CN103252228A - Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet - Google Patents
Preparation method of composite nanomaterial of nano ZnO and graphene nanosheet Download PDFInfo
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- CN103252228A CN103252228A CN2013102279753A CN201310227975A CN103252228A CN 103252228 A CN103252228 A CN 103252228A CN 2013102279753 A CN2013102279753 A CN 2013102279753A CN 201310227975 A CN201310227975 A CN 201310227975A CN 103252228 A CN103252228 A CN 103252228A
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Abstract
The invention discloses a preparation method of a composite nanomaterial of a nano ZnO substrate and a graphene nanosheet. Nano ZnO and the graphene nanosheet are composited to form the composite nanomaterial in a sol-gel method and mechanical alloying combined mode, so that the preparation method is simple and easy to realize and short in reaction time; the finished composite nanomaterial is good in chemical stability; graphene has higher conductivity and can adjust an energy band structure of nano ZnO; nano ZnO has a higher seebeck coefficient, and the nano ZnO substrate and the graphene nanosheet are synthesized, so that interface scattering of phonons can be increased significantly; a recombination rate of an electron-hole pair can be reduced; the appearance of nano ZnO can be adjusted; the heat conductivity of nano ZnO can be reduced; and the photocatalytic efficiency of nano ZnO can be improved. Nitrate of to-be-doped ions comprises any one of aluminum nitrate, ferric nitrate, cobalt nitrate, nickel nitrate, silver nitrate and gold nitrate.
Description
Technical field
The present invention relates to the nanometer new material technology field, especially the preparation method of the composite nano materials of nano-ZnO sill and graphene nanometer sheet.
Background technology
Nanometer technology is one of world today's hard-core technology; it is the collection condensed state physics; colloid chemistry; Coordinative Chemistry; Chemical Kinetics; subjects such as surface and interface chemistry are the interdisciplinary science of one; world developed country is always the emphasis of nano material as scientific research and technological development; the research of nano material will promote the information technology in 2l century; biomedical; environmental protection; the development of automatic technology and energy science; bring revolutionary variation for human life; nano zine oxide has the performance of many special excellences; as piezoelectricity; fluorescence; nontoxic and non-migrating; absorption and scatters ultraviolet ability etc.; the photocatalysis method that with the nano-ZnO is representative has been subjected to paying close attention to widely in theory and the application of organic pollutant removal; simultaneously; nano-ZnO also is the thermoelectric material of a class potentialization; has thermoelectric transfer characteristic efficiently; the wet chemistry method of nano-ZnO has prospect preferably aspect large-scale production; but because use organic dispersing agent; surfactant and organic precursor; make the last handling process complexity; cost is higher; on the other hand; when utilizing the nano-ZnO photocatalytic; owing to nano-ZnO energy gap reason; the electron-hole pair that produces is not only very easily compound and the life-span is shorter; the photoresponse scope is narrower; so need to reduce the recombination rate of electron-hole pair to improve the photocatalysis efficiency of nano-ZnO; when utilizing the nano-ZnO thermoelectricity capability; because the bigger phonon thermal conductivity of nano-ZnO; influenced the further raising of its thermoelectricity capability; so need to reduce the thermal conductivity of nano-ZnO; improve thermal contact resistance; studies show that; with nano-ZnO and material with carbon element combination; such as CNT (CNT) and C60; can improve photocatalysis efficiency and the thermal contact resistance of nano-ZnO effectively; in various material with carbon elements; Graphene is the two-dimentional carbon atom crystal of monatomic thickness, and utilizing the electrical properties of Graphene uniqueness that nano-ZnO is modified with the better composite nano materials of processability has become important research project.
Summary of the invention
The objective of the invention is to overcome the deficiency of existing nano-ZnO production and performance, the preparation method of the composite nano materials of a kind of nano-ZnO sill and graphene nanometer sheet is provided.
