CN102212823B - Method for arranging film sensor on alloy substrate - Google Patents
Method for arranging film sensor on alloy substrate Download PDFInfo
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- CN102212823B CN102212823B CN201110123372XA CN201110123372A CN102212823B CN 102212823 B CN102212823 B CN 102212823B CN 201110123372X A CN201110123372X A CN 201110123372XA CN 201110123372 A CN201110123372 A CN 201110123372A CN 102212823 B CN102212823 B CN 102212823B
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- thin film
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Abstract
The invention discloses a method for producing a film sensor by using a turbine engine blade to be detected or the like as a substrate in the field of film sensors. The method comprises the following steps of: treating the surface of an alloy substrate, depositing a NiCrAlY alloy transition layer on the alloy substrate, separating out metallic aluminum, sputtering a metallic aluminum layer, performing oxidation treatment, setting an Al2O3 ceramic insulating layer, and setting a functional layer and an Al2O3 protective layer of the film sensor. A layer of metallic aluminum is directly sputtered after the aluminum of certain thickness is separated out of the NiCrAlY layer, and the separated aluminum and the sputtered aluminum are uniformly distributed on the surface of the NiCrAlY transition layer and then oxidized to generate an Al2O3 connecting transition layer; and the thickness of the NiCrAlY layer is only about 1/20 of the background technology. Therefore, the method has the characteristics that: the NiCrAlY transition layer is thin, the connecting strength of the NiCrAlY transition layer and the Al2O3 ceramic insulating layer is high, the preparation difficulty and the production cost are low, and the method is safe and reliable during working in the environment of about 1,000 DEG C and can provide accurate and reliable design proof for research and design of a turbine engine and the like.
Description
Technical field
The invention belongs to thin film sensor design and production technical field; Particularly a kind of with turbine engine blade to be measured, combustion chamber inwall etc. as alloy substrate, directly the method for thin film sensor is set on surfaces such as turbine engine blade to be measured, combustion chamber inwalls; This type of thermopair can be widely used in the measurement of turbine engine blade, combustion chamber etc. being carried out the surface temperature distribution state, for the research and the design of turbine engine provides accordingly, more accurate basic data.
Background technology
Modern aeroengine when work, be in the severe environment such as high temperature that fuel gas buring produces, high pressure owing to turbine blade and combustion chamber; Turbine blade and combustor surface temperature sharply raise, produce bigger thermal strain simultaneously, and the temperature distribution of turbine blade and combustor surface and thermal strain thereof are very big to the performance and the influence in life-span of turbine engine; And often there is hot localised points in turbine blade surface and turbine blade etc. is produced serious harm.In aircraft engine design and the experimental study, engine operating temperature is the good and bad important parameter of modern turbine engine performance always in modern times; In order to verify the performance of cold effect effect of high-temperature component such as turbine blade, combustion chamber and thermal barrier coating, accurately parameters such as the temperature distribution of turbine blade and combustor surface and thermal stress state thereof under the surveying work state are most important to the design of mover.
