CN110229643B - Preparation method of titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive and product - Google Patents
Preparation method of titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive and product Download PDFInfo
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- CN110229643B CN110229643B CN201910537580.0A CN201910537580A CN110229643B CN 110229643 B CN110229643 B CN 110229643B CN 201910537580 A CN201910537580 A CN 201910537580A CN 110229643 B CN110229643 B CN 110229643B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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Abstract
The invention relates to a preparation method and a product of titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive. The method comprises the following steps: step one, preparing a polyurethane solution, specifically: taking a proper amount of polyurethane, and adding the polyurethane into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1 for full dissolution to obtain a polyurethane solution with the mass fraction of 10-20 wt.%; step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 100:0.1-50:50, and then dispersing the mixed powder into a mixed solvent to obtain a mixed filler; dispersing the filler in the polyurethane solution to obtain the conductive heat-conducting adhesive; wherein, among the electrically conductive heat-conducting glue: the mass ratio of filler to polyurethane was 0.1:100 and 100: 100. The advantages are that: the preparation method is simple, the operation is convenient, the efficiency is high, the cost is low, and the prepared conductive and heat-conducting adhesive has high bonding strength, excellent conductive and heat-conducting properties and wide application prospect in the field of electronic packaging.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a preparation method and a product of titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive.
Background
The polymer-based conductive adhesive plays a great role in the bonding of electronic components or battery electrodes, but the heat dissipation function of electronic products needs to be enhanced due to the requirements for miniaturization, portability and integration of electronic products. Therefore, the conductive adhesive needs to have stronger heat conductivity and better mechanical properties. At present, in order to obtain high thermal conductivity, the content of a traditional conductive filler added into a polymer adhesive matrix needs to be increased, and the problem caused by the traditional conductive filler is the deterioration of the overall mechanical property of the adhesive. The new high-thermal-conductivity and high-electric-conductivity fillers such as carbon nanotubes and graphene provide a larger development space for the development of the electric-conductivity and heat-conduction adhesive. However, the possibility of completely replacing the traditional filler is severely restricted by factors such as difficulty in preparation and processing of the carbon nano material, high price and the like.
The graphene and the carbon nano tube are mixed and filled in the matrix according to a certain proportion, so that various physical properties of the composite material are improved. The graphene is a two-dimensional material, the carbon nano tube is a one-dimensional material, and the two fillers with different dimensions are orderly connected in the matrix to form an effective space network passage which can orderly transmit heat flow or current. Therefore, the matrix is filled with the multi-dimensional filler through grading, on one hand, a space electric conduction or heat conduction network structure of the composite material is constructed, and an effective heat conduction or electric conduction network is formed, so that the heat conduction performance or electric conduction performance of the composite material is improved. On the other hand, the multi-dimensional spatial connection effectively reduces the percolation value, namely, the performance of the composite material is greatly improved, and simultaneously, the content of the filler is reduced, thereby being beneficial to reducing the cost and improving the processing performance of the composite material.
Titanium diboride (TiB)2) Is the most stable compound of boron and titanium, is combined in a covalent bond mode and belongs to a metalloid compound of a hexagonal system. The boron atom surface and the titanium atom surface in the crystal structure alternately appear to form a two-dimensional network structure, wherein B is combined with the other 3B by covalent bonds, and redundant one electron forms a large pi bond. The layered structure of boron atoms and Ti outer layer electrons similar to graphite determine TiB2Has good electrical and thermal conductivity. Furthermore, TiB2The conductive filler material also has the advantages of high melting point, low density, high hardness, high fracture toughness, good high-temperature mechanical property, stable chemical property, good oxidation resistance, small thermal expansion coefficient and the like, and is a potential conductive filler material. At present, a few research reports exist, titanium diboride is filled into a polymer matrix to enhance the heat conduction or electric conduction performance of the polymer matrix, and the superiority of the titanium diboride as a heat conduction and electric conduction filler is shown. However, how to maximize the performance of titanium diboride requires further research and development.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method and a product of titanium diboride-carbon nanotube-polyurethane conductive and heat-conducting adhesive, and effectively overcoming the defects of the prior art.
The technical scheme for solving the technical problems is as follows:
the preparation method of the titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive comprises the following steps:
step one, preparing a polyurethane solution, specifically: adding polyurethane with a proper amount into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1, heating at 80 ℃ for 1h, and standing for 24h to fully dissolve the polyurethane to obtain a polyurethane solution with a mass fraction of 10-20 wt.%;
step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 100:0.1-50:50, and then dispersing the mixed powder into a mixed solvent of acetone and DMF or DMF and ethanol with the volume ratio of 1:1 to obtain a mixed filler;
dispersing the filler obtained in the step two into the polyurethane solution obtained in the step one to obtain the conductive heat-conducting adhesive;
wherein, in the obtained conductive and heat-conducting adhesive: the mass ratio of filler to polyurethane was 0.1:100 and 100: 100.
