CN107141514A - A kind of high resiliency graphene is combined deformation sensing material and preparation method and application - Google Patents
A kind of high resiliency graphene is combined deformation sensing material and preparation method and application Download PDFInfo
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- CN107141514A CN107141514A CN201710392056.XA CN201710392056A CN107141514A CN 107141514 A CN107141514 A CN 107141514A CN 201710392056 A CN201710392056 A CN 201710392056A CN 107141514 A CN107141514 A CN 107141514A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
Abstract
The invention belongs to the technical field of deformation sensing material, disclose a kind of high resiliency graphene and be combined deformation sensing material and preparation method and application.Method is：(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；(2) cellulose derivative is stirred with graphene oxide dispersion, stood, freeze-drying obtains graphene oxide/cellulose aerogels；(3) graphene oxide/cellulose aerogels are reduced using reducing agent, heated drying, obtains high resiliency graphene and be combined deformation sensing material.The method of the present invention is simple, efficiently, environmental protection；The material of the present invention has preferably stable sensing capabilities, more than the 4000 continuous quick loading and unloading under 70% strained condition, and is restored to the original state in 1 second, and elastic performance is good；In deformation process, the material has stable, the reliable, electrical response of rule.The material of the present invention is used for deformation sensory field.
Description
Technical field
Deformation sensing material preparing technical field is combined the invention belongs to graphene, and in particular to a kind of high resiliency graphene
Compound deformation sensing material and preparation method and application.
Background technology
Dough deformation sensing material can change into the deformation of material electric signal, and be widely used in automobile, electricity
The various fields such as sub- skin, robot and wearable device.And the graphene with satisfactory electrical conductivity and soft elastic is combined gas
Gel obtains the concern of researcher.Because graphene, which is combined deformation sensing material, to be had electrical conductance height, be quick on the draw, believe
Number response is stable turns into preferable flexible sensing material.
However, three-dimensional grapheme aerogel material between graphene sheet layer due to π-π effects and Van der Waals force due to being sent out
It is raw to reunite, cause the avalanche of deformation process middle skeleton.In order to improve the soft elastic of graphene aerogel sensing material, substantial amounts of section
Grind worker to be combined elastomer macromolecule polymer and graphene, so significantly improve graphene composite aerogel can shape
Denaturation.It is notably, although the addition of substantial amounts of high molecular polymer improves the soft elastic of material, also to hinder simultaneously
Hinder and contacted between graphene film, with reducing material electric conductivity and sensing sensitivity.In addition, most polymer
High molecular polymer in compound deformation sensing material is the high polymer material of difficult degradation, and is original with a large amount of toxic reagents
Material, such as patent application CN104056582A discloses that " a kind of constant pressure and dry prepares graphene cross-linking type organic aerogel and charcoal
The method of aeroge ", its preparing raw material employs the toxic reagents such as Resorcino and formaldehyde, the body of serious threat laboratory staff
Body health.The preparation process of most aeroge deformation sensing material is considerably complicated, for example patent application CN106147226A
" elastic conduction hybrid inorganic-organic aeroge and its preparation method and application " is disclosed, it not only employs such as acetone, four
The toxic reagents such as hydrogen furans, and using the higher nano silver wire of cost as conductive filler, preparation process is also considerably complicated, no
Beneficial to large-scale industrial production.
Therefore, research preparation process is simple, soft elastic better performances, the sensitive environmental type of transducing signal, and biology can
The conductive aeroge deformation sensing material of degraded has very huge practical significance.And nowadays conductive graphene/cellulose can
Degraded aeroge deformation sensing material is even more to be rarely reported.
The content of the invention
In view of the deficiency of existing deformation sensing material, deformation is combined it is an object of the invention to provide a kind of high resiliency graphene
The preparation method of sensing material.
Another object of the present invention is to provide the high resiliency graphene obtained by above-mentioned preparation method to be combined deformation sensing
Material.
It is still another object of the present invention to provide the application that above-mentioned high resiliency graphene is combined deformation sensing material.