The metal-base film transmitter technology of preparing that adopts at present is on the alloy substrate, under the temperature about 600 ℃, deposits NiCrAlY (nichrome-chromium-aluminium-yttrium) alloy transition layer with argon gas as reaction medium, employing magnetically controlled sputter method; The NiCrAlY transition layer of preparation separates out processings in vacuum and 1000 ℃ of temperature, with at surperficial precipitating metal aluminium, the aluminium of separating out passes through thermooxidizing generation Al under normal pressure
2O
3Layer; Again at this Al
2O
3On the layer, adopt Al
2O
3Raw material through electron-beam vapor deposition method in 600～900 ℃ of TRs and 10
-310
-2The thick about 20 μ m left and right sides Al of vapor deposition under the pa vacuum
2O
3Ceramic insulating layer; Then at Al
2O
3Preparation thin film sensor functional layer on the ceramic insulating layer; At last under the temperature about 600 ℃, adopt electron-beam vapor deposition method evaporating Al on gained thin film sensor functional layer (thermopair mea) and insulation layer
2O
3Resist.There is following defective in this type of thin film sensor in the preparation process: the one, and in order to make NiCrAlY transition layer and Al
2O
3Good sticking power is arranged between the insulation layer; It is thick and require to be uniformly distributed in the transition layer surface that the Al layer of separating out on the NiCrAlY surface then must reach 1-2 μ m; And thick, the thickness that requires just to need the NiCrAlY layer that will reach that desired Al chromatography goes out is more than 100 μ m, this preparation from transition layer, still transition layer follow-up high-temperature heat treatment process, need reach and substrate between bonding force difficulties very all; The 2nd, the Al that separates out from the NiCrAlY transition layer is generally island and distributes, rather than covering surfaces uniformly, make like this Al that separates out is carried out in the thermal oxidation process, the surface is except forming Al
2O
3In addition, also have the oxide compound that nickel oxide etc. has short texture and produce, this connects transition layer Al to follow-up vapor deposition
2O
3The structure of quality and device produce detrimentally affect, especially, cause Al because of coefficient of thermal expansion (coefficient) differs surpassing under 800 ℃ the high-temperature work environment
2O
3The coming off and then cause disadvantages such as thin film sensor inefficacy of insulation layer.
Summary of the invention
The objective of the invention is defective to the background technology existence; A kind of method that thin film sensor is set on alloy substrate of research and design; To realize on thin film sensor and the incorporate basis of UUT; Reach the difficulty that reduces significantly the requirement and the preparation of NiCrAlY transition region thickness, effectively improve security and safety that transmitter uses under 1000 ℃ of left and right sides Working environments, for the research and the design of turbine engine provides accordingly, purpose such as accurate basic data more.
Solution of the present invention is after former NiCrAlY transition layer is separated out aluminium (Al) element, directly the aluminium (Al) of separating out is carried out oxide treatment, generates Al
2O
3Layer (also having generated tectoriums such as the deleterious nickel oxide of device architecture simultaneously); Change at the NiCrAlY transition layer and separate out certain thickness aluminium (Al) back, adopt the direct sputter layer of metal of the mode aluminium (Al) of magnetron sputtering into; Make the sputter layer of metal aluminium (Al) and the aluminium (Al) of separating out be fused into one and be uniformly distributed in the surface of NiCrAlY1 transition layer, and then to this metallic aluminium (Al) layer carry out oxide treatment, to generate Al
2O
3Connect transition layer, thereby both reduced difficulty significantly, prevented the generation of the oxide compounds such as nickel oxide of short texture again, effectively improve this Al the requirement and the preparation of NiCrAlY transition region thickness
2O
3Connect the Al on transition layer and the vapor deposition thereafter
2O
3The linking intensity of ceramic insulating layer; Press ordinary method at last at Al
2O
3Preparation thin film sensor functional layer and evaporating Al on the ceramic insulating layer
2O
3Resist, thus realize its goal of the invention.Therefore, the present invention's method that thin film sensor is set on alloy substrate comprises:
A. the surface treatment of alloy substrate: elder generation, back adopt acetone and ethanol that the surface of alloy substrate to be measured is cleaned, and clean to be placed on drying under the nitrogen atmosphere;
