CN109081347A - A method of based on mutually separation synthesis porous carbon microsphere - Google Patents
A method of based on mutually separation synthesis porous carbon microsphere Download PDFInfo
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- CN109081347A CN109081347A CN201810787175.XA CN201810787175A CN109081347A CN 109081347 A CN109081347 A CN 109081347A CN 201810787175 A CN201810787175 A CN 201810787175A CN 109081347 A CN109081347 A CN 109081347A
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- porous carbon
- carbon microsphere
- microsphere material
- material preparation
- mutually separated
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000004005 microsphere Substances 0.000 title claims abstract description 16
- 230000015572 biosynthetic process Effects 0.000 title abstract description 3
- 238000003786 synthesis reaction Methods 0.000 title abstract description 3
- 238000000926 separation method Methods 0.000 title description 2
- 239000000463 material Substances 0.000 claims abstract description 24
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 14
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 11
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 11
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000428 dust Substances 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims abstract 6
- 238000000137 annealing Methods 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims description 11
- 239000011259 mixed solution Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 229910052786 argon Inorganic materials 0.000 claims description 7
- 239000012300 argon atmosphere Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 2
- 238000001694 spray drying Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 5
- 238000002791 soaking Methods 0.000 claims 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 239000008236 heating water Substances 0.000 claims 1
- 239000003595 mist Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 239000007921 spray Substances 0.000 claims 1
- -1 kalium ion Chemical class 0.000 abstract description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 abstract description 2
- 238000005191 phase separation Methods 0.000 abstract description 2
- 229910052700 potassium Inorganic materials 0.000 abstract description 2
- 239000011591 potassium Substances 0.000 abstract description 2
- 210000003743 erythrocyte Anatomy 0.000 description 24
- 229910003178 Mo2C Inorganic materials 0.000 description 13
- 238000001291 vacuum drying Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 2
- 238000005087 graphitization Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/949—Tungsten or molybdenum carbides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- 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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The method that the present invention establishes the porous carbon microsphere material based on phase separation principle synthesis, solution is mixed to form by being spray-dried to obtain presoma by the ammonium molybdate, polyvinyl alcohol, deionized water of the ratio containing certain mass, presoma is vacuum dried, after annealing black powder, the powder is handled in the dust technology of heat, be centrifuged, be dried in vacuo after be heat-treated to get to porous carbon microsphere material.Preparation method of the present invention is simple, and yield is higher.Prepared material has excellent porosity and biggish specific surface area, can be used for the fields such as battery, super capacitor, gas sensor, has wide industrial applications prospect.The present invention, using prepared porous carbon microsphere material as battery cathode, illustrates higher storage potassium capacity, outstanding high rate performance and cyclical stability so that kalium ion battery is applied as an example.
Description
[technical field]
The invention belongs to carbon material preparation method fields, and in particular to a kind of porous carbon microsphere material based on phase separation principle
Material and preparation method thereof.
[background technique]
Carbon material is due to the advantages such as its is from a wealth of sources, cheap, thermal stability is good, in energy storage such as battery, super capacitors
The fields such as field and gas sensor, conductive material cause larger concern, are the most commonly used materials of current commercial applications
Material.By taking the application in field of batteries as an example, existing cell negative electrode material is mainly natural graphite and artificial graphite, but Yin Qiben
The restriction of body structure characteristic, graphite cathode material development encounters bottleneck, such as specific capacity reaches capacity, and is persistently large current discharge energy
Power difference etc..Improving carbon material specific capacity main method includes improving effective ratio area, reinforcing material structural stability etc..Carbon is micro-
For ball due to large specific surface area, structure is relatively stable, additionally has preparation simply, pollution-free, it can be achieved that large-scale production etc. is excellent
Point, tool have great prospects for development.
The present invention is intended to provide a kind of simple process, the carbosphere material preparation side that reproducible, yield is high, at low cost
Method.Method of the present invention is spray drying process, micro- based on ammonium molybdate and the mutually isolated red blood cell shape carbon of polyvinyl alcohol
Ball improves production efficiency and production scale.Meanwhile the carbosphere material being prepared is applied to kalium ion battery by the present invention
As cathode, good chemical property has been obtained.
[summary of the invention]
1. provided by the invention a kind of based on the porous carbon microsphere material preparation method mutually separated, according to the following steps into
Row:
(1) 10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, and then 60 DEG C
Water-bath uniform stirring 10h forms the mixed solution of a homogeneous transparent.
(2) step (1) acquired solution is obtained into presoma by the method being spray-dried, wherein speed is 1200ml h-1,
Inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.
