CN104261411B - Preparation method of graphene-like magnesium silicide nanosheets - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- YTHCQFKNFVSQBC-UHFFFAOYSA-N magnesium silicide Chemical compound [Mg]=[Si]=[Mg] YTHCQFKNFVSQBC-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910021338 magnesium silicide Inorganic materials 0.000 title claims abstract description 21
- 239000002135 nanosheet Substances 0.000 title abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 82
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000001354 calcination Methods 0.000 claims abstract description 23
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 59
- 229910002804 graphite Inorganic materials 0.000 claims description 31
- 239000010439 graphite Substances 0.000 claims description 31
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 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
- 239000000843 powder Substances 0.000 claims description 10
- 238000007664 blowing Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 239000008246 gaseous mixture Substances 0.000 claims description 9
- 239000002131 composite material Substances 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
- 230000003647 oxidation Effects 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 230000001590 oxidative effect Effects 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229910052573 porcelain Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000005554 pickling Methods 0.000 claims description 6
- 229910002567 K2S2O8 Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 229910001882 dioxygen Inorganic materials 0.000 claims description 2
- -1 graphite alkene Chemical class 0.000 claims description 2
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical compound CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 28
- 239000000463 material Substances 0.000 abstract description 18
- 239000004065 semiconductor Substances 0.000 abstract description 6
- 238000003980 solgel method Methods 0.000 abstract description 3
- 239000011259 mixed solution Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 39
- 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
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 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
- 238000005253 cladding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
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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 to a species graphene-like magnesium silicide nanometer sheet
Preparation method.
Background technology
Magnesium silicide is narrow bandgap semiconductor material, magnesium silicide with its good thermoelectricity mechanical property, very strong anticorrosive energy
Power, the positive regard having arrived researcher.And, the abundant raw material of si, mg, stratum reserves are big, cheap, make him again
Become a kind of potential new structural material.The application of magnesium silicide extensively, heats including generating electricity, freezing, semiconductor manufacturing,
The fields such as laser, computer realm and military affairs, Aero-Space, automobile making and room-mate's chemical industry.System accordingly, with respect to magnesium silicide
The important meaning of Preparation Method tool, the particularly material of two-dimensional appearance.
All refer to that the pattern of semi-conducting material can have a huge impact to performance, especially in substantial amounts of document report
Lamellar structure can make the performance of semi-conducting material obtain huge improvement.However, current synthesizing magnesium silicide flaky nanometer structure
Report also deficienter, some using section to this pattern, but this method is limited by technology.Therefore, close
A kind of magnesium silicide of laminated structure is become to be still limited by the person's character of the method and material synthesizing, so, up to the present also do not have
The synthesis of class graphene-like magnesium silicide nanometer sheet and application report；This also makes to design new class graphene-like magnesium silicide nanometer sheet
Remain a huge challenge in theoretical research and practical application.
Content of the invention
It is an object of the invention to provide a kind of easy preparation method of new class graphene-like magnesium silicide nanometer sheet, the method
With graphene oxide as template, the positive ethyl ester of silicic acid, the mixed solution of ammoniacal liquor, distilled water and ethanol is solvent, using sol-gel
Method, calcining removing template, are obtained new class graphene-like magnesium silicide nanometer sheet material.
The present invention provides a kind of preparation method of new class graphene-like magnesium silicide nanometer sheet, and its feature includes following step
Rapid:
(1) preparation of graphene oxide: the preparation method of this experiment Graphene is a kind of modified hummers method, tool
Gymnastics conduct, a certain amount of admixed graphite, k2s2o8、p2o5Concentrated sulfuric acid a is added after mixing, after heating certain time, washing, filtration
Obtain after drying pre-oxidizing graphite b；Dried pre-oxidation graphite is aoxidized with concentrated sulfuric acid c interacting depth, and period adds appropriate
kmno4, add water and hydrogen peroxide after constant temperature process, finally processed with watery hydrochloric acid and remove metal ion, after ultrasonic centrifugation, obtain oxygen
Graphite alkene.
(2) sio2Presoma and graphene oxide compound: the positive ethyl ester of different amounts of silicic acid is dispersed in ethanol, water and ammoniacal liquor
Mixed liquor in, obtain solution a, graphene oxide be dispersed in water, obtain solution b, under stirring, solution b is added
Enter in solution a, obtain solution c；Solution c is stirred at room temperature the regular hour, and centrifugation, alcohol obtain sio after washing2Presoma with
The compound d of graphene oxide；Under conditions of blowing air, calcined composite d certain time obtains sio2Nanometer sheet photocatalysis material
Material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder and sio by weight2Nanometer sheet mixes, and puts into
E in porcelain crucible.In tube furnace, use h2As shielding gas, under uniform temperature, calcining certain time obtains class graphite to/ar gaseous mixture
Alkene shape mg2Si nanometer sheet f, pickling removes unreacted mg and obtains pure phase mg2Si nanometer sheet g.
