CN109536892A - A kind of high temperature film sensor heat shock resistance composite insulation layer and preparation method thereof - Google Patents

A kind of high temperature film sensor heat shock resistance composite insulation layer and preparation method thereof Download PDF

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CN109536892A
CN109536892A CN201910043549.1A CN201910043549A CN109536892A CN 109536892 A CN109536892 A CN 109536892A CN 201910043549 A CN201910043549 A CN 201910043549A CN 109536892 A CN109536892 A CN 109536892A
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yzralo
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CN109536892B (en
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赵晓辉
刘洋
熊杰
蒋洪川
张万里
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University of Electronic Science and Technology of China
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Abstract

A kind of high temperature film sensor heat shock resistance composite insulation layer, belongs to film sensor technologies field.The composite insulation layer is followed successively by thermally grown Al from bottom to top2O3Layer, YZrAlO layers, Al2O3Layer, wherein described YZrAlO layers includes amorphous Al2O3Film and disperse are in amorphous Al2O3Doped yttrium ZrO on film2It is nanocrystalline, doped yttrium ZrO2Nanocrystalline size is 10~40nm, element ratio Y:Zr:Al=1:6:(37~74 in YZrAlO layers).Disperse has doped yttrium ZrO in composite insulation layer of the present invention2It is nanocrystalline, ZrO2Nanocrystalline good particle dispersion strengthening and toughening and stress-induced phase transformation toughening effect, have been effectively ensured adhesive force and insulation performance under high temperature and severe thermal shock environment between insulating layer and alloy substrates.

Description

A kind of high temperature film sensor heat shock resistance composite insulation layer and preparation method thereof
Technical field
The invention belongs to film sensor technologies fields, mainly for the high temperature under high temperature, severe thermal shock environment that works Stress release problem between alloy surface thin film sensor insulating layer and alloy substrates specifically provides a kind of high temperature film sensing Device heat shock resistance composite insulation layer and preparation method thereof.
Background technique
Power device of the aero-engine as aviation aircraft, directly affect the safety of aircraft, reliability with Working life.Core component of the turbo blade as aero-engine, long-term work the high temperature of combustion chamber, high pressure, high stress, Under the extreme environment that severe thermal shock and air blast wash away, therefore, the hot-end components such as precise measurement turbo blade surface temperature The distributed intelligence of the parameters such as degree, stress is to the beforehand research experimental study and engineering development of aero-engine using most important.
Mainly there are thin film strain meter, film thermocouple in the thin film sensor that aero-engine hot-end component uses at present Deng.Wherein, the film thermocouple integrated with the parts to be tested, because it is small with size, response is fast, precision is high, to test Environmental disturbances are small, do not destroy many advantages, such as the parts to be tested mechanical structure, become the hot ends such as current aero engine turbine blades The main test mode of component surface temperature parameter.Film thermocouple generally passes through the conjunction of the high temperature such as multi-layer film structure and turbo blade Golden part integration is integrated, is followed successively by Ni based alloy substrate, NiCrAlY transition zone, thermally grown Al from bottom to top2O3Layer, insulation Layer, sensitive layer and protective layer, as shown in Figure 1.Wherein, insulating layer is mostly ceramic material, and ceramic material and alloy substrates heat are swollen Swollen coefficient difference is away from larger, since the micro-crack that stress release generates easily becomes the quick of metallic atom under high temperature and severe thermal shock Diffusion admittance, causing sensitive layer to be connected with alloy substrates makes sensor failure.And micro-crack can reduce insulating layer and alloy-based The adhesive force at bottom causes Sensor section to fall off in the case where air blast washes away.Therefore, it needs in high temperature, severe thermal shock, air blast Lower adhesive force good between alloy substrates is washed away, and keeps the insulating layer of good electrical insulation with substrate.
