CN107201502A - A kind of high temperature film sensor with self-healing composite armor and preparation method thereof - Google Patents

A kind of high temperature film sensor with self-healing composite armor and preparation method thereof Download PDF

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CN107201502A
CN107201502A CN201710311816.XA CN201710311816A CN107201502A CN 107201502 A CN107201502 A CN 107201502A CN 201710311816 A CN201710311816 A CN 201710311816A CN 107201502 A CN107201502 A CN 107201502A
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self
layer
composite armor
ysio
healing
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蒋洪川
王洪敏
刘子良
赵晓辉
蒋书文
张万里
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0664—Carbonitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5806—Thermal treatment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M15/00—Testing of engines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
    • Y02T50/00—Aeronautics or air transport
    • Y02T50/60—Efficient propulsion technologies, e.g. for aircraft

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Abstract

The invention belongs to sensor technical field there is provided a kind of high temperature film sensor with self-healing composite armor and preparation method thereof, to realize sensor miniaturization, filming application；Thin film sensor of the present invention is made up of the substrate, thin film sensor sensitive function layer and self-healing composite armor set gradually from bottom to top, wherein, the structure of the self-healing composite armor is followed successively by YSiO/HfSiBCN periodic multilayer membrane structures from bottom to top, and the orlop of overcoat and the superiors are YSiO hypoxemia diffusion coefficient layer.The present invention is using the self-cure type composite armor with periodic multilayer membrane structure, YSiO hypoxemia diffusion coefficient layer and the antioxidant defense system of HfSiBCN self-healings layer alternating deposit formation " setting up defenses in depth ", so that thin film sensor be able to can work long hours under 600 DEG C~1500 DEG C hot conditions, have the advantages that high temperature resistant, corrosion-resistant, anti-oxidant, response are rapid.

Description

A kind of high temperature film sensor with self-healing composite armor and preparation method thereof
Technical field
The invention belongs to sensor guard technical field, and in particular to a kind of high temperature film with self-healing composite armor Sensor and preparation method thereof.
Background technology
Aero-engine is described as the heart of aviation aircraft.When modern aeroengine works, turbo blade, combustion chamber In the adverse circumstances such as high temperature, the high pressure being in Deng hot junction structure member produced by fuel oil burns, whirlpool under accurate measurement working condition The performance parameter distribution situations such as temperature, strain, the hot-fluid on the hot-end component surface such as impeller blade, combustion chamber are set to aero-engine Count, verify, optimize it is most important.
Compared with traditional sensor, thin film sensor has size small (thickness is μm magnitude), fast response time, array The advantages of changing distribution measuring, smaller influenceed on the parts to be tested and test environment, the special-shaped fine structure in fields such as Aeronautics and Astronautics Part parameter technical field of measurement and test has broad application prospects.However, in the end pieces such as aero-engine heat parameter testing neck Domain, commonly uses the sensor sensing materials such as temperature, strain, hot-fluid, there is the metals such as NiCr, NiSi, Pt, PtRh, PdCr, WRe or conjunction Gold, the sensitive oxide material such as nitride and ITO such as TaN.Under the oxygen-enriched severe corrosive environmental conditions of grade of HTHP, on State these sensitive materials to be oxidized easily and fail, or influenceed to cause performance not by high-temperature fuel gas component (such as partial pressure of oxygen) Break and fail and can not use.Conventional high temperature finishes materials A l2O3, although it is good and low with high-melting-point, anti-oxidant, heat endurance The characteristics such as diffusion coefficient, but Al2O3Film is in preparation process or in the severe ring such as the severe high temperature of aero-engine, thermal shock Under the conditions of border, Al2O3Protective layer may induce generation micro-crack due to stress, and crackle turns into oxygen diffusion admittance so that The coefficient of dispersion of protective layer antioxygenic property is very big, reliability reduction, and then causes component failure；Meanwhile, Al2O3Chemistry it is steady The qualitative corrosive atmosphere for being not enough to resist aero-engine high-temperature fuel gas for a long time.Therefore, to realize sensor miniaturization, it is thin Membranization application, protective layer of the exploitation with characteristics such as good high temperature resistant, corrosion-resistant, inoxidizability, chemical compatibilities is to turn into The key solved the problems, such as.
