CN105018041A - Porous graphene film, and phase-changing energy-storing composite material - Google Patents
Porous graphene film, and phase-changing energy-storing composite material Download PDFInfo
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Abstract
The present invention discloses a porous graphene film and a phase-changing energy-storing composite material, and belongs to the technical field of new materials. The invention aims to provide a phase-changing energy-storing composite material that is high in thermal conductivity, light in weight, and high in energy-storing density. The method comprises: preparing a gel by using a graphene oxide, and then producing a graphene oxide film containing salt ions by using a wet state film forming method; or producing a graphene solution containing a blowing agent by using graphene, and then producing a graphene film containing blowing agent granule in a spraying manner; performing a heat treatment for graphitization on the graphene oxide film and the graphene film to obtain the porous graphene film; and immersing the porous graphene film into a phase-changing energy-storing material until pores of the porous graphene film are fully filled with the phase-changing energy-storing material. The porous graphene film and the phase-changing energy-storing composite material is high in energy density, good in thermal conductivity, low in cost and light in weight. The phase-changing energy-storing composite material is a phase-changing energy-storing heat dissipating composite material that can be applied to an electronic component.
Description
Technical field
The present invention relates to a kind of phase-change energy-storage composite material, particularly relate to a kind of Graphene porous membrane, phase-change energy-storage composite material; Belong to new material technology field.
Background technology
Graphite film one is that in face, thermal conductivity is very high, density light and has high conductivity, the layer structure material formed by carbon.Because the thickness of graphite film can control below 50 microns, and have flexibility, thus the heat sink material be always used as in small space effectively eliminates hot spot.But thinning along with graphite film thickness, cause its cross-sectional area and sharply reduce, therefore heat transfer capacity also sharply declines.In the electron device being coated with graphite film, hot spot heat is difficult to spread apart, and thus the temperature of device is still too high.
As everyone knows, material is understood energy-absorbing and is released energy in phase transition process; Solid-liquid organic phase change material has become phase change material that is of greatest concern, that be most widely used at present.Organic phase change material has the advantages such as energy storage density is high, energy storage easy control of temperature, range of choice are wide, has entered practical and commercialization stage at present in dissipation from electronic devices field.But organic phase change material exist easily leak, encapsulation requires high, the easy shortcoming such as aging, significantly limit its application.On the other hand, lower thermal conductivity is the another one technical bottleneck problem of restriction Organic phase change thermal storage material large-scale promotion application.
The composite material for energy storage that shaping phase-change material is made up of phase change material, polymer support and packaged material, due to micropackaging and the supporting role of high score ascus material, can not flow out during phase change material generation solid-liquid phase change as core, even and if whole matrix material also can keep original shape invariance after core fusing, and have certain intensity; Therefore the performance of phase-change heat-storage material is improved to a certain extent.But adopt organic high molecular polymer coated phase-change material easily to cause thermal conductivity to reduce, energy storage efficiency can be greatly affected; Therefore usual aluminum oxide, magnesium oxide, graphite etc. being dispersed in phase change material as heat conduction additive, reaching by improving phase change material self thermal conductivity the object improving heat absorption heat release power.Although these class methods can improve the heat absorption speed of phase change material, the raising that the thermal diffusivity along with device requires, too increases the add-on of heat conduction additive.Can cause following three problems when loading level is larger: the ratio shared by (1) phase change material declines, composite phase-change material enthalpy of phase change declines more; (2) when loading level is too much, because density is comparatively large, life-time service can cause a small amount of being separated; (3) quality of material and cost increase more.
Graphene is a kind of new carbon, and it has by the tightly packed bi-dimensional cellular shape crystalline structure of monolayer carbon atom, is one of material that thickness is minimum, quality is the lightest, intensity is maximum in the world.In addition, Graphene also possesses good thermal property.Research finds, Graphene thermal conductivity, up to 5000W/m.K, is 10 ~ 100 times of plain metal thermal conductivity.Moreover, the two-dirnentional structure of Graphene easily forms passage of heat in the base, and has that density is little, thermal expansivity is low concurrently and the advantage such as corrosion-resistant, is a kind of desirable weighting material improving thermal conductivity.If using Graphene as enhancement of heat transfer carrier, then can likely overcome the shortcoming that single phase transformation material thermal conductivity is low, shorten compound system thermal response time, improve heat exchange efficiency, improve the radiating efficiency of phase change composite material in electron device heat management.
