CN105018041B - Graphene porous membrane, phase-change energy-storage composite material - Google Patents
Graphene porous membrane, phase-change energy-storage composite material Download PDFInfo
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Abstract
The invention discloses a kind of graphene porous membrane, phase-change energy-storage composite materials, belong to new material technology field；It is intended to provide a kind of phase-change energy-storage composite material that thermal conductivity is high, light-weight, energy storage density is big.Its method is that graphene oxide is prepared into gel, and then releasing thin film-forming method by hygrometric state is made the graphene oxide film containing salt ion；Or the graphene solution containing foaming agent is made in graphene, the graphene film containing blowing-agent particle then is made by spraying method；By above-mentioned graphene oxide film or graphene film graphitization heat treatment, graphene porous membrane is obtained；The graphene porous membrane is immersed in phase-changing energy storage material, until phase-changing energy storage material is filled up completely the micropore of graphene porous membrane.Energy storage density of the present invention is big, thermal conductivity is good, at low cost, light-weight；It is a kind of phase-change accumulation energy heat dissipation composite material can be used for electronic component.
Description
Technical field
The present invention relates to a kind of phase-change energy-storage composite material more particularly to a kind of graphene porous membrane, phase-change accumulation energy are multiple
Condensation material；Belong to new material technology field.
Background technology
That one is thermal conductivitys in face is very high for graphite film, density is light and has high conductivity, the stratiform knot formed by carbon
Structure material.Due to the thickness of graphite film can control at 50 microns hereinafter, and have flexibility, thus have been used as
Heat sink material in small space effectively eliminates heat spot.But with being thinned for graphite film thickness, cause its cross-sectional area
It drastically reduces, therefore heat output also drastically declines.In the electronic device for being covered with graphite film, heat spot heat is difficult to spread
It opens, thus the temperature of device is still excessively high.
It is well known that substance understands energy-absorbing in phase transition process and releases energy；Solid-liquid organic phase change material have become at present most by
The phase-change material pay close attention to, being most widely used.Organic phase change material has energy storage density height, energy storage easy control of temperature, selection
The advantages that range is wide comes into practical and commercialization stage in dissipation from electronic devices field at present.But organic phase change material
The shortcomings of high, easy to aging is required in the presence of easy leakage, encapsulation, is greatly limited their application.On the other hand, lower thermal conductivity is limitation
Another technical bottleneck problem of Organic phase change thermal storage material large-scale promotion application.
The composite material for energy storage that shaping phase-change material is made of phase-change material, macromolecule support and encapsulating material, due to
The micropackaging of macromolecule capsule material and supporting role, the phase-change material as core material will not flow out when solid-liquid phase change occurs, and entire
Composite material can keep original shape invariance after core material fusing, and have certain intensity；Therefore to a certain degree
On improve the performance of phase-change heat-storage material.However, being easy to cause thermal conductivity using organic high molecular polymer cladding phase-change material
Rate reduces, and energy storage efficiency can be greatly affected；Therefore usually that aluminium oxide, magnesia, graphite etc. is equal as heat conduction additive
It is even to be scattered in phase-change material, achieve the purpose that improve heat absorption heat release power by improving phase-change material itself thermal conductivity.This
Although class method can improve the heat absorption speed of phase-change material, with the raising that the thermal diffusivity of device requires, also increases and lead
The addition of hot additive.It can lead to following three problems when loading is larger:（1）Ratio shared by phase-change material declines,
Composite phase-change material enthalpy of phase change declines more；（2）When loading is excessive, since density is larger, long-time service can cause on a small quantity
Phase separation；（3）The quality and cost of material increase more.