The content of the invention
It is an object of the invention to the demand for above technical background, it is proposed that a kind of with self-healing composite armor High temperature film sensor and preparation method thereof.High temperature film sensor is by substrate, thin film sensor sensitive function layer and self-healing Composite armor is constituted, and the self-healing composite armor in the present invention has YSiO/HfSiBCN periodic multilayer membrane structures, As shown in figure 1, its orlop and the superiors are YSiO hypoxemia diffusion coefficient layer.YSiO films have high-melting-point, hypoxemia diffusion The characteristic such as coefficient, low vaporization at high temperature rate, resistant to chemical etching, is a kind of Environmental Barrier Coatings on Si-based Ceramics of good performance；HfSiBCN films have Good insulating properties, antioxygenic property, the sticky B of oxidation generation under the conditions of high-temperature oxygen-enriched2O3、SiO2Glass phase, the two can shape Into pyrex, as healing phase, the crackle and defect filled, healed in overcoat under capillary force action.YSiO is low Diffusion coefficient layer and the antioxidant defense system of HfSiBCN self-healings layer alternating deposit formation " setting up defenses in depth ", to overcome The problem of thin film sensor is oxidized easily under the oxygen-enriched grade environment of HTHP and causes performance degradation or even fail, so that real Existing sensor miniaturization, filming application；Thin film sensor with self-healing composite armor in the present invention can 600 DEG C~ It can be worked long hours under 1500 DEG C of high temperature oxidizing conditions, have the advantages that high temperature resistant, corrosion-resistant, anti-oxidant, response are rapid.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of band self-healing composite armor thin film sensor, by substrate, the thin film sensor set gradually from bottom to top Sensitive function layer and self-healing composite armor are constituted, it is characterised in that the structure of the self-healing composite armor is under And on be followed successively by：YSiO/HfSiBCN periodic multilayer membrane structures, as shown in figure 1, wherein, the orlop of overcoat and most upper Layer is YSiO hypoxemia diffusion coefficient layer.
Further, periodicity n span is in the self-healing composite armor：n≥2.
The thickness of the orlop YSiO hypoxemia diffusion coefficient layer is 1~5 μm, with cover film sensor sensing function Layer；The thickness range of other film layers of self-healing composite armor is 10nm~1 μm.
The substrate is the ceramic substrates such as aluminum oxide, silicon nitride, carborundum, can also be closed for the Ni bases with insulating barrier Golden substrate.
The preparation method of the above-mentioned thin film sensor with self-healing composite armor, including step are as follows：
The pretreatment of step 1. substrate：For ceramic substrates such as aluminum oxide, silicon nitride, carborundum, using acetone, wine Essence and deionized water are successively cleaned by ultrasonic to ceramic substrate surface and dried up with nitrogen gun, then using plasma cleaning； For Ni based alloy substrates, first Ni base superalloy substrates are cleaned by ultrasonic and plasma clean, then in the super conjunction of Ni bases NiCrAlY alloy transitions layer, thermally grown Al are sequentially depositing on golden substrate2O3Layer, Al2O3Insulating barrier, obtains compound substrate, realizes It is electrically insulated between metal substrate and thin film sensor functional layer；
The preparation of step 2. thin film sensor sensitive function layer：Using film preparing technology and patterning process, by film Sensor sensing function is deposited in the dielectric substrate after being handled through step 1, so as to obtain thin film sensor sensitive function layer；
The preparation of step 3.YSiO hypoxemia diffusion coefficient layer：With Y2SiO5Ceramics are target, using rf magnetron sputtering side Method, the sputtering YSiO hypoxemia diffusion coefficient layer on thin film sensor sensitive function layer, and the sensitive work(of thin film sensor is completely covered Ergosphere；Specific process parameter is：Back end vacuum is 5 × 10-4Below Pa, operating air pressure is 0.6~1.0Pa, and sputter gas is O2/ Ar mixed gas, wherein O2Volume fraction 1%~5%, sputtering power is 100~200W, and underlayer temperature is 200~300 DEG C, Sputtering time is controlled, it is 1~5 μm to prepare YSiO hypoxemia diffusion coefficient thickness degree；
