CN106248747A - A kind of preparation method of Graphene mesoporous indium oxide nano composite material - Google Patents
A kind of preparation method of Graphene mesoporous indium oxide nano composite material Download PDFInfo
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- CN106248747A CN106248747A CN201610522224.8A CN201610522224A CN106248747A CN 106248747 A CN106248747 A CN 106248747A CN 201610522224 A CN201610522224 A CN 201610522224A CN 106248747 A CN106248747 A CN 106248747A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of method preparing Graphene mesoporous indium oxide nano composite material.Graphite flake is electrolysed in the electrolyte that eutectic ionic liquid and water form by the method for the present invention, forms graphite flake layer；In oxygen-free environment, microwave, ultrasonic in combination are peeled off, and by gained solution centrifugal, clean and dry deposit, obtaining high-quality Graphene；By the most ultrasonic to Graphene and mesoporous indium oxide nano-particle, sucking filtration is also dried, and obtains Graphene mesoporous indium oxide nano composite material.The present invention uses electrochemical process, and equipment needed thereby is simple, and energy consumption is low；Raw material and electrolyte reusable edible, environmental protection；By Graphene and mesoporous indium oxide nano-particle are combined, it is greatly promoted the gas sensing property of material, is a kind of material preparation method with commercial application value；Prepared Graphene mesoporous indium oxide nano composite material has a wide range of applications potentiality at gas sensor domain.
Description
Technical field
The present invention relates to the preparation method of a kind of Graphene-mesoporous indium oxide nano composite material.
Background technology
Graphene is a kind of New Two Dimensional material with carbon element, and carbon atom forms monolayer two dimension honeybee with hexatomic ring form periodic arrangement
Nest shape structure.Graphene has good pliability, heat conductivity (heat conductivity 5300W/m*K), (resistivity is about for electric conductivity
10-6), optical characteristics, chemical stability and high electron mobility be (more than 15000cm under room temperature2/ V*s), high-specific surface area
(2600m2/ g) etc., it is with a wide range of applications in various fields such as mobile device, Aero-Space, new forms of energy batteries.2004
Year, two scientist An Delie Jim of Univ Manchester UK and the Ke Siteyanuowo love that disappears is shelled by micromechanics
Obtain first from method can the single-layer graphene of stable existence, pushed gate prepared by Graphene open.The most common Graphene system
Preparation Method predominantly organic tool stripping method, oxidation-reduction method, silicon carbide epitaxial growth method and chemical vapour deposition technique.Wherein machinery stripping
Low from method production efficiency；Oxidation-reduction method is the highest to equipment requirements, and preparation process is relatively simple, but the Graphene quality obtained
Relatively low, chemical reaction process produces a large amount of pollution；The Graphene matter that silicon carbide epitaxial growth method and chemical vapour deposition technique produce
Measuring higher, but it is few to there is yield, energy consumption is high, high in cost of production problem.The electrochemical stripping method of graphite is a kind of emerging graphite
Alkene preparation method, the advantages such as it is simple that it has preparation condition, low cost, environmental protection, high-quality Graphene can be obtained and produce
Product.
Gas sensor is the important branch of Modern Transducer Technology.Development and growth in the living standard, people along with science and technology
For the monitoring pay attention to day by day of indusrial toxic harmful gas and room air pollution, therefore find hypersensitivity, high selectivity,
The gas sensitive of high stability becomes the task of top priority.Indium sesquioxide. is that one has highly sensitive semiconductor gas to specific gas
Quick material, its specific surface area of nominal increase can produce more avtive spot from the teeth outwards, thus improve its gas-sensitive property.
But the Indium sesquioxide. material prepared of conventional method is owing to easily reuniting and sintering is grown up, and causes loss and the sensitivity of specific surface area
Declining, its gas sensing property does not reaches the requirement of commercial Application.Mesoporous indium oxide nanoparticle is combined by the present invention with Graphene, can
To efficiently reduce reunion, substantially increase the specific surface area of Indium sesquioxide. nano-particle, this composite for methane, methanol,
The gases such as ethanol, acetaldehyde, acetone have good air-sensitive performance.