Summary of the invention
Easily leak for organic phase change material in prior art, encapsulate and require high, the easy above-mentioned defect such as aging, low thermal conductance, the present invention aims to provide Graphene porous membrane, the phase-change energy-storage composite material that a kind of thermal conductance is high, lightweight, energy storage density is large.
To achieve these goals, the preparation method of matrix material of the present invention is 0.1 ~ 2g/cm by relative density
3graphene porous membrane immerse in organic phase change energy storage material, until this organic phase change energy storage material fills the micropore of described Graphene porous membrane completely.
Preparation method is as follows for the porous membrane of Graphene described in technique scheme:
1) mixture of single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide is prepared into the gel that concentration is 5 ~ 20g/ml;
2) by the mode of hygrometric state release film forming, above-mentioned gel is made the graphene oxide film that thickness is 1 ~ 1000 μm, speed to introduce is 1 ~ 15cm/min;
3) above-mentioned graphene oxide film being immersed mass concentration is soak 1 ~ 100min in the salt ion solution of 1 ~ 10%, pulls out, dries, must containing the graphene oxide film of salt ion;
4) be in 1000 ~ 5000Pa environment by the above-mentioned graphene oxide film containing salt ion in vacuum tightness, or air pressure is 1.01x10
5pa, gas flow are thermal treatment, then furnace cooling in the protection of inert gas environment of 10 ~ 500ml/min; Thermal treatment temp is 1000 ~ 3000 DEG C, temperature rise rate is 1 ~ 30 DEG C/min.
In technique scheme, the preferred technical solution of the present invention is: described single-layer graphene oxide thickness is 1.4 ~ 2nm, mean diameter is 10 ~ 20 μm, described multilayer graphene oxide is the stannic oxide/graphene nano sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.
In technique scheme, the further optimal technical scheme of the present invention is: described salt ion solution is one of calcium chloride, sodium-chlor, magnesium chloride, metabisulfite solution.
In technique scheme, the present invention further optimal technical scheme is: described thermal treatment temp is 1500 ~ 2500 DEG C.
Graphene porous membrane of the present invention can also adopt following methods to prepare:
1) mixture of single-layer graphene or multi-layer graphene or single-layer graphene and multi-layer graphene is distributed in solvent forms the graphene solution that concentration is 0.1 ~ 5mg/ml, add whipping agent, ensure that graphene solution is containing whipping agent 10 ~ 50mg/ml;
2) the above-mentioned graphene solution containing whipping agent is made by the mode of spraying thickness is 1 ~ 1000 μm, graphene film containing blowing-agent particle;
3) be in 1000 ~ 5000Pa environment by the above-mentioned graphene film containing blowing-agent particle in vacuum tightness, or air pressure is 1.01x10
5pa, gas flow are thermal treatment, then furnace cooling in the protection of inert gas environment of 10 ~ 500ml/min; Thermal treatment temp is 1000 ~ 3000 DEG C, temperature rise rate is 1 ~ 30 DEG C/min.
Above-mentioned be that raw material is prepared in the technical scheme of Graphene porous membrane with Graphene, the preferred technical solution of the present invention is: described single-layer graphene thickness is 0.34 ~ 1.4nm, mean diameter is 10 ~ 20 μm, described multi-layer graphene is the graphene nanometer sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.
Above-mentioned be that raw material is prepared in the technical scheme of Graphene porous membrane with Graphene, the further optimal technical scheme of the present invention is: described whipping agent be Cellmic C 121, Diisopropyl azodicarboxylate, OBSH, to one of benzol sulfohydrazide.
Above-mentioned be that raw material is prepared in the technical scheme of Graphene porous membrane with Graphene, the present invention further optimal technical scheme is: described thermal treatment temp is 1500 ~ 2500 DEG C.
In above-mentioned each technical scheme, described organic phase change energy storage material is one of fatty alcohol, lipid acid, paraffin.
Compared with the prior art, the present invention is owing to have employed technique scheme, be that raw material is made containing the graphene oxide film of salt ion or is the graphene film that raw material makes containing blowing-agent particle with Graphene with graphene oxide, then greying thermal treatment will be carried out containing the graphene oxide film of salt ion or containing the graphene film of blowing-agent particle; The salt ion in graphene oxide film not only can be made to melt distillation or the whipping agent in graphene film is decomposed volatilization, finally obtain the film of vesicular structure, and porous membrane can form greying after pyroprocessing, thus improve thermal conductivity.
