CN104801244A - Method for preparing three-dimensional graphene-copper nanowire composite aerogel - Google Patents
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 48
- 239000010949 copper Substances 0.000 title claims abstract description 48
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- 239000002070 nanowire Substances 0.000 title claims abstract description 42
- 239000004964 aerogel Substances 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 29
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 14
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 7
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 7
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 7
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 3
- 230000006835 compression Effects 0.000 abstract description 13
- 238000007906 compression Methods 0.000 abstract description 13
- 239000000017 hydrogel Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000005457 ice water Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing three-dimensional graphene-copper nanowire composite aerogel. The method comprises the following steps: first, preparing copper nanowires; mixing the copper nanowires and an oxidized graphene solution into an ethylene glycol solution; adding ascorbic acid which serves as a reducing agent; carrying out hydrothermal reaction to obtain three-dimensional graphene-copper nanowire composite hydrogel; finally, washing the three-dimensional graphene-copper nanowire composite hydrogel with a hydrazine hydrate solution which is 0.5 wt%; carrying out freeze-dry treatment to obtain the three-dimensional graphene-copper nanowire composite aerogel. The three-dimensional graphene-copper nanowire composite aerogel adopts a three-dimensional porous structure, and has the advantages of being high in compression performance, low in density, high in electric conductivity and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, particularly relate to a kind of preparation method of simple three-dimensional grapheme-copper nano-wire composite aerogel.
Background technology
Graphene, as the unique two-dimension nano materials of one, has the mechanical performance of specific area is large, electron mobility is high, good heat endurance and brilliance, has been widely used in the fields such as electronic device, energy storage, chemical catalysis, environmental pollution improvement.The preparation of laboratory Graphene generally adopts with low cost, the simple oxidation-reduction method of preparation technology, by preparing graphene oxide, then through the cheaper alternative of redox graphene as Graphene.In recent years, three-dimensional grapheme material becomes the study hotspot preparing functionalization graphene material gradually.Relative to original graphite alkene, three-dimensional grapheme, due to its three-dimensional porous structure, has high porosity, large specific area and the feature such as easy to be recycled, is therefore widely used in pollutant adsorbing domain.In addition, good compression performance, higher electrical conductivity, low-density advantage, make it apply on sensor research direction and have great potentiality.But by three-dimensional grapheme prepared by hydro-thermal method, easily cave in, mechanical stability is poor, the requirement in practical application cannot be met.
Copper nano-wire is as one-dimensional metal nano material, and the general character not only with nano material also has its special performance.As: the electron transport ability that one-dimensional square is upwards remarkable, good pliability and catalytic performance.The present invention adopts hydro-thermal method, build three-dimensional grapheme-copper nano-wire composite aquogel, finally composite aerogel is obtained again by freeze drying, not only maintain three-dimensional grapheme three-dimensional porous structure, because adding of copper nanometer enhances its compression performance and mechanical stability, and improve its electric conductivity.
Summary of the invention
For the problem of existing three-dimensional grapheme Material compression performance difference, the object of the invention is to: the preparation method that a kind of three-dimensional grapheme-copper nano-wire composite aerogel is provided.Described composite aerogel good compression property, and preparation method is simple, cost is low, repeatability is high.
The object of the invention is to be achieved through the following technical solutions: the preparation method of a kind of three-dimensional grapheme-copper nano-wire composite aerogel, the method comprises the following steps:
(1) in ethylene glycol, add copper nano-wire, after being uniformly dispersed, add ascorbic acid, add the graphene oxide water solution that concentration is 8mg/ml after being uniformly dispersed, obtain mixed solution; The concentration of graphene oxide in mixed solution is 0.8-1.5mg/ml; The mass ratio of ascorbic acid and graphene oxide is 2:1; The concentration of copper nano-wire in mixed solution is 0.1-0.3mg/ml;
(2) mixed solution that step 1 obtains is transferred to hydrothermal reaction kettle, at 160 DEG C, reacts 6h, reaction terminates rear Temperature fall to room temperature (25 DEG C), obtains composite aquogel;
(3) column composite aquogel is placed in the hydrazine hydrate solution washing by soaking 24h of 0.5wt%, and every 8h changes a hydrazine hydrate solution;
(4), after the composite aquogel washes clean after step 3 being processed, three-dimensional grapheme-copper nano-wire composite aerogel is obtained by freeze drying.
