CN112525062A - Film type resistance strain gauge used in high-pressure hydrogen sulfide environment - Google Patents

Film type resistance strain gauge used in high-pressure hydrogen sulfide environment Download PDF

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CN112525062A
CN112525062A CN202011238415.4A CN202011238415A CN112525062A CN 112525062 A CN112525062 A CN 112525062A CN 202011238415 A CN202011238415 A CN 202011238415A CN 112525062 A CN112525062 A CN 112525062A
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film
sputtering
substrate
strain gauge
target
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CN112525062B (en
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刘哲晔
张�林
张雯丽
张万亮
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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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
    • 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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Abstract

The invention discloses a film type resistance strain gauge used in a high-pressure hydrogen sulfide environment, which comprises a substrate and a film type resistance strain gauge arranged on the upper surface of the substrateThe buffer layer, the insulating layer arranged on the upper surface of the buffer layer, the functional layer arranged on the upper surface of the insulating layer and the 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, the insulating layer is an AlN film, the functional layer is a FeNi alloy film, and the protective layer is CrOxAnd (3) a membrane. In the high-pressure hydrogen sulfide environment, the film type resistance strain gauge can be firmly fixed on the sample and connected with each other in an inorganic manner, so that zero drift and creep deformation are eliminated, and temperature self-compensation is realized, thereby improving the sensitivity of the film type resistance strain gauge and the accuracy of the measurement result.

Description

Film type resistance strain gauge used in high-pressure hydrogen sulfide environment
Technical Field
The invention relates to the technical field of sensors in a high-pressure hydrogen sulfide environment, in particular to a sensor consisting of a Cr film, an AlN film, a FeNi film and CrOxThe film type resistance strain gauge is formed by a film and used in a high-pressure hydrogen sulfide environment.
Background
Hydrogen energy is regarded as the most promising clean energy source in the 21 st century and is an ideal energy carrier. At present, the hydrogen production modes mainly comprise four modes: hydrogen production by fossil fuel, industrial byproduct hydrogen production, hydrogen production by water electrolysis, biomass and other hydrogen production modes. Among them, the economics of natural gas hydrogen production are most significant from a cost perspective. The natural gas resource in China is mainly high-sulfur hydrogen sulfide natural gas resource, and gas fields are mainly distributed in Bohai Bay and Sichuan basins. However, since natural gas having a high content of hydrogen sulfide is used as a raw material, the properties of material parts which operate in a high-pressure environment are deteriorated, fatigue failure occurs, and the service life is reduced.
The cracking of metal material in hydrogen sulfide environment is mainly caused by the penetration of hydrogen atoms generated by the reaction of metal surface and medium into the metal. In the process of exploiting, storing and transporting natural gas containing high-content hydrogen sulfide, a plurality of mechanical parts and parts are loaded and operated in a high-pressure hydrogen sulfide environment as high as tens of megapascals, so that the problem of hydrogen brittleness resistance of the material is urgently solved, and the problems of strength and rigidity of the structure under the combined action of the high-pressure hydrogen sulfide and the mechanical load are also researched. For complex parts, it is very difficult to accurately calculate the stress distribution, so under a high-pressure hydrogen sulfide environment, the measurement of stress strain is indispensable. In the technology of stress-strain electrical measurement and sensing, resistance is the most commonly used measurement method for strain gauges as a measurement signal. However, the resistance of a common foil type resistance strain gauge changes along with the penetration of hydrogen atoms, which causes the zero drift and creep phenomena of the strain gauge to be intensified along with the increase of time and pressure, and seriously influences the accuracy and stability of measurement.