In step (1), described admixed graphite, k2s2o8、p2o5Weight is than for 1:2:2.
In step (1), the ratio of the volume of concentrated sulfuric acid a and admixed graphite quality is 6:1(ml:g).
In step (1), the described heat time is 2 hours, 80 DEG C of heating-up temperature.
In step (1), the consumption of described concentrated sulfuric acid c is 10 times of concentrated sulfuric acid a volume.
In step (1), described kmno4Mass ratio with admixed graphite is 6:1 ~ 10:1, the body of hydrogen peroxide and concentrated sulfuric acid a
Long-pending ratio is 10:3, and the addition of water is 10 times of dioxygen water volume.
In step (1), described watery hydrochloric acid is according to volume ratio 1:10 with commercially available concentrated hydrochloric acid (mass fraction 36% ~ 38%) with water
It is formulated.
In step (2), in described solution a, the positive ethyl ester of silicic acid is 1:40:4:1 to 10 with the volume ratio of ethanol, water, ammoniacal liquor:
40:4:1.
In step (2), in described solution b, in every 20-100ml distilled water, add 0.5-1g graphene oxide, graphite oxide
The quality of alkene 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 is stirred at room temperature is 6 ~ 10h.
In step (2), under conditions of described blowing air, calcining heat is 600 DEG C, and calcination time is 4h.
In step (3), described mg powder is 200 mesh, with sio2The weight of nanometer sheet compares 4:1.
In step (3), described calcining heat is 650 DEG C, and heating rate is 3 DEG C/min, and calcination time is 2-3h, wherein mixed
Conjunction gas is h2Mix according to volume ratio 5:95 with ar.
In step (3), described pickling refers to carry out pickling using watery hydrochloric acid, and watery hydrochloric acid is with commercially available concentrated hydrochloric acid (mass fraction
36% ~ 38%) it is formulated for 1:10 ~ 1:20 according to volume ratio with water.
Brief description
Fig. 1 is the mg prepared by the present invention2The xrd figure of si material.
Fig. 2 is the tem shape appearance figure of material prepared by the present invention: a. graphene oxide, and b. coats sio2Transmission electricity afterwards
Mirror figure, c. removes sio after graphene oxide2Transmission electron microscope picture, d .mg2Si transmission electron microscope picture.
The mg synthesized by the present invention can be drawn by the xrd figure of Fig. 12The pdf card number of si is a kind of cube for 35-0733
Crystal formation fm3m (225) structure.
A figure in Fig. 2 is the transmission electron microscope picture of template graphene oxide synthesized by the present invention, it can be found that graphene oxide
Gauze-like pattern feature, can determine the success of hummer method of modifying used simultaneously；After b figure is coated silica
Transmission electron microscope picture, as can be seen from the figure the marginal portion of material is still the typical feature of graphene oxide, and the main body of material
Part has coated layer of silicon dioxide, and this illustrates that sol-gel process used can be implemented in surface of graphene oxide cladding one
Layer silica；C figure be remove graphene oxide template after silica pattern it is evident that through air atmosphere calcining
Method can remove graphene oxide template effectively, and goes the silica after removing template still to assume graphene oxide
Sheet-like morphology feature；D figure is in h2Under conditions of/ar gaseous mixture is protective gas, mg simple substance is generated with silicon dioxde reaction
mg2The transmission electron microscope picture of si, be may certify that the mg synthesized by the present invention by figure2Si is the structure of a species graphene-like.
Specific embodiment
For a better understanding of the present invention, it is further elucidated with present disclosure with reference to embodiment, but the present invention
Content is not limited solely to the following examples.
Embodiment 1:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of modified hummers side
Method, concrete operations are, 1g admixed graphite, 2g k2s2o8、2g p2o5Add concentrated sulfuric acid 6ml after mixing, be heated to 80 DEG C, keep 2
After hour, obtain after washing, filtration drying pre-oxidizing graphite；Dried pre-oxidation graphite and 60ml concentrated sulfuric acid interacting depth oxygen
Change, period is slowly added to 8g kmno4, after 80 DEG C of process 2h of constant temperature, sequentially add 200ml water and 20ml hydrogen peroxide；Finally with dilute
Hydrochloric acid (water: concentrated hydrochloric acid=10:1) processes and removes deacidification and metal ion, obtains graphene oxide after ultrasonic centrifugation.