Summary of the invention
For above problems of the prior art, the present invention proposes one and utilizes electrochemical process to prepare Graphene to receive
The method of nano composite material.
The preparation method of the graphene nanocomposite material of the present invention, comprises the following steps:
1) two panels graphite flake is connected with power positive cathode respectively as electrode；
2) described electrode is inserted in electrolyte solution, first add 1-5V DC voltage, keep 1-10 minute, carry out preliminary electricity
Solving, then making alive is 5-10V, the persistent period is the 1-5 second, and interval time is the pulse voltage of 1-5 second, is electrolysed 0.5-2 hour, obtains
Obtain graphite flake layer；
3) described electrolyte is placed in oxygen-free environment, carries out microwave, ultrasonic in combination stripping, make graphite flake layer be separated into graphite
Alkene；
4) electrolyte is centrifuged, isolates Graphene, with washing with alcohol, vacuum drying；
5) mesoporous indium oxide nano-particle and Graphene are joined in deionized water, ultrasonic 10-60 minute, be allowed to uniform
Distribution.Sucking filtration, is dried 12-24 hour under 60-80 vacuum environment, can obtain Graphene-mesoporous indium oxide nano composite material.
6) alternatively, in step 5) mesoporous indium oxide nano-particle and graphene solution in add silver nano-grain, super
Sound 10-60 minute, is allowed to be uniformly distributed.Sucking filtration, is dried 12-24 hour under 60-80 vacuum environment, can obtain Graphene-mesoporous
Indium sesquioxide .-silver trielement composite material, can further improve the material sensitivity for gases such as formaldehyde.
Wherein, in step 1) in, graphite flake includes but not limited to high purity graphite, high starch breeding, tabletting graphite etc..Power supply
The voltage of 0-20V can be provided, potential pulse can be generated.
In step 2) in, electrolyte solution is eutectic ionic liquid, by organic cation and inorganic or organic anion
Composition, includes but not limited to carbamide/zinc chloride, carbamide/iron chloride, carbamide/tin trichloride, carbamide/ammonium nitrate, hexanediol/chlorine
Change zinc, choline chloride/zinc chloride, choline chloride/glycerol, acetamide/potassium rhodanate, carbamide/acetamide/ammonium nitrate, carbamide/
Ammonium nitrate/rhodan ammoniums etc., eutectic ionic liquid can be made up of two kinds to four kind of compounds.Electrolyte solution can add few
Amount deionized water, addition is less than the volume of eutectic ionic liquid.A small amount of surfactant is added in electrolyte solution,
Such as hexadecyltrimethylammonium chloride etc., can increase electrolytic efficiency further, surface-active contents is 0-1-1mg/ml.
In step 3) in, above-mentioned electrolyte to be put in 500-2000 watt of microwave, splitting time is 1-10 minute, at the beginning of carrying out
Step peel off, more above-mentioned electrolyte is put in ultrasonic cleaner use 100% power ultrasonic shake 5-20 minute, by graphite
The alkene degree of depth separates.Microwave and ultrasonic in combination are peeled off and Graphene can be made fully to peel off and be scattered in electrolyte.
In step 4) in, electrolyte with the centrifugation 5 minutes of 1000 turns per minute, is removed centrifugal in high speed centrifuge
Pipe basic sediment.Take supernatant with 10000 turns per minute, within centrifugal 10-30 minute, to solid-liquid separation, supernatant is removed, follows
Ring utilizes.Adding EtOH Sonicate concussion and disperse centrifugation the most again to graphene uniform, this step is in triplicate.By institute
Obtain Graphene and be placed under 60-80 vacuum environment dry 12-24 hour.
