CN104152848B - A kind of double-deck photothermal deformation composite and preparation method thereof - Google Patents
A kind of double-deck photothermal deformation composite and preparation method thereof Download PDFInfo
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- CN104152848B CN104152848B CN201410397417.6A CN201410397417A CN104152848B CN 104152848 B CN104152848 B CN 104152848B CN 201410397417 A CN201410397417 A CN 201410397417A CN 104152848 B CN104152848 B CN 104152848B
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Abstract
The present invention relates to a kind of double-deck photothermal deformation composite and preparation method thereof, belong to technical field of solar utilization technique.This composite includes bottom transition zone and top layer active devices, the bottom transition zone of this composite and top layer active devices are sequentially prepared by the preparation method of vapour deposition or magnetron sputtering on base material and form, and wherein bottom transition zone and base material, top layer active devices are to be joined directly together with bottom transition zone and connect.The composite that the present invention relates to has operating temperature height, thermal emissivity rate is high, thermal shock resistance is strong, the feature of life-span length, provides new selection for high-performance optical-thermal conversion material.
Description
Technical field
The invention belongs to technical field of solar utilization technique, particularly to a kind of double-deck photothermal deformation composite.
Technical background
Optical-thermal conversion material is the core material in solar light-heat power-generation field, converts light energy into heat energy, then by substrate material
The conduction heating work medium of material, thermal emissivity rate and the operating temperature of optical-thermal conversion material are the highest, and the conversion efficiency of solar energy is more
High.
Along with photo-thermal power generation constantly develops to high temperature, efficient direction, the operating temperature of dish-style Stirling photo-thermal power generation technology and
The design work temperature of the tower photo-thermal power generation of high temperature has broken through 873K, and the photo-thermal that can work long hours more than this temperature
Transition material still belongs to blank in China.
Current optical-thermal conversion material is concentrated mainly on middle low temperature photothermal deformation field (such as vacuum 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, nitride, carbide,
But current optical-thermal conversion material operating temperature is typically between 573K to 673K.Patent of invention such as Ao Sila company of the U.S.
WO2008/153922, has applied for the receiver for solar energy system, relates to integrated solar receiver-heat energy accumulator
Unit.WO2005/088218 discloses a kind of thermal energy storage system, uses solid graphite to store heat energy, in order to subsequently will
The heat exchanger that heat energy is installed by surface is discharged into fluid.CN102121757A discloses a kind of non-vacuum solar spectrum choosing
Selecting property absorber coatings, this coating use temperature in antivacuum is higher than 400 degrees Celsius, and use temperature in a vacuum is higher than
500 degrees Celsius.CN1360084A refers to a kind of absorbed layer and spatters in nitrogen, air atmosphere for negative electrode with titanium and alloy aluminum
The aluminium nitrogen penetrated+titanium nitrogen-aluminium titanium film and aluminum-nitrogen-oxygen+titanium-nitrogen-oxygen-aluminium titanium film, its antireflection layer is aluminium nitrogen+titanium nitrogen film and aluminum-nitrogen-oxygen
+ titanium-nitrogen-oxygen film, through 350 degrees Celsius under atmospheric condition, 250 hours, or 400 degrees Celsius, 50 hours, or 450 degrees Celsius,
After baking in 80 hours, its solar absorptance is all up more than 0.93, and emissivity is 0.06-0.10.
The reason causing current optical-thermal conversion material operating temperature to improve mainly has 2 points: one is that most of photo-thermal turns
Conversion materials contains the poor composition of temperature tolerance (such as nitrogen oxides, low temperature outside the materials such as oxide, nitride, carbide
Metal), spot corrosion is easily there is when more than 673K works；Two is thermally matched poor performance, and the material of especially more than three layers is difficult to
Overcome the thermal stress change that severe thermal shock under worst hot case causes, directly contribute cracking or peel off.
So, it is thus achieved that a kind of photothermal deformation that can take into account heat endurance and high-heating radiation rate in the environment of high temperature, high thermal shock
Material has important value to hi-temp hi-effective photo-thermal power generation technology.