The present invention realizes micropackaging owing to adopting the Graphene porous membrane with good thermal conductivity to substitute high score ascus material to phase-changing energy storage material, therefore need not add any heat conduction additive in phase change material; Many defects such as matrix material phase change material accounting reduces, enthalpy of phase change decline is more, density increases, easy generation is separated, material cost rising are caused because of excessive interpolation heat conduction additive when thoroughly overcoming organic high molecular polymer coated phase-change material.The present invention has the advantages such as energy storage density is high, thermal conductivity good, cost is low, lightweight; Can be used as the heat sink material of electronic devices and components.
Accompanying drawing explanation
Fig. 1 take graphene oxide as Graphene porous membrane SEM picture prepared by raw material;
Fig. 2 take Graphene as Graphene porous membrane SEM picture prepared by raw material;
Fig. 3 is the side SEM picture of matrix material of the present invention.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Graphene porous membrane, phase-change energy-storage composite material is prepared with graphene oxide:
Embodiment 1
1) mixture of single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide is prepared into the gel that concentration is 5g/ml;
2) by the mode of hygrometric state release film forming, above-mentioned gel is made the graphene oxide film that thickness is 1000 μm, speed to introduce is 1cm/min;
3) above-mentioned graphene oxide film being immersed mass concentration is soak 1min in the salt ion solution of 10%, pulls out, dries, must containing the graphene oxide film of salt ion; Salt ion solution is sodium chloride solution;
4) the above-mentioned graphene oxide film containing salt ion is placed in the process furnace that vacuum tightness is 5000Pa, by the ramp to 3000 DEG C of 1 DEG C/min, it is 0.1 ~ 2g/cm that furnace cooling obtains relative density
3graphene porous membrane;
5) above-mentioned Graphene porous membrane is immersed in organic phase change energy storage material, until this organic phase change energy storage material fills the micropore of described Graphene porous membrane completely.
Embodiment 2, each step is with embodiment 1; Wherein:
Gel strength in step 1) is 20g/ml, step 2) in graphene oxide film thickness be 1 μm, speed to introduce is 15cm/min, salt ion solution in step 3) be 1% magnesium chloride solution, soak time be 100min, in step 4), process furnace vacuum tightness is 1000Pa, temperature rise rate is 30 DEG C/min, target temperature is 1000 DEG C.
Embodiment 3, each step is with embodiment 1; Wherein:
Gel strength in step 1) is 12g/ml, step 2) in graphene oxide film thickness be 500 μm, speed to introduce is 8cm/min, salt ion solution in step 3) be 5% metabisulfite solution, soak time be 50min, in step 4), process furnace vacuum tightness is 3000Pa, temperature rise rate is 15 DEG C/min, target temperature is 2000 DEG C.
Embodiment 4, each step is with embodiment 1; Wherein:
Salt ion solution in step 3) be 5% calcium chloride solution, soak time be 20min, in step 4), process furnace vacuum tightness is 2000Pa, temperature rise rate is 20 DEG C/min, target temperature is 1500 DEG C.
Embodiment 5, each step is with embodiment 1; Wherein:
Salt ion solution in step 3) be 8% calcium chloride solution, soak time be 10min, in step 4), process furnace vacuum tightness is 4000Pa, temperature rise rate is 10 DEG C/min, target temperature is 2500 DEG C.
Embodiment 6, each step is with embodiment 1; Wherein:
Gel strength in step 1) is 5mg/ml, step 2) in graphene oxide film thickness be 10um, speed to introduce is 5cm/min, salt ion solution in step 3) be 10% calcium chloride solution, soak time be 20min, the flow pressing 10ml/min in the process furnace of step 4) injects argon gas, and the air pressure in process furnace is 1.01x10
5pa, temperature rise rate is 10 DEG C/min, target temperature is 2200 DEG C.
Embodiment 7, each step is with embodiment 1; Wherein:
Gel strength in step 1) is 10mg/ml, step 2) in graphene oxide film thickness be 50um, speed to introduce is 10cm/min, salt ion solution in step 3) be 5% calcium chloride solution, soak time be 20min, the flow pressing 500ml/min in the process furnace of step 4) injects argon gas, and the air pressure in process furnace is 1.01x10
5pa, temperature rise rate is 10 DEG C/min, target temperature is 2200 DEG C.
Embodiment 8, each step is with embodiment 1; Wherein:
Gel strength in step 1) is 20mg/ml, step 2) in graphene oxide film thickness for, thickness be 200um, speed to introduce is 15cm/min, salt ion solution in step 3) be 5% metabisulfite solution, soak time be 30min, in step 4), process furnace vacuum tightness is 1000Pa, target temperature is 2800 DEG C.
