CN109957962A - A kind of carboxylic carbon nano-tube-polyurethane guide hotting mask and preparation method thereof - Google Patents
A kind of carboxylic carbon nano-tube-polyurethane guide hotting mask and preparation method thereof Download PDFInfo
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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
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Abstract
The present invention relates to the technical fields of light industry, chemical materials, and in particular to a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask and preparation method thereof.The carboxylic carbon nano-tube-polyurethane guide hotting mask preparation method, including the first step, prepare carboxylic carbon nano-tube；Second step prepares carboxylic carbon nano-tube dispersion liquid；Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution；4th step, electrostatic spinning；5th step, ultrasound anchoring decoration carbon nanotube.Due to being the in the mixed solvent that the carboxylic carbon nano-tube after acidification is first dispersed in acetone and dimethylformamide, then polyurethane is added wherein again, prepare carboxylic carbon nano-tube/polyurethane spinning solution, force carbon nanotube that there is good orientation in polyurethane fiber during the spinning process, and carbon nanotube is completely coated by polyurethane after Static Spinning, continuous thermal conducting path is formed inside polyurethane fiber, and then realizes the purpose of low-carbon nano pipe content and high thermal conductivity coefficient.
Description
Technical field
The present invention relates to the technical fields of light industry, chemical materials, and in particular to a kind of carboxylic carbon nano-tube-polyurethane guide
Hotting mask and preparation method thereof.
Background technique
With the fast development of science and technology, electronic device need to have higher processing speed, higher operation frequency and more
Small size, more stringent requirements are proposed for thermal diffusivity of the people to product, and the heat-sinking capability of electronic device just becomes design and system
It has to consider the problems of when making electronic equipment.Because having excellent mechanicalness, flexibility, flexible can be drawn polymer
Stretching property and excellent processing performance, which become, prepares one of miniature electronic radiating element best candidate material.However, pure high score
The sub- usual thermal coefficient of material is lower, so that dissipation from electronic devices is extremely difficult.Therefore, superior high thermal conductivity macromolecule is prepared
Composite material is extremely necessary and very urgent.
Currently, improve high molecular material heating conduction method be generally divided into prepare Intrinsical heat-conducting polymer material and
Prepare two kinds of filled-type high molecular material.Relative to Intrinsical heat-conducting polymer is prepared, it is added in common high molecular material
The preferable Heat Conduction Material of thermal conductivity, such as carbon nanotube make the two uniformly be mixed to prepare filled-type thermally conductive by certain technique
The technique of high molecular material is simpler, is more able to satisfy actual production requirement, is to prepare heat-conductivity polymer composite at present
Main method.But the addition of a large amount of heat fillings is so that the microstructure of polymer is substantially change, to reduce poly-
Close the mechanical performance and processing performance of object.Furthermore, it is desirable to solve heat filling dispersibility, compatibility, boundary in macromolecule matrix
A series of problems, such as face property.In addition, random distribution of the heat filling in macromolecule matrix is usually formed discontinuous thermal conductive network
Network, significantly increases the interface resistance between filler and filler, limits the raising of thermal coefficient to a certain extent.Therefore,
Prepare one that the polymer composite of low heat filling additive amount high thermal conductivity coefficient is still that current research work is faced
Huge challenge.
During exploring novel thermal interfacial material, carbon nanotube is drawn in the excellent properties that thermally conductive aspect is shown
The great attention (thermal coefficient is about 2000W/mK) for having played people theoretically compared with other heat fillings, is being made
There is advantage outstanding in terms of standby heat-conductive composite material.Therefore, the preparation of the polymer composites of carbon nanotubes is by wide
The concern of big research worker is presently considered to be because its light-weight, corrosion resistance and good, working ability is strong, manufacturing cost is low
One of optimal heat sink material.But since carbon nanotube is lacked as inorganic heat filling and high molecular material poor compatibility etc.
It falls into, greatly limits their application.If it can solve itself and this poor problem of high molecular material compatibility, also, few
Additive amount can form thermal conducting path in high molecular material, further increase the capacity of heat transmission of material, will become to have and well answer
With the high-performance heat filling of prospect.
Summary of the invention
It is an object of the present invention in view of the deficiencies of the prior art, provide a kind of carboxylic carbon nano-tube-polyurethane
The preparation method of heat conducting film, carboxylic carbon nano-tube-polyurethane guide hotting mask obtained by the preparation method have low heat filling
The advantages of additive amount and high thermal conductivity coefficient.
The second object of the present invention is in view of the deficiencies of the prior art, to provide a kind of carboxylic carbon nano-tube-polyurethane
Heat conducting film, the carboxylic carbon nano-tube-polyurethane guide hotting mask have the advantages that low heat filling additive amount and high thermal conductivity coefficient.