The preparation of step 4.HfSiBCN self-healings layer：In B4C target material surfaces symmetrically mount the Hf pieces and Si pieces of same thickness Target is inlayed in formation, inlays target in sputter area inner area relation than meeting：B4C:Hf:Si=65%:15%:20%；Adopt With radio frequency magnetron sputtering method, HfSiBCN self-healings layer is deposited on YSiO hypoxemia diffusion coefficient layer, specific process parameter is： Back end vacuum is 5 × 10-4Below Pa, sputtering pressure is 0.4~0.8Pa, and sputter gas is N2/ Ar=2:8~3:7 gaseous mixtures Body, sputtering power is 100~200W, and underlayer temperature is 400~500 DEG C, controls sputtering time, prepares HfSiBCN self-healings layer Thickness be 10nm~1 μm；
The preparation of step 5. periodic multilayer film and annealing：On the basis of through step 4, step 3, step 4 are kept Technological parameter is constant, repeat step 3, step 4 process, and YSiO hypoxemia diffusion coefficient layer and HfSiBCN self-healings are alternately prepared successively Close layer, and ensure that the superiors are YSiO hypoxemia diffusion coefficient layer, manufacturing cycle number n >=2, wherein, prepared by this step YSiO hypoxemia diffusion coefficient layer and HfSiBCN self-healings layer thickness range are 10nm~1 μm；Then, it is placed on vacuum annealing Made annealing treatment in stove, reduce membrane stress, back end vacuum is 5 × 10-4Below Pa, annealing temperature is 900~1100 DEG C, Annealing soaking time is 1~2h；
The thin film sensor with self-healing composite armor is prepared into, wherein step 3~5 are oneself in the present invention Heal composite armor preparation method.
Beneficial effects of the present invention are：
1st, in the present invention, protective layer is the self-healing composite armor with periodic multilayer membrane structure, YSiO hypoxemia Diffusion coefficient layer and the anti-oxidative defense system of HfSiBCN self-healings layer alternating deposit formation " setting up defenses in depth "；Periodic multilayer Membrane structure can make composite armor in preparation process or the severe Service Environment such as high temperature thermal shock under, can because discharging stress The crackle produced can be induced to deflect in the different component interface of multi-component multi-layer structure, it is to avoid form large-sized penetrability Crackle and lose safeguard function, and extend the diffusion path of oxygen；The size with crack can also be regulated and controled simultaneously, raising is split Line healing efficiency, so as to strengthen the antioxygenic property of protective layer, increases the service life.Self-healing composite armor in the band present invention Thin film sensor be able to can be worked long hours under 600 DEG C~1500 DEG C high temperature oxidizing conditions, with high temperature resistant, it is corrosion-resistant, It is anti-oxidant, respond it is rapid the advantages of.
2nd, in the present invention, YSiO films there is high-melting-point, it is hypoxemia diffusion coefficient, low vaporization at high temperature rate, resistant to chemical etching Etc. characteristic, it is a kind of Environmental Barrier Coatings on Si-based Ceramics of good performance, is placed in outermost layer, oxygen gas and water in environment can be effectively resisted at high temperature The erosion of the corrosive mediums such as steam, salt；Meanwhile, YSiO films can make HfSiBCN films isolate high keto sectional pressure environment, so that greatly Width reduces its oxidation rate, increases the service life.
3rd, in the present invention, HfSiBCN films have good mechanical performance, insulating properties, in less than 1500 DEG C high temperature There is good antioxygenic property, its antioxygenic property is better than HfB under the conditions of oxidation environment2- SiC superhigh temperature composite ceramics is applied Layer, oxidated layer thickness is smaller under identical oxidizing condition；Oxidation generates sticky B under the high temperature conditions2O3、SiO2Glass phase, the two Pyrex can be formed, as healing phase, under capillary force action fill, heal compound anti-oxidation layer in crackle and lack Fall into, and in film surface formation protective layer, stop that oxygen further internally spreads.
Brief description of the drawings
Fig. 1 is self-healing composite armor structural representation (sectional view) in the present invention.
