CN110078465A - A kind of carbon-silica-gold composite aerogel and its application - Google Patents

A kind of carbon-silica-gold composite aerogel and its application Download PDF

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CN110078465A
CN110078465A CN201910445595.4A CN201910445595A CN110078465A CN 110078465 A CN110078465 A CN 110078465A CN 201910445595 A CN201910445595 A CN 201910445595A CN 110078465 A CN110078465 A CN 110078465A
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carbon
silica
gold
composite aerogel
nano
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CN110078465B (en
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俞书宏
詹慧娟
刘建伟
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University of Science and Technology of China USTC
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091Preparation of aerogels, e.g. xerogels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00Selenium; Tellurium; Compounds thereof
    • C01B19/02Elemental selenium or tellurium
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/14Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/34Metals, e.g. ferro-silicon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38Fibrous materials; Whiskers
    • C04B14/386Carbon
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B30/00Compositions for artificial stone, not containing binders
    • C04B30/02Compositions for artificial stone, not containing binders containing fibrous materials
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00Water conservation; Efficient water supply; Efficient water use
    • Y02A20/20Controlling water pollution; Waste water treatment
    • Y02A20/208Off-grid powered water treatment
    • Y02A20/212Solar-powered wastewater sewage treatment, e.g. spray evaporation

Abstract

The present invention provides a kind of carbon-silica-gold composite aerogel and its application, composite aerogel is made by following methods: by the aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response, obtained carbon fiber water gel calcining, obtained carbon pipe fiber aeroge immerses in silica prepolymer solution, supercritical drying is taken out, carbon-silicon dioxide composite aerogel is obtained;Gold nano grain solution is added dropwise on carbon-silicon dioxide composite aerogel surface, is filtered, supercritical drying obtains carbon-silica-gold composite aerogel.The present invention is using one-dimensional tellurium nano-wire as hard template, glucose hydrothermal carbonization, and calcining removal one-dimensional nano line forms three-dimensional carbon pipe fiber aeroge;Silica prepolymer solution enters inside carbon pipe fiber aeroge, and polymerization forms dual network structure, the hydrophily of composite aerogel is improved, conducive to the transmission of subsequent water;Gold nano grain surface plasma resonance effect increases the absorption to sunlight, is conducive to improve photothermal conversion efficiency.

Description

A kind of carbon-silica-gold composite aerogel and its application
Technical field
The invention belongs to nanocomposite aeroge field more particularly to a kind of carbon-silica-gold composite aerogels And its application.
Background technique
The controlledly synthesis of nano material, effectively assembling, and the design of material based on nano material and performance study are phases Close one of premise and guarantee that nano material moves towards practical.Britain's " nature-material " (Nature Materials, 2007 6th phase, page 841) it points out, the physicochemical properties exploitation of material depends not only on the shape and size of itself, also depends on group Fill the collaboration of body.And by the nanometer macro-scale three-dimensional aeroge constructed of assembling primitive due to its unique physicochemical properties, Make it in heat-and sound-insulating, catalysis, the fields such as battery power and photothermal conversion be widely used (" material ", Materials, 2013 6 Volume page 941).
Application about the preparation of aeroge and its in sunlight heat water evaporation field at present, it is seen that following some reports Road:
" advanced material " (volume 29 page 1604031 of Adv.Mater.2017) report using first freezing construct freeze again it is dry Dry method is prepared for the three-dimensional carbon aerogels of macro-scale.The basic process of the method is: by a certain amount of graphite oxide Alkene, carbon nanotube, sodium alginate are dispersed in water, and ultrasonic treatment is sufficiently mixed three kinds of components.Then obtained solution is fallen In the polytetrafluoroethylcontainer container for entering specific shape and size, solid is frozen into after being handled with liquid nitrogen.It is small that it is finally freeze-dried 48 again When, obtain the nanocomposite aeroge with polytetrafluoroethylcontainer container same shape and size.The carbon that this method is prepared Photothermal conversion efficiency of the aeroge under 1 sunlight has reached 83%, but due to graphene, the nano materials such as carbon nanotube Synthesis cost is higher, and in order to keep carbon nanotube well dispersed in water, generally requires additional Chemical modification or length Time ultrasonic treatment etc., also increases cost and operation difficulty to a certain extent.
