CN103979523B - Method for filling multi-walled carbon nano-tubes with cadmium sulfide - Google Patents
Method for filling multi-walled carbon nano-tubes with cadmium sulfide Download PDFInfo
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Abstract
The present invention provides a method for filling multi-walled carbon nano-tubes with cadmium sulfide. The method comprises: carrying out a high temperature treatment of multi-walled carbon nano-tubes by using nitric acid, and ultrasonically dispersing the carbon nano-tubes into water after washing; adding a cadmium source to form a suspension with a cadmium source concentration of 0.1-1.5 mol/L, wherein a molar ratio of the cadmium source to the multi-walled carbon nano-tubes is 0.1-2:1; adjusting the pH value of the suspension to 1-5, carrying out an ultrasonic treatment for 1-4 h, and carrying out a hydrothermal treatment to obtain a reaction solution; evaporating the reaction solution until achieving a dry state to obtain an intermediate product, and washing the intermediate product with dimethyl sulfoxide; and mixing the washed intermediate product and dimethyl sulfoxide, carrying out a solvothermal reaction, centrifugation, and washing to obtain the multi-walled carbon nano-tubes filled with cadmium sulfide. The present invention further provides a cadmium sulfide-filled multi-walled carbon nano-tube composite material. With the method, multi-walled carbon nano-tubes can be filled with cadmium sulfide, wherein the filling rate is more than 60%, and characteristics of simple operation process, mild reaction condition, strong controllability and low production cost are provided.
Description
Technical field
The present invention relates to the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, particularly a kind of method adopting wet chemistry method filling and vulcanization cadmium in multi-walled carbon nano-tubes, belongs to advanced technical field of nanometer material preparation.
Background technology
Cadmium Sulfide is a kind of good narrow-band semiconductor, has excellent photoelectric response, have good application prospect in fields such as phototube, photovaristor, solar cell, photocatalysts to visible ray.But the pattern of Cadmium Sulfide and microstructure very big to its performance impact, especially it very easily reunites in preparation process, easily forms bulk Cadmium Sulfide, performance is reduced greatly.Carbon nanotube is that one has electric-conductivity heat-conductivity high, high-specific surface area, high mechanical strength, the monodimension nanometer material of the premium propertiess such as high absorption, because of its numerous advantage in a lot of high-tech sector as photoelectric material, energy storage material, sensor, biological devices etc. have the unrivaled advantage of traditional material, and cause at subjects such as material, physics, chemistry, biologies and study widely.
By carbon nanotube and Cadmium Sulfide coupling, can in conjunction with the premium properties of bi-material, the matrix material of obtained high photoelectric properties, and studied personnel's extensive concern.Up to now, existing numerous method reports prepares carbon nanotube and cadmium sulfide composite material.(the Jian Cao such as Cao, Jinzhi Sun, Jian Hong, Hanyin Li, Hongzheng Chen, Mang Wang Carbon Nanotube/CdS Core – Shell Nanowires Prepared by a SimpleRoom-Temperature Chemical Reduction Method, Adv.Mater, 2004,16,84-87) report a kind of method of room temperature chemical preparation carbon nanotube Cadmium Sulfide core-shell nano line; (the Istv á n Robel such as Robel, Bruce A.Bunker, and Prashant V.Kamat Single-Walled Carbon Nanotube – CdSNanocomposites as Light-Harvesting Assemblies:Photoinduced Charge TransferInteractions, Adv.Mater.2005,17,2458 – 2463) confirm the fast transfer effect of photogenerated charge therebetween in Cadmium Sulfide carbon nano tube compound material.
