CN110055623A - A kind of high conductivity nickel carbon nanofiber flexible electrode material and preparation method thereof - Google Patents
A kind of high conductivity nickel carbon nanofiber flexible electrode material and preparation method thereof Download PDFInfo
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- CN110055623A CN110055623A CN201910387780.2A CN201910387780A CN110055623A CN 110055623 A CN110055623 A CN 110055623A CN 201910387780 A CN201910387780 A CN 201910387780A CN 110055623 A CN110055623 A CN 110055623A
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- 239000002134 carbon nanofiber Substances 0.000 title claims abstract description 74
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000007772 electrode material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 31
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000002121 nanofiber Substances 0.000 claims abstract description 27
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 23
- 238000006722 reduction reaction Methods 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000003647 oxidation Effects 0.000 claims abstract description 21
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 20
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 12
- 229940078494 nickel acetate Drugs 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 235000021419 vinegar Nutrition 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 18
- 229910052799 carbon Inorganic materials 0.000 description 17
- 239000000463 material Substances 0.000 description 9
- 239000004753 textile Substances 0.000 description 9
- 230000001590 oxidative effect Effects 0.000 description 7
- 150000001412 amines Chemical class 0.000 description 6
- 239000012300 argon atmosphere Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 230000009467 reduction Effects 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/58—Fabrics or filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- 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
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Inorganic Fibers (AREA)
Abstract
A kind of high conductivity nickel carbon nanofiber flexible electrode material provided by the present invention and preparation method thereof, this method is based on electrostatic spinning technique, electrostatic spinning precursor liquid is subjected to obtained first spinning nano fibre after spinning by one-step method, first spinning nano fibre in tube furnace through pre-oxidation and carbothermic reduction reaction after obtain high conductivity nickel carbon nanofiber flexible electrode material.Nano nickel particles are evenly distributed in carbon nano-fiber in the composite material, the high conductivity nickel carbon nanofiber flexible electrode material of the structure not only has high intensity, and high specific surface area, fabulous flexibility but also tool impart the high catalytic activity of composite material and excellent electromagnetic wave absorption performance.The technology provides a kind of simple, efficient, low cost preparation high conductivity nickel carbon nanofiber flexible electrode material method.
Description
Technical field
The invention belongs to field of nanocomposite materials, it is related to a kind of preparing high conductivity nickel carbon nanofiber flexible electrode
Material and preparation method thereof.
Background technique
With the continuous development of science and technology and textile industry, intelligent textile occurs gradually over the public visual field.It will give birth to
The new and high technologies such as object science and technology, computer, new energy technology are dissolved into textile, so that textile is had some specific functions, such as
Temperature control, shape memory, Waterproof Breathable, discoloration etc..The occasion that intelligent textile is applied now is concentrated mainly on fashion, amusement, body
It educates, body-building, medical treatment, building, the fields such as military affairs.Intelligent textile can be divided into wearable intelligent textile and non-wearable
Intelligent textile.Wearable intelligent textile such as military protective clothes, sportswear, infant romper etc. is to the micro- of electronic device
The requirement of type and flexibility is higher.The excellent electric conductivity of carbon nano-fiber, preferable catalytic activity, corrosion resistance are good
Flexibility makes carbon nano-fiber become good to electrode material, is repaired by carrying transition metal etc. to carbon nano-fiber
Decorations, and apply it in flexible electrode, show great application potential.
Chinese invention patent application number discloses a kind of super flexible highly conductive Nano carbon fibers peacekeeping for 201510032525.8
The preparation method of nickel carbon composite cellulosic membrane.This method prepares polymer nanofiber using electrostatic spinning technique, obtains after carbonization
Flexible nano carbon-fiber film, then the coaxial composite cellulosic membrane of nickel carbon is obtained by electro-deposition techniques.Preparation process is more in this method
Complexity need to power on chemical nickel plating in nanofiber using electrochemical workstation, and instrument and equipment is more expensive.