At present, in load sensors developed in China under a high-pressure hydrogen sulfide environment, an organic adhesive is usually used for adhering when a resistance strain gauge is installed, 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 comes into contact with hydrogen sulfide, hydrogen atoms enter the adhesive by adsorption, intrusion, dissolution and diffusion, causing the adhesive to expand by absorbing hydrogen, resulting in failure of the adhesive. In addition, since the adhesive is not a sensing element, is sensitive to environmental conditions, and changes due to time, temperature, and pressure, it tends to be a major factor in causing errors such as strain gauge hysteresis and creep, zero drift, and the like. At present, the common adhesive is not suitable for test application, so that the 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 shedding, zero drift and creep caused by organic adhesive in a high-pressure hydrogen sulfide environment in the prior art, and provides a Cr film, an AlN film, a FeNi film and a CrO filmxThe film type resistance strain gauge is formed by a film and used in a high-pressure hydrogen sulfide environment.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a 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 CrOxAnd (3) a membrane.
The functional layer is sputtered onto 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 thin film type resistance strain gauge comprises the following steps:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument, and fixing and finishing;
(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 nm-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 be below 60-80 ℃; taking out the Al target material and the substrate in the sputtering chamber, and covering a mask plate on the upper surface of the substrate; placing the substrate covered with the mask plate on a sample table of a magnetron sputtering instrument, mounting the FeNi alloy target material 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 the thickness of 15 nm-30 nm on the upper surface of the FeNi filmxFilm of CrOxThe film is used as a protective layer; taking out the sputtered Cr film, AlN film, FeNi film and CrO film in the sputtering chamberxA substrate for the film;
and (3-6) placing the substrate on a heating area of a furnace tube in the vacuum tube furnace, installing insulating furnace plugs at two ends of the furnace tube, and performing vacuum heat treatment to obtain the manufactured film type resistance strain gauge.
Wherein, the pretreatment process of the substrate in the first step is as follows: sequentially grinding the upper surface of the substrate by 400#, 600#, 800#, 1000#, 1500# and 2000# sandpaper step by step, and mechanically polishing by using a 0.1-micrometer diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratch; placing a substrate with a smooth surface in a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to face downwards, 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 cleaning machine, ultrasonically oscillating for 15-20 min, and oscillating and stripping the greasy dirt sundries on the upper surface of the substrate by utilizing the cavitation action of ultrasonic waves in liquid; and after the ultrasonic cleaning is finished, taking out the substrate, 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 be opposite to the centers of a target seat A, a target seat B and a target seat C, enabling the distance between each target seat and the sample turntable to be 60-80 mm, inserting the 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:
the sputtering chamber was evacuated to 1.0X 10-3Heating a substrate to transfer heat to raise the temperature of a substrate of the sample turntable to 100-150 ℃ below Pa, adjusting the bias voltage to 80-100V, introducing argon into a sputtering chamber, controlling the flow of the argon to be 20-25 sccm, raising the air pressure in the sputtering chamber to 1-2 Pa, raising the voltage of a target seat A to 300-400V, performing glow discharge, ionizing the argon to generate argon ions, and bombarding a 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 carrying out pre-sputtering for 5-10 min; after the pre-sputtering process is carried out, the voltage and the current of the target holder A are stabilized, the rotation speed of the sample turntable is controlled to be 2 r/min-4 r/min, the voltage and the current of the target holder A are adjusted to enable the power to reach 90W-120W, the sputtering is carried out for 15 min-25 min continuously, and a Cr film is formed on the upper surface of the substrate.
Preferably, the sputtering parameters of the AlN film process are as follows:
adjusting a temperature controller of a sputtering instrument to raise the substrate temperature of the sample turntable to 250-300 ℃; introducing nitrogen gas with the flow rate of 20sccm-25sccm to ensure that Ar is equal to N2The pressure in the sputtering chamber is 0.5Pa to 0.7Pa during the sputtering process, the power of the C target holder is 120W to 150W during the sputtering process, the sputtering is continued for 60min to 120min, and an AlN film is formed on the surface of the substrate sputtered with the Cr film.
