CN107177905A - A kind of carbon fiber prepared based on discarded bamboo chopsticks hydrothermal carbonization method and its application - Google Patents
A kind of carbon fiber prepared based on discarded bamboo chopsticks hydrothermal carbonization method and its application Download PDFInfo
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- CN107177905A CN107177905A CN201710492244.XA CN201710492244A CN107177905A CN 107177905 A CN107177905 A CN 107177905A CN 201710492244 A CN201710492244 A CN 201710492244A CN 107177905 A CN107177905 A CN 107177905A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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Abstract
Biomass energy obtains the favor of scientists as a kind of new regenerative resource, the characteristics of by its environmental protection, cheap, wide material sources.Discarded bamboo chopsticks do not obtain the processing compared with science, cause very big waste always as a kind of common biomass resource.The present invention is using discarded bamboo chopsticks as raw material, prepare carbon fiber using hydro-thermal method and the technique that is combined of carbonization, and obtained carbon fiber is carried out XRD, SEM, Raman and it is infrared etc. characterize, as a result show, sample is fibre structure, surface covers a large amount of folds, and length is up to 20 200 μm, and diameter is about 3 ~ 5 μm, and carbon fiber is based on agraphitic carbon, with certain degree of graphitization, there be substantial amounts of active function groups on surface, and researching value is high.
Description
Technical field
The present invention relates to a kind of carbon fiber, further specifically it is related to one kind and uses hydrothermal carbonization method by discarded bamboo chopsticks system
For into carbon fiber, belong to field of nanometer material technology.
Background technology
The excessive velocities of world today's traditional energy such as consumption such as oil, coal, remaining primary energy can not expire
The need for the growing economic society of the sufficient mankind, we are badly in need of finding a kind of environmental protection, cheap regenerative resource
To replace traditional energy.And biomass carbon material has the characteristics of some are very outstanding, the need for our mankind can be met.Institute
To find reproducible new energy particularly important for us., can be with China and bamboo chopsticks are as one kind of biomass resource
Say it is to be seen everywhere, but people do not deal carefully with these discarded bamboo chopsticks but, many bamboo chopsticks are all taken as rubbish directly to fire
Burn or fill, this is the huge waste to valuable biomass resource.Invention is prepared discarded bamboo chopsticks using hydrothermal carbonization method
As new biomass carbon material, turn waste into wealth, improve the reasonable utilization rate of discarded bamboo chopsticks, to solve the energy crisis of China
Propose new thinking and method.
Up to the present, the preparation method of very many biomass carbon materials is there is, current most common preparation method
Mainly there are thermal decomposition method, microwave carbonizatin method, vapour deposition process and hydrothermal carbonization method etc..Hydrothermal carbonization method is using biomass as original
Material, water is reaction medium, in sealed container, under certain temperature conditionss, the pressure produced in water itself and inert gas
Under pressurization, occurs complicated reaction, so that biomass to be converted to the method for biomass carbon material.Hydrothermal carbonization method has following
Advantage:(1) hydrothermal carbonization method is relatively low to equipment requirement, and simple to operate, the relatively good control of process;(2) hydrothermal carbonization method
During, the reaction of its own can discharge part energy, so that the energy required for the method is reduced, therefore hydrothermal carbonization method
Energy consumption is relatively low;(3) hydro-thermal reaction is mainly dehydration, the C that effectively can be fixed in abandoned biomass, so its efficiency will height
In other conventional methods, the also suitable environmental protection of hydrothermal carbonization method, generation it is of reduced contamination;(4) hydro-thermal carbon material is different from heat
Decomposition method, it have preferable protection to members such as O, N in biomass, so the oxygen-containing functional group quantity on its surface is substantially more
In the biomass carbon material prepared by other method.These advantages also cause the material prepared to can be widely used in a variety of necks
Domain.
