CN106315565A - Graphene for temperature sensor and preparation method of graphene - Google Patents
Graphene for temperature sensor and preparation method of graphene Download PDFInfo
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- CN106315565A CN106315565A CN201610652359.6A CN201610652359A CN106315565A CN 106315565 A CN106315565 A CN 106315565A CN 201610652359 A CN201610652359 A CN 201610652359A CN 106315565 A CN106315565 A CN 106315565A
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Abstract
The invention discloses graphene for a temperature sensor and a preparation method of the graphene. The method includes the steps that firstly, a graphite raw material and a sodium hydroxide solvent are mixed evenly according to the weight ratio, the mixture is put into a closed oxygen-free reaction vessel and stirred for a reaction, after pressure reduction, suction filtration and washing, filtrate is subjected to vacuum drying and grinding, then the product obtained after drying is uniformly dispersed in deionized water, the dispersion is put into a hydrochloric acid solution and stirred for a reaction, and suspension is obtained; centrifugal sedimentation is carried out two times at the room temperature, sediment is repeatedly washed with absolute ethyl alcohol 1-2 times and then dried, and the graphene can be obtained. The preparation conditions hardly influence the product quality or yield, the product quality and yield are easy to control, and the graphene is suitable for large-scale production.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to a kind of temperature sensor Graphene and preparation method thereof.
Background technology
Graphene is the two-dimentional carbon film of a kind of only one of which atomic thickness, be people find so far unique a kind of by monolayer
The material of atomic building, is connected into hexagonal network by chemical bond between carbon atom in carbon film, due to the chemical bond between carbon atom
Being made up of sp2 hybrid orbital, therefore Graphene is the most indomitable, possess bent, electric conductivity is strong, mechanical strength good, light transmission is good
The good characteristic that other new materials do not possess.Graphene possesses the electric conductivity being not of the common run, and resistivity is the least, and electronics can pole
Migrating efficiently, this respect performance is more much higher than traditional conductor and quasiconductor；Electronics migrates in Graphene and there is not electricity
Son and the collision of atom, can greatly reduce energy loss；Graphene possesses fabulous light transmission, but airtight, Ke Yiyong
Develop a new generation's protective layer material, and can be used to develop transparent electron product and wearable electronic product.Graphene produces
The preparation method of product is various, but there are some drawbacks, is especially difficult to control to product quality and productivity in preparation process, raw
The change of the processing conditions slight variation such as temperature and time during product, brings the biggest shadow will to the quality of product and productivity
Ring, prepare therefore, it is difficult to realize scale.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of temperature sensor Graphene and preparation method thereof, make
Obtaining preparation condition relatively small to product quality and yield impact, product quality and productivity are easily controllable, are suitable for large-scale production.
For realizing object above, the present invention is achieved by the following technical programs:
The preparation method of a kind of temperature sensor Graphene, comprises the following steps:
(1) it is first 10-50:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic close
Close in reaction vessel, stirring reaction 0.5-6h at 40-120 DEG C, after decompression, sucking filtration, washing, filtrate is vacuum dried, grinds
Mill；
(2) by dried product in step (1), deionized water is that 100-1000:1 is dispersed according to weight ratio, and
It is placed in hydrochloric acid solution under the conditions of 0-4 DEG C, stirs reaction 1-4h, be then warming up to 20-40 DEG C of stirring reaction 1-2h, obtain suspended
Liquid；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 5-10min, removes the supernatant, repeats add deionized water and be centrifuged
Process 1-2 time, take precipitum and add dehydrated alcohol, after stirring 5-10min, be centrifuged sedimentation, take precipitum and repeat anhydrous
After washing with alcohol 1-2 time, by precipitum dried；
Preferably, in described step (1), oxygen-free environment is one or more that be full of in nitrogen, argon, helium
Oxygen-free environment.
Preferably, in described step (1), vacuum drying temperature is 80-120 DEG C, and milling time is 10-30min.
Preferably, the described centrifugal rotational speed in step (2) is 4500-6000r/min, and the time is 3-8min.
Preferably, the relative concentration of the described dehydrated alcohol in step (3) is 80%.
Preferably, the temperature being dried in described step (3) is 100-120 DEG C, and the time is 5-10min.
