CN107445145A - A kind of preparation method based on graphene composite material - Google Patents
A kind of preparation method based on graphene composite material Download PDFInfo
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- CN107445145A CN107445145A CN201710676745.3A CN201710676745A CN107445145A CN 107445145 A CN107445145 A CN 107445145A CN 201710676745 A CN201710676745 A CN 201710676745A CN 107445145 A CN107445145 A CN 107445145A
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- composite material
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- graphene
- graphene composite
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/65—Raman scattering
- G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
Abstract
The invention discloses a kind of preparation method based on graphene composite material, including：(1) add graphene oxide into deionized water, ultrasonic disperse handles 1~2h, obtains graphene oxide suspension；(2) silver ammino solution prepared by above-mentioned graphene oxide suspension and just is 5 according to volume ratio:1 mixing, 30~60min of magnetic agitation at 45~60 DEG C, add organic reducing agent, it is 10~12 to adjust pH, and 2~3h, cooling are stirred under 80~90 DEG C of water bath conditions, filter, washed 3~5 times using ethanol and deionized water successively, 10~12h is dried at 40~60 DEG C, obtains silver-colored graphene composite material.Preparation technology of the present invention is simple, using the method in the present invention be prepared based in graphene composite material, silver particles are evenly dispersed in graphene sheet layer, have excellent Raman enhancement effect.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation method based on graphene composite material.
Background technology
The detection of toxic molecule is all very important to body health and environment in biomaterial and liquid, but big
In the case of more, normal Raman spectroscopy is insensitive to the deleterious molecular of extremely low concentration in liquid, can not effectively be detected
Out；And Raman enhancing technology can effectively solve this problem because Raman enhancing technology can have one it is huge
Vibration signal, its intensity is set to improve more than 10 orders of magnitude；It is known that Nano Silver has excellent Raman enhancement effect, and
It is widely used on Raman enhancing probe, the technique for preparing Nano Silver Raman reinforcing material at present has a lot, such as：Electron beam loses
Quarter, nanosphere etching, vacuum vapor deposition method etc.；Then these process costs are high, it is impossible to prepare large scale, flexible Raman strengthening material
Material, seriously restricts its application；In order to solve this problem, a suitable carrier is found, obtains a Nano Silver-carrier
Composite is perhaps a good outlet.
Graphene (Graphene) is the Two-dimensional Carbon atomic crystal of monoatomic thickness, it is considered to be fullerene, CNT
(CNT) and graphite basic structural unit, its unique nanostructured and electrical properties make it have become the state to get most of the attention
Border forward position and study hotspot；Importantly, the big specific surface area of graphene and layer structure, which have become, prepares nano material
Excellent template, by in-situ synthesis, it can effectively prevent the reunion of nano particle from obtaining dispersed nano particle-stone
Black alkene composite.But in the prior art, the preparation technology based on graphene composite material is complicated, the composite of gained
Raman enhancement effect is not obvious enough.
For this reason, it is necessary in view of the above-mentioned problems, a kind of preparation method based on graphene composite material is proposed, it can be solved
Certainly problems of the prior art.
The content of the invention
It is an object of the invention to provide a kind of preparation method based on graphene composite material, to overcome in the prior art
Deficiency.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method based on graphene composite material, including：
(1) add graphene oxide into deionized water, ultrasonic disperse handles 1~2h, obtains graphene oxide suspension；
(2) silver ammino solution prepared by above-mentioned graphene oxide suspension and just is 5 according to volume ratio:1 mixing, 45~
30~60min of magnetic agitation at 60 DEG C, organic reducing agent is added, regulation pH is 10~12, is stirred under 80~90 DEG C of water bath conditions
2~3h is mixed, is cooled down, is filtered, is washed 3~5 times using ethanol and deionized water successively, 10~12h is dried at 40~60 DEG C, is obtained
To silver-graphene composite material.
Preferably, in step (1), the preparation method of the graphene oxide includes：1) 1000mL beakers are placed in frozen water
In bath, the 300ml concentrated sulfuric acids are sequentially added, 8g graphite, 6g sodium nitrate, stir 1~2h；It is less than 10 DEG C of condition in keeping temperature
Under, 30g potassium permanganate is slowly added in beaker, 1~2h is stirred, removes ice-water bath, the magnetic agitation under the conditions of 20~30 DEG C
72~120h, obtain thick liquid；2) add 500mL5wt% sulfuric acid while stirring into thick liquid, continue stirring 1~
2h, adds 20g30wt% hydrogen peroxide and deionized water continues 1~2h of stirring, stands 12~24h, obtains product；3) will production
Thing is washed with 3% watery hydrochloric acid, distillation respectively, centrifugation, removes precipitation, obtains graphene oxide suspension.
Preferably, in step (2), the preparation method of the silver ammino solution includes：By 40mg silver nitrate add 5mL go from
In sub- water, silver nitrate solution is obtained；3% ammoniacal liquor is added dropwise in the silver nitrate solution, is disappeared just to precipitating, obtains silver
Ammonia solution.