Chinese invention patent application number discloses a kind of carbon fiber-transition metal-carbon nanotube for 201710593664.7
The preparation method of flexible nano combination electrode material, this method is using the plant fiber i.e. carbon fiber being carbonized as substrate, in carbon fiber
Surface sputters one layer of transition metal layer, then using the transition metal layer as catalyst, grows not in carbon fiber-transition metal layer
With the CNTs of load capacity.This method need to use magnetron sputtering large scale equipment in the higher cost for preparing material, equipment and target
Higher cost；Simultaneously using inflammable and explosive dangerous goods such as hydrogen, ethylene gas involved in the synthesizing carbon nanotubes, there are certain
Security risk.
It is multiple it is really necessary to provide a kind of flexible silicon carbide/carbon nanofiber easy to operate, at low cost in view of disadvantages described above
The preparation method of condensating fiber membrane material is to solve the above technical problem.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provides a kind of high conductivity nickel carbon nanofiber flexible electrode
Material and preparation method thereof, this method are easy to operate, at low cost.
The present invention is to be achieved through the following technical solutions:
A kind of preparation method of high conductivity nickel carbon nanofiber flexible electrode material, comprising the following steps:
1) nickel acetate, polyacrylonitrile and n,N-Dimethylformamide are mixed, heating stirring obtains electrostatic spinning forerunner
Liquid；The ratio of nickel acetate, polyacrylonitrile and n,N-Dimethylformamide is (1~10mmol): (0.6~1.5g): 10mL；
2) electrostatic spinning precursor liquid is fitted into syringe, syringe is fixed in propulsion device, by electrostatic spinning
Receive to obtain just spinning nano fibre in receiver afterwards；
3) gained is just spun to carbon nano-fiber and carries out carbothermic reduction reaction under air pre-oxidation and argon gas in tube furnace, it is cold
But to obtaining high conductivity nickel carbon nanofiber flexible electrode material after room temperature.
Preferably, in the step 1), 40~80 DEG C of whipping temp, 500~1000r/min of speed of agitator, mixing time
For 10~for 24 hours.
Preferably, in the step 2), electrostatic spinning voltage is 13~18KV, 1~5mm/h of speed of propeller, needle point
To 5~40cm of distance of receiver, needle point to 0~90 ° of receiver angle,
Preferably, in the step 2), receiver is rotating cylinder receiver, flat receiver.
Preferably, in the step 3), the temperature of pre-oxidation is 200~300 DEG C, pre-oxidation heating rate is 1~4 DEG C/
min。
Preferably, in the step 3), carbothermic reduction reaction temperature is 600~1000 DEG C, carbothermic reduction reaction process liter
Warm speed is 3~7 DEG C/min.
The high conductivity nickel carbon nanofiber flexible electrode material of the preparation method preparation, which is characterized in that nickel is received
The diameter of rice grain is in 10~50nm, and nanofiber diameter is in 100~200nm.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention receives the first spinning that electrostatic spinning precursor liquid spinning obtains based on electrostatic spinning technique, through one-step method
Rice fiber, first spinning nano fibre are received in tube furnace by pre-oxidizing and obtaining high conductivity nickel carbon after carbothermic reduction reaction
Rice fiber flexibility electrode material, method are simple, at low cost.In this method of the present invention, high conductivity nickel carbon nanofiber flexible electrical
Pole material forms a high porosity, high-intensitive three-dimensional network knot using carbon nano-fiber as skeleton, between carbon nano-fiber
Structure.Carbon nano-fiber lightweight, high-strength, feature with good conductivity is high conductivity nickel carbon nanofiber flexible electrode material
Basis.Nano nickel particles are evenly distributed in carbon nano-fiber in the composite material, the high conductivity nickel carbon nanometer of the structure
Fiber flexibility electrode material not only have high electric conductivity, high intensity, high specific surface area and fabulous flexibility but also
Tool imparts the high catalytic activity of composite material and excellent electromagnetic wave absorption performance.In addition, high conductivity nickel carbon nanofiber
Flexible electrode material can be repeatedly used when optical electrical is catalyzed.