Graphene is a kind of new carbon, it have by single layer of carbon atom it is tightly packed made of bi-dimensional cellular shape crystal
Structure is that thickness is minimum in the world, quality is most light, maximum intensity one of substance.In addition, graphene is also equipped with good calorifics
Performance.The study found that graphene thermal coefficient is up to 5000W/m.K, it is 10~100 times of common metal thermal conductivity.Not only such as
This, the two-dimensional structure of graphene is easy to form passage of heat in the base, and has both that density is small, coefficient of thermal expansion is low and corrosion-resistant
The advantages that, it is a kind of ideal filler improving thermal conductivity.If can be using graphene as augmentation of heat transfer carrier, it is likely that overcome
The low disadvantage of single phase transformation material thermal conductivity shortens compound system thermal response time, improves heat exchange efficiency, improves phase transformation composite wood
Expect the radiating efficiency in electronic device heat management.
Invention content
It easily leaked for organic phase change material in the prior art, encapsulate the drawbacks described above such as requirement is high, easy to aging, low-heat is led,
The present invention is intended to provide the graphene porous membrane that a kind of thermal conductivity is high, light-weight, energy storage density is big, phase-change energy-storage composite material.
To achieve the goals above, it is 0.1~2g/cm that the preparation method of composite material of the present invention, which is by relative density,3's
Graphene porous membrane immerses in organic phase change energy storage material, until the organic phase change energy storage material is filled up completely the graphene
The micropore of porous membrane.
The preparation method of graphene porous membrane described in above-mentioned technical proposal is as follows：
1）By single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide
Mixture be prepared into the gel of a concentration of 5~20g/ml；
2）The graphene oxide film that thickness is 1~1000 μm is made in above-mentioned gel in such a way that hygrometric state releases film forming,
Speed to introduce is 1~15cm/min；
3）By above-mentioned graphene oxide film immerse mass concentration be 1~10% salt ion solution in impregnate 1~
100min is pulled out, is dried, and obtains the graphene oxide film containing salt ion；
4）By the above-mentioned graphene oxide film containing salt ion vacuum degree be 1000~5000Pa environment in or air pressure be
1.01x105It is heat-treated in Pa, the inert gas shielding environment that gas flow is 10~500ml/min, then furnace cooling；Heat
Treatment temperature is 1000~3000 DEG C, heating rate is 1~30 DEG C/min.
In the above-mentioned technical solutions, the preferred technical solution of the present invention is：The single-layer graphene oxide thickness be 1.4~
2nm, average diameter are 10~20 μm, the stannic oxide/graphene nano piece that the multilayer graphene oxide is 2~5 layers, and thickness is
0.7~10nm, average diameter are at 10~20 μm.
In the above-mentioned technical solutions, the further optimal technical scheme of the present invention is：The salt ion solution be calcium chloride,
One of sodium chloride, magnesium chloride, metabisulfite solution.
In the above-mentioned technical solutions, the further optimal technical scheme of the present invention is：The heat treatment temperature is 1500
~2500 DEG C.
Graphene porous membrane of the present invention can also use following methods to prepare：
1）Single-layer graphene or the mixture of multi-layer graphene or single-layer graphene and multi-layer graphene are distributed to molten
Form the graphene solution of a concentration of 0.1~5mg/ml in agent, foaming agent be added, ensure graphene solution containing foaming agent 10~
50mg/ml；
2）It is 1~1000 μm, containing foaming that thickness, which is made, in the above-mentioned graphene solution containing foaming agent in the way of spraying
The graphene film of agent particle；
3）By the above-mentioned graphene film containing blowing-agent particle vacuum degree be 1000~5000Pa environment in or air pressure be
1.01x105It is heat-treated in Pa, the inert gas shielding environment that gas flow is 10~500ml/min, then furnace cooling；Heat
Treatment temperature is 1000~3000 DEG C, heating rate is 1~30 DEG C/min.
In the above-mentioned technical solution for preparing graphene porous membrane as raw material using graphene, optimization technique side of the invention
Case is：The single-layer graphene thickness is 0.34~1.4nm, average diameter is 10~20 μm, and the multi-layer graphene is 2~5
The graphene nanometer sheet of layer, thickness are 0.7~10nm, average diameter at 10~20 μm.
