CN109913980A - A kind of Heteroatom doping flexibility carbon fiber and its preparation method and application - Google Patents
A kind of Heteroatom doping flexibility carbon fiber and its preparation method and application Download PDFInfo
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- CN109913980A CN109913980A CN201910140255.0A CN201910140255A CN109913980A CN 109913980 A CN109913980 A CN 109913980A CN 201910140255 A CN201910140255 A CN 201910140255A CN 109913980 A CN109913980 A CN 109913980A
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Abstract
A kind of flexible carbon fiber of Heteroatom doping and its preparation method and application, belongs to new energy carbon-based material field.The present invention first cleans up the mankind and other animal hairs, and then directly or through being put into tube furnace after establishment, Heteroatom doping carbon fiber or its carbon fiber fabric is made by the method for vacuum carburization.Prepared carbon fiber is in tubular construction, conductivity is high, flexible, programmable shape, has regulatable aperture and physicochemical properties, and easy functionalization.Such flexible carbon fiber production method is simple, and raw material is cheap and easy to get, easy large scale preparation.By prepared carbon fiber and conjugated polymer it is compound after, can be used as super sensitive, reusable current sensor carrys out circuit for detecting, shows very strong actual application prospect.
Description
Technical field
The invention belongs to new energy carbon-based material technical field, specially one kind can be prepared on a large scale, high conductivity, machinery
It has excellent performance, the regulatable flexibility of physicochemical properties can work out the preparation method and application of carbon fiber
Background technique
With portable and wearable electronic product rapid development, explores and prepare multifunction flexible material and become and grind
Study carefully hot spot.Carbon material due to its cheap and easy to get, very high conductivity and excellent chemical and physical features, portable and
Wearable electronic has shown huge application prospect.Although the carbon fibre material based on carbon nanotube and graphene is wearable
The fields such as electronic device achieve certain success, and still, the preparation process of carbon nano-tube fibre is complicated, lead to its cost very
Height limits its large-scale application.It is urged in addition, can inevitably introduce heavy metal during preparation process carbon nanotube
Agent, cause its in many practical applications (such as semiconductor devices) there are problems；Graphene-based carbon fiber is then
It aoxidizes removing graphite first by strong acid/strong oxidizer, further obtained graphene is re-assemblied and is made.This operation
Process not only takes time and effort, but also the oxidation process of strong acid can cause carbon fiber structural greatly to destroy, to reduce stone
The physical property and electronic property of mertenyl carbon fiber.Based on this, exploring simple preparation process, to carry out large scale preparation performance excellent
Different flexibility, carbon fiber be there is an urgent need to, and chemistry and the long-standing challenge of material science.
To solve the above problems, the present invention will provide a kind of method of vacuum carburization, by the vacuum carburization mankind and other
The hair of animal to manufacture Heteroatom doping carbon fiber on a large scale.Heteroatomic content can be regulated and controled by carburizing temperature, and carbon
The aperture of fiber and fibrous inner structure can be adjusted by hair thickness and type.In addition, method designed by the present invention
Different-shape, carbon fibre material of different nature can be obtained by being worked out before carbonization or after carbonization.Prepared carbon fiber
Dimension or the carbon fibre material that is woven have high conductivity, high flexibility, regulatable physicochemical properties and easily functionalization.
It is the easy large scale preparation of vacuum carburization method flexibility carbon fibre material designed by the present invention, low in cost, show very strong reality
Border application prospect.
Summary of the invention
Object of the present invention is to for the huge actual application prospect of flexible carbon fibre material and current institute haveing excellent performance
Prepare carbon fibre material shortcomings (it is expensive for example, preparation process is complicated, contain heavy metal contaminants, mechanical performance
Difference etc.).The present invention will provide a kind of vacuum carburization strategy, manufacture the miscellaneous of the looks that hold its shape on a large scale by the mankind and animal hair
Atom doped carbon fiber, carbon fiber generated has high conductivity, high flexibility, regulatable Chemical Physics performance, very excellent
Different mechanical property.The invention provides a kind of technical support to prepare high performance flexible carbon fibre material.
The raw material provided by the invention for preparing Heteroatom doping carbon fiber be include human hair, pig hair, horse hair, the rabbit hair, wool,
All animal hairs including dog hair, cat hair, chicken feather, goose feather, duck's down, bear hair etc..