(volume 10 12603 of ACS Appl.Mater.Interfaces 2018 of " American Chemical Society's application material and interface " Page) it reports a kind of preparation method of optically transparent aerosil and is used for the excellent of sunlight heat water evaporation Gesture.Preparation method basic process is as follows: it is first that tetraethyl orthosilicate is molten in methyl alcohol, N, N- dimethyl formyl is then added Amine adds basic catalyst ammonia spirit and carries out catalysis reaction.After reaction 30-90 minutes, the hydrogel that polymerization is formed is small The heart is transferred in ethyl alcohol, is placed 21 days and is continued to cure, and changed an ethyl alcohol every 24 hours.Then supercritical drying obtains gas again Gel.The aerosil of this method preparation is used to penetrate sunlight, and the black matrix material of lower section is enable to absorb sunlight, It is converted into thermal energy.And due to the excellent heat-proof quality of aerosil, the heat of generation is difficult the airsetting by top Glue is transferred in the environment of surrounding.But the process that this method prepares aeroge is cumbersome, and the period is long, the photo-thermal water evaporation thus designed Photothermal conversion efficiency of the system under 1 sunlight is only 55%, and performance is lower.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of carbon-silica-gold composite aerogel and its application, it should Composite aerogel photothermal conversion efficiency with higher.
The present invention provides a kind of carbon-silica-gold composite aerogels, are made by following methods:
By the aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response, carbon fiber water gel is obtained;
The carbon fiber water gel is calcined, carbon pipe fiber aeroge is obtained;
The carbon pipe fiber aeroge is immersed in the prepolymer solution of silica, takes out supercritical drying, obtain carbon- Silicon dioxide composite aerogel;
Gold nano grain solution is added dropwise on the carbon-silicon dioxide composite aerogel surface, is filtered, supercritical drying It is dry, obtain carbon-silica-gold composite aerogel.
Preferably, the temperature of the hydro-thermal reaction is preferably 100~200 DEG C;The time of hydro-thermal reaction is 1~50h.
Preferably, the silica prepolymer solution is made in accordance with the following methods:
Tetraethyl orthosilicate is molten in ethanol, and the aqueous solution of hydrochloric acid is added dropwise in stirring, stirs, adds ammonia spirit, stir It mixes, obtains silica prepolymer solution.
Preferably, the gold nano grain solution is made in accordance with the following methods:
After chlorauric acid solution heating is boiled, under stirring condition and sodium citrate solution mixing, 1~50min of reaction are subsequent 1~10h of continuous stirring, cooling obtain gold nano grain solution.
Preferably, the mass ratio of the material of sodium citrate is in gold chloride and sodium citrate solution in the chlorauric acid solution 0.1~20:0.1~100.
Preferably, the rate that the gold nano grain solution is added dropwise is 0.01~200mL/s.
Preferably, the aqueous dispersions of the one-dimensional tellurium nano-wire are made in accordance with the following methods:
Tellurium dioxide and polyvinylpyrrolidone are dissolved in after water and add ammonium hydroxide and hydrazine hydrate, is stirred, in a kettle Reaction, obtains one-dimensional tellurium nano-wire;
After the one-dimensional tellurium nano-wire centrifugation washing, it is dispersed in water, obtains the aqueous dispersions of one-dimensional tellurium nano-wire.
Preferably, the quality of the tellurium dioxide, the quality of polyvinylpyrrolidone, the volume of water, the volume of ammonium hydroxide and The volume ratio of hydrazine hydrate is (0.1~10) g:(0.1~20) g:(100~500) mL:(0.5~50) mL:(0.1~50) mL.
Preferably, the concentration of the aqueous dispersions of the one-dimensional tellurium nano-wire is 0.1~50mg/mL.
The present invention provides carbon-silica-gold composite aerogels described in a kind of above-mentioned technical proposal in sunlight hot water Application in evaporation field.
The present invention provides a kind of carbon-silica-gold composite aerogels, are made by following methods: by one-dimensional tellurium nanometer The aqueous dispersions and glucose water thermal response of line, obtain carbon fiber water gel;The carbon fiber water gel is calcined, carbon pipe is obtained Fiber aeroge;The carbon pipe fiber aeroge is immersed in silica prepolymer solution, supercritical drying is taken out, obtains Carbon-silicon dioxide composite aerogel;Gold nano grain solution is added dropwise on the carbon-silicon dioxide composite aerogel surface, It filters, supercritical drying obtains carbon-silica-gold composite aerogel.The present invention using one-dimensional tellurium nano-wire as hard template, Hydro-thermal reaction provides external condition for glucose hydrothermal carbonization, and it is fine to form three-dimensional carbon pipe for the one-dimensional nano line inside calcining removal Tie up aeroge;Silica prepolymer solution enters inside carbon pipe fiber aeroge in macropore, and polymerization forms dual network structure, mentions High-carbon-silicon dioxide composite aerogel hydrophily, is conducive to the transmission of subsequent water;Gold nano grain surface plasma resonance effect The absorption to sunlight should be increased, is conducive to improve photothermal conversion efficiency.The results showed that compound gas provided by the invention Gel sunlight average absorption ratio reaches 98% (in 250-2000 nanometer wavelength range), and photothermal conversion is imitated under 1 sunlight Rate reaches 90% or more.
