CN115716925A - Preparation method of ternary interpenetrating network high-thermal-conductivity hydrogel composite material with synergistic effect - Google Patents
Preparation method of ternary interpenetrating network high-thermal-conductivity hydrogel composite material with synergistic effect Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 50
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 230000002195 synergetic effect Effects 0.000 title claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 29
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 24
- 239000000945 filler Substances 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 14
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- IRLPACMLTUPBCL-KQYNXXCUSA-N 5'-adenylyl sulfate Chemical compound C1=NC=2C(N)=NC=NC=2N1[C@@H]1O[C@H](COP(O)(=O)OS(O)(=O)=O)[C@@H](O)[C@H]1O IRLPACMLTUPBCL-KQYNXXCUSA-N 0.000 claims description 10
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000003999 initiator Substances 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- 239000002048 multi walled nanotube Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000005054 agglomeration Methods 0.000 claims description 5
- 230000002776 aggregation Effects 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 239000011231 conductive filler Substances 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 2
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 2
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000499 gel Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 2
- 229920000642 polymer Polymers 0.000 abstract 2
- 230000017525 heat dissipation Effects 0.000 abstract 1
- 239000002114 nanocomposite Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
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Abstract
The invention discloses a preparation method of a ternary interpenetrating network high-thermal-conductivity hydrogel composite material with a synergistic effect, which takes boron nitride and carbon nano tubes as fillers, utilizes the similarity of crystal structures of the boron nitride and the carbon nano tubes, and can generate good synergistic effect. The invention can form stable combination of several polymers with different functions through the form of network interpenetration, thereby realizing the complementation of the performances of the components, having good mechanical property, ensuring that the polymer maintains the flexibility of the high-molecular composite material and simultaneously has the high heat-conducting performance of the material through adding the heat-conducting filler, and being widely applied to the fields of heat dissipation of electronic components and heat conduction of nano composite materials.
Description
Technical Field
The invention relates to a heat-conducting hydrogel, in particular to a preparation method of a ternary interpenetrating network high heat-conducting hydrogel composite material with a synergistic effect.
Background
With the rapid development of miniaturized microelectronics and high integration, the thermal conductivity of materials has become a key technology in the microelectronic manufacturing process. It is difficult for electronic devices to rapidly dissipate heat, resulting in a sharp rise in chip temperature, resulting in low device efficiency and low lifetime, and therefore, there is an urgent need to research materials having good thermal conductivity and excellent mechanical properties.
The hydrogel is a novel high polymer material with a three-dimensional space network structure, and has wide application in the fields of industry, agriculture, biomedicine and the like due to good flexibility and biocompatibility, but the traditional hydrogel has poor mechanical property and low strength, is easy to generate permanent fracture, has a single internal structure and low heat conductivity, and limits the application range of the hydrogel to a great extent. In order to solve the problems, the invention utilizes the interpenetrating network structure to prepare the hydrogel, so that the mechanical property of the material is obviously improved, and the heat conduction characteristic of the hydrogel composite material is effectively improved by adding the heat conduction filler and utilizing the synergistic effect.
Disclosure of Invention
The invention provides a preparation method of a ternary interpenetrating network high-thermal-conductivity hydrogel composite material with a synergistic effect. According to the invention, boron nitride and carbon nanotubes are selected as heat-conducting fillers, the heat-conducting property of the hydrogel is improved through the synergistic effect of the boron nitride and the carbon nanotubes, the mechanical property of the hydrogel is enhanced by utilizing the ternary interpenetrating network structure, and the obtained hydrogel composite material has excellent mechanical property and good heat-conducting property.