Technical scheme of the present invention: in the mode that sol-gel process and mechanical alloying combine nano-ZnO and graphene nanometer sheet are carried out the compound composite nano materials that makes, its preparation method according to the following steps:
A, graphene nanometer sheet is joined concentration is in 85%～95% the sulfuric acid, under 50 ℃～60 ℃ temperature, stirred 10～15 minutes, filter then, wash, drying, with gained sample ball milling 3～4 hours on high energy ball mill, utilize strong acid and high energy mechanical ball milling that graphene nanometer sheet is carried out early stage and handle, improve the dispersiveness of graphene nanometer sheet;
B, 0.1～10% ratio will wait to mix nitrate and the zinc nitrate hexahydrate of ion dissolves in the deionized water in molar ratio, makes the solution I;
C, the NaOH of 0.02～0.04mol is dissolved in wiring solution-forming II in the deionized water, the mass ratio of NaOH and water is 0.5～0.1;
D, solution II and graphene nanometer sheet slowly are added drop-wise under the stirring of atwirl magnetic stirring apparatus in the solution I, Graphene and zinc nitrate mol ratio are 0～0.1, can produce white precipitate, drip the back and continue to stir and it was reacted completely in 1～2 hour;
E, the solution that the D step is obtained filter, the solid product that obtains is used distilled water and absolute ethanol washing 2～3 times again, put into thermostatic drying chamber then and descended dry 10～12 hours at 90～95 ℃, put into Muffle furnace after dried material fully grinds 500～800 ℃ of following roastings 3～4 hours;
Ball milling 3～4 hours on high energy ball mill again after F, the product of roasting cooling that the E step is obtained, ball milling speed 150-250r/min makes the composite nano materials of nano-ZnO sill and graphene nanometer sheet.
The nitrate of ion of waiting to mix comprises any one in aluminum nitrate, ferric nitrate, cobalt nitrate, nickel nitrate, silver nitrate, the nitric acid gold.
The invention has the beneficial effects as follows: the composite nano materials of the synthetic zno-based of the mode that adopts solution chemistry method (sol-gel process) to combine with mechanical alloying and graphene nanometer sheet, the preparation method is simple, the reaction time is short, and the finished product chemical stability is good.
The specific embodiment:
The invention will be further described below in conjunction with embodiment
Embodiment 1
Graphene nanometer sheet is put into the sulfuric acid of 85% concentration, and filtration washing is dry then after stirring 8 minutes under 50 ℃ of temperature, gained sample ball milling 3 hours on high energy ball mill, and rotating speed is 210r/min; The 0.06mol zinc nitrate hexahydrate is dissolved in the 1000ml deionized water, make the solution I, the NaOH that takes by weighing 0.12mol is dissolved in the deionized water of 1500ml, the wiring solution-forming II, under the stirring of atwirl magnetic stirring apparatus, slowly be added drop-wise to the graphene nanometer sheet after the processing of solution II and 0.0048g in the solution I then, obtain white precipitate, dripping back continuation stirring reacted completely it in 1 hour, the solution that obtains filters and with behind distilled water and the absolute ethanol washing 3 times, it is following dry 10 hours to put into 90 ℃ of thermostatic drying chambers, after fully grinding, puts into dried material Muffle furnace 600 ℃ of following roastings 3 hours, material after roasting ball milling 3 hours on high energy ball mill, ball milling speed 180r/min makes finished product;
Embodiment 2
Graphene nanometer sheet filtration washing after stirring 10 minutes under 50 ℃ of temperature of sulfuric acid of 85% concentration is dry then, gained sample ball milling 3 hours on high energy ball mill, rotating speed is 180r/min, 0.00486mol cobalt nitrate and 0.06mol zinc nitrate hexahydrate are dissolved in the 1300ml deionized water, make the solution I, the NaOH that takes by weighing 0.13mol is dissolved in the deionized water of 1600ml, the wiring solution-forming II, graphene nanometer sheet with solution II and 0.0028g slowly is added drop-wise in the solution I under the stirring of atwirl magnetic stirring apparatus then, obtain white precipitate, dripping back continuation stirring reacted completely it in 1 hour, the solution that obtains filters and with behind distilled water and the absolute ethanol washing 2 times, it is following dry 10 hours to put into 90 ℃ of thermostatic drying chambers, after fully grinding, puts into dried material Muffle furnace 700 ℃ of following roastings 3 hours, material after roasting ball milling 3 hours on high energy ball mill, ball milling speed 200r/min makes finished product;
Embodiment 3
Graphene nanometer sheet filtration washing after stirring 10 minutes under 30 ℃ of temperature of sulfuric acid of 85% concentration is dry then, gained sample ball milling 3 hours on high energy ball mill, rotating speed is 170r/min; 0.00316mol silver nitrate and 0.06mol zinc nitrate hexahydrate are dissolved in the 1250ml deionized water, make the solution I, the NaOH that takes by weighing 0.125mol is dissolved in the deionized water of 1500ml, the wiring solution-forming II, graphene nanometer sheet with solution II and 0.0046g slowly is added drop-wise in the solution I under the stirring of atwirl magnetic stirring apparatus then, obtain white precipitate, dripping back continuation stirring reacted completely it in 1 hour, the solution that obtains filters and with behind distilled water and the absolute ethanol washing 3 times, put into 90 ℃ of following dry 10h of thermostatic drying chamber, after fully grinding, puts into dried material Muffle furnace 800 ℃ of following roastings 3 hours, material after roasting ball milling 3 hours on high energy ball mill, ball milling speed 190r/min makes finished product.