In the above-mentioned technical solution for preparing graphene porous membrane as raw material using graphene, the present invention is further preferred
Technical solution is：The foaming agent be azodicarbonamide, azodiisobutyronitrile, OBSH, to one of benzene sulfonyl hydrazide.
In the above-mentioned technical solution for preparing graphene porous membrane as raw material using graphene, the present invention is further excellent
Selecting technology scheme is：The heat treatment temperature is 1500~2500 DEG C.
In above-mentioned each technical solution, the organic phase change energy storage material is one of fatty alcohol, aliphatic acid, paraffin.
Compared with the prior art, the present invention contains by adopting the above-described technical solution, being made as raw material using graphene oxide
The graphene oxide film of salt ion or the graphene film containing blowing-agent particle is made by raw material of graphene, then will contain
The graphene oxide film of salt ion or graphene film containing blowing-agent particle carry out graphitization heat treatment；Can not only it make
Salt ion in graphene oxide film melts distillation or the foaming agent in graphene film is decomposed volatilization, finally obtains
The film of porous structure, and porous membrane can form graphitization after high-temperature process, to improve thermal conductivity.
The present invention stores up phase transformation due to substituting macromolecule capsule material using the graphene porous membrane with good thermal conductivity
Energy material realizes micropackaging, therefore any heat conduction additive need not be added in phase-change material；Thoroughly overcome organic polymer
Composite material phase-change material accounting is caused to reduce because heat conduction additive is excessively added when polymer overmold phase-change material, enthalpy of phase change
Decline many defects such as more, density increases, easy tos produce phase separation, material cost rises.The present invention have energy storage density it is high,
The advantages that thermal conductivity is good, at low cost, light-weight；It can be used as the heat sink material of electronic component.
Description of the drawings
Fig. 1 is the graphene porous membrane SEM pictures prepared as raw material using graphene oxide；
Fig. 2 is the graphene porous membrane SEM pictures prepared as raw material using graphene；
Fig. 3 is the side SEM pictures of composite material of the present invention.
Specific implementation mode
With reference to specific embodiment, the invention will be further described：
Graphene porous membrane, phase-change energy-storage composite material are prepared with graphene oxide：
Embodiment 1
1）By single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide
Mixture be prepared into the gel of a concentration of 5g/ml；
2）The graphene oxide film that thickness is 1000 μm is made in above-mentioned gel in such a way that hygrometric state releases film forming, is released
Speed is 1cm/min；
3）Above-mentioned graphene oxide film is immersed in the salt ion solution that mass concentration is 10% and impregnates 1min, pulls out, dry in the air
It is dry, obtain the graphene oxide film containing salt ion；Salt ion solution is sodium chloride solution；
4）By the above-mentioned graphene oxide film containing salt ion be placed in vacuum degree be 5000Pa heating furnace in, by 1 DEG C/
The rate of min is warming up to 3000 DEG C, and it is 0.1~2g/cm that furnace cooling, which obtains relative density,3Graphene porous membrane；
5）Above-mentioned graphene porous membrane is immersed in organic phase change energy storage material, until the organic phase change energy storage material is complete
The micropore of graphene porous membrane described in full packing.
Embodiment 2, each step is the same as embodiment 1；Wherein：
Step 1）In gel strength be 20g/ml, step 2）In graphene oxide film thickness be 1 μm, speed to introduce
For 15cm/min, step 3）In salt ion solution be 1% magnesium chloride solution, soaking time 100min, step 4）Middle heating
Stove vacuum degree is 1000Pa, heating rate is 30 DEG C/min, target temperature is 1000 DEG C.
Embodiment 3, each step is the same as embodiment 1；Wherein：
Step 1）In gel strength be 12g/ml, step 2）In graphene oxide film thickness be 500 μm, release speed
Degree is 8cm/min, step 3）In salt ion solution be 5% metabisulfite solution, soaking time 50min, step 4）Middle heating
Stove vacuum degree is 3000Pa, heating rate is 15 DEG C/min, target temperature is 2000 DEG C.
