CN104261411A - Preparation method of graphene-like magnesium silicide nanosheets - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 22
- 239000002135 nanosheet Substances 0.000 title abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 83
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 31
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001354 calcination Methods 0.000 claims abstract description 21
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 49
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 46
- 239000011777 magnesium Substances 0.000 claims description 39
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 19
- 239000007789 gas Substances 0.000 claims description 18
- 235000012239 silicon dioxide Nutrition 0.000 claims description 15
- 125000004494 ethyl ester group Chemical group 0.000 claims description 11
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 11
- 238000007664 blowing Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 19
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 238000002474 experimental method Methods 0.000 description 6
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 229960001866 silicon dioxide Drugs 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of preparation of semiconductor materials, and particularly relates to a preparation method of graphene-like magnesium silicide nanosheets. According to the method, by using graphene oxide as a template and a mixed solution of n-ethyl silicate, ammonia water, distilled water and ethanol as a solvent, a sol-gel process and calcination for template removal are performed to obtain the novel graphene-like magnesium silicide nanosheets.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, particularly the preparation method of a kind graphene-like magnesium silicide nanometer sheet.
Background technology
Magnesium silicide is narrow bandgap semiconductor material, magnesium silicide with its good thermoelectricity mechanical property, very strong resistance to corrosion, arrived the positive regard of investigator.And the abundant raw material of Si, Mg, stratum standing stock are large, cheap, make again him become a kind of potential new structural material.The Application Areas of magnesium silicide is extensive, comprises generating, refrigeration heating, the fields such as semiconductor manufacturing, laser, computer realm and military affairs, aerospace, automobile making and room-mate's chemical industry.Therefore, about the meaning that preparation method's tool of magnesium silicide is important, the particularly material of two-dimensional appearance.
In a large amount of bibliographical informations, all mention that the pattern of semiconductor material can have a huge impact performance, especially laminated structure can make the performance of semiconductor material obtain huge improvement.But the report of current synthesizing magnesium silicide flaky nanometer structure is also deficienter, what some utilization was cut into slices arrives this pattern, but this method is subject to the restriction of technology.Therefore, the magnesium silicide synthesizing a kind of sheet structure is still limited to the method for synthesis and the person's character of material, so, up to the present also there is no synthesis and the application report of class graphene-like magnesium silicide nanometer sheet; This also makes to design novel class graphene-like magnesium silicide nanometer sheet and remains a huge challenge in theoretical investigation and practical application.
Summary of the invention
The object of this invention is to provide the preparation method that a kind of novel class graphene-like magnesium silicide nanometer sheet is easy, the method take graphene oxide as template, the positive ethyl ester of silicic acid, the mixing solutions of ammoniacal liquor, distilled water and ethanol is solvent, utilize sol-gel method, calcining removing template, obtained novel class graphene-like magnesium silicide nanometer sheet material.
The invention provides a kind of preparation method of novel class graphene-like magnesium silicide nanometer sheet, its feature comprises the following steps:
(1) preparation of graphene oxide: the preparation method of this experiment Graphene is a kind of Hummers method of modification, and concrete operations are, a certain amount of admixed graphite, K
2s
2o
8, P
2o
5add vitriol oil a after mixing, after heating certain hour, after washing, filtration drying, obtain preoxidation graphite b; Dried preoxidation graphite and vitriol oil c interacting depth are oxidized, and period adds appropriate KMnO
4, add water and hydrogen peroxide after constant temperature process, finally with dilute hydrochloric acid process remove metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the compound of presoma and graphene oxide: the positive ethyl ester of silicic acid of different amount is dispersed in the mixed solution of ethanol, water and ammoniacal liquor, obtains solution A, graphene oxide is dispersed in water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; Solution C at room temperature stirs the regular hour, obtains SiO after centrifugal, alcohol wash
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, calcined composite D certain hour obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder and SiO by weight
2nanometer sheet mixes, and puts into porcelain crucible E.In tube furnace, use H
2/ Ar gas mixture, as protection gas, is calcined certain hour and is obtained class graphene-like Mg under certain temperature
2si nanometer sheet F, pickling is removed unreacted Mg and is obtained pure phase Mg
2si nanometer sheet G.
