CN101792119B - Method for preparing carbon nano tube composite material loaded with nano indium-tin oxide - Google Patents
Method for preparing carbon nano tube composite material loaded with nano indium-tin oxide Download PDFInfo
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- CN101792119B CN101792119B CN2010101420149A CN201010142014A CN101792119B CN 101792119 B CN101792119 B CN 101792119B CN 2010101420149 A CN2010101420149 A CN 2010101420149A CN 201010142014 A CN201010142014 A CN 201010142014A CN 101792119 B CN101792119 B CN 101792119B
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Abstract
The invention relates to a method for preparing a carbon nano tube composite material, in particular to a method for preparing a carbon nano tube composite material loaded with nano indium-tin oxide. The invention solves the problem of complicated process of the traditional method for preparing the carbon nano tube composite material loaded with nano indium-tin oxide. The method comprises the following steps of: preparing an organic phase solution by using indium nitrate, stannic chloride and ethylene glycol methyl ether; preparing an aqueous phase solution by using resorcinol, formaldehyde, sodium carbonate and water; dropwise adding the organic phase solution into the aqueous phase solution to obtain a precursor solution; soaking a porous aluminum oxide template into the precursor solution and standing; then sintering; finally, removing the template by using sodium hydroxide, washing and drying to obtain the carbon nano tube composite material loaded with the nano indium-tin oxide. The invention has simple process and can be used for preparing a hydrogen sensitive element.
Description
Technical field
The present invention relates to the preparation method of carbon nano tube compound material.
Background technology
CNT has characteristics such as hollow, lightweight, high-specific surface area, high conductivity and biocompatibility; And the load oxide has given CNT new characteristic on CNT; Make it have more excellent physics and chemical characteristic, like catalysis, optics, air-sensitive and microwave absorbing property etc.The preparation method of existing metal oxide supported carbon nano tube compound material is: at first prepare or the purchase CNT; Then CNT is carried out surface modification; Then through absorption and electrostatic interaction with the granular precursor of metal oxide attached to carbon nano tube surface; Through heat treatment the presoma of metal oxide is transformed into metal oxide again, thereby obtains the composite of metal oxide supported CNT, this method complex process.
Summary of the invention
The present invention is the problem for the method complex process that solves existing preparation loaded with nano indium tin oxide carbon nano tube compound material, and the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide is provided.
The preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide of the present invention; Carry out according to the following steps: one, take by weighing indium nitrate, stannic chloride and EGME respectively; Indium nitrate wherein: the mol ratio of stannic chloride is 1: (0.1～0.125), indium nitrate: the mol ratio of EGME is 1: (0.1～0.5); And indium nitrate, stannic chloride and EGME joined in the reactor, the condition refluxed 20h～28h at 75 ℃～85 ℃ obtains organic phase solution; Two, take by weighing resorcinol, formaldehyde, sodium carbonate and water respectively; Resorcinol wherein: the mol ratio of formaldehyde is 100: (45～55), resorcinol: the mol ratio of sodium carbonate is 100: (0.08～0.12), resorcinol: the mol ratio of water is 100: (15～20); And with mixing in resorcinol, formaldehyde, sodium carbonate and the water adding reactor; Reconcile pH value to 1～1.5 with hydrochloric acid again, stir 1h～1.5h, obtain aqueous phase solution; Three, take by weighing organic phase solution that obtains through step 1 and the aqueous phase solution that obtains through step 2 respectively; Organic phase solution wherein: the volume ratio of aqueous phase solution is 1: (0.25～0.5); Under stirring condition, organic phase solution is splashed in the aqueous phase solution, continue to stir 1h～1.5h; Static then placement 20h～28h obtains precursor solution; Four, porous alumina formwork is immersed in the precursor solution that step 3 obtains, takes out behind static placement 20min～40min, at room temperature hang 20h～28h; Five, the porous alumina formwork after step 4 is handled is placed in the sintering furnace, under argon gas or nitrogen protection, keeps 0.8h～1.5h after being warming up to 800 ℃～1000 ℃; Six, will be placed on through the porous alumina formwork that step 5 was handled in the dense sodium hydrate aqueous solution that crosses to 0.5mol/L～2mol/L and keep 6h～24h; After spending deionised water, drying then, promptly obtain the carbon nano tube compound material of loaded with nano indium tin oxide.
The preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide of the present invention joins the raw material indium nitrate, the stannic chloride that form indium tin oxide in the precursor that forms CNT, forms presoma; The resorcinol in the presoma and the gel of formaldehyde; Each material evenly is filled in the porous alumina formwork,, indium tin oxide and CNT is generated simultaneously through sintering processes; And combine; On template, form the carbon nano tube compound material of loaded with nano indium tin oxide, remove template again, obtain the carbon nano tube compound material of loaded with nano indium tin oxide.The average grain of indium tin oxide is 15nm～40nm in the composite, and the diameter of CNT is 200nm～250nm, and the present invention generates indium tin oxide and CNT simultaneously, and technology is simple.
Description of drawings
Fig. 1 is the X-ray diffractogram of carbon nano tube compound material of the loaded with nano indium tin oxide of the specific embodiment 20 preparation, and the diffraction maximum of mark ■ symbol is the diffraction maximum of indium tin oxide (ITO); Fig. 2 be the specific embodiment 20 preparation the loaded with nano indium tin oxide carbon nano tube compound material the side retouch the microcosmic micrograph; Fig. 3 be the specific embodiment 20 preparation the loaded with nano indium tin oxide carbon nano tube compound material the cross section retouch the microcosmic micrograph; Fig. 4 is the transmission electron microscope picture of carbon nano tube compound material of the loaded with nano indium tin oxide of the specific embodiment 20 preparation.
The specific embodiment
The specific embodiment one: the preparation method of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment carries out according to the following steps: one, take by weighing indium nitrate, stannic chloride and EGME respectively; Indium nitrate wherein: the mol ratio of stannic chloride is 1: 0.1～0.125, indium nitrate: the mol ratio of EGME is 1: 0.1～0.5; And indium nitrate, stannic chloride and EGME joined in the reactor; Condition refluxed 20h～28h at 75 ℃～85 ℃ obtains organic phase solution; Two, take by weighing resorcinol, formaldehyde, sodium carbonate and water respectively; Resorcinol wherein: the mol ratio of formaldehyde is 100: 45～55, resorcinol: the mol ratio of sodium carbonate is 100: 0.08～0.12, resorcinol: the mol ratio of water is 100: 15～20; And with mixing in resorcinol, formaldehyde, sodium carbonate and the water adding reactor; Reconcile pH value to 1～1.5 with hydrochloric acid again, stir 1h～1.5h, obtain aqueous phase solution; Three, take by weighing organic phase solution that obtains through step 1 and the aqueous phase solution that obtains through step 2 respectively; Organic phase solution wherein: the volume ratio of aqueous phase solution is 1: 0.25～0.5; Under stirring condition, organic phase solution is splashed in the aqueous phase solution, continue to stir 1h～1.5h; Static then placement 20h～28h obtains precursor solution; Four, porous alumina formwork is immersed in the precursor solution that step 3 obtains, takes out behind static placement 20min～40min, at room temperature hang 20h～28h; Five, the porous alumina formwork after step 4 is handled is placed in the sintering furnace, under argon gas or nitrogen protection, keeps 0.8h～1.5h after being warming up to 800 ℃～1000 ℃; Six, will be placed on through the porous alumina formwork that step 5 was handled in the dense sodium hydrate aqueous solution that crosses to 0.5mol/L～2mol/L and keep 6h～24h; After spending deionised water, drying then, promptly obtain the carbon nano tube compound material of loaded with nano indium tin oxide.
The preparation method of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment joins the raw material indium nitrate, the stannic chloride that form indium tin oxide in the precursor that forms CNT, forms presoma; The resorcinol in the presoma and the gel of formaldehyde; Each material evenly is filled in the porous alumina formwork,, indium tin oxide and CNT is generated simultaneously through sintering processes; And combine; On template, form the carbon nano tube compound material of loaded with nano indium tin oxide, remove template again, obtain the carbon nano tube compound material of loaded with nano indium tin oxide.The average grain of indium tin oxide is 15nm～40nm in the composite, and the diameter of CNT is 200nm～250nm, and the present invention generates indium tin oxide and CNT simultaneously, and technology is simple.