Detailed description of the invention
Fig. 1 is the transmission electron microscope figure of 25 nanometers of tellurium nano-wires of diameter;
Fig. 2 is using 25 nanometers of tellurium nano-wires as the transmission electron microscope figure of the three-dimensional carbon fiber water gel of templated synthesis;
Fig. 3 is using 25 nanometers of tellurium nano-wires as the transmission electron microscope figure of the carbon pipe fiber aeroge of templated synthesis;
Fig. 4 is carbon-aerosil transmission electron microscope figure in embodiment 1;
Fig. 5 is carbon-aerosil scanning electron microscope diagram in embodiment 1;
Fig. 6 is the transmission electron microscope figure of gold nano grain;
Fig. 7 is the X ray diffracting spectrum of gold nano grain;
Fig. 8 is carbon-silica-gold aeroge transmission electron microscope figure prepared by embodiment 1;
Fig. 9 is carbon-silica-gold aeroge scanning electron microscope diagram prepared by embodiment 1;
Figure 10 is the optical photograph that carbon-silica-gold aeroge evaporates water under 10 sunlights;
Figure 11 is pure water, carbon-aerosil, carbon-silica-gold aeroge evaporate under 1 sunlight The rate and photothermal conversion efficiency figure of water;
Figure 12 is 35 tellurium nano-wire transmission electron microscope figure of diameter;
Figure 13 is using 35 nanometers of tellurium nano-wires as the transmission electron microscope figure of the three-dimensional carbon fiber water gel of templated synthesis;
Figure 14 is using 35 nanometers of tellurium nano-wires as the transmission electron microscope figure of the carbon pipe fiber aeroge of templated synthesis;
Figure 15 is 55 nanometers of tellurium nano-wire transmission electron microscope figures of diameter;
Figure 16 is using 55 nanometers of tellurium nano-wires of diameter as the transmission electron microscopy of the three-dimensional carbon fiber water gel of templated synthesis Mirror figure;
Figure 17 is aobvious by the transmitted electron of the carbon pipe fiber aeroge of templated synthesis of 55 nanometers of tellurium nano-wires in embodiment 3 Micro mirror figure.
Specific embodiment
The present invention provides a kind of carbon-silica-gold composite aerogels, are made by following methods:
By the aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response, carbon fiber water gel is obtained;
The carbon fiber water gel is calcined, carbon pipe fiber aeroge is obtained;
The carbon pipe fiber aeroge is immersed in silica prepolymer solution, supercritical drying is taken out, obtains carbon-two Aoxidize silicon compound aerogel;
Gold nano grain solution is added dropwise on the carbon-silicon dioxide composite aerogel surface, is filtered, supercritical drying It is dry, obtain carbon-silica-gold composite aerogel.
For the present invention using one-dimensional tellurium nano-wire as hard template, hydro-thermal reaction provides external condition for glucose hydrothermal carbonization, One-dimensional nano line inside calcining removal, forms three-dimensional carbon pipe fiber aeroge;It is fine that silica prepolymer solution enters carbon pipe It ties up inside aeroge in macropore, polymerization forms dual network structure, improves carbon-silicon dioxide composite aerogel hydrophily, favorably In the transmission of subsequent water;Gold nano grain surface plasma resonance effect increases the absorption to sunlight, is conducive to improve light Thermal transition efficiency.
The aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response are obtained carbon fiber water gel by the present invention.At this In invention, the aqueous dispersions of the one-dimensional tellurium nano-wire are preferably made in accordance with the following methods:
Tellurium dioxide and polyvinylpyrrolidone are dissolved in after water and add ammonium hydroxide and hydrazine hydrate, is stirred, in a kettle Reaction, obtains one-dimensional tellurium nano-wire;
After the one-dimensional tellurium nano-wire centrifugation washing, it is dispersed in water, obtains the aqueous dispersions of one-dimensional tellurium nano-wire.
In the present invention, the quality of the tellurium dioxide, the quality of polyvinylpyrrolidone, the volume of water, ammonium hydroxide body Long-pending and hydrazine hydrate volume ratio is preferably (0.1~10) g:(0.1~20) g:(100~500) mL:(0.5~50) mL:(0.1~ 50)mL;More preferably (0.5~5) g:(1~10) g:(50~200) mL:(5~25) mL:(0.5~20) mL;It is being embodied In example, the body of the quality of the tellurium dioxide, the quality of polyvinylpyrrolidone, the volume of water, the volume of ammonium hydroxide and hydrazine hydrate Product is than being specially 0.654g:5g:63.5mL:10mL:1.5mL;Or 0.654g:5g:63.0mL:10mL:2.0mL;Or 0.654g: 5g:64.5mL:10mL:0.5mL.
In the present invention, it is preferably 0.1min~12h that the time stirred after hydrazine hydrate, which is added, more preferably 2min.Anti- Answering the temperature reacted in kettle is preferably 100~200 DEG C, and more preferably 180 DEG C;Time is preferably 1~10h, more preferably 3h.
The diameter of the one-dimensional tellurium nano-wire is preferably 10~100nm, more preferably 25~55nm;In specific embodiment In, the diameter of one-dimensional tellurium nano-wire is 25nm, 35nm or 55nm.