The method have the benefit that
Present invention process is simple and easily operated, and the selection of supplementary material is relatively common, is suitable for large-scale production；The present invention
In the preparation process of Graphene, twice oxidizing process makes the oxidized extent of exfoliation of graphite deeper；Isolated and purified process can obtain
The Graphene of very high purity, and finally give high-quality Graphene.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with the enforcement of the present invention
Example, is clearly and completely described the technical scheme in the embodiment of the present invention.Based on the embodiment in the present invention, this area
The every other embodiment that those of ordinary skill is obtained under not making creative work premise, broadly falls into present invention protection
Scope.
Embodiment 1:
The preparation method of a kind of temperature sensor Graphene, comprises the following steps:
(1) it is first 10:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answering in container, at 40 DEG C, stirring reaction 0.5h, after decompression, sucking filtration, washing, puts into filtrate in the vacuum that temperature is 80 DEG C
Being dried, then grind 10min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 100:1 is dispersed according to weight ratio, is placed in salt
In acid solution, under the conditions of 0 DEG C, 1h is reacted in stirring, is then warming up to 20 DEG C of stirring reaction 1h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 5min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 1 time, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring 5min, is centrifuged sedimentation, takes precipitum
After repetition absolute ethanol washing 1 time, by precipitum dried 5min under conditions of temperature is 100 DEG C, wherein it is centrifuged
Rotating speed is 4500r/min, and the time of each centrifugal sedimentation is 3min.
Embodiment 2:
The preparation method of a kind of temperature sensor Graphene comprises the following steps:
(1) it is first 50:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answering in container, at 120 DEG C, stirring reaction 6h, after decompression, sucking filtration, washing, puts into filtrate in the vacuum that temperature is 120 DEG C
Being dried, then grind 30min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 1000:1 is dispersed according to weight ratio, is placed in
In hydrochloric acid solution, under the conditions of 4 DEG C, 4h is reacted in stirring, is then warming up to 40 DEG C of stirring reaction 2h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 10min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 2 times, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring 10min, is centrifuged sedimentation, takes sedimentation
After thing repetition absolute ethanol washing 1-2 time, by precipitum dried 10min under conditions of temperature is 120 DEG C, wherein
Centrifugal rotational speed is 6000r/min, and the time of each centrifugal sedimentation is 3min.
Embodiment 3:
The preparation method of a kind of temperature sensor Graphene comprises the following steps:
(1) it is first 10:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answer in container, stirring reaction 6h at 40 DEG C, after decompression, sucking filtration, washing, puts in the vacuum that temperature is 80 DEG C dry by filtrate
Dry, then grind 10min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 200:1 is dispersed according to weight ratio, is placed in salt
In acid solution, under the conditions of 0-DEG C, 2h is reacted in stirring, is then warming up to 20 DEG C of stirring reaction 1h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 8min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 1 time, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring 5min, is centrifuged sedimentation, takes precipitum
After repetition absolute ethanol washing 1 time, by precipitum dried 8min under conditions of temperature is 100 DEG C, wherein it is centrifuged
Rotating speed is 5000r/min, and the time of each centrifugal sedimentation is 5min.
Embodiment 4:
The preparation method of a kind of temperature sensor Graphene comprises the following steps:
(1) it is first 40:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answering in container, at 60 DEG C, stirring reaction 3h, after decompression, sucking filtration, washing, puts into filtrate in the vacuum that temperature is 100 DEG C
Being dried, then grind 20min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 500:1 is dispersed according to weight ratio, is placed in salt
In acid solution, under the conditions of 0 DEG C, 2h is reacted in stirring, is then warming up to 20 DEG C of stirring reaction 2h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 10min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 2 times, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring min, is centrifuged sedimentation, takes precipitum
After repetition absolute ethanol washing 1 time, by precipitum dried 6min under conditions of temperature is 120 DEG C, wherein it is centrifuged
Rotating speed is 4500r/min, and the time of each centrifugal sedimentation is 4min.
Embodiment 5:
The preparation method of a kind of temperature sensor Graphene comprises the following steps:
(1) it is first 40:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answer in container, stirring reaction 3h at 80 DEG C, after decompression, sucking filtration, washing, puts in the vacuum that temperature is 80 DEG C dry by filtrate
Dry, then grind 20min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 500:1 is dispersed according to weight ratio, is placed in salt
In acid solution, under the conditions of 2 DEG C, 2h is reacted in stirring, is then warming up to 20 DEG C of stirring reaction 1h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 5min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 1 time, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring 5min, is centrifuged sedimentation, takes precipitum
After repetition absolute ethanol washing 1 time, by precipitum dried 5min under conditions of temperature is 100 DEG C, wherein it is centrifuged
Rotating speed is 6000r/min, and the time of each centrifugal sedimentation is 8min.
