CN104152848A - Double-layer photothermal conversion composite material and preparation method thereof - Google Patents
Double-layer photothermal conversion composite material and preparation method thereof Download PDFInfo
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- CN104152848A CN104152848A CN201410397417.6A CN201410397417A CN104152848A CN 104152848 A CN104152848 A CN 104152848A CN 201410397417 A CN201410397417 A CN 201410397417A CN 104152848 A CN104152848 A CN 104152848A
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Abstract
The invention relates to a double-layer photothermal conversion composite material and a preparation method thereof, and belongs to the technical field of solar energy utilization. The composite material comprises a bottom transition layer and a top high-heat radiation rate layer, wherein the bottom transition layer and the top high-heat radiation rate layer of the composite material are prepared on a substrate material in sequence through a preparation method of vapor deposition or magnetron sputtering; the bottom transition layer and the substrate material are directly connected; and the top high-heat radiation rate layer and the bottom transition layer are also directly connected. The composite material has the characteristics of high working temperature, high heat radiation rate, strong heat shock resistance and long service life, and is a new high-performance photothermal conversion material.
Description
Technical field
The invention belongs to technical field of solar utilization technique, particularly a kind of double-deck photo-thermal conversion matrix material.
Technical background
Optical-thermal conversion material is the core material in solar light-heat power-generation field, by transform light energy, is heat energy, then by the conduction heating working medium of base material, thermal emissivity rate and the working temperature of optical-thermal conversion material are higher, and the efficiency of conversion of sun power is higher.
Along with photo-thermal power generation is constantly to high temperature, efficient future development, the working temperature of dish formula Stirling photo-thermal power generation technology and the design effort temperature of the tower photo-thermal power generation of high temperature have broken through 873K, and the optical-thermal conversion material that can more than temperature work long hours at this still belongs to blank in China.
Current optical-thermal conversion material mainly concentrates on middle low temperature photo-thermal conversion field (as valve tube, blue titanium film, heat-absorbing chamber etc.), although every kind of optical-thermal conversion material all contains the materials such as thermal emissivity rate is high, heat resistance is good oxide compound, nitride, carbide, current optical-thermal conversion material working temperature is generally between 573K to 673K.As the patent of invention WO2008/153922 of U.S. Ao Sila company, applied for the receptor for solar energy system, relate to integrated solar receiver-heat energy accumulator unit.WO2005/088218 discloses a kind of thermal energy storage system, adopts solid graphite to store heat energy, so that by heat energy, the heat exchanger by surface mounting is discharged into fluid subsequently.CN102121757A discloses a kind of non-vacuum solar spectrum selective absorber coatings, and the use temperature of this coating in antivacuum is higher than 400 degrees Celsius, and use temperature is in a vacuum higher than 500 degrees Celsius.CN1360084A relates to is that to take titanium and alloy aluminum be the negative electrode aluminium that sputter forms in nitrogen, air atmosphere nitrogen+titanium nitrogen-aluminium titanium film and aluminum-nitrogen-oxygen+titanium-nitrogen-oxygen-aluminium titanium film to a kind of absorption layer, its antireflection layer is aluminium nitrogen+titanium nitrogen film and aluminum-nitrogen-oxygen+titanium-nitrogen-oxygen film, under atmospheric condition through 350 degrees Celsius, 250 hours, or 400 degrees Celsius, 50 hours, or 450 degrees Celsius, after baking in 80 hours, its solar absorptance all can reach more than 0.93, and emittance is 0.06-0.10.
The reason that causes current optical-thermal conversion material working temperature to improve mainly contains 2 points: the one, and most optical-thermal conversion materials contains the poor composition of temperature tolerance (as oxynitride, low-temperature metal) outside the materials such as oxide compound, nitride, carbide, and spot corrosion easily occurs while working more than 673K; The 2nd, thermal matching can be poor, and especially three layers of above material are difficult to overcome the thermal stresses variation that under worst hot case, severe thermal impacts to cause, and directly cause cracking or peel off.
So, obtain a kind of optical-thermal conversion material that can take into account thermostability and high-heating radiation rate under the environment of high temperature, high thermal shock the efficient photo-thermal generation technology of high temperature had to important value.