The purpose of the present invention is achieved through the following technical solutions：
A kind of high resiliency graphene is combined the preparation method of deformation sensing material, comprises the following steps：
(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；
(2) cellulose derivative is stirred with graphene oxide dispersion, stood, freeze-drying obtains aoxidizing stone
Black alkene/cellulose aerogels；
(3) graphene oxide/cellulose aerogels are reduced using reducing agent, heated drying obtains high resiliency graphite
Alkene is combined deformation sensing material.
Mixing time described in step (2) is 2~4 hours；The time of repose is 2~12 hours；The speed of agitator
For 300-500 revs/min.
The condition of the freeze-drying is -50~-40 DEG C and dried 40~60 hours.
The temperature reduced described in step (3) is 70~80 DEG C, and the time of reduction is 2~4h.
The graphene oxide is obtained by the following method：Using the concentrated sulfuric acid, potassium peroxydisulfate and phosphorus pentoxide are by graphite
Pre-oxidized, then the graphite of pre-oxidation is prepared into by graphene oxide by improved hummers methods.The graphite carries out pre-
Need to be washed using deionized water after oxidation, drying process.The temperature of the drying is 40~60 DEG C.
The concentration of graphene oxide dispersion described in step (1) is 3~7mg/ml.
The temperature stirred described in step (2) is 25~60 DEG C.
Cellulose derivative described in step (2) be sodium carboxymethylcellulose, hydroxyethyl cellulose, hydroxypropyl cellulose,
One or more in hydroxypropyl methyl cellulose.
Graphene oxide and the mass ratio of cellulose derivative 20 in graphene oxide dispersion described in step (2):1~
2:1。
Reducing agent described in step (3) is the one or more in hydrazine hydrate, ascorbic acid or hydroiodic acid.
The reducing agent vapour phase reduction graphene oxide.
The condition of heated drying described in step (3) is to be dried 12~24 hours in 60~120 DEG C.
The high resiliency graphene is combined deformation sensing material and prepared by the above method.
The high resiliency graphene is combined application of the deformation sensing material in deformation sensory field.
The present invention having the beneficial effect that compared with the prior art：
1. the present invention is prepared for a kind of high resiliency graphene and is combined deformation sensing material, the material (i.e. graphene/cellulose
Deformation sensing material) density be 6~8mg/cm3, electrical conductivity (0-70% strains) in deformation range is 6~87S/m；The material
Material more than 4000 continuous quick loading and unloading under 70% strained condition, and restored to the original state in 1 second；, should in deformation process
Material has stable, the reliable, electrical response of rule.
2. the present invention uses environmental protection, biodegradable, and cellulose derivative high polymer material with low cost is carried
The soft elastic of high graphene composite aerogel；
3. preparation method of the present invention is simply efficient, without poisonous polymer reactant, be conducive to industrialized production.
Brief description of the drawings
Fig. 1 is the SEM figures that high resiliency graphene prepared by example 2 is combined deformation sensing material；
Fig. 2 is the stress-strain diagram that high resiliency graphene prepared by example 2 is combined 1000 circulations of deformation sensing material
Figure；
Fig. 3 is combined deformation sensing material 12000 seconds for high resiliency graphene prepared by example 2, and (4000 second compressions recover to follow
Ring) relative resistance R/R0The change in electric of (initial resistance/compression real time resistance)；Small figure in figure is partial enlarged drawing；
Fig. 4 be example 2 in graphene/cellulose strip aeroge rule crooked sensory signal graph；The figure of a, b two is distinguished
Represent resistance variations signal graph of the material when referring to bending and elbow is bent.
Embodiment
The present invention is done with reference to embodiment and accompanying drawing and is further described in detail, but embodiments of the present invention are not limited
In this.
The preparation of graphene oxide：
By 10g flaky graphites and the 100ml concentrated sulfuric acids, 8g potassium peroxydisulfates and 8g phosphorus pentoxides pre-oxidized (80 DEG C,
4 hours), centrifugation, washing (adopt and be washed with deionized to neutrality), dry (50 DEG C are dried in vacuo 12 hours) are pre-oxidized
Graphite；4g is pre-oxidized into graphite, 4g sodium nitrate and the stirring of 104ml sulfuric acid ice bath, 21g potassium permanganate is then added in three batches, instead
4h is answered, moves in 40 DEG C of water-baths and reacts 40min, add 600ml deionized waters, 95 DEG C of insulation 10min is warming up to, adds afterwards
Excess hydrogen peroxide treats that bubble-free is produced, and stands, supernatant liquor falls, and lower floor adds water centrifuge washing to neutrality, 40 DEG C of dryings
12h, obtains graphene oxide.
