CN115011915A - Preparation method of redundant thin-film thermocouple - Google Patents
Preparation method of redundant thin-film thermocouple Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 74
- 239000000919 ceramic Substances 0.000 claims abstract description 43
- 238000004544 sputter deposition Methods 0.000 claims abstract description 39
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- 238000005530 etching Methods 0.000 claims abstract description 15
- 238000004528 spin coating Methods 0.000 claims abstract description 8
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- 238000000034 method Methods 0.000 claims description 16
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- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
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- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
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- 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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- 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
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- 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
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- 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
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5826—Treatment with charged particles
- C23C14/5833—Ion beam bombardment
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5873—Removal of material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K7/00—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements
- G01K7/02—Measuring temperature based on the use of electric or magnetic elements directly sensitive to heat ; Power supply therefor, e.g. using thermoelectric elements using thermoelectric elements, e.g. thermocouples
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- 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
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Abstract
A preparation method of a redundant thin-film thermocouple belongs to the technical field of high-temperature alloy surface temperature measurement. The preparation method of the redundant thin-film thermocouple comprises the following steps: cleaning a ceramic substrate, sputtering a Pt electrode, spin-coating photoresist, exposing, developing, etching the Pt electrode, exposing, developing, sputtering PtRh 10 Gluing, developing and cleaning the substrate. The key technology of the invention is a sputtering film-forming technology, and the technological parameters influencing the sputtering film-forming technology mainly comprise sputtering power, sputtering vacuum degree, sputtering time, substrate temperature and the like. The film thermocouple manufactured by the preparation method of the invention has indexing errorSmall difference, high stability and small size of temperature measuring point.
Description
Technical Field
The invention relates to a preparation method of a redundant thin-film thermocouple, belonging to the technical field of high-temperature alloy surface temperature measurement.
Background
Thin film thermocouple temperature measurement is a common method for obtaining real-time temperature data of high temperature components of aircraft engines. The technology can effectively avoid the overheating phenomenon of the blades of the aircraft engine and provide data support for the design of the engine. However, bonding thin film thermocouples to turbine blades requires the preparation of insulation on the turbine blade, which requires both good insulation and high temperature bonding capability, and is not easily removed. Therefore, it has a certain thickness, which affects the accuracy of the temperature measurement. At present, the heat-insulating layer is generally prepared by multiple layers, such as a bonding layer, a transition layer and the like. The process is complex, the interface stress between materials is large, and the interface stress is large. The thin film thermocouple is easily dropped off under the high pressure of the aircraft engine, which brings a problem to the temperature stability of the thin film thermocouple.
Existing bond coats bond well to metals, particularly superalloys. However, not all of the adhesive coating materials are insulating materials, and the adhesive materials are not stable in conductivity at high temperatures. Therefore, it is necessary to combine bonding technology with insulation technology to ensure accurate measurement of the surface temperature of the superalloy in a high temperature environment.
Existing bond coats are typically very thick, at least tens of microns, which affects heat transfer efficiency. Excessive thickness makes thermal equilibrium between the bond coat of the thermocouple film and the workpiece surface more difficult, and transient temperature measurement is also impossible.
Disclosure of Invention
Aiming at the defects and improvement requirements in the prior art, the invention provides the preparation method of the redundant thin-film thermocouple, and the thin-film thermocouple prepared by the method is subjected to performance test, and the result shows that the thin-film thermocouple prepared by the method has obvious advantages in the aspects of indexing error, stability and the like, and the method has important significance in stable temperature measurement of the thin-film thermocouple.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a redundant thin-film thermocouple mainly comprises the following steps:
step 1: the method comprises the steps of cleaning a ceramic substrate, namely, pre-treating the substrate, namely polishing the Al2O3 ceramic substrate, soaking the substrate in an alcohol solution, then cleaning the substrate by plasma ultrasonic, and then drying the substrate.