Fig. 2 is the structural representation (sectional view) with self-healing composite armor W-Re thin film sensor in the present invention；Its In：1 is substrate, and 2 be the positive and negative thermode of W-Re film thermocouple, and 3 be self-healing composite armor.
Embodiment
The present invention is described in further details with implementation below in conjunction with the accompanying drawings.
A kind of W-Re film thermocouple with self-healing composite armor is provided in the present embodiment, set successively by from bottom to top The Al put2O3The positive negative thermal electrode of ceramic substrate, film thermocouple and self-healing composite armor are constituted, and the self-healing is compound anti- The structure of sheath is followed successively by from bottom to top：YSiO/HfSiBCN periodic multilayer membrane structures, wherein, periodicity n=5, overcoat Orlop and the superiors be YSiO hypoxemia diffusion coefficient layer.
The above-mentioned specific preparation process with self-healing composite armor W-Re film thermocouple is：
Step 1, Al2O3The pretreatment of ceramic substrate：To Al2O3Ceramic substrate surface is cleaned, using acetone, alcohol With deionized water successively to Al2O3The surface of ceramic substrate carries out being cleaned by ultrasonic each 15min, then is dried up with nitrogen gun, drying residual Using plasma cleaning substrate 5min before moisture, plated film；
The preparation of step 2, the positive negative thermal electrode of W-Re film thermocouple：With tungsten-rhenium alloy (WRe5/26) for target, using straight The method for the hard mask version that stream magnetron sputtering matches with Z-shaped hole slot, by Wolfram rhenium heat electric couple positive pole and negative pole priority It is deposited on the Al after being handled through step 12O3In ceramic substrate, using technological parameter：Back end vacuum 5 × 10-4Pa, work Air pressure 0.4Pa, sputtering power 100W, sputter gas Ar flow are 25sccm, control the parameters such as sputtering time, prepare W-Re thin The thickness of film thermocouple both positive and negative polarity is about 2 μm；
It is prepared by step 3, YSiO hypoxemia diffusion coefficient layer：The ceramic liner of the W-Re film thermocouple obtained after through step 2 On bottom, with HIP sintering Y2SiO5For target, sputtered using the method for rf magnetron sputtering in Wolfram rhenium heat electric couple functional layer YSiO hypoxemia diffusion coefficient layer, and Wolfram rhenium heat electric couple functional layer is completely covered；Using technological parameter：Back end vacuum 4 × 10- 4Pa, operating air pressure 0.6Pa, sputter gas O2/ Ar mixed gas, wherein O2Volume fraction 3%, sputtering power 150W, substrate temperature 300 DEG C of degree, controls sputtering time, it is about 3 μm to be prepared into YSiO hypoxemia diffusion coefficient thickness degree；
The preparation of step 4, HfSiBCN self-healings layer：After step 3 has deposited YSiO hypoxemia diffusion coefficient layer, use Target is in B4C targets symmetrically mount thickness identical Hf pieces and target is inlayed in the formation of Si pieces, and it is closed in sputter area inner area System's ratio meets B4C:Hf:Si=65%:15%:20%；Using radio frequency magnetron sputtering method, on YSiO hypoxemia diffusion coefficient layer HfSiBCN self-healings layer is deposited, using technological parameter：Back end vacuum is 3 × 10-4Pa, operating air pressure 0.5Pa, sputter gas Constitute as N2/ Ar=2:8 mixed gas, sputtering power 100W, 450 DEG C of underlayer temperature controls the technological parameters such as sputtering time, system The thickness of standby HfSiBCN self-healings layer is about 0.6 μm；
Step 5, the preparation of periodic multilayer film and annealing：On the basis of through step 4, step 3,4 preparation are kept Technological parameter is constant, repeat step 3, step 4 process, continues to be sequentially prepared YSiO hypoxemia diffusion coefficient layer and HfSiBCN self-healings Close layer, and ensure that outermost layer is YSiO hypoxemia diffusion coefficient layer, manufacturing cycle number n=5, wherein, this step is preparation-obtained YSiO hypoxemia diffusion coefficient thickness degree is about 0.3 μm, and HfSiBCN self-healing thickness degree is about 0.6 μm；Then, place it in Made annealing treatment in vacuum annealing furnace, reduce membrane stress, back end vacuum 5 × 10-4Pa, 1000 DEG C of annealing temperature, annealing Time 2h；
So as to prepare the W-Re film thermocouple with self-healing composite armor.
