CN110395714A - A kind of Sb doped SnO2The preparation method of@carbon nanotube complex electrocaloric film - Google Patents
A kind of Sb doped SnO2The preparation method of@carbon nanotube complex electrocaloric film Download PDFInfo
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- CN110395714A CN110395714A CN201910793284.7A CN201910793284A CN110395714A CN 110395714 A CN110395714 A CN 110395714A CN 201910793284 A CN201910793284 A CN 201910793284A CN 110395714 A CN110395714 A CN 110395714A
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- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 14
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002238 carbon nanotube film Substances 0.000 claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 8
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 4
- 239000007789 gas Substances 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 13
- 238000005485 electric heating Methods 0.000 abstract description 12
- 239000002305 electric material Substances 0.000 abstract description 4
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000007423 decrease Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 229910052787 antimony Inorganic materials 0.000 description 4
- 239000002041 carbon nanotube Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000004965 peroxy acids Chemical class 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000010512 thermal transition Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 239000002071 nanotube Substances 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/02—Oxides
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
- H05B3/34—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater flexible, e.g. heating nets or webs
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Present invention proposition combines the advantage of two class thermo electric materials, prepares a kind of Sb doped SnO2@carbon nanotube complex electrocaloric film: Sb is adulterated by SnO using hydro-thermal method2It loads on carbon nano-tube film, electric heating property is obviously improved compared with pure nano-carbon tube film, and resistance decline is increased to that required power when same temperature is smaller, and heating rate is faster；Laminated film of the invention is a kind of easy to use, energy-saving and environment-friendly flexible electrothermic material, is had a extensive future.
Description
Technical field
The present invention relates to the technical field of electrical-heating film material preparation more particularly to a kind of Sb doped SnO2@carbon nanometer
The preparation method of pipe NEW TYPE OF COMPOSITE electrothermal film material.
Background technique
Electrothermal film technology is a kind of novel electric heating switch technology, it can be effectively saved energy cost, improves energy benefit
Use efficiency.Wherein, performance when metal oxide Electric radiant Heating Film is again with resistivity compared with low and high temperature is stable, anti-oxidant and anti-chemical rotten
The advantages that very competent, production method is simple, raw material are easy to get, are cheap is lost to show one's talent in many materials.
Carbon nanotube has very high thermal conductivity, but there are still thermal transitions at field in terms of electric heating for carbon nano-tube film
The problem that rate is not high, long-time stability are poor.SnO2Film is a kind of transparent conductive film, possess up to 80% visible light it is saturating
The infrared reflectivity for penetrating rate, up to 80%~90% is therefore widely used in film resistor, solar battery, electric heating and turns
Change film etc..SnO2Chemical stability height, excellent adsorption, can be deposited on including a variety of substrates such as glass, ceramic material
On material.Theoretically, the SnO not adulterated2Belong to typical insulator, but due to lattice Lacking oxygen and gap metal ion
In the presence of foring donor level, therefore SnO in forbidden band2It is N-type semiconductor.Being doped to it modified is always research
Hot spot mixes antimony SnO wherein the technology for mixing Sb, F, P is the most mature2The electric heating property of film has had certain progress.
The invention patent proposes, by antimony (Sb) doping stannic oxide (SnO2) and two class thermo electric material phase of carbon nano-tube film
In conjunction with to prepare high performance flexible compound electrothermal film material.The SnO for being adulterated Sb using hydro-thermal method2Carbon is loaded to receive
On mitron film.It is doped with the sample of Sb, resistance decline, electric heating property has a distinct increment compared with pure nano-carbon tube film, rises
Required power is smaller when height is to same temperature, heating rate faster: and flexible, electric heating high conversion rate has a extensive future.
Summary of the invention
The purpose of the present invention: the invention patent proposes a kind of Sb doping SnO2The preparation of@carbon nanotube complex electrocaloric film
Method, specific steps are as follows: use hydro-thermal method by SnO2It loads on carbon nano-tube film, and to SnO2Carry out Sb doping；Presoma
It is sintered at 500 DEG C；The composite carbon nanometer tube film has good Electrothermal Properties, with common carbon nano-tube film
It compares, thermal transition is more efficient, and heating rate also increases；Sb doping can effectively improve conductivity, reduce resistance；This hair
The Sb of bright proposition adulterates SnO2@carbon nanotube is a kind of easy to use, energy-saving and environment-friendly new electrically heating membrane material.
