CN112525062B - Thin film type resistance strain gauge for high-pressure hydrogen sulfide environment - Google Patents
Thin film type resistance strain gauge for high-pressure hydrogen sulfide environment Download PDFInfo
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- CN112525062B CN112525062B CN202011238415.4A CN202011238415A CN112525062B CN 112525062 B CN112525062 B CN 112525062B CN 202011238415 A CN202011238415 A CN 202011238415A CN 112525062 B CN112525062 B CN 112525062B
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 35
- 239000010409 thin film Substances 0.000 title claims abstract description 16
- 239000010408 film Substances 0.000 claims abstract description 123
- 239000000758 substrate Substances 0.000 claims abstract description 104
- 239000010410 layer Substances 0.000 claims abstract description 40
- 229910002555 FeNi Inorganic materials 0.000 claims abstract description 31
- 230000007704 transition Effects 0.000 claims abstract description 19
- 239000002346 layers by function Substances 0.000 claims abstract description 17
- 239000011241 protective layer Substances 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 7
- 239000010935 stainless steel Substances 0.000 claims abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 4
- 238000004544 sputter deposition Methods 0.000 claims description 153
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 64
- 238000000034 method Methods 0.000 claims description 46
- 230000008569 process Effects 0.000 claims description 42
- 229910052786 argon Inorganic materials 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000005498 polishing Methods 0.000 claims description 9
- -1 argon ions Chemical class 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 230000007547 defect Effects 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000007730 finishing process Methods 0.000 claims description 2
- 229910019923 CrOx Inorganic materials 0.000 claims 5
- 238000005259 measurement Methods 0.000 abstract description 6
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 description 16
- 229910052739 hydrogen Inorganic materials 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 14
- 239000000853 adhesive Substances 0.000 description 10
- 230000001070 adhesive effect Effects 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 239000003345 natural gas Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 229910001006 Constantan Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 230000009545 invasion Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- 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
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/08—Ferrous alloys, e.g. steel alloys containing nickel
-
- 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
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive 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
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/042—Coating on selected surface areas, e.g. using masks using masks
-
- 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
- C23C14/0617—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
-
- 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
- C23C14/083—Oxides of refractory metals or yttrium
-
- 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
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon 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
- C23C14/22—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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
- G01L1/2287—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a film type resistance strain gauge for a high-pressure hydrogen sulfide environment, which comprises a substrate, a transition buffer layer arranged on the upper surface of the substrate, an insulating layer arranged on the upper surface of the transition buffer layer, a functional layer arranged on the upper surface of the insulating layer and a protective layer arranged on the upper surface of the functional layer, wherein the transition buffer layer is arranged on the upper surface of the substrate; the substrate is made of 316L stainless steel material, the transition buffer layer is a Cr film, the insulating layer is an AlN film, the functional layer is a FeNi alloy film, and the protective layer is CrO x And (3) a film. In the high-pressure hydrogen sulfide environment, the thin film type resistance strain gauge can be firmly fixed on a sample and is connected with each other to be inorganic, so that zero drift and creep are eliminated, temperature self-compensation is realized, and the sensitivity of the thin film type resistance strain gauge and the accuracy of a measurement result are improved.
Description
Technical Field
The invention relates to the technical field of sensors in high-pressure hydrogen sulfide environments, in particular to a sensor which comprises a Cr film, an AlN film, a FeNi film and CrO x Film-type resistance strain gauge for use in high-pressure hydrogen sulfide environment.
Background
Hydrogen energy is regarded as the clean energy with the most development potential in the 21 st century, and is an ideal energy carrier. At present, the hydrogen production modes mainly comprise four modes: fossil fuel hydrogen production, industrial by-product hydrogen production, electrolyzed water hydrogen production, biomass and other hydrogen production modes. Among them, the economy of natural gas hydrogen production is most remarkable from the viewpoint of cost. The natural gas resources in China are mainly natural gas resources with high content of hydrogen sulfide, and the gas field is mainly distributed in Bohai Bay and Sichuan basin. However, since natural gas having high content of hydrogen sulfide is used as a raw material, the performance of material parts operating in a high-pressure environment is deteriorated, fatigue failure occurs, and the service life is reduced.