The preparation method of the ternary interpenetrating network high-thermal-conductivity hydrogel composite material with the synergistic effect comprises the following steps of:
step 1: pretreatment of thermally conductive fillers
Weighing heat-conducting filler, dispersing the heat-conducting filler in 50mL of n-hexane, performing ultrasonic dispersion uniformly to reduce agglomeration, and then removing the n-hexane to obtain pretreated heat-conducting filler for later use;
step 2: preparation of hydrogel with semi-interpenetrating network structure
Weighing 1-2 parts of PVA, adding the PVA into deionized water, stirring until the PVA is completely dissolved, then adding 15-20 parts of AMPS into the deionized water for dissolving, adding the obtained AMPS solution into the PVA solution, and simultaneously adding 0.03-0.05 part of cross-linking agent, 0.04-0.06 part of initiator and N 2 Reacting for 2-4 h at constant temperature (60 ℃) under protection to obtain PVA-PAMPS semi-interpenetrating network structure hydrogel;
and step 3: preparation of ternary interpenetrating network high-thermal-conductivity hydrogel composite material
Adding the PVA-PAMPS semi-interpenetrating network structure hydrogel obtained in the step 2 into an aqueous solution (10 ml of deionized water) in which 8-10 parts of AA are dissolved, simultaneously adding the heat-conducting filler pretreated in the step 1, 0.06-0.08 part of initiator and 0.08-0.1 part of cross-linking agent, reacting for 2-3 h at 30 ℃ in a closed reactor, uniformly diffusing acrylic acid, boron nitride and multi-walled carbon nanotubes in the gel, and fully washing to remove unreacted monomers and impurities to obtain the PVA-PAMPS-PAA ternary interpenetrating network heat-conducting hydrogel composite material.
The above-mentioned portions are all mass portions.
In the step 1, the heat-conducting filler is boron nitride and a multi-walled carbon nanotube, the proportion of the boron nitride in the heat-conducting filler is 60-90%, and the balance is the carbon nanotube.
The size of the boron nitride is 100nm, the inner diameter of the multi-wall carbon nanotube is 5-8nm, and the outer diameter of the multi-wall carbon nanotube is 10-15nm.
In the step 3, the addition amount of the pretreated heat-conducting filler is 1-3 wt% based on the total mass of the monomers. The total mass of the monomers refers to the total mass of PVA, AMPS and AA.
The cross-linking agent comprises any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.
The initiator comprises any one of ammonium persulfate and potassium persulfate.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the prior art, the network structure obtained by ternary interpenetration is more compact and stable, and the mechanical strength of the prepared hydrogel is obviously higher than that of a common hydrogel product;
2. because the crystal structures of the boron nitride and the carbon nano tube are very similar, good synergistic effect can be generated, and the heat conduction performance of the hydrogel material is effectively improved;
3. the preparation method has the advantages of simple process, low cost, easily controlled preparation conditions and high efficiency.
Drawings
FIG. 1 shows comparative structures of thermal conductivity of hydrogels obtained in different examples and comparative example 1.
FIG. 2 stress-strain curves of the hydrogels obtained in the different examples and comparative example 1.
FIG. 3 shows the comparison of the elastic modulus of the hydrogels obtained in the different examples and comparative example 1.
Detailed description of the preferred embodiments
The present invention will be further illustrated with reference to the following examples, but the embodiments of the present invention are not limited thereto.
Example 1:
the preparation method of the ternary interpenetrating network high thermal conductivity hydrogel composite material with the synergistic effect comprises the following steps:
1. weighing boron nitride and carbon nano tubes (the total addition amount is 3 wt%) in a ratio of 9:1, dissolving the boron nitride and the carbon nano tubes in 50mL of normal hexane, enabling the two groups to be more uniformly dispersed by an ultrasonic dispersion method for 30min, reducing the agglomeration phenomenon, and then removing the normal hexane to obtain the treated boron nitride and carbon nano tubes for later use.
2. Weighing 1.6g of PVA, adding 10ml of deionized water into a three-neck flask, stirring until the PVA is completely dissolved, adding 16g of AMPS into a beaker, dissolving with 20ml of deionized water, adding into the three-neck flask, simultaneously adding 0.09g of N, N '-methylene bisacrylamide and 0.07g of ammonium persulfate, and adding N, N' -methylene bisacrylamide 2 And (3) protecting, and reacting for 3h at constant temperature (60 ℃) to obtain the semi-interpenetrating PVA-PAMPS hydrogel.
3. Putting the semi-interpenetrating PVA-PAMPS hydrogel into a dissolved 9gAA aqueous solution (10 ml deionized water), simultaneously adding boron nitride and carbon nano tubes (0.72g.
