CN101723351A - Method for preparing Bi2Te3/carbon nanotube composite material - Google Patents
Method for preparing Bi2Te3/carbon nanotube composite material Download PDFInfo
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- CN101723351A CN101723351A CN200910155794A CN200910155794A CN101723351A CN 101723351 A CN101723351 A CN 101723351A CN 200910155794 A CN200910155794 A CN 200910155794A CN 200910155794 A CN200910155794 A CN 200910155794A CN 101723351 A CN101723351 A CN 101723351A
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- Prior art keywords
- carbon nanotube
- bi2te3
- compound
- nano tube
- carbon nano
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 52
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title abstract description 6
- 229910002899 Bi2Te3 Inorganic materials 0.000 title abstract 6
- 239000002131 composite material Substances 0.000 title abstract 4
- 239000000463 material Substances 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 14
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000012265 solid product Substances 0.000 claims abstract description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- -1 carbon nano tube compound Chemical class 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007306 functionalization reaction Methods 0.000 claims description 6
- 239000004615 ingredient Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 230000002829 reductive effect Effects 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims description 2
- 230000002950 deficient Effects 0.000 claims description 2
- 238000006396 nitration reaction Methods 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- BDOYKFSQFYNPKF-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]acetic acid;sodium Chemical compound [Na].[Na].OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O BDOYKFSQFYNPKF-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000012279 sodium borohydride Substances 0.000 abstract 1
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000005619 thermoelectricity Effects 0.000 description 2
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004627 transmission electron microscopy Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing a Bi2Te3/carbon nanotube composite material, which comprises the following steps: dissolving acidized carbon nanotubes into aqueous solution of surfactant EDTA, performing ultrasonic dispersion, and adding alkali to adjust the OH- concentration of the solution to between 0.1 and 1mol/L; in a determined molar ratio of Bi to Te of 2:3 through chemical composition analysis of Bi2Te3, dissolving a compound containing Bi element, a compound containing Te element or a Te simple substance into the aqueous solution, and adding a reducing agent NaBH4 with stirring to obtain mixed solution; and stirring and heating the mixed solution in a water bath, centrifugally separating, washing and collecting solid product after the reaction is finished, and drying. In the Bi2Te3/carbon nanotube composite material prepared by the method, the size of Bi2Te3 particles is about between 10 and 20nm; and the Bi2Te3/carbon nanotube composite material combines advantages of the carbon nanotubes and a thermoelectric material and is expected to improve figure of merit.
Description
Technical field
The present invention relates to Bi
2Te
3The preparation method of/carbon nano tube compound material belongs to the semi-conductor thermoelectric material technical field.
Background technology
Thermoelectric material is a kind of semiconductor functional material, it can realize the mutual conversion of heat energy and electric energy, there is important use to be worth and application prospects (B.C.Sales.Thermoelectric materials-Smaller is cooler.Science at thermo-electric generation and focus refrigerating field, 2002,295 (5558): 1248-1249).And Bi
2Te
3Its ZT value can approach 1, is thermoelectric material best under the current room temperature state.The height of thermoelectric device performance directly depends on the size of thermoelectric figure of merit, and therefore, further improve thermoelectric figure of merit ZT is a central topic of thermoelectricity research always.Can effectively improve the performance of focus material by grain refining and reduction crystal grain dimension.
Reduction, the crystal grain thinning of crystal grain in the thermoelectric material (particle) size or make material nanoization; help strengthening the scattering process of phonon on the one hand to heat; thereby reduce thermal conductivity (amplitude is greater than the reduction of specific conductivity); thereby the scattering that can improve current carrier is on the other hand again promoted the Seebeck coefficient; thereby can improve thermoelectric figure of merit (the J.Jortner and C.N.R.Rao.Nanostructured advanced materials.Perspectives and directions.Pure Appl.Chem. of material; 2002,74 (9): 1491-1506.).Therefore with Bi
2Te
3The base thermoelectricity material nanometer has application potential too.