Summary of the invention
It is an object of the invention to the weak point for overcoming prior art, it is provided that a kind of double-deck photothermal deformation composite and
Preparation method.The double-deck photothermal deformation composite that the present invention relates to sets for the base material of actual light hot-cast socket device
Meter, top layer active devices have selected current thermal emissivity rate and the strongest conventional oxide, carbide and the nitrogen of heat endurance
Compound, bottom transition zone have selected that radiance is higher, thermal coefficient of expansion between top layer active devices and base material and
The oxide that top layer active devices and base material are well combined, heat endurance is strong, to meet high temperature optical-thermal conversion material
The actual condition demand that thermal emissivity rate is high, thermal shock resistance is good.
A kind of double-deck photothermal deformation composite that the present invention provides, it is characterised in that: this composite includes bottom transition zone
With top layer active devices, the bottom transition zone of this composite and top layer active devices pass through one on base material
Fixed preparation method is sequentially prepared and forms, wherein bottom transition zone and base material, top layer active devices and bottom transition
Layer is to be joined directly together and connects.
Described base material is the one in Fe base, Ni base, Co base and Cr sill.
The composition of described bottom transition zone more than 80% is SiO2、ZrO2、Y2O3、TiO2In one or more.
The composition of described top layer high radiant rate layer more than 80% is one or more in SiC, C, TiC and BN.
Described bottom transition zone and top layer active devices thickness are 100nm to 5mm.
Described double-deck photothermal deformation composite is 0.5～0.8 in the full-specturm radiation rate of 300K, at the full-specturm radiation of 800K
Rate is 0.65～0.95.
The present invention also provides for a kind of method preparing above-mentioned double-deck photothermal deformation composite, it is characterised in that: first by substrate material
Material pre-processes so that base material oxide skin removes completely and surface roughness reaches more than 5nm；Then gas is passed through
Phase sedimentation or magnetron sputtering method prepare bottom transition zone；Then base material is heat-treated with bottom transition zone, in heat
Surface is repaired after completing by process；Top layer active devices is prepared again by vapour deposition process or magnetron sputtering method；Right
Double-deck photothermal deformation composite is heat-treated, and repairs surface after heat treatment completes, the double-deck photo-thermal of final acquisition
Conversion composite.
The operation principle of the present invention:
The material (such as SiC, C based material, ZrC, TiC and BN) that thermal emissivity rate is high, all there is firm molecular structure,
Thermal coefficient of expansion is relatively low.But in photo-thermal power generation field, in order to effectively realize the acting of solar energy heating medium, optical-thermal conversion material
The most all prepare on Metal Substrate base material.Owing to the material thermal expansion coefficient of metal_based material with high-heating radiation rate differs relatively
Greatly, optical-thermal conversion material is caused to be difficult with under high-temperature work environment.
The present invention utilizes heat radiation to be the feature of material intrinsic property, owing to the heat radiation of material is only by certain thickness surface
Material realizes light and hot conversion to the absorption of electromagnetic wave with radiation, and the surfacing in certain thickness uses intrinsic heat radiation
The material that rate is high is obtained with the high-heating radiation rate performance of integral material, so the present invention uses current thermal emissivity rate and heat steady
The strongest qualitative oxide, carbide and nitride are as top layer high-heating radiation layer material.
The present invention the most also utilizes the method for matched coefficients of thermal expansion, uses thermal coefficient of expansion between top layer high-heating radiation rate coating
With the way of the bottom transition zone of base material, reduce and produced in temperature changing process between integral composite and substrate
Thermal stress, improve composite thermal shock resistance.The present invention be additionally contemplates that simultaneously due to different materials density-of-states distribution not
With, determine that the surface material thickness of its overall thermal radiance performance is the most different, generally 100nm to 2mm, say, that the end
The thermal emissivity rate of layer buffer layer material is also possible to the thermal emissivity rate on integral composite and produces certain impact, so the present invention
The bottom transition zone selected is that radiance is higher, thermal coefficient of expansion is between top layer active devices and base material and top
Layer active devices and the oxide that base material is well combined, heat endurance is strong.