(3) 80 DEG C of vacuum drying 12h of presoma collected, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C
And 2h is kept to obtain Mo2C@C red blood cell shape carbon ball.
(4) 0.1g red blood cell shape Mo2C@C is added in 65ml 5%HNO3 solution, then in 80 DEG C of heating 20h.
(5) sample obtained by step (4) is repeatedly centrifuged, and 80 DEG C of vacuum drying 12h.
(6) sample obtained by step (5) is in the carbon ball that heat treatment 2h at 500 DEG C just obtains porous red blood cell shape.
2. red blood cell shape negative electrode material even pore distribution, large specific surface area, good conductivity that the present invention is prepared into.By institute
It is steady to can express high charge-discharge specific capacity, outstanding high rate performance, good circulation as kalium ion battery cathode for material obtained
Qualitative energy.In addition, the method for the present invention simple process, reproducible, yield is higher, low in cost.
[specific embodiment]
Embodiment 1:10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, then
60 DEG C of water-bath uniform stirring 10h form the mixed solution of a homogeneous transparent.Solution obtains forerunner by the method being spray-dried
Body, wherein speed is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum of presoma of collection are dry
Dry 12h, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C and 2h kept to obtain Mo2C@C red blood cell shape carbon ball.
Embodiment 2:10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, then
60 DEG C of water-bath uniform stirring 10h form the mixed solution of a homogeneous transparent.Solution obtains forerunner by the method being spray-dried
Body, wherein speed is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum of presoma of collection are dry
Dry 12h, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C and 2h kept to obtain Mo2C@C red blood cell shape carbon ball.
0.1g red blood cell shape Mo2C@C is added in 65ml 1%HNO3 solution, then in 80 DEG C of heating 20h.Subsequent sample carries out more
Secondary centrifugation, and 80 DEG C of vacuum drying 12h, heat treatment 2h just obtains porous red blood cell shape carbon ball at 500 DEG C later.
Embodiment 3:10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, then
60 DEG C of water-bath uniform stirring 10h form the mixed solution of a homogeneous transparent.Solution obtains forerunner by the method being spray-dried
Body, wherein speed is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum of presoma of collection are dry
Dry 12h, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C and 2h kept to obtain Mo2C@C red blood cell shape carbon ball.
0.1g red blood cell shape Mo2C@C is added in 65ml 3%HNO3 solution, then in 80 DEG C of heating 20h.Subsequent sample carries out more
Secondary centrifugation, and 80 DEG C of vacuum drying 12h, heat treatment 2h just obtains porous red blood cell shape carbon ball at 500 DEG C later.
Embodiment 4:10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, then
60 DEG C of water-bath uniform stirring 10h form the mixed solution of a homogeneous transparent.Solution obtains forerunner by the method being spray-dried
Body, wherein speed is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum of presoma of collection are dry
Dry 12h, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C and 2h kept to obtain Mo2C@C red blood cell shape carbon ball.
0.1g red blood cell shape Mo2C@C is added in 65ml 5%HNO3 solution, then in 80 DEG C of heating 20h.Subsequent sample carries out more
Secondary centrifugation, and 80 DEG C of vacuum drying 12h, heat treatment 2h just obtains porous red blood cell shape carbon ball at 500 DEG C later.
Embodiment 5:10gAMM (ammonium molybdate) and 4.5gPVA (polyvinyl alcohol) are dissolved in 500ml deionized water respectively, then
60 DEG C of water-bath uniform stirring 10h form the mixed solution of a homogeneous transparent.Solution obtains forerunner by the method being spray-dried
Body, wherein speed is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum of presoma of collection are dry
Dry 12h, then 1 DEG C of min in argon atmosphere-1Rate be heated to 900 DEG C and 2h kept to obtain Mo2C@C red blood cell shape carbon ball.
0.1g red blood cell shape Mo2C@C is added in 65ml 7%HNO3 solution, then in 80 DEG C of heating 20h.Subsequent sample carries out more
Secondary centrifugation, and 80 DEG C of vacuum drying 12h, heat treatment 2h just obtains porous red blood cell shape carbon ball at 500 DEG C later.
Red blood cell shape carbon ball made from above-described embodiment 1 to embodiment 5 is characterized using SEM, utilizes tape measure
The diameter in hole, as a result as shown in the table:
The diameter in hole | |
Embodiment 1 | 0 |
Embodiment 2 | ~65 |
Embodiment 3 | ~130 |
Embodiment 4 | ~205 |
Embodiment 5 | ~255 |
As seen from table, when without nitric acid treatment, SEM does not observe hole.When concentration of nitric acid is relatively low, the diameter in hole is inclined
It is small.As concentration of nitric acid increases, the diameter in hole, which then becomes apparent, to become larger.