Carbon nanotube has become the domestic and international research focus rapidly owing to have excellent performance and exist multiple potential using value, carbon nanotube to have outstanding specific surface area and favorable mechanical, electricity, optical property.Because it has big specific surface area, coat the main means that other nano materials have become surface modification of carbon nanotube and disperseed compound nano-particle on its surface.
Summary of the invention
It is tiny to the purpose of this invention is to provide a kind of particle, helps improving the Bi of thermoelectric figure of merit
2Te
3The preparation method of/carbon nano tube compound material.
Bi of the present invention
2Te
3The preparation method of/carbon nano tube compound material, employing be that low temperature wet is learned synthesis technique, step is as follows:
1) with carbon nanotube at concentrated nitric acid, the vitriol oil or the above two nitration mixture are ultrasonic or reflow treatment 2-5h, or after 300 ℃ of oxide treatment again through pickling, filtering and washing is to neutral, oven dry obtains the carbon nanotube that the surface exists defective or functionalization;
2) carbon nanotube after the step 1) processing being dissolved in concentration is in 5-20g/L disodium ethylene diamine tetraacetate (EDTA) aqueous solution, ultra-sonic dispersion, and add alkali regulator solution OH
-Concentration is 0.1-1mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, and the compound or the Te simple substance that will contain the compound of Bi element and contain the Te element are dissolved in step 2) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 50-200g reductive agent NaBH
4, get mixed solution;
4) with mixed solution stirring heating 12-48h under 70-85 ℃ of water-bath, reaction finishes back centrifugation, washing, collection solid product, and oven dry obtains Bi
2Te
3/ carbon nano tube compound material.
Among the present invention, the compound of the said Bi of containing element is muriate, oxide compound, vitriol, nitrate or the carbonate that contains the Bi element.The compound of the said Te of containing element is muriate, oxide compound, vitriol, nitrate, nitrite or the carbonate that contains the Te element.
The Bi that the inventive method makes
2Te
3/ carbon nano tube compound material, its Bi
2Te
3Particle size is about 10-20nm, evenly is coated on carbon nano tube surface with stratiform, or is connected in the bunchy carbon nano tube surface with Granular forms.This Bi
2Te
3/ carbon nano tube compound material combines the advantage of carbon nanotube and thermoelectric material, is expected to improve thermoelectric figure of merit, is with a wide range of applications.
Description of drawings
Fig. 1 is Bi
2Te
3Be coated on the TEM image of single-root carbon nano-tube;
Fig. 2 is that bunchy carbon tube-surface coats Bi
2Te
3The TEM image.
Embodiment
Embodiment 1
1) with carbon nanotube ultrasonic 2h in concentrated nitric acid solution, filtering and washing is dried to neutral, obtains the carbon nanotube of functionalization.
2) carbon nanotube after the processing of 0.05g step 1) is dissolved in the EDTA aqueous solution that 100mL concentration is 20g/L, ultra-sonic dispersion 30min, and add NaOH, regulator solution OH
-Concentration is 0.5mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, with Bi (NO
3)
35H
2O and Na
2TeO
3Be dissolved in step 2) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 100g reductive agent NaBH
4, get mixed solution;
4) with mixed solution stirring heating 36h under 70 ℃ of water-baths.Reaction finishes the back centrifugation, uses deionized water, absolute ethanol washing, collection solid product, oven dry.Get Bi
2Te
3/ carbon nano tube compound material.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, its result is the Bi of hexagonal structure
2Te
3And carbon nanotube.Adopt 200KV/JEM-2010 (HR) type transmission electron microscopy product pattern, the result is Bi
2Te
3Nano particle evenly is coated on the carbon nano tube surface (see figure 1).The bunchy carbon nano tube surface is connected with dispersive Bi
2Te
3The nano particle (see figure 2).Bi
2Te
3Particle size is 10-20nm.
Embodiment 2
1) carbon nanotube reflux in concentrated nitric acid solution is handled 2h, filtering and washing is dried to neutral, obtains the carbon nanotube of functionalization.