Example 2:
the preparation method of the ternary interpenetrating network high thermal conductivity hydrogel composite material with the synergistic effect comprises the following steps:
1. weighing boron nitride and carbon nano tubes in a ratio of 8:2, dissolving the boron nitride and the carbon nano tubes in 50mL of normal hexane, enabling the two groups to be more uniformly dispersed by an ultrasonic dispersion method for 30min, reducing agglomeration, and then removing the normal hexane to obtain the treated boron nitride and carbon nano tubes for later use.
2. Weighing 1.6g of PVA, adding 10ml of deionized water into a three-neck flask, stirring until the PVA is completely dissolved, adding 16g of AMPS into a beaker, dissolving with 20ml of deionized water, adding into the three-neck flask, simultaneously adding 0.09g of N, N '-methylene bisacrylamide and 0.07g of ammonium persulfate, and adding N, N' -methylene bisacrylamide 2 And (3) protecting, and reacting for 3h at constant temperature (60 ℃) to obtain the semi-interpenetrating PVA-PAMPS hydrogel.
3. Putting the semi-interpenetrating PVA-PAMPS hydrogel into a dissolved 9gAA aqueous solution (10 ml deionized water), simultaneously adding boron nitride and carbon nano tubes (0.64g.
Example 3:
the preparation method of the ternary interpenetrating network high thermal conductivity hydrogel composite material with the synergistic effect comprises the following steps:
1. weighing boron nitride and carbon nano tubes which are 7:3 in proportion, dissolving the boron nitride and the carbon nano tubes in 50mL of n-hexane, enabling the two groups to be more uniformly dispersed by an ultrasonic dispersion method for 30min, reducing the agglomeration phenomenon, and then removing the n-hexane to obtain the treated boron nitride and carbon nano tubes for later use.
2. Weighing 1.6g of PVA, adding 10ml of deionized water into a three-neck flask, stirring until the PVA is completely dissolved, adding 16g of AMPS into a beaker, dissolving with 20ml of deionized water, adding into the three-neck flask, simultaneously adding 0.09g of N, N '-methylene bisacrylamide and 0.07g of ammonium persulfate, and adding N, N' -methylene bisacrylamide 2 And (3) protecting, and reacting for 3h at constant temperature (60 ℃) to obtain the semi-interpenetrating PVA-PAMPS hydrogel.
3. Putting the semi-interpenetrating PVA-PAMPS hydrogel into a dissolved 9gAA aqueous solution (10 ml deionized water), simultaneously adding boron nitride and carbon nano tubes (0.56g.
Example 4:
in example 1, the mixture ratio of boron nitride and carbon nanotubes in step (1) was 9:1 and was replaced by 6:4, and the mass ratio of boron nitride to carbon nanotubes in step (2) was (0.48g.
Example 5:
the mixture ratio of boron nitride and carbon nanotubes in step (1) in example 1 was 9:1 and was changed to 5:5, and the mass ratio of boron nitride to carbon nanotubes in step (2) was (0.4 g.
Example 6:
the total amount of boron nitride and carbon nanotubes added in step (1) in example 1 was replaced with 1wt%, and the rest were unchanged.
The embodiments of the present invention will be described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the technical scope of the present invention should fall within the scope of the present patent.
Comparative example 1:
respectively weighing 1.6g of PVA and 10ml of deionized water into a three-neck flask, uniformly stirring until the PVA and the deionized water are completely dissolved, then weighing 16g of AMPS and 20ml of deionized water, adding the AMPS and the deionized water into the beaker, stirring and dissolving, adding the obtained solution into the three-neck flask, simultaneously adding 0.09g of N, N' -methylene bisacrylamide and 0.07g of ammonium persulfate, and using N to prepare a solution 2 And (3) protecting, and reacting for 3h at constant temperature (60 ℃) to obtain the semi-interpenetrating PVA-PAMPS hydrogel.
FIG. 1 is a comparison result of thermal conductivity of hydrogels obtained in examples 1 to 6 and comparative example 1, and it can be seen from the figure that the introduction of the thermal conductive filler in example 1 increases the network density, forms a high thermal conductive path, reduces phonon scattering, and reduces the interfacial thermal resistance between the filler and the matrix, so that the hydrogel composite material has good thermal conductivity (the thermal conductivity of example 1 is 1.26W/m.K, which is increased by 360% compared with the thermal conductivity of comparative example 1, which is 0.27W/m.K).
