CN109292832A - A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof - Google Patents
A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof Download PDFInfo
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- CN109292832A CN109292832A CN201811496150.0A CN201811496150A CN109292832A CN 109292832 A CN109292832 A CN 109292832A CN 201811496150 A CN201811496150 A CN 201811496150A CN 109292832 A CN109292832 A CN 109292832A
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- transition metal
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- acetate
- metal oxide
- carbon aerogels
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 27
- 239000003292 glue Substances 0.000 title claims abstract description 25
- 229910000314 transition metal oxide Inorganic materials 0.000 title claims abstract description 19
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 21
- 239000004966 Carbon aerogel Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 150000003624 transition metals Chemical class 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 238000005253 cladding Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229910021538 borax Inorganic materials 0.000 claims description 11
- 239000004328 sodium tetraborate Substances 0.000 claims description 11
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 8
- 239000008103 glucose Substances 0.000 claims description 8
- -1 transition metal acetate Chemical class 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229940011182 cobalt acetate Drugs 0.000 claims description 6
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 3
- 229940071125 manganese acetate Drugs 0.000 claims description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000052 vinegar Substances 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 229910021278 Co3O4-2 Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
-
- 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
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention relates to airsetting glue transition metal oxide materials of a kind of size adjustable and preparation method thereof, using carbon aerogels as template, the cladding of transition metal are completed by solvent thermal reaction, then obtain through high-temperature process.Size adjustable of the present invention, preparation process is environmentally friendly, easily operated, and raw material is simple and easy to get, and method is common to transition metal, has a good application prospect.
Description
Technical field
The invention belongs to field of inorganic nano material, in particular to the airsetting glue transiting metal oxidation of a kind of size adjustable
Object material and preparation method thereof.
Background technique
Transition metal oxide (TMOs) usually has elevated oxygen level and shows p-type semiconductor characteristic.They are
It is studied as the potential material of many application fields, including energy storage, is catalyzed, sensor and magnetism etc..Especially in electricity
In terms of chemical energy storage, the transition metal oxide of synthesis nano is considered as improving transition metal oxide chemical property
The negative electrode material of a kind of feasible way, nanostructure can be shortened Li+With interelectrode delivering path, bigger table can also be provided
Area is to promote contact of the electrolyte with electrode to accelerate reaction.Porosity has a significant impact to electrode electro Chemical performance, it is not
The diffusion path of ion can only be shortened, moreover it is possible to effectively facilitate electrolyte penetrate into porous structure in, so that it is guaranteed that inside battery from
The quick transmission of son.TMOs is designed to different nanostructures, such as one-dimensional (nano wire, nanometer by a large amount of researcher
Needle or nanotube), two-dimentional (nanometer sheet) and three-dimensional structure (nanocube or nanosphere).Three-dimensional structure has in various configurations
There is bigger advantage, this helps to adapt to volume expansion, because the stress that unexpected structure change generates may be to each side
To release.Unfortunately, due to the limitation of synthetic method and template, designing three-dimensional intercommunication TMO network is a huge challenge.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of airsetting glue transition metal oxide materials of size adjustable
Material and preparation method thereof, the scantling is adjustable；Preparation process is environmentally friendly, easily operated, and raw material is simple and easy to get, and method was common to
Metal is crossed, is had a good application prospect.
The present invention provides a kind of airsetting glue transition metal oxide materials of size adjustable, using carbon aerogels as mould
Plate is completed the cladding of transition metal by solvent thermal reaction, then obtained through high-temperature process.