One of to achieve the goals above, the present invention adopts the following technical scheme:
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask is provided, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.
In above-mentioned technical proposal, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and the substance in container is stood；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.
In above-mentioned technical proposal, in the step 1 acidification, the temperature of the condensing reflux is 60~80 DEG C, described
The time of condensing reflux is 3~3.5h, and the volume ratio of the water being added and the mixed acid is 2~2.5:1, the time of repose
For 22~26h；
In the step 2 deacidification, centrifugal rotational speed is 8000~15000r/min；The centrifugation number is 6~8 times.
In above-mentioned technical proposal, the first step prepares carboxylic carbon nano-tube, in the mixed acid, the concentrated sulfuric acid and dense
The volume ratio of nitric acid is 2~4:1；
The first step prepares carboxylic carbon nano-tube, and the carbon nanotube and the mass volume ratio of the mixed acid are
10~30g/L.
In above-mentioned technical proposal, the first step prepares carboxylic carbon nano-tube, and the diameter of the carbon nanotube is 10
~20nm, the length of the carbon nanotube are 3~15 μm.
In above-mentioned technical proposal, the second step prepares carboxylic carbon nano-tube dispersion liquid, the in the mixed solvent, acetone
Volume ratio with dimethylformamide is 1:1；
The concentration of the carboxylic carbon nano-tube dispersion liquid is 0.5~1.5mg/mL.
In above-mentioned technical proposal, the third step prepares carboxylic carbon nano-tube/polyurethane spinning solution, and the polyurethane exists
Mass concentration in the carboxylic carbon nano-tube/polyurethane spinning solution is 13~15%.
In above-mentioned technical proposal, the 4th step electrostatic spinning, the voltage of Static Spinning is 10~15kV, Static Spinning it is opposite
Humidity is 20~40%, and the reception distance of Static Spinning is 10~15cm, and the speed of injecting of Static Spinning is 0.08~0.15mm/min,
Syringe needle bore is 21~22G.
In above-mentioned technical proposal, in the 5th step ultrasound anchoring decoration carbon nanotube, ultrasonic power is 400~960W,
Ultrasonic time is 20~60min, and supersonic frequency is 18~22kHz.
To achieve the goals above two, the present invention adopts the following technical scheme:
A kind of carboxylic carbon nano-tube-polyurethane guide hotting mask is provided, is by a kind of carboxylic carbon nano-tube-described above
A kind of carboxylic carbon nano-tube-polyurethane guide hotting mask obtained by the preparation method of polyurethane guide hotting mask.
Compared with prior art, beneficial effect is the present invention:
(1) preparation method of a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask provided by the invention, due to be first will be sour
Carboxylic carbon nano-tube after change is dispersed in the in the mixed solvent of acetone and dimethylformamide, and poly- ammonia is then added wherein again
Ester prepares carboxylic carbon nano-tube/polyurethane spinning solution, and middle carbon nanotube and polyurethane directly melt altogether compared with the prior art
It mixes or adds dispersing Nano carbon tubes after first dissolving polyurethane, the carbon nanotube in the present invention is dispersed more uniformly in polyurethane.
(2) preparation method of a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask provided by the invention, present invention obviates
Traditional hot-forming and blending extrusion molding, and carboxylic carbon nano-tube-polyurethane guide is prepared using electrostatic spinning technique
Hotting mask cleverly forces carbon nanotube to generate polarization in electrostatic field, forces carbon to be received during the spinning process using high-voltage electrostatic field
Mitron has good orientation in polyurethane fiber, and carbon nanotube is completely coated by polyurethane after Static Spinning,
Continuous thermal conducting path is formed inside polyurethane fiber, and then realizes the purpose of low-carbon nano pipe content and high thermal conductivity coefficient.
(3) preparation method of a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask provided by the invention, using the side of ultrasound
Carbon nanotube is uniformly anchored on the carboxylic carbon nano-tube/compound polyurethane material film spun, in poly- ammonia by method
Ester fiber surface forms uniform carbon nanotube coating, and using in the carboxyl and polyurethane material of carbon nano tube surface
The formed hydrogen bond of amino, enables the carbon nanotube for being coated on polyurethane fiber surface to be securely fixed in above, for a long time
Ultrasound is not fallen off.Also, it is coated on the carbon nanotube of polyurethane surface and is complemented each other by the carbon nanotube that polyurethane coats, it is interior
Outer double thermal conducting paths, further increase obtained carboxylic carbon nano-tube-polyurethane guide hotting mask thermal coefficient and thermal diffusivity
Energy.