The cracking of the metal material in the hydrogen sulfide environment is mainly caused by the permeation of hydrogen atoms generated by the reaction of the metal and a medium on the surface of the metal into the metal. In the process of exploiting, storing and transporting natural gas with high content of hydrogen sulfide, many mechanical parts and components are operated under load under the high pressure hydrogen sulfide environment with the pressure of tens of megapascals, not only the problem of hydrogen embrittlement resistance of the material is needed to be solved, but also the problem of strength and rigidity of the structure under the combined action of the high pressure hydrogen sulfide and the mechanical load is needed to be studied. For complex components, accurate calculation of stress distribution is very difficult, and thus measurement of stress strain is indispensable under high pressure hydrogen sulfide environment. In the stress-strain electrical measurement and sensing technology, taking resistance as a measurement signal is the most commonly used measurement method of strain gauges. However, the resistance of a common foil-type resistance strain gauge changes along with the penetration of hydrogen atoms, which can cause zero drift and creep phenomena of the strain gauge to be aggravated along with the increase of time and pressure, and the accuracy and stability of measurement are seriously affected.
At present, the load sensor under the high-pressure hydrogen sulfide environment developed in China is usually stuck by using an organic adhesive for mounting resistance strain time, but the adhesive materials have a series of problems in the high-pressure hydrogen sulfide environment, so that the service life of the strain gauge is greatly limited. In particular, when the adhesive is contacted with hydrogen sulfide, hydrogen atoms may enter the adhesive by adsorption, invasion, dissolution and diffusion, causing the phenomenon of hydrogen absorption expansion, resulting in failure of the adhesive. In addition, since the adhesive is not a sensing element and is sensitive to environmental conditions and changes due to time, temperature and pressure, it is often the main factor causing strain gauge hysteresis and errors such as creep, zero drift, etc. The adhesive commonly used in the current test is not suitable for test application, so that a stable and accurate resistance strain gauge in a high-pressure hydrogen sulfide environment needs to be developed.
Disclosure of Invention
The invention aims to overcome the defects of strain gauge falling, zero drift and creep caused by the organic adhesive in the high-pressure hydrogen sulfide environment in the prior art, and provides a preparation method of a composite material consisting of a Cr film, an AlN film, a FeNi film and CrO x Film-type resistance strain gauge for use in high-pressure hydrogen sulfide environment.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a thin film type resistance strain gauge used in a high-pressure hydrogen sulfide environment comprises a substrate, a transition buffer layer arranged on the upper surface of the substrate, an insulating layer arranged on the upper surface of the transition buffer layer, a functional layer arranged on the upper surface of the insulating layer and a protective layer arranged on the upper surface of the functional layer; the substrate is made of 316L stainless steel material, the transition buffer layer is a Cr film, and the insulating layer is an AlN film.
Preferably, the functional layer is a FeNi alloy film, and the protective layer is CrO x And (3) a film.
The functional layer is sputtered on the insulating layer by a mask plate method. The mask plate is manufactured by laser processing after size design by adopting a photoetching technology.
A preparation method of a film type resistance strain gauge comprises the following steps:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument for fixation and arrangement;
(3-2) putting the Cr target and the Al target into a sputtering chamber, sputtering a Cr film on the upper surface of the substrate to form a Cr film with the thickness of 100 nm-300 nm, and taking the Cr film as a transition buffer layer;
(3-3) introducing nitrogen into the sputtering chamber, sputtering an AlN film with the thickness of 200-400 nm on the upper surface of the Cr film, and taking the AlN film as an insulating layer;
(3-4) powering off the magnetron sputtering instrument, stopping introducing nitrogen, and reducing the temperature in the sputtering chamber to below 60-80 ℃; taking out the Al target and the substrate in the sputtering chamber, and covering the upper surface of the substrate with a mask plate; placing the substrate covered with the mask plate on a sample stage of a magnetron sputtering instrument, mounting a FeNi alloy target on a B target seat, and sputtering a grid-shaped FeNi film with the thickness of 600nm-1200nm on the mask plate;
(3-5) introducing oxygen into the sputtering chamber, and sputtering CrO with a thickness of 15-30 nm on the upper surface of the FeNi film x Film of CrO x The film serves as a protective layer; taking out the sputtering chamber and sputtering Cr film, alN film, feNi film and CrO x A substrate of the film;
and (3-6) placing the substrate on a heating zone of a furnace tube in a vacuum tube furnace, installing heat insulation furnace plugs at two ends of the furnace tube, and performing vacuum heat treatment to obtain the manufactured film type resistance strain gauge.
