CN101343529B - Method for preparing composite phase-changing material - Google Patents
Method for preparing composite phase-changing material Download PDFInfo
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- CN101343529B CN101343529B CN2007100121025A CN200710012102A CN101343529B CN 101343529 B CN101343529 B CN 101343529B CN 2007100121025 A CN2007100121025 A CN 2007100121025A CN 200710012102 A CN200710012102 A CN 200710012102A CN 101343529 B CN101343529 B CN 101343529B
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Abstract
The invention relates to a preparation method of the phase change material, in particular to a preparation method of the compound phase change material which has a higher latent heat of phase change and a high thermal conductivity under the solid and the liquid states. The preparation steps are as follows: firstly, metal nanowires are prepared; secondly, the metal nanowires are dispersed into an organic solvent; thirdly, an organic phase change material and the mixture are mixed; fourthly, the mixture is dispersed by ultrasonic under the condition of heating, and the organic solvent is removed. The phase change material prepared by the method has the advantages that the art is simple, the cost is low, and the thermal conductivity of the organic phase change material is enhanced greatly while the latent heat of phase change is maintained, thus the performance of the organic phase change material is improved effectively, and the application scope is greatly developed.
Description
Technical field
The present invention relates to the preparation of phase change material, a kind of specifically have higher latent heat of phase change, and all have the very preparation method of high thermal conductivity coefficient composite phase-change material under solid and liquid state.
Background technology
The energy is the basis of human survival and social development, and at present the utilizable energy of people can be divided into two classes: conventional energy resources and renewable energy source, and wherein conventional energy resources just fossil energy accounted for the overwhelming majority of the human used energy.Along with development of human society, people to the demand of the energy also in quick growth.Energy dilemma has become one of main factor of restriction social development.So people invest energy-conservation and renewable energy source domain to sight one after another.The storage of heat energy is exactly one of them importance.And phase change material has also caused people's extensive interest as the basic substance of thermal energy storage.Produce and life in many energy, as the valley period power of sun power, industrial exhaust heat, industrial waste heat and electrical network can etc., all exist a time difference between the supply and demand.Use phase change material these energy can be stored earlier, and then stable supply is used in needs.Under many circumstances, our release rate of the energy that will store is very fast.This just requires our employed phase change material will have the high capacity of heat transmission to improve the storage speed of heat energy.But all very low just because of the capacity of heat transmission that is suitable for as the organic substance of phase change material, therefore limited their application to a great extent.
Along with the fast development of microelectronics industry, electron device is miniaturization and high-power day by day.This just requires a large amount of heats of transferred-electron device generation in time.At present main adopt thermal source with heat sink between the adding heat interfacial material reach this purpose.When electron device runs into improper operating mode suddenly, the electric current of uprushing makes electron device produce a large amount of heats in a short time.This moment must be rapidly with transfer of heat in order to avoid burn electron device.Obviously, the phase change material that possesses the high capacity of heat transmission is a kind of very ideal heat interfacial material.It can infiltrate to greatest extent after the liquefaction thermal source and heat sink between small space reduce the negative impact that air brings, can absorb the thermal shocking of moment in the high capacity of heat transmission of maintenance simultaneously apace, keep the works better of electron device to greatest extent.Therefore the phase change material of studying high heat conduction becomes the focus of current phase change material research field.
The method that is used for strengthening the phase change material heat-transfer capability at present mainly contains following three kinds: 1) try every possible means on the encapsulating structure of phase change material: phase change material is encapsulated in shell structure with high capacity of heat transfer or ribbed pipe such as aluminium dish, the metal tube.Improve heat transfer efficiency by the contact area that increases PCM and thermal source.2) in phase change material, add filler as tinsel, metal ring, metal-powder, stupalith, carbon fiber, carbon black and graphite etc. with high thermal conductivity.As when utilizing carbon fiber to improve the capacity of heat transmission of phase change material, carbon fiber is deposited in the phase change material in an orderly manner, utilize the characteristics of the good radially capacity of heat transmission of having of carbon fiber to improve heat energy from the quick transmission of thermal source to phase change material.3) phase change material is embedded in the metal base with high capacity of heat transmission.For example: phase change material is carried out at its surface electrical deposited copper, being formed on the matrix material that is inlaid with phase change material in the copper base material again after microcapsule coat.These methods have all improved the apparent capacity of heat transmission of phase change material effectively, but also have some problems.There is anisotropy and excessive etc. such as complex structure, the capacity of heat transmission to the sacrifice of heat storage capacity.Therefore still the method for the capacity of heat transmission of the new raising phase change material of necessary searching.