And 2, step: sputtering Pt electrode, namely sputtering the Al2O3 ceramic substrate, and then naturally cooling.
And step 3: spin coating photoresist, namely uniformly coating the Al2O3 ceramic substrate to be finished in the previous step, and then drying.
And 4, step 4: and (4) exposing the Al2O3 ceramic substrate which is about to finish the previous step.
And 5: and developing, namely developing the Al2O3 ceramic substrate which is about to finish the previous step, and then drying.
Step 6: and etching the Pt electrode, namely performing dry etching on Pt in an ion beam etching machine, cleaning the ceramic substrate by using plasma water, and drying.
And 7: and (4) exposing, namely repeating the exposing step.
And 8: and developing, namely placing the exposed Pt layer electrode into a developing solution for developing, dissolving the hot point part of the photoresist, and forming the Pt layer electrode with the hot point removed.
And step 9: sputtering PtRh10 electrode, namely putting the Al2O3 ceramic substrate which is going to finish the previous step into an ultra-vacuum sputtering system, repeating the sputtering process and then drying.
Step 10: and (3) gluing, namely, spin-coating photoresist on the sputtered Rh electrode, and placing the ceramic substrate coated with the photoresist on an exposure machine for exposure by using the prepared mask plate.
Step 11: and developing, namely, placing the Rh layer exposed in the previous step in a developing solution for developing, patterning the photoresist into the shape of the Rh electrode, and etching Rh in an ion beam etching machine to obtain a complete graph of the Rh layer.
Step 12: and cleaning the substrate, namely placing the coated ceramic substrate in corrosive liquid to remove residual photoresist, performing micro-ultrasonic oscillation to more thoroughly remove the photoresist, and then performing laser cutting on the prepared thin-film thermocouple to form an independent redundant thin-film thermocouple device.
The preparation process of the method mainly comprises the processes of pretreatment of the substrate, sputtering film formation, exposure, development, etching and the like. The quality of the manufacturing process directly influences the performance of the thin film thermocouple.
The shutdown technology of the invention is a sputtering film-forming technology, the sputtering film-forming of the thin film thermocouple is essentially the process of forming and growing the thin film electrode, and the technological parameters influencing the thin film sputtering process mainly comprise: sputtering power, sputtering vacuum degree, sputtering time, substrate temperature and the like.
Compared with the prior art, the invention has the beneficial effects that: the method for preparing the redundant thin-film thermocouple has obvious advantages in the aspects of indexing error, stability and the like, and has important significance in stable temperature measurement of the thin-film thermocouple.
Drawings
FIG. 1 is a flow chart of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly and completely apparent, the technical solutions of the present invention will be described below with reference to the flowchart of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the protection scope of the present invention.
The first embodiment is as follows: the following steps specifically describe the manufacturing process flow of the thin film thermocouple.
Pretreatment for cleaning a ceramic substrate: firstly, mixing nano calcium carbonate powder and a small amount of deionized water into paste, dipping the paste nano calcium carbonate into a cotton ball, and then carrying out Al treatment 2 O 3 And polishing the ceramic substrate for 3-5 minutes. After polishing was completed, the Al was rinsed with copious amounts of deionized water 2 O 3 A ceramic substrate. Then, the substrate was cleaned in an acetone solution for 10 minutes, and then taken out and immersed in an alcohol solution for 10 minutes, followed by ultrasonic cleaning with a large amount of plasma water for 5 minutes. Putting the cleaned ceramic substrate into a drying box, keeping the temperature constant at 100 ℃,the time period required was 30 minutes.