(4) preparation method of a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask provided by the invention has preparation method
Simply, production cost is low, and can be used in the characteristics of being mass produced, and prepared carboxylic carbon nano-tube-polyurethane
Heat conducting film has excellent heating conduction and mechanical property.
(5) a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask provided by the invention, by functional modification carbon nanotube
At modified carbon nano tube surface contains carboxyl functional group, and carboxyl functional group can be with the amino official on polyurethane high molecule chain
Can group forms Hyarogen-bonding, Hyarogen-bonding is for reducing between carbon nanotube and carbon nanotube and carbon nanotube and poly- ammonia
Interface phonon scatters between ester, reduces thermal resistance between interface, and improving thermal conductivity has apparent effect.In addition, the carbon after functionalization
Nanotube can further decrease the difference of the interfacial surface tension of carbon nanotube and polyurethane, so that carbon nanotube is easier to be gathered
Urethane wetting reduces existing gap therebetween, further decreases obtained carboxylic carbon nano-tube-polyurethane guide hotting mask
Interface resistance.
Detailed description of the invention
Fig. 1 is a kind of structural representation of carboxylic carbon nano-tube-polyurethane guide hotting mask obtained by the embodiment of the present invention 1
Figure.Wherein, Carbon nanotube represents carboxylic carbon nano-tube, and TPU fiber represents polyurethane fiber.
Fig. 2 is a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask dissipating when heated obtained by the embodiment of the present invention 1
Hot schematic diagram.Wherein, Carbon nanotube represents carboxylic carbon nano-tube, and TPU fiber represents polyurethane fiber.
Fig. 3 is that the comparison of the carboxylic carbon nano-tube and untreated carbon nanotube prepared in the embodiment of the present invention 1 is infrared
There is carboxyl functional group on spectrogram, the surface that this figure demonstrates obtained carboxylic carbon nano-tube.Wherein, a curve represents carboxyl
The infrared spectrogram of carbon nano tube, b curve represent the infrared spectrogram of untreated carbon nanotube.
Fig. 4 is the comparison of carboxylic carbon nano-tube made from the embodiment of the present invention 1-polyurethane guide hotting mask and pure polyurethane film
Infrared spectrogram, this figure demonstrate carboxylic carbon nano-tube in carboxylic carbon nano-tube produced by the present invention-polyurethane guide hotting mask
There is interaction force between polyurethane.Wherein, the b curve in figure represents carboxylic carbon nano-tube-polyurethane guide hotting mask, and a is bent
Line represents pure polyurethane film.
Fig. 5 is a kind of Thermal Synthetic Analysis spectrum of carboxylic carbon nano-tube-polyurethane guide hotting mask made from the embodiment of the present invention 1
Figure.This figure is in order to prove percentage composition of the carbon nanotube in polyurethane.Wherein, b curve represents obtained carboxylated carbon and receives
Mitron-polyurethane guide hotting mask, a curve represent polyurethane.
Fig. 6 is carboxylic carbon nano-tube made from the embodiment of the present invention 1-polyurethane guide hotting mask SEM and TEM figure.This figure
In order to illustrate distribution of the carbon nanotube on polyurethane film.Wherein, a is the carboxylated carbon nanometer that electrostatic spinning obtains
Pipe/compound polyurethane material film scanning electron microscope (SEM) photograph, b are carboxylic carbon nano-tube-polyurethane guide hotting mask scanning electron microscope (SEM) photograph,
C is carboxylic carbon nano-tube/compound polyurethane material film surface chart that electrostatic spinning obtains, and d is carboxylic carbon nano-tube-
The transmission electron microscope picture of polyurethane guide hotting mask.
Fig. 7 is carboxylic carbon nano-tube made from the embodiment of the present invention 1-polyurethane guide hotting mask at different temperatures thermally conductive
Coefficient summary view.Wherein, a curve represents the thermal coefficient of vertical direction, and b curve represents the thermal coefficient of horizontal direction.
Fig. 8 is that carboxylic carbon nano-tube made from the embodiment of the present invention 1/compound polyurethane material film and carboxylated carbon are received
Mitron-polyurethane guide hotting mask stress strain diagram.This figure will not sacrifice original to prove to be added after carbon nanotube in the present invention
Carry out the flexibility of high molecular material.Wherein, the polyurethane film of a curve in figure represents the carboxylic carbon nano-tube that electrostatic spinning obtains
/ compound polyurethane material film, b curve represent carboxylic carbon nano-tube-polyurethane guide hotting mask.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
Embodiment 1.