Common high temperature insulating material is Al2O3, but Al2O3Brittleness is high, be difficult to happen under stress plastic deformation and Dislocation movement by slip, therefore easily generate micro-crack under high temperature and thermal shock environments and be even broken, cause its high temperature to be applied by tight It limits again.Application No. is 200910131181.0, patent names are as follows: aluminum oxide toughening structure ceramic material and preparation method thereof Patent document in propose a kind of aluminum oxide toughening structure ceramic material, group becomes 78~85wt% of aluminium oxide, yttrium Stable Oxygen Change 13~20wt% of zirconium, 0.5~2wt% of titanium dioxide;Wherein yttrium stable zirconium oxide by 97mol% zirconium oxide and 3mol% Yttrium oxide composition;The fracture toughness of aluminum oxide toughening structure ceramic material obtained is 6.00~7.50MPam1/2, fracture Toughness compares simple Al2O3Material (3~4MPam1/2) be obviously improved.However, this patent is directed to block ceramic Toughening, it is completely different with nano-level thin-membrane insulating layer.In order to solve the problems, such as the stress release of insulating layer and alloy substrates, it is badly in need of The design and preparation method of composite isolated layer.
Summary of the invention
It is an object of the invention to propose that a kind of high temperature film sensor is used for defect present in above-mentioned background technique Heat shock resistance composite insulation layer and preparation method thereof, the composite insulation layer can guarantee sensitive layer and alloy-based at least at 1000 DEG C Good electrical isolation between bottom.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of high temperature film sensor heat shock resistance composite insulation layer, including 3-tier architecture, are followed successively by hot life from bottom to top Long Al2O3Layer, YZrAlO layers, Al2O3Layer, wherein described YZrAlO layers includes amorphous Al2O3Film and disperse are in amorphous Al2O3 Doped yttrium ZrO on film2It is nanocrystalline, doped yttrium ZrO2Nanocrystalline size is 10~40nm, element ratio Y in YZrAlO layers: Zr:Al=1:6:(37~74).
Wherein, described YZrAlO layers and Al2O3Layer is sequentially deposited at thermally grown Al using the methods of evaporation, sputtering2O3Layer On.
Further, described YZrAlO layers with a thickness of 0.5~2 μm.
A kind of preparation method of high temperature film sensor heat shock resistance composite insulation layer, specifically includes the following steps:
Step 1 posts the YZr alloys target of Al piece using surface as target, wherein atomic ratio Y:Zr=in YZr alloys target 1:6, Al piece cover YZr alloy target area 1/2~2/3, the flow-rate ratio of oxygen and argon gas be 1:(20~25), sputtering pressure It is 100~300W for 0.2~1Pa, sputtering power, under conditions of sputter temperature is 26~400 DEG C, using DC reactive sputtering Method is in thermally grown Al2O3The YZrAlO film that deposition thickness is 0.5~2 μm on layer;
Step 2, the Al for being not less than 99.99wt% with purity2O3Particle is 10 in vacuum degree as evaporation source-4~10- 5Under conditions of Pa, deposition rate are 0.2~1.5nm/s, depositing temperature is 26~400 DEG C, electronic beam current is 80~120mA, adopt 2~5 μm of Al is deposited on the YZrAlO film that step 1 obtains with the method for Electron beam evaporation2O3Film;
Step 3, YZrAlO layers and electron beam evaporation Al of band for obtaining step 22O3The composite substrate of layer is placed in heat-treatment furnace Interior, anneal 5~10h under the conditions of air atmosphere, 1000~1100 DEG C of temperature, and the composite insulation layer can be obtained.
A kind of thin film sensor is followed successively by alloy substrate, NiCrAlY alloy transition layer, composite insulation layer, thin from bottom to top Film sensors functional layer, Al2O3Protective layer, wherein the composite insulation layer is the composite insulation layer of above structure.