Embodiment 4, each step is the same as embodiment 1；Wherein：
Step 3）In salt ion solution be 5% calcium chloride solution, soaking time 20min, step 4）Middle heating furnace is true
Reciprocal of duty cycle is 2000Pa, heating rate is 20 DEG C/min, target temperature is 1500 DEG C.
Embodiment 5, each step is the same as embodiment 1；Wherein：
Step 3）In salt ion solution be 8% calcium chloride solution, soaking time 10min, step 4）Middle heating furnace is true
Reciprocal of duty cycle is 4000Pa, heating rate is 10 DEG C/min, target temperature is 2500 DEG C.
Embodiment 6, each step is the same as embodiment 1；Wherein：
Step 1）In gel strength be 5mg/ml, step 2）In graphene oxide film thickness be 10um, release speed
Degree is 5cm/min, step 3）In salt ion solution be 10% calcium chloride solution, soaking time 20min, step 4）Plus
Argon gas is injected by the flow of 10ml/min in hot stove, the air pressure in heating furnace is 1.01x105Pa, heating rate be 10 DEG C/min,
Target temperature is 2200 DEG C.
Embodiment 7, each step is the same as embodiment 1；Wherein：
Step 1）In gel strength be 10mg/ml, step 2）In graphene oxide film thickness be 50um, release speed
Degree is 10cm/min, step 3）In salt ion solution be 5% calcium chloride solution, soaking time 20min, step 4）Plus
Argon gas is injected by the flow of 500ml/min in hot stove, the air pressure in heating furnace is 1.01x105Pa, heating rate be 10 DEG C/
Min, target temperature are 2200 DEG C.
Embodiment 8, each step is the same as embodiment 1；Wherein：
Step 1）In gel strength be 20mg/ml, step 2）In graphene oxide film thickness be, thickness is
200um, speed to introduce 15cm/min, step 3）In salt ion solution be 5% metabisulfite solution, soaking time be
30min, step 4）Middle heating furnace vacuum degree is 1000Pa, target temperature is 2800 DEG C.
In the above embodiments, the single-layer graphene oxide thickness is 1.4~2nm, average diameter is 10~20 μm,
It is 0.7~10nm, average diameter 10 that the multilayer graphene oxide, which selects 2~5 layers of stannic oxide/graphene nano piece, thickness,
~20 μm.The organic phase change energy storage material is one of fatty alcohol, aliphatic acid, paraffin.
Graphene porous membrane, phase-change energy-storage composite material are prepared with graphene oxide：
Embodiment 9
1）Single-layer graphene or the mixture of multi-layer graphene or single-layer graphene and multi-layer graphene are distributed to molten
The graphene solution of a concentration of 0.1mg/ml is formed in agent, foaming agent is added, and ensures graphene solution 50mg/ml containing foaming agent；
Foaming agent is azodicarbonamide；
2）Thickness is made in the above-mentioned graphene solution containing foaming agent to be 1 μm, contain blowing-agent particle in the way of spraying
Graphene film；
3）By the above-mentioned graphene film containing blowing-agent particle be placed in vacuum degree be 5000Pa heating furnace in, by 1 DEG C/
The rate of min is warming up to 3000 DEG C, and it is 0.1~2g/cm that furnace cooling, which obtains relative density,3Graphene porous membrane；
4）Above-mentioned graphene porous membrane is immersed in organic phase change energy storage material, until the organic phase change energy storage material is complete
The micropore of graphene porous membrane described in full packing.