B. at deposition NiCrAlY alloy transition layer on the alloy substrate: adopt conventional magnetically controlled sputter method with the NiCrAlY alloy deposition on the alloy substrate after the processing of step A, as transition layer, must be with the composite base plate of NiCrAlY alloy transition layer;
C. separating out of metallic aluminium: step B gained composite base plate is placed in the vacuum heat treatment furnace, 10
-3-10
-5Under Pa vacuum and the 900-1300 ℃ temperature condition, be heated to thickness that metallic aluminium separates out reach 100-300nm after, cool to normal temperature with the furnace, must separate out the composite base plate of layer with NiCrAlY alloy transition layer and metallic aluminium;
D. splash-proofing sputtering metal aluminium lamination: on the composite base plate after handling, adopt conventional magnetically controlled sputter method that metallic aluminium (Al) is deposited on aluminium to separate out on the layer through step C; The metallic aluminium (Al) that makes sedimentary metallic aluminium (Al) and separate out is fused into one and the thickness of uniform distribution (covering) in NiCrAlY transition layer surface only reaches 1-2 μ m, changes step e then and carries out oxide treatment;
E. oxide treatment: under oxygen atmosphere, at the uniform velocity be warming up to 900-1100 ℃ after, constant temperature 4-10h (hour), what make the metallic aluminium layer thickness is completely oxidized to Al more than 50%
2O
3Afterwards, be cooled to room temperature, must be with NiCrAlY alloy transition layer and Al
2O
3The composite base plate that connects transition layer;
F., Al is set
2O
3Ceramic insulating layer: adopt conventional vacuum vapour deposition, will place under vacuum atmosphere and 500-600 ℃, adopt high purity Al through the composite base plate after the step e oxide treatment
2O
3Be the vapor deposition raw material, at the Al of composite base plate
2O
3The thick Al of surface deposition 3-10 μ m that connects transition layer
2O
3The pottery, as insulation layer;
G., thin film sensor functional layer and Al are set
2O
3Resist: will place through the composite base plate that step F makes under the vacuum atmosphere by ordinary method, and adopt magnetron sputtering or electron beam evaporation method at Al
2O
3Each thin film sensor is set on the ceramic insulating layer; Then at Al
2O
3Ceramic insulating layer and sensor function laminar surface still by ordinary method, under vacuum atmosphere and 500-600 ℃ of temperature, the method that adopts electron beam evaporation is at Al
2O
3Al on the surperficial vapor deposition of insulation layer and thin film sensor
2O
3Resist, to Al
2O
3The upper surface of resist is that 1.0-2.0 μ m ends to the thickness of thin film sensor upper surface; Thereby make thin film sensor according to the invention.
Above institute art alloy substrate is Ni base alloy sheets or stainless steel substrate.At conventional magnetically controlled sputter method described in the step D is direct current magnetron sputtering process, radio-frequency magnetron sputter method or medium frequency magnetron sputtering method, is 6.0 * 10 in back of the body end vacuum tightness
-4Pa, operating air pressure are under 0.5Pa and the room temperature condition, and the Al that is not less than 99.99wt% in purity is target, be to be not less than 99.999% argon gas to carry out sputter process as the sputter medium with volume percent purity.The said conventional vacuum vapour deposition of step F, its vacuum tightness are 10
-3-10
-5Pa, and said employing high purity Al
2O
3Be vapor deposition raw material, raw material A l
2O
3Purity be not less than 99.99wt%.
The present invention is owing to be employed in the direct sputter layer of metal of the mode aluminium (Al) that the NiCrAlY transition layer is separated out certain thickness aluminium (Al) back, adopted magnetron sputtering; Make the sputter layer of metal aluminium (Al) and the aluminium (Al) of separating out be fused into one and be uniformly distributed in the surface of NiCrAlY1 transition layer, and then to this metallic aluminium (Al) layer carry out oxide treatment, to generate Al
2O
3Connect transition layer; The thickness of employing the inventive method NiCrAlY transition layer is reduced to about 5 μ m of the present invention, promptly is merely about 1/20th of background technology from 100 μ m of background technology, thereby has reduced the difficulty of NiCrAlY transition layer preparation and the cost of preparation significantly; Security and safety that thin film sensor uses have effectively been improved simultaneously under 1000 ℃ of environment.Thereby the present invention to have thin thickness, preparation difficulty and a production cost of NiCrAlY transition layer low, and can effectively improve and Al
2O
3The linking intensity of ceramic insulating layer is high, makes it can be at Working environment safety, the reliable operation about 1000 ℃, is characteristics such as exploitation, the design of the research of turbine engine and product innovation provides accurately, reliable design considerations.
