CN107230559A - A kind of preparation method of porous oxidation cerium composite - Google Patents
A kind of preparation method of porous oxidation cerium composite Download PDFInfo
- Publication number
- CN107230559A CN107230559A CN201710507135.0A CN201710507135A CN107230559A CN 107230559 A CN107230559 A CN 107230559A CN 201710507135 A CN201710507135 A CN 201710507135A CN 107230559 A CN107230559 A CN 107230559A
- Authority
- CN
- China
- Prior art keywords
- aqueous solution
- nitrate aqueous
- template
- preparation
- porous
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 27
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 230000003647 oxidation Effects 0.000 title claims abstract description 19
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 62
- 239000011259 mixed solution Substances 0.000 claims abstract description 45
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 26
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 19
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 19
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 13
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 13
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 13
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000010792 warming Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- 239000011572 manganese Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 description 18
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 4
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003643 water by type Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- 238000001069 Raman spectroscopy Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000007772 electrode material Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacturing & Machinery (AREA)
Abstract
The invention discloses a kind of preparation method of porous oxidation cerium composite, specifically implement according to following steps：Step 1, the template aqueous solution is prepared；Step 2, the ammonium ceric nitrate aqueous solution is prepared respectively and manganese nitrate aqueous solution is prepared, and then the ammonium ceric nitrate aqueous solution and manganese nitrate aqueous solution are mixed, mixed solution A is obtained；Step 3, the template aqueous solution made from step 1 is added in mixed solution made from step 2, stirs 1h 5h, obtain mixed solution B；Step 4, the mixed solution B that step 3 is obtained is washed, it is then placed in baking oven and is dried at a temperature of 30 DEG C 80 DEG C, dried product is warming up to calcining 2h 6h at 500 DEG C 800 DEG C with 1 DEG C/min, 10 DEG C/min heating rate under an argon atmosphere, porous C eO is obtained2/ MnO/C composites.The present invention is prepared for porous C eO using sodium carboxymethylcellulose as template using template2/ MnO/C composites, preparation technology is simple, cost is low, reaction temperature and reaction time are easy to control.
Description
Technical field
The invention belongs to composite material and preparation method thereof technical field, it is related to a kind of preparation side of porous oxidation cerium composite
Method.
Background technology
CeO2With good redox characteristic, but electric conductivity and structural stability are poor.Work as Ce4+It is reduced to Ce3+When, always
It is can occur lattice dilatation.Therefore, CeO is used alone2It is not fine as performance during electrode material.Have well to prepare
Capacitive property, high rate performance, the high-performance super capacitor of energy density and cyclical stability, by CeO2With carbon material or its
He combines metal oxide.Transition metal oxide MnO has cost low, environment-friendly, the advantages of theoretical specific capacity is high, is one
Plant the material with good chemical property.And existing experimental method is all simply by CeO2It is combined, and is prepared with MnO
The manganese oxide gone out is all the manganese oxide of multivalent state, also not simultaneously by CeO2, the preparation method that is combined of MnO and C, due to
The good conductivity of carbon material, can compensate for CeO2Defect.Therefore, it is of the invention by CeO2, MnO combined to manufacture high property with C
Can electrode material for super capacitor.Composite is prepared into porous pattern, then can increase the specific surface area of material, so as to enter
One step improves the chemical property of material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of porous oxidation cerium composite, the compound of porous pattern is made
Material, chemical property is good.
The technical solution adopted in the present invention is, a kind of preparation method of porous oxidation cerium composite, specifically according to
Lower step is implemented：
Step 1, the template aqueous solution is prepared；
Step 2, the ammonium ceric nitrate aqueous solution is prepared respectively and manganese nitrate aqueous solution is prepared, then by the ammonium ceric nitrate aqueous solution and
Manganese nitrate aqueous solution is mixed, and obtains mixed solution A；
Step 3, the template aqueous solution made from step 1 is added in mixed solution made from step 2, stirs 1h-5h,
Obtain mixed solution B；
Step 4, the mixed solution B that step 3 is obtained is washed, be then placed in baking oven at a temperature of 30 DEG C -80 DEG C
Drying, 500 DEG C -800 DEG C are warming up to by dried product with 1 DEG C/min-10 DEG C/min heating rate under an argon atmosphere
Lower calcining 2h-6h, obtains porous C eO2/ MnO/C composites.
The features of the present invention is also resided in,
Template in step 1 is that the concentration of the template aqueous solution is 1%-5% from sodium carboxymethylcellulose.
