CN115851242A - Aramid fiber carbon nano dispersion liquid and preparation method thereof - Google Patents
Aramid fiber carbon nano dispersion liquid and preparation method thereof Download PDFInfo
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- CN115851242A CN115851242A CN202211411660.XA CN202211411660A CN115851242A CN 115851242 A CN115851242 A CN 115851242A CN 202211411660 A CN202211411660 A CN 202211411660A CN 115851242 A CN115851242 A CN 115851242A
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Abstract
The invention discloses an aramid fiber carbon nano dispersion liquid and a preparation method thereof, aiming at solving the defect that a graphene material cannot be uniformly dispersed when the existing graphene and carbon nano tube are compounded, so that the prepared composite material has the mechanical property and the heat conductivity.
Description
Technical Field
The invention relates to an aramid fiber carbon nano dispersion liquid and a preparation method thereof, in particular to an aramid fiber modified carbon nano material dispersion liquid and a preparation method thereof, belonging to the field of new nano materials.
Background
In the thermal efficiency management technology of electronic components, carbon materials are often used as highly thermally conductive materials, such as Graphene Oxide (GO) and Carbon Nanotubes (CNT), due to their advantages of light weight, corrosion resistance, good mechanical properties, excellent thermal conductivity, small thermal expansion coefficient, and the like. The Graphene Oxide (GO) is used as a precursor material for synthesizing and preparing graphene, and the surface of the Graphene Oxide (GO) is provided with a large number of hydrophilic groups (-COOH, -OH and the like), so that the graphene oxide can stably exist in most solvents and is not agglomerated, but compared with graphene, the introduction of oxygen-containing groups destroys the structural integrity of the graphene oxide to a certain extent, and the doping points also serve as positions for scattering phonons and electrons, so that the electric conduction and heat conduction performances of the graphene oxide are greatly reduced, and the effective exertion of the thermoelectric performance is limited. The Carbon Nanotube (CNT) can be regarded as formed by curling graphene or a graphene sheet, two ends of the carbon nanotube are covered by hemispherical large fullerene molecules, the carbon nanotube can be divided into a multi-wall carbon nanotube, a double-wall carbon nanotube and a single-wall carbon nanotube according to different layers of the graphene forming the CNT curl, the Carbon Nanotube (CNT) has a main heat conduction mode of lattice vibration phonon heat conduction and has extremely high heat conductivity, wherein the heat conduction coefficient of the single-wall carbon nanotube can reach 3900W/(m.K), and the heat conduction coefficient of the multi-wall carbon nanotube is 3500W/(m.K).
In the prior art, a pure carbon composite film can be obtained by compounding a graphene film and carbon nanotubes, wherein the carbon nanotubes can make up for the crystal boundary defect of graphene, and fully exert the advantages of the graphene film and the carbon nanotubes, so that the mechanical property and the thermal conductivity of the film are improved. For example: in the invention patent with publication number CN103725263A, graphene and carbon nanotubes are stirred, ultrasonically dispersed and fully mixed uniformly, the graphene and the carbon nanotubes are fully reacted under hydrothermal or solvothermal conditions, and after the reaction is finished and the solvent is removed, the graphene-carbon nanotube composite material with the entangled network structure can be obtained.
However, the comprehensive performance of the GO/CNT composite film added with the CNT in the prior art does not reach an ideal value, and the mechanical property and the heat resistance can not be simultaneously considered. The addition of CNTs does not significantly improve the vertical-plane thermal conductivity of graphene, because CNTs have poor dispersibility in graphene matrix and the ability to link CNTs to graphene sheets is still poor. For graphene materials, the two-dimensional structure and the huge specific surface area of the graphene materials make the graphene materials difficult to disperse and easy to agglomerate, and the agglomeration is irreversible, so that the heat conduction performance of the graphene powder is greatly influenced; the carbon nanotubes have a high length-diameter ratio and a large surface area, so that a large van der waals attraction force exists between the tubes, the tubes are hardly dissolved, and are mutually wound and crosslinked, and strong agglomeration and entanglement phenomena occur, so that in order to effectively improve the comprehensive performance of the carbon nanotubes and graphene composite materials, the dispersion performance of the graphene materials in the composite materials is inevitably required to be improved.