Preferably, the specification of the FeNi alloy target material is as follows: the element proportion composition is 25-40% of Ni and the balance of Fe; the impurity content is less than 0.01%, the void 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 in the process of sputtering the FeNi film are as follows:
the sputtering chamber is evacuated to 5.0X 10-4Heating the substrate to 200-300 ℃ below Pa, introducing argon with the flow of 20-25 sccm, and controlling the air pressure in the sputtering chamber to be 0.2-0.3 Pa in the sputtering process; the power of the target seat B in the sputtering process is 250 +/-5W, and the sputtering time is 40-60 min.
Preferably, CrO is sputteredxThe sputtering parameters in the film process were:
adjusting a temperature controller of a sputtering instrument to reduce the substrate temperature of the sample turntable to 100-150 ℃; introducing oxygen gas with a flow rate of 30 sccm-50 sccm to make Ar and O21 (1.8-2.2), the air pressure in the sputtering chamber is 0.5 +/-0.3 Pa in the sputtering process, the power of the target seat A in the sputtering process is 50W-100W, the sputtering time is 10 min-15 min, and CrO is formed on the surface of the substrate sputtered with the FeNi filmxA film;
the vacuum heat treatment process comprises the following steps:
vacuumizing a furnace tube of a 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 of the argon is 5L/min-7L/min; setting the heating temperature of a vacuum tube furnace to be 600-800 ℃ and preserving the heat for 8-10 hours; and (4) 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 invention has the beneficial effects that:
1) compared with the resistance strain gauge pasted by the common adhesive, the film type resistance strain gauge directly grows on the substrate in a film form, and 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, forms carbon compound when forming a thin film, prevents the extension of tissue defects, reduces the dislocation density, and better relieves the generation between the substrate and the insulating layerStress concentration; the AlN film is used as an insulating layer, and the resistivity is improved by reducing the irregular scattering of electrons at a crystal boundary and an interface; the FeNi film is a single-phase iron-based solid solution and has a bcc structure, so that the hydrogen solubility and the hydrogen diffusion coefficient are lower, and the invasion of hydrogen in the film type resistance strain gauge is greatly reduced; CrOxThe film is used as a protective layer and forms CrO and CrO2、Cr2O3Mixed oxides, further preventing hydrogen permeation, while CrOxThe film has high hardness, can protect the surface of the functional layer and has the function of resisting friction and abrasion.
3) Cr/AlN/FeNi/CrO in high pressure hydrogen sulfide environmentxThe film type resistance strain gauge composed of the multilayer film can be firmly fixed on a test sample, and the mutual connection is inorganic, so that zero drift and creep deformation are eliminated, and the temperature self-compensation is realized, thereby improving the sensitivity of the strain gauge and the accuracy of the measurement result.
Drawings
FIG. 1 is a schematic structural view of a cross-section of the present invention;
FIG. 2 is an enlarged view of a subjective graph and a functional layer template according to the present invention;
FIG. 3 is a graph comparing creep performance of a conventional bonded constantan foil type resistance strain gauge and the invention under an 8MPa hydrogen sulfide environment.
In the figure: 1. the structure 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, 8 and a mask plate.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1
As shown in fig. 1 and fig. 2, a thin film resistance strain gauge for use in a high-pressure hydrogen sulfide environment includes a substrate 1, a transition buffer layer 2 disposed on an upper surface of the substrate, an insulating layer 3 disposed on an upper surface of the transition buffer layer, a functional layer 4 disposed on an upper surface of the insulating layer, and a protective layer 5 disposed on an 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. Two leads 7 are connected with the protective layer 5 through solder 6;
a preparation method of a thin film type resistance strain gauge comprises the following steps:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument, and fixing and finishing;
and sequentially grinding the upper surface of the substrate by 400#, 600#, 800#, 1000#, 1500# and 2000# sandpaper step by step, and mechanically polishing by using a 0.1-micrometer diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratch. Placing a substrate with a smooth surface in a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to face downwards, and pouring acetone and alcohol into the beaker in a ratio of 1:1. And (3) placing the beaker with the substrate into an ultrasonic cleaning machine, carrying out ultrasonic oscillation for 15min, and oscillating and stripping the greasy dirt impurities on the upper surface of the substrate by utilizing the cavitation action of the ultrasonic waves in the liquid. And after the ultrasonic cleaning is finished, taking out the substrate, 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 fast ion coating instrument); the pretreated substrate is placed on a sample turntable in a sputtering chamber, the cleaned surface of the substrate faces downwards and is opposite to the centers of a target seat A, a target seat B and a target seat C, the distance between each target seat and the sample turntable is 65 mm, and after a heating substrate is inserted into the back of the sample turntable, the substrate is fixed by using a clamp.