The content of the invention
The discarded bamboo chopsticks collected from dining room are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thickness are whittled into pocket knife
0.05cm), Constant Temp. Oven is put into, is dried 2-4 hours at 40-60 DEG C, the bamboo scraps after drying is put into equipped with 3-
In the polytetrafluoroethyllining lining stainless steel high pressure water heating kettle of 5mol/L KOH reaction dissolvents, lid is tightened, water heating kettle is put into temperature
Degree is set as in 160-200 DEG C of Constant Temp. Oven, is taken out after 2-4h, is cooled to room temperature, takes out sample, uses high-purity washing
Wash and filter, to filtrate pH=7, then sample is put into the Constant Temp. Oven that temperature is 50-80 DEG C and dries and weighs,
Obtained sample is put into the ceramic crucible of cleaning, is put into high-temperature atmosphere tube furnace, is passed through the High Purity Nitrogen that purity is 99.99%
Gas.Under conditions of nitrogen flow is 100-200mL/min, tube furnace is raised to 700- with 6-10 DEG C/min speed from room temperature
1000 DEG C, keeping temperature 4-8h is carbonized, after carbonization terminates, and is taken out the sample in crucible, is washed with 3-5mol/L watery hydrochloric acid
Filtering is washed, and 2-4h is dried under conditions of 60-90 DEG C, final carbon fibre material is obtained.
Above-mentioned reaction dissolvent can also be NaOH in addition to KOH.
Obtained after the quality before and after weighing sample experiments, the mass loss rate of bamboo wood material is 43-49%.
Carbon fiber will be obtained and carry out the physical properties such as XRD, SEM, Raman spectrum and infrared spectrum sign.
Carbon fibre material is subjected to XRD signs, takes sample to be put in right amount on instrument objective table, adjustment voltage and current point
Not Wei 40kV, 250mA, sweep speed be 10 °/min, the θ of scanning range 2 be 10 °~80 °, carbon fibre material is scanned, obtained
To the XRD spectrum of material, it can be seen that occurring a wider diffraction maximum at 20 ° or so, corresponding crystal face is (002),
Carbon fibre material that this explanation is prepared is primarily present form for agraphitic carbon, and at 44 ° of collection of illustrative plates there is also diffraction maximum, it is right
(100) crystal face of graphite is answered, this represents that sample has certain degree of graphitization, and the crystalline substance in carbon fiber can be obtained from collection of illustrative plates
Face is based on (002).X-ray diffraction intensity from (002) crystal face is set to I (002), the X-ray from (100) crystal face is spread out
When penetrating intensity and being set to I (100), 2.5≤[I (002)/I (100)]≤2.9 are met.
Carbon fibre material is subjected to SEM shape characteristic analyses, amplify 3000 times to carbon fibre material obtains phase with 30000 times
The SEM figures answered.Picture is observed it can be found that the carbon material prepared by us is mainly fibre structure, the distribution of carbon fiber is compared
Uniformly, the length of carbon fiber is up to 20-200 μm, about 3-5 μm of diameter, and carbon fiber surface is dispersed with substantial amounts of fold.This
Illustrate that it can be applied among the electrode material of sorbing material or battery as a kind of new material.
Carbon fibre material is subjected to Raman spectrum analysis, takes sample to be placed in right amount on slide, is flattened with cover glass rearmounted
In on objective table, viewing angle is adjusted, Raman spectrogram is obtained.Picture is observed it can be found that there are two peaks obvious.Keep left
The corresponding Raman shift 1360cm of side-1The peak at place is referred to as D peaks, and effect is defect in the crystal structure for can embody carbon material
Quantity, defects count it is more just explanation samples disordering degree it is higher.And the corresponding Raman shift 1600cm on right side-1Place
For G peaks, illustrate that carbon material has certain degree of graphitization, while also demonstrating the result of XRD diffraction analysis.In experimental study
In, we are by D peaks and G peak intensity ratio IsD/IGAs the randomness factor of carbon-based material.Sample ID/IGValue be 1.0-1.1,
This explanation material internal has certain defect.
Carbon fibre material is subjected to Fourier infrared spectrum analysis, FFIR (FTIR) can be studied point
The structure and chemical bond, the measure and molecular symmetry of such as force constant of son, the key of molecule can be determined using method of infrared spectrophotometry
Long and bond angle, and thus speculate molecule steric-configuration.The power of chemical bond can be deduced according to the force constant of gained, by normal frequency
Computational Thermodynamics function etc..According to the Fourier infrared spectrum figure of carbon fibre material it can be found that sample is in 3200-3500cm-1
There is a peak in place, this is the absworption peak of hydroxyl, in 1610cm-1And 1730cm-1The absworption peak at place belongs to C=C (aromatic rings) and shaken
Dynamic peak and C=O (ester, carboxyl or carbonyl) vibration peak, illustrate that biomass carbon material surface has more active function groups, have
There is certain feature.