In step 5) in, mesoporous indium oxide nano-particle can be prepared as follows: first uses hydro-thermal method under 25-35
Synthesizing mesoporous silicon dioxide, adds in a small amount of ethanol by above-mentioned silicon dioxide and nitric hydrate indium, stirs in Teflon beaker
5-20 minute, until solvent volatilizees completely.Remaining solid is put in ceramic crucible, batch-type furnace is heated to 250 holdings three
Hour.Add sodium hydroxide solution the most in the product, dissolve mesoporous silicon oxide.By gained solution centrifugal, after outwelling supernatant,
Being washed with deionized three times, drying can obtain mesoporous indium oxide nano-particle, and the aperture of above-mentioned mesoporous indium oxide nano-particle is
2-50 nanometer.
Advantages of the present invention:
The present invention mainly uses electrochemical process to prepare Graphene-mesoporous indium oxide nano composite material, and equipment needed thereby is simple,
Energy consumption is low；Raw material and electrolyte reusable edible, environmental protection.Graphene-mesoporous indium oxide nano composite material the shape of preparation
Looks are complete, and defect is few, and specific surface area is big, and gas sensing property is high.
Accompanying drawing explanation
Fig. 1 is the Graphene according to embodiment of the present invention-mesoporous indium oxide nano composite material schematic diagram；
Fig. 2 is the Graphene-mesoporous indium oxide according to embodiment of the present invention-silver ternary nano composite material signal
Figure；
Label declaration:
1, Graphene；2, mesoporous indium oxide nano-particle；3, Graphene；4, silver nano-grain；5, mesoporous indium oxide nanometer
Granule；
Detailed description of the invention
Below in conjunction with the accompanying drawings, by embodiment, the present invention will be further described.
Embodiment one
The preparation method of the Graphene of the present embodiment-mesoporous indium oxide nano composite material, comprises the following steps:
1) two panels 4cm*10cm*0.5cm strip high purity graphite sheet is connected with power positive cathode respectively as electrode, electricity
Source voltage is adjustable in the range of 0-20V, can generate potential pulse；
2) choline chloride and zinc chloride being mixed according to the ratio 1: 2 of the amount of material, on magnetic stirring apparatus, 80 heating 5 are little
Time, after solid starts to melt, start stirring until forming colourless transparent liquid.Aforesaid liquid is put into 70 drying 12 in baking oven
Hour, put in drying baker standby；
3) 150ml choline chloride/zinc chloride (embodiment two can use choline chloride/glycerol, 60) eutectic ion is taken
Liquid is put in 500ml beaker, adds 150ml deionized water, stirs, and the 1mol/L sodium hydroxide adding 3ml is molten
Liquid makes electrolyte ph be 12.Being inserted by described electrode in electrolyte, immersing part is 5cm, and electrode spacing is 3cm, in electrolysis
Liquid adds 50mg surfactant hexadecyltrimethylammonium chloride, and is heated to 90.First add 5V DC voltage, keep 5 points
Clock, then making alive is 10V, the persistent period is 5 seconds, and the pulse spacing is the pulse voltage of 2 seconds, is electrolysed 1 hour, it is thus achieved that graphite flake
Layer；
4) being put into by electrolyte in 1000 watts of microwaves, splitting time is 5 minutes, tentatively peels off, then by above-mentioned electrolysis
Liquid is put into and is used the power ultrasonic of 100% to shake in ultrasonic cleaner 20 minutes, the Graphene degree of depth is separated.
5) electrolyte is put into the centrifugation 5 minutes with 1000 turns per minute in high speed centrifuge, removes at the bottom of centrifuge tube
Portion's deposit, can recycle as graphite electrode after deposit tabletting.Take supernatant and leave 15 points of the heart with per minute 10000
Clock, removes supernatant.Add the concussion of 20ml EtOH Sonicate and disperse centrifugation the most again to graphene uniform, repeat this step
Rapid three times.Gained Graphene is placed under 70 vacuum environments and is dried 12 hours.
