CN110358298A - A kind of carbon nanowalls/macromolecule composite construction thermal interfacial material and preparation method thereof - Google Patents
A kind of carbon nanowalls/macromolecule composite construction thermal interfacial material and preparation method thereof Download PDFInfo
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- CN110358298A CN110358298A CN201910622416.XA CN201910622416A CN110358298A CN 110358298 A CN110358298 A CN 110358298A CN 201910622416 A CN201910622416 A CN 201910622416A CN 110358298 A CN110358298 A CN 110358298A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention discloses a kind of based on ultra-thin thermal interfacial material of vertical carbon nanowalls/macromolecule composite construction and preparation method thereof；The thermal interfacial material is made of continuous, vertical arrangement carbon nanowalls and macromolecule matrix；Thermal interfacial material use first in press plasma gas phase deposition method, deposition growing forms continuous, vertical carbon nanowalls structure, then using macromolecule as matrix, progress is compound, improves thermal conductivity outside thermal interfacial material face, solves the problems, such as that thermal conductivity is low outside its face.
Description
Technical field
The present invention relates to a kind of carbon nanowalls/macromolecule composite construction thermal interfacial materials and preparation method thereof, belong to chemistry
Material Field.
Background technique
The micromation of electronic component and integrated more stringent requirements are proposed to heat dissipation performance.The environment of overheat will affect
Its service life and operational reliability.Due to the presence of microscopic surface roughness, the real contact area of two solids only accounts for it
The 1 ~ 2% of apparent contact area, rest part are only then 0.026Wm by thermal conductivity-1K-1Air filling, in heat source and heat sink
Between form big thermal contact resistance, limit shedding for heat.
In order to solve this problem, thermal interfacial material be used in heat source and it is heat sink between fill the air gap, reduce contact
Thermal resistance improves radiating efficiency.Traditional thermal interfacial material mainly by some highly heat-conductive carbon/ceramic porcelain fillings for example boron nitride, aluminium nitride,
Aluminium oxide etc. is mixed into polymeric matrix, and thermal conductivity is mostly 1 ~ 5Wm-1K-1, it is difficult to solve electronics industry high power high density envelope
Heat dissipation problem brought by filling.
Graphene has been widely used for solving heat dissipation problem due to the thermal conductivity of its superelevation.It is currently used to prepare graphite
The method of alkenyl thermal interfacial material mainly includes following two categories: 1) directly graphene being blended with macromolecule matrix, such method
It is easy to operate, but since the dispersion unevenness of graphene is low so as to cause sample thermal conductivity；2) template mainly has ice crystal template
Method and two kinds of nickel foam template, ice crystal template is difficult to improve graphene content, and thermal conductivity is often lower；Made with nickel foam
Tend to reach higher graphene content for template, and the graphene of CVD growth has a higher quality, thus thermal conductivity compared with
It is high.(Fang, the H. such as Bai; Zhao, Y.; Zhang, Y.; Ren, Y.; Bai, S.L. Three-dimensional
graphene foam-filled elastomer composites with high thermal and mechanical
Properties. ACS Appl. Mater. Interfaces 2017,9,26447-26459.) using nickel foam as
Template, when graphene content is only 11.6wt%, transverse thermal conductivity can achieve 28.77Wm-1K-1, but it is constrained to nickel
The characteristic of foam itself, longitudinal thermal conductivity be not still high.In addition to this, most work at present can not will be graphene-based
The thickness of thermal interfacial material is reduced to micron dimension, therefore it is still difficult to meet growing heat dissipation and package requirements.
Summary of the invention
For the above technical problems, the purpose of the present invention is: propose a kind of carbon nanowalls/macromolecule composite junction
Structure thermal interfacial material and preparation method thereof improves thermal conductivity outside thermal interfacial material face.
The technical solution of the invention is as follows is achieved: a kind of hot interface material of carbon nanowalls/macromolecule composite construction
Material, including carbon nanowalls and polymer-based end；The carbon nanowalls are stacked by the graphene perpendicular to substrate, are had and are connected
Continuous, vertical structure；The macromolecule matrix is compressible macromolecular elastomer.
In thermal interfacial material provided by the present application, there is continuous, vertical carbon nanowalls structure, and pass through spin coating, true
The methods of empty assistant soakage and macromolecular elastomer matrix are compound.