Disclosure of Invention
The invention aims to provide an aramid fiber carbon nano dispersion liquid and a preparation method thereof, aiming at solving the defect that a graphene material cannot be uniformly dispersed when the existing graphene and carbon nano tube are compounded, so that the prepared composite material has the mechanical property and the heat conductivity, and the interaction between the graphene and the carbon nano tube is improved through the introduction of aramid fiber nano fibers, so that the prepared composite material has the effects of excellent mechanical property and high heat conductivity coefficient.
The invention is realized by the following technical scheme: a method for preparing an aramid carbon nanodispersion solution, comprising the steps of:
(1) Mixing aramid fiber and KOH with dimethyl sulfoxide according to the mass ratio of 1: 1-1: 2, stirring to form an ANF/DMSO solution, adding water into the ANF/DMSO solution according to the volume ratio of 1: 1-4: 1 of the water to the ANF/DMSO solution, and stirring to obtain the ANF/DMSO/H 2 Carrying out suction filtration, washing and homogenization on the O solution to prepare an aramid nanofiber dispersion liquid;
(2) Mixing and dispersing 0.005-0.05 part of carbon nanotube powder, 0.005-0.1 part of dispersing agent, 0.005-0.1 part of stabilizing agent and 1 part of water according to parts by weight to prepare a carbon nanotube dispersion liquid, and adding the aramid nano-fiber dispersion liquid obtained in the step (1) into the carbon nanotube dispersion liquid to prepare a modified carbon nanotube dispersion liquid;
(3) Adding graphene oxide into water, controlling the mass concentration of the graphene oxide to be 0.005-1%, stirring to prepare a graphene dispersion liquid, and adding the modified carbon nano tube dispersion liquid obtained in the step (2) into the graphene dispersion liquid to obtain the aramid carbon nano dispersion liquid.
In the step (1), the size length of the aramid fiber is 1 to 13 μm.
In the step (1), the mass ratio of the water added into the ANF/DMSO solution to the solvent in the solution is 1: 1-1: 50.
In the step (2), the length of the carbon nanotube powder is more than 5 um.
In the step (2), one or more compounds selected from the group consisting of compounds of the following formula (1), TNRDIS, disponer 983, FA 196, FX 9086, sodium glycocholate and derivatives thereof, sodium glycodeoxycholate and derivatives thereof, sodium chenodeoxycholate and derivatives thereof, sodium taurocholate and derivatives thereof, sodium deoxycholate and derivatives thereof, polyvinylpyrrolidone and derivatives thereof, polyvinyl caprolactam and derivatives thereof, polyvinyl acetamide and derivatives thereof, and sodium dodecylbenzenesulfonate,
wherein R is 1 is-OH, -ONa, -NH 3 C 2 O 2 Na、-NHCH 2 COOH、-N 2 H 8 C 4 SO 4 Na or-NH 5 C 2 SO 3 Na，R 2 is-H, -OH, halogen, -OCH 3 、-OCH 2 CH 3 Or an ester group having 2 to 8 carbon atoms.
In the step (2), the stabilizer is selected from one or more of a polymer stabilizer DNA/RNA, cellulose and derivatives thereof, and sodium carboxymethyl cellulose.
In the step (2), the aramid nano-fiber aqueous dispersion and the carbon nano-tube dispersion are mixed according to the volume ratio of 1: 1-1: 2.
In the step (3), the modified carbon nanotube dispersion liquid and the graphene dispersion liquid are mixed according to the volume ratio of 2.5: 50-50: 100.
The invention also provides the aramid fiber carbon nano dispersion liquid prepared by the method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The invention provides a mixed dispersion liquid of modified CNT and GO, which can be used for preparing a film product with high heat conductivity and excellent mechanical properties, can be used for the surface of an electronic component and shows an excellent heat dissipation effect, and therefore, has a good application prospect in the existing high-power-density device and microelectronic integrated assembly equipment.