Heteroatom doping carbon fiber production method provided by the invention, include the following three steps:
(1) by hair and other animal hairs, simultaneously cleaning down one is arrived three times in acetone, ethyl alcohol and deionized water respectively,
Then it is dried for standby under 60 to 100 degrees Celsius；
(2) under vacuum conditions (0 pa is to 101.325 kPas) by presoma prepared by (1), 300 to 1200 degrees Celsius
Carbonization 1 to 10 hour, cooled to room temperature obtains Heteroatom doping single flexible carbon fiber.
(3) presoma prepared by (1) is prelisted and certain shape is made, then under vacuum conditions, 300 to 1200 take the photograph
Family name's degree is carbonized 1 to 10 hour, and cooled to room temperature obtains Heteroatom doping carbon fiber preform.
(4) single flexible carbon fiber prepared by (2) is directly compiled to certain shape, prepares carbon fiber preform.
(5) carbon fiber prepared by (2) and poly- diacetylenic acid is compound, prepared carbon fiber composite can be used as super
It is sensitive, reusable electric current indicator detection circuit.
Raw material of the present invention is cheap and easy to get, and preparation method is simple, easy to industrialized production.The Heteroatom doping prepared by hair
Carbon fiber has very high conductivity in room temperature, and conductivity is up to 600 Siemens/cms, and has very high anti-oxidant
Property, it 60 seconds patterns of calcination can not change under 1300 degrees Celsius of butane flames.The Heteroatom doping carbon fiber overall diameter
50 nanometers to 100 microns, 30 nanometers to 50 microns of interior diameter, and there is very high flexibility, and can further work out.The vacuum
Carbonization method can be carbonized all animal hairs, and obtain flexible carbon fibre material, and have a wide range of applications range.
Invention also provides the compound methods for preparing high-performance current indicator of carbon fiber and conjugated polymer.
For example, bis- pentadecane diacetylenic acid of 12- is supported on prepared flexible carbon fiber by 10, then at room temperature,
The UV Light initiation in 2 hours of 254 nano wave lengths polymerize, and obtains the carbon fibre composite of poly- diine acid functionalization.This is multiple
Condensation material can detecte 1 to 100 milliampere of direct current or alternating current.When 10 milliamperes of electric current passes through composite fibre, color exists
It is changed into red from blue in 0.2 second, shows very fast to electric current and sensitive indicative.Meanwhile in 254 nano wave lengths
UV Light under, red poly- diacetylenic acid composite and flexible carbon fiber can become again in 5 seconds blue, shown extremely strong
Reusability.Moreover, restoring the characteristic of primitive color after this electrochromism and discoloration again with ultraviolet light can repeat
1000 times or more, illustrate great actual application prospect.
The advantages and positive effects of the present invention:
The vacuum carburization mankind and other animal hairs proposed by the invention manufacture Heteroatom doping flexibility carbon fiber on a large scale
The method of dimension is easily mass produced, and raw material is cheap and easy to get.Prepared carbon fiber has high flexibility, high conductivity, excellent machine
Tool performance can be compiled into various devices.The aperture of carbon fiber can be adjusted by hair thickness and type.Different sizes,
The carbon fibre material of different structure can be prelisted the hair made by working out single carbon fiber or direct carbonization after carbonization
It obtains, to meet various application demands, there is very strong actual application prospect.In addition, flexible carbon fiber prepared by the present invention
Easy functionalization can show with the compound preparation high sensitivity of polymer, reusable current sense line in circuit detection field
Very strong application prospect out.
Compared to relatively generally existing at present carbon nanotube or graphene carbon fiber, raw material of the present invention is cheap and easy to get, preparation side
Method is simple, easy large scale preparation, and the flexible carbon fibre material mechanical performance that this method is prepared is high.Prepared by this method
Carbon fiber and polymer it is compound after, prepared carbon fibre composite can be used as function admirable, the electric current that can be recycled
Line is sensed, illustrates huge application prospect in circuit detection field.
