CN206396529U - The device of CNT is grown in serialization carbon fiber surface - Google Patents

The device of CNT is grown in serialization carbon fiber surface Download PDF

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Publication number
CN206396529U
CN206396529U CN201621358909.5U CN201621358909U CN206396529U CN 206396529 U CN206396529 U CN 206396529U CN 201621358909 U CN201621358909 U CN 201621358909U CN 206396529 U CN206396529 U CN 206396529U
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China
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carbon fiber
cnt
gas
serialization
fiber surface
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CN201621358909.5U
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Chinese (zh)
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王延相
郑林宝
王成国
王兴辉
秦建杰
路瑞佼
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Shandong University
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Shandong University
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Abstract

The utility model discloses a kind of device that CNT is grown in serialization carbon fiber surface, belong to the preparation facilities field of CNT.The device of the present utility model that CNT is produced in serialization carbon fiber surface, including body of heater two ends are provided with the chemical vapor deposition stove of opening;The gas-tight sealing for preventing air from entering furnace chamber is respectively arranged at the both ends open of the chemical vapor deposition stove, wherein one end open, which is on the extractor fan being provided with the outside of gas-tight sealing for waste gas to be extracted into outdoor, the gas-tight sealing, installs gas flowmeter;It is additionally provided with and is employed by motor belt motor in the device for continuously conveying of conveying carbon fiber on the outside of the both ends open of the chemical vapor deposition stove.The utility model can overcome the deficiencies in the prior art, realize CNT in the homogenization growth of serialization carbon fiber surface and industrialized production.