The concentration of the ammonium ceric nitrate aqueous solution is 0.0005mol/L-0.0015mol/L in step 2.
The concentration of manganese nitrate aqueous solution is 0.0005mol/L-0.0015mol/L in step 2.
The ammonium ceric nitrate aqueous solution and manganese nitrate aqueous solution mixed volume ratio in step 2 are 1-3：1-3.
The template aqueous solution and the mixed volume of mixed solution A ratio are 1-3 in step 3：1-3.
The cleaning solution that washing in step 4 is used is deionized water.
The beneficial effects of the invention are as follows the present invention is prepared for many using sodium carboxymethylcellulose as template using template
Hole CeO2/ MnO/C composites, preparation technology is simple, cost is low, reaction temperature and reaction time are easy to control, product electric conductivity
It is good with structural stability.
Brief description of the drawings
Fig. 1 is the porous C eO obtained by a kind of preparation method embodiment 1 of porous oxidation cerium composite of the invention2/
The XRD spectra of MnO/C composites；
Fig. 2 is the porous C eO obtained by a kind of preparation method embodiment 2 of porous oxidation cerium composite of the invention2/
The Raman collection of illustrative plates of MnO/C composites；
Fig. 3 is the porous C eO obtained by a kind of preparation method embodiment 3 of porous oxidation cerium composite of the invention2/
The SEM photograph of MnO/C composites；
Fig. 4 is the porous C eO obtained by a kind of preparation method embodiment 4 of porous oxidation cerium composite of the invention2/
The TEM photos of MnO/C composites；
Fig. 5 is the porous C eO obtained by a kind of preparation method embodiment 5 of porous oxidation cerium composite of the invention2/
MnO/C composites are used for the cyclical stability figure of ultracapacitor.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of porous oxidation cerium composite of the present invention, specifically implements according to following steps：
Step 1, compound concentration is used as the template aqueous solution for 1%-5% from sodium carboxymethyl cellulose solution.
Step 2, compound concentration is the 0.0005mol/L-0.0015mol/L ammonium ceric nitrate aqueous solution and compound concentration respectively
For 0.0005mol/L-0.0015mol/L manganese nitrate aqueous solution, then the ammonium ceric nitrate aqueous solution and manganese nitrate aqueous solution are pressed
It is 1-3 according to volume ratio：1-3 is mixed, and obtains mixed solution A；
Step 3, it is 1-3 according to volume ratio by mixed solution A made from the template aqueous solution made from step 1 and step 2：
1-3 is mixed, and is stirred 1h-5h, is obtained mixed solution B；
Step 4, the mixed solution B that step 3 is obtained is washed using deionized water, be then placed in baking oven 30
Dried at a temperature of DEG C -80 DEG C, dried product is heated up with 1 DEG C/min-10 DEG C/min heating rate under an argon atmosphere
2h-6h is calcined to 500 DEG C -800 DEG C, porous C eO is obtained2/ MnO/C composites.
The present invention uses 50% manganese nitrate in manganese nitrate aqueous solution.
Embodiment 1
Compound concentration is used as template for 1% sodium carboxymethyl cellulose solution；Another compound concentration is 0.0008mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.0008mol/L；Then it is 0.0008mol/L nitre to take 10L concentration
Sour cerium aqueous ammonium and 10L concentration mix for 0.0008mol/L manganese nitrate aqueous solution, obtain mixed solution A；Take 10L templates
The agent aqueous solution is added in mixed solution A, then stirs 1h, obtains mixed solution B；By the mixed solution B being stirred spend from
Sub- water washing, is then placed in baking oven and is dried at a temperature of 40 DEG C, by gained sample under an argon atmosphere with 2 DEG C/min after drying
Heating rate, 2h is calcined at 500 DEG C, that is, obtains porous C eO2/ MnO/C composites.
As shown in figure 1, the porous C eO obtained by embodiment 12The XRD spectra of/MnO/C composites, can be with from Fig. 1
See that prepared sample has CeO really2And MnO.
Embodiment 2
Compound concentration is used as template for 1% sodium carboxymethyl cellulose solution；Another compound concentration is 0.001mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.001mol/L；Then it is 0.001mol/L nitric acid to take 10L concentration
Cerium aqueous ammonium and 20L concentration mix for 0.001mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 10L template water
Solution is added in mixed solution A, when then stirring 2h, obtains mixed solution B；By the mixed solution B deionizations being stirred
Water washing；It is then placed in baking oven and is dried at a temperature of 40 DEG C, by gained sample under an argon atmosphere with 3 DEG C/min's after dries
Heating rate, calcines 4h at 500 DEG C, that is, obtains porous C eO2/ MnO/C composites.
