CN105755438B - A kind of high-temperature self-compensating multi-layer compound film strain gauge and preparation method thereof - Google Patents
A kind of high-temperature self-compensating multi-layer compound film strain gauge and preparation method thereof Download PDFInfo
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- CN105755438B CN105755438B CN201610194927.2A CN201610194927A CN105755438B CN 105755438 B CN105755438 B CN 105755438B CN 201610194927 A CN201610194927 A CN 201610194927A CN 105755438 B CN105755438 B CN 105755438B
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- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
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Abstract
The present invention provides a kind of high-temperature self-compensating multi-layer compound film strain gauge and preparation method thereof, and the strain gauge includes superalloy components substrate, alumina insulating layer, the first TaN strained layer, PdCr strained layer, the 2nd TaN strained layer, aluminium oxide or silicon oxide protective layer and Pt electrode.Using superalloy components as substrate, the Dual ion beam sputtering deposition alumina insulation film in substrate, the r. f. magnetron sputtering TaN and PdCr self-compensating strain layer on insulation film, double ion beam sputtered aluminium oxide or silicon oxide protective layer on strained layer.The present invention is suitable for the real-time measurement the component course of work；Using TaN and PdCr alloy strained layer, influence of the temperature change to component strain measurement is overcome, high temperature measurement precision is greatly improved；It is good using ion beam sputtering aluminium oxide or silicon oxide protective layer compact structure, binding force, extraordinary protective effect is played to functional structure.
Description
Technical field
The present invention relates to thin film sensor design and production technical fields, specifically, being related to one kind in superalloy components
On be prepared in situ, the high temperature film strain gauge with temperature self-compensation function and preparation method thereof.
Background technique
For long-term running component at high temperature, creep is to cause the principal element of failure.For example, modern turbine boat
In empty engine technology, turbo blade work high temperature, high pressure, highly corrosive extreme environment in.Therefore turbo blade is set
Meter becomes vital link in engine design and manufacture with selection.In order to determine turbine engine blade structural model and
Assessment to blade new material performance, the mechanical behavior of real-time monitoring blade are necessary.
Traditional foil gauge has metal wire type or foil gage.And thin film strain meter is compared to traditional foil gauge, it is thick
Degree in micron dimension, may be implemented it is in situ make and measurement, the influence of the structure of tested component can be ignored, corresponding speed is fast,
Test accuracy height, high sensitivity.
It is prepared in situ strain gauge on metal component, the high-temperature insulation of device and substrate is always the weight for restricting real-time monitoring
Want factor.Insulating materials generally selects aluminum oxide film.Such as patent " a kind of semiconductive thin film high temperature deformation sensor "
(CN103900460A) aluminum oxide film that the method by reactive sputtering mentioned in deposits.This method prepares aluminum oxide film
Required condition is harsh, needs accurately to control the flow-rate ratio of oxygen and argon gas, and reacts and carry out at high temperature, to equipment
It is required that stringenter, manufacturing cost is also relatively high.Reactive sputtering aluminium oxide there is also a drawback be in sputtering process, such as
The control of really bar part is bad, it is easy to target " poisoning " phenomenon occur, be that sputtering process is unable to complete, will seriously affect the matter of film
Amount.The first high-temperature process mentioned in patent " a kind of thin film strain meter and preparation method thereof " (CN103921500A)
NiCoCrAlY alloy substrates generate 1~2 μm of alumina transition layer, then deposit 10~15 μ using the method for electron beam evaporation
The aluminium oxide of m.When the excessive layer of high-temperature process NiCoCrAlY, it is easy to generate the conductivity such as NiO higher than ten times of aluminium oxide or more
Oxide will seriously affect the insulating properties of insulating film.The disadvantages of this method is complicated there is also preparation process.
Since the variation of temperature can generate biggish resistance when electric resistance wire strain gauge works in the extreme environment of engine
Variation is big so as to cause measurement result deviation.And the composite strain membrane structure for using temperature-coefficient of electrical resistance (TCR) small can subtract
Delay this effect.And PdCr alloy has positive TCR, TaN to have the reasonable combination of both negative TCR to can be obtained by TCR's nearly zero
Self compensation laminated film strain gauge.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of high temperature being prepared in situ on high temperature alloy structural member
Self compensation multi-layer compound film strain gauge and preparation method thereof not only realizes the in situ measurement at high temperature to metal component,
And the overall dimensions of device are thinned, enormously simplify manufacture craft.