The invention has the beneficial effects that: the preparation method is simple, the operation is convenient, the efficiency is high, the cost is low, and the prepared conductive and heat-conducting adhesive has high bonding strength, excellent conductive and heat-conducting properties and wide application prospect in the field of electronic packaging.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the titanium diboride is industrial-grade flaky titanium diboride.
The further scheme has the beneficial effects that the performance of the conductive adhesive meets the standard, and the effective preparation of the titanium diboride-carbon nanotube-polyurethane conductive adhesive is promoted.
Further, the carbon nanotube is a multi-walled or single-walled carbon nanotube.
The further scheme has the beneficial effects that the performance of the conductive adhesive meets the standard, and the effective preparation of the titanium diboride-carbon nanotube-polyurethane conductive adhesive is promoted.
Further, the polyurethane is a linear polyurethane.
The further scheme has the beneficial effect of promoting the good preparation of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive.
Further, in the second step, the solid content of the obtained mixed filler is 5 wt.%.
The beneficial effect of adopting the further scheme is that the subsequent good preparation of the conductive and heat-conducting adhesive is facilitated.
Also provides a product of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive prepared by the preparation method of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive.
The beneficial effects are that: the prepared conductive and heat-conducting adhesive has high bonding strength and excellent conductive and heat-conducting properties.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
The first embodiment is as follows: the preparation method of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive comprises the following steps:
step one, preparing a polyurethane solution, specifically: adding polyurethane with a proper amount into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1, heating for 1h at 80 ℃, standing for 24h to fully dissolve the polyurethane, and obtaining a polyurethane solution with a mass fraction of 10 wt.%;
step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 100:0.1, and then dispersing the mixed powder into a mixed solvent of acetone and DMF or DMF and ethanol with the volume ratio of 1:1 to obtain a mixed filler with the solid content of 5 wt.%;
dispersing the filler obtained in the step two in the polyurethane solution obtained in the step one, specifically dispersing the filler in the polyurethane solution by adopting a mode of ultrasonic dispersion for 1 hour or mechanical stirring for 5 hours and the like to obtain the conductive heat-conducting adhesive;
wherein, in the obtained conductive and heat-conducting adhesive: the mass ratio of filler to polyurethane was 0.1: 100.
Preferably, the titanium diboride is industrial-grade flaky titanium diboride; the carbon nano tube is a multi-wall or single-wall carbon nano tube; the polyurethane is linear polyurethane.
The resistivity of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive prepared by the embodiment is 1 × 10-4Omega cm, thermal conductivity of 0.8W/mK, and shear strength of 5 MPa.
The second embodiment is a preparation method of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive, which includes the following steps:
step one, preparing a polyurethane solution, specifically: adding polyurethane with a proper amount into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1, heating for 1h at 80 ℃, standing for 24h to fully dissolve the polyurethane, and obtaining a polyurethane solution with a mass fraction of 15 wt.%;
step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 80:20, and then dispersing the mixed powder in a mixed solvent of acetone and DMF or DMF and ethanol with the volume ratio of 1:1 to obtain mixed filler with the solid content of 5 wt.%;
dispersing the filler obtained in the step two in the polyurethane solution obtained in the step one, specifically dispersing the filler in the polyurethane solution by adopting a mode of ultrasonic dispersion for 1 hour or mechanical stirring for 5 hours and the like to obtain the conductive heat-conducting adhesive;
wherein, in the obtained conductive and heat-conducting adhesive: the mass ratio of filler to polyurethane was 70: 100.
The other steps are the same as those of the first embodiment.
Titanium diboride prepared in this example-carbon nanotube-polyurethane conductive heat-conducting adhesive with resistivity of 1.5 x 10-5Omega cm, thermal conductivity of 1.1W/mK, and shear strength of 20 MPa.
The preparation method of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive comprises the following steps:
step one, preparing a polyurethane solution, specifically: adding polyurethane with a proper amount into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1, heating at 80 ℃ for 1h, and standing for 24h to fully dissolve the polyurethane to obtain a polyurethane solution with a mass fraction of 20 wt.%;
step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 50:50, and then dispersing the mixed powder in a mixed solvent of acetone and DMF or DMF and ethanol with the volume ratio of 1:1 to obtain a mixed filler with the solid content of 5 wt.%;
dispersing the filler obtained in the step two in the polyurethane solution obtained in the step one, specifically dispersing the filler in the polyurethane solution by adopting a mode of ultrasonic dispersion for 1 hour or mechanical stirring for 5 hours and the like to obtain the conductive heat-conducting adhesive;
wherein, in the obtained conductive and heat-conducting adhesive: the mass ratio of filler to polyurethane was 100: 100.