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Wherein, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and the substance in container is stood for 24 hours；In the present embodiment, it is condensed back
Temperature be 70 DEG C, time of condensing reflux is 3.2h, and the volume ratio of the water and mixed acid that are added is 2.2:1；In mixed acid,
The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3:1；The mass volume ratio of carbon nanotube and mixed acid is 20g/L；In the present embodiment, carbon
The diameter of nanotube is 15nm, and the length of carbon nanotube is 10 μm；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.This implementation
In example, centrifugal rotational speed 12000r/min；Being centrifuged number is 7 times.
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；In the present embodiment, mix
In bonding solvent, the volume ratio of acetone and dimethylformamide is 1:1；The concentration of carboxylic carbon nano-tube dispersion liquid is 1mg/mL.
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；In the present embodiment, polyurethane is in carboxylic
Mass concentration in base carbon nano tube/polyurethane spinning solution is 14%.
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；In the present embodiment, the voltage of Static Spinning is 12kV, Static Spinning
Relative humidity be 30%, the reception of Static Spinning distance is 13cm, and the speed of injecting of Static Spinning is 0.12mm/min, syringe needle bore
For 21.5G.
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.In the present embodiment, ultrasonic power 700W, ultrasonic time 40min, supersonic frequency 20kHz.
Embodiment 2.
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Wherein, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and standing 22h is carried out to the substance in container；In the present embodiment, it is condensed back
Temperature be 60 DEG C, time of condensing reflux is 3.5h, and the volume ratio of the water and mixed acid that are added is 2:1；It is dense in mixed acid
The volume ratio of sulfuric acid and concentrated nitric acid is 2:1；The mass volume ratio of carbon nanotube and mixed acid is 10g/L；In the present embodiment, carbon is received
The diameter of mitron is 10nm, and the length of carbon nanotube is 3 μm；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.This implementation
In example, centrifugal rotational speed 8000r/min；Being centrifuged number is 6 times.
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；In the present embodiment, mix
In bonding solvent, the volume ratio of acetone and dimethylformamide is 1:1；The concentration of carboxylic carbon nano-tube dispersion liquid is 0.5mg/
mL。
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；In the present embodiment, polyurethane is in carboxylic
Mass concentration in base carbon nano tube/polyurethane spinning solution is 13%.
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；In the present embodiment, the voltage of Static Spinning is 10kV, Static Spinning
Relative humidity be 20%, the reception of Static Spinning distance is 10cm, and the speed of injecting of Static Spinning is 0.08mm/min, syringe needle bore
For 21G.
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.In the present embodiment, ultrasonic power 400W, ultrasonic time 60min, supersonic frequency 18kHz.
Embodiment 3.
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Wherein, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and standing 26h is carried out to the substance in container；In the present embodiment, it is condensed back
Temperature be 80 DEG C, time of condensing reflux is 3h, and the volume ratio of the water and mixed acid that are added is 2.5:1；It is dense in mixed acid
The volume ratio of sulfuric acid and concentrated nitric acid is 4:1；The mass volume ratio of carbon nanotube and mixed acid is 30g/L；In the present embodiment, carbon is received
The diameter of mitron is 20nm, and the length of carbon nanotube is 15 μm；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.This implementation
In example, centrifugal rotational speed 15000r/min；Being centrifuged number is 8 times.
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；In the present embodiment, mix
In bonding solvent, the volume ratio of acetone and dimethylformamide is 1:1；The concentration of carboxylic carbon nano-tube dispersion liquid is 1.5mg/
mL。
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；In the present embodiment, polyurethane is in carboxylic
Mass concentration in base carbon nano tube/polyurethane spinning solution is 15%.
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；In the present embodiment, the voltage of Static Spinning is 15kV, Static Spinning
Relative humidity be 40%, the reception of Static Spinning distance is 15cm, and the speed of injecting of Static Spinning is 0.15mm/min, syringe needle bore
For 22G.
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.In the present embodiment, ultrasonic power 960W, ultrasonic time 60min, supersonic frequency 22kHz.
Embodiment 4.
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Wherein, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and standing 23h is carried out to the substance in container；In the present embodiment, it is condensed back
Temperature be 65 DEG C, time of condensing reflux is 3.1h, and the volume ratio of the water and mixed acid that are added is 2.1:1；In mixed acid,
The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2.5:1；The mass volume ratio of carbon nanotube and mixed acid is 15g/L；In the present embodiment,
The diameter of carbon nanotube is 12nm, and the length of carbon nanotube is 7 μm；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.This implementation
In example, centrifugal rotational speed 10000r/min；Being centrifuged number is 6 times.