Beneficial effect of the present invention is: the method for the invention prepares that three-dimensional grapheme-copper nano-wire composite aerogel size is controlled, simple for process, abundant raw materials, with low cost, be easy to promote.Prepared three-dimensional grapheme-copper nano-wire composite aerogel has three-dimensional porous structure, and specific area is large, density is little, electrical conductivity high.And owing to adding copper nano-wire, composite aerogel has good compression performance and mechanical stability.In sum, these features make this composite aerogel have huge application prospect in pollutant absorption, ultracapacitor, sensor field.
Accompanying drawing explanation
Fig. 1 is the exterior appearance of three-dimensional grapheme-copper nano-wire composite aerogel prepared by the present invention;
Fig. 2 is the scanning electron microscopic picture of three-dimensional grapheme-copper nano-wire composite aerogel that reference B reactant ratio obtains;
Fig. 3 is the scanning electron microscopic picture of three-dimensional grapheme-copper nano-wire composite aerogel that reference C reactant ratio obtains;
Fig. 4 is the XRD picture of three-dimensional grapheme-copper nano-wire composite aerogel prepared by the present invention;
Fig. 5 is the audio-visual picture before the compression verification compression of three-dimensional grapheme-copper nano-wire composite aerogel prepared by the present invention, after compression neutralization compression.
Detailed description of the invention
The present invention prepares a kind of three-dimensional grapheme-copper nano-wire composite aerogel.Graphene has as a kind of special two-dimension nano materials the heat endurance and mechanical performance that specific area is large, electron mobility is high, good.The present invention adopts the graphene oxide solution of low concentration to form three dimensional hydrogel structure by the self assembly of hydro-thermal reaction redox graphene, and the π-π formed between graphene film and sheet ensure that the stability of this structure.Copper nanometer is evenly distributed in this three-dimensional structure, the effect that composite aerogel not only structurally provides support is formed with Graphene, enhance the stability of structure, and the machinery of this composite aerogel and electric property are improved due to the good pliability of copper nano-wire and remarkable electron transport ability.This aeroge has three-dimensional porous structure in sum, and specific area is large, density is little, electrical conductivity is high, good compression performance and mechanical stability.
Further illustrate technical solution of the present invention below in conjunction with specific embodiment, these embodiments can not be interpreted as it is restriction to technical solution.
The preparation method of the graphene oxide in following examples is: slowly by the 270ml concentrated sulfuric acid/phosphoric acid mixing acid (H in ice-water bath
2sO
4: H
3pO
3=9:1, V/V) drop to and be equipped with in 2g natural graphite powder beaker and keep stirring, slowly add 12g potassium permanganate subsequently, after mixing, beaker is transferred in 50 DEG C of water-baths and reacts 12h.After completion of the reaction, 300ml frozen water is added in beaker, after being cooled to room temperature, then drip 5ml 30% hydrogen peroxide, obtain glassy yellow product.Finally product is used respectively hydrochloric acid, deionized water centrifuge washing, until pH=6, rotating speed is 8000r/min, and last freeze drying obtains graphene oxide.