The number of the one-dimensional tellurium nano-wire centrifugation washing is preferably 1~5 time, more preferably 1 time by the present invention.One-dimensional tellurium Nano wire is preferably dispersed in 10~200mL water, more preferably 40mL;The moisture for the one-dimensional tellurium nano-wire being dispersed in water The concentration of dispersion liquid is preferably 0.1~50mg/mL, more preferably 13mg/mL.
In the present invention, the volume ratio of water is preferably in the aqueous dispersions of the quality of the glucose and one-dimensional tellurium nano-wire (0.1~10) g:(10~200) mL;More preferably 2g:40mL.
After obtaining carbon fiber water gel, the present invention calcines the carbon fiber water gel, obtains carbon pipe fiber aeroge.? In the present invention, acetone soak is changed again after preferably impregnating using ethyl alcohol before the carbon fiber water gel calcining;The immersion hydrogel Ethyl alcohol volume and carbon fiber water gel mass ratio be preferably (1~500) mL:(1~200) mg;More preferably (10~ 250) mL:(10~100) mg.The time that ethyl alcohol impregnates carbon fiber water gel is preferably 1~20 day, and more preferably 2~10 days, tool In body embodiment, the time that ethyl alcohol impregnates carbon fiber water gel is 3 days.Impregnate the ethyl alcohol of carbon fiber water gel preferably every 1~ 20h is changed once, and more preferable 8h is changed once.Ethyl alcohol uses acetone soak after impregnating;The volume of acetone and the matter of carbon fiber water gel Amount is than being (1~500) mL:(1~200) mg;More preferably (10~250) mL:(10~100) mg.Acetone soak carbon fiber water The time of gel is preferably 1~20 day, more preferably 2~10 days, in specific embodiment, acetone soak carbon fiber water gel when Between be 3 days.The acetone for impregnating carbon fiber water gel preferably changes once every 1~20h, and more preferable 8h is changed once.
In the present invention, the supercritical drying preferably uses CO 2 supercritical dry.The supercritical drying Time is preferably 1~50h, more preferably 10~25h;In a particular embodiment, the time of supercritical drying is preferably 15h.
The present invention immerses the carbon pipe fiber aeroge in silica prepolymer solution, takes out supercritical drying, obtains To carbon-silicon dioxide composite aerogel.In the present invention, the silica prepolymer solution is made in accordance with the following methods:
Tetraethyl orthosilicate is molten in ethanol, and the aqueous solution of hydrochloric acid is added dropwise in stirring, stirs, adds ammonia spirit, stir It mixes, obtains silica prepolymer solution.
In the present invention, the mass ratio of the tetraethyl orthosilicate and ethyl alcohol is preferably 0.1~10:0.1~50, more preferably For 0.2~5:10~40;In specific embodiment, the mass ratio of the tetraethyl orthosilicate and ethyl alcohol is 0.46:35.32.
In the present invention, the molten speed stirred afterwards in ethanol of tetraethyl orthosilicate is preferably 100~1000rpm, more excellent It is selected as 300~800rpm, most preferably 550~650rpm;In specific embodiment, tetraethyl orthosilicate is molten to be stirred afterwards in ethanol Speed be 600rpm.The tetraethyl orthosilicate molten time stirred afterwards in ethanol is preferably 0.1~20min, more preferably 3~ 10min, most preferably 4~6min;In specific embodiment, the tetraethyl orthosilicate molten time stirred afterwards in ethanol is 5min.
In the present invention, the mass concentration of the aqueous solution of the hydrochloric acid is preferably 0.1~50%, more preferably 0.5~ 25%;In a particular embodiment, the mass concentration of the aqueous solution of the hydrochloric acid is preferably 1.5%.The aqueous solution of hydrochloric acid is added dropwise Speed is preferably 1~200 μ L/s, more preferably 5~100 μ L/s;In a particular embodiment, the speed of the aqueous solution of hydrochloric acid is added dropwise For 10 μ L/s.It is preferably 100~1000rpm that the speed stirred after the aqueous solution of hydrochloric acid, which is added dropwise, more preferably 300~800rpm; In a particular embodiment, the speed of the stirring is 600rpm.Be added dropwise time for stirring after the aqueous solution of hydrochloric acid be preferably 0.1~ 20h, more preferably 0.5~10h;In specific embodiment, the time that the aqueous solution of hydrochloric acid is added dropwise is 1h.In a particular embodiment, The dosage of the aqueous solution of hydrochloric acid is preferably 0.5~50mL, more preferably 3.464mL.