Nano material is a kind of active material of rising in recent years.Because it has the specific surface area of super large, it was once placed high hopes to be used for improving the capacity of heat transmission of material by people.But might reduce the capacity of heat transmission of material on the contrary in the phon scattering that nanoparticle/substrate interface produces.Metal nanometer line has very high length-to-diameter ratio.When heat energy can be avoided phon scattering during along with axially the propagating of metal nanometer line effectively.Therefore we think that in phase change material interpolation metal nanometer line should be able to strengthen the capacity of heat transmission of phase change material effectively.The trial that we carry out shows: when being evenly dispersed in metal nanometer line in the phase change material, not only can obtain having the phase-changing energy storage material of the very high capacity of heat transmission, and metal nanometer line has surpassed metal nanoparticle out and away to the enhanced degree of the material capacity of heat transmission., can be filled at an easy rate along with the generation of phase transformation (liquefaction) in the various small spaces simultaneously, so this material also can be made a kind of good heat interfacial material and uses because the size of metal nanometer line is also very little.
Summary of the invention
The purpose of this invention is to provide a kind of metal nanometer line/Fatty Alcohol(C12-C14 and C12-C18) (acid) composite phase-change material preparation method, carry out metal nanometer line and organic phase change material compound with super-high heat-conductive performance.The purer organic phase change material of the capacity of heat transmission of the composite phase-change material after compound has increased significantly.And the preparation technology of material is simple, and cost is lower, is a kind of good phase change material.
Another object of the present invention is that a kind of have the phase change material of the high capacity of heat transmission to be used as good heat interfacial material.
For achieving the above object, the technical solution used in the present invention is:
A kind of have a very preparation method of the composite phase-change material of high thermal conductivity coefficient, and specific operation process is:
Copper or nano silver wire are distributed in the organic solvent, add organic phase change material, dispersed mixture and remove organic solvent under the temperature of 2～40 ℃ of the fusing points that is higher than organic phase change material; Remove organic solvent must and heating, ultrasonic dispersing carry out simultaneously, and organic solvent that must the general just can finish ultrasonic dispersing after removing fully;
Described organic solvent is that boiling point is 30～100 ℃ a volatile organic solvent under the normal pressure; Described organic phase change material is the positive monohydroxy-alcohol of C12-C26 straight chain (as: lauryl alcohol, tetradecyl alcohol, hexadecanol and/or positive hexacosyl alcohol) of even number of carbon atoms, or the positive monocarboxylic acid of C8-C26 straight chain of even number of carbon atoms (as: n-caprylic acid, TETRADECONIC ACID, palmitic acid, stearic acid and/or positive hydroxyhexacosanoic acid); The addition of copper or nano silver wire is 10～60% of an organic phase change material weight.
Described organic solvent is a methyl alcohol, ethanol, and propyl alcohol, Virahol, ether, propyl ether, isopropyl ether, the first positive propyl ether, tetrahydrofuran (THF), sherwood oil and/or acetone, its addition are copper or nano silver wire weight 10～20 times.
Described copper nano-wire prepares synthetic under heating condition by the wet chemistry reduction method, be specially: in the aqueous solution, with the cupric nitrate is raw material, hydrazine hydrate is that reductive agent, quadrol are that complexing agent, sodium hydroxide are stablizer, and the molar ratio scope between cupric nitrate, reductive agent, complexing agent, stablizer and the water is: 1: 2.5～3: 70～80: 2000～3000: 6200～32000; 60～160 ℃ of synthesis temperatures; Generated time 1～3h.