The specific embodiment two: what this embodiment and the specific embodiment one were different is: indium nitrate in the step 1: the mol ratio of stannic chloride is 1: 0.11～0.12, indium nitrate: the mol ratio of EGME is 1: 0.15～0.45.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: what this embodiment was different with the specific embodiment one or two is: indium nitrate in the step 1: the mol ratio of stannic chloride is 1: 0.115, indium nitrate: the mol ratio of EGME is 1: 0.25.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what this embodiment was different with one of specific embodiment one to three is: in the step 1 at condition refluxed 21h～27h of 78 ℃～83 ℃.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what this embodiment was different with one of specific embodiment one to four is: in the step 1 at 80 ℃ condition refluxed 20h.Other is identical with one of specific embodiment one to four.
The specific embodiment six: what this embodiment was different with one of specific embodiment one to five is: resorcinol in the step 2: the mol ratio of formaldehyde is 100: 47～53, resorcinol: the mol ratio of sodium carbonate is 100: 0.09～0.11, resorcinol: the mol ratio of water is 100: 16～19.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what this embodiment was different with one of specific embodiment one to six is: resorcinol in the step 2: the mol ratio of formaldehyde is 100: 50, resorcinol: the mol ratio of sodium carbonate is 100: 0.10, resorcinol: the mol ratio of water is 100: 18.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what this embodiment was different with one of specific embodiment one to seven is: reconcile pH value to 1.1～1.4 with hydrochloric acid in the step 2, stir 1.1h～1.4h.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what this embodiment was different with one of specific embodiment one to eight is: reconcile pH value to 1.3 with hydrochloric acid in the step 2, stir 1.2h.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: what this embodiment was different with one of specific embodiment one to nine is: organic phase solution in the step 3: the volume ratio of aqueous phase solution is 1: 0.3～0.45.Other is identical with one of specific embodiment one to nine.
The specific embodiment 11: what this embodiment was different with one of specific embodiment one to ten is: organic phase solution in the step 3: the volume ratio of aqueous phase solution is 1: 0.3.Other is identical with one of specific embodiment one to ten.
The specific embodiment 12: what this embodiment was different with one of specific embodiment one to 11 is: after in the step 3 organic phase solution being splashed into aqueous phase solution, continue to stir 1.1h～1.4h, static then placement 21h～27h.Other is identical with one of specific embodiment one to 11.
The specific embodiment 13: what this embodiment was different with one of specific embodiment one to 12 is: after in the step 3 organic phase solution being splashed into aqueous phase solution, continue to stir 1.3h, static then placement 25h.Other is identical with one of specific embodiment one to 12.
The specific embodiment 14: what this embodiment was different with one of specific embodiment one to 13 is: be 25min～35min static standing time in the step 4, and at room temperature open assembly time is 21h～27h.Other is identical with one of specific embodiment one to 13.
The specific embodiment 15: what this embodiment was different with one of specific embodiment one to 14 is: be 30min static standing time in the step 4, and at room temperature open assembly time is 24h.Other is identical with one of specific embodiment one to 14.
The specific embodiment 16: what this embodiment was different with one of specific embodiment one to 15 is: keep 1.0h～1.4h after being warming up to 850 ℃～950 ℃ in the step 5.Other is identical with one of specific embodiment one to 15.
The specific embodiment 17: what this embodiment was different with one of specific embodiment one to 16 is: keep 1.2h after being warming up to 900 ℃ in the step 5.Other is identical with one of specific embodiment one to 16.
The specific embodiment 18: what this embodiment was different with one of specific embodiment one to 17 is: in the dense sodium hydrate aqueous solution that crosses to 0.6mol/L～1.8mol/L, keep 7h～18h in the step 6.Other is identical with one of specific embodiment one to 17.
The specific embodiment 19: what this embodiment was different with one of specific embodiment one to 17 is: in the dense sodium hydrate aqueous solution that crosses to 1.5mol/L, keep 12h in the step 6.Other is identical with one of specific embodiment one to 17.