In the present invention, the mass concentration of ammonia spirit is preferably 0.1~50%, and more preferably 0.5~25%;Specific In embodiment, the mass concentration of the ammonium hydroxide is 3.6%.It is preferably 100~1000rpm that the speed stirred after ammonium hydroxide, which is added, more Preferably 300~800rpm;In a particular embodiment, the mixing speed after ammonium hydroxide is added is 600rpm.It is stirred after ammonium hydroxide is added Time be preferably 0.1~50min, more preferably 5~30min;In a particular embodiment, time for stirring is after ammonium hydroxide being added 20min。
In the present invention, the time that carbon pipe fiber aeroge immerses in silica prepolymer solution is preferably 1~50h, More preferably 10~30h;In a particular embodiment, the time in carbon pipe fiber aeroge immersion silica prepolymer solution is 24h。
The time of supercritical drying is preferably 1~50h after taking-up, more preferably 10~30h;In a particular embodiment, it takes The time of supercritical drying is 15h after out.
After obtaining carbon-silicon dioxide composite aerogel, gold nano grain solution is added dropwise to the carbon-titanium dioxide by the present invention It on silicon compound aerogel surface, filters, supercritical drying obtains carbon-silica-gold composite aerogel.
In the present invention, the gold nano grain solution is made in accordance with the following methods:
After chlorauric acid solution heating is boiled, under stirring condition and sodium citrate solution mixing, 1~50min of reaction are subsequent 1~10h of continuous stirring, cooling obtain silica prepolymer solution.
In the present invention, the chlorauric acid solution is preferably disposed in heating in round-bottomed flask and boils;The appearance of the round-bottomed flask Amount is 10~500mL.It is preferably 100~1000rpm that the speed stirred after chlorauric acid solution, which is added, more preferably 300~ 800rpm;In a particular embodiment, it is 600rpm that the speed stirred after chlorauric acid solution, which is added,.
The molar concentration of the sodium citrate solution is preferably 0.1~100mmol/L, more preferably 5~60mmol/L;? In specific embodiment, the molar concentration of sodium citrate solution is 38.8mmol/L.Mixing speed after sodium citrate solution is added Preferably 100~1000rpm, more preferably 300~800rpm;In a particular embodiment, it is stirred after sodium citrate solution being added Speed be 600rpm.Time for continuing heating is preferably 10~30min after sodium citrate solution is added, more preferably 15min.
In the present invention, the speed for gold nano grain solution being added dropwise is preferably 0.01~200mL/s, more preferably 0.05~ 100mL/s;In specific example, the speed that gold nano grain solution is added dropwise is 0.1mL/s.
The present invention is by filtering so that the acceleration of gold nano grain solution flows through inside aeroge, then is collected and filtered with bottle,suction The liquid of outflow.It is dry that CO 2 supercritical is carried out after suction filtration;The time of supercritical drying is preferably 1~50h, more preferably 10~25h;In a particular embodiment, the time of supercritical drying is 15h after suction filtration.
Method provided by the invention is prepared for a kind of three component nano composite aerogels, and the composite aerogel sunlight is average Absorptivity reaches 98% (in 250~2000 nanometer wavelength ranges), under 1 sunlight photothermal conversion efficiency reach 90% with On.
In order to further illustrate the present invention, multiple to a kind of carbon-silica-gold provided by the invention below with reference to embodiment It closes aeroge and its application is described in detail, but they cannot be interpreted as limiting the scope of the present invention.
Drug and reagent used are purchased from Sinopharm Chemical Reagent Co., Ltd. in following embodiment, and hydro-thermal is closed anti- Answering container is the stainless steel cauldron of Fujian Sheng Xin Machinery Co., Ltd. production.
Embodiment 1
1. the synthesis of 25 nanometers of diameter (nm) tellurium nano-wires
63 milliliters of (mL) deionized waters, 0.654 gram of (g) tellurium dioxide, 5g are added in 100mL ptfe autoclave After stirring 20 minutes (min), 10mL ammonium hydroxide is added in polyvinylpyrrolidone, after 20min, 2mL hydrazine hydrate is added, stirs 2min Afterwards, it is put into 3 hours (h) of reaction in 180 degrees Celsius of (DEG C) baking ovens, is taken out, it is cooling.
Fig. 1 is the transmission electron microscope figure of 25 nanometers of tellurium nano-wires of diameter;
2. the synthesis of three-dimensional carbon fiber water gel
The 75mL diameter that the method for being prepared as described above is obtained is the tellurium line centrifugation of 25nm, then is centrifuged after washing one time, It is dissolved in 40mL water, 2g glucose is added, after stirring 5h, be put into 180 DEG C of hydro-thermal reactions in 50mL ptfe autoclave For 24 hours, it is taken out after cooling and obtains three-dimensional carbon fiber water gel.3d is impregnated with ethyl alcohol, after 8h replaces an ethyl alcohol, then uses acetone 3d is impregnated, after 8h replaces an acetone, after the dry 15h of CO 2 supercritical, obtains three-dimensional carbon fiber aeroge.
Fig. 2 is using 25 nanometers of tellurium nano-wires as the transmission electron microscope figure of the three-dimensional carbon fiber water gel of templated synthesis.