When total reaction solution volume is 200～1000mL, mol ratio between hydrazine hydrate, quadrol and sodium hydroxide and the cupric nitrate is respectively 2.5～3: 1,70～80: 1,2000～3000: in 1 the scope, and the concentration＞98wt% of the concentration 0.05～0.15M of the raw material copper nitrate solution of selecting for use, the concentration V/V 30～50% of hydrazine hydrate, quadrol, the concentration 5～15M of sodium hydroxide solution.
Described nano silver wire prepares synthetic under heating condition by the wet chemistry reduction method, be specially: be that raw material, ethylene glycol are that reductive agent and solvent, polyvinylpyrrolidone are stablizer with the Silver Nitrate, when the preparation nano wire, Silver Nitrate, ethylene glycol, the molar ratio of polyvinylpyrrolidone is: 1: 400～950: 5～10.
At first, prepare Silver Nitrate/ethylene glycol solution and polyvinylpyrrolidone/ethylene glycol solution respectively in the preparation building-up process, Silver Nitrate/ethylene glycol solution concentration is 0.1～0.15M, the polyvinylpyrrolidonemolecules molecules amount is 30000～60000, polyvinylpyrrolidone/ethylene glycol solution concentration is 0.35～0.4M, then polyvinylpyrrolidone/ethylene glycol solution is joined in Silver Nitrate/ethylene glycol solution, polyvinylpyrrolidone is pressed monomer and is calculated, mol ratio between control polyvinylpyrrolidone and the Silver Nitrate is 5～10: 1, and total reaction solution volume is 70～160mL.
The diameter of copper or nano silver wire is between 30～70 nanometers, and length is between 5～50 microns; Described dispersing mode can be mechanical stirring or ultrasonic dispersing.
The present invention has following advantage:
1. preparation is simple, and cost is lower.Synthesizing at heating condition of metal nanometer line finished, and moderate being easy to of temperature controlled, and be raw materials used all cheap and easy to get.The compound of metal nanometer line and organic phase change material realizes that by mechanical stirring and ultrasonic dispersing process is simple and convenient.
2. improved the capacity of heat transmission of organic phase change material significantly, described composite phase-change material has higher latent heat of phase change simultaneously.
3. described composite phase-change material also can be used as a kind of good heat interfacial material and uses.
In a word, by the phase change material that the inventive method makes, technology is simple, cost is low, in the higher latent heat of phase change of maintenance, has improved the thermal conductivity of organic phase change material greatly, thereby improved the performance of organic phase change material effectively, expanded its range of application significantly.
Description of drawings
Fig. 1 contrasts synoptic diagram for the heat storage capacity of the phase-change thermal storage ability that is obtained by DSC test of the specific embodiment of the invention 1 and pure tetradecyl alcohol;
Fig. 2 is the contrast synoptic diagram of the capacity of heat transmission and the pure tetradecyl alcohol capacity of heat transmission of the specific embodiment of the invention 1;
Fig. 3 can try hard to for the phase-change thermal storage that is obtained by DSC test of the specific embodiment of the invention 2;
Fig. 4 is the capacity of heat transmission figure of the specific embodiment of the invention 2;
Fig. 5 can try hard to for the phase-change thermal storage that is obtained by DSC test of the specific embodiment of the invention 3;
Fig. 6 is the capacity of heat transmission figure of the specific embodiment of the invention 3
Embodiment
Embodiment 1
1) synthetic copper nano-wire: get the copper nitrate solution 12mL of 0.1M, mix, add the quadrol of 6mL 99% again, mix with the aqueous sodium hydroxide solution (7M) of 360mL.Add 0.36mL50% (V/V) hydrazine hydrate, put into the water-bath of 60 degree after mixing, take out cooling after 2 hours.Filtration obtains copper nano-wire.Repeat repeatedly to obtain the copper nano-wire of capacity.