(2) According to the method, the aramid nano-fiber is introduced into the system in the mode of the aramid nano-fiber water dispersion liquid, so that a strong pi-pi interaction can exist between the aramid nano-fiber and GO and CNT, and a longitudinal bridged reinforced network can be formed by further connecting and bridging in a composite membrane material prepared by the aramid nano-fiber water dispersion liquid, so that the problems of poor dispersity of the CNT in GO and poor mechanical properties of a membrane are solved better, and the composite membrane material with high heat conductivity coefficient is prepared.
(3) According to the invention, the aramid nano-fiber water dispersion liquid and the carbon nanotube dispersion liquid are mixed to prepare the modified carbon nanotube, the whole modification system takes water as a solvent, and similarly, the graphene oxide dispersion liquid also takes water as a solvent, so that the raw materials are nontoxic and easy to obtain, and the cost is lower.
Drawings
FIG. 1 is a cross-sectional profile of GO/CNT/ANF film in example 4 (left: 10 μm, right: 5 μm).
FIG. 2 is a cross-sectional profile of GO/CNT film of comparative example 2 (left: 10 μm, right: 5 μm).
FIG. 3 is a cross-sectional profile of the ANF/CNT film of comparative example 3 (left: 10 μm, right: 5 μm).
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
adding 1g of aramid fiber (PPTA) fiber (1 to 13 mu m) and 1.5g of KOH into 500ml of dimethyl sulfoxide, adding 20ml of deionized water, and magnetically stirring for 4 hours to form an ANF/DMSO solution; and adding deionized water into the ANF/DMSO solution according to the volume ratio of the deionized water to the ANF/DMSO solution of 4: 1, magnetically stirring for 1h, washing with the deionized water for multiple times under the assistance of vacuum filtration to remove redundant KOH and DMSO, and uniformly dispersing with a homogenizer at the rotating speed of 20000rpm to obtain the aramid nanofiber dispersion liquid.
Adding 0.5g of carbon nanotube powder (more than 5 mu m) into 100ml of deionized water, adding 0.25g of compound (2), 0.25g of sodium deoxycholate, 0.25g of DNA0.25g of cellulose, mixing, and dispersing by ball milling (or using ultrasonic, three-roll milling, dyno-mill grinding, stirring, extruding and other methods to replace ball milling to achieve good dispersion effect) to obtain the carbon nanotube dispersion liquid.
And mixing the aramid nano-fiber dispersion liquid with the carbon nano-tube dispersion liquid with the same volume, and uniformly dispersing by using a homogenizer at the rotating speed of 10000rpm to prepare the modified carbon nano-tube dispersion liquid.
Adding graphene oxide into deionized water, controlling the mass concentration of the graphene oxide to be 0.005%, magnetically stirring for 2 hours to prepare a graphene dispersion liquid, mixing the modified carbon nanotube dispersion liquid and the graphene dispersion liquid according to the volume ratio of 50% to 50%, and magnetically stirring for 4 hours to prepare the homogeneously dispersed aramid fiber carbon nano dispersion liquid.
Example 2:
adding 1g of aramid fiber (PPTA) fiber (1 to 13 mu m) and 1.5g of KOH into 500ml of dimethyl sulfoxide, adding 100ml of deionized water, and magnetically stirring for 6 hours to form an ANF/DMSO solution; and adding deionized water into the ANF/DMSO solution according to the volume ratio of the deionized water to the ANF/DMSO solution of 1: 1, magnetically stirring for 2 hours, washing with the deionized water for multiple times under the assistance of vacuum filtration to remove redundant KOH and DMSO, and uniformly dispersing with a homogenizer at the rotating speed of 20000rpm to obtain the aramid nanofiber dispersion liquid.
Adding 2.0g of carbon nanotube powder (more than 5 mu m) into 100ml of deionized water, adding 0.5g of compound (3), 0.5g of polyvinylpyrrolidone, 0.5g of DNA0.5g and 0.5g of cellulose, mixing, and performing ball milling dispersion to obtain the carbon nanotube dispersion liquid.