The present invention also provides a kind of preparation method of the airsetting glue transition metal oxide material of size adjustable, packets
It includes:
(1) it is add to deionized water borax and glucose to form solution, solution is placed in baking oven and is reacted, obtain carbon
Gel；Carbon gel detergent is dry, obtain carbon aerogels；
(2) by step (1) carbon aerogels and transition metal acetate be added in ethylene glycol, carry out solvent heat it is anti-
It answers, obtained solution filtering and washing is dry, obtain the carbon aerogels for being adsorbed with transition metal；Wherein, carbon aerogels, transition gold
Belong to acetate, the mass ratio of ethylene glycol is 1:1:100-120；
(3) by step (2) be adsorbed with transition metal carbon aerogels carry out high-temperature process to get.
Borax, glucose in the step (1) and the mass ratio of deionized water are 1:5-100:5-100.
Oven temperature in the step (1) is 160-200 DEG C, reaction time 6-10h.
Carbon gel is successively washed using water and ethyl alcohol in the step (1)；Drying temperature is 80 DEG C.
Transition metal acetate in the step (2) is ferric acetate, cobalt acetate, nickel acetate or manganese acetate.
Solvent thermal reaction in the step (2) specifically: 10-15h is reacted at 110-130 DEG C, at 160-180 DEG C
React 1-3h.
Drying in the step (2) specifically: vacuumized under the conditions of 80 DEG C.
High-temperature process temperature in the step (3) is 400-600 DEG C, and the high-temperature process time is 3-5h.
Beneficial effect
Size adjustable of the present invention；Preparation process is environmentally friendly, easily operated, and raw material is simple and easy to get, and method is common to transition metal,
It has a good application prospect.
Detailed description of the invention
Fig. 1-4 is the SEM figure of the airsetting glue transition metal oxide material of embodiment 1-4 preparation respectively；
Fig. 5 a-b is the SEM figure of the airsetting glue transition metal oxide material of embodiment 5-6 preparation respectively；
Fig. 6 a is the XRD diagram of airsetting glue transition metal oxide material prepared by embodiment 1,5,6；
Fig. 6 b-d is the XRD diagram of the airsetting glue transition metal oxide material of embodiment 2-4 preparation respectively.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) borax and glucose are add to deionized water with the mass ratio of 1:26, wherein borax and deionized water
Mass ratio is 1:30, and solution is placed in 180 DEG C of baking oven reaction 8h, prepares carbon gel；
(2) carbon gel is successively washed with water and ethyl alcohol respectively and is dried to obtain carbon aerogels in 80 DEG C of baking ovens；
(3) carbon aerogels and cobalt acetate are added in ethylene glycol, solvent thermal reaction 14h, wherein successively anti-at 120 DEG C
12h is answered, reacts 2h at 170 DEG C；
(4) in the solution filtering and washing of step (3) preparation and vacuum drying under the conditions of at 80 DEG C, transition has been adsorbed
The carbon aerogels of metal；
(5) sample that step (4) obtains is subjected to 500 DEG C of high-temperature process 4h in air, obtains airsetting glue transition gold
Belong to oxide material, is denoted as Co3O4-1。
Embodiment 2
Difference from example 1 is that: step (3) cobalt acetate changes ferric acetate preparation airsetting glue oxo transition metal into
Compound material, is denoted as Fe2O3。
Embodiment 3
Difference from example 1 is that: step (3) cobalt acetate changes nickel acetate preparation airsetting glue oxo transition metal into
Compound material, is denoted as NiO.
Embodiment 4
Difference from example 1 is that: step (3) cobalt acetate changes manganese acetate preparation airsetting glue oxo transition metal into
Compound material, is denoted as Mn3O4。
Embodiment 5
Difference from example 1 is that: the mass ratio of step (1) borax, glucose and water is changed to 1:65:75 preparation
Airsetting glue transition metal oxide material, is denoted as Co3O4-2。
Embodiment 6
Difference from example 1 is that: the mass ratio of step (3) borax, glucose and water is changed to 1:9:11 preparation
Airsetting glue transition metal oxide material, is denoted as Co3O4-3。
The airsetting glue transition metal that embodiment 1-6 is prepared is characterized using scanning electron microscope (SEM), XRD
The pattern and chemical composition of oxide material, result are as follows:
(1) SEM test result (Fig. 1-4) shows: the airsetting glue oxo transition metal for the different transition metal being prepared
The microscopic appearance that compound material is presented is similar, is mutually to be accumulated and connected by the spheric granules of 20 rans, forms three
The network of dimension.