Summary of the invention
The object of the invention is for overcoming the weak point of prior art, a kind of double-deck photo-thermal conversion matrix material and preparation method thereof is provided.The double-deck photo-thermal conversion matrix material the present invention relates to designs for the base material of actual light thermal conversion device, top layer high-heating radiation rate layer has been selected all stronger conventional oxide compound, carbide and nitride of current thermal emissivity rate and thermostability, bottom transition layer has selected that radiant ratio is higher, thermal expansivity between top layer high-heating radiation rate layer and base material, with top layer high-heating radiation rate layer and base material is combined well, thermostability is strong oxide compound, to meet the actual condition demand that high temperature optical-thermal conversion material thermal emissivity rate is high, thermal shock resistance is good.
A kind of double-deck photo-thermal conversion matrix material provided by the invention, it is characterized in that: this matrix material comprises bottom transition layer and top layer high-heating radiation rate layer, the bottom transition layer of this matrix material and top layer high-heating radiation rate layer are prepared from successively by certain preparation method on base material, and wherein bottom transition layer is directly and is connected with bottom transition layer with base material, top layer high-heating radiation rate layer.
Described base material is a kind of in Fe base, Ni base, Co base and Cr sill.
More than 80% composition of described bottom transition layer is SiO
2, ZrO
2, Y
2o
3, TiO
2in one or more.
More than 80% composition of described top layer high radiant rate layer is one or more in SiC, C, TiC and BN.
Described bottom transition layer and top layer high-heating radiation rate layer thickness are 100nm to 5mm.
It is 0.5～0.8 in the full-specturm radiation rate of 300K that described double-deck photo-thermal is changed matrix material, in the full-specturm radiation rate of 800K, is 0.65～0.95.
The present invention also provides a kind of method of preparing above-mentioned double-deck photo-thermal conversion matrix material, it is characterized in that: first base material is carried out to pre-treatment, base material oxide skin is removed completely and more than surfaceness reaches 5nm; Then by vapour deposition process or magnetron sputtering method, prepare bottom transition layer; Then base material and bottom transition layer are heat-treated, after thermal treatment completes, effects on surface is repaired; By vapour deposition process or magnetron sputtering method, prepare top layer high-heating radiation rate layer again; Double-deck photo-thermal conversion matrix material is heat-treated, and after thermal treatment completes, effects on surface is repaired, and finally obtains double-deck photo-thermal conversion matrix material.
Principle of work of the present invention:
The material that thermal emissivity rate is high (as SiC, C based material, ZrC, TiC and BN), all have firm molecular structure, thermal expansivity is lower.But in photo-thermal power generation field, in order effectively to realize the acting of solar heating medium, optical-thermal conversion material is often all prepared on metal matrix base material.Because the material thermal expansion coefficient of metal_based material and high-heating radiation rate differs larger, cause optical-thermal conversion material under high-temperature work environment, to be difficult to use.
It is the feature of material intrinsic property that the present invention utilizes thermal radiation, because the thermal radiation of material only realizes light and hot conversion by certain thickness surfacing to electromagnetic absorption and radiation, surfacing in certain thickness adopts the high material of intrinsic thermal emissivity rate just can obtain the high-heating radiation rate performance of integral material, thus the present invention adopt current thermal emissivity rate and thermostability all stronger oxide compound, carbide and nitride as top layer high-heating radiation layer material.
The present invention also utilizes the method for matched coefficients of thermal expansion simultaneously, adopt thermal expansivity between the way of the bottom transition layer of top layer high-heating radiation rate coating and base material, reduce the thermal stresses producing between integral composite and substrate in temperature changing process, improve matrix material thermal shock resistance.The present invention also considers because the density-of-states distribution of differing materials is different simultaneously, the surface material thickness that determines its overall thermal radiant ratio performance is also different, be generally 100nm to 2mm, the thermal emissivity rate that is to say bottom buffer layer material also likely produces certain influence to the thermal emissivity rate of integral composite, so the bottom transition layer that the present invention selects is, radiant ratio is higher, thermal expansivity between top layer high-heating radiation rate layer and base material, with top layer high-heating radiation rate layer and base material is combined well, thermostability is strong oxide compound.
The double-deck photo-thermal the present invention relates to is changed matrix material and is not contained at 873K temperature easily ablated composition (C based material is non-graphite-phase) completely, and in a series of high-heating radiation rate candidate materials, find the rational design of material scheme of heat coupling under worst hot case, the working temperature of existing photo-thermal conversion matrix material is significantly brought up to 873K from 573-673K.