Detailed description of the invention
Fig. 1 is the stereoscan photograph and digital photograph of the flexible carbon fiber prepared by hair vacuum carburization, wherein (1) is
The digital photograph of flexible carbon fiber；(2) stereoscan photograph of flexible carbon fiber surface；It (3) is flexible carbon fiber cross section
Stereoscan photograph；
Fig. 2 is that the internal stereoscan photograph and number that multi-compartment structural flexibility carbon fiber is presented is prepared by rabbit hair vacuum carburization
Code photo, wherein the digital photograph of (1) flexibility carbon fiber；(2) scanning in flexible carbon fiber inside multicell structural carbon fiber section
Electromicroscopic photograph；It (3) is the stereoscan photograph of flexible carbon fiber surface；
Fig. 3 is the stereoscan photograph and digital photograph that flexible carbon fiber is prepared by wool vacuum carburization, wherein (1) is flexible
The digital photograph of hollow carbon fiber；(2) stereoscan photograph of flexible carbon fiber surface；It (3) is flexible carbon fiber cross section
Stereoscan photograph；
Fig. 4 is to prepare flexible carbon fiber stereoscan photograph by pig hair vacuum carburization, wherein (1) is that flexible carbon fiber is transversal
The stereoscan photograph in face；(2) stereoscan photograph of flexible carbon fiber surface；
Fig. 5 is that flexible carbon fiber stereoscan photograph is prepared by horsetail vacuum carburization, wherein (1) is that flexible carbon fiber is horizontal
The stereoscan photograph in section；(2) stereoscan photograph of flexible carbon fiber surface；
Fig. 6 is the digital photograph of the lattice-like material of the flexible carbon fiber establishment prepared by hair vacuum carburization；
Fig. 7 is the digital photograph of the carbon film of the flexible carbon fiber proper alignment prepared by hair vacuum carburization；
Fig. 8 is the digital photograph of the staggered carbon film of flexible carbon fiber prepared by hair vacuum carburization；
Fig. 9 is the digital photograph of the cloth-like carbon material of the flexible carbon fiber establishment prepared by hair vacuum carburization；
Figure 10 is the digital photograph of the pigtail carbon material of the flexible carbon fiber establishment prepared by hair vacuum carburization；
Electromicroscopic photograph of the Figure 11 for the flexible carbon fiber and conjugated polymer prepared by hair vacuum carburization after compound, wherein
(1) individual carbon fibers surface electromicroscopic photograph；(2) carbon fiber/poly- two acid deficients composite material surface electromicroscopic photograph；
Figure 12 is the digital photograph that flexible carbon fiber/Conjugated Polymer Composites are applied in direct current electro-detection；
Figure 13 is the Raman spectrum of the compound carbon fiber of PDA, wherein the Raman spectrum of (1) original compound carbon fiber of PDA；
(2) become the Raman spectrum of the red compound carbon fiber of PDA from blue after electric current stimulation；(3) the red compound carbon fiber of PDA
Become the Raman spectrum of blue again again under the ultraviolet light stimulus of 254nm；
Specific embodiment
Below by some case study on implementation, illustrative explanation and help further understand the present invention, but embodiment details
Merely to illustrating the present invention, technical solution all under present inventive concept is not represented, therefore should not be understood as to the present invention
The restriction of total technical solution.For the technician, some unsubstantialities without departing from present inventive concept increase and change, example
Such as to change or replace with the technical characteristic of same or similar technical effect, the scope of the present invention is belonged to.
Embodiment 1 is prepared flexible tubular carbon fiber by human hair
By human hair in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it dries at 80 degrees celsius.Clean human hair is intercepted 10 centimetres, and is put into corundum Noah's ark, in the vacuum degree of 0.06 pa
Under, it is carbonized 2 hours in 1000 degrees Celsius, flexible tubular carbon fiber can be obtained, as shown in Figure 1.
Embodiment 2 prepares internal multicell structural flexibility carbon fiber by rabbit hair
By rabbit hair in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it dries at 60 c.Clean rabbit hair is intercepted 3 centimetres, and is put into corundum Noah's ark, in the vacuum degree of 0.01 pa
Under, it is carbonized 1 hour in 800 degrees Celsius, internal multicell structural flexibility carbon fiber can be obtained, as shown in Figure 2.
Embodiment 3 is sent out the flexible carbon fiber of preparation by wool
By wool in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity, and
It is dried under 100 degrees Celsius.Clean wool is intercepted 2 centimetres, and is put into corundum Noah's ark, under the vacuum degree of 1 pa, is taken the photograph in 600
Family name's degree is carbonized 3 hours, flexible carbon fiber can be obtained, as shown in Figure 3.
Embodiment 4 prepares flexible carbon fiber by pig hair
By the hair of pig in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, with decontamination, and
It is dried under 70 degrees Celsius.By clean 2.5 centimetres of interception of pig hair, and it is put into corundum Noah's ark, under the vacuum degree of 0.05 pa, in
700 degrees Celsius are carbonized 4 hours, flexible carbon fiber can be obtained, as shown in Figure 4.
Embodiment 5 prepares flexible carbon fiber by horsetail
By horse tail hair in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity, and
It dries at 60 c.Clean horse tail hair is intercepted 4 centimetres, and is put into corundum Noah's ark, under the vacuum degree of 2 pas, in 900
Degree Celsius carbonization 1 hour, flexible carbon fibre material can be obtained, as shown in Figure 5.