The pretreatment process of the substrate in the first step specifically comprises the following steps: sequentially polishing the upper surface of the substrate step by using 400# abrasive paper, 600# abrasive paper, 800# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper, and mechanically polishing by using a 0.1 mu m diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratches; placing a substrate with a smooth surface into a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to be downward, and pouring acetone and alcohol into the beaker in a ratio of 1:1 or 1:2. Placing the beaker with the substrate into an ultrasonic cleaner, oscillating ultrasonically for 15-20 min, and oscillating and stripping greasy dirt and impurities on the upper surface of the substrate by utilizing cavitation of ultrasonic waves in liquid; and taking out the substrate after the ultrasonic cleaning is finished, and drying for later use.
Preferably, the fixing and finishing process comprises the steps of:
respectively fixing a Cr target and an Al target on an A target seat and a C target seat in a sputtering chamber; placing the pretreated substrate on a sample turntable in a sputtering chamber, enabling the cleaned surface of the substrate to face downwards and to face the centers of an A target seat, a B target seat and a C target seat, enabling the distance between each target seat and the sample turntable to be 60 mm-80 mm, inserting a heating substrate into the back of the sample turntable, and fixing the substrate by using a clamp.
Preferably, the process of sputtering the Cr film includes the steps of:
evacuating the sputtering chamber to 1.0X10 -3 Pa or lower, heat transfer is performed by heating the substrate to make the sampleThe temperature of the substrate of the turntable is raised to 100-150 ℃, the bias voltage is regulated to 80-100V, argon is introduced into a sputtering chamber, the flow rate of the argon is controlled to 20-25 sccm, the air pressure in the sputtering chamber is raised to 1 Pa-2 Pa, the voltage of the target seat A is raised to 300-400V for glow discharge, the argon is ionized, argon ions are generated, and the argon ions bombard the Cr target, so that the target is sputtered; adjusting the working air pressure in the sputtering chamber to 0.3+/-0.2 Pa, and performing pre-sputtering for 5-10 min; after stabilizing the voltage and current of the target seat A through a pre-sputtering process, controlling the rotation speed of the sample turntable to be 2 r/min-4 r/min, regulating the voltage and current of the target seat A to enable the power to reach 90W-120W, and continuously sputtering for 15 min-25 min to form a Cr film on the upper surface of the substrate.
Preferably, the sputtering parameters of the AlN film process are:
adjusting a temperature controller of the sputtering instrument to enable the substrate temperature of the sample turntable to be increased to 250-300 ℃; introducing nitrogen with the flow of 20-25 sccm to make Ar: N 2 1 (0.8-1.2), wherein the air pressure in a sputtering chamber is 0.5 Pa-0.7 Pa in the sputtering process, the power of a C target seat is 120W-150W in the sputtering process, and the sputtering is continued for 60 min-120 min, so that an AlN film is formed on the surface of the substrate on which the Cr film is sputtered.
Preferably, the specification of the FeNi alloy target is: the element proportion is Ni 25-40%, fe balance; the impurity content is less than 0.01%, the cavity defect is less than 1.0mm, the crack is less than 0.1mm, and the grain size is less than 50-60 μm.
Preferably, the sputtering parameters during the sputtering of the FeNi film are:
evacuating the sputtering chamber to 5.0X10 -4 Heating the substrate to 200-300 ℃ below Pa, and introducing argon with the flow of 20-25 sccm, wherein the air pressure in a sputtering chamber is 0.2-0.3 Pa in the sputtering process; the power of the B target seat in the sputtering process is 250+/-5W, and the sputtering time is 40-60 min.
Preferably, crO is sputtered x The sputtering parameters in the film process are:
adjusting a temperature controller of the sputtering instrument to enable the substrate temperature of the sample turntable to be reduced to 100-150 ℃; introducing oxygen with flow rate of 30 sccm-50 sccm to make Ar: O 2 1 (1.8-2.2), sputtering in the sputtering processThe indoor air pressure is 0.5 plus or minus 0.3Pa, the power of the target seat A is 50W-100W in the sputtering process, the sputtering time is 10 min-15 min, and CrO is formed on the surface of the substrate on which the FeNi film is sputtered x A membrane;
the vacuum heat treatment process comprises the following steps:
vacuumizing the furnace tube of the vacuum tube furnace to below 0.3MPa, and introducing argon into the furnace tube, wherein the argon is used for protecting the surface of the film type resistance strain gauge, so that the flow rate of the argon is 5L/min-7L/min; setting the heating temperature of the vacuum tube furnace to 600-800 ℃ and preserving the heat for 8-10 hours; and after the heat preservation time is up, the vacuum tube furnace is powered off, and when the temperature in the vacuum tube furnace is lower than 150 ℃, the film type resistance strain gauge is taken out.