Embodiment 1
(1) graphene oxide ultrasonic disperse is obtained dense in deionized water (ultrasonic power is 100W, ultrasound 2 hours)
Spend the graphene oxide water solution for 5mg/ml；
(2) sodium carboxymethylcellulose powder is added in graphene oxide water solution made from step (1), 40 DEG C of water-bath bars
Part is stirred together for 2 hours (rotating speed of stirring is 400 revs/min), the wherein quality of graphene oxide and sodium carboxymethylcellulose
Than 20:1, then stand make mixed solution full cross-linked within 12 hours, -40 DEG C of Cheng Bing, then vacuum freeze drying (- 40 DEG C,
20Pa) 60 hours, obtain graphene oxide/cellulose aerogels；
(3) using hydrazine hydrate vapour phase reduction graphene oxide/cellulose aerogels, (reduction temperature is 80 DEG C, recovery time
For 3h, hydrazine hydrate steam reduction aeroge in a kettle .), dried 12 hours in 120 DEG C, obtain high resiliency graphene complex
Become sensing material RGO/CMC-1.The density of material manufactured in the present embodiment is 8g/cm-3, it is highly restorable after compression
50%, electrical conductivity is 6S/m when without strain.
Embodiment 2
(1) graphene oxide ultrasonic disperse is obtained dense in deionized water (ultrasonic power is 100W, ultrasound 2 hours)
Spend the graphene oxide water solution for 5mg/ml；
(2) sodium carboxymethylcellulose powder is added into 40 DEG C of water-bath bars in graphene oxide water solution made from step (1)
Part is stirred together for 2 hours (rotating speed of stirring is 400 revs/min), the wherein quality of graphene oxide and sodium carboxymethylcellulose
Than 10:1, then stand make mixed solution full cross-linked within 12 hours, -40 DEG C of Cheng Bing, then vacuum freeze drying (- 40 DEG C,
20Pa) 60 hours, obtain graphene oxide/cellulose aerogels；
(3) using hydrazine hydrate vapour phase reduction graphene oxide/cellulose aerogels, (reduction temperature is 80 DEG C, recovery time
For 3h, hydrazine hydrate steam reduction aeroge in a kettle .), dried 12 hours in 120 DEG C, obtain high resiliency graphene complex
Become sensing material RGO/CMC-2.
The SEM figures that high resiliency graphene manufactured in the present embodiment is combined deformation sensing material are as shown in Figure 1；1000 circulations
Stress-strain curve diagram it is as shown in Figure 2.
The density of material manufactured in the present embodiment is 6g/cm-3, it is elastic preferable, after 70% strain compression 4000 times highly still
The 97% of resilient, electrical conductivity is 10S/m when without strain, and electrical conductivity is 87S/m during 70 strain.
The relative resistance R/R of material manufactured in the present embodiment 12000 seconds (4000 second compressions recover circulation)0(initial resistance/
Compress real time resistance) change in electric figure it is as shown in Figure 3；Rule crooked sensory signal graph is as shown in figure 4, the figure of wherein a, b two
Resistance variations signal graph of the material when referring to bending and elbow is bent is represented respectively.From the figure 3, it may be seen that the material of the present embodiment has stabilization
Sensing capabilities, compression 4000 times after response signal still stablize.As shown in Figure 4, the material tool of the present embodiment is regular curved
Song response.
Embodiment 3
(1) graphene oxide ultrasonic disperse is obtained dense in deionized water (ultrasonic power is 100W, ultrasound 2 hours)
Spend the graphene oxide water solution for 5mg/ml；
(2) sodium carboxymethylcellulose powder is added into 40 DEG C of water-bath bars in graphene oxide water solution made from step (1)
Part is stirred together for 2 hours (rotating speed of stirring is 400 revs/min), the wherein quality of graphene oxide and sodium carboxymethylcellulose
Than 5:1, then standing makes mixed solution full cross-linked in 12 hours, -40 DEG C of Cheng Bing, then vacuum freeze drying (- 40 DEG C, 20Pa)
60 hours, obtain graphene oxide/cellulose aerogels；
(3) using hydrazine hydrate vapour phase reduction graphene oxide/cellulose aerogels, (reduction temperature is 80 DEG C, recovery time
For 3h, hydrazine hydrate steam reduction aeroge in a kettle .), dried 12 hours in 120 DEG C, obtain final high resiliency graphene
Compound deformation sensing material RGO/CMC-3.The density of material manufactured in the present embodiment is 6.7g/cm-3, typically, 70% should for elasticity
Highly restorable 80% after variable compression 10 times, electrical conductivity is 8.6S/m when without strain.