The technical scheme is that a kind of Sb doped SnO2The preparation method of@carbon nanotube complex electrocaloric film, feature
It is, by 10 × 10cm of area2Carbon nano-tube film certain time is impregnated in alkene hydrochloric acid, respectively use deionized water, ethyl alcohol
After flushing, film is impregnated into certain time in concentrated nitric acid, is rinsed again with deionized water, ethyl alcohol, in 60 DEG C of constant temperature of baking oven
Drying；Then, the processed film of two steps acid is immersed into SnCl4, NaOH and SbCl3Mixed reaction solution in, solvent be go from
The mixture of sub- water and ethyl alcohol carries out hydro-thermal reaction in 150 DEG C of reaction kettles, dry after flushing；Finally, dry film is set
In in tube furnace, under inert gas protection, 500 DEG C of sintering is warming up to 5 DEG C/minute of rate, film is taken out after cooling, is obtained
To final product.
As optimal selection, carbon nano-tube film needs successively carry out the processing of two step acid in alkene hydrochloric acid and concentrated nitric acid, use
Deionized water, ethyl alcohol rinse.
As optimal selection, the mass percent concentration of aqueous hydrochloric acid solution is 3~10wt.%, and the concentration of concentrated nitric acid is 65
~68 wt.%, the soaking time in two kinds of acid solutions are all 6 hours.
As optimal selection, when reaction mixture is prepared, deionized water and ethyl alcohol volume ratio 2: 1, total volume is 15~
45 mL pass through magnetic agitation sufficiently dissolution in 30 minutes, SnCl4, NaOH and SbCl3The respective optimum concentration range of three is followed successively by
30~150mM, 100~500mM and 1.0~2.0mM.
As optimal selection, the temperature of hydro-thermal reaction is 150 DEG C, and the reaction time is 6~12 hours.
It as optimal selection, is sintered under constant 500 DEG C of temperature inert gas shieldings, the time is 20~40 minutes.
Beneficial effects of the present invention:
The present invention is by antimony (Sb) doping stannic oxide (SnO2) and two class thermo electric material of carbon nano-tube film carry out it is compound, mention
The high electrical heating efficiency of pure nano-carbon tube film, overcomes the deficiency of the flexible difference of oxide.The laminated film has good
Electrothermal Properties, compared with common carbon nano-tube film, thermal transition is more efficient, and heating rate also increases；Sb doping can
It effectively improves conductivity, reduce resistance, it is a kind of easy to use, energy-saving and environment-friendly new electrically heating membrane material.
Detailed description of the invention:
Fig. 1 is that carbon nano-tube film (a) is after the processing of two step acid in embodiment 1 and the surface (b) coats Sb doped SnO2
The SEM picture of composite carbon nanometer tube film.
Fig. 2 is the Sb doped SnO that embodiment 1 obtains2Performance test is electrically heated after composite carbon nanometer tube thin-film package
Sample.
Fig. 3 is the temperature-power relationship curve graph of four kinds of different sample tests.
Fig. 4 is the resistance-temperature relationship curve graph of four kinds of different sample tests.
Fig. 5 is temperature-electric heating time history of four kinds of different sample tests.
Specific embodiment
A kind of Sb doped SnO of the present invention2The preparation of@carbon nanotube complex electrocaloric film, specific embodiment are as follows:
Embodiment 1
By 10 × 10cm of area2Carbon nano-tube film 6 hours are impregnated in alkene hydrochloric acid, respectively use deionized water, second
After alcohol rinses, film is impregnated into 6 hours in concentrated nitric acid, is rinsed again with deionized water, ethyl alcohol, in 60 DEG C of constant temperature of baking oven
Drying obtains the processed carbon nano-tube film sample of two steps acid.
Embodiment 2
On the basis of embodiment 1, the processed film of two steps acid is immersed into SnCl4, NaOH and SbCl3Hybrid reaction
In solution, solvent is the mixture of deionized water and ethyl alcohol, carries out hydro-thermal in 150 DEG C of reaction kettles, dry after flushing；Finally,
Dry film is placed in tube furnace, in inert gas N2Under protection, 500 DEG C of sintering 20 are warming up to 5 DEG C/minute of rate
Minute, film is taken out after cooling, obtains final product Sb doped SnO2@carbon nanotube compound electro-thermal membrane material.