3. the preparation of macro-scale carbon pipe fiber aeroge
The three-dimensional carbon fiber aeroge that the method for being prepared as described above is obtained is placed in sizeable porcelain boat, and plug arrives tube furnace In, it is sealed, leads to nitrogen or argon gas, setting heating cooling process: be raised to 900 DEG C from 30 DEG C in 180min, kept at 900 DEG C 120min, then 180min cool to 30 DEG C.After cooling, takes out, obtain macro-scale carbon pipe fiber aeroge.
It is using 25 nanometers of tellurium nano-wires as the transmission electron microscopy of the carbon pipe fiber aeroge of templated synthesis referring to Fig. 3, Fig. 3 Mirror figure.
4. the preparation of carbon-aerosil
0.46g tetraethyl orthosilicate is added in 35.32g ethyl alcohol, stirs 5min at 600 revs/min (rpm), then to its The middle hydrochloric acid solution that 3.464mL mass concentration is added dropwise and is 1.5%.After stirring 1h, it is 3.57% that 3.50mL mass concentration, which is added, Ammonia spirit, continuing stirring 10min. will stand for 24 hours in carbon pipe fiber aeroge immersion silica performed polymer obtained above, After obtained carbon-silica hydrogel supercritical drying 15h, carbon-aerosil is obtained.
Fig. 4 is carbon-aerosil transmission electron microscope figure in embodiment 1;Fig. 5 is carbon-two in embodiment 1 The scanning electron microscope diagram of silica aerogel.
5. the preparation of carbon-silica-gold aeroge
It is that 1 mM every liter (mM) chlorauric acid solution is added in 250mL round-bottomed flask by 100mL concentration, heating is boiled, The sodium citrate that 100mL concentration is 38.8mM is added in whipping process, stops heating after reacting 15min, continues to stir 1h, it is cooling After obtain gold nano grain solution.
Fig. 6 is the transmission electron microscope figure of gold nano grain.Fig. 7 is the X ray diffracting spectrum of gold nano grain.
The gold nano grain solution of synthesis is added drop-wise on carbon-silicon dioxide composite aerogel surface, is filtered and is accelerated solution stream Inside aeroge, the liquid of outflow, obtained carbon-silica-Jinsui River gel supercritical drying are finally collected with bottle,suction After 15h, carbon-silica-gold aeroge is obtained.
Fig. 8 is carbon-silica-gold aeroge transmission electron microscope figure prepared by embodiment 1;Fig. 9 is embodiment 1 Carbon-silica-gold aeroge scanning electron microscope diagram of preparation.
Figure 10 is the optical photograph that carbon-silica-gold aeroge evaporates water under 10 sunlights.
Figure 11 is pure water, carbon-aerosil, carbon-silica-gold aeroge evaporate under 1 sunlight The rate and photothermal conversion efficiency figure of water.As can be seen from Figure 11: carbon-silica-gold aeroge is under 1 sunlight Evaporate the rate and photothermal conversion efficiency highest of water, respectively 1.32kg/m2/ h and 90.4%.
Embodiment 2
1. the synthesis of 35 nanometers of diameter (nm) tellurium nano-wires
63.5 milliliters of (mL) deionized waters of addition in 100mL ptfe autoclave, 0.654 gram of (g) tellurium dioxide, After stirring 20 minutes (min), 10mL ammonium hydroxide is added in 5g polyvinylpyrrolidone, and after 20min, 1.5mL hydrazine hydrate, stirring is added After 2min, it is put into 3 hours (h) of reaction in 180 degrees Celsius of (DEG C) baking ovens, is taken out, it is cooling, obtain diameter 35nm tellurium nano-wire.
Figure 12 is 35 tellurium nano-wire transmission electron microscope figure of diameter.
2. the synthesis of three-dimensional carbon fiber water gel
The 75mL diameter that the method for being prepared as described above is obtained is the tellurium line centrifugation of 35nm, then is centrifuged after washing one time, It is dissolved in 40mL water, 2g glucose is added, after stirring 5h, be put into 180 DEG C of hydro-thermal reactions in 50mL ptfe autoclave For 24 hours, it is taken out after cooling and obtains three-dimensional carbon fiber water gel.3d is impregnated with ethyl alcohol, after 8h replaces an ethyl alcohol, then uses acetone 3d is impregnated, after 8h replaces an acetone, after the dry 15h of CO 2 supercritical, obtains three-dimensional carbon fiber aeroge.
Figure 13 is using 35 nanometers of tellurium nano-wires as the transmission electron microscope figure of the three-dimensional carbon fiber water gel of templated synthesis.
3. the preparation of macro-scale carbon pipe fiber aeroge
The three-dimensional carbon fiber aeroge that the method for being prepared as described above is obtained is placed in sizeable porcelain boat, and plug arrives tube furnace In, it is sealed, leads to nitrogen or argon gas, setting heating cooling process: be raised to 900 DEG C from 30 DEG C in 180min, kept at 900 DEG C 120min, then 180min cool to 30 DEG C.After cooling, takes out, obtain macro-scale carbon pipe fiber aeroge.