Embodiment 6 is compiled into lattice-like material by flexible carbon fiber
By hair respectively in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it is dried under 70 degrees Celsius.Clean hair is intercepted 4 centimetres, and is placed in two panels quartz plate, wherein hair and hair
Between there are gaps.The hair that quartz plate is clamped is put into corundum Noah's ark, under the vacuum degree of 0.04 pa, in 600 degrees Celsius of carbon
Change 2 hours, flexible tubular carbon fiber can be obtained, then by the interlaced establishment of carbon fiber, lattice-like material, such as Fig. 6 can be obtained
It is shown.
The membranaceous carbon material of embodiment 7, the same sequence proper alignment of flexible carbon fiber establishment
By hair respectively in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it is dried under 90 degrees Celsius.Peace and quiet hair is intercepted 5 centimetres, and is put into corundum Noah's ark by the same direction, in 0.06 pa
It under vacuum degree, is carbonized 1 hour in 1000 degrees Celsius, the membranaceous carbon materials by flexible carbon fiber same direction proper alignment can be obtained
Material, as shown in Figure 7.
The staggered membranaceous carbon material that embodiment 8, flexible carbon fiber are worked out
By hair respectively in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it dries at 60 c.Peace and quiet hair is intercepted 5 centimetres, and is put into corundum Noah's ark by different directions establishment, 0.04
It under the vacuum degree of pa, is carbonized 2 hours in 800 degrees Celsius, can be obtained by the staggered membranaceous carbon material of flexible carbon fiber, such as scheme
Shown in 8.
The cloth-like carbon material that embodiment 9, flexible carbon fiber are worked out
By hair respectively in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it is dried under 70 degrees Celsius.Peace and quiet hair is intercepted 4.5 centimetres, and is compiled into cloth-like structure, corundum Noah's ark is put into, 1
Under the vacuum degree of pa, it is carbonized 2 hours in 700 degrees Celsius, cloth-like carbon material can be obtained, as shown in Figure 9.
The preparation for the pigtail carbon material that embodiment 10, flexible carbon fiber are worked out
By hair respectively in acetone, ethyl alcohol and deionized water ultrasonication and cleaning down three times, to remove impurity,
And it dries at 80 degrees celsius.The hair cleaned up is intercepted 11 centimetres, and is compiled into pigtail pattern and is put into corundum Noah's ark,
It under the vacuum degree of 0.01 pa, is carbonized 2 hours under 1000 degrees Celsius, the pigtail material of flexible carbon fiber composition can be obtained, such as scheme
Shown in 10.
Embodiment 11 prepares the poly- compound carbon fiber of two acid deficients
The tetrahydrofuran solution for configuring 10,12-, the bis- pentadecane diacetylenic acid of 10 mg/mls, is prepared by embodiment 1 soft
Property carbon fiber immerse precursor liquid in, evaporate solvent at room temperature.Before polymerization, by treated, flexible carbon fiber is placed in vent cabinet cruelly
Dew 24 hours, at room temperature, polymerize 2 hours under the ultraviolet light of 254 nano wave lengths, the compound carbon fiber of polymer can be obtained, and such as schemes
Shown in 11.
Embodiment 12, application
Power supply is provided with direct current digital power table, in compound carbon fiber access circuit prepared by embodiment 11, when passing through 7
When the electric current of milliampere, compound carbon fiber became red from blue in 0.2 second.Power supply is closed, is irradiated and is become with 254 nano-ultraviolet lights
Carbon fiber after color can be become again again original blue (as shown in figure 12) in 15 seconds by red, the process repeatable 50
It is secondary, show very strong reusability and stability (as shown in figure 13).
Claims (12)
1. a kind of preparation method for the Heteroatom doping carbon fiber that can be prepared on a large scale, it is characterised in that specific step is as follows:
(1) hair or other animal hairs are flushed three times in acetone, ethyl alcohol and deionized water at 60 to 100 degrees Celsius respectively
Under be dried for standby；
(2) the processed hair of step (1) is sheared or is compiled into required pattern, be placed in corundum Noah's ark, be put into tube furnace；
(3) presoma prepared by (2) is carbonized 1 to 10 hour for 300 to 1200 degrees Celsius under vacuum conditions, is naturally cooled to
Room temperature obtains the carbon fibre material of Heteroatom doping individual carbon fibers or establishment.