Description

The device of CNT is grown in serialization carbon fiber surface
Technical field
The utility model belongs to the preparation facilities field of CNT, and in particular to one kind is looked unfamiliar in serialization carbon fiber surface The device of long CNT.
Background technology
Since CNT Lijima discoveries since 1991, with its excellent physics, chemistry and electrical properties, as scientific research The focus of worker's research.The tensile strength of CNT is up to 100GPa, and Young's modulus is up to 1TPa, is a kind of preferably multiple Condensation material strengthens phase.Nowadays carbon fiber-based composite material is widely used in physical culture, medical treatment, automobile and aerospace field.But It is that single carbon fiber prepares composite with resin-bonded, because carbon fiber surface is smooth inert, is soaked during with resin-bonded Lubricant nature is poor, and interface adhesion is weaker, and mechanical adhesion center is few, and frictional force is small, between the carbon fiber composite layer for causing preparation Shear strength (ILSS) and interface shear strength (IFSS) are relatively low, and the unsticking that fiber and resin occur in production application is slided Phenomenon is moved, is unfavorable for its production and application.
CNT and carbon fiber, can be preferably with reference to preparing many chis of carbon fiber/carbon nanotube with as carbon material Reinforcement, the characteristics of effectively can either playing respective are spent, while can also increase carbon fiber specific surface area, enhancing and tree is used as Fat wellability more preferably, effectively plays high intensity, the high-modulus feature of composite.
Currently with chemical vapor deposition (CVD) method carbon fiber/carbon nanometer is prepared in carbon fiber surface growth CNT Pipe multi-scale reinforcing body is most commonly seen method.This method is all that the carbon fiber of destarch is passed through into surface modification treatment, then In its catalyst supported on surface precursor solution, and then the carbon fiber for being loaded with catalyst precursor is inserted in CVD stoves, By setting heating cooling process, first be passed through reducibility gas under reduction temperature is reduced into graininess by catalyst precursor, The growth that carbon-source gas carry out CNT is passed through under growth temperature again.But it is currently that such a method is that substep is carried out, also Serialization, large-scale industrial production can not be carried out, while the result that this pilot production is brought is in carbon fiber surface Often due to the winding twisting of fiber, the CNT for causing carbon fiber surface growth to obtain is uneven, these seriously govern The development in this experiment field.
In summary there is provided a kind of effective CVD device in the uniform carbon nanometer of serialization carbon fiber surface growth in situ Pipe is very necessary.
The content of the invention
The purpose of this utility model, which is that invention is a kind of, to be grown using chemical vapour deposition technique in serialization carbon fiber surface The process units of CNT, it is simple in construction easily to build, and realize CNT carbon fiber surface homogenization growth and Industrialized production.
In order to solve the above technical problems, the utility model offer technical scheme is as follows:
A kind of device that CNT is grown in serialization carbon fiber surface, including body of heater two ends are provided with the change of opening Gaseous phase deposition stove is learned, wherein:
The air seal for preventing air from entering furnace chamber is respectively arranged at the both ends open of the chemical vapor deposition stove Device, wherein one end open are in the extractor fan being provided with the outside of gas-tight sealing for waste gas to be extracted into outdoor, institute State and gas flowmeter is installed on gas-tight sealing;
It is additionally provided with and is employed by motor belt motor in the company of conveying carbon fiber on the outside of the both ends open of the chemical vapor deposition stove Continuous conveyer.
Wherein, the gas-tight sealing is three-level nitrogen curtain, and the device for continuously conveying is by the guide roller that is connected with each other Composition.
Further, the thermocouple for being used for controlling cavity temperature is housed on the chemical vapor deposition stove.
The utility model has the advantages that:
The utility model provides one kind and grows CNT in serialization carbon fiber surface using chemical vapour deposition technique Device, it is simple in construction easily to build, the deficiencies in the prior art can be overcome, homogenization of the CNT in carbon fiber surface is realized Growth and industrialized production.Gas-tight sealing can prevent air from entering furnace chamber so that the reduction and growth of CNT are not It is disturbed;Waste gas can be timely extracted into outdoor by extractor fan, it is ensured that experiment is normally carried out;Gas flowmeter contributes in real time Control is passed through the flow of various gases so that reduction reaction and growth course are more accurate;Device for continuously conveying causes carbon fiber Serialization, saves artificial quickening experiment rhythm.Chemical vapor deposition stove of the present utility model is open type, can serialization, big Scale carries out pilot production, and experimentation is simple to operate, and energy-efficient, solving sealed CVD stoves can only be carried out on a small quantity every time The preparation of sample, and consume energy it is larger the problem of.Avoid twisting of the carbon fiber in whole process simultaneously so that CNT exists Carbon fiber surface is more uniformly distributed distribution, improves the performance of carbon fiber/carbon nanotube multi-scale reinforcing body.
Brief description of the drawings
Fig. 1 is the dress that utilization chemical vapour deposition technique of the present utility model grows CNT in serialization carbon fiber surface Put schematic diagram;
Fig. 2 is the dress that utilization chemical vapour deposition technique of the present utility model grows CNT in serialization carbon fiber surface The scanning electron microscopic picture for the carbon fiber/carbon nanotube multi-scale reinforcing body put;
Fig. 3 is the dress that utilization chemical vapour deposition technique of the present utility model grows CNT in serialization carbon fiber surface The schematic flow sheet put.
Embodiment
The utility model provides one kind and produces CNT in serialization carbon fiber surface using chemical vapour deposition technique Device, to make the purpose of this utility model, technical scheme and effect clearer, clear and definite, one is entered to the utility model below Step is described in detail.It should be appreciated that specific embodiment described herein is not used to limit only to explain the utility model The utility model.
Embodiment 1
The device of the present utility model that CNT is grown in serialization carbon fiber surface, such as Fig. 1, including body of heater two ends are equal 4. the chemical vapor deposition stove for being provided with opening, is respectively arranged to prevent air at the both ends open of chemical vapor deposition stove 4. Into the gas-tight sealing of furnace chamber 3. 2., wherein one end open is in the outside of gas-tight sealing 2. and is provided with for will be useless 7. gas be extracted into the extractor fan of outdoor, and waste gas can be produced in experimentation, is escaped by stove both ends open, is produced in laboratory Pollution, is efficiently extracted into outdoor by extractor fan 7. by waste gas in time.Gas-tight sealing is 2. upper to install gas flowmeter 6., the continuous transmission employed by motor belt motor in conveying carbon fiber 1. is additionally provided with the outside of the both ends open of chemical vapor deposition stove 4. Device is 8..
It is of the present utility model serialization carbon fiber surface grow CNT device have it is simple in construction easily build, The deficiencies in the prior art can be overcome, homogenization growth and the advantage of industrialized production of the CNT in carbon fiber surface is realized. 2. gas-tight sealing can prevent air from entering furnace chamber so that the reduction and growth of CNT are interference-free;Extractor fan 7. waste gas can be timely extracted into outdoor, it is ensured that experiment is normally carried out;It is each that 6. gas flowmeter contributes to control to be in real time passed through Plant the flow of gas so that reduction reaction and growth course are more accurate;8. device for continuously conveying causes carbon fiber serialization, section Less manpower accelerates experiment rhythm.Chemical vapor deposition stove of the present utility model be open type, can serialization, given birth on a large scale Production experiment, experimentation is simple to operate, and energy-efficient, the preparation of a small amount of sample can only be carried out every time by solving sealed CVD stoves, And consume energy it is larger the problem of.Avoid twisting of the carbon fiber in whole process simultaneously so that CNT is in carbon fiber surface Distribution is more uniformly distributed, the performance of carbon fiber/carbon nanotube multi-scale reinforcing body is improved.
Before the growth CNT experiment of serialization carbon fiber surface, nitrogen valve is first turned on, adjustment air flow rate is extremely OK range, drains furnace chamber 3. interior air, is then turned on extractor fan 7. to take what is produced in experimentation away at any time Waste gas, and furnace chamber is 3. prohibited from entering air in whole experiment process in the presence of three-level nitrogen curtain, it is ensured that experiment is just Often carry out.Chemical vapor deposition stove 4. temperature program(me) is then set, heating cooling is 5. carried out to stove by thermocouple is gone back Former and growth experiment;By adjusting motor hauling speed and reduction temperature, the difference of time and gas flow, Ke Yijin are set The reduction growth experiment of row different technical parameters.
Embodiment 2
The side of CNT is produced using the device of the present utility model in carbon fiber surface producing Nano carbon tubes continuously Method, comprises the following steps:
Step 1:Chemical vapor deposition stove is warming up to 450 DEG C under helium atmosphere;
Step 2:The carbon fiber of load cobalt nitrate Catalyst precursor solutions is incorporated into step 1 by continuous transmission system Chemical vapor deposition stove in, be passed through hydrogen and be passed through with 0.6L/min speed in furnace chamber and reduced;
Step 3:Reduction is carried out after 10min, and chemical vapor deposition stove is warming up into 600 DEG C under helium atmosphere, helium Flow is passed through for 5L/min;
Step 4:The carbon fiber for the load reduction rear catalyst that step 2 is obtained is incorporated into step by continuous transmission system In 3 chemical vapor deposition stove, it is passed through hydrogen and propylene carries out carbon nano tube growth, the flow of acetylene is 0.6L/min;
Step 5:Grow after 10min, chemical vapor deposition stove carries out cooling down under helium atmosphere, that is, obtain carbon fine Dimension/CNT multi-scale reinforcing body.
From the point of view of the combination of embodiment 1 and embodiment 2 obtains carbon fiber/carbon nanotube multi-scale reinforcing body, such as Fig. 2, carbon Nanotube is all evenly distributed in carbon fiber surface, the diameter narrow distribution of CNT, is 20nm or so, the length of CNT It is different with the change of growth time, it is 150nm-10um, catalyst granules is located at the top of CNT, and growth pattern is Apical growth.
The utility model provides one kind and grows CNT in serialization carbon fiber surface using chemical vapour deposition technique Device, the deficiencies in the prior art can be overcome, realize CNT serialization carbon fiber surface homogenization growth and industry Metaplasia is produced, such as Fig. 3.First, compared with existing sealed chemical vapor deposition stove, chemical vapor deposition stove of the present utility model For open type, can serialization, carry out pilot production on a large scale, experimentation is simple to operate, energy-efficient, solves sealed Chemical vapor deposition stove can only carry out the preparation of a small amount of sample every time, and the problem of consume energy larger.Second, based on serialization, open Put in the reduction and growth course that chemical vapor deposition is tested in the chemical vapor deposition stove of formula, the utility model, carbon fiber is all Can quickly it leave at the heating of stove area, it is to avoid the influence in Liao Lu areas temperature-rise period to fiber, meanwhile, quickly leave stove area and also may be used To provide reliable data in time more to further investigate catalyst reduction and carbon nanotube growth process.3rd, this practicality is new Type is more traditional close in the carbon fiber/carbon nanotube multi-scale reinforcing body that serialization carbon fiber surface growth CNT is prepared Envelope formula chemical vapour deposition technique, it is to avoid the reduction of fibre strength caused by twisting of the carbon fiber in whole process so that carbon Nanotube is more uniformly distributed distribution in carbon fiber surface, to next preparing composite there is provided excellent basis.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, the scope of this specification record is all considered to be.
Described above is preferred embodiment of the present utility model, it is noted that for the ordinary skill of the art For personnel, on the premise of principle described in the utility model is not departed from, some improvements and modifications can also be made, these improvement Protection domain of the present utility model is also should be regarded as with retouching.