(3-2) placing 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 200nm, and taking the Cr film as a transition buffer layer;
the sputtering chamber is vacuumized to 8.0 x 10-4Pa, heating the substrate to transfer heat so as to raise the substrate temperature of the sample turntable to 120 ℃, adjusting the bias voltage to 95V, introducing argon into the sputtering chamber, controlling the flow of the argon to be 22sccm, raising the air pressure in the sputtering chamber to 1.8Pa, raising the voltage of the target seat A to 300V 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 0.25Pa, and carrying out pre-sputtering for 5 min; through the pre-sputtering process, the A target holderAfter the voltage and current are stable, the rotation speed of the sample turntable is controlled to be 4r/min, the voltage and current of the A target holder are adjusted to enable the power to reach 110W, sputtering is continued for 15min, and a Cr film is formed 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;
adjusting the temperature controller of the sputtering instrument to raise the substrate temperature of the sample turntable to 250 deg.C, increasing the atomic energy participating in the chemical combination reaction during sputtering, increasing the crystallinity of the film, introducing nitrogen gas with flow rate of 22sccm, and introducing Ar into the film21:1, the gas pressure in the sputtering chamber during sputtering is 0.6Pa, the power of the C target holder during sputtering is 120W, and the sputtering is continued for 60min, so that an AlN film is formed on the surface of the substrate sputtered with the Cr film.
(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 material 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 table of a magnetron sputtering instrument, mounting the FeNi alloy target material on a B target seat, and sputtering a grid-shaped FeNi film with the thickness of 800nm on the mask plate;
the specification of the FeNi alloy target material is as follows: the element proportion composition is 35 percent of Ni and 65 percent of Fe; the impurity content is less than 0.01%, the void 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 FeNi film sputtering process are as follows:
the sputtering chamber was evacuated to 3.0X 10-4Pa, heating the substrate to 300 ℃, introducing argon with the flow of 20sccm, and keeping the air pressure in the sputtering chamber at 0.2Pa in the sputtering process; the power of the target seat B in the sputtering process is 250W, the sputtering power is increased within a certain range, and the surface grain density and the element content can be increased; the sputtering time was 40 min.