2) preparation copper nano-wire/tetradecyl alcohol composite phase-change material: get the 0.86g copper nano-wire, add 15mL acetone, magnetic agitation 1.5 hours, ultrasonic dispersing 0.5 hour, the acetone that volatilizees then is to remaining 1.5mL, add the 0.60g tetradecyl alcohol again, place 50 degree water-bath ultrasonic dispersing to volatilize fully said mixture, take out cooling and promptly obtain copper nano-wire/tetradecyl alcohol composite phase-change material to acetone.Wherein contain copper nano-wire 59wt%
3) heat accumulation test:
The thermal energy storage performance test of described composite phase-change material is carried out on the DSC141 type differential scanning calorimeter (DSC) that French SETARAM company produces, and specific operation process is:
1) composite phase-change material that makes is carefully ground to form tiny powder in agate mortar, cross 300 mesh sieves;
2) will put into sample crucible through the composite phase-change material weighing 5～10mg after grinding, at the fusing point of organic phase change material up and down in 40 ℃ the temperature range, scan with the temperature rise rate of 10 ℃/min;
3) program of using instrument to carry handles to determine initial transformation temperature, phase transformation peak temperature and the latent heat of phase change of composite phase-change material to experimental result;
Described composite phase-change material through with metal nanometer line compound after, more simple organic phase change material, its heat storage capacity descends along with the increase of the addition of metal nanometer line, its minimum latent heat of phase change is 85～95J/g.
Be specially: will cross 300 mesh sieves through the composite phase-change material after grinding, weighing 6.4mg puts into the sample crucible of DSC instrument, in 0～80 ℃ temperature range, scans with the temperature rise rate of 10 ℃/min.The program of using instrument to carry is handled the latent heat of phase change that obtains material to experimental result.
4) thermal conductivity test:
Heat conductivility test to described composite phase-change material is carried out on the HotDisc thermal constant analyser that Sweden Hot Disc company produces, and operating process can be:
1) composite phase-change material that makes is carefully ground to form tiny powder in agate mortar, cross 300 mesh sieves;
2) will depress to two right cylinders at 20MPa through the composite phase-change material after grinding, the probe clip of thermal constant analyser in the middle of two right cylinders, will be clamped the thermal conductivity of two right cylinders with the mensuration material with a clip again;
Employed measured power is 0.05～0.1W, and the employed test duration is 2.5～10s; The thermal conductivity of described composite phase-change material increases significantly with the increase of metal nanometer line addition.Behind the copper nano-wire that adds 59wt%, thermal conductivity can reach 2.85W/mK, and pure organic phase change material has only 0.32W/mK.
Be specially: will cross 300 mesh sieves through the composite phase-change material after grinding, depress to two right cylinders at 20MPa, with the probe clip of thermal constant analyser in the middle of two right cylinders, clamp two right cylinders to measure the thermal conductivity of material with a clip again, measured power is 0.1W, and the employed test duration is 2.5s.
Embodiment 2
1) synthetic copper nano-wire: get the copper nitrate solution 12mL of 0.1M, mix, add the quadrol of 6mL 99% again, mix with the aqueous sodium hydroxide solution (7M) of 360mL.Add 0.36mL50% (V/V) hydrazine hydrate, put into the water-bath of 60 degree after mixing, take out cooling after 2 hours.Filtration obtains copper nano-wire.Repeat repeatedly to obtain the copper nano-wire of capacity.
2) preparation copper nano-wire/tetradecyl alcohol composite phase-change material: get the 0.53g copper nano-wire, add 15mL acetone, magnetic agitation 1.5 hours, ultrasonic dispersing 0.5 hour, the acetone that volatilizees then is to remaining 1.5mL, add the 1.00g tetradecyl alcohol again, place 50 degree water-bath ultrasonic dispersing to volatilize fully said mixture, take out cooling and promptly obtain copper nano-wire/tetradecyl alcohol composite phase-change material to acetone.Wherein contain copper nano-wire 34.6wt%
3) heat accumulation test: will cross 300 mesh sieves through the composite phase-change material after the grinding, weighing 6.0mg puts into the sample crucible of DSC instrument, in 0～80 ℃ temperature range, scans with the temperature rise rate of 10 ℃/min.The program of using instrument to carry is handled the latent heat of phase change that obtains material to experimental result.