The foregoing is only a specific embodiment of the invention, any feature disclosed in this specification, except non-specifically Narration, can alternative features equivalent by other or with similar purpose replaced；Disclosed all features or all sides Method or during the step of, in addition to mutually exclusive feature and/or step, can be combined in any way.

Claims (5)

1. a kind of high temperature film sensor with self-healing composite armor, is passed by the substrate, the film that set gradually from bottom to top Sensor sensitive function layer, self-healing composite armor are constituted；Characterized in that, the self-healing composite armor is by YSiO The periodic multilayer thin film system that hypoxemia diffusion coefficient layer and HfSiBCN self-healings layer alternating deposit are constituted, i.e. YSiO/ HfSiBCN periodic multilayer films, wherein, the orlop of self-healing composite armor and the superiors are YSiO hypoxemia diffusion coefficients Layer.
2. the high temperature film sensor with self-healing composite armor as described in claim 1, it is characterised in that the self-healing Periodicity >=2 of composite armor.
3. the high temperature film sensor with self-healing composite armor as described in claim 1, it is characterised in that the self-healing In composite armor, orlop YSiO hypoxemia diffusion coefficient thickness degree is 1~5 μm, and thin film sensor sensitive function is completely covered Layer；Other thin film layer thickness of self-healing composite armor are 10nm~1 μm.
4. the high temperature film sensor with self-healing composite armor as described in claim 1, it is characterised in that the substrate is Aluminum oxide, silicon nitride, carborundum or the Ni based alloy substrates with insulating barrier.
5. the preparation method with self-healing composite armor high temperature film sensor as described in claim 1, including step are as follows：
The pretreatment of step 1. substrate：For ceramic substrates such as aluminum oxide, silicon nitride, carborundum, using acetone, alcohol and Deionized water is successively cleaned by ultrasonic to ceramic substrate surface and dried up with nitrogen gun, then using plasma cleaning；For Ni based alloy substrates, are first cleaned by ultrasonic and plasma clean to Ni base superalloy substrates, are then served as a contrast in Ni base superalloys NiCrAlY alloy transitions layer, thermally grown Al are sequentially depositing on bottom2O3Layer, Al2O3Insulating barrier, obtains compound substrate, realizes metal It is electrically insulated between substrate and thin film sensor sensitive function layer；
The preparation of step 2. thin film sensor sensitive function layer：Using film preparing technology and patterning process, by sensitive function Layer is deposited in the dielectric substrate after being handled through step 1, so as to obtain thin film sensor sensitive function layer；
The preparation of step 3.YSiO hypoxemia diffusion coefficient layer：With Y2SiO5Ceramics are target, using radio frequency magnetron sputtering method, The upper sputtering sedimentation YSiO hypoxemia diffusion coefficient layer of thin film sensor sensitive function layer obtained through step 2, and sensitivity is completely covered Functional layer；Specific process parameter is：Back end vacuum is 5 × 10-4Below Pa, operating air pressure is 0.6~1.0Pa, sputter gas For O2/ Ar mixed gas, wherein O2Volume fraction 1%~5%, sputtering power is 100~200W, and underlayer temperature is 200~300 DEG C, sputtering time is controlled, it is 1~5 μm to prepare YSiO hypoxemia diffusion coefficient thickness degree；
The preparation of step 4.HfSiBCN self-healings layer：In B4C target material surfaces symmetrically mount thickness identical Hf pieces and Si pieces are formed Target is inlayed, target is inlayed in sputter area inner area relation than meeting：B4C:Hf:Si=65%:15%:20%；Using penetrating Frequency magnetically controlled sputter method, the deposition HfSiBCN self-healing layers on the YSiO hypoxemia diffusion coefficient layer obtained through step 3；Specific work Skill parameter is：Back end vacuum is 5 × 10-4Below Pa, operating air pressure is 0.4~0.8Pa, and sputter gas is N2/ Ar=2:8~ 3:7 mixed gas, sputtering power is 100~200W, and underlayer temperature is 400~500 DEG C, controls sputtering time, prepares HfSiBCN The thickness of self-healing layer is 10nm~1 μm；
The preparation of step 5. periodic multilayer film and annealing：On the basis of through step 4, step 3,4 technological parameter are kept Constant, repeat step 3, step 4 process alternately prepare YSiO hypoxemia diffusion coefficient layer and HfSiBCN self-healings layer successively, and really It is YSiO hypoxemia diffusion coefficient layer to protect the superiors, manufacturing cycle number n >=2, wherein, be prepared into YSiO hypoxemia diffusion coefficient layer and HfSiBCN self-healing thickness degree is 10nm~1 μm；Then, it is placed in vacuum annealing furnace and is made annealing treatment, it is thin to reduce Membrane stress, back end vacuum is 5 × 10-4Below Pa, annealing temperature is 900~1100 DEG C, and annealing soaking time is 1~2h；
The band self-healing composite armor thin film sensor is prepared into, wherein, step 3-5 is self-healing composite armor Preparation method.