Sputtering a Pt electrode: drying the well dried Al 2 O 3 The substrate was placed in an RMS-4000L ultra-vacuum sputtering system and the vacuum in the sputtering chamber was adjusted to 5X 10 -4 Pa, setting the anode voltage to 50V, then opening the switch of the argon in the parallel cavity, and introducing the argon until the vacuum degree of the sputtering cavity reaches 6.0 multiplied by 10 -3 Pa, the accelerating gate voltage was adjusted to 100V, then the cathode voltage was slowly adjusted until 15V was reached, and then sputtering of a 20 μm Pt layer was started. And after the sputtering is finished, placing the coated substrate base plate in a cavity with certain vacuum degree for natural cooling for about 4 hours, and then taking out.
Spin coating a photoresist: al sputtered with Pt electrode using BP212 type positive photoresist 2 O 3 Uniformly coating the ceramic substrate, keeping the rotating speed of a glue homogenizing machine at about 3500r/min, and drying the ceramic substrate in a drying box at 100 ℃ for 30min after glue homogenizing.
Exposure: and (3) placing the ceramic substrate after the glue homogenizing and drying on an exposure machine, placing the prepared mask plate on the substrate, wherein the size of the substrate and the mask plate has no large error, and exposing the substrate coated with the photoresist for about 80 seconds.
And (3) developing: and (3) placing the exposed ceramic substrate into a developing solution for developing, wherein the exposed part of the pattern is dissolved away because the spin coating is positive photoresist, and the unexposed part is left. Preparing a developing solution from the developing solution and water in a volume ratio of 1:3, developing by adopting an immersion method for 150 seconds, and then putting the developed ceramic substrate into a drying box at the temperature of 80 ℃ for drying.
Etching the Pt electrode: and carrying out dry etching on Pt in an ion beam etching machine, setting the main cathode to be 6.0A, adjusting the accelerating voltage to be 300V, and controlling the etching rate to be 30 nm/min. Thereby obtaining a finished pattern of the Pt layer, cleaning the ceramic substrate with plasma water, and drying the cleaned ceramic substrate in a drying box with the temperature of 80 ℃.
Exposure: and repeating the exposure step, and further exposing the Pt electrode etched in the last step by using the Pt layer mask plate for removing the hot junction, so that the shape of the Pt layer for removing the hot junction is formed conveniently.
And (3) developing: and (3) placing the exposed Pt layer electrode into a developing solution for developing, dissolving the hot-point part of the photoresist, and forming the Pt layer electrode with the hot-point removed.
Sputtering PtRh 10 An electrode: the ceramic substrate was then placed in an RMS-4000L ultra-vacuum sputtering system and the sputtering process was repeated, maintaining the vacuum of the sputter adjusted to 5.5X 10 -3 Pa, then start sputtering 30 μm of PtRh 10 . And after the sputtering is finished, naturally cooling the coated substrate in a cavity with a certain vacuum degree for about 4 hours, and then taking out.
Gluing: and (3) spin-coating photoresist on the sputtered Rh electrode, and placing the ceramic substrate coated with the photoresist on an exposure machine for exposure by using the prepared mask plate.
And (3) developing: and (3) placing the Rh layer exposed in the previous step in a developing solution for developing, patterning the photoresist into the shape of an Rh electrode, and etching Rh in an ion beam etching machine to obtain a complete graph of the Rh layer.
Cleaning the substrate: and placing the coated ceramic substrate in corrosive liquid to remove the residual photoresist, and performing micro-ultrasonic oscillation to more thoroughly remove the photoresist. And after the photoresist is completely dissolved, washing by using deionized water, putting the washed ceramic substrate into a drying box with the temperature of 80 ℃ for drying, setting the drying time to be 30min, repeating the preparation process, sputtering and depositing a second group of thin film electrodes, and finally performing laser cutting on the prepared thin film thermocouple to form an independent redundant thin film thermocouple device.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (10)
1. A preparation method of a redundant thin-film thermocouple is characterized by comprising the following steps: (a) cleaning the ceramic substrate; (b) sputtering a Pt electrode; (c) spin-coating a photoresist; (d) exposing; (e) developing; (f) etching the Pt electrode; (g) exposing; (h) developing; (i) sputtering PtRh 10 (ii) a (j) Gluing; (k) developing; (l) And cleaning the substrate.