And mixing the aramid nano-fiber dispersion liquid with the carbon nano-tube dispersion liquid with the same volume, and uniformly dispersing by using a homogenizer at the rotating speed of 10000rpm to prepare the modified carbon nano-tube dispersion liquid.
Adding graphene oxide into deionized water, controlling the mass concentration of the graphene oxide to be 0.008%, magnetically stirring for 3 hours to prepare a graphene dispersion liquid, mixing the modified carbon nanotube dispersion liquid and the graphene dispersion liquid according to the volume ratio of 50% to 50%, and magnetically stirring for 4 hours to prepare the uniformly dispersed aramid fiber carbon nano dispersion liquid.
Example 3:
adding 1g of aramid fiber (PPTA) fiber (1 to 13 mu m) and 1.5g of KOH into 500ml of dimethyl sulfoxide, adding 20ml of deionized water, and magnetically stirring for 4 hours to form an ANF/DMSO solution; and adding 50ml of deionized water into the ANF/DMSO solution according to the volume ratio of the deionized water to the ANF/DMSO solution of 4: 1, magnetically stirring for 1h, washing with deionized water for many times under the assistance of vacuum filtration to remove redundant KOH and DMSO, and uniformly dispersing at 20000rpm by using a homogenizer to obtain the aramid nano-fiber dispersion liquid.
Adding 0.5g of carbon nanotube powder (more than 5 mu m) into 100ml of deionized water, adding 0.25g of compound (2), 0.25g of sodium deoxycholate, 0.25g of DNA0.25g and 0.25g of cellulose, mixing, and performing ball milling dispersion to obtain the carbon nanotube dispersion liquid.
Mixing the aramid nano-fiber dispersion liquid with 2 times of volume of carbon nano-tube dispersion liquid, and uniformly dispersing by using a homogenizer at the rotating speed of 15000rpm to prepare the modified carbon nano-tube dispersion liquid.
Adding graphene oxide into deionized water, controlling the mass concentration of the graphene oxide to be 0.05%, magnetically stirring for 2 hours to prepare a graphene dispersion liquid, mixing the modified carbon nanotube dispersion liquid and the graphene dispersion liquid according to the volume ratio of 15% to 85%, and magnetically stirring for 4 hours to prepare the homogeneously dispersed aramid fiber carbon nano dispersion liquid.
Example 4: GO/CNT/ANF films
And (3) carrying out vacuum filtration on the aramid carbon nano dispersion liquid obtained in the embodiment 1, and drying in a 70 ℃ oven to form a film, thus obtaining the GO/CNT/ANF film.
Comparative example 1: GO/CNT/ANF films
GO/CNT/ANF films were prepared in the same manner as in examples 1 and 4, except that: mixing the aramid nano-fiber dispersion liquid and the carbon nano-tube dispersion liquid according to a volume ratio of 15% to 85%, and mixing the modified carbon nano-tube dispersion liquid and the graphene dispersion liquid according to a volume ratio of 25% to 75%.
Comparative example 2: GO/CNT thin films
A carbon nanotube dispersion and a graphene dispersion were prepared in the same manner as in example 1.
And preparing and mixing the carbon nano tube dispersion liquid and the graphene dispersion liquid according to the mass ratio of 15% to 85%, and stirring for 4 hours by magnetic force to obtain the GO/CNT dispersion liquid with homogeneous dispersion. And (3) carrying out vacuum filtration on the prepared solution, and drying in a 70 ℃ oven to form a film, thus obtaining the GO/CNT film.
Comparative example 3: ANF/CNT film
A carbon nanotube dispersion was prepared in the same manner as in example 1, and an aramid nanofiber aqueous dispersion was prepared in the same manner as in example 2.
And mixing the aramid nano-fiber water dispersion liquid with the carbon nano-tube dispersion liquid with the same volume, and uniformly dispersing by using a homogenizer at the rotating speed of 10000rpm to obtain the CNT/ANF dispersion solution. And (3) carrying out vacuum filtration on the prepared solution, and drying in a 70 ℃ oven to form a film, thus obtaining the ANF/CNT film.