The double-deck photothermal deformation composite that the present invention relates to is entirely free of composition (C system the most ablated at a temperature of 873K
Material is non-graphite phase), and under finding at worst hot case in a series of high-heating radiation rate candidate materials thermally matched reasonably
Design of material scheme, is greatly improved 873K by the operating temperature of existing photothermal deformation composite from 573-673K.
To sum up, the double-deck light of stable performance under the present invention finally obtains a kind of operating temperature height, thermal emissivity rate height, high temperature thermal shock
Hot-cast socket composite.
Accompanying drawing explanation
Fig. 1 is double-deck photothermal deformation composite schematic diagram.
In accompanying drawing, the list of parts representated by each label is as follows:
1, base material, 2, bottom transition zone, 3, top layer active devices.
Detailed description of the invention
Below by detailed description of the invention, the present invention will be further described, but is not meant to the limit to scope
System.
Embodiment 1
On Ni sill, ZrO is prepared by physical vaporous deposition2-Y2O3/ SiC bilayer photothermal deformation composite:
Use the Ni alloy substrate of 300 × 300 sizes as base material；
Polishing successively Ni alloy substrate with the sand paper of 400 mesh, 800 mesh and 1200 mesh respectively, scale removal also ensures table
Surface roughness is at more than 10nm；
Ni alloy substrate after polishing is carried out 10min in water ultrasonically treated；
Use 40% ethanol solution and acetone soln clean successively ultrasonically treated after Ni alloy substrate surface；
Ni alloy substrate after being processed on surface is positioned in Pvd equipment, selects target ZrO2And Y2O3Simultaneously
Deposition, vacuum 7 × 10-3Pa, range 500mm, electronic beam current intensity 60mA, substrate deposition temperature 523K.Through anti-
Multiple deposition, obtaining thickness on Ni alloy substrate is the ZrO of 3mm2-Y2O3Bottom transition zone；
To deposit ZrO2-Y2O3The Ni alloy substrate of bottom transition zone is placed in Equipment for Heating Processing, with the intensification of 5K/min
Speed is heated to 1073K, is incubated 1h；It is cooled to 973K, 873K, 673K, during insulation with the cooling velocity of 2K/min
Between be 2h, subsequently with stove cool down；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 10nm, below 500nm；
Material after being polished on surface is placed in Pvd equipment, selects target SiC, vacuum 7 × 10-3Pa, target
Away from 500mm, electronic beam current intensity 40mA, substrate temperature 523K.Through repeatedly depositing, at ZrO2-Y2O3Bottom transition
The SiC top layer active devices that thickness is 2mm is obtained on layer；
The Ni alloy substrate depositing two-layer compound coating is placed in Equipment for Heating Processing, heats with the programming rate of 5K/min
To 873K, it is incubated 1h；Being cooled to 773K, 673K, 473K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 50nm；
Finally on Ni alloy substrate, obtain desired ZrO2-Y2O3/ SiC bilayer photothermal deformation composite.
Embodiment 2
On Fe sill, TiO is prepared by magnetron sputtering method and chemical vapour deposition technique2/ TiC bilayer photothermal deformation composite wood
Material:
Use the hemispherical Fe alloy substrate of a diameter of 50mm as base material；
Polishing successively Fe alloy substrate with the sand paper of 400 mesh, 800 mesh and 1200 mesh respectively, scale removal also ensures table
Surface roughness is at more than 5nm；
Fe alloy substrate after polishing is carried out 10min in water ultrasonically treated；
Use 40% ethanol solution and acetone soln clean successively ultrasonically treated after Fe alloy substrate surface；
Fe alloy substrate after being processed on surface is positioned in magnetron sputtering apparatus, uses metal Ti target, reacting gas O2,
Sputter gas Ar, reaction pressure 2Pa, underlayer temperature 573K, by Ar pre-sputtering 1min, Fe alloy substrate obtains
Thickness is the TiO of 50nm2Bottom transition zone；
By depositing Ti O2The Fe alloy substrate of bottom transition zone is placed in Equipment for Heating Processing, adds with the programming rate of 5K/min
Heat, to 973K, is incubated 1h；Being cooled to 873K, 773K, 673K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 500nm；
Material after being polished on surface is placed in chemical vapor depsotition equipment, and depositing temperature is 1323K, and furnace pressure is
0.1MPa, titanium source is TiCl4, carbon source is CH4, CH4It is passed directly in stove, TiCl4Bring in stove by hydrogen, then
At TiO2The TiC top layer active devices that thickness is 50nm is obtained on bottom transition zone；
The Fe alloy substrate depositing two-layer compound coating is placed in Equipment for Heating Processing, heats with the programming rate of 5K/min
To 973K, it is incubated 1h；Being cooled to 873K, 773K, 673K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 50nm；
Finally on Fe alloy substrate, obtain desired TiO2/ TiC bilayer photothermal deformation composite.