In step (1), described admixed graphite, K
2s
2o
8, P
2o
5weight ratio is 1:2:2.
In step (1), the volume of vitriol oil a and the ratio of admixed graphite quality are 6:1(ml:g).
In step (1), described heat-up time is 2 hours, Heating temperature 80 DEG C.
In step (1), the consumption of described vitriol oil c is 10 times of vitriol oil a volume.
In step (1), described KMnO
4be 6:1 ~ 10:1 with the mass ratio of admixed graphite, the volume ratio of hydrogen peroxide and vitriol oil a is 10:3, and the add-on of water is 10 times of hydrogen peroxide volume.
In step (1), described dilute hydrochloric acid is formulated according to volume ratio 1:10 with commercially available concentrated hydrochloric acid (massfraction 36% ~ 38%) and water.
In step (2), in described solution A, the volume ratio of the positive ethyl ester of silicic acid and ethanol, water, ammoniacal liquor is 1:40:4:1 to 10:40:4:1.
In step (2), in described solution B, in every 20-100ml distilled water, add 0.5-1g graphene oxide, the quality of graphene oxide and the positive ethyl ester of silicic acid and volume ratio 1:1 ~ 1:10(g:ml).
In step (2), the time that described solution C at room temperature stirs is 6 ~ 10h.
In step (2), under the condition of described blowing air, calcining temperature is 600 DEG C, and calcination time is 4h.
In step (3), described Mg powder is 200 orders, with SiO
2the weight ratio 4:1 of nanometer sheet.
In step (3), described calcining temperature is 650 DEG C, and temperature rise rate is 3 DEG C/min, and calcination time is 2-3h, and wherein gas mixture is H
2mix according to volume ratio 5:95 with Ar.
In step (3), described pickling refers to adopt dilute hydrochloric acid to carry out pickling, and dilute hydrochloric acid is that 1:10 ~ 1:20 is formulated with commercially available concentrated hydrochloric acid (massfraction 36% ~ 38%) and water according to volume ratio.
Accompanying drawing explanation
The Mg of Fig. 1 prepared by the present invention
2the XRD figure of Si material.
The TEM shape appearance figure of Fig. 2 material prepared by the present invention: a. graphene oxide, b. coated Si O
2after transmission electron microscope picture, c. removes SiO after graphene oxide
2transmission electron microscope picture, d .Mg
2si transmission electron microscope picture.
The Mg synthesized by the present invention can be drawn by the XRD figure of Fig. 1
2the Pdf card of Si number for 35-0733 be a kind of cubic Fm3M (225) structure.
The transmission electron microscope picture of a figure template graphene oxide synthesized by the present invention in Fig. 2, can find the pattern feature of the tulle shape of graphene oxide, can determine the success of Hummer method of modifying used simultaneously; B figure is the transmission electron microscope picture after coated silica, as can be seen from the figure the edge section of material is still the typical feature of graphene oxide, and the coated layer of silicon dioxide of the main part of material, which illustrate sol-gel method used and can be implemented in the coated layer of silicon dioxide of surface of graphene oxide; C figure be remove graphene oxide template after the pattern of silicon-dioxide, the method clearly through air atmosphere calcining can remove graphene oxide template effectively, and the silicon-dioxide removed after template still presents the sheet-like morphology feature of graphene oxide; D figure is at H
2/ Ar gas mixture is under the condition of shielding gas, and Mg simple substance and silicon dioxde reaction generate Mg
2the transmission electron microscope picture of Si, can prove the Mg synthesized by the present invention by figure
2si is the structure of a kind graphene-like.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
embodiment 1:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of Hummers method of modification, and concrete operations are, 1g admixed graphite, 2g K
2s
2o
8, 2g P
2o
5add vitriol oil 6ml after mixing, be heated to 80 DEG C, keep after 2 hours, after washing, filtration drying, obtain preoxidation graphite; Dried preoxidation graphite and 60ml vitriol oil interacting depth are oxidized, and period slowly adds 8g KMnO
4, after constant temperature 80 DEG C process 2h, add 200ml water and 20ml hydrogen peroxide successively; Finally use dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) process remove acid and metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the positive ethyl ester of silicic acid of the compound of presoma and graphene oxide: 1ml is dispersed in the mixed solution of 40ml ethanol, 4ml water and 1ml ammoniacal liquor, obtains solution A, and 1.0g graphene oxide is dispersed in 40ml water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; After solution C at room temperature stirs 6h, after centrifugal, alcohol wash, obtain SiO
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, 600 DEG C of calcined composite D, calcination time is 4h, obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder (200 order) 0.4g and SiO
2nanometer sheet 0.1g mixes, and puts into porcelain crucible E; In tube furnace, use H
2(5%), Ar(95%) gas mixture as protection gas, 650 DEG C calcining 2h, obtain class graphene-like Mg
2si nanometer sheet F, finally uses dilute hydrochloric acid (water: concentrated hydrochloric acid=20:1) to process the unreacted Mg of removal and obtains pure phase G.