CN201710311816.XA 2017-05-05 2017-05-05 A kind of high temperature film sensor with self-healing composite armor and preparation method thereof Pending CN107201502A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN108106748A (en) * 2017-11-09 2018-06-01 中国电子科技集团公司第四十八研究所 A kind of flexibility ablation resistance film and preparation method thereof
CN108165929A (en) * 2017-12-28 2018-06-15 中国科学院宁波材料技术与工程研究所 A kind of self-healing coating and preparation method and application
WO2019109717A1 (en) * 2017-12-07 2019-06-13 华中科技大学 Method of densifying high temperature anti-oxidation coating for tungsten-rhenium thermocouple
CN112011773A (en) * 2020-08-14 2020-12-01 中国科学院宁波材料技术与工程研究所 Yttrium silicate coating and preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1870493A2 (en) * 2006-06-21 2007-12-26 General Electric Company Strain tolerant coating for environmental protection
CN106498355A (en) * 2016-10-20 2017-03-15 电子科技大学 A kind of high temperature film sensor antioxidation composite armor and its manufacture method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1870493A2 (en) * 2006-06-21 2007-12-26 General Electric Company Strain tolerant coating for environmental protection
CN106498355A (en) * 2016-10-20 2017-03-15 电子科技大学 A kind of high temperature film sensor antioxidation composite armor and its manufacture method

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
P.ZEMAN ET AL.: "Superior high-temperature oxidation resistance of magnetron sputtered Hf–B–Si–C–N film", 《CERAMICS INTERNATIONAL》 *
PETER MECHNICH: "Y2SiO5 coatings fabricated by RF magnetron sputtering", 《SURFACE & COATINGS TECHNOLOGY》 *
强颖怀主编: "《材料表面工程技术》", 31 May 2016, 中国矿业大学出版社 *
邓飞等: "硅酸钇高温抗氧化涂层的研究进展", 《硅酸盐通报》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108106748A (en) * 2017-11-09 2018-06-01 中国电子科技集团公司第四十八研究所 A kind of flexibility ablation resistance film and preparation method thereof
WO2019109717A1 (en) * 2017-12-07 2019-06-13 华中科技大学 Method of densifying high temperature anti-oxidation coating for tungsten-rhenium thermocouple
CN108165929A (en) * 2017-12-28 2018-06-15 中国科学院宁波材料技术与工程研究所 A kind of self-healing coating and preparation method and application
CN108165929B (en) * 2017-12-28 2019-10-11 中国科学院宁波材料技术与工程研究所 A kind of self-healing coating and the preparation method and application thereof
CN112011773A (en) * 2020-08-14 2020-12-01 中国科学院宁波材料技术与工程研究所 Yttrium silicate coating and preparation method and application thereof
CN112011773B (en) * 2020-08-14 2022-10-18 中国科学院宁波材料技术与工程研究所 Yttrium silicate coating and preparation method and application thereof

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