In the various embodiments described above, described single-layer graphene oxide thickness is 1.4 ~ 2nm, mean diameter is 10 ~ 20 μm, and described multilayer graphene oxide selects the stannic oxide/graphene nano sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.Described organic phase change energy storage material is one of fatty alcohol, lipid acid, paraffin.
Graphene porous membrane, phase-change energy-storage composite material is prepared with graphene oxide:
Embodiment 9
1) mixture of single-layer graphene or multi-layer graphene or single-layer graphene and multi-layer graphene is distributed in solvent forms graphene solution that concentration is 0.1mg/ml, add whipping agent, ensure that graphene solution is containing whipping agent 50mg/ml; Whipping agent is Cellmic C 121;
2) the above-mentioned graphene solution containing whipping agent is made by the mode of spraying thickness is 1 μm, graphene film containing blowing-agent particle;
3) the above-mentioned graphene film containing blowing-agent particle is placed in the process furnace that vacuum tightness is 5000Pa, by the ramp to 3000 DEG C of 1 DEG C/min, it is 0.1 ~ 2g/cm that furnace cooling obtains relative density
3graphene porous membrane;
4) above-mentioned Graphene porous membrane is immersed in organic phase change energy storage material, until this organic phase change energy storage material fills the micropore of described Graphene porous membrane completely.
Embodiment 10, each step embodiment 9; Wherein:
Graphene solution concentration in step 1) is 5mg/ml, and wherein containing whipping agent 10mg/ml, whipping agent is Diisopropyl azodicarboxylate; Step 2) in graphene film thickness be 1000 μm, in step 3), process furnace vacuum tightness is 1000Pa, temperature rise rate is 30 DEG C/min, target temperature is 1000 DEG C.
Embodiment 11, each step embodiment 9; Wherein:
Graphene solution concentration in step 1) is 2.5mg/ml, wherein containing whipping agent 30mg/ml, whipping agent is OBSH; Step 2) in graphene film thickness be 500 μm, in step 3), the vacuum tightness of process furnace is 3000Pa, temperature rise rate is 15 DEG C/min, target temperature is 2000 DEG C.
Embodiment 12, each step embodiment 9; Wherein:
Whipping agent in step 1) is to benzol sulfohydrazide, graphene solution containing whipping agent 20mg/ml, and in step 3), process furnace vacuum tightness is 4000Pa, temperature rise rate is 20 DEG C/min, target temperature is 1500 DEG C.
Embodiment 13, each step embodiment 9; Wherein:
Whipping agent in step 1) be OBSH, graphene solution containing whipping agent 40mg/ml, in step 3), process furnace vacuum tightness is 2000Pa, temperature rise rate is 10 DEG C/min, target temperature is 2500 DEG C.
Embodiment 14, each step is with embodiment 9; Wherein:
Graphene solution in step 1) is containing whipping agent 10mg/ml, and whipping agent is OBSH; Step 2) graphene film thickness is 50 μm, the flow pressing 100ml/min in step 3) process furnace injects argon gas, and the air pressure in process furnace is 1.01x10
5pa, temperature rise rate is 10 DEG C/min, target temperature is 2800 DEG C.
Embodiment 15, each step is with embodiment 9; Wherein:
Graphene solution concentration in step 1) is 1mg/ml, and wherein containing whipping agent 15mg/ml, whipping agent is OBSH; Step 2) graphene film thickness is 100 μm, in step 3), process furnace vacuum tightness is 1000Pa, temperature rise rate is 10 DEG C/min, target temperature is 2800 DEG C.
Embodiment 16, each step is with embodiment 9; Wherein:
Graphene solution concentration in step 1) is 5mg/ml, and wherein containing whipping agent 50mg/ml, whipping agent is Cellmic C 121; Step 2) graphene film thickness is 200 μm, the flow pressing 100ml/min in step 3) process furnace injects argon gas, and the air pressure in process furnace is 1.01x10
5pa, temperature rise rate is 10 DEG C/min, target temperature is 2800 DEG C.
In the various embodiments described above, described single-layer graphene thickness is 0.34 ~ 1.4nm, mean diameter is 10 ~ 20 μm, and described multi-layer graphene is the graphene nanometer sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.Described organic phase change energy storage material is one of fatty alcohol, lipid acid, paraffin.