Nano nickel particles are uniformly distributed in high conductivity nickel carbon nanofiber flexible electrode material prepared by the present invention
In carbon nano-fiber, the diameter of the nano nickel particles of the structure is in 10~50nm, and nanofiber diameter is in 100~200nm.
Detailed description of the invention
Fig. 1 is the X-ray diffraction of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1
(XRD) map；
Fig. 2 is that the scanning electron of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1 is aobvious
Micro mirror (SEM) 30000 × photo；
Fig. 3 is that the scanning electron of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1 is aobvious
Micro mirror (SEM) 100000 × photo；
Fig. 4 is that the transmitted electron of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1 is aobvious
Micro mirror (TEM) photo；
Fig. 5 is the impedance diagram of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
The present invention provides the preparation methods of high conductivity nickel carbon nanofiber flexible electrode material, including with:
1) by nickel acetate (C4H6NiO4), polyacrylonitrile (PAN) and n,N-Dimethylformamide (DMF) mixing, heating stirs
It mixes, obtains electrostatic spinning precursor liquid；
2) electrostatic spinning precursor liquid is fitted into syringe, is fixed in propulsion device through syringe, propeller is set
Sample introduction speed, the distance and angle of setting electrostatic spinning voltage, adjustment needle point to receiver, after spinning after a period of time
To first spinning nano fibre；
3) spinning nano fibre at the beginning of gained is carried out to carbothermic reduction reaction under air pre-oxidation and argon gas in tube furnace, it is cooling
High conductivity nickel carbon nanofiber flexible electrode material is obtained after to room temperature；
Nickel acetate (C in the step 1)4H6NiO4): n,N-Dimethylformamide (DMF)=(1~10mmol): 10mL,
Polyacrylonitrile (PAN): n,N-Dimethylformamide (DMF)=(0.6~1.5g): 10mL, 40~80 DEG C of whipping temp, stirring turns
500~1000r/min of speed, mixing time be 10~for 24 hours.
Electrostatic spinning voltage is 13~18KV, 1~5mm/h of speed of propeller, needle point to receiver in the step 2)
5~40cm of distance, for needle point to 0~90 ° of receiver angle, 100~300nm of first spinning nano fibre diameter, receiver is rotation
Formula cylinder receiver, flat receiver.
The temperature pre-oxidized in the step 3) is 200~300 DEG C, and pre-oxidation heating rate is 1~4 DEG C/min, carbon heat
Reduction reaction temperature is 600~1000 DEG C, and carbothermic reduction reaction process heating rate is 3~7 DEG C/min.
Nano nickel particles are uniformly distributed in high conductivity nickel carbon nanofiber flexible electrode material prepared by the present invention
In carbon nano-fiber, the diameter of the nano nickel particles of the structure is in 10~50nm, and nanofiber diameter is in 100~300nm.
Embodiment 1:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 1.0g that weigh 2mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 60 DEG C, speed of agitator 800r/min, and mixing time obtains electrostatic spinning after being 10h
Precursor liquid；
Step 2: it is 3mm/h, spinning voltage 15KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 18cm to receiver distance, the angle of needle point and receiver is 45 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is
Rotating cylinder receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
260 DEG C, heating rate is 2 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 600 DEG C, and heating rate is 5 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
10nm, carbon nanocoils diameter~150nm.
Embodiment 2:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 0.6g that weigh 1mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 40 DEG C, speed of agitator 500r/min, and mixing time obtains electrostatic spinning after being 10h
Precursor liquid；
Step 2: it is 1mm/h, spinning voltage 13KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 5cm to receiver distance, the angle of needle point and receiver is 90 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is rotation
Rotatable cylinder receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
200 DEG C, heating rate is 1 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 600 DEG C, and heating rate is 3 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
20nm, carbon nanocoils diameter~170nm.