The present invention solves the above problems used technical solution are as follows:
According to an aspect of the present invention, a kind of high-temperature self-compensating multi-layer compound film strain gauge, the strain gauge are provided
Including superalloy components substrate, alumina insulating layer, the first TaN strained layer, PdCr strained layer, the 2nd TaN strained layer, oxidation
Aluminium or silicon oxide protective layer and Pt electrode, in which:
Alumina insulating layer is deposited in superalloy components substrate；First TaN strained layer is deposited on alumina insulating layer
On；PdCr strained layer is deposited on the first TaN strained layer, and the 2nd TaN strained layer is deposited on PdCr strained layer；Aluminium oxide or oxygen
SiClx protective layer is covered on the 2nd TaN strained layer；Pt electrode deposition on alumina insulating layer and with side wall simultaneously with the
One TaN strained layer, PdCr strained layer, the 2nd TaN strained layer are connected with aluminium oxide or silicon oxide protective layer, while Pt electrode is upper
Surface is exposed to except aluminium oxide or silicon oxide protective layer for lead.
Preferably, the strain gauge is prepared in situ in superalloy components substrate, and superalloy components substrate is answered
With temperature at 500~1200 DEG C.
Preferably, in the first TaN strained layer, PdCr strained layer and the 2nd TaN strained layer, PdCr strained layer is located at
Among first TaN strained layer and the 2nd TaN strained layer, the first TaN strained layer, PdCr strained layer and the 2nd TaN strained layer are common
The composite strain layer of sandwich structure is formed, i.e. composition self-compensating strain layer, to eliminate resistance temperature effect.
According to another aspect of the present invention, a kind of preparation side of high-temperature self-compensating multi-layer compound film strain gauge is provided
Method, described method includes following steps:
Step 1, cleaning superalloy components substrate；
Step 2, with double ion beam sputtered machine, the sputtering sedimentation alumina insulating layer in superalloy components substrate；
Step 3, the first TaN strained layer of reaction magnetocontrol sputtering in the superalloy components substrate for completing step 2；
Step 4, the rf magnetron sputtering PdCr strained layer in the superalloy components substrate for completing step 3；
Step 5, the 2nd TaN strained layer of reaction magnetocontrol sputtering in the superalloy components substrate for completing step 4；
Step 6, the spin coating photoresist on the component for completing above-mentioned steps carry out UV exposure using strained layer mask plate, show
Shadow；
Step 7, using ion etching, sputtering has the first TaN strained layer, PdCr strained layer and the 2nd TaN to answer after development
Strain layer pattern is formed on the sandwich structure composite strain layer component of change layer；
Step 8 washes away photoresist using acetone, and deionized water cleaning is dry；
Step 9, again complete above-mentioned steps component surface spin coating photoresist, utilize electrode layer mask plate carry out UV exposure
Light, development；
Step 10, complete above-mentioned steps component surface magnetron sputtering Pt electrode；
Step 11 washes away photoresist using acetone, and deionized water cleaning is dry；
Step 12, using double ion beam sputtered machine, in the component surface sputtering sedimentation aluminium oxide or oxygen for completing above-mentioned steps
SiClx protective layer.
Preferably, in step 2, the alumina insulating layer with a thickness of 2~4 μm, depositing target used is
99.99% high-purity sapphire target.
It is highly preferred that the Al:O stoichiometric ratio of the alumina insulating layer is 2:3 in step 2.
Preferably, in step 3, the first TaN strained layer with a thickness of 100~400nm.
Preferably, in step 4, the PdCr strained layer with a thickness of 200~600nm.
Preferably, in step 5, the 2nd TaN strained layer with a thickness of 100~400nm.
Preferably, in step 12, the aluminium oxide or silicon oxide protective layer with a thickness of 1~2 μm, protective layer of alumina
Deposition target used is 99.99% high-purity sapphire target.
It is highly preferred that the Al:O stoichiometric ratio of the protective layer of alumina is 2:3 in step 12.
More than the present invention each preferred parameter designing can obtain the theory of evolution metering aluminum oxide film of ratio and enough
Thickness, to guarantee the good insulating properties of alumina insulating film and to the good protectiveness of strained layer.It ensure that composite strain layer is each
The best proportion of thickness degree, so that the temperature-coefficient of electrical resistance of strain gauge is close to zero.