(3-5) introducing oxygen into the sputtering chamber, and sputtering CrO with the thickness of 20nm on the upper surface of the FeNi filmxFilm of CrOxThe film is used as a protective layer; taking out the sputtered Cr film, AlN film, FeNi film and CrO film in the sputtering chamberxA substrate for the film;
for adjusting sputtering apparatusThe temperature controller is used for reducing the substrate temperature of the sample turntable to 150 ℃; introducing oxygen at a flow rate of 40sccm to obtain Ar and O2The ratio of the sputtering gas to the sputtering gas is 1:2, the air pressure in the sputtering chamber is 0.7Pa in the sputtering process, the power of an A target seat in the sputtering process is 80W, the sputtering is continued for 10min, and CrO is formed on the surface of the substrate sputtered with the FeNi filmxA film;
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 a furnace tube of the vacuum tube furnace to 0.2MPa, and introducing argon into the furnace tube, wherein the argon is used for protecting the surface of the thin film type resistance strain gauge, so that the flow of the argon is 7L/min; setting the heating temperature of a vacuum tube furnace to 800 ℃ and preserving the heat for 8 hours; under the condition, the heat treatment 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 deformation performance of the ordinary adhered constantan foil type resistance strain gauge with that of the film type resistance strain gauge used in the high-pressure hydrogen sulfide environment, a multifunctional static strain measuring instrument is adopted to measure the strain value of the resistance strain gauge in the environment box. The specific process of the test is as follows:
step 1: respectively welding two leads on welding spots of the resistance strain gauge by using an electric iron, and then welding a lead at the inner end of a joint on the environment box and the leads together by using a wiring terminal;
step 2: slowly putting the welded resistance strain gauge into an environment box, connecting the resistance strain gauge with a strain gauge (JM 3811 static strain tester) through a lead at the outer end of a joint on the environment box, connecting the resistance strain gauge to a PC terminal through a USB lead of the strain gauge, covering an upper cover of the environment box, and sealing the environment box by using bolts;
and step 3: opening the molecular pump, firstly pumping out gas in a pipeline connected with the environment box, then opening an upper valve of the environment box, completely pumping out air in the environment box to ensure that the pressure in the environment box becomes-0.1 MPa, then closing the upper valve of the environment box, and finally closing the molecular pump;
and 4, step 4: opening strain acquisition software on a PC terminal, introducing hydrogen sulfide gas into the environment box until the pressure reaches 8MPa, stretching the resistance strain gauge to a certain deformation in the environment box, keeping for 30 hours, and observing the change condition of the strain value on the strain gauge.
Fig. 3 shows creep curves of a common adhered constantan foil type resistance strain gauge and the film type resistance strain gauge used in a high-pressure hydrogen sulfide environment under an 8MPa hydrogen sulfide gas environment. As can be seen from fig. 3, after 5 hours of strain recovery, the hydrogen-induced strain residue of the conventional constantan resistance 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 use performance of the resistance strain gauge.
Example 2
The present embodiment is different from embodiment 1 in that:
the Cr film is used as a transition buffer layer and has the thickness of 300 nm.
The sputtering chamber is evacuated to 5.0X 10-4Pa, heating the substrate to heat so as to raise the substrate temperature of the sample turntable to 100 ℃, adjusting the bias voltage to 80V, introducing argon into the 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 the 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 carrying out pre-sputtering for 10 min; after the pre-sputtering process is carried out, the voltage and the current of the target holder A are stabilized, the autorotation speed of the sample turntable is controlled to be 2r/min, the voltage and the current of the target holder A are adjusted to enable the power to reach 120W, the sputtering is carried out for 25min continuously, and a Cr film is formed on the upper surface of the substrate.
The other contents are the same as those in embodiment 1.
Example 3
The present embodiment is different from embodiment 1 in that:
sputtering an AlN film with the thickness of 400nm on the upper surface of the Cr film to form an AlN insulating layer;
adjusting the temperature controller of the sputtering instrument to raise the substrate temperature of the sample turntable to 300 ℃, and introducing 25sccm of nitrogen gas to ensure that Ar is equal to N21:1.2, wherein the air pressure in a sputtering chamber in the sputtering process is 0.5Pa, the power of a C target holder in the sputtering process is 150W, the sputtering is continued for 120min, and an AlN film is formed on the surface of the substrate sputtered with the Cr film;
sputtering a grid FeNi film on a mask plate, wherein the thickness of the grid FeNi film is 1000nm and is used as a functional layer;
the sputtering parameters in the FeNi film sputtering process are as follows: the sputtering chamber was evacuated to 1.0X 10-4Pa, heating the substrate to 200 ℃, introducing argon with the flow of 22sccm, and keeping the air pressure in the sputtering chamber at 0.3Pa in the sputtering process; the power of the B target holder in the sputtering process is 255W, and the sputtering time is 60 min.
The other contents are the same as those of embodiment 1.