The preparation method of copper nano-wire is: preparation method is according to the people such as the Y.Chang (Y.Chang that disclosed method is carried out on Langmuir; M.L.Lye; H.C.Zeng; Large-Scale Synthesis of High-QualityUltralong Copper Nanowires.Langmuir, 2005,21,3746-3748.).Be specially: the NaOH solution of configuration 15M, get 20ml and to be added in single port flask and heating water bath to 60 DEG C, drip 1ml 0.1MCu (NO
3)
2to NaOH solution and vigorous stirring, then add 0.16ml anhydrous ethylenediamine successively, 25ul mass fraction is the N of 35%
2h
4the aqueous solution, after stirring 45s, leaves standstill reaction 90min.After completion of the reaction, flask is placed in ice-water bath, after being cooled to 10 DEG C, being suspended with the product of one deck rufous at superjacent, sopping up solution with dropper, retain the rufous product on upper strata, finally use water and alcohol mixed solution centrifuge washing rufous product, centrifugal rotational speed 6000rpm/min, centrifugation time 10min, repeated washing 5 times, obtains copper nano-wire powder after vacuum drying.
Embodiment 1
Be added to the water by obtained graphite oxide, ultrasonic 4h obtains graphene oxide water solution, and wherein graphene oxide solution concentration is 8mg/ml.Get 4 beakers (being labeled as A ~ D respectively respectively) and add 18ml, 18ml, 16.25ml, 16.25ml ethylene glycol respectively, make the amount in 4 beakers equal, in beaker, add copper nano-wire, ascorbic acid, graphene oxide solution according to the proportioning shown in table 1 successively; Finely dispersed mixed solution is formed by mechanical agitation and ultrasonic wave process after often kind of material adds.Again mixed solution in beaker is transferred in the polytetrafluoroethyllining lining of autoclave respectively, reactor is reacted 6h as in 160 DEG C of air dry ovens, after question response terminates, by reactor Temperature fall to room temperature (25 DEG C), obtain three-dimensional grapheme-copper nano-wire composite aquogel.Taken out by the column composite aquogel be obtained by reacting, as the hydrazine hydrate solution washing by soaking 24h of 0.5wt%, and every 8h changes a hydrazine hydrate solution.Finally the product freeze drying of washes clean is obtained three-dimensional grapheme-copper nano-wire composite aerogel.
Table 1. reactant ratio
| A | B | C | D | |
| Ethylene glycol (ml) | 18 | 18 | 16.25 | 16.25 |
| Copper nano-wire (mg) | 2 | 4 | 4 | 6 |
| Ascorbic acid (mg) | 32 | 32 | 60 | 30 |
| Graphene oxide solution (ml) | 2 | 2 | 3.75 | 3.75 |
Fig. 1 is the three-dimensional grapheme-copper nano-wire composite aerogel audio-visual picture obtained with reference to B reactant ratio, and aeroge is cylindric, measures its density and is about 2.5mg/cm
3.
Fig. 2,3 be respectively the three-dimensional grapheme-copper nano-wire composite aerogel obtained with reference to B and C reactant ratio scanning electron microscopic picture (due to the scanning electron microscopic picture of A and D and B and C similar, therefore no longer illustrate), obviously can find out the fold of Graphene, copper nano-wire, three-dimensional porous microstructure in figure.Three-dimensional porous structure is formed owing to forming pi-pi bond between two-dimensional graphene, copper nanometer is interspersed to be distributed in graphene three-dimensional structure, and three-dimensional grapheme-copper nano-wire composite aerogel is had, and specific area is large, low-density, good mechanical performance and high conductivity.
The XRD collection of illustrative plates of three-dimensional grapheme-copper nano-wire composite aerogel that Fig. 4 obtains for reference B reactant ratio, as can be seen from the figure Graphene (002) diffraction maximum occurred at 24.3 °, with copper face-centered cubic crystal structure (111), (200), (220) diffraction maximum, show that in product, graphene oxide is reduced, only have elemental copper to exist, there is not other oxide of copper.
Fig. 5 is the three-dimensional grapheme-copper nano-wire composite aerogel pictorial diagram obtained, and compressed by sample, to about 40% of original height after compression, after unclamping pressure, sample returns back to original, uncompressed state.