CN102173408A discloses the method for the adjustable carbon nanotube Cadmium Sulfide shell core composite material of core-shell structure of a kind of Co deposited synthesis shell thickness of slow releasing sulphur source, CN101624175B discloses a kind of method of coprecipitation method controlledly synthesis Cadmium Sulfide carbon nanotube shell core heterojunction composite, and CN101070153B discloses cadminium sulfide coated carbon nano tube composite nano material prepared by a kind of irradiation synthesis method.Because there is heterojunction between carbon nanotube prepared by the multiple method reported and cadmium sulfide composite material, promoting the fast transfer of electronics and being separated, improve the photoelectric properties of Cadmium Sulfide, can be used for multiple research field, as photochemical catalysis, optoelectronic pole, gas sensor etc.But at present institute reports that matrix material is that Cadmium Sulfide deposits or on the carbon nanotubes coated mostly, and the research be filled in by Cadmium Sulfide in carbon nanotube is also little.And carbon nanotube has the inner duct enriching size uniformity, can ensure that being filled into the intraluminal active specy of hollow is in nanoscale, has good nanometer confinement effect.Cadmium Sulfide is filled in the cadmium sulfide nano-particles that can be fixed size in carbon nanotube, stops the reunion of Cadmium Sulfide, again can in conjunction with the excellent photoelectric properties of carbon nanotube.In addition, for photocatalysis to degrade organic matter pollutent, carbon nanotube is due to its huge specific surface area and surface hydrophobicity, to coexist pollutent especially organic pollutant there is very strong adsorptive power, this inrichment can increase Cadmium Sulfide and contact with organic, thus improves its photocatalysis performance.Therefore, the heterojunction composite that Cadmium Sulfide is filled in carbon nanotube has huge application potential by photoelectricity and photocatalysis field.
Filling carbon nano-pipe mainly contains in-situ synthesis, physics completion method and chemical completion method.Because in-situ synthesis is high to equipment requirements, complicated operation, physics completion method is only suitable for the material of some low surface tensions, narrow application range, and chemical completion method to be a kind of operating procedure simple, the conventional completion method that controllability is strong.Existing many kinds of substance is in the news and is filled in carbon nanotube by chemical method.Pan etc. use wet-chemical by capillary action by Rh, Mn, Li, Fe (Xiulian Pan, Zhongli Fan, Wei Chen, Yunjie Ding, Hongyuan Luo and Xinhe BaoEnhanced ethanol production inside carbon-nanotube reactors containing catalytic particles, Nature Materials, 2007,7,507 – 511) and Fe
2o
3(Wei Chen, Xiulian Pan, Marc-GeorgWillinger, Dang Sheng Su, and Xinhe Bao, Facile Autoreduction of Iron Oxide/CarbonNanotube Encapsulates, J.Am.Chem.Soc., 2006,128,3136-3137) be filled in carbon nanotube.Technical scheme disclosed in CN101456079A uses identical method by plumbous nano-particles filled in carbon nanotube, and the filling of simple substance and oxide compound can adopt and first presoma is filled in carbon nanotube then dry process and obtaining under reduction or oxidizing atmosphere.And the technical scheme that US6090363A provides is when adopting the method to fill to Cadmium Sulfide sulfides, often use H
2the highly toxic substances such as S are as sulphur source, and operating procedure is complicated.Wet-chemical filling and vulcanization cadmium operating procedure is simple, mild condition, safety is controlled, but rarely have report so far, (the Qing Huang and LianGao such as Huang, Synthesis and characterization of CdS/multiwalled carbon nanotube heterojunctions, Nanotechnology15.2004.855-1860) find that there is small part Cadmium Sulfide when preparing carbon nanotube and supporting the matrix material of Cadmium Sulfide and be filled in carbon nanotube, but filling ratio is very low.
In sum, provide a kind of selectivity high, preparation cost is low, the method be effectively filled in carbon nanotube can be this area problem demanding prompt solution by Cadmium Sulfide.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, Cadmium Sulfide can optionally be filled in multi-walled carbon nano-tubes by the method, and reaction conditions is gentle, controllability is strong, production cost is low.