The specific embodiment 20: the preparation method of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment carries out according to the following steps: one, take by weighing indium nitrate, stannic chloride and EGME respectively; Indium nitrate wherein: the mol ratio of stannic chloride is 1: 0.115, indium nitrate: the mol ratio of EGME is 1: 0.35; And indium nitrate, stannic chloride and EGME joined in the reactor; Condition refluxed 24h at 80 ℃ obtains organic phase solution; Two, take by weighing resorcinol, formaldehyde, sodium carbonate and water respectively; Resorcinol wherein: the mol ratio of formaldehyde is 100: 50, resorcinol: the mol ratio of sodium carbonate is 100: 0.10, resorcinol: the mol ratio of water is 100: 18; And with mixing in resorcinol, formaldehyde, sodium carbonate and the water adding reactor; Reconcile pH value to 1 with hydrochloric acid again, stir 1h, obtain aqueous phase solution; Three, take by weighing organic phase solution that obtains through step 1 and the aqueous phase solution that obtains through step 2 respectively; Organic phase solution wherein: the volume ratio of aqueous phase solution is 1: 0.45; Under stirring condition, organic phase solution is splashed in the aqueous phase solution, continue to stir 1h; Static then placement 24h obtains precursor solution; Four, porous alumina formwork is immersed in the precursor solution that step 3 obtains, takes out behind the static again placement 30min, and at room temperature hang 24h; Five, the porous alumina formwork after step 4 is handled is placed in the sintering furnace, under argon gas or nitrogen protection, keeps 1h after being warming up to 800 ℃; Six, will pass through the porous alumina formwork that step 5 handled and be placed on dense crossing to after keeping 10h in the sodium hydrate aqueous solution of 1.6mol/L; Spend deionised water; And then under 100 ℃ of conditions dry 1h, promptly obtain the carbon nano tube compound material of loaded with nano indium tin oxide.
The X ray diffracting spectrum of the carbon nano tube compound material of the loaded with nano indium tin oxide (ITO) of this embodiment preparation is as shown in Figure 1; The carbon hollow pipe that is as can beappreciated from fig. 1 synthesized is an amorphous carbon, and the diffraction maximum of mark ■ symbol is the diffraction maximum of indium tin oxide (ITO); The scanning microcosmic micrograph of the carbon nano tube compound material side of the loaded with nano indium tin oxide of this embodiment preparation is as shown in Figure 2; The scanning microcosmic micrograph in the cross section of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment preparation is as shown in Figure 3; The carbon nano tube compound material that from Fig. 2 and Fig. 3, can find out the loaded with nano indium tin oxide for preparing through this embodiment is a kind of hollow tubular material; Nano indium tin oxide particle appendix is on the face CNT; The external diameter of pipe is 200nm～250nm, and wall thickness is 20nm～50nm; The transmission electron microscope picture of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment preparation is as shown in Figure 4; Can clearly be seen that nano indium tin oxide (ITO) particle appendix on the face CNT from Fig. 4, the nano indium tin oxide particle grain size is 15nm～40nm.
The preparation method of the carbon nano tube compound material of the loaded with nano indium tin oxide of this embodiment joins the raw material indium nitrate, the stannic chloride that form indium tin oxide in the precursor that forms CNT, forms presoma; The resorcinol in the presoma and the gel of formaldehyde; Each material evenly is filled in the porous alumina formwork,, indium tin oxide and CNT is generated simultaneously through sintering processes; And combine; On template, form the carbon nano tube compound material of loaded with nano indium tin oxide, remove template again, obtain the carbon nano tube compound material of loaded with nano indium tin oxide; Indium tin oxide and CNT are generated simultaneously, and technology is simple.
Claims (10)
1. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide; The preparation method who it is characterized in that the carbon nano tube compound material of loaded with nano indium tin oxide carries out according to the following steps: one, take by weighing indium nitrate, stannic chloride and EGME respectively; Indium nitrate wherein: the mol ratio of stannic chloride is 1: (0.1～0.125), indium nitrate: the mol ratio of EGME is 1: (0.1～0.5); And indium nitrate, stannic chloride and EGME joined in the reactor; Condition refluxed 20h～28h at 75 ℃～85 ℃ obtains organic phase solution; Two, take by weighing resorcinol, formaldehyde, sodium carbonate and water respectively; Resorcinol wherein: the mol ratio of formaldehyde is 100: (45～55), resorcinol: the mol ratio of sodium carbonate is 100: (0.08～0.12), resorcinol: the mol ratio of water is 100: (15～20); And with mixing in resorcinol, formaldehyde, sodium carbonate and the water adding reactor; Reconcile pH value to 1～1.5 with hydrochloric acid again, stir 1h～1.5h, obtain aqueous phase solution; Three, take by weighing organic phase solution that obtains through step 1 and the aqueous phase solution that obtains through step 2 respectively; Organic phase solution wherein: the volume ratio of aqueous phase solution is 1: (0.25～0.5); Under stirring condition, organic phase solution is splashed in the aqueous phase solution, continue to stir 1h～1.5h; Static then placement 20h～28h obtains precursor solution; Four, porous alumina formwork is immersed in the precursor solution that step 3 obtains, takes out behind static placement 20min～40min, at room temperature hang 20h～28h; Five, the porous alumina formwork after step 4 is handled is placed in the sintering furnace, under argon gas or nitrogen protection, keeps 0.8h～1.5h after being warming up to 800 ℃～1000 ℃; Six, will be placed on through the porous alumina formwork that step 5 was handled in the dense sodium hydrate aqueous solution that crosses to 0.5mol/L～2mol/L and keep 6h～24h; After spending deionised water, drying then, promptly obtain the carbon nano tube compound material of loaded with nano indium tin oxide.
2. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 1 is characterized in that indium nitrate in the step 1: the mol ratio of stannic chloride is 1: (0.11～0.12), indium nitrate: the mol ratio of EGME is 1: (0.15～0.45).
3. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 1 and 2 is characterized in that in the step 1 condition refluxed 21h～27h at 78 ℃～83 ℃.
4. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 3 is characterized in that resorcinol in the step 2: the mol ratio of formaldehyde is 100: (47～53), resorcinol: the mol ratio of sodium carbonate is 100: (0.09～0.11), resorcinol: the mol ratio of water is 100: (16～19).
5. according to the preparation method of the carbon nano tube compound material of claim 1,2 or 4 described loaded with nano indium tin oxides, it is characterized in that reconciling pH value to 1.1～1.4 with hydrochloric acid in the step 2 stirring 1.1h～1.4h.
6. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 5 is characterized in that organic phase solution: the volume ratio of aqueous phase solution is 1: (0.3～0.45).
7. according to the preparation method of the carbon nano tube compound material of claim 1,2,4 or 6 described loaded with nano indium tin oxides; After it is characterized in that in the step 3 organic phase solution splashed into aqueous phase solution; Continue to stir 1.1h～1.4h, static then placement 21h～27h.
8. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 7 is characterized in that be 25min～35min static standing time in the step 4, and at room temperature open assembly time is 21h～27h.
9. according to the preparation method of the carbon nano tube compound material of claim 1,2,4,6 or 8 described loaded with nano indium tin oxides, keep 1.0h～1.4h after it is characterized in that being warming up in the step 5 850 ℃～950 ℃.
10. the preparation method of the carbon nano tube compound material of loaded with nano indium tin oxide according to claim 7 is characterized in that in the dense sodium hydrate aqueous solution that crosses to 0.6mol/L～1.8mol/L, keeping 7h～18h in the step 6.
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| US9598287B2 (en) | 2014-05-27 | 2017-03-21 | Qatar University | Method of synthesizing carbon nanorods and nanowires |
| CN104600307B (en) * | 2015-01-13 | 2017-02-08 | 上海交通大学 | Preparation method of multiwalled carbon nanotube for lithium air battery positive electrode |
| CN105445423B (en) * | 2015-11-18 | 2017-12-15 | 济南大学 | A kind of preparation method and application of the gas sensor based on indium tin oxide hydridization multi-walled carbon nanotube |
| CN110783543B (en) * | 2019-10-24 | 2020-11-03 | 安徽师范大学 | Cobalt/carbon nanotube/sulfur particle microcapsule composite material, preparation method thereof, lithium-sulfur battery positive electrode and lithium-sulfur battery |
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| CN101018736A (en) * | 2004-06-23 | 2007-08-15 | 图卢兹国家工艺协会 | Method for selectively producing ordered carbon nanotubes |
| CN101269809A (en) * | 2008-04-29 | 2008-09-24 | 东华大学 | Method for preparing composite material of nano-indium stannum oxide/multi-wall carbon nano-tube |
| CN101293645A (en) * | 2008-06-06 | 2008-10-29 | 东华大学 | Method for preparing indium tin oxide assembled carbon nano-tube composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101018736A (en) * | 2004-06-23 | 2007-08-15 | 图卢兹国家工艺协会 | Method for selectively producing ordered carbon nanotubes |
| CN101269809A (en) * | 2008-04-29 | 2008-09-24 | 东华大学 | Method for preparing composite material of nano-indium stannum oxide/multi-wall carbon nano-tube |
| CN101293645A (en) * | 2008-06-06 | 2008-10-29 | 东华大学 | Method for preparing indium tin oxide assembled carbon nano-tube composite material |
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