(2) sio2Presoma and graphene oxide compound: the positive ethyl ester of silicic acid of 1ml be dispersed in 40ml ethanol, 4ml water and
In the mixed liquor of 1ml ammoniacal liquor, obtain solution a, 1.0g graphene oxide is dispersed in 40ml water, obtain solution b, in stirring shape
Under state, solution b is added in solution a, obtains solution c；After solution c is stirred at room temperature 6h, centrifugation, alcohol obtain sio after washing2
Presoma and the compound d of graphene oxide；Under conditions of blowing air, 600 DEG C of calcined composite d, calcination time is 4h, obtains
To sio2Nanosheet photocatalytic material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder (200 mesh) 0.4g and sio2The mixing of nanometer sheet 0.1g is all
Even, put into e in porcelain crucible；In tube furnace, use h2(5%), ar(95%) gaseous mixture as shielding gas, 650 DEG C calcining 2h, obtain
Class graphene-like mg2Si nanometer sheet f, finally processes the unreacted mg of removal with watery hydrochloric acid (water: concentrated hydrochloric acid=20:1) and obtains pure phase
g.
Embodiment 2:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of modified hummers side
Method, concrete operations are, 1g admixed graphite, 2g k2s2o8、2g p2o5Add concentrated sulfuric acid 6ml after mixing, be heated to 80 DEG C, keep 2
After hour, obtain after washing, filtration drying pre-oxidizing graphite；Dried pre-oxidation graphite and 60ml concentrated sulfuric acid interacting depth oxygen
Change, period is slowly added to 8g kmno4, after 80 DEG C of process 2h of constant temperature, sequentially add 200ml water and 20ml hydrogen peroxide；Finally with dilute
Hydrochloric acid (water: concentrated hydrochloric acid=10:1) processes and removes deacidification and metal ion, obtains graphene oxide after ultrasonic centrifugation.
(2) sio2Presoma and graphene oxide compound: the positive ethyl ester of silicic acid of 2ml be dispersed in 40ml ethanol, 4ml water and
In the mixed liquor of 1ml ammoniacal liquor, obtain solution a, 0.5g graphene oxide is dispersed in 40ml water, obtain solution b, in stirring shape
Under state, solution b is added in solution a, obtains solution c；After solution c is stirred at room temperature 6h, centrifugation, alcohol obtain sio after washing2
Presoma and the compound d of graphene oxide；Under conditions of blowing air, 600 DEG C of calcined composite d, calcination time is 4h, obtains
To sio2Nanosheet photocatalytic material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder (200 mesh) 0.4g and sio2The mixing of nanometer sheet 0.1g is all
Even, put into e in porcelain crucible；In tube furnace, use h2(5%), ar(95%) gaseous mixture as shielding gas, 650 DEG C calcining 2h, obtain
Class graphene-like mg2Si nanometer sheet f, finally processes the unreacted mg of removal with watery hydrochloric acid (water: concentrated hydrochloric acid=10:1) and obtains pure phase
g.
Embodiment 3:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of modified hummers side
Method, concrete operations are, 1g admixed graphite, 2g k2s2o8、2g p2o5Add concentrated sulfuric acid 6ml after mixing, be heated to 80 DEG C, keep 2
After hour, obtain after washing, filtration drying pre-oxidizing graphite；Dried pre-oxidation graphite and 60ml concentrated sulfuric acid interacting depth oxygen
Change, period is slowly added to 8g kmno4, after 80 DEG C of process 2h of constant temperature, sequentially add 200ml water and 20ml hydrogen peroxide；Finally with dilute
Hydrochloric acid (water: concentrated hydrochloric acid=10:1) processes and removes deacidification and metal ion, obtains graphene oxide after ultrasonic centrifugation.
(2) sio2Presoma and graphene oxide compound: the positive ethyl ester of silicic acid of 5ml be dispersed in 40ml ethanol, 4ml water and
In the mixed liquor of 1ml ammoniacal liquor, obtain solution a, 0.5g graphene oxide is dispersed in 40ml water, obtain solution b, in stirring shape
Under state, solution b is added in solution a, obtains solution c；After solution c is stirred at room temperature 6h, centrifugation, alcohol obtain sio after washing2
Presoma and the compound d of graphene oxide；Under conditions of blowing air, 600 DEG C of calcined composite d, calcination time is 4h, obtains
To sio2Nanosheet photocatalytic material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder (200 mesh) 0.4g and sio2The mixing of nanometer sheet 0.1g is all
Even, put into e in porcelain crucible；In tube furnace, use h2(5%), ar(95%) gaseous mixture as shielding gas, 650 DEG C calcining 2h, obtain
Class graphene-like mg2Si nanometer sheet f, finally processes the unreacted mg of removal with watery hydrochloric acid (water: concentrated hydrochloric acid=10:1) and obtains pure phase
g.