Optionally, the carbon nanowalls with a thickness of 1 ~ 150 μm, density is 0.1 ~ 0.3g/cm3。
Optionally, the thermal interfacial material with a thickness of 1 ~ 150 μm, density is 0.7 ~ 1.2g/cm3。。
Optionally, outside the face of the thermal interfacial material thermal conductivity between 10 ~ 25Wm-1K-1, graphene content between 5 ~
10wt%。
In this application, outside face thermal conductivity be thermal interfacial material normal direction.
Present invention also provides a kind of above-mentioned carbon nanowalls/macromolecule matrix composite construction ultra-thin thermal interfacial material systems
Preparation Method: the method that plasma gas phase deposition is pressed in use, deposition growing form continuous, vertical carbon nanowalls structure, and
Using macromolecule as matrix, progress is compound, and the thermal interfacial material can be obtained.
Specifically, preparation method includes:
A) using clean silicon wafer as growth substrate, plasma gas phase deposition technology is pressed in utilization, carries out carbon nanowalls deposition
Growth is obtained with continuous, vertical structure carbon nanowalls；
B) it by obtained carbon nanowalls by the method for spin coating, is carried out with high polymer elastic matrix compound, obtains vertical carbon nanometer
Wall/macromolecule composite construction；
C) vertical carbon nanowalls/macromolecule composite construction is removed from silicon substrate to get to the independent thermal interfacial material.
Optionally, the carbon nanowalls deposition pressure is 0.1 ~ 10Torr.
Preferably, the carbon nanowalls deposition pressure is 600 ~ 800Pa.
Optionally, the carbon nanowalls deposition power is 3 ~ 21kW；The carbon nanowalls sedimentation time is 0.5 ~ 25min；
Preferably, the carbon nanowalls deposition power is 15 ~ 18kW；The carbon nanowalls sedimentation time is 10 ~ 15min.
The upper limit of the carbon nanowalls deposition power is selected from 15kW, 18kW, 21kW；Under the carbon nanowalls deposition power
Limit is selected from 3kW, 5kW, 8kW.
The online of the carbon nanowalls sedimentation time is selected from 15min, 20min, 25min；The carbon nanowalls sedimentation time
Lower limit be selected from 0.5min, 5.5min, 10.5min.
Optionally, described high molecular compound to be at least realized by the following method:
The methods of impregnated by spin coating, vacuum aided, so that macromolecule matrix enters carbon nanowalls gap, can be obtained described
Carbon nanowalls/macromolecule matrix composite construction.
Optionally, the spin coating revolving speed is 2000 ~ 5000rpm, and spin-coating time is 0.5 ~ 2min.
Preferably, the spin coating revolving speed is 3000 ~ 4000rpm, and spin-coating time is 1 ~ 1.5min.
Optionally, the macromolecule matrix includes but is not limited to polyurethane (PU), dimethyl silicone polymer (PDMS), rubber
(NR) etc. with the macromolecular elastomer of compressibility.
Due to the application of the above technical scheme, compared with the prior art, the invention has the following advantages:
The present invention is obtained using plasma gas phase deposition technology is pressed in utilizing with continuous, vertical structure carbon nanowalls, and
It is compound with the progress of high polymer elastic matrix, solve the problems, such as that thermal conductivity is low outside thermal interfacial material face.
Thermal conductivity is between 10 ~ 25Wm outside the face of thermal interfacial material provided by the present application-1K-1, graphene content between 5 ~
10wt%。
Detailed description of the invention
Technical scheme of the present invention is further explained with reference to the accompanying drawing:
Attached drawing 1 is the preparation process schematic diagram of thermal interfacial material of the invention；
Attached drawing 2 is the Raman spectrogram of carbon nanowalls in embodiment 1；
Attached drawing 3 is the Scanning Electron microscope photo of carbon nanowalls cross section in embodiment 1；
Attached drawing 4 is the Scanning Electron microscope photo of pattern at the top of thermal interfacial material in embodiment 1.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.Unless otherwise instructed, real
It applies raw material employed in example and is all from commercially available, unprocessed direct use；Instrument and equipment employed in embodiment is equal
Using manufacturer's recommended parameter.
Raw material and reagent use herein:
Dimethyl silicone polymer (PDMS): Dow corning company；
Argon gas, methane, hydrogen: Ningbo City east of a river Hua Yu chemical gases business department.
Instrument and equipment:
In embodiment, carbon nanowalls growth uses MPCVD system (Anhui Bei Yike equipment and technology Co., Ltd)；
Carbon nanowalls are compound using the desk-top sol evenning machine of KW-4A type in macromolecule；
Thermal conductivity is measured using LFA467 laser isotope (Netzsch, Germany) outside the face of sample；
The pattern of sample is measured using field emission scanning electron microscope (QuantaFEG250, FEI, USA).