To sum up, the present invention finally obtain that a kind of working temperature is high, thermal emissivity rate is high, the double-deck photo-thermal conversion matrix material of stable performance under high temperature thermal shock.
Accompanying drawing explanation
Fig. 1 is double-deck photo-thermal conversion matrix material schematic diagram.
In accompanying drawing, the list of parts of each label representative is as follows:
1, base material, 2, bottom transition layer, 3, top layer high-heating radiation rate layer.
Embodiment
Below by embodiment, the present invention will be further described, but and do not mean that limiting the scope of the invention.
Embodiment 1
By physical vaporous deposition, on Ni sill, prepare ZrO
2-Y
2o
3the double-deck photo-thermal conversion of/SiC matrix material:
Adopt the Ni alloy substrate of 300 * 300 sizes as base material;
With 400 orders, 800 orders and the 1200 object sand paper Ni alloy substrate of polishing successively, scale removal also guarantees that surfaceness is more than 10nm respectively;
Ni alloy substrate after polishing is carried out to 10min supersound process in water;
The ethanolic soln of use 40% and acetone soln clean the Ni alloy substrate surface after supersound process successively;
Ni alloy substrate after surface treatment is positioned in Pvd equipment, selects target ZrO
2and Y
2o
3deposit vacuum tightness 7 * 10 simultaneously
-3pa, range 500mm, electronic beam current intensity 60mA, substrate deposition temperature 523K.Through repeatedly depositing, on Ni alloy substrate, obtain the ZrO that thickness is 3mm
2-Y
2o
3bottom transition layer;
ZrO will be deposited
2-Y
2o
3the Ni alloy substrate of bottom transition layer is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 1073K, insulation 1h; Speed of cooling with 2K/min is cooled to 973K, 873K, 673K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 10nm, below 500nm;
Material after surface finish is placed in Pvd equipment, selects target SiC, vacuum tightness 7 * 10
-3pa, range 500mm, electronic beam current intensity 40mA, substrate temperature 523K.Through repeatedly depositing, at ZrO
2-Y
2o
3on bottom transition layer, obtaining thickness is the SiC top layer high-heating radiation rate layer of 2mm;
The Ni alloy substrate that deposits two-layer compound coating is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 873K, insulation 1h; Speed of cooling with 2K/min is cooled to 773K, 673K, 473K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 50nm;
The final ZrO that obtains expectation on Ni alloy substrate
2-Y
2o
3the double-deck photo-thermal conversion of/SiC matrix material.
Embodiment 2
By magnetron sputtering method and chemical Vapor deposition process, on Fe sill, prepare TiO
2the double-deck photo-thermal conversion of/TiC matrix material:
The semisphere Fe alloy substrate that employing diameter is 50mm is as base material;
With 400 orders, 800 orders and the 1200 object sand paper Fe alloy substrate of polishing successively, scale removal also guarantees that surfaceness is more than 5nm respectively;
Fe alloy substrate after polishing is carried out to 10min supersound process in water;
The ethanolic soln of use 40% and acetone soln clean the Fe alloy substrate surface after supersound process successively;
Fe alloy substrate after surface treatment is positioned in magnetron sputtering equipment, adopts metal Ti target, reactant gases O
2, sputter gas Ar, reaction pressure 2Pa, underlayer temperature 573K with Ar pre-sputtering 1min, obtains the TiO that thickness is 50nm on Fe alloy substrate
2bottom transition layer;
By depositing Ti O
2the Fe alloy substrate of bottom transition layer is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 973K, insulation 1h; Speed of cooling with 2K/min is cooled to 873K, 773K, 673K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 500nm;
Material after surface finish is placed in chemical vapor depsotition equipment, and depositing temperature is 1323K, and furnace pressure is 0.1MPa, and titanium source is TiCl
4, carbon source is CH
4, CH
4directly pass in stove TiCl
4by hydrogen, bring in stove, so at TiO
2on bottom transition layer, obtaining thickness is the TiC top layer high-heating radiation rate layer of 50nm;
The Fe alloy substrate that deposits two-layer compound coating is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 973K, insulation 1h; Speed of cooling with 2K/min is cooled to 873K, 773K, 673K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 50nm;
The final TiO that obtains expectation on Fe alloy substrate
2the double-deck photo-thermal conversion of/TiC matrix material.