A kind of preparation method of thin film sensor, specifically includes the following steps:
The surface treatment of step 1, alloy substrate: alloy substrate surface is processed by shot blasting first, is then successively used Industrial degreaser, acetone, ethyl alcohol and deionized water clean the surface of alloy substrate, spare with being dried with nitrogen after cleaning;
The preparation of step 2, NiCrAlY alloy transition layer: using the method for d.c. sputtering by NiCrAlY alloy deposition in warp On step 1 treated alloy substrate, the composite substrate with NiCrAlY alloy transition layer is obtained, wherein NiCrAlY alloy mistake Cross layer with a thickness of 10~20 μm;
Step 3, thermally grown Al2O3The preparation of layer: the composite substrate obtained after step 2 processing is placed in heat-treatment furnace, 10-3Aluminium is analysed under the conditions of Pa vacuum environment below and 900 DEG C~1100 DEG C temperature handles 5~10h;Then, keep 900~ 1100 DEG C of temperature are simultaneously passed through oxygen to normal pressure, and 5~10h of oxidation processes, temperature control is cooled to room temperature to obtain band NiCrAlY alloy transition Layer and thermally grown Al2O3The composite substrate of layer;
Step 4, YZrAlO layers of preparation: the YZr alloys target of Al piece is posted as target using surface, wherein YZr alloys target Middle atomic ratio Y:Zr=1:6, Al piece cover the 1/2~2/3 of YZr alloy target area, are 1:(20 in the flow-rate ratio of oxygen and argon gas ~25) it under conditions of, sputtering pressure is 0.2~1Pa, sputtering power is 100~300W, sputter temperature is 26~400 DEG C, uses The method of the DC reactive sputtering YZrAlO that deposition thickness is 0.5~2 μm on the composite substrate obtained after step 3 processing is thin Film obtains YZrAlO layers;
Step 5, Al2O3The preparation of layer: it is not less than the Al of 99.99wt% with purity2O3Particle is as evaporation source, in vacuum Degree is 10-4~10-5Pa, deposition rate are 0.2~1.5nm/s, depositing temperature is 26~400 DEG C, electronic beam current be 80~ Under conditions of 120mA, 2~5 are deposited on the composite substrate obtained after step 4 processing using the method for Electron beam evaporation μm Al2O3Film;It then, will be with YZrAlO layers and electron beam evaporation Al2O3The composite substrate of layer is placed in heat-treatment furnace, Anneal 5~10h under the conditions of air atmosphere, 1000~1100 DEG C of temperature;
The preparation of step 6, thin film sensor functional layer: the composite substrate that step 5 is obtained is placed in vacuum cavity, is used The method of magnetron sputtering prepares thin film sensor functional layer on the composite substrate that step 5 obtains;
Step 7, Al2O3The preparation of protective layer: it is steamed using the method for electron beam evaporation on the surface of thin film sensor functional layer Plate the Al with a thickness of 1~5 μm2O3Protective layer;To obtain thin film sensor of the present invention.
Further, alloy substrate described in step 1 is nickel-base alloy substrate.
Further, Al is prepared described in step 72O3When protective layer, vacuum degree 10-4~10-5Pa, not using purity Al lower than 99.99wt%2O3Target.
Compared with prior art, the invention has the benefit that
1, in a kind of thin film sensor composite insulation layer provided by the invention, the YZrAlO layers of meeting after undergoing high annealing Grow the tetragonal phase doped yttrium ZrO of 10~40nm diameter2Equi-axed crystal is simultaneously distributed in even dispersion, as shown in Figure 2,3.Due to There are the ZrO of disperse2Particle potential barrier with higher, makes crackle diffusion hindered, improves energy to failure, to play good Particle dispersion strengthening and toughening effect;Meanwhile when stress results from or crackle diffuses to ZrO2When at particle, due to stress induced ZrO2Phase transformation is generated, the generation or diffusion of crackle are prevented, to play good stress-induced phase transformation toughening effect;It is good Particle dispersion strengthening and toughening and stress-induced phase transformation toughening effect, have been effectively ensured insulating layer under high temperature and severe thermal shock environment Adhesive force between alloy substrates.