The beneficial effects of the invention are as follows:
1) Compared with the resistance strain gauge stuck by the common adhesive, the film type resistance strain gauge directly grows on the substrate in a film form, so that the problems of strain transmission error and pressure influence caused by the adhesive are avoided while hydrogen contact is reduced.
2) The Cr film is used as a transition buffer layer, and carbon compounds are formed when the film is formed, so that the extension of tissue defects is prevented, the dislocation density is reduced, and the stress concentration generated between the substrate and the insulating layer is well relieved; the AlN film is used as an insulating layer, and the resistivity is improved by reducing irregular scattering of electrons at a grain boundary and an interface; the FeNi film is a single-phase iron-based solid solution and is in a bcc structure, so that the FeNi film has lower hydrogen solubility and hydrogen diffusion coefficient, and the invasion of hydrogen in the film-type resistance strain gauge is greatly reduced; crO (CrO) x The film is used as a protective layer to form CrO and CrO 2 、Cr 2 O 3 Mixed oxide, further preventing penetration of hydrogen, while CrO x The film has high hardness, can protect the surface of the functional layer and has the function of friction and abrasion resistance.
3) Cr/AlN/FeNi/CrO in high-pressure hydrogen sulfide environment x The film resistance strain gauge composed of multiple layers of films can be firmly fixed on a sample and are connected with each other in an inorganic way, so that zero drift and creep are eliminated, temperature self-compensation is realized, and the sensitivity of the strain gauge is improvedAnd accuracy of the measurement results.
Drawings
FIG. 1 is a schematic cross-sectional view of one construction of the present invention;
FIG. 2 is an enlarged view of a subjective and functional layer template of the present invention;
fig. 3 is a graph comparing creep performance of a conventional bonded Kang Tongbo resistance strain gauge with the present invention in an 8MPa hydrogen sulfide environment.
In the figure: 1. the device comprises a substrate, 2, a transition buffer layer, 3, an insulating layer, 4, a functional layer, 5, a protective layer, 6, solder, 7, a lead wire, 8 and a mask plate.
Detailed Description
The invention is further described below with reference to the drawings and detailed description.
Example 1
As shown in fig. 1 and 2, a thin film type resistance strain gauge for use in a high-pressure hydrogen sulfide environment comprises a substrate 1, a transition buffer layer 2 arranged on the upper surface of the substrate, an insulating layer 3 arranged on the upper surface of the transition buffer layer, a functional layer 4 arranged on the upper surface of the insulating layer, and a protective layer 5 arranged on the upper surface of the functional layer; the substrate is made of 316L stainless steel material, the transition buffer layer is a Cr film, and the insulating layer is an AlN film. The functional layer is a FeNi alloy film. The two leads 7 are connected with the protective layer 5 through solder 6;
a preparation method of a film type resistance strain gauge comprises the following steps:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument for fixation and arrangement;
sequentially polishing the upper surface of the substrate step by using 400# abrasive paper, 600# abrasive paper, 800# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper, and mechanically polishing by using a 0.1 mu m diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratches. Placing the substrate with the smooth surface into a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to be downward, and pouring acetone and alcohol into the beaker in a ratio of 1:1. Placing the beaker with the substrate into an ultrasonic cleaner, oscillating for 15min by ultrasonic, and oscillating and stripping greasy dirt and impurities on the upper surface of the substrate by cavitation of ultrasonic in liquid. And taking out the substrate after the ultrasonic cleaning is finished, and drying for later use.
Respectively fixing a Cr target and an Al target on an A target seat and a C target seat in a sputtering chamber of a magnetron sputtering instrument (JGP 450 type rapid ion plating instrument); placing the pretreated substrate on a sample turntable in a sputtering chamber, enabling the cleaned surface of the substrate to face downwards and to face the centers of an A target seat, a B target seat and a C target seat, enabling the distance between each target seat and the sample turntable to be 65 mm, inserting a heating substrate into the back of the sample turntable, and fixing the substrate by using a clamp.