embodiment 2:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of Hummers method of modification, and concrete operations are, 1g admixed graphite, 2g K
2s
2o
8, 2g P
2o
5add vitriol oil 6ml after mixing, be heated to 80 DEG C, keep after 2 hours, after washing, filtration drying, obtain preoxidation graphite; Dried preoxidation graphite and 60ml vitriol oil interacting depth are oxidized, and period slowly adds 8g KMnO
4, after constant temperature 80 DEG C process 2h, add 200ml water and 20ml hydrogen peroxide successively; Finally use dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) process remove acid and metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the positive ethyl ester of silicic acid of the compound of presoma and graphene oxide: 2ml is dispersed in the mixed solution of 40ml ethanol, 4ml water and 1ml ammoniacal liquor, obtains solution A, and 0.5g graphene oxide is dispersed in 40ml water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; After solution C at room temperature stirs 6h, after centrifugal, alcohol wash, obtain SiO
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, 600 DEG C of calcined composite D, calcination time is 4h, obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder (200 order) 0.4g and SiO
2nanometer sheet 0.1g mixes, and puts into porcelain crucible E; In tube furnace, use H
2(5%), Ar(95%) gas mixture as protection gas, 650 DEG C calcining 2h, obtain class graphene-like Mg
2si nanometer sheet F, finally uses dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) to process the unreacted Mg of removal and obtains pure phase G.
embodiment 3:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of Hummers method of modification, and concrete operations are, 1g admixed graphite, 2g K
2s
2o
8, 2g P
2o
5add vitriol oil 6ml after mixing, be heated to 80 DEG C, keep after 2 hours, after washing, filtration drying, obtain preoxidation graphite; Dried preoxidation graphite and 60ml vitriol oil interacting depth are oxidized, and period slowly adds 8g KMnO
4, after constant temperature 80 DEG C process 2h, add 200ml water and 20ml hydrogen peroxide successively; Finally use dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) process remove acid and metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the positive ethyl ester of silicic acid of the compound of presoma and graphene oxide: 5ml is dispersed in the mixed solution of 40ml ethanol, 4ml water and 1ml ammoniacal liquor, obtains solution A, and 0.5g graphene oxide is dispersed in 40ml water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; After solution C at room temperature stirs 6h, after centrifugal, alcohol wash, obtain SiO
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, 600 DEG C of calcined composite D, calcination time is 4h, obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder (200 order) 0.4g and SiO
2nanometer sheet 0.1g mixes, and puts into porcelain crucible E; In tube furnace, use H
2(5%), Ar(95%) gas mixture as protection gas, 650 DEG C calcining 2h, obtain class graphene-like Mg
2si nanometer sheet F, finally uses dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) to process the unreacted Mg of removal and obtains pure phase G.