2) carbon nanotube after the processing of 0.03g step 1) is dissolved in the EDTA aqueous solution that 100mL concentration is 10g/L, ultra-sonic dispersion 30min, and add NaOH, regulator solution OH
-Concentration is 0.8mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, with Bi (NO
3)
35H
2O and TeO
2Be dissolved in step 2) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 50g reductive agent NaBH
4, get mixed solution;
4) with mixed solution stirring heating 48h under 70 ℃ of water-baths.Reaction finishes the back centrifugation, uses deionized water, absolute ethanol washing, collection solid product, oven dry.Get Bi
2Te
3/ carbon nano tube compound material, Bi
2Te
3Particle size is 10-20nm.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, its result is the Bi of hexagonal structure
2Te
3And carbon nanotube.
Embodiment 3
1) with carbon nanotube ultrasonic 3h in concentrated sulfuric acid solution, filtering and washing is dried to neutral, obtains the carbon nanotube of functionalization.
2) carbon nanotube after the processing of 0.06g step 1) is dissolved in the EDTA aqueous solution that 100mL concentration is 15g/L, ultra-sonic dispersion 30min, and add NaOH, regulator solution OH
-Concentration is 0.4mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, with BiCl
3And Na
2TeO
3Be dissolved in step 2) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 80g reductive agent NaBH
4, get mixed solution;
4) with mixed solution at 80 ℃ of following stirring heating 24h of water-bath.Reaction finishes the back centrifugation, uses deionized water, absolute ethanol washing, collection solid product, oven dry.Get Bi
2Te
3/ carbon nano tube compound material.Bi
2Te
3Particle size is 10-20nm.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, its result is the Bi of hexagonal structure
2Te
3And carbon nanotube.
Embodiment 4
1) with carbon nanotube ultrasonic 3h in concentrated nitric acid solution, filtering and washing is dried to neutral.Obtain the carbon nanotube of functionalization.
2) carbon nanotube after the processing of 0.025g step 1) is dissolved in the EDTA aqueous solution that 100mL concentration is 5g/L, ultra-sonic dispersion 30min, and add NaOH, regulator solution OH
-Concentration is 1mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, with BiCl
3Be dissolved in step 2 with Te simple substance) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 60g reductive agent NaBH
4, get mixed solution;
4) with mixed solution at 85 ℃ of following stirring heating 12h of water-bath.Reaction finishes the back centrifugation, uses deionized water, absolute ethanol washing, collection solid product, oven dry.Get Bi
2Te
3/ carbon nano tube compound material.Bi
2Te
3Particle size is 10-20nm.
Adopt the thing phase of Rigaku-D/MAX-2550PC type X ray polycrystalline diffractometer assay products, its result is the Bi of hexagonal structure
2Te
3And carbon nanotube.
Claims (3)
1. Bi
2Te
3The preparation method of/carbon nano tube compound material, its step comprises:
1) with carbon nanotube at concentrated nitric acid, the vitriol oil or the above two nitration mixture are ultrasonic or reflow treatment 2-5h, or after 300 ℃ of oxide treatment again through pickling, filtering and washing is to neutral, oven dry obtains the carbon nanotube that the surface exists defective or functionalization;
2) carbon nanotube after the step 1) processing being dissolved in concentration is in the 5-20g/L disodium ethylene diamine tetra-acetic acid aqueous solution, ultra-sonic dispersion, and adding alkali regulator solution OH-concentration is 0.1-1mol/L;
3) according to Bi
2Te
3The determined Bi of chemical ingredients: the mol ratio of Te is 2: 3, and the compound or the Te simple substance that will contain the compound of Bi element and contain the Te element are dissolved in step 2) the aqueous solution in, stir down according to every mole of Bi
2Te
3Add 50-200g reductive agent NaBH
4, get mixed solution;
4) with mixed solution stirring heating 12-48h under 70-85 ℃ of water-bath, reaction finishes back centrifugation, washing, collection solid product, and oven dry obtains Bi
2Te
3/ carbon nano tube compound material.
2. Bi according to claim 1
2Te
3The preparation method of/carbon nano tube compound material, the compound that it is characterized in that the said Bi of containing element is muriate, oxide compound, vitriol, nitrate or the carbonate that contains the Bi element.