(3-2) after the Cr target and the Al target are placed in a sputtering chamber, sputtering a Cr film on the upper surface of the substrate to form a Cr film with the thickness of 200nm, and taking the Cr film as a transition buffer layer;
evacuating the sputtering chamber to 8.0X10 -4 Pa, heating the substrate to transfer heat to enable the temperature of the substrate of the sample turntable to be increased to 120 ℃, adjusting the bias voltage to 95V, introducing argon into a sputtering chamber, controlling the flow of the argon to be 22sccm, increasing the air pressure in the sputtering chamber to 1.8Pa, enabling the voltage of the target seat A to be increased to 300V for glow discharge, enabling the argon to be ionized, generating argon ions, enabling the argon ions to bombard Cr target, and causing sputtering of the target; adjusting the working air pressure in the sputtering chamber to 0.25Pa, and performing pre-sputtering for 5min; after stabilizing the voltage and current of the target seat A through the pre-sputtering process, controlling the rotation speed of the sample turntable at 4r/min, regulating the voltage and current of the target seat A to enable the power to reach 110W, and continuously sputtering for 15min to form a Cr film on the upper surface of the substrate.
(3-3) introducing nitrogen into the sputtering chamber, sputtering an AlN film with the thickness of 200nm on the upper surface of the Cr film, and taking the AlN film as an insulating layer;
the temperature controller of the sputtering instrument is regulated to raise the substrate temperature of the sample turntable to 250 ℃, increase the atomic energy participating in the chemical combination reaction in the sputtering process, ensure high film crystallinity, and lead the nitrogen flow to be 22sccm to lead Ar to N 2 The pressure in the sputtering chamber is 0.6Pa in the sputtering process, the power of the C target seat in the sputtering process is 120W, the sputtering is continued for 60min, and an AlN film is formed on the surface of the substrate on which the Cr film is sputtered.
(3-4) powering off the magnetron sputtering instrument, stopping introducing nitrogen, and reducing the temperature in the sputtering chamber to 50 ℃; taking out the Al target and the substrate in the sputtering chamber, and covering the upper surface of the substrate with a mask plate 8; placing the substrate covered with the mask plate on a sample stage of a magnetron sputtering instrument, mounting an FeNi alloy target on a B target seat, and sputtering a grid-shaped FeNi film with the thickness of 800nm on the mask plate;
the FeNi alloy target has the following specification: the element proportion composition is Ni 35 percent and Fe 65 percent; the impurity content is less than 0.01%, the cavity defect is less than 1.0mm, the crack is less than 0.1mm, and the grain size is less than 60 μm.
The sputtering parameters in the process of sputtering the FeNi film are as follows:
evacuating the sputtering chamber to 3.0X10 -4 Pa, heating the substrate to 300 ℃, and introducing argon with the flow of 20sccm, wherein the air pressure in a sputtering chamber is 0.2Pa in the sputtering process; the power of the B target seat is 250W in the sputtering process, and the sputtering power is increased within a certain range, so that the surface grain density and the element content can be increased; the sputtering time was 40min.
(3-5) introducing oxygen into the sputtering chamber, and sputtering CrO with a thickness of 20nm on the upper surface of the FeNi film x Film of CrO x The film serves as a protective layer; taking out the sputtering chamber and sputtering Cr film, alN film, feNi film and CrO x A substrate of the film;
adjusting a temperature controller of the sputtering instrument to enable the temperature of the substrate of the sample turntable to be reduced to 150 ℃; introducing oxygen with flow rate of 40sccm to make Ar: O 2 The pressure in the sputtering chamber is 0.7Pa in the sputtering process, the power of the target seat A in the sputtering process is 80W, the sputtering is continued for 10min, and CrO is formed on the surface of the substrate on which the FeNi film is sputtered x A membrane;
and (3-6) placing the substrate on a heating zone of a furnace tube in a vacuum tube furnace (NBD-0 series open type high temperature furnace), installing heat insulation furnace plugs at two ends of the furnace tube, and performing vacuum heat treatment to obtain the manufactured film type resistance strain gauge.