Embodiment 4:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of modified hummers side
Method, concrete operations are, 1g admixed graphite, 2g k2s2o8、2g p2o5Add concentrated sulfuric acid 6ml after mixing, be heated to 80 DEG C, keep 2
After hour, obtain after washing, filtration drying pre-oxidizing graphite；Dried pre-oxidation graphite and 60ml concentrated sulfuric acid interacting depth oxygen
Change, period is slowly added to 8g kmno4, after 80 DEG C of process 2h of constant temperature, sequentially add 200ml water and 20ml hydrogen peroxide；Finally with dilute
Hydrochloric acid (water: concentrated hydrochloric acid=10:1) processes and removes deacidification and metal ion, obtains graphene oxide after ultrasonic centrifugation.
(2) sio2Presoma and graphene oxide compound: the positive ethyl ester of silicic acid of 8ml be dispersed in 40ml ethanol, 4ml water and
In the mixed liquor of 1ml ammoniacal liquor, obtain solution a, 1.0g graphene oxide is dispersed in 40ml water, obtain solution b, in stirring shape
Under state, solution b is added in solution a, obtains solution c；After solution c is stirred at room temperature 6h, centrifugation, alcohol obtain sio after washing2
Presoma and the compound d of graphene oxide；Under conditions of blowing air, 600 DEG C of calcined composite d, calcination time is 4h, obtains
To sio2Nanosheet photocatalytic material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder (200 mesh) 0.4g and sio2The mixing of nanometer sheet 0.1g is all
Even, put into e in porcelain crucible；In tube furnace, use h2(5%), ar(95%) gaseous mixture as shielding gas, 650 DEG C calcining 2h, obtain
Class graphene-like mg2Si nanometer sheet f, finally processes the unreacted mg of removal with watery hydrochloric acid (water: concentrated hydrochloric acid=10:1) and obtains pure phase
g.
Embodiment 5:
(1) preparation of graphene oxide: the preparation method of this experiment graphene oxide is a kind of modified hummers side
Method, concrete operations are, 1g admixed graphite, 2g k2s2o8、2g p2o5Add concentrated sulfuric acid 6ml after mixing, be heated to 80 DEG C, keep 2
After hour, obtain after washing, filtration drying pre-oxidizing graphite；Dried pre-oxidation graphite and 60ml concentrated sulfuric acid interacting depth oxygen
Change, period is slowly added to 8g kmno4, after 80 DEG C of process 2h of constant temperature, sequentially add 200ml water and 20ml hydrogen peroxide；Finally with dilute
Hydrochloric acid (water: concentrated hydrochloric acid=10:1) processes and removes deacidification and metal ion, obtains graphene oxide after ultrasonic centrifugation.
(2) sio2Presoma is compound with graphene oxide: the positive ethyl ester of silicic acid of 10ml is dispersed in 40ml ethanol, 4ml water
In the mixed liquor of 1ml ammoniacal liquor, obtain solution a, 1.0g graphene oxide is dispersed in 100ml water, obtain solution b, stirring
Mix under state, solution b is added in solution a, obtain solution c；After solution c is stirred at room temperature 6h, centrifugation, alcohol obtain after washing
sio2Presoma and the compound d of graphene oxide；Under conditions of blowing air, 600 DEG C of calcined composite d, calcination time is
4h, obtains sio2Nanosheet photocatalytic material.
(3) class graphene-like mg2The preparation of si nanometer sheet: take mg powder (200 mesh) 0.4g and sio2The mixing of nanometer sheet 0.1g is all
Even, put into e in porcelain crucible；In tube furnace, use h2(5%), ar(95%) gaseous mixture as shielding gas, 650 DEG C calcining 2h, obtain
Class graphene-like mg2Si nanometer sheet f, finally processes the unreacted mg of removal with watery hydrochloric acid (water: concentrated hydrochloric acid=10:1) and obtains pure phase
g.