Embodiment 3
By SnCl4, NaOH and SbCl3Mixed reaction solution in SbCl3To remove, other conditions and embodiment 2 are identical,
Obtain SnO2@carbon nano-tube compound film material.
Embodiment 4
By sintering process is removed in inert gas in embodiment 2, other conditions and embodiment 3 are identical, obtain SnO2Forerunner
Body@carbon nano-tube compound film material (un-sintered).
Embodiment 5
Change SnCl4, NaOH and SbCl3Mixed reaction solution intermediate ion concentration, other conditions and embodiment 2 are identical.
Fig. 1 (a) is the SEM picture that the carbon nano-tube film of any processing is not carried out after 1 liang of embodiment step acid is handled, figure
1 (b) is load Sb doped SnO2The SEM picture of carbon nano-tube film after cladding.By scheming the carbon it can be seen from (a) in film
Nanotube, which has, compares big L/D ratio, acid treated the random free arrangement of carbon nanotube, to form in the film a large amount of
Crosslinking in place of, these crosslinking points enable film to have good self-supporting, at the same also make carbon nano-tube film into
One step has been machined with a possibility that more.It can be seen that staggered carbon nano tube surface is coated without other substances, therefore hole
Rate is larger.It can be seen that, Sb doped SnO has been loaded from Fig. 1 (b)2Carbon nano-tube film, integrally become more close, it is single
One layer of Sb doped SnO of carbon nano tube surface uniform fold2Solid coating.
After four kinds of different samples prepared by the embodiment 1-4 of preparation are packaged, connect metal wire, being electrically heated property
It can test, as shown in Figure 2.Temperature-power curve: Fig. 3 is the temperature-power relationship curve graph of four kinds of different sample tests.By
Figure is as it can be seen that the temperature of four groups of samples linearly rises with the increase of power；The only temperature of the carbon nano-tube film through peracid treatment
Minimum with the rate of power rise, hydro-thermal method loads SnO2Unsintered carbon nano-tube film, temperature are higher under equal-wattage.
In contrast, by sintered SnO2Enveloped carbon nanometer tube laminated film and Sb adulterate SnO2Carbon nano-tube film, they
Temperature rate-of-rise it is higher.It can be seen that Sb doped SnO2The electric heating property of@carbon nanotube compound electro-thermal membrane material is best:
Lower attainable temperature highest of equal-wattage, the power for reaching a certain mutually synthermal needs are minimum.
It can be seen from Fig. 4 that the relationship of four groups of sample resistance sizes is load SnO in entire temperature-rise period2And the carbon being sintered
Nano-tube film resistance is maximum, the SnO for adulterating Sb and being sintered2Carbon nano-tube film takes second place, and next is load SnO2It does not burn
The sample of knot, only the resistance of the pure nano-carbon tube film sample through peracid treatment is minimum.Demonstrating can be improved Sb incorporation
SnO2Carrier concentration, to promote its conductivity.The resistance value of sintered two groups of samples is increased with temperature and is reduced, and is presented
More apparent characteristic of semiconductor out, and the variation of other two groups of samples is then less obvious.Result explanation, sintered sample
Carbon nano-tube film and Sb are preferably adulterated into SnO2Two kinds of thermo electric material combinations among the strong ones have larger excellent on properties
Gesture.
Heating-temperature lowering curve reflects heating and the rate of temperature fall of each group sample, is measure electric heating material performance one
Item important indicator.Fig. 5 is temperature-electric heating time history of the lower four groups of sample tests of 25W firm power, i.e. heating feelings
Condition and the cooling situation after cutting off the power.It is known from figures that, the carbon nano-tube film heating rate through peracid treatment
It is minimum, load SnO in four groups of samples2But unsintered carbon nano-tube film heating rate is slightly above the thin of acid processing
Film illustrates SnO2There is certain promotion to the electric heating property for promoting film.And sintered SnO2Carbon nano-tube film and Sb doping
SnO2Carbon nano-tube film, their heating rate then further get a promotion.