Vacuumizing the furnace tube of the vacuum tube furnace to 0.2MPa, and then introducing argon into the furnace tube, wherein the argon is used for protecting the surface of the film type resistance strain gauge, so that the flow rate of the argon is 7L/min; setting the heating temperature of the vacuum tube furnace to 800 ℃ and preserving the heat for 8 hours; the heat treatment under the condition can eliminate the film stress, increase the bonding force between film layers, reduce the defect density and optimize the film quality; and after the heat preservation time is up, the vacuum tube furnace is powered off, and when the temperature in the vacuum tube furnace is lower than 100 ℃, the film type resistance strain gauge is taken out.
In order to compare the creep performance of a normally stuck constantan foil type resistance strain gauge with that of a thin film type resistance strain gauge used in a high-pressure hydrogen sulfide environment, a multifunctional static strain gauge is used for measuring the strain value of the resistance strain gauge in an environment box. The test comprises the following specific processes:
step 1: welding two leads on welding spots of the resistance strain gauge respectively by using an electric soldering iron, and then welding wires at the inner ends of the joints on the environment box with the leads by using a wiring terminal;
step 2: slowly placing the welded resistance strain gauge into an environment box, connecting the strain gauge with a strain gauge (JM 3811 static strain tester) through a wire at the outer end of a connector on the environment box, connecting the strain gauge with a PC terminal through a USB wire of the strain gauge, covering an upper cover of the environment box, and sealing the environment box through bolts;
step 3: opening a molecular pump, firstly pumping out the gas in a pipeline connected with the environment box, then opening an upper valve of the environment box, pumping out the air in the environment box completely, enabling the pressure in the environment box to be 0.1MPa below zero, closing the upper valve of the environment box, and finally closing the molecular pump;
step 4: and opening strain acquisition software on the PC terminal, introducing hydrogen sulfide gas into the environment box until the pressure reaches 8MPa, stretching the resistance strain gauge to a certain deformation amount in the environment box and keeping the deformation amount for 30 hours, and observing the change condition of a strain value on the strain gauge.
Fig. 3 shows creep curves of a normally-adhered constantan foil type resistance strain gauge and the thin film type resistance strain gauge used in a high-pressure hydrogen sulfide environment in an 8MPa hydrogen sulfide gas environment. As can be seen from fig. 3, after the strain recovery for 5 hours, the hydrogen induced strain residual of the conventional constantan strain gauge is still large, the creep recovery is slow, and the difference from the thin film resistance strain gauge in the high-pressure hydrogen sulfide environment is very obvious. Therefore, the thin film type resistance strain gauge in the high-pressure hydrogen sulfide environment has better resilience, can return to the initial strain more quickly after hydrogen is discharged, and has better resistance strain gauge service performance.
Example 2
This embodiment differs from embodiment 1 in that:
the Cr film was used as a transition buffer layer with a thickness of 300nm.
Evacuating the sputtering chamber to 5.0X10 -4 Pa, heating the substrate to transfer heat to enable the temperature of the substrate of the sample turntable to be raised to 100 ℃, adjusting the bias voltage to 80V, introducing argon into a sputtering chamber, controlling the flow of the argon to be 25sccm, raising the air pressure in the sputtering chamber to 1.8Pa, raising the voltage of the target seat A to 350V for glow discharge, ionizing the argon to generate argon ions, and bombarding Cr target by the argon ions to cause sputtering of the target; adjusting the working air pressure in the sputtering chamber to 0.15Pa, and performing pre-sputtering for 10min; after stabilizing the voltage and current of the target seat A through the pre-sputtering process, controlling the rotation speed of the sample turntable at 2r/min, regulating the voltage and current of the target seat A to enable the power to reach 120W, and continuously sputtering for 25min to form a Cr film on the upper surface of the substrate.
The other contents are the same as those in embodiment 1.
Example 3
This embodiment differs from embodiment 1 in that:
sputtering an AlN film with the thickness of 400nm on the upper surface of the Cr film to serve as an AlN insulating layer;
the temperature controller of the sputtering instrument is adjusted to raise the substrate temperature of the sample turntable to 300 ℃, and the nitrogen flow is 25sccm to enable Ar to N 2 The pressure in the sputtering chamber is 0.5Pa in the sputtering process, the power of the C target seat in the sputtering process is 150W, the sputtering is continued for 120min, and an AlN film is formed on the surface of the substrate on which the Cr film is sputtered;
sputtering a grid-shaped FeNi film with the thickness of 1000nm on the mask plate to serve as a functional layer;
the sputtering parameters in the process of sputtering the FeNi film are as follows: evacuating the sputtering chamber to 1.0X10 -4 Pa, heating the substrate to 200 ℃, introducing argon with the flow of 22sccm, and sputteringThe air pressure in the sputtering chamber in the process is 0.3Pa; the power of the B target seat in the sputtering process is 255W, and the sputtering time is 60min.