Claims (5)
1. the preparation method of a species graphene-like magnesium silicide nanometer sheet is it is characterised in that comprise the following steps:
(1)sio2Presoma is compound with graphene oxide: positive for silicic acid ethyl ester is dispersed in the mixed liquor of ethanol, water and ammoniacal liquor,
Obtain solution a, graphene oxide be dispersed in water, obtain solution b, under stirring, solution b is added in solution a,
Obtain solution c；Solution c is stirred at room temperature the regular hour, and centrifugation, alcohol obtain sio after washing2Presoma and graphene oxide
Compound d；Under conditions of blowing air, calcined composite d certain time obtains class graphene-like sio2Nanometer sheet；
(2) class graphene-like mg2The preparation of si nanometer sheet: take mg powder and sio by weight2Nanometer sheet mixes, and puts into porcelain earthenware
E in crucible；In tube furnace, use h2As shielding gas, under uniform temperature, calcining certain time obtains class graphene-like to/ar gaseous mixture
mg2Si nanometer sheet f, pickling removes unreacted mg and obtains pure phase mg2Si nanometer sheet g；
In described step (1), in described solution a, the positive ethyl ester of silicic acid is 1:40:4:1 to 10 with the volume ratio of ethanol, water, ammoniacal liquor:
40:4:1；In described solution b, in every 20-100ml distilled water, add 0.5-1g graphene oxide, graphene oxide is with silicic acid just
The quality of ethyl ester and volume ratio 1:1～1:10 (g:ml)；
Described mg powder and sio2The weight of nanometer sheet compares 4:1；Described calcining heat is 650 DEG C, and heating rate is 3 DEG C/min, calcining
Time is 2-3h, and wherein gaseous mixture is h2Mix according to volume ratio 5:95 with ar.
2. the preparation method of a species graphene-like magnesium silicide nanometer sheet as claimed in claim 1 is it is characterised in that described oxygen
The preparation process of graphite alkene is as follows: a certain amount of admixed graphite, k2s2o8、p2o5Concentrated sulfuric acid a, heating one timing is added after mixing
Between after, washing, obtain after filtration drying pre-oxidizing graphite b；Dried pre-oxidation graphite is aoxidized with concentrated sulfuric acid c interacting depth,
Period adds appropriate kmno4, constant temperature adds water and hydrogen peroxide after processing, is finally processed with watery hydrochloric acid and remove metal ion, ultrasonic
Graphene oxide is obtained after centrifugation.
3. a species graphene-like magnesium silicide nanometer sheet as claimed in claim 2 preparation method it is characterised in that: described
Admixed graphite, k2s2o8、p2o5Weight is than for 1:2:2；The ratio of the volume of concentrated sulfuric acid a and admixed graphite quality is 6:1 (ml:g)；
The described heat time is 2 hours, 80 DEG C of heating-up temperature；The consumption of described concentrated sulfuric acid c is 10 times of concentrated sulfuric acid a volume；Described
kmno4Mass ratio with admixed graphite is 6:1～10:1, and hydrogen peroxide is 10:3 with the volume ratio of concentrated sulfuric acid a, and the addition of water is
10 times of dioxygen water volume；Described watery hydrochloric acid is according to volume ratio 1 with the commercially available concentrated hydrochloric acid of mass fraction 36%～38% with water:
10 are formulated.
4. a species graphene-like magnesium silicide nanometer sheet as claimed in claim 1 preparation method it is characterised in that: step
(1), in, the time that described solution c is stirred at room temperature is 6～10h；Under conditions of described blowing air, calcining heat is 600
DEG C, calcination time is 4h.
5. a species graphene-like magnesium silicide nanometer sheet as claimed in claim 1 preparation method it is characterised in that: step
(2), in, described mg powder is 200 mesh；Described pickling refers to carry out pickling using watery hydrochloric acid, watery hydrochloric acid be with mass fraction 36%～
38% commercially available concentrated hydrochloric acid is formulated for 1:10～1:20 according to volume ratio with water.
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| DE60313294T2 (en) * | 2002-02-15 | 2008-03-06 | Toudai Tlo, Ltd. | MAGNESIUM BASED COMPOSITE MATERIAL AND METHOD OF MANUFACTURING THEREOF |
| CN102249239A (en) * | 2011-06-08 | 2011-11-23 | 浙江大学 | Preparation method for preparing high-purity simple substance silicon from agricultural wastes |
| CN102275939A (en) * | 2011-07-28 | 2011-12-14 | 浙江大学 | Preparation method of two-dimensional porous silica nanosheet |
| CN103991903B (en) * | 2014-06-04 | 2016-06-15 | 江苏大学 | A kind of preparation method of mixed phase titanium dioxide nanosheet photocatalyst |
| CN104030290B (en) * | 2014-06-30 | 2016-03-09 | 金之坚 | The method of nano-silicon is produced with rice husk |
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