(2) SEM test result (Fig. 5 a-b) shows: the airsetting glue cobaltosic oxide material being prepared as the result is shown,
By changing borax, glucose and the ratio of water, the size of spheric granules is successfully regulated and controled, and with borax content
It reducing, the diameter of particle increases to 45 rans, and the borax ratio of addition is reduced, and the diameter of particle becomes smaller as 15nm or so,
Demonstrate the size adjustable of airsetting glue transition metal oxide material.
(3) XRD test result (Fig. 6 a-d) shows: the material characteristics diffraction maximum of preparation respectively with corresponding metal oxide
Standard card it is corresponding, illustrate to be successfully prepared airsetting glue transition metal oxide material, the preparation method to iron, cobalt,
Several transition metal of nickel, manganese are general.
Claims (9)
1. a kind of airsetting glue transition metal oxide material of size adjustable, it is characterised in that: using carbon aerogels as template, lead to
It crosses solvent thermal reaction and completes the cladding of transition metal, then obtained through high-temperature process.
2. a kind of preparation method of the airsetting glue transition metal oxide material of size adjustable, comprising:
(1) it is add to deionized water borax and glucose to form solution, solution is placed in baking oven and is reacted, it is solidifying to obtain carbon
Glue；Carbon gel detergent is dry, obtain carbon aerogels；
(2) by step (1) carbon aerogels and transition metal acetate be added in ethylene glycol, carry out solvent thermal reaction, will
Obtained solution filtering and washing is dry, obtains the carbon aerogels for being adsorbed with transition metal；Wherein, carbon aerogels, transition metal vinegar
Hydrochlorate, ethylene glycol mass ratio be 1:1:100-120；
(3) by step (2) be adsorbed with transition metal carbon aerogels carry out high-temperature process to get.
3. preparation method according to claim 2, it is characterised in that: borax, glucose in the step (1) and go from
The mass ratio of sub- water is 1:5-100:5-100.
4. preparation method according to claim 2, it is characterised in that: the oven temperature in the step (1) is 160-200
DEG C, reaction time 6-10h.
5. preparation method according to claim 2, it is characterised in that: carbon gel uses water and ethyl alcohol in the step (1)
Successively wash；Drying temperature is 80 DEG C.
6. preparation method according to claim 2, it is characterised in that: the transition metal acetate in the step (2) is
Ferric acetate, cobalt acetate, nickel acetate or manganese acetate.
7. preparation method according to claim 2, it is characterised in that: the solvent thermal reaction in the step (2) specifically:
10-15h is reacted at 110-130 DEG C, reacts 1-3h at 160-180 DEG C.
8. preparation method according to claim 2, it is characterised in that: the drying in the step (2) specifically: 80 DEG C of items
It is vacuumized under part.
9. preparation method according to claim 2, it is characterised in that: the high-temperature process temperature in the step (3) is
400-600 DEG C, the high-temperature process time is 3-5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811496150.0A CN109292832A (en) | 2018-12-07 | 2018-12-07 | A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811496150.0A CN109292832A (en) | 2018-12-07 | 2018-12-07 | A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof |
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| CN109292832A true CN109292832A (en) | 2019-02-01 |
Family
ID=65142789
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| CN201811496150.0A Pending CN109292832A (en) | 2018-12-07 | 2018-12-07 | A kind of airsetting glue transition metal oxide material of size adjustable and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109806872A (en) * | 2019-03-12 | 2019-05-28 | 东华大学 | A kind of application of three-dimensional carbon doped cobaltic-cobaltous oxide material |
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Application publication date: 20190201 |