The other contents are the same as those of example 1.
Example 4
This embodiment differs from embodiment 1 in that:
sputtering CrO x The thickness of the film was 30nm, and the sputtering parameters were: adjusting a temperature controller of the sputtering instrument to enable the temperature of the substrate of the sample turntable to be reduced to 120 ℃; introducing oxygen with flow rate of 48sccm to make Ar: O 2 The ratio of the sputtering pressure to the sputtering pressure is 1:2.2, the air pressure in the sputtering chamber is 0.8Pa, the power of the target seat A in the sputtering process is 100W, the sputtering is continued for 15min, and CrO is formed on the surface of the substrate on which the FeNi film is sputtered x A membrane;
vacuumizing the furnace tube of the vacuum tube furnace to 0.3MPa, and then introducing argon into the furnace tube, wherein the argon is used for protecting the surface of the film type resistance strain gauge, so that the flow rate of the argon is 6L/min; the heating temperature of the vacuum tube furnace was set at 600℃and kept for 10 hours.
The other contents are the same as in example 1.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (7)
1. The preparation method of the film type resistance strain gauge used in the high-pressure hydrogen sulfide environment is characterized by comprising the following steps:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument for fixation and arrangement;
(3-2) putting the Cr target and the Al target into a sputtering chamber, sputtering a Cr film on the upper surface of the substrate to form a Cr film with the thickness of 100 nm-300 nm, and taking the Cr film as a transition buffer layer; the process of sputtering the Cr film comprises the following steps: evacuating the sputtering chamber to 1.0X10 -3 Heating the substrate to heat transfer to make the substrate temperature of the sample turntable to 100-150deg.C, regulating bias voltage to 80V-100V, introducing argon into the sputtering chamber, controlling the flow of the argon to be 20sccm-25sccm, increasing the air pressure in the sputtering chamber to 1 Pa-2 Pa, increasing the voltage of the target seat A to 300V-400V for glow discharge, ionizing the argon to generate argon ions, and bombarding the Cr target by the argon ions to cause sputtering of the target; adjusting the working air pressure in the sputtering chamber to 0.3+/-0.2 Pa, and performing pre-sputtering for 5-10 min; after stabilizing the voltage and current of the target seat A through a pre-sputtering process, controlling the rotation speed of the sample turntable to be 2 r/min-4 r/min, regulating the voltage and current of the target seat A and the target seat B to enable the power to reach 90W-120W, and continuously sputtering for 15 min-25 min to form a Cr film on the upper surface of the substrate;
(3-3) introducing nitrogen into the sputtering chamber, sputtering an AlN film with the thickness of 200-400 nm on the upper surface of the Cr film, and taking the AlN film as an insulating layer; the sputtering parameters of the AlN film process are as follows: adjusting a temperature controller of a sputtering instrument to enable the substrate temperature of a sample turntable to be raised to 250-300 ℃, introducing nitrogen with the flow of 20-25 sccm to enable Ar to be 1 (0.8-1.2), enabling the air pressure in a sputtering chamber to be 0.5 Pa-0.7 Pa in the sputtering process, enabling the power of a C target seat to be 120W-150W in the sputtering process, and continuously sputtering for 60-120 min, so as to form an AlN film on the surface of a substrate on which a Cr film is sputtered;
(3-4) powering off the magnetron sputtering instrument, stopping introducing nitrogen, and reducing the temperature in the sputtering chamber to below 60-80 ℃; taking out the Al target and the substrate in the sputtering chamber, and covering a mask plate (8) on the upper surface of the substrate; placing the substrate covered with the mask plate on a sample stage of a magnetron sputtering instrument, mounting a FeNi alloy target on a B target seat, and sputtering a grid-shaped FeNi film with the thickness of 600nm-1200nm on the mask plate; the sputtering parameters in the process of sputtering the FeNi film are as follows: vacuumizing the sputtering chamber to below 5.0X10-4 Pa, heating the substrate to 200-300 ℃, and introducing argon with the flow of 20-25 sccm, wherein the air pressure in the sputtering chamber is 0.2-0.3 Pa in the sputtering process; the power of the B target seat is 250+/-5W in the sputtering process, and the sputtering time is 40-60 min;
(3-5) introducing oxygen into the sputtering chamber, sputtering a CrOx film with the thickness of 15-30 nm on the upper surface of the FeNi film, and taking the CrOx film as a protective layer; the sputtering parameters in the process of sputtering the CrOx film are as follows: adjusting a temperature controller of the sputtering instrument to enable the substrate temperature of the sample turntable to be reduced to 100-150 ℃; introducing oxygen with the flow of 30 sccm-50 sccm to enable Ar to be O2 to be 1 (1.8-2.2), wherein the air pressure in a sputtering chamber is 0.5+/-0.3 Pa in the sputtering process, the power of an A target seat in the sputtering process is 50W-100W, the sputtering time is 10 min-15 min, and a CrOx film is formed on the surface of the substrate on which the FeNi film is sputtered; taking out the substrate sputtered with the Cr film, the AlN film, the FeNi film and the CrOx film in the sputtering chamber;
and (3-6) placing the substrate on a heating zone of a furnace tube in a vacuum tube furnace, installing heat insulation furnace plugs at two ends of the furnace tube, and performing vacuum heat treatment to obtain the manufactured film type resistance strain gauge.