In order to achieve the above object, the invention provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, the method comprises the following steps:
Step one: pyroprocessing is carried out to multi-walled carbon nano-tubes with nitric acid, after cleaning by multi-walled carbon nano-tubes ultrasonic disperse in water;
Step 2: add cadmium source, the concentration forming cadmium source is the suspension liquid of 0.1mol/L-1.5mol/L, wherein, the mol ratio of described cadmium source and described multi-walled carbon nano-tubes is (0.1-2): 1, and the pH value of suspension liquid is adjusted to 1-5, after supersound process, carry out hydrothermal treatment consists, obtain reaction soln;
Step 3: obtain intermediate product by after above-mentioned reaction soln evaporate to dryness, clean intermediate product by dimethyl sulfoxide (DMSO);
Step 4: mixed with dimethyl sulfoxide (DMSO) by the intermediate product after cleaning, after carrying out solvent thermal reaction, centrifugal, cleaning, obtains the multi-walled carbon nano-tubes being filled with Cadmium Sulfide.
In multi-walled carbon nano-tubes provided by the present invention filling and vulcanization cadmium method in, nitric acid adopt concentrated nitric acid; Preferably, the concentration of the nitric acid adopted is 50-70wt%; More preferably, the concentration of the nitric acid adopted is 65wt%.
In multi-walled carbon nano-tubes provided by the present invention filling and vulcanization cadmium method in, preferably, the cadmium source adopted comprises the combination of one or more in Cadmium chloride fine powder, cadmium acetate and cadmium nitrate etc.
In the multi-walled carbon nano-tubes that the present invention carries filling and vulcanization cadmium method in, preferably, the internal diameter of the multi-walled carbon nano-tubes adopted is 3-20nm.
In the present invention, the measurement of the internal diameter of multi-walled carbon nano-tubes conventionally carries out statistical measurement, and the molar weight of carbon nanotube is then calculated by the quality of the carbon nanotube molar mass (being about 12g/mol) divided by carbon.
According to specific embodiment of the invention scheme, pH is regulated to use the protonic acid such as hydrochloric acid, nitric acid.
In the multi-walled carbon nano-tubes that the present invention carries filling and vulcanization cadmium method in, preferably, in described step one, the treatment temp of pyroprocessing is 120-150 DEG C, and the treatment time is 1-24h.
In the multi-walled carbon nano-tubes that the present invention carries filling and vulcanization cadmium method in, preferably, in described step 2 when carrying out hydrothermal treatment consists, the temperature of hydrothermal treatment consists is 80-170 DEG C, and the treatment time is 1-24h.
In the multi-walled carbon nano-tubes that the present invention carries filling and vulcanization cadmium method in, preferably, in described step 3, with dimethyl sulfoxide (DMSO) cleaning intermediate product 1-5 time.
In the multi-walled carbon nano-tubes that the present invention carries filling and vulcanization cadmium method in, preferably, in described step 4, the temperature of solvent thermal reaction is 150-250 DEG C, and the time is 1-24h.
According to specific embodiment of the invention scheme, when cleaning by dimethyl sulfoxide (DMSO) in step 3, add appropriate dimethyl sulfoxide (DMSO), cleaning object can be reached.
According to specific embodiment of the invention scheme, in step 4, the addition of dimethyl sulfoxide (DMSO) is according to carrying out the volume of container (such as reactor) of solvent thermal reaction and fixed, is generally no more than 60% of volume of a container.
In multi-walled carbon nano-tubes provided by the present invention filling and vulcanization cadmium method in, dimethyl sulfoxide (DMSO) is both as the solvent of cleaning reagent and solvent thermal reaction, also in reaction system, introduce sulphur source simultaneously, work with cadmium source one, with filling and vulcanization cadmium in multi-walled carbon nano-tubes.
According to specific embodiment of the invention scheme, the ultrasonic disperse in step one carries out 10min under 90Hz, and the supersound process in step 2 processes 1-4h under 90Hz.
Present invention also offers the matrix material of filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, it is prepared by aforesaid method.
In multi-walled carbon nano-tubes provided by the present invention, the matrix material of filling and vulcanization cadmium belongs to heterojunction composite, carbon nanotube has good confinement and conductivity, Cadmium Sulfide is filled into the particle diameter that can reduce Cadmium Sulfide in carbon nanotube, produce synergistic effect, make the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes become a kind of photoelectricity and photocatalyst material efficiently, can be used as photocatalyst, the optoelectronic pole material of solar cell and the negative material of lithium cell.