embodiment 4:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of Hummers method of modification, and concrete operations are, 1g admixed graphite, 2g K
2s
2o
8, 2g P
2o
5add vitriol oil 6ml after mixing, be heated to 80 DEG C, keep after 2 hours, after washing, filtration drying, obtain preoxidation graphite; Dried preoxidation graphite and 60ml vitriol oil interacting depth are oxidized, and period slowly adds 8g KMnO
4, after constant temperature 80 DEG C process 2h, add 200ml water and 20ml hydrogen peroxide successively; Finally use dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) process remove acid and metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the positive ethyl ester of silicic acid of the compound of presoma and graphene oxide: 8ml is dispersed in the mixed solution of 40ml ethanol, 4ml water and 1ml ammoniacal liquor, obtains solution A, and 1.0g graphene oxide is dispersed in 40ml water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; After solution C at room temperature stirs 6h, after centrifugal, alcohol wash, obtain SiO
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, 600 DEG C of calcined composite D, calcination time is 4h, obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder (200 order) 0.4g and SiO
2nanometer sheet 0.1g mixes, and puts into porcelain crucible E; In tube furnace, use H
2(5%), Ar(95%) gas mixture as protection gas, 650 DEG C calcining 2h, obtain class graphene-like Mg
2si nanometer sheet F, finally uses dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) to process the unreacted Mg of removal and obtains pure phase G.
embodiment 5:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of Hummers method of modification, and concrete operations are, 1g admixed graphite, 2g K
2s
2o
8, 2g P
2o
5add vitriol oil 6ml after mixing, be heated to 80 DEG C, keep after 2 hours, after washing, filtration drying, obtain preoxidation graphite; Dried preoxidation graphite and 60ml vitriol oil interacting depth are oxidized, and period slowly adds 8g KMnO
4, after constant temperature 80 DEG C process 2h, add 200ml water and 20ml hydrogen peroxide successively; Finally use dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) process remove acid and metal ion, ultrasonic centrifugal after obtain graphene oxide.
(2) SiO
2the positive ethyl ester of silicic acid of the compound of presoma and graphene oxide: 10ml is dispersed in the mixed solution of 40ml ethanol, 4ml water and 1ml ammoniacal liquor, obtain solution A, 1.0g graphene oxide is dispersed in 100ml water, obtain solution B, under whipped state, solution B is joined in solution A, obtain solution C; After solution C at room temperature stirs 6h, after centrifugal, alcohol wash, obtain SiO
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, 600 DEG C of calcined composite D, calcination time is 4h, obtains SiO
2nanosheet photocatalytic material.
(3) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder (200 order) 0.4g and SiO
2nanometer sheet 0.1g mixes, and puts into porcelain crucible E; In tube furnace, use H
2(5%), Ar(95%) gas mixture as protection gas, 650 DEG C calcining 2h, obtain class graphene-like Mg
2si nanometer sheet F, finally uses dilute hydrochloric acid (water: concentrated hydrochloric acid=10:1) to process the unreacted Mg of removal and obtains pure phase G.
?
Claims (6)
1. the preparation method of a kind graphene-like magnesium silicide nanometer sheet, is characterized in that comprising the following steps:
(1) SiO
2the compound of presoma and graphene oxide: be dispersed in the mixed solution of ethanol, water and ammoniacal liquor by positive for silicic acid ethyl ester, obtain solution A, graphene oxide is dispersed in water, obtain solution B, under whipped state, joins solution B in solution A, obtains solution C; Solution C at room temperature stirs the regular hour, obtains SiO after centrifugal, alcohol wash
2the mixture D of presoma and graphene oxide; Under the condition of blowing air, calcined composite D certain hour obtains SiO
2nanometer sheet;
(2) class graphene-like Mg
2the preparation of Si nanometer sheet: get Mg powder and SiO by weight
2nanometer sheet mixes, and puts into porcelain crucible E; In tube furnace, use H
2/ Ar gas mixture, as protection gas, is calcined certain hour and is obtained class graphene-like Mg under certain temperature
2si nanometer sheet F, pickling is removed unreacted Mg and is obtained pure phase Mg
2si nanometer sheet G.
2. the preparation method of a kind graphene-like magnesium silicide nanometer sheet as claimed in claim 1, it is characterized in that, the preparation process of described graphene oxide is as follows: a certain amount of admixed graphite, K
2s
2o
8, P
2o
5add vitriol oil a after mixing, after heating certain hour, after washing, filtration drying, obtain preoxidation graphite b; Dried preoxidation graphite and vitriol oil c interacting depth are oxidized, and period adds appropriate KMnO
4, add water and hydrogen peroxide after constant temperature process, finally with dilute hydrochloric acid process remove metal ion, ultrasonic centrifugal after obtain graphene oxide.