Embodiment 3
On Co sill, SiO is prepared by physical vaporous deposition and chemical vapour deposition technique2/ C bilayer photothermal deformation is combined
Material:
Use the Ni alloy substrate of 20 × 50 sizes as base material；
Polishing successively Co alloy substrate with the sand paper of 400 mesh, 800 mesh and 1200 mesh respectively, scale removal also ensures table
Surface roughness is at more than 10nm；
Co alloy substrate after polishing is carried out 10min in water ultrasonically treated；
Use 40% ethanol solution and acetone soln clean successively ultrasonically treated after Co alloy substrate surface；
Co alloy substrate after being processed on surface is positioned in Pvd equipment, selects target SiO2, vacuum
7×10-3Pa, range 500mm, electronic beam current intensity 60mA, substrate deposition temperature 473K.Through repeatedly depositing,
The SiO that thickness is 2 μm is obtained on Co alloy substrate2Bottom transition zone；
To deposit SiO2The Co alloy substrate of bottom transition zone is placed in Equipment for Heating Processing, with the programming rate of 5K/min
It is heated to 773K, is incubated 1h；Being cooled to 673K, 573K with the cooling velocity of 2K/min, temperature retention time is 2h, with
After with stove cool down；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 10nm, below 500nm；
Material after being polished on surface is placed in chemical vapor depsotition equipment, and carbon source is CH4, reacting gas H2, pressure 5Pa,
Plate spacing 90mm, plate pressure 1000V.Through repeatedly depositing, at SiO2The C that thickness is 2 μm is obtained on bottom transition zone
Film top layer active devices；
The Co alloy substrate depositing two-layer compound coating is placed in Equipment for Heating Processing, heats with the programming rate of 5K/min
To 873K, it is incubated 1h；Being cooled to 773K, 673K, 473K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 100nm；
Finally on Co alloy substrate, obtain desired SiO2/ C bilayer photothermal deformation composite.
Embodiment 4
On Cr sill, TiO is prepared by magnetron sputtering method2/ BN bilayer photothermal deformation composite
Use the circular Fe alloy substrate of a diameter of 40mm as base material；
Polishing successively Fe alloy substrate with the sand paper of 400 mesh, 800 mesh and 1200 mesh respectively, scale removal also ensures table
Surface roughness is at more than 5nm；
Fe alloy substrate after polishing is carried out 10min in water ultrasonically treated；
Use 40% ethanol solution and acetone soln clean successively ultrasonically treated after Fe alloy substrate surface；
Cr alloy substrate after being processed on surface is positioned in magnetron sputtering apparatus, uses metal Ti target, reacting gas O2,
Sputter gas Ar, reaction pressure 2Pa, underlayer temperature 573K, by Ar pre-sputtering 1min, Cr alloy substrate obtains
Thickness is the TiO of 500nm2Bottom transition zone；
By depositing Ti O2The Cr alloy substrate of bottom transition zone is placed in Equipment for Heating Processing, adds with the programming rate of 5K/min
Heat, to 973K, is incubated 1h；Being cooled to 873K, 773K, 673K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 500nm；
Material after being polished on surface is placed in magnetron sputtering apparatus, selection BN target, range 5cm, sputtering power 150W,
Underlayer temperature 673K, operating air pressure 1Pa, then at TiO2The BN top layer that thickness is 500nm is obtained on bottom transition zone
Active devices；
The Cr alloy substrate depositing two-layer compound coating is placed in Equipment for Heating Processing, heats with the programming rate of 5K/min
To 973K, it is incubated 1h；Being cooled to 873K, 773K, 673K with the cooling velocity of 2K/min, temperature retention time is 2h,
Cool down with stove subsequently；
With sand paper, is polished in surface after cooling so that surface roughness is at more than 5nm, below 200nm；
Finally on Cr alloy substrate, obtain desired TiO2/ BN bilayer photothermal deformation composite.