The GO/CNT/ANF films prepared in the above example 4 and the comparative example 1 are respectively immersed in 100ml of L-ascorbic acid solution of 25mg/ml, reduced in a water bath at 80 ℃ for 30min, taken out, washed with deionized water for several times, and then naturally dried. And then carrying out hot-pressing reduction treatment on the film, setting the temperature of an upper plate and a lower plate of a double-flat-plate hot press to be 200 ℃, preheating, sequentially coating the front surface and the back surface of the film sample by using transparent PI sheets, marking the film sample by name, clamping the film sample in a steel plate, sending the film sample into the hot press, setting the pressure to be 10MPa, and taking out the sample after 15min to obtain a sample A and a comparative sample I.
And (3) respectively carrying out hot-pressing reduction treatment on the GO/CNT film and the ANF/CNT film prepared in the comparative examples 2 and 3, setting the temperatures of an upper plate and a lower plate of a double-flat-plate hot press to be 200 ℃, preheating, then sequentially coating the front and the back of the film sample with transparent PI sheets, making a name mark, clamping the film sample in a steel plate, sending the film sample into the hot press, setting the pressure to be 10MPa, and taking out the sample after 15min to obtain a comparative sample II and a comparative sample III.
The test is carried out by taking the sample A, the comparative sample I, the comparative sample II and the comparative sample III as follows:
(1) Film topography testing
Observations were made with a field emission scanning electron microscope (FE-SEM) (Inspect-F, FEI, finland) at an accelerated voltage of 15kV, and the results are shown in FIG. 1 (sample A), FIG. 2 (comparative sample II) and FIG. 3 (comparative sample III).
Among these, the thin film material shown in fig. 1 has a good layered structure, where rGO flakes are parallel to the film plane, and ANFs and CNTs are present between the rGO flakes, forming a good network structure. The cross-sectional morphology of the GO film shown in fig. 2 is a stacked layered structure, partial gaps exist between graphene oxide layers, carbon nanotubes are loaded on the surface of graphene oxide, the carbon nanotubes form a connected network structure between graphene layers, air pores between graphene layers are effectively filled, but the filled network does not form a dense connection. The SWCNT and ANF tightly interwoven ANF/CNT network shown in fig. 3 can distribute stress evenly over the frame, improving mechanical properties, but lacking a support structure for the lamellae.
(2) Thermal conductivity test
The thermal diffusivity, alpha, of the film was measured with LFA 467. The specific heat capacity of the sample Cp is measured by DSC, and the density ρ of the sample is measured by archimedes' principle as the density of the film: the weight m1 of the sample in the air is first weighed, then the sample is put into an ethanol solution, and the weight m2 of the sample in the ethanol solution is weighed. The measurement environment is: the ethanol density was 0.79 g/cm3 at 25 ℃. Can be calculated by the formula:
film thermal conductivity λ = α × ρ × Cp.
(3) Mechanical Property test
The mechanical properties of the film are tested by adopting an American INSTRON universal material testing machine, and each group of samples are tested for three times to obtain an average value.
The performance parameters of the test are shown in table 1.
TABLE 1
From the above table 1, it can be seen that the composite heat conductive film with low conductivity and high tensile strength can be prepared by the method of the present invention, and the specific performance index system required by the heat dissipation component of the electronic device is satisfied. Comparative example 1 although a film having a density and a thermal conductivity equivalent to each other can be prepared by changing the mixing volume ratio of the dispersion, the mechanical properties are significantly reduced and the electrical conductivity is increased, which may be caused by the deterioration of the dispersion properties of the aramid fiber in the graphene. Comparative example 2 is a GO/CNT film preparation process, and due to the introduction of graphene material, the thermal conductivity of the GO/CNT film can reach 48.4939W/m × k, but the GO/CNT film has poor mechanical properties and high electrical conductivity. Comparative example 3 is a preparation process of an ANF/CNT film, and due to the introduction of aramid fibers, the mechanical properties of the film are enhanced, and at the same time, the conductivity is obviously increased.