Embodiment 3
By physical vaporous deposition and chemical Vapor deposition process, on Co sill, prepare SiO
2the double-deck photo-thermal conversion of/C matrix material:
Adopt the Ni alloy substrate of 20 * 50 sizes as base material;
With 400 orders, 800 orders and the 1200 object sand paper Co alloy substrate of polishing successively, scale removal also guarantees that surfaceness is more than 10nm respectively;
Co alloy substrate after polishing is carried out to 10min supersound process in water;
The ethanolic soln of use 40% and acetone soln clean the Co alloy substrate surface after supersound process successively;
Co alloy substrate after surface treatment is positioned in Pvd equipment, selects target SiO
2, vacuum tightness 7 * 10
-3pa, range 500mm, electronic beam current intensity 60mA, substrate deposition temperature 473K.Through repeatedly depositing, on Co alloy substrate, obtain the SiO that thickness is 2 μ m
2bottom transition layer;
SiO will be deposited
2the Co alloy substrate of bottom transition layer is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 773K, insulation 1h; Speed of cooling with 2K/min is cooled to 673K, 573K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 10nm, below 500nm;
Material after surface finish is placed in chemical vapor depsotition equipment, and carbon source is CH
4, reactant gases H
2, pressure 5Pa, distance between plates 90mm, plate is pressed 1000V.Through repeatedly depositing, at SiO
2on bottom transition layer, obtaining thickness is the C film top layer high-heating radiation rate layer of 2 μ m;
The Co alloy substrate that deposits two-layer compound coating is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 873K, insulation 1h; Speed of cooling with 2K/min is cooled to 773K, 673K, 473K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 100nm;
The final SiO that obtains expectation on Co alloy substrate
2the double-deck photo-thermal conversion of/C matrix material.
Embodiment 4
By magnetron sputtering method, on Cr sill, prepare TiO
2the double-deck photo-thermal conversion of/BN matrix material
The circular Fe alloy substrate that employing diameter is 40mm is as base material;
With 400 orders, 800 orders and the 1200 object sand paper Fe alloy substrate of polishing successively, scale removal also guarantees that surfaceness is more than 5nm respectively;
Fe alloy substrate after polishing is carried out to 10min supersound process in water;
The ethanolic soln of use 40% and acetone soln clean the Fe alloy substrate surface after supersound process successively;
Cr alloy substrate after surface treatment is positioned in magnetron sputtering equipment, adopts metal Ti target, reactant gases O
2, sputter gas Ar, reaction pressure 2Pa, underlayer temperature 573K with Ar pre-sputtering 1min, obtains the TiO that thickness is 500nm on Cr alloy substrate
2bottom transition layer;
By depositing Ti O
2the Cr alloy substrate of bottom transition layer is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 973K, insulation 1h; Speed of cooling with 2K/min is cooled to 873K, 773K, 673K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 500nm;
Material after surface finish is placed in magnetron sputtering equipment, selects BN target, range 5cm, sputtering power 150W, underlayer temperature 673K, operating air pressure 1Pa, so at TiO
2on bottom transition layer, obtaining thickness is the BN top layer high-heating radiation rate layer of 500nm;
The Cr alloy substrate that deposits two-layer compound coating is placed in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 973K, insulation 1h; Speed of cooling with 2K/min is cooled to 873K, 773K, 673K, and soaking time is 2h, subsequently furnace cooling;
Cooling polish with sand paper effects on surface afterwards, makes surfaceness more than 5nm, below 200nm;
The final TiO that obtains expectation on Cr alloy substrate
2the double-deck photo-thermal conversion of/BN matrix material.
In above-mentioned four embodiment, when the main component of top layer high-heating radiation rate layer and bottom transition layer accounts for 80% when above, by reasonable doping, still can realize or approach the expected performance of double-layer composite material.
Although described one or more embodiments of the present invention, however, only still it should be understood that otherwise depart from the spirit and scope of the present invention, just can make various changes.Therefore, other embodiments fall within the scope of the claims.