Embodiment 3:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 1.5g that weigh 10mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 80 DEG C, speed of agitator 1000r/min, and mixing time is to obtain electrostatic spinning afterwards for 24 hours
Precursor liquid；
Step 2: it is 5mm/h, spinning voltage 18KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 40cm to receiver distance, the angle of needle point and receiver is 0 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is rotation
Rotatable cylinder receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
300 DEG C, heating rate is 4 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 1000 DEG C, and heating rate is 7 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
20nm, carbon nanocoils diameter~200nm.
Embodiment 4:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 0.8g that weigh 4mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 60 DEG C, speed of agitator 600r/min, and mixing time obtains electrostatic spinning after being 15h
Precursor liquid；
Step 2: it is 4mm/h, spinning voltage 16KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 30cm to receiver distance, the angle of needle point and receiver is 30 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is
Flat receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
240 DEG C, heating rate is 2 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 700 DEG C, and heating rate is 5 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
15nm, carbon nanocoils diameter~130nm.
Embodiment 5:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 1.2g that weigh 6mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 60 DEG C, speed of agitator 600r/min, and mixing time obtains electrostatic spinning after being 18h
Precursor liquid；
Step 2: it is 3mm/h, spinning voltage 14KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 25cm to receiver distance, the angle of needle point and receiver is 60 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is
Flat receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
260 DEG C, heating rate is 3 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 600 DEG C, and heating rate is 4 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
13nm, carbon nanocoils diameter~140nm.
Embodiment 6:
Step 1: the polyacrylonitrile (PAN) of the nickel acetate and 1.3g that weigh 8mmol is dissolved in the N of 10mL, N- dimethyl formyl
In amine (DMF), heating stirring, temperature is 80 DEG C, speed of agitator 1000r/min, and mixing time obtains electrostatic spinning after being 20h
Precursor liquid；
Step 2: it is 4mm/h, spinning voltage 17KV, needle point that spinning precursor liquid, which is fitted into setting fltting speed in propeller,
It is 30cm to receiver distance, the angle of needle point and receiver is 60 °, and just spinning nano fibre is obtained after spinning 5h；Receiver is
Flat receiver；
Step 3: the first carbon nano-fiber that spins being put into tube furnace pre-oxidation treatment under air conditions, Pre oxidation is
280 DEG C, heating rate is 2 DEG C/min, preoxidation time 2h；Wait which carbon thermal reduction is carried out after the completion of pre-oxidizing under an argon atmosphere
Processing, carbothermic reduction reaction temperature are 800 DEG C, and heating rate is 5 DEG C/min, up to high conductivity nickel carbon after being cooled to room temperature
Nanofiber flexible electrode material.
Nano nickel particles diameter in high conductivity nickel carbon nanofiber flexible electrode material obtained by the present embodiment~
20nm, carbon nanocoils diameter~180nm.
Comparative example
According to the method for embodiment 1, nickel acetate is only not added, prepares carbon nano-fiber, as a comparison material.
Fig. 1 is the X-ray diffraction of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1
(XRD) map, it can be seen from the figure that the object of products therefrom be mutually carbon and nickel and nickel content it is higher, crystallinity is preferable.
Fig. 2 is that the scanning electron of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1 is aobvious
Micro mirror (SEM) 30000 × photo, Fig. 3 are high conductivity nickel carbon nanofiber flexible electrode materials prepared by the embodiment of the present invention 1
Scanning electron microscope (SEM) 100000 × photo of material, it can be concluded that the diameter and nickel of carbon nano-fiber from two width figures
The size of nano particle, wherein the diameter of carbon nano-fiber is about 500nm, and the diameter of nano nickel particles is about 40nm；
Fig. 4 is that the transmitted electron of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1 is aobvious
Micro mirror (TEM) photo, as can be seen from the figure particle is also to be uniformly distributed in fibrous inside, and the diameter of nickel particle is about
40nm；
Fig. 5 is the impedance diagram of high conductivity nickel carbon nanofiber flexible electrode material prepared by the embodiment of the present invention 1, from
It can be seen that the pure carbon nano-fiber materials prepared compared to comparative example, the embodiment of the present invention 1 are prepared highly conductive in impedance diagram
Property nickel carbon nanofiber flexible electrode material impedance be substantially better than prepared pure carbon nano-fiber materials.