As shown in Fig. 2 being the porous C eO obtained by embodiment 22The Raman collection of illustrative plates of/MnO/C composites, from Fig. 2
It can be seen that prepared sample strictly CeO2/ MnO/C composite.
Embodiment 3
Compound concentration is used as template for 2% sodium carboxymethyl cellulose solution；Another compound concentration is 0.001mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.0005mol/L；Then it is 0.001mol/L nitric acid by 10L concentration
Cerium aqueous ammonium and 30L concentration mix for 0.0005mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 30L templates
The aqueous solution is added in mixed solution A, then stirs 1h；The mixed solution being stirred is washed with deionized；It is then placed in
Dried in baking oven at a temperature of 80 DEG C, by gained sample under an argon atmosphere with 5 DEG C/min heating rate after drying, 800
3h is calcined at DEG C, that is, obtains porous C eO2/ MnO/C composites.
As shown in figure 3, being the porous C eO obtained by embodiment 32The SEM photograph of/MnO/C composites, can from Fig. 3
To see that prepared material is porous pattern.
Embodiment 4
Compound concentration is used as template for 3% sodium carboxymethyl cellulose solution；Another compound concentration is 0.0005mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.001mol/L；Then it is 0.0005mol/L nitric acid by 30L concentration
Cerium aqueous ammonium and 10L concentration mix for 0.001mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 40L template water
Solution is added in mixed solution A, then stirs 5h, obtains mixed solution B；By the mixed solution B deionized waters being stirred
Washing；It is then placed in baking oven and is dried at a temperature of 60 DEG C, by gained sample under an argon atmosphere with 5 DEG C/min liter after dries
Warm speed, calcines 6h at 600 DEG C, that is, obtains porous C eO2/ MnO/C composites.
As shown in figure 4, being the porous C eO obtained by embodiment 42The TEM photos of/MnO/C composites, enter from Fig. 4
One step can determine that prepared material is loose structure.
Embodiment 5
Compound concentration is used as template for 5% sodium carboxymethyl cellulose solution；Another compound concentration is 0.0005mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.0015mol/L；Then it is 0.0005mol/L nitre by 20L concentration
Sour cerium aqueous ammonium and 10L concentration mix for 0.0015mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 60L templates
The agent aqueous solution is added in mixed solution A, then stirs 1h, mixed solution B；By the mixed solution B deionized waters being stirred
Washing；It is then placed in baking oven and is dried at a temperature of 40 DEG C, by gained sample under an argon atmosphere with 6 DEG C/min liter after dries
Warm speed, calcines 3h at 700 DEG C, that is, obtains porous C eO2/ MnO/C composites.
As shown in figure 5, being the porous C eO obtained by embodiment 52/ MnO/C composites are used for the circulation of ultracapacitor
Stability diagram, shows that prepared composite has good chemical property according to cyclical stability figure.
Embodiment 6
Compound concentration is used as template for 3% sodium carboxymethyl cellulose solution；Another compound concentration is 0.0015mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.001mol/L；Then it is 0.0015mol/L nitric acid by 20L concentration
Cerium aqueous ammonium and 30L concentration mix for 0.001mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 40L template water
Solution is added in mixed solution A, then stirs 3h, obtains mixed solution B；By the mixed solution B deionized waters being stirred
Washing；It is then placed in baking oven and is dried at a temperature of 30 DEG C, by gained sample under an argon atmosphere with 10 DEG C/min's after dries
Heating rate, calcines 3h at 600 DEG C, that is, obtains porous C eO2/ MnO/C composites.
Embodiment 7
Compound concentration is used as template for 5% sodium carboxymethyl cellulose solution；Another compound concentration is 0.0005mol/L
The ammonium ceric nitrate aqueous solution and the manganese nitrate aqueous solution that concentration is 0.0015mol/L；Then it is 0.0005mol/L nitre by 10L concentration
Sour cerium aqueous ammonium and 10L concentration mix for 0.0015mol/L manganese nitrate aqueous solution, obtain mixed solution A；By 60L templates
The agent aqueous solution is added in mixed solution A, then stirs 3h, mixed solution B；By the mixed solution B deionized waters being stirred
Washing；It is then placed in baking oven and is dried at a temperature of 50 DEG C, by gained sample under an argon atmosphere with 1 DEG C/min liter after dries
Warm speed, calcines 5h at 800 DEG C, that is, obtains porous C eO2/ MnO/C composites.