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；In the present embodiment, mix
In bonding solvent, the volume ratio of acetone and dimethylformamide is 1:1；The concentration of carboxylic carbon nano-tube dispersion liquid is 0.8mg/
mL。
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；In the present embodiment, polyurethane is in carboxylic
Mass concentration in base carbon nano tube/polyurethane spinning solution is 13.5%.
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；In the present embodiment, the voltage of Static Spinning is 11kV, Static Spinning
Relative humidity be 25%, the reception of Static Spinning distance is 11cm, and the speed of injecting of Static Spinning is 0.1mm/min, syringe needle bore
For 21.5G.
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.In the present embodiment, ultrasonic power 500W, ultrasonic time 30min, supersonic frequency 19kHz.
Embodiment 5.
A kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask, it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
Carboxylic carbon nano-tube is made in nanotube, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Wherein, the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to
After mixed acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, then toward the container
Middle addition water, it is cooling after reflux to be condensed, and standing 25h is carried out to the substance in container；In the present embodiment, it is condensed back
Temperature be 75 DEG C, time of condensing reflux is 3.4h, and the volume ratio of the water and mixed acid that are added is 2.4:1；In mixed acid,
The volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 3.5:1；The mass volume ratio of carbon nanotube and mixed acid is 25g/L；In the present embodiment,
The diameter of carbon nanotube is 18nm, and the length of carbon nanotube is 13 μm；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, so
Precipitating after taking centrifugation afterwards is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.This implementation
In example, centrifugal rotational speed 14000r/min；Being centrifuged number is 7 times.
Second step prepares carboxylic carbon nano-tube dispersion liquid: dispersing third for carboxylic carbon nano-tube made from the first step
The in the mixed solvent of ketone and dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；In the present embodiment, mix
In bonding solvent, the volume ratio of acetone and dimethylformamide is 1:1；The concentration of carboxylic carbon nano-tube dispersion liquid is 1.3mg/
mL。
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube made from step 1 point
Polyurethane is added in dispersion liquid, carboxylic carbon nano-tube/polyurethane spinning solution is made after dissolution；In the present embodiment, polyurethane is in carboxylic
Mass concentration in base carbon nano tube/polyurethane spinning solution is 14.5%.
Electrostatic spinning: 4th step carries out Static Spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution
Silk obtains carboxylic carbon nano-tube/compound polyurethane material film；In the present embodiment, the voltage of Static Spinning is 14kV, Static Spinning
Relative humidity be 35%, the reception of Static Spinning distance is 14cm, and the speed of injecting of Static Spinning is 0.14mm/min, syringe needle bore
For 21G.
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxyl
Carbon nano tube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, and it is poly- to obtain the carboxylic carbon nano-tube-
Urethane heat conducting film.In the present embodiment, ultrasonic power 800W, ultrasonic time 50min, supersonic frequency 21kHz.
Map phenetic analysis:
(1) heat conduction film structure illustrates map analysis:
As shown in Figure 1, carboxylic carbon nano-tube produced by the present invention-polyurethane guide hotting mask structural schematic diagram is depicted,
By Static Spinning carboxylic carbon nano-tube/polyurethane mixed solution, carboxylic carbon nano-tube can be inside polyurethane fiber
Form thermal conducting path, as shown in figure 1 shown in magnifying glass, in addition, in Fig. 6 TEM figure further demonstrate carbon nanotube can be poly-
Thermal conducting path is formed inside urethane, it is multiple in the good carboxylic carbon nano-tube/polyurethane of Static Spinning by ultrasonic anchoring techniques later
Carbon nanotube is anchored on condensation material film.- COOH in carboxylic carbon nano-tube can in urethane structural unit-
- NH- functional group in NHCO- forms hydrogen bond, and then allows carbon nanotube to be firmly anchored on polyurethane fiber cloth and do not fall off.Cause
This, can be formed simultaneously thermal conducting path with outer surface inside polyurethane fiber by the way that a small amount of carbon nanotube is added, and
Strong Hyarogen-bonding is formed, the interaction force between carbon nanotube and polyurethane is increased, and promotes the scattering of phonon,
Further improve obtained carboxylic carbon nano-tube-polyurethane guide hotting mask heat dissipation and heat-transfer capability.Obtained simultaneously
Carboxylic carbon nano-tube-polyurethane guide hotting mask can allow hot steam preferably to distribute raising protection due to porous fibre structure
The ability of electronic component.
In addition, a kind of heat dissipation schematic diagram of carboxylic carbon nano-tube-polyurethane guide hotting mask of Fig. 2 when heated.Due to carboxylic
Carbon nanotube in the connection of base carbon nano tube transverse and longitudinal and polyurethane fiber can accelerate rate of heat dispation, and Fig. 2 is more intuitive
Illustrate the reason of heat conducting film thermal coefficient improves.