According to above result, the three-dimensional grapheme that the present invention prepares-copper nano-wire composite aerogel density is little, electrical conductivity is high, good compression property, mechanical stability are strong, and this composite aerogel can adsorb at pollutant, are used widely in ultracapacitor, sensor field.
Claims (1)
1. a preparation method for three-dimensional grapheme-copper nano-wire composite aerogel, it is characterized in that, the method comprises the following steps:
(1) in ethylene glycol, add copper nano-wire, after being uniformly dispersed, add ascorbic acid, add the graphene oxide water solution that concentration is about 8mg/ml after being uniformly dispersed, obtain mixed solution; The concentration of graphene oxide in mixed solution is about 0.8-1.5mg/ml; The mass ratio of ascorbic acid and graphene oxide is about 2:1; The concentration of copper nano-wire in mixed solution is about 0.1-0.3mg/ml;
(2) mixed solution that step 1 obtains is transferred to hydrothermal reaction kettle, at 160 DEG C, reacts about 6h, reaction terminates rear Temperature fall to room temperature, obtains column composite aquogel;
(3) column composite aquogel is placed in the hydrazine hydrate solution washing by soaking 24h of 0.5wt%, and every 8h changes a hydrazine hydrate solution;
(4), after the composite aquogel washes clean after step 3 being processed, three-dimensional grapheme-copper nano-wire composite aerogel is obtained by freeze drying.
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| CN105499600A (en) * | 2015-12-15 | 2016-04-20 | 中国科学院上海高等研究院 | Method for preparing silver nanowire-graphene composite aerogel |
| CN105551327A (en) * | 2016-03-07 | 2016-05-04 | 浙江理工大学 | Interactive pronunciation correcting system and method based on soft electronic skin |
| CN105583408A (en) * | 2015-12-22 | 2016-05-18 | 浙江理工大学 | Preparation method and application of Cu nanowire-reduced graphene oxide three-dimensional porous film |
| CN105772741A (en) * | 2016-04-26 | 2016-07-20 | 中国科学院深圳先进技术研究院 | Three-dimensional structure aerogel with copper nanowires coated with graphene and preparation method of three-dimensional structure aerogel and application of three-dimensional structure aerogel |
| CN105788875A (en) * | 2016-03-02 | 2016-07-20 | 西北师范大学 | Cobaltosic oxide nanowire/reduction-oxidization graphene hydrogel composite material and preparation method and application therefor |
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| CN106653159A (en) * | 2016-12-29 | 2017-05-10 | 中国科学院深圳先进技术研究院 | Preparation method and application for composite elastomer containing graphene coated copper nanowire |
| CN106683909A (en) * | 2017-01-23 | 2017-05-17 | 信阳师范学院 | In-situ preparation method for cubic copper oxide/graphene aerogel composite material |
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| CN113039152A (en) * | 2018-08-30 | 2021-06-25 | 纽约州立大学研究基金会 | Graphene material-metal nanocomposite material and preparation and use methods thereof |
| CN113039152B (en) * | 2018-08-30 | 2023-01-10 | 纽约州立大学研究基金会 | Graphene material-metal nanocomposite material and preparation and use methods thereof |
| CN110860287A (en) * | 2019-11-07 | 2020-03-06 | 湖北工业大学 | Preparation method of graphene/copper nanocrystalline composite catalytic material |
| CN110860287B (en) * | 2019-11-07 | 2022-08-19 | 湖北工业大学 | Preparation method of graphene/copper nanocrystalline composite catalytic material |
| CN111250007A (en) * | 2020-01-17 | 2020-06-09 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Preparation method of pure metal aerogel and flexible composite material |
| CN111268669A (en) * | 2020-01-20 | 2020-06-12 | 洛阳理工学院 | Preparation method of graphene/silver nanowire composite aerogel |
| CN112588276A (en) * | 2020-12-30 | 2021-04-02 | 南京中设石化工程有限公司 | Absorbent for absorbing ethylene in methanol-to-olefin reaction product and process thereof |
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