In multi-walled carbon nano-tubes provided by the present invention, the matrix material of filling and vulcanization cadmium is a kind of matrix material adopting wet chemistry method obtained, by hydrothermal method pre-treatment cadmium source and multi-walled carbon nano-tubes, cadmium source is at high temperature filled in multi-walled carbon nano-tubes efficiently, then solvent heat treatment (introducing sulphur source) is also carried out in the cadmium source optionally outside wash tube, worked in sulphur source and cadmium source one, the obtained multi-walled carbon nano-tubes being filled with Cadmium Sulfide.
In multi-walled carbon nano-tubes provided by the present invention, the method for filling and vulcanization cadmium is compared with prior art, has following advantages:
Cadmium Sulfide can be filled in multi-walled carbon nano-tubes by method provided by the invention, and the filling ratio of Cadmium Sulfide, higher than 60%, improves the utilization ratio to carbon nanotube inner duct.Simultaneously, method of the present invention is used to be filled in carbon nanotube by Cadmium Sulfide, utilize the confinement effect of carbon nanotube, effectively can stop the reunion of Cadmium Sulfide, be filled into obtained a kind of cadmium sulfide nano-particles high dispersing the heterojunction composite in carbon nanotube.
The reaction conditions of method provided by the present invention is gentle, and controllability is strong, and operating procedure is simple, and do not need to add catalyzer, production cost is low.
Accompanying drawing explanation
The TEM picture of the matrix material of filling and vulcanization cadmium in the multi-walled carbon nano-tubes of Fig. 1 prepared by embodiment 1;
The TEM picture of the matrix material of filling and vulcanization cadmium in the multi-walled carbon nano-tubes of Fig. 2 prepared by embodiment 2;
The TEM picture of the matrix material of filling and vulcanization cadmium in the multi-walled carbon nano-tubes of Fig. 3 prepared by embodiment 3;
The TEM picture of the matrix material of filling and vulcanization cadmium in the multi-walled carbon nano-tubes of Fig. 4 prepared by embodiment 4;
The TEM picture of the matrix material of filling and vulcanization cadmium in the multi-walled carbon nano-tubes of Fig. 5 prepared by embodiment 5.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
This enforcement provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, and the method specifically comprises the following steps:
Step one: get the multi-walled carbon nano-tubes (internal diameter 7-15nm) that 0.15g external diameter is 40-60nm, process 12h with 10mL concentrated nitric acid (65wt%) at 140 DEG C, after cleaning, ultrasonic disperse is in 15mL clear water;
Step 2: add 2.8g cadmium acetate, forming suspension liquid, is the HNO of 6M by concentration
3the pH value of suspension liquid is adjusted to 3, proceeds in 23mL reactor after supersound process 2h, at 120 DEG C of process 12h;
Step 3: above-mentioned solution is obtained intermediate product after evaporate to dryness at 80 DEG C, cleans intermediate product 3 times by dimethyl sulfoxide (DMSO);
Step 4: add 15mL dimethyl sulfoxide (DMSO), proceeds to 23mL reactor, 160 DEG C of solvent thermal reaction 12h, centrifugal, and cleaning, obtains the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes.
In the multi-walled carbon nano-tubes prepare the present embodiment, the matrix material of filling and vulcanization cadmium carries out TEM test, the TEM picture that test obtains as shown in Figure 1, carry out statistics to Fig. 1 can obtain, in this matrix material, the Cadmium Sulfide of about 80% has been filled in the duct of carbon nanotube, cadmium sulfide nano-particles high dispersing, uniform particle diameter, median size is 5nm.