In conclusion, the invention actually provides the GO/CNT/ANF dispersion liquid for preparing the film with the specific performance index system, and the heat conductivity coefficient and the tensile strength of the prepared filmAnd the conductivity can meet a specific index range, namely: thermal conductivity at 25 ℃:4.5 to 4.8W/m x k; density: 1.2 to 1.3 g/cm 3 (ii) a Tensile strength: 60 to 65 MPa; conductivity: 11 to 12.5S/cm. The films of comparative examples 1 to 3 are not suitable for use in heat dissipation parts of electronic devices because the index properties do not satisfy the index system.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (9)
1. A method for preparing an aramid carbon nano dispersion liquid is characterized by comprising the following steps: the method comprises the following steps:
(1) Mixing aramid fiber and KOH with dimethyl sulfoxide according to the mass ratio of 1: 1-1: 2, stirring to form an ANF/DMSO solution, adding water into the ANF/DMSO solution according to the volume ratio of 1: 1-4: 1 of the water to the ANF/DMSO solution, and stirring to obtain the ANF/DMSO/H 2 Carrying out suction filtration, washing and homogenization on the O solution to prepare an aramid nano-fiber dispersion liquid;
(2) Mixing and dispersing 0.005-0.05 part of carbon nanotube powder, 0.005-0.1 part of dispersing agent, 0.005-0.1 part of stabilizing agent and 1 part of water according to parts by weight to prepare a carbon nanotube dispersion liquid, and adding the aramid nano-fiber dispersion liquid obtained in the step (1) into the carbon nanotube dispersion liquid to prepare a modified carbon nanotube dispersion liquid;
(3) Adding graphene oxide into water, controlling the mass concentration of the graphene oxide to be 0.005-1%, stirring to prepare a graphene dispersion liquid, and adding the modified carbon nanotube dispersion liquid obtained in the step (2) into the graphene dispersion liquid to obtain the aramid carbon nano dispersion liquid.
2. The method of claim 1, wherein: in the step (1), the size length of the aramid fiber is 1 to 13 μm.
3. The method of claim 1, wherein: in the step (1), the mass ratio of the water added into the ANF/DMSO solution to the solvent in the solution is 1: 1-1: 50.
4. The method of claim 1, wherein: in the step (2), the length of the carbon nanotube powder is more than 5 um.
5. The method of claim 1, wherein: in the step (2), one or more compounds selected from the group consisting of compounds of the following formula (1), TNRDIS, disponer 983, FA 196, FX 9086, sodium glycocholate and derivatives thereof, sodium glycodeoxycholate and derivatives thereof, sodium chenodeoxycholate and derivatives thereof, sodium taurocholate and derivatives thereof, sodium deoxycholate and derivatives thereof, polyvinylpyrrolidone and derivatives thereof, polyvinyl caprolactam and derivatives thereof, polyvinyl acetamide and derivatives thereof, and sodium dodecylbenzenesulfonate,
wherein R is 1 is-OH, -ONa, -NH 3 C 2 O 2 Na、-NHCH 2 COOH、-N 2 H 8 C 4 SO 4 Na or-NH 5 C 2 SO 3 Na，R 2 is-H, -OH, halogen, -OCH 3 、-OCH 2 CH 3 Or an ester group having 2 to 8 carbon atoms.
6. The method of claim 1, wherein: in the step (2), the stabilizer is selected from one or more of a polymer stabilizer DNA/RNA, cellulose and derivatives thereof, and sodium carboxymethyl cellulose.
7. The method of claim 1, wherein: in the step (2), the aramid nano-fiber aqueous dispersion and the carbon nano-tube dispersion are mixed according to the volume ratio of 1: 1-1: 2.
8. The method of claim 1, wherein: in the step (3), the modified carbon nanotube dispersion liquid and the graphene dispersion liquid are mixed according to the volume ratio of 2.5: 50-50: 100.
9. An aramid carbon nanodispersion prepared by the method of any one of claims 1-8.
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