed.
By bismuth chloride, selenium powder, cuprous oxide according to 3:5:It is 1g that 2 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 10g polyvinylpyrrolidone, pour in water heating kettle, add 50mL water to make fully to dissolve, then will be ground
Material is poured in water heating kettle and is stirred, and water heating kettle is put in autoclave；
Autoclave is put in 200 DEG C of baking oven, reaction time 48h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 50 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
The stereoscan photograph of product is as shown in figure 1, the XRD curve of product is as shown in Figure 2.Fig. 3 is that the multiplying power of material is filled
Discharge test figure.As can be seen from Figure 3 with the increase of cycle-index, its capacity gradually tends towards stability, and illustrates this
Material has preferable cycle performance.
Embodiment 2
Under room temperature, the ratio with mol ratio as NaCl-KCl=0.5 weighs the complex salt that total amount is 10 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By bismuth chloride, selenium powder, cuprous oxide according to 2:2:It is 1g that 1 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 1g polyvinylpyrrolidone, pour in water heating kettle, add 20mL water to make fully to dissolve, then by ground material
Pour in water heating kettle and stir, water heating kettle is put in autoclave；
Autoclave is put in 150 DEG C of baking oven, reaction time 24h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 70 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 3
Under room temperature, with mol ratio as LiNO3-KNO3=1 ratio weighs the complex salt that total amount is 20 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By bismuth oxide, selenium powder, cuprous oxide according to 1:2:It is 1g that 1 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 1gPVP, pour in water heating kettle, add 20mL water to make fully to dissolve, more ground material is poured into water heating kettle
In stir, water heating kettle is put in autoclave；
Autoclave is put in 200 DEG C of baking oven, reaction time 48h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 80 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 4
Under room temperature, with mol ratio as LiNO3-KNO3=0.5 ratio weighs the complex salt that total amount is 20 grams, is poured into
Grind 20min in mortar, be allowed to be sufficiently mixed.
By bismuth nitrate, selenium powder, cuprous oxide according to 2:2:It is 1.5g that 3 mol ratio carries out weighing total amount, after grinding uniformly
Composite molten salt is poured into and is ground again, make powder homogeneous；
Weigh 3.8g hydrazine hydrate, pour in water heating kettle, add 38mL water to make fully to dissolve, more ground material is poured into water
Stir in hot kettle, water heating kettle is put in autoclave；
Autoclave is put in 250 DEG C of baking oven, reaction time 72h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 80 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 5
Under room temperature, with mol ratio as LiNO3-KNO3=1 ratio weighs the complex salt that total amount is 15 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By bismuth nitrate, selenium powder, cuprous oxide according to 2:2:It is 1.5g that 1 mol ratio carries out weighing total amount, after grinding uniformly
Composite molten salt is poured into and is ground again, make powder homogeneous；
Weigh 3.8g hydrazine hydrate, pour in water heating kettle, add 38mL water to make fully to dissolve, more ground material is poured into water
Stir in hot kettle, water heating kettle is put in autoclave；
Autoclave is put in 240 DEG C of baking oven, reaction time 72h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 80 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 6
Under room temperature, with mol ratio as LiCl：The ratio of KCl=0.2 weighs the complex salt that total amount is 20 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By bismuth oxide, selenium powder, cuprous oxide according to 1:2:It is 2g that 1 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 5g polyethylene glycol, pour in water heating kettle, add 100mL water to make fully to dissolve, more ground material is poured into
Stir in water heating kettle, water heating kettle is put in autoclave；
Autoclave is put in 200 DEG C of baking oven, reaction time 48h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 50 DEG C of drying box drying the BiCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 7
Under room temperature, with mol ratio as LiCl：The ratio of KCl=0.2 weighs the complex salt that total amount is 20 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By lanthanum chloride, selenium powder, cuprous oxide according to 1:2:It is 2g that 1 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 5g polyethylene glycol, pour in water heating kettle, add 100mL water to make fully to dissolve, more ground material is poured into
Stir in water heating kettle, water heating kettle is put in autoclave；
Autoclave is put in 200 DEG C of baking oven, reaction time 48h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 50 DEG C of drying box drying the LaCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Embodiment 8
Under room temperature, the ratio with mol ratio as NaCl-KCl=0.5 weighs the complex salt that total amount is 10 grams, is poured into and grinds
Grind 20min in alms bowl, be allowed to be sufficiently mixed.
