CN107970960A - A kind of preparation method of MoP, FeP, redox graphene three-phase composite material - Google Patents
A kind of preparation method of MoP, FeP, redox graphene three-phase composite material Download PDFInfo
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- CN107970960A CN107970960A CN201711231175.3A CN201711231175A CN107970960A CN 107970960 A CN107970960 A CN 107970960A CN 201711231175 A CN201711231175 A CN 201711231175A CN 107970960 A CN107970960 A CN 107970960A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 49
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000002604 ultrasonography Methods 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 17
- 239000002243 precursor Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- -1 sodium hypophosphites Chemical class 0.000 claims description 10
- 230000004224 protection Effects 0.000 claims description 8
- 238000009413 insulation Methods 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 238000011144 upstream manufacturing Methods 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 5
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims description 4
- 239000011574 phosphorus Substances 0.000 claims description 4
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims description 3
- 239000011733 molybdenum Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims 2
- 239000010439 graphite Substances 0.000 claims 2
- 239000000243 solution Substances 0.000 description 13
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000010802 sludge Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004502 linear sweep voltammetry Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- RTQMYJXQIDQHMH-UHFFFAOYSA-N iron;propan-2-one Chemical compound [Fe].CC(C)=O RTQMYJXQIDQHMH-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/188—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with chromium, molybdenum, tungsten or polonium
- B01J27/19—Molybdenum
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/28—Phosphorising
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
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Abstract
A kind of preparation method of MoP, FeP, redox graphene three-phase composite material, it is characterized in that, ferric acetyl acetonade and acetyl acetone are loaded on graphene oxide, as presoma, MoP, FeP, redox graphene three-phase composite material are obtained by the interior phosphatization of high temperature, short time.
Description
Technical field
The present invention relates to the preparing technical field of nano material, particularly a kind of MoP, FeP, redox graphene three-phase
The preparation method of composite material, and its application in terms of electro-catalysis hydrolyzes production hydrogen.
Background technology
Cleaning and regenerative resource there is an urgent need to promoted electrolysis aquatic products hydrogen catalyst exploration.Recently, transition metal
Phosphide (TMP) is had proved to be with high activity, the HER catalyst of high stability, and not only in strongly acidic solution, and
And in for strong basicity and neutral medium, there is the faradic efficiency close to 100%.Largely research shows, nano hybridization
The advantages of thing can combine each component as catalyst, and cooperative effect is produced in heterogeneous interface, greatly improve catalysis
H2-producing capacity.Therefore the preparation of nano-complex is increasingly paid attention to be subject to research staff.But traditional phosphating sludge preparation side
Method is cumbersome, and required phosphatization temperature higher (>=850 DEG C), time length (>=5h), obtained phosphating sludge sinters substantially, catalytic activity drop
It is low.Therefore it is most important to find a kind of preparation method of suitable phosphating sludge and phosphating sludge compound.Oxidation is utilized in the present invention
The peptizaiton that reduced graphene plays, is prepared for MoP, FeP, redox graphene three-phase composite material.
The content of the invention
In order to overcome the drawbacks described above of the prior art, the present invention provides a kind of MoP, FeP, redox graphene three-phase
The preparation method of composite material.
A kind of MoP, FeP of the present invention, the preparation method of redox graphene three-phase composite material use following technology
Scheme：
The preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, load second on graphene oxide
Acyl acetone iron and acetyl acetone, as presoma, MoP, FeP, redox stone are obtained by the interior phosphatization of high temperature, short time
Black alkene three-phase composite material.
The preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, comprise the following steps：
(1) a certain amount of acetyl acetone and ferric acetyl acetonade are dissolved in a certain amount of ethanol, after by a certain amount of oxidation
Graphene dispersion is in above-mentioned solution；
(2) take part steps (1) to obtain sample, be placed on the graphene oxide-loaded acetyl obtained in baking oven after 80 DEG C of drying
Acetone iron and acetylacetone,2,4-pentanedione molybdenum composite material are as presoma；
(3) sample for obtaining step (2) is placed in tube furnace with a certain amount of sodium hypophosphite and carries out phosphatization；
(4) take samples with water and ethanol after phosphatization to rinse repeatedly several times, then dry.
Further, the adding proportion of acetyl acetone and ferric acetyl acetonade is mass ratio 1-2 in step (1)：1-2.
Further, in step (3), 750 DEG C -850 DEG C of phosphatization temperature, phosphorus China's time 1h.
The preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, comprise the following steps：150mg second
Acyl acetone iron and 150mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then disperses 100mg graphene oxides
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure, obtain compound
Presoma, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, 100mg is above-mentioned multiple
Compound presoma is placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-1.5h, heating speed
Spend for 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
The preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, comprise the following steps：100mg second
Acyl acetone iron and 200mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then disperses 100mg graphene oxides
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure, obtain compound
Presoma, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, 100mg is above-mentioned multiple
Compound presoma is placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-1.5h, heating speed
Spend for 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
The preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, comprise the following steps：200mg second
Acyl acetone iron and 100mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then disperses 100mg graphene oxides
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure, obtain compound
Presoma, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, 100mg is above-mentioned multiple
Compound presoma is placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-1.5h, heating speed
Spend for 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
MoP, FeP prepared by the present invention, redox graphene composite material, can complete phosphorus in the low temperature shorter time
Change, and the addition of redox graphene can effectively prevent the particle aggregation of phosphide.The MoP of the method for the present invention preparation,
FeP, redox graphene, can be used as the electro-catalysis production hydrogen catalyst of excellent performance, with higher catalytic activity and well
Stability.MoP, FeP, the redox graphene of the method for the present invention preparation can be synthesized largely, it is not necessary to expensive device, can be extensive
Hydrogen catalyst is produced for electro-catalysis.
Brief description of the drawings
Fig. 1 is MoP, FeP, the XRD analysis figure of redox graphene.
Fig. 2 is three electrode test case study on implementation, six MoP, FeP, redox graphene three-phase composite material electro-catalysis production hydrogen
The linear sweep voltammetry curve of performance.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
Personnel's all other embodiments obtained on the premise of without creative work, belong to the scope of protection of the invention.
A kind of MoP, FeP of the present invention, the preparation method of redox graphene three-phase composite material, first in oxidation stone
Ferric acetyl acetonade and acetyl acetone are loaded on black alkene, as presoma, by the interior phosphatization of high temperature, short time obtain MoP,
FeP, redox graphene three-phase composite material.
Proposed by the present invention is MoP, FeP, the preparation method of redox graphene three-phase composite material, including following step
Suddenly：
1. a certain amount of acetyl acetone and ferric acetyl acetonade are dissolved in a certain amount of ethanol, after by a certain amount of oxidation stone
Black alkene is dispersed in above-mentioned solution.Preferably, its optimal preparation method is：The adding proportion of acetyl acetone and ferric acetyl acetonade is
1:1 (mass ratio).
2. taking part steps 1 to obtain sample is placed on the graphene oxide-loaded acetylacetone,2,4-pentanedione obtained in baking oven after 80 DEG C of drying
Iron and acetylacetone,2,4-pentanedione molybdenum composite material are as presoma.
3. the sample that step 2 is obtained is placed in tube furnace with a certain amount of sodium hypophosphite and carries out phosphatization, it is preferred that it is most
Good preparation method is：800 DEG C of phosphatization temperature, phosphorus China's time 1h.
4. taking samples with water and ethanol after phosphatization to rinse repeatedly several times, then dry.
Compared with existing MoP, it is an advantage of the invention that in lower temperature (750-850 DEG C) and short period (0.5-1.5h)
Interior completion phosphatization, obtains MoP, FeP redox redox graphene.This MoP, FeP, redox grapheme material tool
There is superior electrolysis water H2-producing capacity.When this material is attached in rotating disk electrode (r.d.e) with 0.3mg/cm2, overpotential is
During 180mV, current density can reach 30mA/cm2.
Specific embodiment：
As shown in Figure 1, it is MoP, FeP, the XRD analysis figure of redox graphene.
Embodiment one：150mg ferric acetyl acetonades and 150mg acetyl acetones are dissolved in 30ml ethanol, ultrasound 30 minutes, so
100mg graphene oxides are distributed to above-mentioned solution afterwards, ultrasound 30 minutes, transfers the solution into 80 DEG C of baking ovens after ultrasound exposure
In 24 it is small when dry, obtain compound precursor.Room temperature is subsequently cooled to, collects product.
Sodium hypophosphite (1.0g) is placed in the upstream side of tube furnace, above-mentioned compound precursor (100mg) is placed in another
Downstream in a porcelain boat, by sample in 750 DEG C of heating and thermal insulation 0.5h, firing rate is 3 DEG C/min.Then under Ar2 protections certainly
So it is cooled to room temperature.
Embodiment two：In precursor synthesis：100mg ferric acetyl acetonades and 200mg acetyl acetones are dissolved in 30ml ethanol
In, ultrasound 30 minutes, is then distributed to above-mentioned solution, ultrasound 30 minutes after ultrasound exposure will be molten by 100mg graphene oxides
Liquid is transferred to when 24 is small in 80 DEG C of baking ovens and dries, and obtains compound precursor.Other processing are the same as implementation example one.
Embodiment three：In precursor synthesis：200mg ferric acetyl acetonades and 100mg acetyl acetones are dissolved in 30ml ethanol
In, ultrasound 30 minutes, is then distributed to above-mentioned solution, ultrasound 30 minutes after ultrasound exposure will be molten by 100mg graphene oxides
Liquid is transferred to when 24 is small in 80 DEG C of baking ovens and dries, and obtains compound precursor.Other processing are the same as implementation example one.
Example IV：Phosphatization temperature is arranged to 800 DEG C, other processing are the same as implementation example one.
Embodiment five：Phosphatization temperature is arranged to 850 DEG C, other processing are the same as implementation example one.