3. the preparation method of a kind graphene-like magnesium silicide nanometer sheet as claimed in claim 2, is characterized in that: described admixed graphite, K
2s
2o
8, P
2o
5weight ratio is 1:2:2; The volume of vitriol oil a and the ratio of admixed graphite quality are 6:1(ml:g); Described heat-up time is 2 hours, Heating temperature 80 DEG C; The consumption of described vitriol oil c is 10 times of vitriol oil a volume; Described KMnO
4be 6:1 ~ 10:1 with the mass ratio of admixed graphite, the volume ratio of hydrogen peroxide and vitriol oil a is 10:3, and the add-on of water is 10 times of hydrogen peroxide volume; Described dilute hydrochloric acid is formulated according to volume ratio 1:10 with commercially available concentrated hydrochloric acid (massfraction 36% ~ 38%) and water.
4. the preparation method of a kind graphene-like magnesium silicide nanometer sheet as claimed in claim 1, is characterized in that: in described step (1), in described solution A, and the volume ratio of the positive ethyl ester of silicic acid and ethanol, water, ammoniacal liquor is 1:40:4:1 to 10:40:4:1; In described solution B, in every 20-100ml distilled water, add 0.5-1g graphene oxide, the quality of graphene oxide and the positive ethyl ester of silicic acid and volume ratio 1:1 ~ 1:10(g:ml).
5. the preparation method of a kind graphene-like magnesium silicide nanometer sheet as claimed in claim 1, it is characterized in that: in step (1), the time that described solution C at room temperature stirs is 6 ~ 10h; Under the condition of described blowing air, calcining temperature is 600 DEG C, and calcination time is 4h.
6. the preparation method of a kind graphene-like magnesium silicide nanometer sheet as claimed in claim 1, it is characterized in that: in step (2), described Mg powder is 200 orders, with SiO
2the weight ratio 4:1 of nanometer sheet; Described calcining temperature is 650 DEG C, and temperature rise rate is 3 DEG C/min, and calcination time is 2-3h, and wherein gas mixture is H
2mix according to volume ratio 5:95 with Ar; Described pickling refers to adopt dilute hydrochloric acid to carry out pickling, and dilute hydrochloric acid is that 1:10 ~ 1:20 is formulated with commercially available concentrated hydrochloric acid (massfraction 36% ~ 38%) and water according to volume ratio.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114380292A (en) * | 2022-01-21 | 2022-04-22 | 深圳大学 | Preparation method and application of magnesium silicide two-dimensional nanosheet, and preparation method and application of hydrogen-releasing hydrogel wound dressing |
| CN114427086A (en) * | 2022-01-08 | 2022-05-03 | 华中科技大学 | Al (aluminum)2O3Nanosheet-reinforced ZrO2Tritium-resistant coating and preparation method thereof |
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| CN102275939A (en) * | 2011-07-28 | 2011-12-14 | 浙江大学 | Preparation method of two-dimensional porous silica nanosheet |
| CN103991903A (en) * | 2014-06-04 | 2014-08-20 | 江苏大学 | Method for preparing mixed-phase titanium dioxide nanosheet photocatalyst |
| CN104030290A (en) * | 2014-06-30 | 2014-09-10 | 金之坚 | Method for producing nanometer silicon by adopting rice hull |
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| CN114427086A (en) * | 2022-01-08 | 2022-05-03 | 华中科技大学 | Al (aluminum)2O3Nanosheet-reinforced ZrO2Tritium-resistant coating and preparation method thereof |
| CN114427086B (en) * | 2022-01-08 | 2022-10-11 | 华中科技大学 | Al (aluminum) 2 O 3 Nanosheet-reinforced ZrO 2 Tritium-resistant coating and preparation method thereof |
| CN114380292A (en) * | 2022-01-21 | 2022-04-22 | 深圳大学 | Preparation method and application of magnesium silicide two-dimensional nanosheet, and preparation method and application of hydrogen-releasing hydrogel wound dressing |
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| CN104261411B (en) | 2017-01-18 |
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