The attainable equilibrium temperature of each group sample institute is widely different: under equal-wattage, the sample of acid processing is attainable
Temperature is minimum, less than 70 DEG C；In contrast, load SnO2But the unsintered attainable temperature of sample is higher, can stablize
About 80 DEG C；And sintered two groups of samples, then it can reach the temperature close to 100 DEG C.During Temperature fall after cutting off the power,
The rate of temperature fall of two groups of samples through oversintering is also slightly above remaining two groups of sample, and surface is easier to radiate.
Claims (6)
1. a kind of Sb doped SnO2The preparation method of@carbon nanotube complex electrocaloric film, which is characterized in that by 10 × 10cm of area2's
Carbon nano-tube film impregnates certain time in alkene hydrochloric acid, and after being rinsed respectively with deionized water, ethyl alcohol, film is soaked in concentrated nitric acid
Certain time is steeped, is rinsed with deionized water, ethyl alcohol, is dried in 60 DEG C of constant temperature of baking oven again；Then, two step acid are processed
Film immerse SnCl4, NaOH and SbCl3Mixed reaction solution in, solvent be deionized water and ethyl alcohol mixture, 150
Hydro-thermal reaction is carried out in DEG C reaction kettle, it is dry after flushing；Finally, dry film is placed in tube furnace, protected in inert gas
Under shield, 500 DEG C of sintering are warming up to 5 DEG C/minute of rate, film is taken out after cooling, obtains final product.
2. a kind of Sb doped SnO according to claim 12The preparation method of@carbon nanotube complex electrocaloric film, feature exist
In carbon nano-tube film needs successively carry out the processing of two step acid in alkene hydrochloric acid and concentrated nitric acid, are rinsed with deionized water, ethyl alcohol.
3. the mass percent concentration of aqueous hydrochloric acid solution is 3~10wt.%, the concentration of concentrated nitric acid is 65~68wt.%, at two kinds
Soaking time in acid solution is all 6 hours.
4. a kind of Sb doped SnO according to claim 12The preparation method of@carbon nanotube complex electrocaloric film, feature exist
In reaction solution SnCl4, NaOH and SbCl3Mixed solution；When preparation, deionized water and ethyl alcohol volume ratio 2: 1, total volume
For 15~45mL, pass through magnetic agitation sufficiently dissolution in 30 minutes, SnCl4, NaOH and SbCl3The respective optimum concentration range of three
It is followed successively by 30~150mM, 100~500mM and 1~2mM.
5. a kind of Sb doped SnO according to claim 12The preparation method of@carbon nanotube complex electrocaloric film, feature exist
In the optimum temperature of hydro-thermal reaction is 150 DEG C, and the reaction time is 6~12 hours.
6. a kind of Sb doped SnO according to claim 12The preparation method of@carbon nanotube complex electrocaloric film, feature exist
In being sintered at a temperature of constant 500 DEG C, inert gas shielding (N2, Ar gas is ok), the time is 20~40 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453766A (en) * | 2020-04-09 | 2020-07-28 | 吉林大学 | One-dimensional MWCNTs @ SnO2Core-shell structure, preparation method thereof and application of core-shell structure to positive electrode of lead-carbon battery |
| CN113439908A (en) * | 2021-06-10 | 2021-09-28 | 深圳市顺成欣电子材料有限公司 | Heating shoe-pad that generate heat performance is good |
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| CN105712428A (en) * | 2016-02-01 | 2016-06-29 | 南京理工大学 | Antimony-doped tin oxide-carbon nanotube compounded adsorptive electrode and preparation method thereof |
| CN109068418A (en) * | 2018-06-15 | 2018-12-21 | 盐城工学院 | A kind of SnO2Composite carbon nanometer tube Electric radiant Heating Film and preparation method thereof |
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- 2019-08-23 CN CN201910793284.7A patent/CN110395714B/en active Active
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| CN103713016A (en) * | 2013-12-26 | 2014-04-09 | 武汉工程大学 | Palladium-doped stannic oxide wrapped carbon nano tube as well as preparation method and application of nano tube |
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|---|---|---|---|---|
| CN111453766A (en) * | 2020-04-09 | 2020-07-28 | 吉林大学 | One-dimensional MWCNTs @ SnO2Core-shell structure, preparation method thereof and application of core-shell structure to positive electrode of lead-carbon battery |
| CN113439908A (en) * | 2021-06-10 | 2021-09-28 | 深圳市顺成欣电子材料有限公司 | Heating shoe-pad that generate heat performance is good |
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