4) thermal conductivity test: will cross 300 mesh sieves through the composite phase-change material after grinding, depress to two right cylinders at 20MPa, with the probe clip of thermal constant analyser in the middle of two right cylinders, clamp two right cylinders to measure the thermal conductivity of material with a clip again, measured power is 0.05W, and the employed test duration is 5s.
Embodiment 3
1) synthesis of silver nano-wire:
1) getting the 2.50g polyvinylpyrrolidone is dissolved in and obtains the solution that concentration is 0.36M in the 62mL ethylene glycol.This solution vigorous stirring in 160 ℃ of oil baths was refluxed 2 hours.
2) 0.62g AgNO3 is dissolved in the 30mL ethylene glycol, the speed of this solution with 0.5mL/min is added drop-wise in the aforementioned solution, simultaneously vigorous stirring.Drip the back restir and refluxed 1 hour, then cool to room temperature.
3) add the acetone of 10 times of volumes in the above-mentioned reaction product mixed solution, left standstill 24 hours, discard the yellow clear liquid in upper strata.Lower sediment is filtered and is obtained nano silver wire.
2) preparation nano silver wire/tetradecyl alcohol composite phase-change material: get the 1.00g nano silver wire, add 15mL acetone, magnetic agitation 1.5 hours, ultrasonic dispersing 0.5 hour, the acetone that volatilizees then is to remaining 1.5mL, add the 0.60g tetradecyl alcohol again, place 50 degree water-bath ultrasonic dispersing to volatilize fully said mixture, take out cooling and promptly obtain nano silver wire/tetradecyl alcohol composite phase-change material to acetone.Wherein contain nano silver wire 62.5wt%
3) heat accumulation test: will cross 300 mesh sieves through the composite phase-change material after the grinding, weighing 6.3mg puts into the sample crucible of DSC instrument, in 0～80 ℃ temperature range, scans with the temperature rise rate of 10 ℃/min.The program of using instrument to carry is handled the latent heat of phase change that obtains material to experimental result.
4) thermal conductivity test: will cross 300 mesh sieves through the composite phase-change material after grinding, depress to two right cylinders at 20MPa, with the probe clip of thermal constant analyser in the middle of two right cylinders, clamp two right cylinders to measure the thermal conductivity of material with a clip again, measured power is 0.05W, and the employed test duration is 5s.
Claims (7)
1. the preparation method of a composite phase-change material is characterized in that:
Copper or nano silver wire are distributed in the organic solvent, add organic phase change material, dispersed mixture and remove organic solvent under the temperature of 2～40 ℃ of the fusing points that is higher than organic phase change material; Removing organic solvent must carry out simultaneously with heating, ultrasonic dispersing, and just can finish ultrasonic dispersing after organic solvent must being removed fully;
Described organic solvent is that boiling point is 30～100 ℃ a volatile organic solvent under the normal pressure; Described organic phase change material is the positive monohydroxy-alcohol of C12-C26 straight chain of even number of carbon atoms, or the positive monocarboxylic acid of C8-C26 straight chain of even number of carbon atoms; The addition of copper or nano silver wire is 10～60% of an organic phase change material weight; Described organic solvent is an ether, propyl ether, and isopropyl ether, the first positive propyl ether, tetrahydrofuran (THF), sherwood oil and/or acetone, its addition are copper or nano silver wire weight 10～20 times.
2. according to the described preparation method of claim 1, it is characterized in that: described organic phase change material is lauryl alcohol, tetradecyl alcohol, hexadecanol, stearyl alcohol, eicosanol, behenyl alcohol, tetracosanol, hexacosyl alcohol, n-caprylic acid, laurostearic acid, TETRADECONIC ACID, palmitic acid, stearic acid, 20 acid, behenic acid, tetracosanoic acid or positive hydroxyhexacosanoic acid.
3. according to the described preparation method of claim 1, it is characterized in that: the diameter of copper or nano silver wire is between 30～70 nanometers, and length is between 5～50 microns.