Compared with the prior art, beneficial effects of the present invention are:
The present invention uses 3-5mol/L KOH solutions to prepare bamboo fibre for solvent, and the mass loss rate of bamboo wood material is 43-
49%.Physical property sign is carried out to carbon fiber, it has been found that the material carbon fiber after carbonization is uniformly dispersed, and length is up to 20-
200 μm, about 3-5 μm of diameter, sample surfaces have a large amount of folds, and with certain degree of graphitization, mainly with without fixed
Based on type carbon, there be substantial amounts of oxygen-containing functional group on surface.These all illustrate that it has certain research as a kind of new material
Value.Also, the wide material sources of discarded bamboo chopsticks, it is cheap, but never obtain the processing of the mankind properly.The present invention is obtained
This new material can be as electrode material or sorbing material, with important Research Significance.
Brief description of the drawings
【Fig. 1】For the digital photograph of the bamboo wood material of various concentrations KOH solution processing;
【Fig. 2】For the XRD spectrum of carbon fiber;
【Fig. 3】The SEM for being carbon fiber under different amplification figures (a) amplify 3000 times, and (b) amplifies 30000 times;
【Fig. 4】For the Raman spectrogram of carbon fiber;
【Fig. 5】The infrared spectrogram of carbon fiber.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
The disposable bamboo chopsticks for collecting are cleaned up, and are whittled into bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm), and
3h is dried at 50 DEG C.Afterwards, 1g bamboo scraps are put into the polytetrafluoroethyllining lining of the 3mol/L KOH solutions equipped with 70mL not
In steel high pressure water heating kettle of becoming rusty, lid is tightened.Water heating kettle is put into temperature to be set as in 180 DEG C of Constant Temp. Oven, after 4h
Take out.After water heating kettle is cooled to room temperature, twist the lid off, open hydro-thermal tank, take out sample, with high-purity water washing and filter, extremely
Sample, is then put into the Constant Temp. Oven that temperature is 60 DEG C and dries and weigh by filtrate pH=7.Sample is put into clean
Crucible in, cover tightly lid, be put into high-temperature atmosphere tube furnace.The air-tightness of tube furnace is checked, 99.99% High Purity Nitrogen is passed through
Gas.Nitrogen flow is adjusted after 150mL/min, tube furnace is raised into 800 DEG C, carbonisation from room temperature with 8 DEG C/min speed
In to ensure that nitrogen is sufficient constantly.Rise to after 800 DEG C, keeping temperature 4h.After carbonization terminates, the sample in crucible is taken out, is used
4mol/L watery hydrochloric acid washing and filtering, and 2h is dried at 80 DEG C, obtain carbon fibre material.
Embodiment 2
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 2 hours at 40 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 5mol/L KOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 160 DEG C of Constant Temp. Oven, 4h
After take out, be cooled to room temperature, take out sample, washing suction filtration to filtrate is neutrality, and sample then is put into the electricity that temperature is 50 DEG C
Dry and weigh in hot thermostatic drying chamber, after by sample be transferred to cleaning crucible in, be put into high-temperature atmosphere tube furnace, be passed through pure
Spend the high pure nitrogen for 99.99%.Nitrogen flow is set as 100mL/min, and by tube furnace with 6 DEG C/min speed from room temperature
1000 DEG C are raised to, keeping temperature 4h is carbonized, after carbonization terminates, take out the sample in crucible, washed with 4mol/L watery hydrochloric acid
Filtering is washed, and 4h is dried at 60 DEG C, carbon fibre material is obtained.
Embodiment 3
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 4 hours at 60 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 4mol/L KOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 200 DEG C of Constant Temp. Oven, 2h
After take out, be cooled to room temperature, take out sample, with high-purity water washing and filter, to filtrate pH=7, sample is then put into temperature
To dry and weighing in 80 DEG C of Constant Temp. Ovens, in the crucible that sample is put into cleaning, high-temperature atmosphere tube furnace is put into,
It is passed through 99.99% high pure nitrogen that gas flow is 200mL/min.Tube furnace is raised to 10 DEG C/min speed from room temperature
800 DEG C, keeping temperature 4h is carbonized, after carbonization terminates, and takes out the sample in crucible, washed with 4mol/L watery hydrochloric acid
Filter, and 3h is dried at 70 DEG C, obtain carbon fibre material.