Claims (3)

1. a kind of device that CNT is grown in serialization carbon fiber surface, it is characterised in that be respectively provided with including body of heater two ends There is the chemical vapor deposition stove of opening, wherein:
The gas-tight sealing for preventing air from entering furnace chamber is respectively arranged at the both ends open of the chemical vapor deposition stove, Wherein one end open is in the extractor fan being provided with the outside of gas-tight sealing for waste gas to be extracted into outdoor, the gas Gas flowmeter is installed on sealing device;
It is additionally provided with and is employed by motor belt motor in the continuous biography of conveying carbon fiber on the outside of the both ends open of the chemical vapor deposition stove Send device.
2. the device according to claim 1 that CNT is grown in serialization carbon fiber surface, it is characterised in that described Gas-tight sealing is three-level nitrogen curtain, the device for continuously conveying by the guide roller group that is connected with each other into.
3. the device according to claim 1 that CNT is grown in serialization carbon fiber surface, it is characterised in that described The thermocouple for being used for controlling cavity temperature is housed on chemical vapor deposition stove.
CN201621358909.5U 2016-12-12 2016-12-12 The device of CNT is grown in serialization carbon fiber surface Expired - Fee Related CN206396529U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108221361A (en) * 2016-12-12 2018-06-29 山东大学 In the device and method of serialization carbon fiber surface growth carbon nanotube
CN115538157A (en) * 2022-10-27 2022-12-30 湖南博翔新材料有限公司 Method for producing carbon nano tube modified silicon carbide fiber by continuous vapor deposition method

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108221361A (en) * 2016-12-12 2018-06-29 山东大学 In the device and method of serialization carbon fiber surface growth carbon nanotube
CN115538157A (en) * 2022-10-27 2022-12-30 湖南博翔新材料有限公司 Method for producing carbon nano tube modified silicon carbide fiber by continuous vapor deposition method
CN115538157B (en) * 2022-10-27 2024-02-23 湖南博翔新材料有限公司 Method for producing carbon nanotube modified silicon carbide fiber by continuous vapor deposition method

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