2. The method according to claim 1, wherein the step of (a) cleaning the ceramic substrate comprises: firstly, mixing nano calcium carbonate powder and a small amount of deionized water into paste, dipping the paste nano calcium carbonate into a cotton ball, and then carrying out Al treatment 2 O 3 Polishing the ceramic substrate for 3-5 min, and washing Al with a large amount of deionized water after polishing 2 O 3 Cleaning the residual calcium carbonate on the ceramic substrate, cleaning the substrate in acetone solution for 10 minutes, taking out the substrate, soaking the substrate in alcohol solution for 10 minutes, and ultrasonically cleaning the substrate for 5 minutes by using a large amount of plasma water to ensure Al 2 O 3 The water on the surface of the ceramic substrate is not gathered into beads and is uniformly distributed on the surface of the substrate. And (3) putting the cleaned ceramic substrate into a drying box, keeping the temperature constant at 100 ℃ and keeping the time for 30 minutes.
3. The (b) sputtered Pt electrode of claim 1, wherein the (b) sputtered Pt electrode step is:drying the well dried Al 2 O 3 And (3) placing the substrate base plate into an ultra-vacuum sputtering system, opening a switch of argon in the parallel cavity, placing the coated substrate base plate into a cavity with a certain vacuum degree for natural cooling after sputtering is finished, and then taking out.
4. The (c) spin-on resist of claim 1, wherein the (c) spin-on resist step is: al sputtered with Pt electrode by positive photoresist 2 O 3 And uniformly coating the ceramic substrate with glue, and drying the ceramic substrate in a drying box after the coating is finished.
5. The (d) exposure of claim 1, wherein the (d) exposure step is: and (3) placing the ceramic substrate after being coated with the glue and dried on an exposure machine, placing the prepared mask plate on the substrate, and exposing the substrate coated with the photoresist.
6. The (e) developer of claim 1, wherein said (e) developing step is: and placing the exposed ceramic substrate into a developing solution for developing, and then placing the developed ceramic substrate into a drying box for drying.
7. The (f) etching Pt electrode of claim 1, wherein the (f) etching Pt electrode step is: and carrying out dry etching on Pt in an ion beam etching machine, cleaning the ceramic substrate with plasma water, and drying the cleaned ceramic substrate in a drying box.
8. The (i) sputtered PtRh10 electrode of claim 1, wherein the (i) sputtered PtRh10 electrode comprises: and (3) putting the ceramic substrate into an ultra-vacuum sputtering system, repeating the sputtering process, and after sputtering is finished, naturally cooling the coated substrate in a cavity with a certain vacuum degree and taking out the substrate.
9. -glue according to claim 1, characterized in that said step (j) of gluing consists in: and (3) spin-coating photoresist on the sputtered Rh electrode, and placing the ceramic substrate coated with the photoresist on an exposure machine for exposure by using the prepared mask plate.
10. The (l) cleaned substrate of claim 1, wherein the (l) cleaned substrate step is: and placing the coated ceramic substrate in corrosive liquid to remove residual photoresist, washing with deionized water, placing the washed ceramic substrate in a drying box for drying, repeating the preparation process, sputtering and depositing a second group of thin film electrodes, and finally performing laser cutting on the prepared thin film thermocouple to form an independent redundant thin film thermocouple device.
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| CN202210425779.6A CN115011915A (en) | 2022-04-22 | 2022-04-22 | Preparation method of redundant thin-film thermocouple |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0228525A (en) * | 1988-07-19 | 1990-01-30 | Tanaka Kikinzoku Kogyo Kk | Thin film thermocouple |
| JPH0282169A (en) * | 1988-09-20 | 1990-03-22 | Tanaka Kikinzoku Kogyo Kk | Substrate for measuring temperature coefficient of resistance of thin film |
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