Embodiment 4
(1) graphene oxide ultrasonic disperse is obtained dense in deionized water (ultrasonic power is 100W, ultrasound 2 hours)
Spend the graphene oxide water solution for 5mg/ml；
(2) sodium carboxymethylcellulose powder is added into 40 DEG C of water-bath bars in graphene oxide water solution made from step (1)
Part is stirred together for 2 hours (rotating speed of stirring is 400 revs/min), the wherein quality of graphene oxide and sodium carboxymethylcellulose
Than 2:1, then standing makes mixed solution full cross-linked in 12 hours, -40 DEG C of Cheng Bing, then vacuum freeze drying (- 40 DEG C, 20Pa)
60 hours, obtain graphene oxide/cellulose aerogels；
(3) using hydrazine hydrate vapour phase reduction graphene oxide/cellulose aerogels, (reduction temperature is 80 DEG C, recovery time
For 3h, hydrazine hydrate steam reduction aeroge in a kettle .), dried 12 hours in 120 DEG C, obtain final high resiliency graphene
Compound deformation sensing material RGO/CMC-4.The density of material manufactured in the present embodiment is 7.3g/cm-3, 70% strain compression 10 times
Afterwards highly restorable 76%, electrical conductivity is 9.2S/m when without strain.
Embodiment 5
(1) graphene oxide ultrasonic disperse is obtained dense in deionized water (ultrasonic power is 100W, ultrasound 2 hours)
Spend the graphene oxide water solution for 5mg/ml；
(2) it is 40 DEG C of water bath conditions in graphene oxide water solution made from hydroxyethyl cellulose addition step (1) are common
Stirring 2 hours, the wherein mass ratio 10 of graphene oxide and hydroxyethyl cellulose:1, then standing fills mixed solution in 12 hours
Divide and be crosslinked, -40 DEG C of Cheng Bing, then vacuum freeze drying (- 40 DEG C, 20Pa) 60 hours, obtain graphene oxide/cellulose airsetting
Glue；
(3) using hydrazine hydrate vapour phase reduction graphene oxide/cellulose aerogels, (reduction temperature is 80 DEG C, recovery time
For 3h, hydrazine hydrate steam reduction aeroge in a kettle .), dried 12 hours in 120 DEG C, obtain high resiliency graphene complex
Become sensing material.Material manufactured in the present embodiment is similar to Example 2.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not limited by examples detailed above
System, it is other it is any without departing from spirit of the invention and the change made under principle, modification, replacement, combine, simplification is
Effect.
Claims (10)
1. a kind of high resiliency graphene is combined the preparation method of deformation sensing material, it is characterised in that：Comprise the following steps：
(1) graphene oxide ultrasonic disperse is obtained into graphene oxide dispersion in water；
(2) cellulose derivative is stirred with graphene oxide dispersion, stand, freeze-drying, obtain graphene oxide/
Cellulose aerogels；
(3) graphene oxide/cellulose aerogels are reduced using reducing agent, heated drying, obtains high resiliency graphene and answer
Close deformation sensing material.
2. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(2) mixing time described in is 2~4 hours；The time of repose is 2~12 hours；The temperature stirred described in step (2) is
25~60 DEG C.
3. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(2) condition being freeze-dried described in is -50~-40 DEG C and dried 40~60 hours.
4. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(3) temperature reduced described in is 70~80 DEG C, and the time of reduction is 2~4h.
5. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(2) cellulose derivative described in is sodium carboxymethylcellulose, and hydroxyethyl cellulose, hydroxypropyl cellulose, hydroxypropyl methyl is fine
One or more in dimension element；
Reducing agent described in step (3) is the one or more in hydrazine hydrate, ascorbic acid or hydroiodic acid.
6. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(2) graphene oxide and the mass ratio of cellulose derivative 20 in graphene oxide dispersion described in:1~2:1.
7. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(1) concentration of graphene oxide dispersion described in is 3~7mg/ml；
The condition of heated drying described in step (3) is to be dried 12~24 hours in 60~120 DEG C.
8. high resiliency graphene is combined the preparation method of deformation sensing material according to claim 1, it is characterised in that：Step
(1) graphene oxide is obtained by the following method described in：Using the concentrated sulfuric acid, potassium peroxydisulfate and phosphorus pentoxide carry out graphite
Pre-oxidation, then the graphite of pre-oxidation is prepared into by graphene oxide by improved hummers methods.
9. the high resiliency graphene that a kind of preparation method as described in any one of claim 1~8 is obtained is combined deformation sensing material
Material.
10. high resiliency graphene is combined the application of deformation sensing material according to claim 9, it is characterised in that：The height
Elastic graphite alkene is combined application of the deformation sensing material in deformation sensory field.
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| PCT/CN2017/115855 WO2018218930A1 (en) | 2017-05-27 | 2017-12-13 | High elastic deformation sensing graphene composite material, preparation method therefor, and use thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107840971A (en) * | 2017-10-27 | 2018-03-27 | 华南理工大学 | It is a kind of that from adhering to, wearable power is quick to sense composite aquogel and preparation method thereof |
| CN108148224A (en) * | 2017-12-12 | 2018-06-12 | 明基材料有限公司 | Graphene/cellulose composite aerogel and its manufacturing method |
| TWI637990B (en) * | 2017-11-29 | 2018-10-11 | 明基材料股份有限公司 | Graphene/cellulose aerogel composite and manufacturing method thereof |
| WO2018218930A1 (en) * | 2017-05-27 | 2018-12-06 | 华南理工大学 | High elastic deformation sensing graphene composite material, preparation method therefor, and use thereof |
| CN109559851A (en) * | 2018-11-15 | 2019-04-02 | 中南大学 | A kind of graphene electrocardioelectrode and preparation method thereof |
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| CN107840971A (en) * | 2017-10-27 | 2018-03-27 | 华南理工大学 | It is a kind of that from adhering to, wearable power is quick to sense composite aquogel and preparation method thereof |
| TWI637990B (en) * | 2017-11-29 | 2018-10-11 | 明基材料股份有限公司 | Graphene/cellulose aerogel composite and manufacturing method thereof |
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| CN108148224A (en) * | 2017-12-12 | 2018-06-12 | 明基材料有限公司 | Graphene/cellulose composite aerogel and its manufacturing method |
| CN112341671A (en) * | 2017-12-12 | 2021-02-09 | 明基材料有限公司 | Graphene/cellulose composite aerogel and manufacturing method thereof |
| CN110161080A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | The preparation method of highly sensitive gas sensor based on graphene aerogel |
| CN109559851A (en) * | 2018-11-15 | 2019-04-02 | 中南大学 | A kind of graphene electrocardioelectrode and preparation method thereof |
| CN110375637A (en) * | 2019-08-13 | 2019-10-25 | 电子科技大学 | A kind of composite conducting elastomer selfreparing strain transducer and preparation method thereof |
| CN112662099A (en) * | 2020-12-11 | 2021-04-16 | 广东彩乐智能包装科技有限公司 | Stress sensing conductive aerogel and preparation method thereof |
| CN112852145A (en) * | 2021-01-08 | 2021-05-28 | 天津科技大学 | Novel nanocellulose-based pressure sensing material and preparation method thereof |
| CN113716551A (en) * | 2021-08-30 | 2021-11-30 | 中国科学院兰州化学物理研究所 | Three-dimensional graphene superelastomer, preparation method and application thereof, and flexible piezoresistive sensor |
| CN114350030A (en) * | 2021-12-30 | 2022-04-15 | 华南理工大学 | Biomass-based aerogel photothermal material and preparation method and application thereof |
| CN115746379A (en) * | 2022-11-10 | 2023-03-07 | 中国科学院兰州化学物理研究所 | Three-dimensional graphene composite aerogel and preparation method and application thereof |
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