4. according to the described preparation method of claim 1, it is characterized in that: described copper nano-wire prepares synthetic under heating condition by the wet chemistry reduction method, be specially,
In the aqueous solution, with the cupric nitrate is raw material, hydrazine hydrate is that reductive agent, quadrol are that complexing agent, sodium hydroxide are stablizer, and the molar ratio scope between cupric nitrate, reductive agent, complexing agent, stablizer and the water is: 1: 2.5～3: 70～80: 2000～3000: 6200～32000; 60～160 ℃ of synthesis temperatures; Generated time 1～3h.
5. according to the described preparation method of claim 4, it is characterized in that: the concentration＞98wt% of the concentration 0.05～0.15M of selected raw material copper nitrate solution, the concentration V/V 30～50% of hydrazine hydrate, quadrol, the concentration 5～15M of sodium hydroxide solution.
6. according to the described preparation method of claim 1, it is characterized in that: described nano silver wire prepares synthetic under heating condition by the wet chemistry reduction method, be specially, with the Silver Nitrate is that raw material, ethylene glycol are that reductive agent and solvent, polyvinylpyrrolidone are stablizer, when the preparation nano wire, the molar ratio of Silver Nitrate, ethylene glycol, polyvinylpyrrolidone is: 1: 400～950: 5～10; Polyvinylpyrrolidone is pressed monomer and is calculated.
7. according to the described preparation method of claim 6, it is characterized in that: prepare Silver Nitrate/ethylene glycol solution and polyvinylpyrrolidone/ethylene glycol solution respectively in the preparation building-up process, Silver Nitrate/ethylene glycol solution concentration is 0.1～0.15M, the polyvinylpyrrolidonemolecules molecules amount is 30000～60000, polyvinylpyrrolidone/ethylene glycol solution concentration is 0.35～0.4M, then polyvinylpyrrolidone/ethylene glycol solution is joined in Silver Nitrate/ethylene glycol solution, polyvinylpyrrolidone is pressed monomer and is calculated, and the mol ratio between control polyvinylpyrrolidone and the Silver Nitrate is 5～10: 1.
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| CN101856035B (en) * | 2010-05-28 | 2012-08-15 | 中国科学院上海应用物理研究所 | Method for preparing nano silicon wire/ nano silver composite material |
| DE102010017706B4 (en) * | 2010-07-02 | 2012-05-24 | Rent-A-Scientist Gmbh | Process for the preparation of silver nanowires |
| WO2012044287A1 (en) * | 2010-09-29 | 2012-04-05 | Empire Technology Development Llc | Phase change energy storage in ceramic nanotube composites |
| CN102002344A (en) * | 2010-11-06 | 2011-04-06 | 大连理工大学 | Ultrasonic promoting method for preparing organic/inorganic hybridization phase-change energy storage material |
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| CN104162657A (en) * | 2014-07-21 | 2014-11-26 | 江苏大学 | Super-long copper nanowire and preparing method thereof |
| CN114209830B (en) * | 2014-11-25 | 2023-12-22 | 纽菲斯有限公司 | phase change nanoparticles |
| CN104616837B (en) * | 2015-02-02 | 2017-01-25 | 华南师范大学 | Preparation method of plane ordered metal nanowire superposed transparent conducting thin film |
| CN106225254A (en) * | 2016-09-30 | 2016-12-14 | 王义东 | A kind of round-the-clock multipurpose photovoltaic stores hot systems and method |
| CN107446554B (en) * | 2017-09-22 | 2020-09-18 | 浙江海洋大学 | Preparation method of wide phase-change temperature zone shape-stabilized phase-change material |
| CN111909662B (en) * | 2020-08-28 | 2021-07-02 | 广东工业大学 | Composite phase-change material and preparation method thereof |
| CN112842672A (en) * | 2021-02-21 | 2021-05-28 | 大理大学 | Lasting bacteriostasis type hot compress physiotherapy bag |
| CN116113217B (en) * | 2023-02-18 | 2023-08-22 | 广东工业大学 | Flexible heat-conducting ionic liquid phase-change gel material and preparation method and application thereof |
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