FIG. 2 is a stress-strain graph of hydrogels obtained in various examples and comparative examples; the compressive strength of the hydrogel of comparative example 1 was 0.021MPa, and the compressive strength of the hydrogel prepared by the method of the present invention (example 1) was 0.075MPa, which is 3.5 times that of comparative example 1, and thus the hydrogel had good mechanical properties and could withstand a wider range of stresses.
As can be seen from FIG. 3, the elastic modulus of example 1 is 0.77MPa, the elastic modulus of comparative example 1 is 0.21MPa, and the elastic modulus of example 1 is increased by 260% compared with that of comparative example 1, mainly because the three monomers have high crosslinking degrees through a two-step method, the network structure is more stable, and the heat-conductive filler also plays a role of reinforcing the matrix, so that the elastic modulus of the hydrogel composite material is obviously increased.
In combination with the above, the prepared hydrogel composite material has excellent mechanical properties (higher elastic modulus) and good heat conduction characteristics (higher thermal conductivity).
Claims (8)
1. A preparation method of a ternary interpenetrating network high-thermal conductivity hydrogel composite material with a synergistic effect is characterized by comprising the following steps: the method comprises the following steps:
step 1: pretreatment of thermally conductive fillers
Weighing heat-conducting filler, dispersing the heat-conducting filler in n-hexane, performing ultrasonic dispersion uniformly to reduce agglomeration, and then removing the n-hexane to obtain pretreated heat-conducting filler for later use;
step 2: preparation of hydrogel with semi-interpenetrating network structure
Weighing 1-2 parts of PVA, adding the PVA into deionized water, stirring until the PVA is completely dissolved, then adding 15-20 parts of AMPS into the deionized water for dissolving, adding the obtained AMPS solution into the PVA solution, and simultaneously adding 0.03-0.05 part of cross-linking agent, 0.04-0.06 part of initiator and N 2 Reacting at constant temperature under protection to obtain PVA-PAMPS semi-interpenetrating network structure hydrogel;
and step 3: preparation of ternary interpenetrating network high-thermal-conductivity hydrogel composite material
And (3) adding the PVA-PAMPS semi-interpenetrating network structure hydrogel obtained in the step (2) into an aqueous solution in which 8-10 parts of AA are dissolved, simultaneously adding the heat-conducting filler pretreated in the step (1), 0.06-0.08 part of initiator and 0.08-0.1 part of cross-linking agent, reacting in a closed reactor, uniformly diffusing acrylic acid and the pretreated heat-conducting filler in gel, and fully washing to remove unreacted monomers and impurities to obtain the PVA-PAMPS-PAA ternary interpenetrating network heat-conducting hydrogel composite material.
2. The method of claim 1, wherein:
in the step 1, the heat-conducting filler is boron nitride and a multi-walled carbon nanotube, the proportion of the boron nitride in the heat-conducting filler is 60-90%, and the balance is the carbon nanotube.
3. The method of claim 2, wherein:
the size of the boron nitride is 100nm, the inner diameter of the multi-wall carbon nanotube is 5-8nm, and the outer diameter is 10-15nm.
4. The method of claim 1, wherein:
in the step 2, the reaction temperature is 60 ℃, and the reaction time is 2-4 h.
5. The method of claim 1, wherein:
in the step 3, the addition amount of the pretreated heat-conducting filler is 1-3 wt% based on the total mass of the monomers.
6. The method of claim 1, wherein:
in the step 3, the reaction temperature is 30 ℃ and the reaction time is 2-3 h.
7. The method of claim 1, wherein:
the cross-linking agent comprises any one of ethylene glycol dimethacrylate and N, N-methylene bisacrylamide.
8. The method of claim 1, wherein:
the initiator comprises any one of ammonium persulfate and potassium persulfate.
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| WO2003093327A1 (en) * | 2002-05-01 | 2003-11-13 | Hokkaido Technology Licensing Office Co., Ltd. | Gel having multiple network structure and method for preparation thereof |
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