By cerium chloride, selenium powder, cuprous oxide according to 2:2:It is 1g that 1 mol ratio carries out weighing total amount, will after grinding uniformly
Composite molten salt is poured into and is ground, makes powder homogeneous；
Weigh 1g polyvinylpyrrolidone, pour in water heating kettle, add 20mL water to make fully to dissolve, then by ground material
Pour in water heating kettle and stir, water heating kettle is put in autoclave；
Autoclave is put in 150 DEG C of baking oven, reaction time 24h, closes baking oven after the arrival of question response time.
Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol for several times, finally adopt respectively
The mode of centrifugation is collected product and is placed in 70 DEG C of drying box drying the CeCuSeO sample obtaining synthesizing.Simultaneously by material system
Battery electrode is become to carry out electro-chemical test.
Electro-chemical test partly with embodiment 1, the prepared materials show experiment knot almost identical with embodiment 1
Really.
Claims (4)
1. a kind of preparation method of quaternary lamellar compound, is characterized in that comprising the steps：
(1) grind composite molten salt：Under room temperature, by two kinds of composite molten salt with mol ratio for (0.2～1)：1 ratio weighs total
Measure as 5～20 grams, be poured into grinding 10～30min in mortar, be allowed to be sufficiently mixed；
(2) grind raw material：By ln compound, selenium powder, cuprous oxide according to (1～3)：(2～5)：(1～3) mol ratio is claimed
Amount, raw material total amount is (0.05～0.2) with the mass ratio of composite molten salt total amount：1, after grinding uniformly, composite molten salt is poured into
It is ground, make powder homogeneous again；
(3) configure reaction solution：Weigh reducing agent, pour in water heating kettle, add water be allowed to mass percent concentration be 5%～
20%, fully dissolve, more ground material in step (2) is poured in water heating kettle stir, water heating kettle is put into autoclave
In, then water heating kettle is put in baking oven；Reaction condition：Oven temperature is 150～250 DEG C, and the reaction time is 24～72h, water
Volume be 25～100mL, the material quality concentration that in the aqueous solution, step (2) is ground be 0.02～0.05g/mL；
(4) last handling process：Take out autoclave and allow it be cooled to room temperature, deionized water and washes of absolute alcohol number respectively
Secondary, finally it is placed in 50～80 DEG C of drying box drying the sample obtaining synthesizing using collecting product by the way of centrifugation.
2. the preparation method of quaternary lamellar compound according to claim 1 is it is characterised in that described composite molten salt
System is LiCl-KCl, NaCl-KCl, MgCl2-KCl、Li2SO4-K2SO4、AlCl3One of-NaCl or NaSCN-KSCN
Or it is several.
3. the preparation method of quaternary lamellar compound according to claim 1 is it is characterised in that in described step (2)
Ln compound is in bismuth oxide, bismuth chloride, bismuth nitrate, bismuth citrate, lanthanum nitrate, lanthanum chloride, cerium chloride or cerous nitrate
Plant or several.
4. quaternary lamellar compound according to claim 1 preparation method it is characterised in that in described step 3 also
Former dose is one or more of polyethylene glycol, polyvinylpyrrolidone or hydrazine hydrate.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643085A (en) * | 2012-04-13 | 2012-08-22 | 清华大学 | Bi Cu 1-x SeO-based oxide thermoelectric ceramic material and preparation method thereof |
| CN102655204A (en) * | 2012-04-28 | 2012-09-05 | 北京航空航天大学 | Sr-doping oxide BiCuSeO thermoelectric material and preparation method thereof |
| CN103011838A (en) * | 2012-10-24 | 2013-04-03 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of BiCuSeO-based pyroelectric oxide powder |
-
2016
- 2016-08-29 CN CN201610750756.7A patent/CN106395764B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102643085A (en) * | 2012-04-13 | 2012-08-22 | 清华大学 | Bi Cu 1-x SeO-based oxide thermoelectric ceramic material and preparation method thereof |
| CN102655204A (en) * | 2012-04-28 | 2012-09-05 | 北京航空航天大学 | Sr-doping oxide BiCuSeO thermoelectric material and preparation method thereof |
| CN103011838A (en) * | 2012-10-24 | 2013-04-03 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of BiCuSeO-based pyroelectric oxide powder |
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