The finished product that above embodiment is obtained carries out phenetic analysis and performance test proves: the band structure that Graphene has higher electrical conductivity and can regulate nano-ZnO, nano-ZnO has higher Seebeck coefficient, the nano-ZnO sill is by the synthesizing graphite alkene nanometer sheet, can significantly increase the interface scattering of phonon, reduce the recombination rate of electron-hole pair, regulate the pattern of nano-ZnO, thereby reduce the thermal conductivity of nano-ZnO, improve the photocatalysis efficiency of nano-ZnO.
Claims (2)
1. the preparation method of the composite nano materials of nano-ZnO and graphene nanometer sheet, it is characterized in that the mode that combines with sol-gel process and mechanical alloying carries out the compound composite nano materials that makes with nano-ZnO and graphene nanometer sheet, its preparation method according to the following steps:
A, graphene nanometer sheet is joined concentration is in 85%～95% the sulfuric acid, under 50 ℃～60 ℃ temperature, stirred 10～15 minutes, filter then, wash, drying, with gained sample ball milling 3～4 hours on high energy ball mill, utilize strong acid and high energy mechanical ball milling that graphene nanometer sheet is carried out early stage and handle, improve the dispersiveness of graphene nanometer sheet;
B, 0.1～10% ratio will wait to mix nitrate and the zinc nitrate hexahydrate of ion dissolves in the deionized water in molar ratio, makes the solution I;
C, the NaOH of 0.02～0.04mol is dissolved in wiring solution-forming II in the deionized water, the mass ratio of NaOH and water is 0.5～0.1;
D, solution II and graphene nanometer sheet slowly are added drop-wise under the stirring of atwirl magnetic stirring apparatus in the solution I, Graphene and zinc nitrate mol ratio are 0～0.1, can produce white precipitate, drip the back and continue to stir and it was reacted completely in 1～2 hour;
E, the solution that the D step is obtained filter, the solid product that obtains is used distilled water and absolute ethanol washing 2～3 times again, put into thermostatic drying chamber then and descended dry 10～12 hours at 90～95 ℃, put into Muffle furnace after dried material fully grinds 500～800 ℃ of following roastings 3～4 hours;
F, product of roasting cooling back that the E step is obtained ball milling 3～4 hours on high energy ball mill, ball milling speed 150-250r/min makes the composite nano materials of nano-ZnO sill and graphene nanometer sheet.
2. the preparation method of the composite nano materials of nano-ZnO according to claim 1 and graphene nanometer sheet
,The nitrate of ion of it is characterized in that waiting mixing comprises any one in aluminum nitrate, ferric nitrate, cobalt nitrate, nickel nitrate, silver nitrate, the nitric acid gold.
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| CN103482615A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Preparation method of foamed graphene-ZnO composite material |
| CN103922388A (en) * | 2014-04-10 | 2014-07-16 | 常州大学 | Preparation method of conductive graphene/zinc aluminium oxide composite |
| CN104759282A (en) * | 2014-12-01 | 2015-07-08 | 青岛科技大学 | Novel method for microwave-assisted preparation of zinc oxide/graphene/silver nano-composite photocatalyst |
| CN104959161A (en) * | 2015-06-17 | 2015-10-07 | 新乡学院 | Method for preparing conjugated molecular hybridization semiconductor photocatalytic material by using mechanochemistry |
| CN105126820A (en) * | 2015-09-23 | 2015-12-09 | 长沙理工大学 | Preparation method of three-dimensional graphene/tungsten-based nanosheet/magnesium doped zinc oxide layer-by-layer assembly structure |
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| CN106349663A (en) * | 2016-08-29 | 2017-01-25 | 佛山市高明区尚润盈科技有限公司 | Preparing method for polylactic acid antibacterial radiation-resistant masterbatch |
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| CN107398265A (en) * | 2017-08-09 | 2017-11-28 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene oxide catalysis material |
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| CN105126820A (en) * | 2015-09-23 | 2015-12-09 | 长沙理工大学 | Preparation method of three-dimensional graphene/tungsten-based nanosheet/magnesium doped zinc oxide layer-by-layer assembly structure |
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| CN107398265A (en) * | 2017-08-09 | 2017-11-28 | 张家港市汇鼎新材料科技有限公司 | A kind of preparation method based on graphene oxide catalysis material |
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Application publication date: 20130821 |