2. preparation method according to claim 1, which is characterized in that the carbonization presoma can be a variety of hairs, example
Such as human hair, the rabbit hair, horse hair, pig hair, wool, ox hair, duck's down, chicken feather, goose feather, monkey hair, dog hair, cat hair, all animals of bear hair
Hair.
3. preparation method according to claim 1, which is characterized in that the hair presoma can have a variety of establishment sides
Method obtains the structures such as single structure, pigtail, hair cluster.
4. according to claim 1, preparation method described in 2 and 3, which is characterized in that carbonization vacuum degree is 0 pa to 101.325 thousand
Between pa.
5. according to claim 1, preparation method described in 2 and 3, which is characterized in that carburizing temperature range is 300 to 1200 Celsius
Degree, heating rate are 3 to 10 degrees celsius/minutes, and carbonization time 1 to 10 hour, nitrogen, sulphur atom content existed in obtained carbon material
Between 5% to 20% range.
6. according to claim 1, preparation method described in 2 and 3, which is characterized in that carbon fiber and establishment prepared by step (3)
Carbon material is single hollow carbon fiber, carbon pigtail, carbon grid, the structures such as carbon film.
7. according to claim 1,2 and 3 preparation method, which is characterized in that obtained by preparation method described in step (3)
Heteroatom doping carbon fiber inner hollow, internal diameter are about between 10 nanometers to 100 microns, and outer is 10 nanometers to 200 microns.
8. according to claim 1, method described in 2 and 3, which is characterized in that the conductance of prepared Heteroatom doping carbon fiber
Rate has very high inoxidizability between 50 to 2000 Siemens/cms, can be under 1300 degrees Celsius, in air
60 seconds holding primary morphologies of calcination do not change.
9. according to claim 1, method described in 2 and 3, which is characterized in that the Heteroatom doping prepared by human hair vacuum carburization
Carbon fiber has good mechanical property, and tensile strength is up to 100 to 400 megapascal.
10. a kind of vacuum carburization method described in claim 1,2,3,4,5.
11. Heteroatom doping tubulose carbon fiber and other structural carbon materials that a kind of claim 1,2 and 3 preparation methods obtain.
12. preparation method according to claim 6 or 7, which is characterized in that the Heteroatom doping carbon fiber can load
The further functionalization of polymer.The wherein specific practice of load aggregation object are as follows: will be obtained according to power 1,2 and 3 preparation methods
To carbon fiber be immersed in 0.1 to 100 mM every liter 10,12-, bis- pentadecane diacetylenic acid tetrahydrofuran solution in, in room temperature
Lower solvent evaporation, and in ventilation exposure 2-48 hours.Then at room temperature, in the UV Light 0.5 of 254 nano wave lengths to
Initiation polymerisation step obtains the compound carbon fibre material of poly- diine acid functionalization within 5 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111554888A (en) * | 2020-04-09 | 2020-08-18 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1089534A (en) * | 1963-11-21 | 1967-11-01 | Siemens Planiawerke Ag | The carbonization of animal fibre materials |
| KR100749125B1 (en) * | 2006-11-24 | 2007-08-13 | 지에스칼텍스 주식회사 | Hollow carbon fiber using hair and method for manufacturing the same |
| CN107195480A (en) * | 2017-04-11 | 2017-09-22 | 国家纳米科学中心 | A kind of flexible, porous carbon material and preparation method and application |
| CN108745399A (en) * | 2018-05-28 | 2018-11-06 | 南开大学 | Heteroatom doping porous carbon membranes and its preparation method and application |
-
2019
- 2019-02-25 CN CN201910140255.0A patent/CN109913980A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1089534A (en) * | 1963-11-21 | 1967-11-01 | Siemens Planiawerke Ag | The carbonization of animal fibre materials |
| KR100749125B1 (en) * | 2006-11-24 | 2007-08-13 | 지에스칼텍스 주식회사 | Hollow carbon fiber using hair and method for manufacturing the same |
| CN107195480A (en) * | 2017-04-11 | 2017-09-22 | 国家纳米科学中心 | A kind of flexible, porous carbon material and preparation method and application |
| CN108745399A (en) * | 2018-05-28 | 2018-11-06 | 南开大学 | Heteroatom doping porous carbon membranes and its preparation method and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111554888A (en) * | 2020-04-09 | 2020-08-18 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
| CN111554888B (en) * | 2020-04-09 | 2022-04-29 | 天津工业大学 | Anode material containing rabbit hair hollow carbon fibers for lithium-sulfur battery and preparation method thereof |
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Application publication date: 20190621 |