6) at 35 times with polymer, butanol, hydrochloric acid for starting material with water full-boiled process synthesizing mesoporous silicon dioxide, by above-mentioned titanium dioxide
Silicon and nitric hydrate indium add in 10ml ethanol, stir 10 minutes, until solvent volatilizees completely in Teflon beaker.Will residue
Solid is put in ceramic crucible, is heated to 250 holding 3 hours in batch-type furnace.Add the 1mol/L hydrogen of 50ml the most in the product
Sodium hydroxide solution, dissolves mesoporous silicon oxide.Gained solution is put in high speed centrifuge with the speed of 5000 turns per minute from
The heart 10 minutes, after outwelling supernatant, uses 10ml deionized water wash three times respectively, dries 12 hours 60, can obtain mesoporous oxidation
Indium nanometer particle.The aperture of above-mentioned mesoporous indium oxide nano-particle is 2-50 nanometer.
7) mesoporous indium oxide nano-particle and Graphene are joined in deionized water, ultrasonic 30 minutes, be allowed to uniformly divide
Cloth.Sucking filtration, is dried 12 hours under 70 vacuum environments, can obtain Graphene-mesoporous indium oxide nano composite material, as shown in Figure 1.
Embodiment two
The preparation method of the Graphene-mesoporous indium oxide-silver ternary nano composite material of the present embodiment, including following step
Rapid:
1) two panels 4cm*10cm*0.5cm strip high purity graphite sheet is connected with power positive cathode respectively as electrode, electricity
Source voltage is adjustable in the range of 0-20V, can generate potential pulse；
2) choline chloride and glycerol being mixed according to the ratio 1: 2 of the amount of material, on magnetic stirring apparatus, 80 heating 5 are little
Time, after solid starts to melt, start stirring until forming colourless transparent liquid.Aforesaid liquid is put into 70 drying 12 in baking oven
Hour, put in drying baker standby；
3) take 150ml choline chloride/glycerol eutectic ionic liquid and put in 500ml beaker, add 150ml deionization
Water, stirs, and the 1mol/L sodium hydroxide solution adding 3ml makes electrolyte ph be 12.Described electrode is inserted electricity
Solving in liquid, immersing part is 5cm, and electrode spacing is 3cm, adds 50mg surfactant cetyl trimethyl in the electrolytic solution
Ammonium chloride, and it is heated to 60.First adding 5V DC voltage, keep 5 minutes, then making alive is 10V, the persistent period is 5 seconds, interpulse
It is divided into the pulse voltage of 2 seconds, is electrolysed 1 hour, it is thus achieved that graphite flake layer；
4) being put into by electrolyte in 1000 watts of microwaves, splitting time is 5 minutes, tentatively peels off, then by above-mentioned electrolysis
Liquid is put into and is used the power ultrasonic of 100% to shake in ultrasonic cleaner 20 minutes, the Graphene degree of depth is separated.
5) electrolyte is put into the centrifugation 5 minutes with 1000 turns per minute in high speed centrifuge, removes at the bottom of centrifuge tube
Portion's deposit, can recycle as graphite electrode after deposit tabletting.Take supernatant and leave 15 points of the heart with per minute 10000
Clock, removes supernatant.Add the concussion of 20ml EtOH Sonicate and disperse centrifugation the most again to graphene uniform, repeat this step
Rapid three times.Gained Graphene is placed under 70 vacuum environments and is dried 12 hours.
6) at 35 times with polymer, butanol, hydrochloric acid for starting material with water full-boiled process synthesizing mesoporous silicon dioxide, by above-mentioned titanium dioxide
Silicon and nitric hydrate indium add in 10ml ethanol, stir 10 minutes, until solvent volatilizees completely in Teflon beaker.Will residue
Solid is put in ceramic crucible, is heated to 250 holding 3 hours in batch-type furnace.Add the 1mol/L hydrogen of 50ml the most in the product
Sodium hydroxide solution, dissolves mesoporous silicon oxide.Gained solution is put in high speed centrifuge with the speed of 5000 turns per minute from
The heart 10 minutes, after outwelling supernatant, uses 10ml deionized water wash three times respectively, dries 12 hours 60, can obtain mesoporous oxidation
Indium nanometer particle.The aperture of above-mentioned mesoporous indium oxide nano-particle is 2-50 nanometer.