Flexible silicon carbide/carbon nanofiber composite fiber membrane material prepared by the present invention at least has following advantages:
In this method, high conductivity nickel carbon nanofiber flexible electrode material is using carbon nano-fiber as skeleton, between carbon nano-fiber
Form a high porosity, high-intensitive three-dimensional net structure.Carbon nano-fiber lightweight, high-strength, feature with good conductivity is
The basis of high conductivity nickel carbon nanofiber flexible electrode material.Nano nickel particles are evenly distributed in carbon in the composite material
In nanofiber, the high conductivity nickel carbon nanofiber flexible electrode material of the structure not only has high electric conductivity, and high is strong
Degree, high specific surface area and fabulous flexibility but also tool impart the high catalytic activity of composite material and excellent electromagnetic wave
Absorbent properties.In addition, high conductivity nickel carbon nanofiber flexible electrode material can be repeatedly used when optical electrical is catalyzed.This
Invention provides a kind of with the high conductivity nickel carbon nanofiber flexible electrode material of good optical electrical catalytic performance and its letter
Single, low cost preparation process.
Claims (7)
1. a kind of preparation method of high conductivity nickel carbon nanofiber flexible electrode material, which is characterized in that including following step
It is rapid:
1) nickel acetate, polyacrylonitrile and n,N-Dimethylformamide are mixed, heating stirring obtains electrostatic spinning precursor liquid；Vinegar
The ratio of sour nickel, polyacrylonitrile and n,N-Dimethylformamide is (1~10mmol): (0.6~1.5g): 10mL；
2) electrostatic spinning precursor liquid is fitted into syringe, syringe is fixed in propulsion device, after electrostatic spinning
Receiver receives to obtain just spinning nano fibre；
3) gained is just spun to carbon nano-fiber and carries out carbothermic reduction reaction under air pre-oxidation and argon gas in tube furnace, be cooled to
High conductivity nickel carbon nanofiber flexible electrode material is obtained after room temperature.
2. the preparation method of high conductivity nickel carbon nanofiber flexible electrode material according to claim 1, feature exist
In, in the step 1), 40~80 DEG C of whipping temp, 500~1000r/min of speed of agitator, mixing time be 10~for 24 hours.
3. the preparation method of high conductivity nickel carbon nanofiber flexible electrode material according to claim 1, feature exist
In, in the step 2), electrostatic spinning voltage be 13~18KV, 1~5mm/h of speed of propeller, needle point to receiver away from
From 5~40cm, needle point is to 0~90 ° of receiver angle.
4. the preparation method of high conductivity nickel carbon nanofiber flexible electrode material according to claim 1, feature exist
In in the step 2), receiver is rotating cylinder receiver, flat receiver.
5. the preparation method of high conductivity nickel carbon nanofiber flexible electrode material according to claim 1, feature exist
In in the step 3), the temperature of pre-oxidation is 200~300 DEG C, and pre-oxidation heating rate is 1~4 DEG C/min.
6. the preparation method of high conductivity nickel carbon nanofiber flexible electrode material according to claim 1, feature exist
In in the step 3), carbothermic reduction reaction temperature is 600~1000 DEG C, and carbothermic reduction reaction process heating rate is 3~7
℃/min。
7. the high conductivity nickel carbon nanofiber of the preparation of preparation method described according to claim 1~any one of 6 is flexible
Electrode material, which is characterized in that the diameter of nano nickel particles is in 10~50nm, and nanofiber diameter is in 100~200nm.
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| CN116121909A (en) * | 2022-09-09 | 2023-05-16 | 河北光兴半导体技术有限公司 | Nickel carbon nanofiber preparation method and nickel carbon nanofiber |
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