Description of drawings
Fig. 1 is a thin film sensor structural representation of the present invention (sectional view).
Among the figure: 1. alloy substrate to be measured, 2. alloy transition layer, 3.Al
2O
3Connect transition layer, 4.Al
2O
3Ceramic insulating layer, 5. (film) sensor function layer, 6.Al
2O
3Resist.
Embodiment
With the basic alloy sheets of nickel (Ni) as alloy substrate to be measured 1, and to prepare K type NiCr-NiSi thermopair thin film sensor above that be example:
A. the surface treatment of alloy substrate: adopting the basic alloy sheets of nickel (Ni) of (length * wide * thick) 30 * 95 * 5mm is alloy substrate 1 to be measured, and elder generation, back adopt acetone and ethanol that the surface of alloy substrate to be measured is cleaned, and cleans and is placed on drying under the nitrogen atmosphere;
B. on alloy substrate, deposit NiCrAlY alloy transition layer: it is 6.0 * 10 that the Ni base alloy substrate 1 that cleans up is placed vacuum tightness
-4In the vacuum of pa (promptly the carrying on the back end vacuum) environment; With the NiCrAlY alloy is target; Input purity is that the argon gas of 99.999% (volume percent) is as the sputter medium; At 600 ℃ of temperature, power 200W, sputtering pressure (WP) is under the condition of 0.5Pa, adopt dc magnetron sputtering method with the NiCrAlY alloy deposition on Ni base alloy substrate 1, deposit thickness 5 μ m, must cover the composite base plate of NiCrAlY alloy transition layer 2;
C. separating out of metallic aluminium: the composite base plate that step B makes is put into vacuum heat treatment furnace, 5 * 10
-4After rising to 1000 ℃ under the pa vacuum condition, with the heat-up rate of 10 ℃/min, constant temperature (processing) 5h, under vacuum condition, cool to normal temperature with the furnace then; This process separates out the Al element in the transition layer to the surface, forms the thick metal aluminium lamination of the about 200nm of one deck on the transition layer surface;
D. splash-proofing sputtering metal aluminium lamination: will be placed back of the body end vacuum tightness by the composite base plate that step C makes is 6.0 * 10
-4In the sputter process device of pa; With purity is that 99.99% Al is a target; Input purity is that the argon gas of 99.999% (volume percent) is as the sputter medium; At room temperature, power 100W, sputtering pressure (operating air pressure) is under the condition of 0.5Pa, adopts dc magnetron sputtering method that Al is deposited on the composite base plate, makes sedimentary metallic aluminium (Al) and the metallic aluminium (Al) of separating out be fused into one and is uniformly distributed on NiCrAlY transition layer 2 surfaces; Its thickness reaches 1.5 μ m to be ended, and obtains the composite base plate that the surface evenly covers the metal aluminium lamination;
E. oxide treatment: the composite base plate that step D makes is put into atmosphere sintering furnace; Feeding purity and be 99.999% oxygen, rise to 1000 ℃, constant temperature with the heat-up rate of 15 ℃/min and handle 6h, is Al with the top thick metallic aluminium complete oxidation of 0.95 μ m of the metal aluminium lamination on composite base plate surface
2O
3(0.95 μ m is thick at this moment is Al with the lower section
2O
3With the mixed layer of Al) back, stop to heat and continue logical oxygen and end up to being cooled to room temperature, obtain surface coverage Al
2O
3The composite base plate that connects transition layer 3;
F is provided with Al
2O
3Ceramic insulating layer: is 6.0 * 10 with the composite base plate after step e is handled in back of the body end vacuum
-4Under the condition of pa, to adopt purity be the Al of 99.999wt%
2O
3Being the vapor deposition raw material, is vapor deposition under the condition of 60mA at 550 ℃, vapor deposition electronic beam current, with Al
2O
3Be deposited on the composite base plate, getting thickness is the Al of 8 μ m
2O
3 Ceramic insulating layer 4;
G., thin film sensor functional layer and Al are set
2O
3Resist: in back of the body end vacuum is 6.0 * 10
-4Pa is target with argon gas as reaction medium, Ni90Cr10 and Ni97Si3, room temperature, and power be that 100W, operating air pressure are under the condition of 0.4Pa, adopt conventional magnetically controlled sputter method at Al
2O
3The surface of ceramic insulating layer 4 deposits NiCr-NiSi thermopair that 2, thickness are 1 μ m successively as (film) sensor function layer 5; Then, be 6.0 * 10 in back of the body end vacuum
-4Pa, employing purity are the Al of 99.999wt%
2O
3Being the vapor deposition raw material, is under the condition of 60mA at 550 ℃, vapor deposition electronic beam current, still adopts conventional electrical beam evaporation method at Al
2O
3The surperficial evaporating Al of insulation layer 4 and (film) sensor function layer 5
2O
3Resist 6 ends to (film) sensor function layer 5 upper surface 1.5 μ m are thick; Thereby make metal-base film transmitter according to the invention.