2, in a kind of thin film sensor composite insulation layer provided by the invention, YZrAlO layers in through a long time high annealing Afterwards, the ZrO generated in YZrAlO film2Crystal grain has filled up most of hole and gap, and YZrAlO and aluminium oxide thermally expand Coefficients match, chemical bonding is close, therefore the crystal grain of growth in situ and alumina insulating layer interface cohesion are preferable;Meanwhile in height ZrO during temperature is YZrAlO layers lower2Particle can absorb stress and switch to monoclinic phase and volume increase by 4%~7%, thus effectively stop The diffusion and extension of micro-crack reduce the channel of metallic atom diffusion, to improve under high temperature and thermal shock environments The insulation performance of composite insulation layer.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of thin film sensor in background technique;
Fig. 2 is section electron microscope (SEM) figure for the YZrAlO layer that embodiment (b) and comparative example (a) obtain;
Fig. 3 is the X-ray diffractogram (XRD) of embodiment, the YZrAlO layer that comparative example obtains and Si substrate;Wherein, PDF#50-1089 is tetragonal phase ZrO2Standard PDF card;
Fig. 4 is that the insulation resistance for the Ni based alloy substrate with composite insulation layer that embodiment obtains varies with temperature curve Figure.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
A kind of preparation method of the thin film sensor based on composite insulation layer provided by the invention, specifically includes following step It is rapid:
The surface treatment of step 1, Ni based alloy substrate: alloy substrate surface is processed by shot blasting first, then successively It is cleaned using the surface of industrial degreaser, acetone, ethyl alcohol and deionized water to Ni based alloy substrate, is blown after cleaning with nitrogen Do spare, using plasma cleaning base plate before plated film;
The preparation of step 2, NiCrAlY alloy transition layer: using the method for d.c. sputtering by NiCrAlY alloy deposition in warp On step 1 treated Ni based alloy substrate, the composite substrate with NiCrAlY alloy transition layer is obtained, wherein NiCrAlY is closed Golden transition zone with a thickness of 10~20 μm;
Step 3, thermally grown Al2O3The preparation of layer: the composite substrate obtained after step 2 processing is placed in heat-treatment furnace, 10-3Aluminium is analysed under the conditions of Pa vacuum environment below and 900 DEG C~1100 DEG C temperature handles 5~10h;Then, keep 900~ 1100 DEG C of temperature are simultaneously passed through oxygen to normal pressure, 5~10h of oxidation processes, and temperature control is cooled to room temperature that (cooling rate control is 5~10 DEG C/min), obtain band NiCrAlY alloy transition layer and thermally grown Al2O3The composite substrate of layer;
Step 4, YZrAlO layers of preparation: the YZr alloys target of Al piece is posted as target using surface, wherein YZr alloys target Purity be not less than 99.99wt%, the 1/2 of atomic ratio Y:Zr=1:6, Al piece covering YZr alloy target area in YZr alloys target~ 2/3, be 1:(20~25 in the flow-rate ratio of oxygen and argon gas), sputtering pressure be 0.2~1Pa, sputtering power be 100~300W, Under conditions of sputter temperature is 26~400 DEG C, using the method for DC reactive sputtering in the composite base obtained after step 3 processing The YZrAlO film that deposition thickness is 0.5~2 μm on plate, obtains YZrAlO layers;
Step 5, Al2O3The preparation of layer: it is not less than the Al of 99.99wt% with purity2O3Particle is as evaporation source, in vacuum Degree is 10-4~10-5Pa, deposition rate are 0.2~1.5nm/s, depositing temperature is 26~400 DEG C, electronic beam current be 80~ Under conditions of 120mA, 2~5 are deposited on the composite substrate obtained after step 4 processing using the method for Electron beam evaporation μm Al2O3Film;It then, will be with YZrAlO layers and electron beam evaporation Al2O3The composite substrate of layer is placed in heat-treatment furnace, Anneal 5~10h under the conditions of air atmosphere, 1000~1100 DEG C of temperature;
The preparation of step 6, thin film sensor functional layer: the composite substrate that step 5 is obtained is placed in vacuum cavity, is used The method of magnetron sputtering prepares thin film sensor functional layer on the composite substrate that step 7 obtains;
Step 7, Al2O3The preparation of protective layer: it is steamed using the method for electron beam evaporation on the surface of thin film sensor functional layer Plate the Al with a thickness of 1~5 μm2O3Protective layer;It is not less than the Al of 99.99wt% with purity2O3Particle is as evaporation source, in vacuum Degree is 10-4~10-5Pa, deposition rate are 0.2~1.5nm/s, depositing temperature is 26~400 DEG C, electronic beam current be 80~ Under conditions of 120mA, 2~5 are deposited on the composite substrate obtained after step 4 processing using the method for Electron beam evaporation μm Al2O3Film;To obtain thin film sensor of the present invention.