Figure 14 is using 35 nanometers of tellurium nano-wires as the transmission electron microscope figure of the carbon pipe fiber aeroge of templated synthesis.
4. the preparation of carbon-aerosil
0.46g tetraethyl orthosilicate is added in 35.32g ethyl alcohol, stirs 5min at 600 revs/min (rpm), then to its The middle hydrochloric acid solution that 3.464mL mass concentration is added dropwise and is 1.5%.After stirring 1h, it is 3.57% that 3.50mL mass concentration, which is added, Ammonia spirit, continuing stirring 10min. will stand for 24 hours in carbon pipe fiber aeroge immersion silica performed polymer obtained above, After obtained carbon-silica hydrogel supercritical drying 15h, carbon-aerosil is obtained.
5. the preparation of carbon-silica-gold aeroge
It is that 1 mM every liter (mM) chlorauric acid solution is added in 250mL round-bottomed flask by 100mL concentration, heating is boiled, The sodium citrate that 100mL concentration is 38.8mM is added in whipping process, stops heating after reacting 15min, continues to stir 1h, it is cooling After obtain gold nano grain solution, the gold nano grain solution of synthesis is added drop-wise on carbon-silicon dioxide composite aerogel surface, take out Filter accelerates solution to flow through inside aeroge, and the liquid of outflow is finally collected with bottle,suction, and obtained carbon-silica-Jinsui River is solidifying After glue supercritical drying 15h, carbon-silica-gold aeroge is obtained.
Carbon-silica-gold aeroge prepared by embodiment 2 evaporates the rate of water under 1 sunlight and photo-thermal turns Changing efficiency is respectively 1.33kg/m2/ h and 91.1%.
Embodiment 3
1. the synthesis of 55 nanometers of diameter (nm) tellurium nano-wires
64.5 milliliters of (mL) deionized waters of addition in 100mL ptfe autoclave, 0.654 gram of (g) tellurium dioxide, After stirring 20 minutes (min), 10mL ammonium hydroxide is added in 5g polyvinylpyrrolidone, and after 20min, 0.5mL hydrazine hydrate, stirring is added After 2min, it is put into 3 hours (h) of reaction in 180 degrees Celsius of (DEG C) baking ovens, is taken out, it is cooling.
Figure 15 is 55 nanometers of tellurium nano-wire transmission electron microscope figures of diameter.
2. the synthesis of three-dimensional carbon fiber water gel
The 75mL diameter that the method for being prepared as described above is obtained is the tellurium line centrifugation of 55nm, then is centrifuged after washing one time, It is dissolved in 40mL water, 2g glucose is added, after stirring 5h, be put into 180 DEG C of hydro-thermal reactions in 50mL ptfe autoclave For 24 hours, it is taken out after cooling and obtains three-dimensional carbon fiber water gel.3d is impregnated with ethyl alcohol, after 8h replaces an ethyl alcohol, then uses acetone 3d is impregnated, after 8h replaces an acetone, after the dry 15h of CO 2 supercritical, obtains three-dimensional carbon fiber aeroge.
Figure 16 is using 55 nanometers of tellurium nano-wires of diameter as the transmission electron microscopy of the three-dimensional carbon fiber water gel of templated synthesis Mirror figure.
3. the preparation of macro-scale carbon pipe fiber aeroge
The three-dimensional carbon fiber aeroge that the method for being prepared as described above is obtained is placed in sizeable porcelain boat, and plug arrives tube furnace In, it is sealed, leads to nitrogen or argon gas, setting heating cooling process: be raised to 900 DEG C from 30 DEG C in 180min, kept at 900 DEG C 120min, then 180min cool to 30 DEG C.After cooling, takes out, obtain macro-scale carbon pipe fiber aeroge.
Figure 17 is aobvious by the transmitted electron of the carbon pipe fiber aeroge of templated synthesis of 55 nanometers of tellurium nano-wires in embodiment 3 Micro mirror figure.
4. the preparation of carbon-aerosil
0.46g tetraethyl orthosilicate is added in 35.32g ethyl alcohol, stirs 5min at 600 revs/min (rpm), then to its The middle hydrochloric acid solution that 3.464mL mass concentration is added dropwise and is 1.5%.After stirring 1h, it is 3.57% that 3.50mL mass concentration, which is added, Ammonia spirit, continuing stirring 10min. will stand for 24 hours in carbon pipe fiber aeroge immersion silica performed polymer obtained above, After obtained carbon-silica hydrogel supercritical drying 15h, carbon-aerosil is obtained.