Claims (10)
1. a double-deck photo-thermal is changed matrix material, it is characterized in that: this matrix material comprises bottom transition layer and top layer high-heating radiation rate layer, the bottom transition layer of this matrix material and top layer high-heating radiation rate layer are prepared from successively on base material, and wherein bottom transition layer is directly and is connected with bottom transition layer with base material, top layer high-heating radiation rate layer;
Described bottom transition layer main component is SiO
2, ZrO
2, Y
2o
3, TiO
2in one or more;
Described top layer high-heating radiation rate layer main component is one or more in SiC, C, TiC and BN.
2. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: described base material is a kind of in Fe base, Ni base, Co base and Cr sill.
3. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: double-deck photo-thermal is changed matrix material into ZrO
2-Y
2o
3/ SiC matrix material, TiO
2/ TiC matrix material, SiO
2/ C matrix material or TiO
2/ BN matrix material.
4. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: described double-deck photo-thermal conversion composite material surface roughness is at 5nm to 200nm.
5. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: described bottom transition layer and top layer high-heating radiation rate layer thickness are 100nm to 5mm.
6. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: it is 0.5～0.8 at the full spectrum thermal emissivity rate of 300K that described double-deck photo-thermal is changed matrix material, is 0.65～0.95 at the full spectrum thermal emissivity rate of 800K.
7. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: the working temperature that described double-deck photo-thermal is changed matrix material is 800K to 1200K.
8. according to the double-deck photo-thermal conversion matrix material described in claim 1, it is characterized in that: when the main component of described top layer high-heating radiation rate layer and described bottom transition layer accounts for 80% when above, by reasonable doping, still can realize or approach the expected performance of double-layer composite material.
9. the double-deck photo-thermal as described in claim 1-8 is changed a preparation method for matrix material, it is characterized in that:
Step 1, carries out pre-treatment by base material, base material oxide skin is removed completely and more than surfaceness reaches 5nm;
Step 2, prepares bottom transition layer by vapour deposition process or magnetron sputtering method;
Step 3, heat-treats base material and bottom transition layer, and after thermal treatment completes, effects on surface is repaired;
Step 4, prepares top layer high-heating radiation rate layer by vapour deposition process or magnetron sputtering method;
Step 5, heat-treats double-deck photo-thermal conversion matrix material, and after thermal treatment completes, effects on surface is repaired, and finally obtains double-deck photo-thermal conversion matrix material.
10. double-deck photo-thermal as claimed in claim 9 is changed a preparation method for matrix material, it is characterized in that:
In described step 1, with 400 orders, 800 orders and the 1200 object sand paper described base material of polishing successively, scale removal also guarantees that surfaceness is more than 5nm respectively; Base material after polishing is carried out to supersound process in water; Ethanolic soln and the acetone soln of use 40% clean the base material after supersound process successively.
In described step 5, described heat treatment step is for to be placed in the alloy substrate of the two-layer compound coating having deposited in equipment for Heating Processing, with the heat-up rate of 5K/min, is heated to 973K, insulation 1h; Speed of cooling with 2K/min is cooled to 873K, 773K, 673K, and soaking time is 2h, subsequently furnace cooling.
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|---|---|---|---|
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|---|---|---|---|
| CN201410397417.6A CN104152848B (en) | 2014-08-13 | 2014-08-13 | A kind of double-deck photothermal deformation composite and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437351A (en) * | 2018-11-22 | 2019-03-08 | 鲁东大学 | A kind of preparation method of foam titanium dichloride load active carbon optical-thermal conversion material |
| CN112234136A (en) * | 2020-09-15 | 2021-01-15 | 武汉纺织大学 | High-efficiency fiber-based thermoelectric energy supply material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103946645A (en) * | 2011-11-14 | 2014-07-23 | 丰田自动车株式会社 | Solar-thermal conversion member, solar-thermal conversion device, and solar thermal power generation device |
-
2014
- 2014-08-13 CN CN201410397417.6A patent/CN104152848B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103946645A (en) * | 2011-11-14 | 2014-07-23 | 丰田自动车株式会社 | Solar-thermal conversion member, solar-thermal conversion device, and solar thermal power generation device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109437351A (en) * | 2018-11-22 | 2019-03-08 | 鲁东大学 | A kind of preparation method of foam titanium dichloride load active carbon optical-thermal conversion material |
| CN112234136A (en) * | 2020-09-15 | 2021-01-15 | 武汉纺织大学 | High-efficiency fiber-based thermoelectric energy supply material and preparation method thereof |
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