Embodiment six：Phosphatization temperature soaking time is arranged to 1h, other processing are the same as implementation example four.As shown in Fig. 2, it is
Three electrode test MoP, FeP, the linear sweep voltammetry of redox graphene three-phase composite material electro-catalysis H2-producing capacity are bent
Line.
Embodiment seven：Phosphatization temperature soaking time is arranged to 1.5h, other processing are the same as implementation example four.
It should be understood that although with reference to its exemplary embodiment, particularly shown and description is carried out to the present invention,
It should be understood by those skilled in the art that without departing substantially from by spirit of the invention as defined in the claims and model
Under conditions of enclosing, the change of various forms and details can be carried out wherein, can carry out any combination of various embodiments.
Claims (7)
1. the preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, it is characterised in that in graphite oxide
Ferric acetyl acetonade and acetyl acetone are loaded on alkene, as presoma, by the interior phosphatization of high temperature, short time obtain MoP, FeP,
Redox graphene three-phase composite material.
2. the preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, it is characterised in that including following step
Suddenly：
(1) a certain amount of acetyl acetone and ferric acetyl acetonade are dissolved in a certain amount of ethanol, after by a certain amount of graphite oxide
Alkene is dispersed in above-mentioned solution；
(2) take part steps (1) to obtain sample, be placed on the graphene oxide-loaded acetylacetone,2,4-pentanedione obtained in baking oven after 80 DEG C of drying
Iron and acetylacetone,2,4-pentanedione molybdenum composite material are as presoma；
(3) sample for obtaining step (2) is placed in tube furnace with a certain amount of sodium hypophosphite and carries out phosphatization；
(4) take samples with water and ethanol after phosphatization to rinse repeatedly several times, then dry.
3. the preparation method of a kind of MoP, FeP according to claim 2, redox graphene three-phase composite material, its
It is characterized in that：The adding proportion of acetyl acetone and ferric acetyl acetonade is mass ratio 1-2 in step (1)：1-2.
4. the preparation method of a kind of MoP, FeP according to claim 2, redox graphene three-phase composite material, its
It is characterized in that：In step (3), 750 DEG C -850 DEG C of phosphatization temperature, phosphorus China's time 1h.
5. the preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, it is characterised in that including following step
Suddenly：150mg ferric acetyl acetonades and 150mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then aoxidizes 100mg
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure graphene dispersion,
Compound precursor is obtained, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, will
The above-mentioned compound precursors of 100mg are placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-
1.5h, firing rate are 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
6. the preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, it is characterised in that including following step
Suddenly：100mg ferric acetyl acetonades and 200mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then aoxidizes 100mg
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure graphene dispersion,
Compound precursor is obtained, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, will
The above-mentioned compound precursors of 100mg are placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-
1.5h, firing rate are 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
7. the preparation method of a kind of MoP, FeP, redox graphene three-phase composite material, it is characterised in that including following step
Suddenly：200mg ferric acetyl acetonades and 100mg acetyl acetones are dissolved in 30ml ethanol, and ultrasound 30 minutes, then aoxidizes 100mg
To above-mentioned solution, ultrasound 30 minutes, transfers the solution into dried when 24 is small in 80 DEG C of baking ovens after ultrasound exposure graphene dispersion,
Compound precursor is obtained, is subsequently cooled to room temperature, collects product；1.0g sodium hypophosphites are placed in the upstream side of tube furnace, will
The above-mentioned compound precursors of 100mg are placed in the downstream in another porcelain boat, by sample in 750 DEG C of -850 DEG C of heating and thermal insulation 0.5h-
1.5h, firing rate are 3 DEG C/min, then the cooled to room temperature under Ar2 protections.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108654659A (en) * | 2018-05-11 | 2018-10-16 | 重庆文理学院 | A kind of phosphating sludge/graphene composite nano material and preparation method thereof |
| CN111211309A (en) * | 2020-01-17 | 2020-05-29 | 上海应用技术大学 | Phosphorus-doped graphene-coated iron oxide composite material and preparation method and application thereof |
| CN113072044A (en) * | 2021-03-25 | 2021-07-06 | 安徽师范大学 | Core-shell structure FeP nano-chain, preparation method thereof and application thereof in battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108654659A (en) * | 2018-05-11 | 2018-10-16 | 重庆文理学院 | A kind of phosphating sludge/graphene composite nano material and preparation method thereof |
| CN111211309A (en) * | 2020-01-17 | 2020-05-29 | 上海应用技术大学 | Phosphorus-doped graphene-coated iron oxide composite material and preparation method and application thereof |
| CN113072044A (en) * | 2021-03-25 | 2021-07-06 | 安徽师范大学 | Core-shell structure FeP nano-chain, preparation method thereof and application thereof in battery |
| CN113072044B (en) * | 2021-03-25 | 2022-06-21 | 安徽师范大学 | Core-shell structure FeP nano-chain, preparation method thereof and application thereof in battery |
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