Table 1 is immersed in the paraffin melted by the Graphene porous membrane prepared by above-mentioned section Example, is packed into the thermal conductivity data of at room temperature testing after forming matrix material of the present invention in the micropore of Graphene porous membrane completely until paraffin:
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/cm 3） | 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, can observe from Fig. 1, Fig. 2: Graphene porous membrane prepared by the present invention has abundant cavernous structure, the filling that can be organic phase change energy storage material provides more space and contact interface; Can observe from Fig. 3: Graphene porous membrane fully can absorb paraffin and form matrix material of the present invention.
Claims (10)
1. Graphene porous membrane, a phase-change energy-storage composite material, is characterized in that preparation method is: be 0.1 ~ 2g/cm by relative density
3graphene porous membrane immerse in organic phase change energy storage material, until this organic phase change energy storage material fills the micropore of described Graphene porous membrane completely.
2. Graphene porous membrane according to claim 1, phase-change energy-storage composite material, is characterized in that Graphene porous membrane preparation method is as follows:
1) mixture of single-layer graphene oxide or multilayer graphene oxide or single-layer graphene oxide and multilayer graphene oxide is prepared into the gel that concentration is 5 ~ 20g/ml;
2) by the mode of hygrometric state release film forming, above-mentioned gel is made the graphene oxide film that thickness is 1 ~ 1000 μm, speed to introduce is 1 ~ 15cm/min;
3) above-mentioned graphene oxide film being immersed mass concentration is soak 1 ~ 100min in the salt ion solution of 1 ~ 10%, pulls out, dries, must containing the graphene oxide film of salt ion;
4) the above-mentioned graphene oxide film containing salt ion being placed in vacuum tightness is 1000 ~ 5000Pa environment, or air pressure is 1.01x10
5pa, gas flow are thermal treatment, then furnace cooling in the protection of inert gas environment of 10 ~ 500ml/min; Thermal treatment temp is 1000 ~ 3000 DEG C, temperature rise rate is 1 ~ 30 DEG C/min.
3. Graphene porous membrane according to claim 2, phase-change energy-storage composite material, it is characterized in that: described single-layer graphene oxide thickness is 1.4 ~ 2nm, mean diameter is 10 ~ 20 μm, described multilayer graphene oxide is the stannic oxide/graphene nano sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.
4. Graphene porous membrane according to claim 2, phase-change energy-storage composite material, is characterized in that: described salt ion solution is one of calcium chloride, sodium-chlor, magnesium chloride, metabisulfite solution.
5. Graphene porous membrane according to claim 2, phase-change energy-storage composite material, is characterized in that: described thermal treatment temp is 1500 ~ 2500 DEG C.
6. Graphene porous membrane according to claim 1, phase-change energy-storage composite material, is characterized in that Graphene porous membrane preparation method is as follows:
1) mixture of single-layer graphene or multi-layer graphene or single-layer graphene and multi-layer graphene is distributed in solvent forms the graphene solution that concentration is 0.1 ~ 5mg/ml, add whipping agent, ensure that graphene solution is containing whipping agent 10 ~ 50mg/ml;
2) the above-mentioned graphene solution containing whipping agent is made by the mode of spraying thickness is 1 ~ 1000 μm, graphene film containing blowing-agent particle;
3) the above-mentioned graphene film containing blowing-agent particle being placed in vacuum tightness is 1000 ~ 5000Pa environment, or air pressure is 1.01x10
5pa, gas flow are thermal treatment, then furnace cooling in the protection of inert gas environment of 10 ~ 500ml/min; Thermal treatment temp is 1000 ~ 3000 DEG C, temperature rise rate is 1 ~ 30 DEG C/min.
7. Graphene porous membrane according to claim 6, phase-change energy-storage composite material, it is characterized in that: described single-layer graphene thickness is 0.34 ~ 1.4nm, mean diameter is 10 ~ 20 μm, described multi-layer graphene is the graphene nanometer sheet of 2 ~ 5 layers, and its thickness is that 0.7 ~ 10nm, mean diameter are at 10 ~ 20 μm.
8. Graphene porous membrane according to claim 6, phase-change energy-storage composite material, is characterized in that: described whipping agent be Cellmic C 121, Diisopropyl azodicarboxylate, OBSH, to one of benzol sulfohydrazide.
9. Graphene porous membrane according to claim 6, phase-change energy-storage composite material, is characterized in that: described thermal treatment temp is 1500 ~ 2500 DEG C.
10. according to Graphene porous membrane, the phase-change energy-storage composite material in claim 1 ~ 9 described in any one, it is characterized in that: described organic phase change energy storage material is one of fatty alcohol, lipid acid, paraffin.
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