The thickness that adopts NiCrAlY transition layer 2 in the metal-base film transmitter of present embodiment preparation only 5 μ m, in the time of 1000 ℃, Al
2O
3The resistance of ceramic insulating layer 4 reaches 5k Ω, satisfies the request for utilization of high temperature with the metal-base film transmitter fully; Whole metal-base film transmitter can safety, use reliably in 1000 ℃ of environment.
Claims (4)
1. method that thin film sensor is set on alloy substrate comprises:
A. the surface treatment of alloy substrate: elder generation, back adopt acetone and ethanol that the surface of alloy substrate to be measured is cleaned, and clean to be placed on drying under the nitrogen atmosphere;
B. at deposition NiCrAlY alloy transition layer on the alloy substrate: adopt conventional magnetically controlled sputter method with the NiCrAlY alloy deposition on the alloy substrate after the processing of step A, as transition layer, must be with the composite base plate of NiCrAlY alloy transition layer;
C. separating out of metallic aluminium: step B gained composite base plate is placed in the vacuum heat treatment furnace, 10
-3-10
-5Under Pa vacuum and the 900-1300 ℃ temperature condition, be heated to thickness that metallic aluminium separates out reach 100-300nm after, cool to normal temperature with the furnace, must separate out the composite base plate of layer with NiCrAlY alloy transition layer and metallic aluminium;
D. splash-proofing sputtering metal aluminium lamination: on the composite base plate after handling, adopt conventional magnetically controlled sputter method that metallic aluminium is deposited on aluminium to separate out on the layer through step C; Make sedimentary metallic aluminium and the metallic aluminium of separating out be fused into one and be uniformly distributed in the surperficial thickness of NiCrAlY transition layer only to reach 1-2 μ m, change step e then and carry out oxide treatment;
E. oxide treatment: under oxygen atmosphere, at the uniform velocity be warming up to 900-1100 ℃ after, constant temperature 4-10h, what make the metallic aluminium layer thickness is completely oxidized to Al more than 50%
2O
3Afterwards, be cooled to room temperature, must be with NiCrAlY alloy transition layer and Al
2O
3The composite base plate that connects transition layer;
F., Al is set
2O
3Ceramic insulating layer: adopt conventional vacuum vapour deposition, will place under vacuum atmosphere and 500-600 ℃, adopt high purity Al through the composite base plate after the step e oxide treatment
2O
3Be the vapor deposition raw material, at the Al of composite base plate
2O
3The thick Al of surface deposition 3-10 μ m that connects transition layer
2O
3The pottery, as insulation layer;
G., thin film sensor functional layer and Al are set
2O
3Resist: will place through the composite base plate that step F makes under the vacuum atmosphere by ordinary method, and adopt magnetron sputtering or electron beam evaporation method at Al
2O
3Each thin film sensor is set on the ceramic insulating layer; Then at Al
2O
3Ceramic insulating layer and each thin film sensor functional layer surface still by ordinary method, under vacuum atmosphere and 500-600 ℃ of temperature, the method that adopts electron beam evaporation is at Al
2O
3Al on the surperficial vapor deposition of insulation layer and each thin film sensor functional layer
2O
3Resist, to Al
2O
3The upper surface of resist is that 1.0-2.0 μ m ends to the thickness of each thin film sensor functional layer upper surface; Thereby make said thin film sensor.