Embodiment 10, each step embodiment 9；Wherein：
Step 1）In a concentration of 5mg/ml of graphene solution, wherein 10mg/ml containing foaming agent, foaming agent is that azo two is different
Butyronitrile；Step 2）In graphene film thickness be 1000 μm, step 3）Middle heating furnace vacuum degree is 1000Pa, heating rate is
30 DEG C/min, target temperature be 1000 DEG C.
Embodiment 11, each step embodiment 9；Wherein：
Step 1）In graphene solution a concentration of 2.5mg/ml, wherein 30mg/ml containing foaming agent, foaming agent OBSH；
Step 2）In graphene film thickness be 500 μm, step 3）The vacuum degree of middle heating furnace is 3000Pa, heating rate 15
DEG C/min, target temperature be 2000 DEG C.
Embodiment 12, each step embodiment 9；Wherein：
Step 1）In foaming agent be to benzene sulfonyl hydrazide, graphene solution 20mg/ml containing foaming agent, step 3）Middle heating furnace
Vacuum degree is 4000Pa, heating rate is 20 DEG C/min, target temperature is 1500 DEG C.
Embodiment 13, each step embodiment 9；Wherein：
Step 1）In foaming agent be OBSH, graphene solution 40mg/ml containing foaming agent, step 3）Middle heating furnace vacuum degree
It is 10 DEG C/min for 2000Pa, heating rate, target temperature is 2500 DEG C.
Embodiment 14, each step is the same as embodiment 9；Wherein：
Step 1）In graphene solution 10mg/ml containing foaming agent, foaming agent OBSH；Step 2）Graphene film thickness
It is 50 μm, step 3）Argon gas is injected by the flow of 100ml/min in heating furnace, the air pressure in heating furnace is 1.01x105Pa rises
Warm rate is 10 DEG C/min, target temperature is 2800 DEG C.
Embodiment 15, each step is the same as embodiment 9；Wherein：
Step 1）In a concentration of 1mg/ml of graphene solution, wherein 15mg/ml containing foaming agent, foaming agent OBSH；Step
Rapid 2）Graphene film thickness is 100 μm, step 3）Middle heating furnace vacuum degree is 1000Pa, heating rate is 10 DEG C/min, mesh
It is 2800 DEG C to mark temperature.
Embodiment 16, each step is the same as embodiment 9；Wherein：
Step 1）In a concentration of 5mg/ml of graphene solution, wherein 50mg/ml containing foaming agent, foaming agent is azo diformazan
Amide；Step 2）Graphene film thickness is 200 μm, step 3）In heating furnace argon gas, heating are injected by the flow of 100ml/min
Air pressure in stove is 1.01x105Pa, heating rate is 10 DEG C/min, target temperature is 2800 DEG C.
In the above embodiments, the single-layer graphene thickness is 0.34~1.4nm, average diameter is 10~20
μm, the graphene nanometer sheet that the multi-layer graphene is 2~5 layers, thickness is 0.7~10nm, average diameter at 10~20 μm.
The organic phase change energy storage material is one of fatty alcohol, aliphatic acid, paraffin.
Table 1 is to immerse the graphene porous membrane prepared by above-mentioned section Example in the paraffin melted, waits for that paraffin is complete
Full packing enters in the micropore of graphene porous membrane and forms the thermal conductivity data tested at room temperature after composite material of the present invention：
Table 1：Section Example properties of sample is tested
| Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 14 | Embodiment 15 | Embodiment 16 | |
| Enthalpy of phase change（J/g） | 181.5 | 162.3 | 140.2 | 170.5 | 175.3 | 165.9 |
| Density（g/cm3） | 1.51 | 1.76 | 1.83 | 1.62 | 1.59 | 1.65 |
| Thermal conductivity（W/mk） | 95.3 | 120.3 | 140.8 | 110.6 | 109.6 | 115.3 |
In addition, being observed that from Fig. 1, Fig. 2：Graphene porous membrane prepared by the present invention has abundant poroid knot
Structure can provide more spaces and contact interface for the filling of organic phase change energy storage material；From Fig. 3 it is observed that：Graphene
Porous membrane can fully absorb paraffin and form composite material of the present invention.