Embodiment 2
This enforcement provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, and the method specifically comprises the following steps:
Step one: get the multi-walled carbon nano-tubes (internal diameter 7-15nm) that 0.15g external diameter is 40-60nm, process 12h with 10mL concentrated nitric acid (65wt%) at 140 DEG C, after cleaning, ultrasonic disperse is in 15mL clear water;
Step 2: add 5.6g cadmium acetate, forming suspension liquid, is the HNO of 6M by concentration
3the pH value of suspension liquid is adjusted to 3, proceeds in 23mL reactor after supersound process 2h, at 120 DEG C of process 12h;
Step 3: above-mentioned solution is obtained intermediate product after evaporate to dryness at 80 DEG C, cleans intermediate product 3 times by dimethyl sulfoxide (DMSO);
Step 4: add 15mL dimethyl sulfoxide (DMSO), proceeds to 23mL reactor, 160 DEG C of solvent thermal reaction 12h, centrifugal, and cleaning, obtains the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes.
In the multi-walled carbon nano-tubes prepare the present embodiment, the matrix material of filling and vulcanization cadmium carries out TEM test, the TEM picture that test obtains as shown in Figure 2, carry out statistics to Fig. 2 can obtain, in this matrix material, the Cadmium Sulfide of about 70% is filled in the duct of carbon nanotube, cadmium sulfide nano-particles in pipe still high dispersing, uniform particle diameter, median size is 5nm.
Embodiment 3
This enforcement provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, and the method specifically comprises the following steps:
Step one: get the multi-walled carbon nano-tubes (internal diameter 5-12nm) that 0.15g external diameter is 30-50nm, process 12h with 10mL concentrated nitric acid (65wt%) at 140 DEG C, after cleaning, ultrasonic disperse is in 15mL clear water;
Step 2: add 2.8g cadmium acetate, forming suspension liquid, is the HNO of 6M by concentration
3the pH value of suspension liquid is adjusted to 3, proceeds in 23mL reactor after supersound process 2h, at 120 DEG C of process 12h;
Step 3: above-mentioned solution is obtained intermediate product after evaporate to dryness at 80 DEG C, cleans intermediate product 3 times by dimethyl sulfoxide (DMSO);
Step 4: add 15mL dimethyl sulfoxide (DMSO), proceeds to 23mL reactor, 160 DEG C of solvent thermal reaction 12h, centrifugal, and cleaning, obtains the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes.
In the multi-walled carbon nano-tubes prepare the present embodiment, the matrix material of filling and vulcanization cadmium carries out TEM test, the TEM picture that test obtains as shown in Figure 3, carry out statistics to Fig. 3 can obtain, in this matrix material, the Cadmium Sulfide of 80% is about had to be filled in the duct of carbon nanotube, cadmium sulfide nano-particles high dispersing, uniform particle diameter, median size is 4nm.
Embodiment 4
This enforcement provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, and the method specifically comprises the following steps:
Step one: get the multi-walled carbon nano-tubes (internal diameter 3-5nm) that 0.15g external diameter is 8-15nm, process 12h with 10mL concentrated nitric acid (65wt%) at 140 DEG C, after cleaning, ultrasonic disperse is in 15mL clear water;
Step 2: adding 2.8g cadmium acetate and form suspension liquid, is the HNO of 6M by concentration
3the pH value of suspension liquid is adjusted to 3, proceeds in 23mL reactor after supersound process 2h, at 120 DEG C of process 12h;
Step 3: above-mentioned solution is obtained intermediate product after evaporate to dryness at 80 DEG C, cleans intermediate product 3 times by dimethyl sulfoxide (DMSO);
Step 4: add 15mL dimethyl sulfoxide (DMSO), proceeds to 23mL reactor, 160 DEG C of solvent thermal reaction 12h, centrifugal, and cleaning, obtains the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes.
In the multi-walled carbon nano-tubes prepare the present embodiment, the matrix material of filling and vulcanization cadmium carries out TEM test, the TEM picture that test obtains as shown in Figure 4, carry out statistics to Fig. 4 can obtain, in this matrix material, the Cadmium Sulfide being greater than 60% is had to be filled in the duct of carbon nanotube, cadmium sulfide nano-particles high dispersing, uniform particle diameter, median size is 3nm.