(2) infrared spectrum analysis of carboxylic carbon nano-tube:
Infrared spectrum analysis is carried out to carboxylic carbon nano-tube obtained in embodiment 1 and untreated carbon nanotube, such as
Shown in Fig. 3, curve a represents the infrared spectrogram of carboxylic carbon nano-tube, and curve b represents the infrared of untreated carbon nanotube
Spectrogram, as can be known from Fig. 3, compared with untreated carbon nanotube, carboxylic carbon nano-tube of the invention is in 3440cm-1Ground
There is stronger absorption peak in side, which corresponds to the stretching vibration peak of-OH, in 1631cm-1Place has obvious-COOH's
Stretching vibration peak, and the stretching vibration peak of-COOH of untreatment carbon nanotube almost it is impure.As the above analysis, carboxyl
- OH and-the COOH functional group on carbon nano tube surface are more abundant.
(3) carboxylic carbon nano-tube/polyurethane guide hotting mask infrared spectrum analysis:
Pass through the interaction force of infrared spectroscopic study carboxylic carbon nano-tube and polyurethane film.In the spectrum of Fig. 4
In, 3321cm-1It is the stretching vibration peak of N-H key in polyurethane chain, 2937cm at wave number-1It is the flexible vibration of-CH key at wave number
Strong absorption peak belongs to the absorption peak of-H-N-COO-, in addition to this, 1529cm-1 at dynamic peak, 1729cm-1 and 1596cm-1
The bending vibration of N-H key and the absorption peak of C-O are respectively belonging to the peak at 1076cm-1 wave number.When carboxylic carbon nano-tube is spun
When in polyurethane fibre and being anchored on polyurethane fiber surface, 3321cm-1, 2937cm-1, 1729cm-1, 1529cm-1With
1076cm-1The absorption peak at place has been displaced to 3315cm respectively-1, 2935cm-1, 1728cm-1, 1526cm-1And 1072cm-1.Wave number
Offset mean the carbon nanotube after carboxylated and there are interaction forces between polyurethane fiber film, and carbon can be promoted
It is nanometer tube modified to form good thermal conducting path up in polyurethane fiber film surface.
(4) carboxylic carbon nano-tube@polyurethane film and carboxylic carbon nano-tube/polyurethane guide hotting mask SEM and TEM figure:
A is carboxylic carbon nano-tube/compound polyurethane material film scanning electron microscope (SEM) photograph that electrostatic spinning obtains in Fig. 6,
It can be seen from the figure that fiber surface has smooth but has protrusion, illustrate that carboxylic carbon nano-tube, and can be in fibrous inside
Thermal conducting path is formed, figure d carboxylic carbon nano-tube-polyurethane guide hotting mask transmission electron microscope picture further demonstrates the idea.Scheme b
It is anchored the carboxylic carbon nano-tube-polyurethane guide hotting mask surface sweeping electron microscope obtained after carboxylic carbon nano-tube for ultrasound, from figure
In it can be seen that carboxylic carbon nano-tube is uniformly dispersed in fiber surface, can be formed in fiber surface good thermally conductive logical
Road promotes the heat dissipation and the capacity of heat transmission of polyurethane fiber film.Figure c is carboxylic carbon nano-tube/polyurethane that electrostatic spinning obtains
The sectional view of composite material film illustrates that the composite material is layered porous material, and the presence of carbon nanotube promotes heat
Transmitting, cavernous structure can dissipate the hot gas that component generates in wet environment, further protect electronic component.
(5) thermally conductive data test:
For carboxylic carbon nano-tube-polyurethane guide Hot-film measurements obtained in embodiment 1 thermal coefficient, from thermally conductive number
According to can be seen that obtained carboxylic carbon nano-tube/polyurethane guide hotting mask thermal coefficient with anisotropy, horizontal direction is most
Big thermal coefficient can reach 6.01W/ (mK), be 3~4 times of commercially available heat-conducting silicone grease as shown in curve b in Fig. 7；Perpendicular to flat
Face direction thermal coefficient is slightly lower but can also reach 1.70W/ (mK) as shown in curve a in Fig. 7, is higher than commercially available thermally conductive silicone oil
1.5W/(m·K).No matter carboxylic carbon nano-tube/polyurethane guide hotting mask is vertically also horizontally oriented all significant in the capacity of heat transmission
Raising.