Embodiment
Using Ni based alloy as substrate, the composite insulation layer in the present invention is prepared on it and prepares Pt electrode on the insulating layer For, comprising the following steps:
The surface treatment of step 1, Ni based alloy substrate: substrate surface is processed by shot blasting first, is then successively used Industrial degreaser, acetone, ethyl alcohol and deionized water carry out being cleaned by ultrasonic each 15min to the surface of Ni based alloy substrate, use nitrogen 30min is dried after rifle drying at 200 DEG C and removes residual moisture, using plasma cleaning base plate about 5min before plated film;
The preparation of step 2, NiCrAlY alloy transition layer: it is true that the Ni based alloy substrate that step 1 cleans up is placed in back end Reciprocal of duty cycle is 5.0 × 10-4In the vacuum environment of Pa, using NiCrAlY alloys target as target, sputter gas is Ar, sputtering pressure is Under conditions of 0.4Pa, sputtering power 200W, base reservoir temperature are 450 DEG C, using the method for d.c. sputtering by NiCrAlY alloy It is deposited on through on step 1 treated nickel-base alloy substrate, deposited film thickness is about 16 μm, obtains covering NiCrAlY alloy The composite substrate of transition zone;
Step 3, thermally grown Al2O3The preparation of layer: the composite substrate obtained after step 2 processing is placed in heat-treatment furnace, 5 × 10-4It is warming up to 1050 DEG C under the vacuum condition of Pa, with the rate of 5 DEG C/min, and analyses aluminium processing at a temperature of 1050 DEG C 6h;Then, 1050 DEG C of temperature are kept and are passed through oxygen to normal pressure, oxidation processes 6h stops heating and continues to be passed through oxygen, with 5 DEG C/the rate temperature control of min is cooled to room temperature only, obtain surface covering NiCrAlY alloy transition layer and thermally grown Al2O3Layer is answered Close substrate;
Step 4, YZrAlO layers of preparation: the YZr alloys target of Al piece is posted as target using surface, wherein YZr alloys target Purity be not less than 99.99wt%, the 2/3 of atomic ratio Y:Zr=1:6, Al piece covering YZr alloy target area in YZr alloys target, It is 4 × 10 in vacuum degree-4Under the vacuum condition of Pa, being passed through gas flow ratio is O2: the mixed gas of Ar=1:24, sputtering pressure 0.4Pa provides sputtering power to target using direct current power source, and sputtering power 120W, sputtering time 5h are handled through step 3 About 1.5 μm of deposition thickness of YZrAlO film on the composite substrate obtained afterwards;
Step 5, Al2O3The preparation of layer: it is not less than the Al of 99.99wt% with purity2O3Particle is as evaporation source, in vacuum Degree is 8 × 10-5Under conditions of Pa, deposition rate 0.5nm/s, depositing temperature are 26 DEG C, electronic beam current is 100mA, using electricity The Al of the method for beamlet vacuum coating 2 μm of deposition on the composite substrate obtained after step 4 processing2O3Film;Then, by band YZrAlO layers and electron beam evaporation Al2O3The composite substrate of layer is placed in heat-treatment furnace, in air atmosphere, 1050 DEG C of temperature conditions Lower annealing 6h;
The preparation of step 6, Pt electrode: it is 5.0 × 10 that the composite substrate after step 5 annealing, which is placed in back end vacuum degree,-4Pa Vacuum environment in, using Pt target as target, sputter gas be Ar, sputtering pressure 0.4Pa, sputtering power 90W, substrate temperature Under conditions of degree is 26 DEG C, the Pt electricity for being about 200nm by the thickness of 5mm × 5mm using the method for d.c. sputtering and hard mask Pole is deposited on the composite substrate after step 5 annealing;To obtain the Ni based alloy with composite insulation layer of the present invention Substrate simultaneously prepares Pt electrode on the insulating layer.