The other steps are the same as those of the first embodiment.
The resistivity of the titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive prepared by the embodiment is 10 multiplied by 10-5Omega cm, thermal conductivity of 1.5W/mK, and shear strength of 8 MPa.
The preparation principle comprises the following steps:
titanium diboride has large pi bonds, and carbon nanotubes also have large delocalized pi bonds, so after the carbon nanotubes are mixed with the titanium diboride, two filler particles are assembled together through strong pi-pi conjugate interaction, and a certain space structure can be formed. In addition, the hydrophilic group of the titanium diboride has certain interaction with the hydrophilic group of the polyurethane, and can promote the dispersion of the carbon nano tube in the polyurethane. In addition, the filler has good dispersibility in polyurethane, and can form a heat conduction or electric conduction path: the plate structure of the titanium diboride can improve the contact area among the fillers, the reinforcing effect is caused in the two-dimensional direction, the one-dimensional carbon nano tubes are used as bridges to connect the titanium diboride fillers, a plurality of electric conduction and heat conduction paths are formed among the fillers to form a space network, and the electric conduction and heat conduction performance of the adhesive are improved. Meanwhile, the filling of the titanium diboride and the carbon nano tubes with high heat conductivity enables the conductive adhesive to have excellent heat conductivity.
The whole preparation process is simple, the operation is convenient, the efficiency is high, the cost is low, and the prepared conductive and heat-conducting adhesive has high bonding strength, excellent conductive and heat-conducting properties and wide application prospect in the field of electronic packaging.
Compared with the prior art, the invention has the beneficial effects that:
1) in the invention, a small amount of carbon nano tubes are added in addition to the two-dimensional titanium diboride filler, so that better electric and heat conducting properties can be obtained.
2) The use amount of the whole filler is reduced while better electric and thermal conductivity is ensured, and the improvement of mechanical property and the reduction of cost are facilitated.
3) The titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive prepared by the invention has low resistivity of 1 multiplied by 10-4-10×10-5Omega cm, thermal conductivity of 0.8-1.5W/mK, and shear strength of 5-20 MPa.
The titanium diboride-carbon nanotube-polyurethane conductive and heat-conducting adhesive is prepared by utilizing various (including but not limited to the three embodiments), has high bonding strength, excellent conductive and heat-conducting properties and wide application prospect in the field of electronic packaging.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A preparation method of titanium diboride-carbon nanotube-polyurethane conductive heat-conducting adhesive is characterized by comprising the following steps:
step one, preparing a polyurethane solution, specifically: adding polyurethane with a proper amount into a mixed solvent of acetone and DMF or DMF and ethanol with a volume ratio of 1:1, heating at 80 ℃ for 1h, and standing for 24h to fully dissolve the polyurethane to obtain a polyurethane solution with a mass fraction of 10-20 wt.%;
step two, preparing the mixed filler of the titanium diboride powder and the carbon nano tube powder, which comprises the following steps: mixing titanium diboride powder and carbon nano tube powder according to the mass fraction of 100:0.1-50:50, and then dispersing the mixed powder into a mixed solvent of acetone and DMF or DMF and ethanol with the volume ratio of 1:1 to obtain a mixed filler;
dispersing the filler obtained in the step two into the polyurethane solution obtained in the step one to obtain the conductive heat-conducting adhesive;
wherein, in the obtained conductive and heat-conducting adhesive: the mass ratio of filler to polyurethane was 0.1:100 and 100: 100.
2. The method for preparing titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive according to claim 1, wherein the method comprises the following steps: the titanium diboride is industrial-grade flaky titanium diboride.
3. The method for preparing titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive according to claim 1, wherein the method comprises the following steps: the carbon nanotube is a multi-walled or single-walled carbon nanotube.
4. The method for preparing titanium diboride-carbon nanotube-polyurethane conductive and heat-conductive adhesive according to claim 1, wherein the method comprises the following steps: the polyurethane is linear polyurethane.
5. The method for preparing titanium diboride-carbon nanotube-polyurethane electric and heat conducting adhesive according to any one of claims 1 to 4, wherein the method comprises the following steps: in the second step, the solid content of the obtained mixed filler is 5 wt.%.
6. A product of the titanium diboride-carbon nanotube-polyurethane electric and heat conducting adhesive prepared by the preparation method of the titanium diboride-carbon nanotube-polyurethane electric and heat conducting adhesive as claimed in any one of claims 1 to 5.
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| CN111621139B (en) * | 2020-06-29 | 2022-04-08 | 江西伟普科技有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
| CN112063345B (en) * | 2020-08-18 | 2022-07-19 | 湖南创瑾科技有限公司 | Nano conductive heat-conducting adhesive and application thereof |
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