(6) stress-strain analysis:
Stress-strain test has been carried out for carboxylic carbon nano-tube/polyurethane guide hotting mask obtained in embodiment 1.From
It can be seen that the addition of carboxylic carbon nano-tube considerably increases the Young's modulus of tunica fibrosa, from original 2.42MPa in Fig. 8
4.36MPa is increased, has increased 114%, it is obvious to illustrate that the addition of carboxylic carbon nano-tube increases tunica fibrosa Young's modulus, breaks
It splits elongation and only only reduces original 12%, with the methods of physical mixed compared to the obvious advantage, not only without changing fiber
Flexibility further improves its Young's modulus.
Finally it should be noted that the above examples are only used to illustrate the technical scheme of the present invention rather than protects to the present invention
The limitation of range, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should be managed
Solution, can with modification or equivalent replacement of the technical solution of the present invention are made, without departing from technical solution of the present invention essence and
Range.
Claims (10)
1. a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask preparation method, it is characterised in that: it the following steps are included:
The first step prepares carboxylic carbon nano-tube: handling carbon nanometer by the mixed acid being formulated by the concentrated sulfuric acid and concentrated nitric acid
It manages and carboxylic carbon nano-tube is made, the structure that there is the carboxylic carbon nano-tube Formulas I to indicate:
Second step, prepare carboxylic carbon nano-tube dispersion liquid: by carboxylic carbon nano-tube made from the first step be scattered in acetone and
The in the mixed solvent of dimethylformamide, stirs evenly, and carboxylic carbon nano-tube dispersion liquid is made；
Third step prepares carboxylic carbon nano-tube/polyurethane spinning solution: toward carboxylic carbon nano-tube dispersion liquid made from step 1
Carboxylic carbon nano-tube/polyurethane spinning solution is made in middle addition polyurethane after dissolution；
Electrostatic spinning: 4th step carries out electrostatic spinning to carboxylic carbon nano-tube made from third step/poly- polyurethane spinning solution and obtains
To carboxylic carbon nano-tube/compound polyurethane material film；
5th step, ultrasound anchoring decoration carbon nanotube: using ultrasonic anchoring techniques, using ultrasonic reaction synthesizer by carboxylated carbon
Nanotube is anchored on carboxylic carbon nano-tube/compound polyurethane material film, obtains the carboxylic carbon nano-tube-polyurethane
Heat conducting film.
2. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In: the first step prepares carboxylic carbon nano-tube, comprising the following steps:
Step 1, acidification: being added carbon nanotube in a reservoir, and configures the mixed acid of the concentrated sulfuric acid and concentrated nitric acid, to be mixed
After acid is cooling, mixed acid is added in the container equipped with carbon nanotube, and is condensed back, is then added into the container
Enter water, it is cooling after reflux to be condensed, and the substance in container is stood；
Step 2, deacidification: the substance after step 1 is stood removes supernatant, takes lower layer's solution to carry out centrifugal treating, then takes
Precipitating after centrifugation is filtered by vacuum, and is washed with water, until it is neutral, obtain carboxylic carbon nano-tube.
3. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 2, feature exist
In: in the step 1 acidification, the temperature of the condensing reflux is 60~80 DEG C, the time of the condensing reflux is 3~
The volume ratio of 3.5h, the water being added and the mixed acid is 2~2.5:1, and the time of repose is 22~26h；
In the step 2 deacidification, centrifugal rotational speed is 8000~15000r/min；The centrifugation number is 6~8 times.
4. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In the carboxylic carbon nano-tube for preparing of: the first step, the mixed acid, the volume ratio of the concentrated sulfuric acid and concentrated nitric acid is 2~4:
1；
The first step prepares carboxylic carbon nano-tube, and the mass volume ratio of the carbon nanotube and the mixed acid is 10~
30g/L。
5. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In: the first step prepares carboxylic carbon nano-tube, and the diameter of the carbon nanotube is 10~20nm, the carbon nanotube
Length is 3~15 μm.
6. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In: the second step prepares carboxylic carbon nano-tube dispersion liquid, the in the mixed solvent, the volume of acetone and dimethylformamide
Than for 1:1；
The concentration of the carboxylic carbon nano-tube dispersion liquid is 0.5~1.5mg/mL.
7. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
Prepare carboxylic carbon nano-tube/polyurethane spinning solution in: the third step, the polyurethane the carboxylic carbon nano-tube/
Mass concentration in polyurethane spinning solution is 13~15%.
8. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In: the 4th step electrostatic spinning, the voltage of Static Spinning are 10~15kV, and the relative humidity of Static Spinning is 20~40%, electrostatic
The reception distance of spinning is 10~15cm, and the speed of injecting of Static Spinning is 0.08~0.15mm/min, and syringe needle bore is 21~22G.