Comparative example
Using Ni based alloy as substrate, the composite insulation layer in the present invention is prepared on it, preparation process is the same as embodiment difference It is, the YZr alloys target of Al piece is posted on surface in step 4, and Al piece covers the 1/8 of YZr alloy target area.
The structure of the composite insulation layer of preparation of the embodiment of the present invention is tested and is analyzed with performance below:
Fig. 2 is section electron microscope (SEM) figure for the YZrAlO layer that embodiment (b) and comparative example (a) obtain;Wherein, Comparative example film has more gap and hole, and crystal grain is high-visible, and crystallite dimension is 40~70nm, and embodiment film is opposite Densification is difficult to find out obvious crystal grain in figure.
Fig. 3 is the X-ray diffractogram (XRD) of embodiment, the YZrAlO layer that comparative example obtains and Si substrate;Wherein, PDF#50-1089 is tetragonal phase ZrO2Standard PDF card;Show that the YZrAlO layer that embodiment obtains is that 10~40nm of band yttrium is mixed Miscellaneous ZrO2Nanocrystalline amorphous Al2O3Film.
Fig. 4 is that the insulation resistance for the Ni based alloy substrate with composite insulation layer that embodiment obtains varies with temperature curve Figure;As shown in Figure 4, for the insulating layer that embodiment obtains in room temperature within the scope of 1000 DEG C, insulation resistance is in approximate index variation rule Rule, insulation resistance is greater than 100K Ω at 1000 DEG C, this illustrates that insulating layer has good insulation performance within the scope of less than 1000 DEG C, It can satisfy being electrically insulated between device and metallic substrates.

Claims (6)

1. a kind of high temperature film sensor heat shock resistance composite insulation layer, including 3-tier architecture, are followed successively by thermally grown from bottom to top Al2O3Layer, YZrAlO layers, Al2O3Layer, wherein described YZrAlO layers includes amorphous Al2O3Film and disperse are in amorphous Al2O3It is thin Doped yttrium ZrO on film2It is nanocrystalline, doped yttrium ZrO2Nanocrystalline size is 10~40nm, element ratio Y:Zr in YZrAlO layers: Al=1:6:(37~74).
2. high temperature film sensor heat shock resistance composite insulation layer according to claim 1, which is characterized in that described YZrAlO layers and Al2O3Layer is sequentially deposited at thermally grown Al using evaporation or sputtering method2O3On layer.
3. high temperature film sensor heat shock resistance composite insulation layer according to claim 1, which is characterized in that described YZrAlO layers with a thickness of 0.5~2 μm.