Compared with prior art, the present invention have it is following the utility model has the advantages that
The present invention uses double ion beam sputtered alumina insulating film and protective layer, and film forming is uniform, fine and close, high-temperature insulation
It is functional.Wherein, alumina insulating film can guarantee the proper device operation being prepared in situ in superalloy components without by
The influence of conductive substrates.Further, the influence that 2~4 μm of thickness generates the operation of component can be ignored, and realize not
It influences to carry out in situ measurement under conditions of component operates normally.Aluminium oxide or silicon oxide protective layer make to answer because of its fine and close characteristic
Become figure under extreme working environment from corroding, guarantees the normal work of device.
The TaN/PdCr composite strain layer that the present invention uses, the temperature-coefficient of electrical resistance according to TaN are negative value, the resistance of PdCr
Temperature coefficient is positive value, and the two is reasonable must to modulate to obtain the composite strain layer of temperature-coefficient of electrical resistance nearly zero, counteracts resistance-type and answers
Become meter as the intrinsic resistance-temperature characteristic of material and caused by measurement error, greatly improve the precision of strain measurement.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon:
Fig. 1 is the high-temperature self-compensating strain gauge structure schematic diagram that one embodiment of the invention is deposited directly on metal component.
Fig. 2 is the top view (B-B for the high-temperature self-compensating strain gauge that one embodiment of the invention is deposited directly on metal component
Cross-sectional view).
In figure: 1 being nickel based metal construction basis, 2 be alumina insulating layer, 3 be TaN strained layer, 4 be PdCr strained layer, 5
It is aluminium oxide or silicon oxide protective layer for TaN strained layer, 6,7 is Pt electrode.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
It as shown in Figure 1 and Figure 2, is the structural schematic diagram for the high-temperature self-compensating strain gauge being deposited directly on metal component,
In, Fig. 2 is B-B cross-sectional view shown in Fig. 1, and the section of A-A shown in Fig. 2, that is, Fig. 1.
Referring to attached drawing 1-2: a kind of high-temperature self-compensating multi-layer compound film strain gauge being deposited directly on hardware,
It include: nickel based metal construction basis 1, alumina insulating layer 2, TaN strained layer 3, PdCr strained layer 4, TaN strained layer 5, aluminium oxide
Or silicon oxide protective layer 6, Pt electrode 7, in which:
Alumina insulating layer 2 is deposited on nickel based metal construction basis 1；TaN strained layer 3 is deposited on alumina insulating layer 2
On；PdCr strained layer 4 is deposited on TaN strained layer 3；TaN strained layer 5 is deposited on PdCr strained layer 4；Aluminium oxide or silica
Protective layer 6 is covered on TaN strained layer 5；Pt electrode 7 is deposited on alumina insulating layer 2 and is strained simultaneously with aN with side wall
Layer 3, PdCr strained layer 4, TaN strained layer 5 are connected with aluminium oxide or silicon oxide protective layer 6, while the upper surface exposure of Pt electrode 7
Lead is used for except aluminium oxide or silicon oxide protective layer 6.
In above-mentioned strain gauge: the PdCr strained layer 4 is located among TaN strained layer 3 and TaN strained layer 5, TaN strained layer
3, the composite strain layer of sandwich structure is collectively formed in PdCr strained layer 4, TaN strained layer 5, to eliminate resistance temperature effect.
In above-mentioned strain gauge: the alumina insulating layer 2 is prepared using double ion beam sputtered system, realizes oxidation aluminum
Standby technique simplifies.Simultaneously as the film consistency prepared by double ion beam sputtered system is high, uniformity is good, so aluminium oxide
The thickness of insulating layer 2 only 2~4 μm of insulation effects that can reach a high temperature.
In above-mentioned strain gauge: since the PdCr strained layer 4 varies with temperature positive TCR, TaN strained layer is with temperature
Variation has negative TCR, and the two is reasonable to arrange in pairs or groups, and can modulate to obtain TCR close to zero composite strain layer, substantially increase strain
The precision of measurement.
As a preferred embodiment, the strain gauge is prepared in situ on nickel based metal construction basis 1, superalloy components
The application temperature of substrate 1 is at 500~1200 DEG C.