9. a kind of preparation method of carboxylic carbon nano-tube-polyurethane guide hotting mask according to claim 1, feature exist
In: in the 5th step ultrasound anchoring decoration carbon nanotube, ultrasonic power is 400~960W, and ultrasonic time is 20~60min,
Supersonic frequency is 18~22kHz.
10. a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask, it is characterised in that: be by claim 1 to 9 any one institute
A kind of poly- ammonia of carboxylic carbon nano-tube-obtained by a kind of carboxylic carbon nano-tube-polyurethane guide hotting mask preparation method stated
Ester heat conducting film.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112229317A (en) * | 2020-10-09 | 2021-01-15 | 袁涌 | Flexible sensing film with large deformation performance and monitoring function and preparation method thereof |
| CN114751478A (en) * | 2022-04-11 | 2022-07-15 | 扬州大学 | Nanofiber membrane for solar interface evaporation and preparation method and application thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1746343A (en) * | 2005-09-14 | 2006-03-15 | 东华大学 | Carbon nanometer tube composite fibre with high orientation and production thereof |
| CN101487148A (en) * | 2009-02-24 | 2009-07-22 | 东华大学 | Complex fiber with high conductivity, high elasticity and stress sensing property and preparation thereof |
| US20090326128A1 (en) * | 2007-05-08 | 2009-12-31 | Javier Macossay-Torres | Fibers and methods relating thereto |
| CN101724981A (en) * | 2009-11-05 | 2010-06-09 | 南京大学 | Method for preparing multi-wall carbon nano-tube loaded thermoplastic polyurethane film |
| CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
| CN103895293A (en) * | 2014-03-05 | 2014-07-02 | 符思敏 | Nanofiber membrane fabric with modified self-cleaning carbon nano tube and preparation method |
| KR20160139264A (en) * | 2015-05-27 | 2016-12-07 | 국방과학연구소 | 3-dimenstinal nanofiber membrane and Method of manufacturing the same using liquid collector |
| CN106223013A (en) * | 2016-08-11 | 2016-12-14 | 西南交通大学 | A kind of conductive fiber preparation method based on CNT |
| CN106609396A (en) * | 2016-09-30 | 2017-05-03 | 郑州大学 | Elastic electric-conductive nano-fiber yarns and preparation method for same |
-
2019
- 2019-03-14 CN CN201910193604.5A patent/CN109957962B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1746343A (en) * | 2005-09-14 | 2006-03-15 | 东华大学 | Carbon nanometer tube composite fibre with high orientation and production thereof |
| US20090326128A1 (en) * | 2007-05-08 | 2009-12-31 | Javier Macossay-Torres | Fibers and methods relating thereto |
| CN101487148A (en) * | 2009-02-24 | 2009-07-22 | 东华大学 | Complex fiber with high conductivity, high elasticity and stress sensing property and preparation thereof |
| CN101724981A (en) * | 2009-11-05 | 2010-06-09 | 南京大学 | Method for preparing multi-wall carbon nano-tube loaded thermoplastic polyurethane film |
| CN103194858A (en) * | 2013-04-23 | 2013-07-10 | 北京化工大学 | Elastomer composite with high dielectric constant and low dielectric loss and preparation method thereof |
| CN103895293A (en) * | 2014-03-05 | 2014-07-02 | 符思敏 | Nanofiber membrane fabric with modified self-cleaning carbon nano tube and preparation method |
| KR20160139264A (en) * | 2015-05-27 | 2016-12-07 | 국방과학연구소 | 3-dimenstinal nanofiber membrane and Method of manufacturing the same using liquid collector |
| CN106223013A (en) * | 2016-08-11 | 2016-12-14 | 西南交通大学 | A kind of conductive fiber preparation method based on CNT |
| CN106609396A (en) * | 2016-09-30 | 2017-05-03 | 郑州大学 | Elastic electric-conductive nano-fiber yarns and preparation method for same |
Non-Patent Citations (2)
| Title |
|---|
| 朱朦琪等: ""混杂功能化碳纳米管/聚氨酯复合材料的制备及性能"", 《材料研究学报》 * |
| 李清文: "《碳纳米管纤维》", 31 July 2018, 国防工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112229317A (en) * | 2020-10-09 | 2021-01-15 | 袁涌 | Flexible sensing film with large deformation performance and monitoring function and preparation method thereof |
| CN114751478A (en) * | 2022-04-11 | 2022-07-15 | 扬州大学 | Nanofiber membrane for solar interface evaporation and preparation method and application thereof |
| CN114751478B (en) * | 2022-04-11 | 2023-11-21 | 扬州大学 | Nanofiber membrane for solar energy interface evaporation and preparation method and application thereof |
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