2. The method of manufacturing a thin film resistance strain gauge for use in a high pressure hydrogen sulfide environment of claim 1, wherein the substrate pretreatment process comprises the steps of:
sequentially polishing the upper surface of the substrate step by using 400# abrasive paper, 600# abrasive paper, 800# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper, and mechanically polishing by using a 0.1 mu m diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratches; placing a substrate with a smooth surface into a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to be downward, and pouring acetone and alcohol into the beaker in a ratio of 1:1 or 1:2; placing the beaker with the substrate into an ultrasonic cleaner, oscillating ultrasonically for 15-20 min, and oscillating and stripping greasy dirt and impurities on the upper surface of the substrate by utilizing cavitation of ultrasonic waves in liquid; and taking out the substrate after the ultrasonic cleaning is finished, and drying for later use.
3. The method of manufacturing a thin film resistance strain gauge for use in a high pressure hydrogen sulfide environment of claim 1, wherein the fixing and finishing process comprises the steps of:
respectively fixing a Cr target and an Al target on an A target seat and a C target seat in a sputtering chamber; placing the pretreated substrate on a sample turntable in a sputtering chamber, enabling the cleaned surface of the substrate to face downwards and to face the centers of an A target seat, a B target seat and a C target seat, enabling the distance between each target seat and the sample turntable to be 60 mm-80 mm, inserting a heating substrate into the back of the sample turntable, and fixing the substrate by using a clamp.
4. The method for manufacturing a thin film resistance strain gauge for use in a high pressure hydrogen sulfide environment of claim 1, wherein the FeNi alloy target has the following specifications: the element proportion is Ni 25-40%, fe balance; the impurity content is less than 0.01%, the cavity defect is less than 1.0mm, the crack is less than 0.1mm, and the grain size is less than 50-60 μm.
5. The method for manufacturing a thin film resistance strain gauge for use in a high pressure hydrogen sulfide environment as claimed in claim 1,
the vacuum heat treatment process comprises the following steps:
vacuumizing the furnace tube of the vacuum tube furnace to below 0.3MPa, and introducing argon into the furnace tube of the vacuum tube furnace, wherein the argon is used for protecting the surface of the film type resistance strain gauge, so that the flow rate of the argon is 5L/min-7L/min; setting the heating temperature of the vacuum tube furnace to 600-800 ℃ and preserving the heat for 8-10 hours; and after the heat preservation time is up, the vacuum tube furnace is powered off, and when the temperature in the vacuum tube furnace is lower than 150 ℃, the film type resistance strain gauge is taken out.
6. A thin film resistance strain gauge prepared by the method for preparing a thin film resistance strain gauge in high pressure hydrogen sulfide environment according to claim 1, comprising a substrate (1), a transition buffer layer (2) arranged on the upper surface of the substrate, an insulating layer (3) arranged on the upper surface of the transition buffer layer, a functional layer (4) arranged on the upper surface of the insulating layer, and a protective layer (5) arranged on the upper surface of the functional layer; the substrate is made of 316L stainless steel material, the transition buffer layer is a Cr film, and the insulating layer is an AlN film.
7. The gauge according to claim 6, wherein the functional layer is a FeNi alloy film.
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