As shown in Fig. 1, a kind of carbon nanowalls of the present invention/macromolecule matrix composite construction thermal interfacial material, tool
There is continuous, vertical carbon nanowalls structure, and multiple with macromolecular elastomer matrix by the methods of spin coating, vacuum aided dipping
It closes.
The thermal conducting path outside carbon nano-structured offer face in the thermal interfacial material.
The preparation method of thermal interfacial material at least includes the following steps:
Press plasma gas phase deposition technology in utilization, the carbon nanowalls structure that deposition growing is continuous, vertical, and by itself and high score
Elastic matrix progress is compound, is removed after the completion, the thermal interfacial material can be obtained.
Optionally, the carbon nanowalls deposition pressure is 0.1 ~ 10Torr；
Preferably, the carbon nanowalls deposition pressure is 600 ~ 800Pa.
Optionally, the carbon nanowalls deposition power is 3 ~ 21kW；The carbon nanowalls sedimentation time is 0.5 ~ 25min；
Preferably, the carbon nanowalls deposition power is 15 ~ 18kW；The carbon nanowalls sedimentation time is 10 ~ 15min.
Optionally, the macromolecule is compound can at least be realized by the following method:
The methods of impregnated by spin coating, vacuum aided, so that macromolecule matrix enters carbon nanowalls gap, can be obtained described
Carbon nanowalls/macromolecule matrix composite construction.
Optionally, the spin coating revolving speed is 2000 ~ 5000rpm, and spin-coating time is 0.5 ~ 2min；
Preferably, the spin coating revolving speed is 3000 ~ 4000rpm, and spin-coating time is 1 ~ 1.5min.
Optionally, the high molecular material includes but is not limited to polyurethane (PU), dimethyl silicone polymer (PDMS), rubber
Glue (NR) etc. has the macromolecular elastomer of compressibility.
Embodiment 1:
Silicon wafer is cut to the square piece of 35 × 35mm2,10min is cleaned by ultrasonic in acetone soln, the silicon wafer after cleaning is placed in
On the water-cooled copper platform of middle pressure plasma gas phase deposition system, being passed through flow velocity is 21slm argon gas so that system pressure to be adjusted to
800Pa.It is passed through hydrogen (0.8slm) and methane (80sccm) gaseous mixture, and deposition power is adjusted to 18kW progress gas phase and is sunk
Product, adjusting sedimentation time are 15min.Obtained carbon nanowalls and PDMS are carried out to compound, each PDMS that 50mg is added, with
4000rpm revolving speed spin coating 1min, repeats five times.Silicon substrate is etched away using HF, the thermal interfacial material can be obtained, be denoted as sample
Product 1#.
Embodiment 2:
Silicon wafer is cut to the square piece of 35 × 35mm2,10min is cleaned by ultrasonic in acetone soln, the silicon wafer after cleaning is placed in
On the water-cooled copper platform of middle pressure plasma gas phase deposition system, being passed through flow velocity is 21slm argon gas so that system pressure to be adjusted to
800Pa.It is passed through hydrogen (0.8slm) and methane (80sccm) gaseous mixture, and deposition power is adjusted to 18kW progress gas phase and is sunk
Product, adjusting sedimentation time are 10min.Obtained carbon nanowalls and PDMS are carried out to compound, each PDMS that 50mg is added, with
4000rpm revolving speed spin coating 1min, repeats five times.Silicon substrate is etched away using HF, the thermal interfacial material can be obtained, be denoted as sample
Product 2#.
Embodiment 3:
Silicon wafer is cut to the square piece of 35 × 35mm2,10min is cleaned by ultrasonic in acetone soln, the silicon wafer after cleaning is placed in
On the water-cooled copper platform of middle pressure plasma gas phase deposition system, being passed through flow velocity is 21slm argon gas so that system pressure to be adjusted to
800Pa.It is passed through hydrogen (0.8slm) and methane (80sccm) gaseous mixture, and deposition power is adjusted to 18kW progress gas phase and is sunk
Product, adjusting sedimentation time are 5min.Obtained carbon nanowalls and PDMS are carried out to compound, each PDMS that 50mg is added, with
4000rpm revolving speed spin coating 1min, repeats five times.Silicon substrate is etched away using HF, the thermal interfacial material can be obtained, be denoted as sample
Product 3#.
Embodiment 4:
It is with 1 difference of example: spin coating number is increased to 10 times, sample 4# is denoted as.