Cerium source and manganese source are directly mixed using sodium carboxymethylcellulose as template, pass through the step system of template one by the present invention
There must be the CeO of porous pattern2/ MnO/C composites, utilize the huge specific surface area of loose structure and the good conduction of carbon
Property, it can apply in fields such as ultracapacitors.
Claims (7)
1. a kind of preparation method of porous oxidation cerium composite, it is characterised in that specifically implement according to following steps：
Step 1, the template aqueous solution is prepared；
Step 2, the ammonium ceric nitrate aqueous solution is prepared respectively and manganese nitrate aqueous solution is prepared, then by the ammonium ceric nitrate aqueous solution and nitric acid
The manganese aqueous solution is mixed, and obtains mixed solution A；
Step 3, the template aqueous solution made from step 1 is added in mixed solution made from step 2, stirs 1h-5h, obtain
Mixed solution B；
Step 4, the mixed solution B that step 3 is obtained is washed, is then placed in baking oven and is dried at a temperature of 30 DEG C -80 DEG C,
Dried product is warming up at 500 DEG C -800 DEG C with 1 DEG C/min-10 DEG C/min heating rate under an argon atmosphere and calcined
2h-6h, obtains porous C eO2/ MnO/C composites.
2. the preparation method of a kind of porous oxidation cerium composite according to claim 1, it is characterised in that in step 1
Described template is that the concentration of the template aqueous solution is 1%-5% from sodium carboxymethylcellulose.
3. a kind of preparation method of porous oxidation cerium composite according to claim 2, it is characterised in that the step
The concentration of the ammonium ceric nitrate aqueous solution is 0.0005mol/L-0.0015mol/L in 2.
4. a kind of preparation method of porous oxidation cerium composite according to claim 3, it is characterised in that the step
The concentration of manganese nitrate aqueous solution is 0.0005mol/L-0.0015mol/L in 2.
5. the preparation method of a kind of porous oxidation cerium composite according to claim 4, it is characterised in that in step 2
The described ammonium ceric nitrate aqueous solution and manganese nitrate aqueous solution mixed volume ratio are 1-3：1-3.
6. a kind of preparation method of porous oxidation cerium composite according to claim 5, it is characterised in that the step
The template aqueous solution and the mixed volume of mixed solution A ratio are 1-3 in 3：1-3.
7. the preparation method of a kind of porous oxidation cerium composite according to claim 1, it is characterised in that in step 4
The cleaning solution that described washing is used is deionized water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710507135.0A CN107230559B (en) | 2017-06-28 | 2017-06-28 | A kind of preparation method of porous oxidation cerium composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710507135.0A CN107230559B (en) | 2017-06-28 | 2017-06-28 | A kind of preparation method of porous oxidation cerium composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107230559A true CN107230559A (en) | 2017-10-03 |
| CN107230559B CN107230559B (en) | 2018-09-11 |
Family
ID=59935158
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710507135.0A Active CN107230559B (en) | 2017-06-28 | 2017-06-28 | A kind of preparation method of porous oxidation cerium composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107230559B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697799A (en) * | 2019-10-16 | 2020-01-17 | 河南电池研究院有限公司 | Preparation method of porous lithium ion battery anode material |
| CN111151237A (en) * | 2020-01-20 | 2020-05-15 | 云南电网有限责任公司电力科学研究院 | Preparation method of noble metal catalyst |
| CN114939407A (en) * | 2022-07-06 | 2022-08-26 | 四川大学 | Method for synthesizing loose porous manganese oxide and composite oxide thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249952A (en) * | 2008-03-27 | 2008-08-27 | 上海交通大学 | Method for preparing self-doping nitrogen grading porous oxide by using biomass template |
| CN102786094A (en) * | 2012-08-10 | 2012-11-21 | 同济大学 | Preparation method and application of mesoporous manganese oxide material |
| CN102915844A (en) * | 2012-11-09 | 2013-02-06 | 华东理工大学 | Method for preparing different-electrode composite materials of carbon plate/manganese dioxide nanometer sheet and application thereof |
-
2017
- 2017-06-28 CN CN201710507135.0A patent/CN107230559B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101249952A (en) * | 2008-03-27 | 2008-08-27 | 上海交通大学 | Method for preparing self-doping nitrogen grading porous oxide by using biomass template |