5. the preparation of carbon-silica-gold aeroge
It is that 1 mM every liter (mM) chlorauric acid solution is added in 250mL round-bottomed flask by 100mL concentration, heating is boiled, The sodium citrate that 100mL concentration is 38.8mM is added in whipping process, stops heating after reacting 15min, continues to stir 1h, it is cooling After obtain gold nano grain solution, the gold nano grain solution of synthesis is added drop-wise on carbon-silicon dioxide composite aerogel surface, take out Filter accelerates solution to flow through inside aeroge, and the liquid of outflow is finally collected with bottle,suction, and obtained carbon-silica-Jinsui River is solidifying After glue supercritical drying 15h, carbon-silica-gold aeroge is obtained.
Carbon-silica-gold aeroge prepared by embodiment 3 evaporates the rate of water under 1 sunlight and photo-thermal turns Changing efficiency is respectively 1.31kg/m2/ h and 90.0%.
As seen from the above embodiment, the present invention provides a kind of carbon-silica-gold composite aerogels, by following methods It is made: by the aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response, obtaining carbon fiber water gel;By the carbon fiber water Gel calcining, obtains carbon pipe fiber aeroge;The carbon pipe fiber aeroge is immersed in silica prepolymer solution, is taken out Supercritical drying obtains carbon-silicon dioxide composite aerogel;It is multiple that gold nano grain solution is added dropwise to the carbon-silica It closes on aeroge surface, filters, supercritical drying obtains carbon-silica-gold composite aerogel.The present invention is received with one-dimensional tellurium Rice noodles are as hard template, and hydro-thermal reaction provides external condition for glucose hydrothermal carbonization, the one-dimensional nano line inside calcining removal, Form three-dimensional carbon pipe fiber aeroge;Silica prepolymer solution enters inside carbon pipe fiber aeroge in macropore, polymerize shape Network structure in pairs improves carbon-silicon dioxide composite aerogel hydrophily, is conducive to the transmission of subsequent water;Gold nano grain Surface plasma resonance effect increases the absorption to sunlight, is conducive to improve photothermal conversion efficiency.The results showed that this The composite aerogel sunlight average absorption ratio that invention provides reaches 98% (in 250-2000 nanometer wavelength range), too at 1 Photothermal conversion efficiency reaches 90% or more under sunlight.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (10)

1. a kind of carbon-silica-gold composite aerogel, is made by following methods:
By the aqueous dispersions of one-dimensional tellurium nano-wire and glucose water thermal response, carbon fiber water gel is obtained;
The carbon fiber water gel is calcined, carbon pipe fiber aeroge is obtained;
The carbon pipe fiber aeroge is immersed in silica prepolymer solution, supercritical drying is taken out, obtains carbon-titanium dioxide Silicon compound aerogel;
Gold nano grain solution is added dropwise on the carbon-silicon dioxide composite aerogel surface, is filtered, supercritical drying obtains To carbon-silica-gold composite aerogel.
2. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the temperature of the hydro-thermal reaction Preferably 100~200 DEG C of degree;The time of hydro-thermal reaction is 1~50h.
3. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the silica pre-polymerization Liquid solution is made in accordance with the following methods:
Tetraethyl orthosilicate is molten in ethanol, and the aqueous solution of hydrochloric acid is added dropwise in stirring, stirs, adds ammonia spirit, stirs, Obtain silica prepolymer solution.
4. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the gold nano grain is molten Liquid is made in accordance with the following methods:
After chlorauric acid solution heating is boiled, is mixed under stirring condition with sodium citrate solution, continue to stir after reacting 1~50min 1~10h is mixed, it is cooling, obtain gold nano grain solution.
5. carbon-silica-gold composite aerogel according to claim 4, which is characterized in that in the chlorauric acid solution The mass ratio of the material of sodium citrate is 0.1~20:0.1~100 in gold chloride and sodium citrate solution.
6. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the gold nano grain is molten The rate that drop adds is 0.01~200mL/s.
7. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the one-dimensional tellurium nano-wire Aqueous dispersions be made in accordance with the following methods:
Tellurium dioxide and polyvinylpyrrolidone are dissolved in after water and add ammonium hydroxide and hydrazine hydrate, stirs, reacts in a kettle, Obtain one-dimensional tellurium nano-wire;
After the one-dimensional tellurium nano-wire centrifugation washing, it is dispersed in water, obtains the aqueous dispersions of one-dimensional tellurium nano-wire.
8. carbon-silica-gold composite aerogel according to claim 7, which is characterized in that the matter of the tellurium dioxide The volume ratio of amount, the quality of polyvinylpyrrolidone, the volume of water, the volume of ammonium hydroxide and hydrazine hydrate is (0.1~10) g:(0.1 ~20) g:(100~500) mL:(0.5~50) mL:(0.1~50) mL.
9. carbon-silica-gold composite aerogel according to claim 1, which is characterized in that the one-dimensional tellurium nano-wire Aqueous dispersions concentration be 0.1~50mg/mL.
10. a kind of any one of claim 1~9 carbon-silica-gold composite aerogel is in sunlight heat water evaporation field In application.
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