Claims (9)
1. a kind of graphene porous membrane, phase-change energy-storage composite material, it is characterised in that preparation method is：It is by relative density
0.1~2g/cm3Graphene oxide porous membrane immerse in organic phase change energy storage material, until the organic phase change energy storage material
It is filled up completely the micropore of the graphene oxide porous membrane；Wherein, the graphene oxide porous membrane preparation method is as follows：
1) by the mixed of single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide
Close the gel that object is prepared into a concentration of 5~20g/ml；
2) the graphene oxide porous membrane that thickness is 1~1000 μm is made in above-mentioned gel in such a way that hygrometric state releases film forming,
Speed to introduce is 1~15cm/min；
3) by above-mentioned graphene oxide porous membrane immerse mass concentration be 1~10% salt ion solution in impregnate 1~
100min is pulled out, is dried, and obtains the graphene oxide porous membrane containing salt ion；
4) it is in 1000~5000Pa environment or air pressure that by above-mentioned, the graphene oxide porous membrane containing salt ion, which is placed in vacuum degree,
For 1.01x105It is heat-treated in Pa, the inert gas shielding environment that gas flow is 10~500ml/min, then furnace cooling；
Heat treatment temperature is 1000~3000 DEG C, heating rate is 1~30 DEG C/min.
2. graphene porous membrane according to claim 1, phase-change energy-storage composite material, it is characterised in that：The single layer
Graphene oxide thickness is 1.4~2nm, average diameter is 10~20 μm, the oxidation that the multilayer graphene oxide is 2~5 layers
Graphene nanometer sheet, thickness are 0.7~10nm, average diameter at 10~20 μm.
3. graphene porous membrane according to claim 1, phase-change energy-storage composite material, it is characterised in that：The salt from
Sub- solution is one of calcium chloride, sodium chloride, magnesium chloride, metabisulfite solution.
4. graphene porous membrane according to claim 1, phase-change energy-storage composite material, it is characterised in that：At the heat
It is 1500~2500 DEG C to manage temperature.
5. a kind of graphene porous membrane, phase-change energy-storage composite material, it is characterised in that preparation method is：It is by relative density
0.1~2g/cm3Graphene porous membrane immerse in organic phase change energy storage material, until the organic phase change energy storage material is complete
Fill the micropore of the graphene porous membrane；Wherein, the graphene porous membrane preparation method is as follows：
1) single-layer graphene or the mixture of multi-layer graphene or single-layer graphene and multi-layer graphene are distributed in solvent
The graphene solution of a concentration of 0.1~5mg/ml is formed, foaming agent is added, ensures graphene solution 10~50mg/ containing foaming agent
ml；
2) thickness is made in the above-mentioned graphene solution containing foaming agent to be 1~1000 μm, contain foaming agent in the way of spraying
The graphene film of grain；
3) by the above-mentioned graphene film containing blowing-agent particle be placed in vacuum degree be 1000~5000Pa environment in or air pressure be
1.01x105It is heat-treated in Pa, the inert gas shielding environment that gas flow is 10~500ml/min, then furnace cooling；Heat
Treatment temperature is 1000~3000 DEG C, heating rate is 1~30 DEG C/min.
6. graphene porous membrane according to claim 5, phase-change energy-storage composite material, it is characterised in that：The single layer
Graphene thickness is 0.34~1.4nm, average diameter is 10~20 μm, the graphene nano that the multi-layer graphene is 2~5 layers
Piece, thickness are 0.7~10nm, average diameter at 10~20 μm.
7. graphene porous membrane according to claim 5, phase-change energy-storage composite material, it is characterised in that：The foaming
Agent be azodicarbonamide, azodiisobutyronitrile, OBSH, to one of benzene sulfonyl hydrazide.
8. graphene porous membrane according to claim 5, phase-change energy-storage composite material, it is characterised in that：At the heat
It is 1500~2500 DEG C to manage temperature.
9. graphene porous membrane, phase-change energy-storage composite material according to any one of claim 1~8, feature
It is：The organic phase change energy storage material is one of fatty alcohol, aliphatic acid, paraffin.
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