| CN102786094A (en) * | 2012-08-10 | 2012-11-21 | 同济大学 | Preparation method and application of mesoporous manganese oxide material |
| CN102915844A (en) * | 2012-11-09 | 2013-02-06 | 华东理工大学 | Method for preparing different-electrode composite materials of carbon plate/manganese dioxide nanometer sheet and application thereof |
Non-Patent Citations (4)
| Title |
|---|
| HUAIHAO ZHANG 等: "Hierarchical porous MnO2 CeO2 with high performance for supercapacitor electrodes", 《CHEMICAL ENGINEERING JOURNAL》 * |
| MUHAMMAD ADIL MANSOOR 等: "Effect of synergic cooperation on optical and photoelectrochemical properties of CeO2–MnO composite thin films", 《NEW J.CHEM.》 * |
| 李兵红 等: "掺CeO2纳米MnO2非对称超级电容器的研究", 《电子元件与材料》 * |
| 李赵华 等: "超级电容器用CeO2/MnO 3D石墨烯复合材料的制备", 《复合材料学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110697799A (en) * | 2019-10-16 | 2020-01-17 | 河南电池研究院有限公司 | Preparation method of porous lithium ion battery anode material |
| CN111151237A (en) * | 2020-01-20 | 2020-05-15 | 云南电网有限责任公司电力科学研究院 | Preparation method of noble metal catalyst |
| CN114939407A (en) * | 2022-07-06 | 2022-08-26 | 四川大学 | Method for synthesizing loose porous manganese oxide and composite oxide thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107230559B (en) | 2018-09-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106185937B (en) | A kind of preparation method of carbon nano-particle/two-dimensional layer carbonization titanium composite material | |
| CN105000886B (en) | A kind of macroscopic three dimensional Fe3O4@graphene aerogels ultra light composite and preparation method | |
| CN107230559B (en) | A kind of preparation method of porous oxidation cerium composite material | |
| CN106219515B (en) | Synthetic method with the empty spherical nitrogen-doped carbon material of special crosslinking | |
| CN105478120A (en) | Preparation method for red mud-based iron-series catalyst and application of red mud-based iron-series catalyst in hydrogen production through cracking of methane | |
| CN103285891B (en) | Preparation method of bismuth oxide halide-titanium oxide nanotube array composite photo-catalytic membrane | |
| CN105161314B (en) | Nano-nickel oxide/nickel/graphene composite material and its preparation method and application | |
| CN108097261B (en) | Efficient and stable iron-manganese composite oxide catalyst and preparation method and application thereof | |
| CN110898794B (en) | Preparation method of lithium ion sieve | |
| CN104692344A (en) | Preparation method of mesoporous graphite-phase carbon nitride material | |
| Venugopal et al. | New α-Zn 2 V 2 O 7/carbon nanotube nanocomposite for supercapacitors | |
| CN107662944A (en) | Nano zircite preparation method | |
| CN103332689A (en) | Preparation method and application of porous graphene nano band | |
| CN109665525A (en) | A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon | |
| CN104307318A (en) | Preparation method of zinc oxide normal-temperature desulfurizing agent | |
| CN105679552A (en) | Thiourea-formaldehyde resin based electrode material of super capacitor and preparation method and application of electrode material | |
| CN103832997A (en) | Graphene/carbon black composite material, preparation method and application thereof | |
| CN105289642A (en) | Method for preparing copper-manganese composite oxide of porous structure | |
| CN109192952A (en) | A kind of cobalt disulfide/carbon nano-fiber composite material and preparation method thereof | |
| CN103738957A (en) | Graphene surface pore-forming method | |
| CN105271438A (en) | Preparation method of magnesium cobaltate porous structure electrode material with double-sea urchin shape | |
| CN105197999B (en) | A kind of Hemicentrotus seu Strongylocentrotus dendroid γ-MnO2preparation method and electro-catalysis application | |
| CN104591118B (en) | A kind of preparation method of three-dimensional shape graphene/carbon nano-tube compounded microbeads | |
| CN104599863B (en) | A kind of method for preparing composite, composite and its application | |
| CN104211052B (en) | Preparation method of porous graphene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210813 Address after: 715299 No. 32, Xichang street, Chengcheng County, Weinan City, Shaanxi Province Patentee after: Chengcheng Haitai Electronic Material Co.,Ltd. Address before: 710021 Shaanxi city of Xi'an province Weiyang University Park Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right |