4. a kind of preparation method of high temperature film sensor heat shock resistance composite insulation layer, specifically includes the following steps:
Step 1 posts the YZr alloys target of Al piece using surface as target, wherein atomic ratio Y:Zr=1:6 in YZr alloys target, Al piece cover YZr alloy target area 1/2~2/3, be 1:(20~25 in the flow-rate ratio of oxygen and argon gas), sputtering pressure be Under conditions of 0.2~1Pa, sputtering power are 100~300W, sputter temperature is 26~400 DEG C, using the side of DC reactive sputtering Method is in thermally grown Al2O3The YZrAlO film that deposition thickness is 0.5~2 μm on layer;
Step 2, with Al2O3Particle is 10 in vacuum degree as evaporation source-4~10-5Pa, deposition rate be 0.2~1.5nm/s, Under conditions of depositing temperature is 26~400 DEG C, electronic beam current is 80~120mA, using the method for Electron beam evaporation in step 2~5 μm of Al is deposited on rapid 1 obtained YZrAlO film2O3Film;
Step 3, YZrAlO layers and electron beam evaporation Al of band for obtaining step 22O3The composite substrate of layer is placed in heat-treatment furnace, Anneal 5~10h under the conditions of air atmosphere, 1000~1100 DEG C of temperature, and the composite insulation layer can be obtained.
5. a kind of thin film sensor is followed successively by alloy substrate, NiCrAlY alloy transition layer, composite insulation layer, film from bottom to top Sensor function layer, Al2O3Protective layer, wherein the composite insulation layer is compound inslation described in any one of claims 1 to 4 Layer.
6. a kind of preparation method of thin film sensor, specifically includes the following steps:
The surface treatment of step 1, alloy substrate: being first processed by shot blasting alloy substrate surface, then successively using industry Degreaser, acetone, ethyl alcohol and deionized water clean the surface of alloy substrate, spare with being dried with nitrogen after cleaning;
The preparation of step 2, NiCrAlY alloy transition layer: using the method for d.c. sputtering by NiCrAlY alloy deposition in through step On 1 treated alloy substrate, the composite substrate with NiCrAlY alloy transition layer is obtained, wherein NiCrAlY alloy transition layer With a thickness of 10~20 μm;
Step 3, thermally grown Al2O3The preparation of layer: the composite substrate obtained after step 2 processing is placed in heat-treatment furnace, 10-3Aluminium is analysed under the conditions of Pa vacuum environment below and 900 DEG C~1100 DEG C temperature handles 5~10h;Then, 900~1100 are kept DEG C temperature is simultaneously passed through oxygen to normal pressure, 5~10h of oxidation processes, temperature control be cooled to room temperature to obtain band NiCrAlY alloy transition layer and Thermally grown Al2O3The composite substrate of layer;
Step 4, YZrAlO layers of preparation: the YZr alloys target of Al piece is posted as target using surface, wherein YZr alloys target Central Plains Son ratio Y:Zr=1:6, Al piece cover YZr alloy target area 1/2~2/3, the flow-rate ratio of oxygen and argon gas be 1:(20~ 25) under conditions of, sputtering pressure is 0.2~1Pa, sputtering power is 100~300W, sputter temperature is 26~400 DEG C, using straight The method YZrAlO that deposition thickness is 0.5~2 μm on the composite substrate obtained after step 3 processing for flowing reactive sputtering is thin Film obtains YZrAlO layers;
Step 5, Al2O3The preparation of layer: it is not less than the Al of 99.99wt% with purity2O3Particle is as evaporation source, in vacuum degree 10-4~10-5Pa, deposition rate are 0.2~1.5nm/s, depositing temperature is 26~400 DEG C, electronic beam current is 80~120mA's Under the conditions of, 2~5 μm are deposited on the composite substrate obtained after step 4 processing using the method for Electron beam evaporation Al2O3Film;It then, will be with YZrAlO layers and electron beam evaporation Al2O3The composite substrate of layer is placed in heat-treatment furnace, in atmosphere Anneal 5~10h under the conditions of atmosphere, 1000~1100 DEG C of temperature;
The preparation of step 6, thin film sensor functional layer: the composite substrate that step 5 is obtained is placed in vacuum cavity, using magnetic control The method of sputtering prepares thin film sensor functional layer on the composite substrate that step 5 obtains;
Step 7, Al2O3The preparation of protective layer: thickness is deposited on the surface of thin film sensor functional layer using the method for electron beam evaporation The Al that degree is 1~5 μm2O3Protective layer;To obtain thin film sensor of the present invention.
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