Further, it is based on above structure, the present invention goes back the above-mentioned high-temperature self-compensating multi-layer compound film of optimization design and answers
The preparation method for becoming meter, specifically comprises the following steps:
Step 1: being cleaned by ultrasonic nickel based metal construction basis 1 with dehydrated alcohol, acetone, deionized water；
Step 2: nickel based metal construction basis 1 being put into double ion beam sputtered machine, using high-purity sapphire target, is extracted into this
Bottom vacuum 10-3~10-4Pa is passed through Ar gas and O2Gas, adjusting operating air pressure is 10-2Pa, sputtering sedimentation alumina insulating layer 2
Thickness is to 2~4 μm；
Deposition target used is 99.99% high-purity sapphire target；The Al:O stoichiometry of the alumina insulating layer 2
Than for 2:3；
Step 3: the nickel based metal construction basis 1 for completing step 2 being put into magnetron sputter, is evacuated to 10-3~10-4Pa, is passed through nitrogen, adjusts 0~10Pa of operating air pressure, sputtering power 100W, sputter the thickness of TaN strained layer 3 to 100~
400nm；
Step 4: magnetron sputtering PdCr strained layer 4 takes out base vacuum to 10-3~10-4Pa is passed through Ar gas, adjusts work gas
Pressure is 0~10Pa, and sputtering power is 100~400W, sputters the thickness of PdCr strained layer 4 to 200~600nm；
Step 5: the nickel based metal construction basis 1 for completing step 4 being put into magnetron sputter, is evacuated to 10-3~10-4Pa, is passed through nitrogen, adjusts 0~10Pa of operating air pressure, sputtering power 100W, sputter the thickness of TaN strained layer 5 to 100~
400nm；
Step 6: the spin coating photoresist on the component for completing above-mentioned steps carries out UV exposure using strained layer mask plate, shows
Shadow；
Step 7: utilizing ion etching, sputtering has TaN strained layer 3, PdCr strained layer 4 and TaN strained layer 5 after development
Strain layer pattern is formed on sandwich structure composite strain layer component；
Step 8: washing away photoresist using acetone, deionized water cleaning is dry；
Step 9: again in the component surface spin coating photoresist for completing above-mentioned steps, carrying out UV exposure using electrode layer mask plate
Light, development；
Step 10: in the component surface magnetron sputtering Pt electrode 7 for completing above-mentioned steps, taking out base vacuum to 10-3~10- 4Pa is passed through Ar gas, and adjusting operating air pressure is 0~10Pa, and sputtering power is 100~400W；
Step 11: washing away photoresist using acetone, deionized water cleaning is dry；
Step 12: the component for completing above-mentioned steps being put into double ion beam sputtered machine, using high-purity sapphire target, is extracted into
Base vacuum 10-3~10-4Pa is passed through Ar gas and O2Gas, adjusting operating air pressure is 10-2Pa, the oxygen of 1~2 μ m thick of sputtering sedimentation
Change aluminium or silicon oxide protective layer 6；
Deposition target used is 99.99% high-purity sapphire target；The Al:O stoichiometry of the protective layer of alumina
Than for 2:3.
In the present embodiment, the TaN strained layer 3, PdCr strained layer 4, TaN strained layer 5 film thickness can be according to need
It is adjusted.
The present invention fine and close, uniform feature using double ion beam sputtered system film forming, will utilize the oxidation of this method preparation
Aluminium insulating film is applied to superalloy components substrate and strains the high-temperature insulation of strained layer.And according to the temperature of TaN and PdCr
Resistance characteristic is prepared for self-compensating high-temp strain strained layer.Manufacture craft of the present invention is simple, low in cost, strain gauge performance
Reliably, it is able to solve the predicament encountered at present to the component strain real-time monitoring to work under high temperature environment.