Comparative example 1:4.5gPVA (polyvinyl alcohol) is dissolved in 500ml deionized water, then 60 DEG C of water-bath uniform stirring 10h
Form the mixed solution of a homogeneous transparent.Solution obtains presoma by the method being spray-dried, and wherein speed is 1200ml
h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum drying 12h of presoma of collection, then in argon atmosphere
1℃min-1Rate be heated to 900 DEG C and 2h kept to obtain red blood cell shape carbon ball.
Comparative example 2:4.5gPVA (polyvinyl alcohol) is dissolved in 500ml deionized water, then 60 DEG C of water-bath uniform stirring 10h
Form the mixed solution of a homogeneous transparent.Solution obtains presoma by the method being spray-dried, and wherein speed is 1200ml
h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.80 DEG C of vacuum drying 12h of presoma of collection, then in argon atmosphere
1℃min-1Rate be heated to 900 DEG C and 2h kept to obtain red blood cell shape carbon ball.0.1g red blood cell shape Mo2C@C is added to
In 65ml 5%HNO3 solution, then in 80 DEG C of heating 20h.Subsequent sample is repeatedly centrifuged, and 80 DEG C of vacuum drying 12h,
Heat treatment 2h just obtains porous red blood cell shape carbon ball at 500 DEG C later.
By above-described embodiment 1, embodiment 4, comparative example 1,2 gained sample of comparative example progress Raman characterization.In 1350cm-1It is left
Right position is denoted as the peak D.In 1600cm-1The position of left and right is denoted as the peak G.Utilize ID/IGRatio to come the stone that judges carbon material
Blackization degree.
ID/IG | |
Embodiment 1 | 1.048 |
Embodiment 4 | 1.053 |
Comparative example 1 | 0.919 |
Comparative example 2 | 1.04 |
As seen from table, generally speaking, having added the carbon source of ammonium molybdate, comparatively degree of graphitization is higher;Carry out dilute nitre of heat
Acid treated material degree of graphitization also all slightly improves.
By above-described embodiment 1, embodiment 4, comparative example 1, carbosphere material obtained by comparative example 2 as working electrode,
Potassium is button cell to be assembled into, in 0.1A g to electrode-1Under current density, cycle performance of battery is tested.As a result such as following table institute
Show:
As seen from table, specific discharge capacity is 54mAhg after the material of pure PVA 50 circulations-1, Mo2C@C red blood cell shape carbon ball
Specific discharge capacity is 300mAhg after 50 circulations-1.Two materials specific discharge capacity after the dust technology of heat is handled well all obtains one
Determine the raising of degree.
Claims (8)
1. a kind of based on the porous carbon microsphere material preparation method mutually separated, which comprises the following steps:
(1) polyvinyl alcohol and ammonium molybdate are mixed with deionized water according to a certain percentage, then 60 DEG C of water-bath uniform stirring 10h shapes
At the mixed solution of a homogeneous transparent;
(2) step (1) acquired solution is obtained into white powder by the method being spray-dried;
(3) heat treatment obtains the black powder containing molybdenum element in argon gas after being dried in vacuo white powder;
(4) black powder obtained by step (3) is added into dust technology HNO3 solution, then carries out heating water bath;
(5) sample obtained by step (4) is repeatedly centrifuged, is then dried in vacuo;
(6) sample obtained by step (5) is heat-treated to obtain porous carbon microsphere.
2. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that carbon
Source is the mixture of ammonium molybdate and polyvinyl alcohol, and mass ratio is between 1:1~3:1.
3. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that spray
Mist rate of drying is 1200ml h-1, inlet temperature is 220 DEG C, and outlet temperature is 100 DEG C.
4. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that molybdenum
Sour ammonium occurs mutually to separate with polyvinyl alcohol in spray drying.
5. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that true
Empty drying temperature is 60~90 DEG C, and drying time is 6h or more, 80 DEG C of preferred drying temperature, drying time 12h.
6. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that dilute
Concentration of nitric acid is 1%~9%, more preferably 5%.
7. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that preceding
Drive body annealing conditions are as follows: in argon atmosphere, 1~2 DEG C of min-1Being heated to 900 DEG C of soaking times is 1~3h, preferred 2h.
8. according to claim 1 a kind of based on the porous carbon microsphere material preparation method mutually separated, it is characterised in that power
The heat treatment temperature of sharp 1 step (5) is 450~550 DEG C, and soaking time is 1~3h, and preferred 500 DEG C, soaking time is
2h。
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Application publication date: 20181225 |