7) mesoporous indium oxide nano-particle, Graphene and silver nano-grain are joined in deionized water, ultrasonic 30 minutes,
It is allowed to be uniformly distributed.Sucking filtration, is dried 12 hours under 70 vacuum environments, can obtain Graphene-mesoporous indium oxide-silver nanoparticle composite wood
Material, as shown in Figure 2.
It is finally noted that, publicize and implement the purpose of mode and be that help is further appreciated by the present invention, but ability
Those of skill will appreciate that of territory: without departing from the spirit and scope of the invention and the appended claims, various replacements and
Amendment is all possible.Therefore, the present invention should not be limited to embodiment disclosure of that, the scope of protection of present invention with
Claims define in the range of standard.
Claims (5)
1. the preparation method of Graphene-mesoporous indium oxide nano composite material, it is characterised in that described preparation method includes
Following steps:
1) two panels graphite flake is connected with power positive cathode respectively as electrode；
2) described electrode is inserted in electrolyte solution, first add DC voltage preliminary electrolysis, then add pulse voltage deep electrolytic,
To graphite flake layer；
3) described electrolyte is placed in oxygen-free environment, carries out microwave, ultrasonic in combination stripping, make graphene sheet layer be separated into graphite
Alkene；
4) electrolyte is centrifuged, isolates Graphene, with washing with alcohol, vacuum drying；
5) mesoporous indium oxide nano-particle and Graphene are joined in deionized water, ultrasonic, it is allowed to be uniformly distributed.Gained is molten
Liquid sucking filtration, is dried under vacuum conditions, obtains Graphene-mesoporous indium oxide nano composite material.
2. preparation method as claimed in claim 1, it is characterised in that in step 2) in, described electrolyte solution is water and low
1: 1 (volume ratio) mixture of congruent melting ionic liquid.
3. eutectic ionic liquid as claimed in claim 2, it is characterised in that by organic cation and inorganic or organic the moon from
Son composition, include but not limited to carbamide/zinc chloride, carbamide/iron chloride, carbamide/tin trichloride, carbamide/ammonium nitrate, hexanediol/
Zinc chloride, choline chloride/zinc chloride, choline chloride/glycerol, acetamide/potassium rhodanate, carbamide/acetamide/ammonium nitrate, urine
Element/ammonium nitrate/rhodan ammoniums etc., eutectic ionic liquid can be made up of two kinds to four kind of compounds.
4. preparation method as claimed in claim 1, it is characterised in that in step 2) in, added DC voltage is 1-5V, keeps
Time is 1-10 minute, and added pulse voltage is 5-10V, and the pulse duration is the 1-5 second, and interpulse period is the 1-5 second, always
Electrolysis time is 0.5-2 hour.
5. preparation method as claimed in claim 1, it is characterised in that in step 5) in, mesoporous indium oxide nano-particle and stone
The mass ratio of ink alkene is between 1: between 10-1: 1.
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Cited By (5)
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| CN107381621A (en) * | 2017-06-07 | 2017-11-24 | 常州欧康铭化工有限公司 | A kind of preparation method of mesoporous indium oxide |
| CN109455706A (en) * | 2018-12-13 | 2019-03-12 | 东莞理工学院 | A kind of preparation method of sulfonated graphene load indium oxide gas sensitive |
| CN109628983A (en) * | 2019-02-26 | 2019-04-16 | 西南大学 | A kind of preparation method of metal-graphite alkene composite-plated material |
| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
| CN111718493A (en) * | 2020-06-10 | 2020-09-29 | 江南大学 | Method for preparing MAMS-1 nanosheet by liquid-phase stripping method and application thereof |
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| CN109954509A (en) * | 2018-12-04 | 2019-07-02 | 山东科技大学 | A kind of preparation method and application of silicon carbide-based photochemical catalyst |
| CN109455706A (en) * | 2018-12-13 | 2019-03-12 | 东莞理工学院 | A kind of preparation method of sulfonated graphene load indium oxide gas sensitive |
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| CN111718493A (en) * | 2020-06-10 | 2020-09-29 | 江南大学 | Method for preparing MAMS-1 nanosheet by liquid-phase stripping method and application thereof |
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