Preferably, in step (2), the organic reducing agent is selected from aldehyde, formic acid, formic acid esters, glucose, maltose, fructose
In one kind.
Preferably, the mass ratio of silver and graphene is 1 in the silver-graphene composite material:0.1~1.
Compared with prior art, the advantage of the invention is that：Preparation technology of the present invention is simple, using the method in the present invention
Be prepared based in graphene composite material, silver particles are evenly dispersed in graphene sheet layer, have excellent Raman
Enhancement effect.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The present invention discloses a kind of preparation method based on graphene composite material, including：
(1) add graphene oxide into deionized water, ultrasonic disperse handles 1~2h, obtains graphene oxide suspension；
(2) silver ammino solution prepared by above-mentioned graphene oxide suspension and just is 5 according to volume ratio:1 mixing, 45~
30~60min of magnetic agitation at 60 DEG C, organic reducing agent is added, regulation pH is 10~12, is stirred under 80~90 DEG C of water bath conditions
2~3h is mixed, is cooled down, is filtered, is washed 3~5 times using ethanol and deionized water successively, 10~12h is dried at 40~60 DEG C, is obtained
To silver-graphene composite material.
Wherein, the mass ratio of silver and graphene is 1 in the silver-graphene composite material being prepared according to the above method:
0.1~1.
In above-mentioned steps (2), the organic reducing agent is in aldehyde, formic acid, formic acid esters, glucose, maltose, fructose
It is a kind of.
In one embodiment, the preparation method of the graphene oxide includes：
1) 1000mL beakers are placed in ice-water bath, sequentially add the 300ml concentrated sulfuric acids, 8g graphite, 6g sodium nitrate, stirring 1
~2h；Under conditions of keeping temperature is less than 10 DEG C, 30g potassium permanganate is slowly added in beaker, 1~2h is stirred, removes ice
Water-bath, 72~120h of magnetic agitation under the conditions of 20~30 DEG C, obtain thick liquid；
2) add 500mL5wt% sulfuric acid while stirring into thick liquid, continue 1~2h of stirring, add
20g30wt% hydrogen peroxide and deionized water continues 1~2h of stirring, stands 12~24h, obtains product；
3) product is washed with 3% watery hydrochloric acid, distillation respectively, centrifugation, removes precipitation, obtained graphene oxide and suspend
Liquid.
In one embodiment, the preparation method of the silver ammino solution includes：40mg silver nitrate is added into 5mL deionized waters
In, obtain silver nitrate solution；3% ammoniacal liquor is added dropwise in the silver nitrate solution, is disappeared just to precipitating, it is molten to obtain silver-colored ammonia
Liquid.
Embodiment
1st, graphene oxide is prepared
1) 1000mL beakers are placed in ice-water bath, sequentially add the 230ml concentrated sulfuric acids, 10g graphite, 5g sodium nitrate, stirring
2h；Under conditions of keeping temperature is less than 10 DEG C, 30g potassium permanganate is slowly added in beaker, 2h is stirred, removes ice-water bath,
The magnetic agitation 120h under the conditions of 25 DEG C, obtain thick liquid；
2) add 500mL5wt% sulfuric acid while stirring into thick liquid, continue to stir 2h, add 20g30wt%
Hydrogen peroxide and deionized water continue stir 2h, stand 20h, obtain product；
3) product is washed with 3% watery hydrochloric acid, distillation respectively, centrifugation, removes precipitation, obtained graphene oxide and suspend
Liquid.
2nd, silver ammino solution is prepared
40mg silver nitrate is added in 5mL deionized waters, obtains silver nitrate solution；3% ammoniacal liquor is added dropwise to described
In silver nitrate solution, disappeared just to precipitating, obtain silver ammino solution.
3rd, prepare and be based on graphene composite material
(1) graphene oxide made from the method in 1 is added in deionized water, ultrasonic disperse handles 1~2h, obtains
To graphene oxide suspension；
(2) it is 5 according to volume ratio with the silver ammino solution that the method in 2 is prepared by above-mentioned graphene oxide suspension:1
Mixing, 30~60min of magnetic agitation at 60 DEG C, formic acid esters is added, the pH for adjusting solution is 11, is stirred under 90 DEG C of water bath conditions
2h is mixed, is cooled down, is filtered, is washed 3~5 times using ethanol and deionized water successively, 10h is dried at 60 DEG C, obtains silver-graphene
Composite.
