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Determining apparatus and method for amorphous carbon content in carbon nanometer tubes

A carbon nanotube and amorphous carbon technology, applied in the field of chemical analysis, can solve the problems of inaccurate test results, large errors, small observation range and objects, etc.

Inactive Publication Date: 2011-09-21
SHENZHEN DYNANONIC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

P.X.Hou et al. in Carbon, 2002, Pages 81-85, used TEM and TGA to analyze the content of multi-walled carbon nanotubes (MWNT). Due to the large error of TEM, there are many human factors, and it is also because the scope of observation and the object are too small that the observation The results are clearly uncertain
However, the TGA method is significantly affected by the content and composition of catalyst impurities in the sample. In addition, due to the large amount of heat released when air reacts with amorphous carbon, the local temperature exceeds the combustion temperature of carbon nanotubes, resulting in inaccurate test results and large errors. Big; B.Kitiyanan etc. in Chem.Phys.Lett.317 (2000) 497. Introduced the standard TPO method to quantitatively analyze the content of SWNT and MWNT, the error of this method is also very large, the main reason is the same as TGA

Method used

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  • Determining apparatus and method for amorphous carbon content in carbon nanometer tubes
  • Determining apparatus and method for amorphous carbon content in carbon nanometer tubes
  • Determining apparatus and method for amorphous carbon content in carbon nanometer tubes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1.1 Sample preparation

[0050]1.1.1 Take about 1.3g of multi-walled carbon nanotube sample 6 and put it into a vacuum oven at 170°C to dry for 3 hours;

[0051] 1.1.2 Accurately weigh 1.00g of multi-walled carbon nanotube sample 6, add 0.01g of nickel oxide lithium powder, and mix well.

[0052] 1.2 Determination

[0053] 1.2.1 Add the dried multi-walled carbon nanotube sample m=0.1375g (wherein the catalyst m 2 = 0.0014g).

[0054] 1.2.2 After constant weight, accurately weigh the total mass m of the U-shaped tube 5 and the multi-walled carbon nanotube sample 6 0 =6.5730.

[0055] 1.2.3 Install the U-shaped tube 5 containing the multi-walled carbon nanotube sample 6 in the heating furnace 7 .

[0056] 1.2.4 Move the sample stage 8 from the slide bar 9b to 9a, open the carbon dioxide pressure reducing valve, and control the flow rate of carbon dioxide at 20ml / min.

[0057] 1.2.5 Turn on the temperature controller 14 to heat the U-shaped tube 5 through the heating...

Embodiment 2

[0065] 2.1 Sample preparation

[0066] 2.1.1 Take about 1.3g of double-walled carbon nanotube sample 6 and put it into a vacuum oven at 170°C to dry for 3 hours;

[0067] 2.1.2 Accurately weigh 1.00 g of double-walled carbon nanotube sample 6 (sampling observation, see Figure 3a ), add 0.01g of nickel oxide powder, and mix well.

[0068] 2.2 Determination

[0069] 2.2.1 Add the dried double-walled carbon nanotube sample m=0.2363g (wherein the catalyst m 2 = 0.0024 g).

[0070] 2.2.2 After constant weight, accurately weigh the total mass m of U-shaped tube 5 and double-walled carbon nanotube sample 6 0 = 6.4776 g.

[0071] 2.2.3 Install the U-shaped tube 5 equipped with the double-walled carbon nanotube sample 6 in the heating furnace 7 .

[0072] 2.2.4 Move the sample stage 8 from the slide bar 9b to 9a, open the carbon dioxide pressure reducing valve, and control the flow rate of carbon dioxide at 20ml / min.

[0073] 2.2.5 Turn on the temperature controller 14 to heat ...

Embodiment 3

[0081] In order to determine that the amount of reduction has only amorphous carbon, we will measure again the sample (sample in embodiment 2) that has been determined:

[0082] 3.1 Determination

[0083] 3.1.1 The total mass of the sample and the U-shaped tube 5 is measured in Example 2 0 = 6.4665g.

[0084] 3.1.2 Install the U-shaped tube 5 equipped with the double-walled carbon nanotube sample 6 in the heating furnace 7 .

[0085] 3.1.3 Move the sample stage 8 from the slide bar 9b to 9a, open the carbon dioxide pressure reducing valve, and control the flow rate of carbon dioxide at 20ml / min.

[0086] 3.1.4 Turn on the temperature controller 14 to heat the U-shaped tube 5 through the heating furnace 7 .

[0087] 3.1.5 Raise the temperature from room temperature to 700°C (heating rate 20°C / min), keep the temperature constant for 30min, and turn off the heating furnace 7.

[0088] 3.1.6 When the temperature drops to (200±20)°C, turn off the carbon dioxide gas.

[0089] 3...

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Abstract

A method for determining amorphous carbon content in nanocarbon tube includes heating nanocarbon tube sample in U form tube at 500 - 1000 deg.c, using carbon dioxide and transition metal oxide as catalyst combination to generate oxidizing reaction at U form tube bottom, weighing and calculating out loss amount of U form tube and nanocarbon tube total weight before reaction and after reaction, using loss amount as amorphous carbon content.

Description

technical field [0001] The invention relates to the measurement of amorphous carbon content in carbon nanotubes, belongs to the field of chemical analysis, and is suitable for the measurement of amorphous carbon content in various carbonaceous materials. Background technique [0002] At present, there are many methods for preparing carbon nanotubes, and the preparation process of various carbon nanotubes is accompanied by the generation of amorphous carbon, which is entrapped or covered in the carbon nanotube products. The amount of its content directly affects the performance of carbon nanotube products, and how to accurately measure amorphous carbon is very important. Since it is difficult to separate amorphous carbon and carbon nanotubes, among the known methods in the world, there is no method that can accurately measure the content of amorphous carbon in carbon nanotubes. JoseE et al. in Chemical Physics Letters 2003, Pages 302-309, introduced the use of 1-Id / Ig in the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N5/04
Inventor 孔令涌王允实杨海燕
Owner SHENZHEN DYNANONIC