Embodiment 4
The disposable bamboo chopsticks for collecting are cleaned up, and are whittled into bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm).It
Afterwards, 1g bamboo scraps are put into the polytetrafluoroethyllining lining stainless steel high pressure water heating kettle of the 6mol/L KOH solutions equipped with 70mL,
Tighten lid.Water heating kettle is put into temperature to be set as in 180 DEG C of Constant Temp. Oven, taken out after 2h.Treat that water heating kettle is cooled down
To after room temperature, twist the lid off, open hydro-thermal tank, take out sample, with high-purity water washing and filter, be neutrality to filtrate, then will
Sample is put into the Constant Temp. Oven that temperature is 50 DEG C and dries and weigh.Sample is put into clean crucible, covered tightly
Lid, is put into high-temperature atmosphere tube furnace.The air-tightness of tube furnace is checked, 99.99% high pure nitrogen is passed through, gas flow is adjusted
For 120mL/min.Tube furnace is raised to 800 DEG C from room temperature with 9 DEG C/min speed, to ensure that nitrogen is sufficient not in carbonisation
It is disconnected.Rise to after 800 DEG C, keeping temperature 4h.After carbonization terminates, the sample in crucible is taken out, is washed with 3.5mol/L watery hydrochloric acid
Filtering, and 2h is dried at 90 DEG C, obtain carbon fibre material.
Embodiment 5
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 4 hours at 60 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 3mol/L KOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 200 DEG C of Constant Temp. Oven, 2h
After take out, be cooled to room temperature, take out sample, washing and filtering to filtrate is neutrality, and sample then is put into the electricity that temperature is 80 DEG C
Dry and weigh in hot thermostatic drying chamber, in the crucible that sample is put into cleaning, be put into high-temperature atmosphere tube furnace, be passed through gas stream
Measure 99.99% nitrogen for 160mL/min.Tube furnace is raised to 800 DEG C, keeping temperature with 10 DEG C/min speed from room temperature
4h is carbonized, after carbonization terminates, and is taken out the sample in crucible, with watery hydrochloric acid washing and filtering and is dried, obtains carbon fibre material.
Embodiment 6
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 4 hours at 60 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 2mol/L KOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 200 DEG C of Constant Temp. Oven, 2h
After take out, be cooled to room temperature, take out sample, with high-purity water washing and filter, to filtrate pH=7, sample is then put into temperature
To dry and weighing in 80 DEG C of Constant Temp. Ovens, the loss late of bamboo wood material is 39.2%, and bamboo wood material is not changed into fine
Tie up shape.
Embodiment 7
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 4 hours at 60 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 1mol/L KOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 200 DEG C of Constant Temp. Oven, 2h
After take out, be cooled to room temperature, take out sample, with high-purity water washing and filter, to filtrate pH=7, sample is then put into temperature
To dry and weighing in 80 DEG C of Constant Temp. Ovens, the loss late of bamboo wood material is 36.5%, and bamboo wood material is not changed into fine
Tie up shape.
Embodiment 8
Bamboo chopsticks are cleaned up, bamboo scraps shape (long 2cm, wide 0.3cm, thick 0.05cm) is whittled into, is put into Constant Temp. Oven,
Dried 4 hours at 60 DEG C, the bamboo scraps after drying are put into the polytetrafluoroethyllining lining equipped with 3mol/L NaOH reaction dissolvents
In stainless steel high pressure water heating kettle, lid is tightened, water heating kettle is put into temperature is set as in 200 DEG C of Constant Temp. Oven, 2h
After take out, be cooled to room temperature, take out sample, with high-purity water washing and filter, be neutrality to filtrate, sample is then put into temperature
To dry and weighing in 80 DEG C of Constant Temp. Ovens, in the crucible that sample is put into cleaning, high-temperature atmosphere tube furnace is put into,
It is passed through 99.99% nitrogen that gas flow is 140mL/min.Tube furnace is raised to 800 with 10 DEG C/min speed from room temperature
DEG C, keeping temperature 4h is carbonized, after carbonization terminates, and takes out the sample in crucible, with 4mol/L watery hydrochloric acid washing and filtering, and
3h is dried at 70 DEG C, carbon fibre material is obtained.