Example 4
The present embodiment is different from embodiment 1 in that:
sputtering of CrOxThe thickness of the film was 30nm, and the sputtering parameters were: adjusting a temperature controller of a sputtering instrument to reduce the substrate temperature of the sample turntable to 120 ℃; introducing oxygen at a flow rate of 48sccm to obtain Ar and O2The ratio of the sputtering gas to the sputtering gas is 1:2.2, the air pressure in the sputtering chamber is 0.8Pa in the sputtering process, the power of an A target seat in the sputtering process is 100W, the sputtering is continued for 15min, and CrO is formed on the surface of the substrate sputtered with the FeNi filmxA film;
vacuumizing a furnace tube of the vacuum tube furnace to 0.3MPa, and introducing argon into the furnace tube, wherein the argon is used for protecting the surface of the thin film type resistance strain gauge, so that the flow of the argon is 6L/min; the heating temperature of the vacuum tube furnace is set to 600 ℃ and kept for 10 hours.
The other contents are the same as in embodiment 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (10)

1. A film type resistance strain gauge used in a high-pressure hydrogen sulfide environment is characterized by 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.
2. The thin film resistance strain gauge according to claim 1, wherein the functional layer is an FeNi alloy film.
3. A method for manufacturing a thin film resistance strain gauge suitable for use in the method of claim 1, comprising the steps of:
(3-1) placing the pretreated substrate in a sputtering chamber of a magnetron sputtering instrument, and fixing and finishing;
(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 nm-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 be below 60-80 ℃; taking out the Al target material 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 table of a magnetron sputtering instrument, mounting the FeNi alloy target material 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 the thickness of 15 nm-30 nm on the upper surface of the FeNi filmxFilm of CrOxThe film is used as a protective layer; taking out the sputtered Cr film, AlN film, FeNi film and CrO film in the sputtering chamberxA substrate for the film;
and (3-6) placing the substrate on a heating area of a furnace tube in the vacuum tube furnace, installing insulating furnace plugs at two ends of the furnace tube, and performing vacuum heat treatment to obtain the manufactured film type resistance strain gauge.
4. The method of manufacturing a thin film resistance strain gauge according to claim 3, wherein the pre-treating process of the substrate comprises the steps of:
sequentially grinding the upper surface of the substrate by 400#, 600#, 800#, 1000#, 1500# and 2000# sandpaper step by step, and mechanically polishing by using a 0.1-micrometer diamond spray polishing agent to ensure that the upper surface of the substrate is smooth and has no scratch; placing a substrate with a smooth surface in a beaker with dust-free cloth laid at the bottom, enabling the smooth surface of the substrate to face downwards, 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 cleaning machine, ultrasonically oscillating for 15-20 min, and oscillating and stripping the greasy dirt sundries on the upper surface of the substrate by utilizing the cavitation action of ultrasonic waves in liquid; and after the ultrasonic cleaning is finished, taking out the substrate, and drying for later use.
5. The method for manufacturing a thin film resistance strain gauge according to claim 3, 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 be opposite to the centers of a target seat A, a target seat B and a target seat C, enabling the distance between each target seat and the sample turntable to be 60-80 mm, inserting the heating substrate into the back of the sample turntable, and fixing the substrate by using a clamp.
6. The method for manufacturing a thin film resistance strain gauge according to claim 3, wherein the process of sputtering the Cr film comprises the following steps:
the interior of the sputtering chamber is pumped to be vacuum of 1.0 multiplied by 10-3Pa or less, heating the substrate to transfer heatRaising the substrate temperature of a product turntable to 100-150 ℃, adjusting the bias voltage to 80-100V, introducing argon into a sputtering chamber, controlling the flow of the argon to be 20-25 sccm, raising the air pressure in the sputtering chamber to 1-2 Pa, raising the voltage of a target seat A to 300-400V 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 carrying out pre-sputtering for 5-10 min; after the pre-sputtering process is carried out, the voltage and the current of the target holder A are stabilized, the rotation speed of the sample turntable is controlled to be 2 r/min-4 r/min, the voltage and the current of the target holder A and the target holder B are adjusted to enable the power to reach 90W-120W, the sputtering is carried out for 15 min-25 min continuously, and a Cr film is formed on the upper surface of the substrate.