Embodiment 5:
It is with 2 difference of example: spin coating number is increased to 10 times, sample 5# is denoted as.
Embodiment 6:
It is with 3 difference of example: spin coating number is increased to 10 times, sample 6# is denoted as.
Raman spectrum and scanning electron microscope analysis are carried out to the carbon nanowalls of deposition growing in example 1 ~ 3 respectively；Respectively to sample
Product 1# ~ 6# is scanned electron microscope analysis.
Raman spectrum is typical generation with example 1 the results show that Raman signatures of the structure with typical carbon nanowalls
Table, as shown in Figure 2.
Scanning electron microscope the results show that carbon nanowalls have continuous, vertical structure, thickness with sedimentation time increase
And become larger, with example 1 for Typical Representative, scanning electron microscopic picture is as shown in Figure 3.
Scanning electron microscope is Typical Representative with example 1, sweeps the results show that PDMS is substantially filled with the gap of carbon nanowalls
It is as shown in Figure 4 to retouch electron microscopic picture.
It carries out thermal conductivity outside face to sample 1# ~ 6# respectively to test, test result, which shows sample 1# ~ 6#, higher face
Outer thermal conductivity, thermal conductivity is between 10 ~ 25Wm outside face-1K-1。
Thermal conductivity is 24.5Wm outside the face of sample 1#-1K-1；
Thermal conductivity is 17.3Wm outside the face of sample 2#-1K-1；
Thermal conductivity is 14.4Wm outside the face of sample 3#-1K-1；
Thermal conductivity is 18.5Wm outside the face of sample 4#-1K-1；
Thermal conductivity is 14.8Wm outside the face of sample 5#-1K-1；
Thermal conductivity is 10.7Wm outside the face of sample 6#-1K-1。
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (9)
1. a kind of carbon nanowalls/macromolecule composite construction thermal interfacial material, it is characterised in that: including carbon nanowalls and polymer-based
Bottom；The carbon nanowalls are stacked by the graphene perpendicular to substrate, have continuous, vertical structure；It is described polymer-based
Body is compressible macromolecular elastomer.
2. carbon nanowalls according to claim 1/macromolecule composite construction thermal interfacial material, it is characterised in that: the carbon
For the thickness of nm wall at 1 ~ 150 μm, density is 0.1 ~ 0.3g/cm3。
3. carbon nanowalls according to claim 1/macromolecule composite construction thermal interfacial material, it is characterised in that: the heat
Thermal conductivity is between 10 ~ 25Wm outside the face of boundary material-1K-1, 5 ~ 10wt% of graphene content.
4. a kind of preparation side of the described in any item carbon nanowalls of claims 1 to 3/macromolecule composite construction thermal interfacial material
Method, it is characterised in that: the method that plasma gas phase deposition is pressed in use, deposition growing form continuous, vertical carbon nanowalls
Structure, and using high molecular material as matrix, progress is compound, and the thermal interfacial material can be obtained.
5. the preparation method according to claim 4, it is characterised in that: the carbon nanowalls deposition pressure be 0.1 ~
10Torr, the carbon nanowalls deposition power are 3 ~ 21kW, and the carbon nanowalls sedimentation time is 0.5 ~ 25min.
6. the preparation method according to claim 4, it is characterised in that: the carbon nanowalls deposition pressure is 600 ~ 800Pa,
The carbon nanowalls deposition power is 15 ~ 18kW, and the carbon nanowalls sedimentation time is 10 ~ 15min.
7. the preparation method according to claim 4, it is characterised in that: the high molecular material and carbon nanowalls Combined Mining
The method impregnated with spin coating or vacuum aided, so that high molecular material enters carbon nanowalls gap.
8. the preparation method according to claim 4, it is characterised in that: the high molecular material is with compressibility
Macromolecular elastomer.
9. the preparation method according to claim 4 or 8, it is characterised in that: the high molecular material be polyurethane (PU),
The combination of one or more of dimethyl silicone polymer (PDMS) or rubber (NR).
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Address after: Room 207, building 8, No.78, Keling Road, hi tech city, Suzhou City, Jiangsu Province, 215000 Applicant after: SUZHOU RENYONGDE IOT TECHNOLOGY Co.,Ltd. Address before: Room 208, Shishan Street Office Building, No. 109 Dengwei Road, Huqiu District, Suzhou City, Jiangsu Province Applicant before: SUZHOU RENYONGDE IOT TECHNOLOGY Co.,Ltd. |
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Application publication date: 20191022 |