Embodiment 5
This enforcement provides the method for filling and vulcanization cadmium in a kind of multi-walled carbon nano-tubes, and the method specifically comprises the following steps:
Step one: get the multi-walled carbon nano-tubes (internal diameter 7-15nm) that 0.15g external diameter is 40-60nm, process 12h with 10mL concentrated nitric acid (65wt%) at 140 DEG C, after cleaning, ultrasonic disperse is in 15mL clear water;
Step 2: add 1.92g Cadmium chloride fine powder, forming suspension liquid, is the HNO of 6M by concentration
3the pH value of suspension liquid is adjusted to 3, proceeds in 23mL reactor after supersound process 2h, at 120 DEG C of process 12h;
Step 3: above-mentioned solution is obtained intermediate product after evaporate to dryness at 80 DEG C, cleans intermediate product 3 times by dimethyl sulfoxide (DMSO);
Step 4: add 15mL dimethyl sulfoxide (DMSO), proceeds to 23mL reactor, 160 DEG C of solvent thermal reaction 12h, centrifugal, and cleaning, obtains the matrix material of filling and vulcanization cadmium in multi-walled carbon nano-tubes.
In the multi-walled carbon nano-tubes prepare the present embodiment, the matrix material of filling and vulcanization cadmium carries out TEM test, the TEM picture that test obtains as shown in Figure 5, carry out statistics to Fig. 5 can obtain, in this matrix material, the Cadmium Sulfide of about 80% is filled in the duct of carbon nanotube, cadmium sulfide nano-particles high dispersing, uniform particle diameter, median size is 5nm.
Claims (7)
1. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes, it comprises the following steps:
Step one: pyroprocessing is carried out to multi-walled carbon nano-tubes with nitric acid, after cleaning by multi-walled carbon nano-tubes ultrasonic disperse in water;
Step 2: add cadmium source, the concentration forming cadmium source is the suspension liquid of 0.1mol/L-1.5mol/L, wherein, the mol ratio of described cadmium source and described multi-walled carbon nano-tubes is 0.1-2:1, and the pH value of suspension liquid is adjusted to 1-5, after supersound process 1-4h, carry out hydrothermal treatment consists, the temperature of hydrothermal treatment consists is 80-170 DEG C, and the treatment time is 1-24h, obtains reaction soln;
Step 3: obtain intermediate product by after described reaction soln evaporate to dryness, clean intermediate product by dimethyl sulfoxide (DMSO);
Step 4: mixed with dimethyl sulfoxide (DMSO) by the intermediate product after cleaning, after carrying out solvent thermal reaction, centrifugal, cleaning, obtain the multi-walled carbon nano-tubes being filled with Cadmium Sulfide, wherein, the temperature of solvent thermal reaction is 150-250 DEG C, and the time is 1-24h.
2. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1, wherein, the concentration of described nitric acid is 50-70wt%.
3. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1 and 2, wherein, the concentration of described nitric acid is 65wt%.
4. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1, wherein, described cadmium source comprises the combination of one or more in Cadmium chloride fine powder, cadmium acetate and cadmium nitrate.
5. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1, wherein, the internal diameter of described multi-walled carbon nano-tubes is 3-20nm.
6. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1, wherein, the treatment temp of described pyroprocessing is 120-150 DEG C, and the treatment time is 1-24h.
7. the method for filling and vulcanization cadmium in multi-walled carbon nano-tubes according to claim 1, wherein, in described step 3, with dimethyl sulfoxide (DMSO) cleaning intermediate product 1-5 time.
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| CN101157437A (en) * | 2007-10-23 | 2008-04-09 | 浙江大学 | Method for preparing carbon nano-tube/CdS nano flower composite material |
| CN102294250A (en) * | 2011-05-27 | 2011-12-28 | 北京大学 | Three-dimensional carbon nanotube nano composite catalyst, and preparation method and application thereof |
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| CN101157437A (en) * | 2007-10-23 | 2008-04-09 | 浙江大学 | Method for preparing carbon nano-tube/CdS nano flower composite material |
| CN102294250A (en) * | 2011-05-27 | 2011-12-28 | 北京大学 | Three-dimensional carbon nanotube nano composite catalyst, and preparation method and application thereof |
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