Embodiment 6:
The preparation method of a kind of temperature sensor Graphene comprises the following steps:
(1) it is first 50:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answering in container, at 80 DEG C, stirring reaction 3h, after decompression, sucking filtration, washing, puts into filtrate in the vacuum that temperature is 120 DEG C
Being dried, then grind 20min, wherein oxygen-free environment is one or more the anaerobic ring being full of in nitrogen, argon, helium
Border；
(2) by dried product in step (1), deionized water is that 100:1 is dispersed according to weight ratio, is placed in salt
In acid solution, under the conditions of 2 DEG C, 2h is reacted in stirring, is then warming up to 20 DEG C of stirring reaction 1h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum
Middle addition deionized water also carries out centrifugal sedimentation after stirring 10min, removes the supernatant, repeats to add deionized water and is centrifuged
Process 2 times, take precipitum adding relative concentration is the dehydrated alcohol of 80%, after stirring 10min, is centrifuged sedimentation, takes sedimentation
After thing repetition absolute ethanol washing 2 times, by precipitum dried 10min, Qi Zhongli under conditions of temperature is 120 DEG C
Heart rotating speed is 6000r/min, and the time of each centrifugal sedimentation is 8min.
Above example only in order to technical scheme to be described, is not intended to limit；Although with reference to previous embodiment
The present invention is described in detail, it will be understood by those within the art that: it still can be to aforementioned each enforcement
Technical scheme described in example is modified, or wherein portion of techniques feature is carried out equivalent；And these amendment or
Replace, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (6)
1. the preparation method of a temperature sensor Graphene, it is characterised in that comprise the following steps:
(1) it is first 10-50:1 mix homogeneously by graphite raw material, sodium hydroxide solvent according to weight ratio, is placed in anaerobic airtight instead
Answer in container, stirring reaction 0.5-6h at 40-120 DEG C, after decompression, sucking filtration, washing, filtrate is vacuum dried, grinds；
(2) by dried product in step (1), deionized water is that 100-1000:1 is dispersed according to weight ratio, is placed in
In hydrochloric acid solution, under the conditions of 0-4 DEG C, 1-4h is reacted in stirring, is then warming up to 20-40 DEG C of stirring reaction 1-2h, obtains suspension；
(3) reacted suspension in step (2) is centrifuged at room temperature sedimentation, removes the supernatant, precipitum adds
Carry out centrifugal sedimentation after entering deionized water and stirring 5-10min, remove the supernatant, repeat to add deionized water centrifugal mistake
Journey 1-2 time, takes precipitum and adds dehydrated alcohol, after stirring 5-10min, be centrifuged sedimentation, take precipitum and repeat dehydrated alcohol
After washing 1-2 time, by precipitum dried.
The preparation method of temperature sensor Graphene the most according to claim 1, it is characterised in that described step
(1) in, oxygen-free environment is one or more the oxygen-free environment being full of in nitrogen, argon, helium.
The preparation method of temperature sensor Graphene the most according to claim 1, it is characterised in that described step
(1) in, vacuum drying temperature is 80-120 DEG C, and milling time is 10-30min.
The preparation method of temperature sensor Graphene the most according to claim 1, it is characterised in that described step
(2) centrifugal rotational speed in is 4500-6000r/min, and the time is 3-8min.
The preparation method of temperature sensor Graphene the most according to claim 1, it is characterised in that described step
(3) relative concentration of the dehydrated alcohol in is 80%.
The preparation method of temperature sensor Graphene the most according to claim 1, it is characterised in that described step
(3) temperature being dried in is 100-120 DEG C, and the time is 5-10min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109304952A (en) * | 2018-09-01 | 2019-02-05 | 哈尔滨工程大学 | A kind of preparation method of the printable formula temperature sensor of the ionic liquid containing pyrenyl |
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| CN102921422A (en) * | 2012-11-06 | 2013-02-13 | 常州大学 | Preparation of magnetic nano Cu-Fe3O4/grapheme composite catalyst and application of composite catalyst in reduction of nitro-compounds |
| CN103864069A (en) * | 2014-03-26 | 2014-06-18 | 天津师范大学 | Method for preparing graphene by taking carbon nanotubes with discontinuous tube walls as raw materials |
| CN104386679A (en) * | 2014-11-13 | 2015-03-04 | 苏州经贸职业技术学院 | Method for preparing graphene oxide and graphene |
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