To sum up, the ion beam sputtering alumina insulating film that the present invention uses, thickness is thin, reliable performance, the influence to component
It is negligible, suitable for the real-time measurement the component course of work；Using TaN and PdCr alloy strained layer, made by self compensation
With the temperature coefficient TCR for the resistance for making strain gauge close to 0, influence of the temperature change to component strain measurement is overcome, high temperature is made
Measurement accuracy greatly improves；It is good using ion beam sputtering aluminium oxide or silicon oxide protective layer compact structure, binding force, to function knot
Structure plays extraordinary protective effect.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (10)
1. a kind of high-temperature self-compensating multi-layer compound film strain gauge, which is characterized in that the strain gauge includes superalloy components
Substrate (1), alumina insulating layer (2), the first TaN strained layer (3), PdCr strained layer (4), the 2nd TaN strained layer (5), oxidation
Aluminium or silicon oxide protective layer (6) and Pt electrode (7), in which: alumina insulating layer (2) is deposited on superalloy components substrate (1)
On；First TaN strained layer (3) is deposited on alumina insulating layer (2)；PdCr strained layer (4) is deposited on the first TaN strained layer
(3) on；2nd TaN strained layer (5) is deposited on PdCr strained layer (4)；Aluminium oxide or silicon oxide protective layer (6) are covered in second
On TaN strained layer (5)；Pt electrode (7) be deposited on alumina insulating layer (2) and with side wall simultaneously with the first TaN strained layer
(3), PdCr strained layer (4), the 2nd TaN strained layer (5) are connected with aluminium oxide or silicon oxide protective layer (6), while Pt electrode (7)
Upper surface be exposed to except aluminium oxide or silicon oxide protective layer (6) for lead.
2. a kind of high-temperature self-compensating multi-layer compound film strain gauge according to claim 1, which is characterized in that described answers
Become meter to be prepared in situ on superalloy components substrate (1), the application temperature of superalloy components substrate (1) is 500~1200
℃。
3. a kind of high-temperature self-compensating multi-layer compound film strain gauge according to claim 1, which is characterized in that described
In one TaN strained layer (3), PdCr strained layer (4) and the 2nd TaN strained layer (5), PdCr strained layer (4) is located at the first TaN strain
Layer (3) and the 2nd TaN strained layer (5) are intermediate, the first TaN strained layer (3), PdCr strained layer (4) and the 2nd TaN strained layer (5)
The composite strain layer of sandwich structure is collectively formed, i.e. composition self-compensating strain layer, to eliminate resistance temperature effect.
4. a kind of preparation method of the described in any item high-temperature self-compensating multi-layer compound film strain gauges of claim 1-3, special
Sign is that described method includes following steps:
Step 1, cleaning superalloy components substrate (1)；
Step 2, with double ion beam sputtered machine, the sputtering sedimentation alumina insulating layer (2) on superalloy components substrate (1)；
Step 3, the first TaN strained layer (3) of reaction magnetocontrol sputtering in the superalloy components substrate (1) for completing step 2；
Step 4, the rf magnetron sputtering PdCr strained layer (4) in the superalloy components substrate (1) for completing step 3；
Step 5, the 2nd TaN strained layer (5) of reaction magnetocontrol sputtering in the superalloy components substrate (1) for completing step 4；
Step 6, the spin coating photoresist on the component for completing above-mentioned steps carry out UV exposure, development using strained layer mask plate；
Step 7, using ion etching, sputtering has the first TaN strained layer (3), PdCr strained layer (4) and the 2nd TaN after development
Strain layer pattern is formed on the sandwich structure composite strain layer component of strained layer (5)；
Step 8 washes away photoresist using acetone, and deionized water cleaning is dry；
Step 9, again complete above-mentioned steps component surface spin coating photoresist, using electrode layer mask plate carry out UV exposure,
Development；
Step 10, complete above-mentioned steps component surface magnetron sputtering Pt electrode (7)；
Step 11 washes away photoresist using acetone, and deionized water cleaning is dry；
Step 12, using double ion beam sputtered machine, in the component surface sputtering sedimentation aluminium oxide or silica for completing above-mentioned steps
Protective layer (6).
5. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In, in step 2, the alumina insulating layer (2) with a thickness of 2~4 μm.
6. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In target used in the alumina insulating layer (2) and protective layer of alumina deposition is that 99.99% high ethereal blue is precious
Stone target.
7. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In the Al:O stoichiometric ratio of the alumina insulating layer (2) and the protective layer of alumina is 2:3.
8. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In, in step 3, the first TaN strained layer (3) with a thickness of 100~400nm；In step 5, the 2nd TaN strain
Layer (5) with a thickness of 100~400nm.
9. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In, in step 4, the PdCr strained layer (4) with a thickness of 200~600nm.
10. a kind of preparation method of high-temperature self-compensating multi-layer compound film strain gauge according to claim 4, feature exist
In, in step 12, the aluminium oxide or silicon oxide protective layer (6) with a thickness of 1~2 μm.
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