In aforementioned four embodiment, when the main component of top layer active devices and bottom transition zone accounts for more than 80%, logical
Cross rationally doping, still can realize or close to the expected performance of double-layer composite material.
Although it have been described that one or more embodiments of the present invention, nevertheless, it will be understood that, without departing from
The spirit and scope of the present invention, so that it may be variously modified.Therefore, other embodiments are intended to fall within the scope of the appended claims.
Claims (10)
1. a double-deck photothermal deformation composite, it is characterised in that: this composite include bottom transition zone and
Top layer active devices, the bottom transition zone of this composite and top layer active devices are on base material
Being sequentially prepared and form, wherein bottom transition zone and base material, top layer active devices are equal with bottom transition zone
Connect for being joined directly together；
The composition of described bottom transition zone more than 80% is SiO2、ZrO2、Y2O3、TiO2In one or
Several；
The composition of described top layer active devices more than 80% be the one in SiC, C, TiC and BN or
Several.
2. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: described base
Bottom material is the one in Fe base, Ni base, Co base and Cr sill.
3. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: double-deck photo-thermal
Change composite into ZrO2-Y2O3/ SiC ceramic matrix composite material, TiO2/ TiC composite, SiO2/ C composite
Or TiO2/ BN composite.
4. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: described bilayer
Photothermal deformation composite material surface roughness is at 5nm to 200nm.
5. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: the described end
Layer transition zone and top layer active devices thickness are 100nm to 5mm.
6. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: described is double
Layer photothermal deformation composite is 0.5～0.8 at the full spectrum thermal emissivity rate of 300K, and complete at 800K composes hot spoke
The rate of penetrating is 0.65～0.95.
7. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: described is double
The operating temperature of layer photothermal deformation composite is 800K to 1200K.
8. according to the double-deck photothermal deformation composite described in claim 1, it is characterised in that: when described top
When the main component of layer active devices and described bottom transition zone accounts for more than 80%, by rationally doping,
Still can realize or close to the expected performance of double-layer composite material.
9. a preparation method for the double-deck photothermal deformation composite as described in claim 1-8, its feature exists
In:
Step one, pre-processes base material so that base material oxide skin removes completely and surface is thick
Rugosity reaches more than 5nm；
Step 2, prepares bottom transition zone by vapour deposition process or magnetron sputtering method；
Step 3, is heat-treated with bottom transition zone base material, carries out surface after heat treatment completes
Finishing；
Step 4, prepares top layer active devices by vapour deposition process or magnetron sputtering method；
Step 5, is heat-treated double-deck photothermal deformation composite, carries out surface after heat treatment completes
Finishing, the double-deck photothermal deformation composite of final acquisition.
10. a preparation method for double-deck photothermal deformation composite as claimed in claim 9, its feature exists
In:
In described step one, polish successively described substrate material with the sand paper of 400 mesh, 800 mesh and 1200 mesh respectively
Material, scale removal also ensures that surface roughness is at more than 5nm；Base material after polishing is entered in water
Row is ultrasonically treated；Use 40% ethanol solution and acetone soln clean successively ultrasonically treated after base material.
In described step 5, described heat treatment step is that the alloy substrate of the two-layer compound coating deposited is placed in Re Chu
In reason equipment, it is heated to 973K with the programming rate of 5K/min, is incubated 1h；Cooling velocity with 2K/min
Being cooled to 873K, 773K, 673K, temperature retention time is 2h, cools down with stove subsequently.
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| 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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| 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 |
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