7. The method for manufacturing the thin film resistance strain gauge according to claim 3, wherein the sputtering parameters of the AlN film process are as follows:
adjusting the temperature controller of the sputtering instrument to raise the substrate temperature of the sample turntable to 250-300 deg.c and introducing nitrogen in the flow rate of 20-25 sccm to Ar in the amount of N2The pressure in the sputtering chamber is 0.5Pa to 0.7Pa during the sputtering process, the power of the C target holder is 120W to 150W during the sputtering process, the sputtering is continued for 60min to 120min, and an AlN film is formed on the surface of the substrate sputtered with the Cr film.
8. The method for manufacturing a thin film resistance strain gauge according to claim 3, wherein the FeNi alloy target has the following specifications: the element proportion composition is 25-40% of Ni and the balance of Fe; the impurity content is less than 0.01%, the void defect is less than 1.0mm, the crack is less than 0.1mm, and the grain size is less than 50-60 μm.
9. The method for manufacturing the thin film resistance strain gauge according to claim 3, wherein sputtering parameters in the FeNi film sputtering process are as follows:
the sputtering chamber is evacuated to 5.0X 10-4Heating the substrate to 200-300 ℃ below Pa, introducing argon with the flow of 20-25 sccm, and controlling the air pressure in the sputtering chamber to be 0.2-0.3 Pa in the sputtering process; the power of the B target holder in the sputtering process is250 plus or minus 5W, and the sputtering time is 40 min-60 min.
10. The method of claim 3, wherein the sputtered CrO is used to form a film-type resistance strain gaugexThe sputtering parameters in the film process were:
adjusting a temperature controller of a sputtering instrument to reduce the substrate temperature of the sample turntable to 100-150 ℃; introducing oxygen gas with a flow rate of 30 sccm-50 sccm to make Ar and O21 (1.8-2.2), the air pressure in the sputtering chamber is 0.5 +/-0.3 Pa in the sputtering process, the power of the target seat A in the sputtering process is 50W-100W, the sputtering time is 10 min-15 min, and CrO is formed on the surface of the substrate sputtered with the FeNi filmxA film; 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 thin film type resistance strain gauge, so that the flow of the argon is 5L/min-7L/min; setting the heating temperature of a vacuum tube furnace to be 600-800 ℃ and preserving the heat for 8-10 hours; and (4) 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.
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GB1247269A (en) * 1968-07-25 1971-09-22 Oki Electric Ind Co Ltd Method of producing tantalum nitride film resistors
JP2000331808A (en) * 1999-05-24 2000-11-30 Toshiba Tec Corp Thin-film resistor, forming method thereof and strain gauge using the same
CN101437663A (en) * 2004-11-09 2009-05-20 得克萨斯大学体系董事会 Fabrication and application of nanofiber ribbons and sheets and twisted and non-twisted nanofiber yarns
CN107267944A (en) * 2017-07-05 2017-10-20 电子科技大学 High temperature film semibridge system strain ga(u)ge and preparation method with temperature self-compensation
CN107532274A (en) * 2015-04-30 2018-01-02 冯·阿登纳有限公司 Method and coating unit
CN107574415A (en) * 2017-08-16 2018-01-12 电子科技大学 A kind of metal-base film sensor gradual transition layer and preparation method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1247269A (en) * 1968-07-25 1971-09-22 Oki Electric Ind Co Ltd Method of producing tantalum nitride film resistors
JP2000331808A (en) * 1999-05-24 2000-11-30 Toshiba Tec Corp Thin-film resistor, forming method thereof and strain gauge using the same
CN101437663A (en) * 2004-11-09 2009-05-20 得克萨斯大学体系董事会 Fabrication and application of nanofiber ribbons and sheets and twisted and non-twisted nanofiber yarns
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