Embodiment 9
According to the experiment condition in embodiment 1.Only change KOH concentration, its concentration be 1mol/L, 2mol/L, 4mol/L,
5mol/L and 6mol/L.Bamboo fibre after observation experiment, comparative experimental data, it has been found that 1mol/L and 2mol/L is in experiment
Front and rear mass loss rate is 36.5% and 39.2%, although than other concentration KOH solution it is low, but we can from Fig. 1
To be evident that, bamboo wood material is not changed into threadiness, therefore the KOH solution of low concentration can not extract bamboo fibre
Come.And 4mol/L, 5mol/L and 6mol/L can extract the bamboo fibre in bamboo scraps completely, but the mass loss rate after experiment
Reach 47.4%, 48.9% and 54.6%.According to data above it was found that mass loss and the KOH solution of bamboo wood material
Concentration is that the quality loss rate of bamboo wood material under the conditions of height correlation, 1mol/L KOH solutions only has 36.5%, 6mol/L KOH molten
Liquid has reached surprising 54.6%.Therefore, KOH solution concentration is higher, and the mass loss of bamboo wood material is bigger.And 3-5mol/L
KOH solution can not only extract bamboo fibre, and its mass loss is also lower than 6mol/L KOH solution.In view of manufacture bamboo fibre
Efficiency and cost, the treated bamboo wood material of final choice 3-5mol/L KOH solutions is carbonized and carries out physical property table
Levy.
Claims (10)
- The carbon fibre material that 1. discarded bamboo chopsticks are made a kind of use hydrothermal carbonization method, it is characterised in that adopted based on discarded bamboo chopsticks It is prepared from hydrothermal carbonization method, preparation method is as follows:Discarded bamboo chopsticks are cleaned after drying, the polytetrafluoro for filling aqueous slkali is put into Reacted in ethene inner liner stainless steel high pressure water heating kettle, taken out after reaction completely and wash and dry, be then placed on sample logical It is carbonized in the high-temperature atmosphere tube furnace for entering protective gas, then obtains carbon fibre material with the drying of hydrochloric acid washing and filtering.
- 2. carbon fibre material according to claim 1, it is characterised in that;Described carbon fibre material is put in into X-ray to spread out Penetrate on instrument objective table, adjustment operating voltage is 40kV, electric current is 250mA, and sweep speed is 10 °/min, and the θ of scanning range 2 is 10 ° ~ 80 °, it is scanned, occurs the diffraction maximum that a crystal face is (002) at 20 ° or so, (100) crystal face diffraction occur at 44 ° or so Peak, and based on (002) crystal face, the X-ray diffraction intensity from (002) crystal face is set to I (002), from (100) crystal face When X-ray diffraction intensity is set to I (100), 2.5≤[I (002)/I (100)]≤2.9 are met.
- 3. carbon fibre material according to claim 2, it is characterised in that the carbon fibre material carries out SEM shape characteristics Analysis, the length of carbon fiber is up to 20-200 μm, and width is 3-5 μm, and carbon fiber surface is dispersed with substantial amounts of fold.
- 4. carbon fibre material according to claim 3, it is characterised in that the carbon fibre material carries out Raman spectrum point Analysis, Raman shift 1360cm-1The peak at place is designated as D peaks, and corresponding intensity is designated as ID, the cm of Raman shift 1600-1Place for G peaks, it is right The intensity answered is designated as IG, by D peaks and G peak intensity ratio IsD/IGIt is designated as the randomness factor of carbon fibre material, ID/IGValue be 1.0-1.1。
- 5. carbon fibre material according to claim 4, it is characterised in that carbon fibre material is subjected to Fourier infrared spectrum Analysis, carbon fibre material is in 3200-3500cm-1There is a hydroxyl absorption peak in place, in 1610cm-1The peak at place belongs to aromatic rings Vibration peak, 1730cm-1The absworption peak at place belongs to ester, carboxyl or carbonyl vibration peak.
- 6. carbon fibre material according to claim 5, it is characterised in that described aqueous slkali is KOH or NaOH.
- 7. carbon fibre material according to claim 6, it is characterised in that in the carbonisation, heating rate is 6-10 DEG C/min, carburizing temperature is 700-1000 DEG C, and carbonization time is 4-8h.
- 8. carbon fibre material according to claim 7, it is characterised in that the concentration of the aqueous slkali is 3-5mol/L.
- 9. carbon fibre material according to claim 8, it is characterised in that the protective gas is inert gas.
- 10. a kind of any described carbon fibre materials of claim 1-9 can be applied in sorbing material or battery material.
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CN111211329A (en) * | 2020-01-15 | 2020-05-29 | 重庆工商大学 | Water candle cattail-shaped MoS2Carbon nanofiber composite material and preparation method and application thereof |
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CN106676677A (en) * | 2017-02-06 | 2017-05-17 | 信阳师范学院 | Method for preparing hollow carbon fiber from biomass material |
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CN106676677A (en) * | 2017-02-06 | 2017-05-17 | 信阳师范学院 | Method for preparing hollow carbon fiber from biomass material |
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Application publication date: 20170919 |