Method in the present invention is obtained based in graphene composite material, and silver particles uniform particle diameter, it is dispersed in
In graphene sheet layer, the reunion of particle can be effectively prevented, the addition of silver particles causes the Raman of the composite in the present invention
Signal intensity greatly enhances.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (5)
- A kind of 1. preparation method based on graphene composite material, it is characterised in that including：(1) add graphene oxide into deionized water, ultrasonic disperse handles 1~2h, obtains graphene oxide suspension；(2) silver ammino solution prepared by above-mentioned graphene oxide suspension and just is 5 according to volume ratio:1 mixing, at 45~60 DEG C 30~60min of lower magnetic agitation, add organic reducing agent, regulation pH be 10~12, under 80~90 DEG C of water bath conditions stir 2~ 3h, cool down, filter, washed 3~5 times using ethanol and deionized water successively, 10~12h is dried at 40~60 DEG C, obtain silver- Graphene composite material.
- 2. the preparation method according to claim 1 based on graphene composite material, it is characterised in that in step (1), institute Stating the preparation method of graphene oxide includes：1) 1000mL beakers are placed in ice-water bath, sequentially add the 300ml concentrated sulfuric acids, 8g Graphite, 6g sodium nitrate, stir 1~2h；Under conditions of keeping temperature is less than 10 DEG C, 30g potassium permanganate is slowly added to beaker In, 1~2h is stirred, removes ice-water bath, 72~120h of magnetic agitation under the conditions of 20~30 DEG C, obtains thick liquid；2) to glutinous 500mL5wt% sulfuric acid is added in thick liquid while stirring, continues 1~2h of stirring, add 20g30wt% hydrogen peroxide and Deionized water continues 1~2h of stirring, stands 12~24h, obtains product；3) product is washed with 3% watery hydrochloric acid, distillation respectively Wash, centrifuge, remove precipitation, obtain graphene oxide suspension.
- 3. the preparation method according to claim 1 based on graphene composite material, it is characterised in that in step (2), institute Stating the preparation method of silver ammino solution includes：40mg silver nitrate is added in 5mL deionized waters, obtains silver nitrate solution；By 3% Ammoniacal liquor be added dropwise in the silver nitrate solution, to precipitate just disappear, obtain silver ammino solution.
- 4. the preparation method according to claim 1 based on graphene composite material, it is characterised in that in step (2), institute State the one kind of organic reducing agent in aldehyde, formic acid, formic acid esters, glucose, maltose, fructose.
- 5. the preparation method according to claim 1 based on graphene composite material, it is characterised in that the silver-graphitic The mass ratio of silver and graphene is 1 in alkene composite:0.1~1.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365456A (en) * | 2017-09-15 | 2017-11-21 | 厦门万新橡胶有限公司 | A kind of novel graphite alkene is modified heat conductive rubber |
| CN110426433A (en) * | 2019-08-23 | 2019-11-08 | 衡阳师范学院 | A kind of the nitrogen-doped graphene composite material and preparation method and application of silver-Prussian blue load |
| CN111678908A (en) * | 2020-06-17 | 2020-09-18 | 华中农业大学 | Graphene silver SERS composite substrate and preparation method thereof |
| WO2021072633A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Preparation method for rgo/ag composite nano material |
| CN113957300A (en) * | 2021-10-26 | 2022-01-21 | 广东远光电缆实业有限公司 | Preparation process of super heat-resistant aluminum alloy wire |
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| CN102160998A (en) * | 2011-04-25 | 2011-08-24 | 北京航空航天大学 | Preparation method of graphene-silver nano particle composite material |
| CN104384524A (en) * | 2014-11-19 | 2015-03-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing flake graphite single/multiple load precious metal nano particles |
| CN106398397A (en) * | 2016-08-23 | 2017-02-15 | 中国工程物理研究院材料研究所 | Method for preparing monodisperse graphene based nano silver composite |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102160998A (en) * | 2011-04-25 | 2011-08-24 | 北京航空航天大学 | Preparation method of graphene-silver nano particle composite material |
| CN104384524A (en) * | 2014-11-19 | 2015-03-04 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing flake graphite single/multiple load precious metal nano particles |
| CN106398397A (en) * | 2016-08-23 | 2017-02-15 | 中国工程物理研究院材料研究所 | Method for preparing monodisperse graphene based nano silver composite |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107365456A (en) * | 2017-09-15 | 2017-11-21 | 厦门万新橡胶有限公司 | A kind of novel graphite alkene is modified heat conductive rubber |
| CN110426433A (en) * | 2019-08-23 | 2019-11-08 | 衡阳师范学院 | A kind of the nitrogen-doped graphene composite material and preparation method and application of silver-Prussian blue load |
| CN110426433B (en) * | 2019-08-23 | 2021-08-27 | 衡阳师范学院 | silver-Prussian blue loaded nitrogen-doped graphene composite material and preparation method and application thereof |
| WO2021072633A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Preparation method for rgo/ag composite nano material |
| CN111678908A (en) * | 2020-06-17 | 2020-09-18 | 华中农业大学 | Graphene silver SERS composite substrate and preparation method thereof |
| CN113957300A (en) * | 2021-10-26 | 2022-01-21 | 广东远光电缆实业有限公司 | Preparation process of super heat-resistant aluminum alloy wire |
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