3. Bi according to claim 1
2Te
3The preparation method of/carbon nano tube compound material, the compound that it is characterized in that the said Te of containing element is muriate, oxide compound, vitriol, nitrate, nitrite or the carbonate that contains the Te element.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910155794A CN101723351A (en) | 2009-12-18 | 2009-12-18 | Method for preparing Bi2Te3/carbon nanotube composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910155794A CN101723351A (en) | 2009-12-18 | 2009-12-18 | Method for preparing Bi2Te3/carbon nanotube composite material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101723351A true CN101723351A (en) | 2010-06-09 |
Family
ID=42445010
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910155794A Pending CN101723351A (en) | 2009-12-18 | 2009-12-18 | Method for preparing Bi2Te3/carbon nanotube composite material |
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|---|---|
| CN (1) | CN101723351A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738929A (en) * | 2013-09-03 | 2014-04-23 | 吉林化工学院 | Preparation of graded bismuth telluride micrometer structure with simple solvothermal method |
| CN105833859A (en) * | 2016-04-22 | 2016-08-10 | 上海电机学院 | Preparation method for Bi serial amorphous catalyst loaded on carbon nano tube |
| CN105859274A (en) * | 2016-03-31 | 2016-08-17 | 山东大学 | A temperature-controllable oxide thermoelectric material, a preparing method thereof and applications of the oxide thermoelectric material |
| CN108502870A (en) * | 2018-05-25 | 2018-09-07 | 湖南大学 | Modified carbon nano tube tube material and its preparation method and application |
| CN108675731A (en) * | 2018-06-11 | 2018-10-19 | 青岛理工大学 | Nano modified thermoelectric mortar and preparation method thereof, and intelligent cathode protection and degradation self-monitoring system and preparation method for thermoelectric structure |
| CN112316935A (en) * | 2020-11-25 | 2021-02-05 | 正太新材料科技有限责任公司 | Preparation method for degrading and separating flaky Bi-based catalytic pigment |
| CN115259139A (en) * | 2022-06-14 | 2022-11-01 | 江西理工大学 | Method for nano-crystallizing bismuth telluride and compounding nano-crystallized bismuth telluride and carbon nano tube film |
-
2009
- 2009-12-18 CN CN200910155794A patent/CN101723351A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738929A (en) * | 2013-09-03 | 2014-04-23 | 吉林化工学院 | Preparation of graded bismuth telluride micrometer structure with simple solvothermal method |
| CN105859274A (en) * | 2016-03-31 | 2016-08-17 | 山东大学 | A temperature-controllable oxide thermoelectric material, a preparing method thereof and applications of the oxide thermoelectric material |
| CN105833859A (en) * | 2016-04-22 | 2016-08-10 | 上海电机学院 | Preparation method for Bi serial amorphous catalyst loaded on carbon nano tube |
| CN108502870A (en) * | 2018-05-25 | 2018-09-07 | 湖南大学 | Modified carbon nano tube tube material and its preparation method and application |
| CN108675731A (en) * | 2018-06-11 | 2018-10-19 | 青岛理工大学 | Nano modified thermoelectric mortar and preparation method thereof, and intelligent cathode protection and degradation self-monitoring system and preparation method for thermoelectric structure |
| CN112316935A (en) * | 2020-11-25 | 2021-02-05 | 正太新材料科技有限责任公司 | Preparation method for degrading and separating flaky Bi-based catalytic pigment |
| CN112316935B (en) * | 2020-11-25 | 2022-05-24 | 正太新材料科技有限责任公司 | Preparation method for degrading and separating flaky Bi-based catalytic pigment |
| CN115259139A (en) * | 2022-06-14 | 2022-11-01 | 江西理工大学 | Method for nano-crystallizing bismuth telluride and compounding nano-crystallized bismuth telluride and carbon nano tube film |
| CN115259139B (en) * | 2022-06-14 | 2024-02-02 | 江西理工大学 | Bismuth telluride nanocrystallization and method for compounding bismuth telluride with carbon nano tube film |
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Open date: 20100609 |