2. by the said method that thin film sensor is set of claim 1, it is characterized in that said alloy substrate is Ni base alloy sheets or stainless steel substrate on alloy substrate.
3. by the said method that thin film sensor is set of claim 1, it is characterized in that at conventional magnetically controlled sputter method described in the step D be direct current magnetron sputtering process, radio-frequency magnetron sputter method or medium frequency magnetron sputtering method on alloy substrate, is 6.0 * 10 in back of the body end vacuum tightness
-4Pa, operating air pressure are under 0.5Pa and the room temperature condition, and the Al that is not less than 99.99wt% in purity is target, be to be not less than 99.999% argon gas to carry out sputter process as the sputter medium with volume percent purity.
4. by the said method that thin film sensor is set of claim 1, it is characterized in that conventional vacuum vapour deposition described in the step F, its vacuum tightness are 10 on alloy substrate
-3-10
-5Pa, and said employing high purity Al
2O
3Be vapor deposition raw material, raw material A l
2O
3Purity be not less than 99.99wt%.
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|---|---|---|---|
| CN201110123372XA CN102212823B (en) | 2011-05-13 | 2011-05-13 | Method for arranging film sensor on alloy substrate |
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|---|---|---|---|
| CN201110123372XA CN102212823B (en) | 2011-05-13 | 2011-05-13 | Method for arranging film sensor on alloy substrate |
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| CN102212823B true CN102212823B (en) | 2012-11-07 |
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Families Citing this family (9)
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| CN103266320B (en) * | 2013-05-30 | 2016-01-20 | 电子科技大学 | A kind of High temperature oxidation resistant film sensor and production method thereof |
| CN103486961B (en) * | 2013-05-31 | 2016-05-18 | 电子科技大学 | With member and the preparation method of thin film sensor |
| CN103921500B (en) * | 2014-04-30 | 2016-01-13 | 电子科技大学 | A kind of thin film strain takes into account its preparation method |
| CN104149416B (en) * | 2014-08-22 | 2016-01-20 | 电子科技大学 | A kind of Metal Substrate high-temperature insulating layer and preparation method thereof |
| CN104789926B (en) * | 2015-03-10 | 2017-06-09 | 电子科技大学 | A kind of preparation method of metal-base film sensor |
| CN105908142B (en) * | 2016-04-15 | 2018-08-14 | 大连交通大学 | A kind of high temperature film strain gauge and preparation method thereof |
| CN106498355B (en) * | 2016-10-20 | 2018-08-21 | 电子科技大学 | A kind of high temperature film sensor anti-oxidant composite armor and its manufacturing method |
| CN106595910A (en) * | 2016-11-08 | 2017-04-26 | 中国电子科技集团公司第四十八研究所 | Stress sensor and preparation method thereof |
| CN112853295A (en) * | 2021-01-07 | 2021-05-28 | 中北大学 | Preparation method for constructing gradient transition structure of thin film sensor by oxygen ion implantation |
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| CN101894904A (en) * | 2010-07-15 | 2010-11-24 | 电子科技大学 | Metal-base film thermocouple and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101894904A (en) * | 2010-07-15 | 2010-11-24 | 电子科技大学 | Metal-base film thermocouple and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张以忱,巴德纯,马胜歌.薄膜热阻微传感器技术.<<真空>>.2004,第41卷(第5期),24-28. |
| 薄膜热阻微传感器技术;张以忱,巴德纯,马胜歌;<<真空>>;20040930;第41卷(第5期);24-28 * |
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