CN104062047B - High pressure of hydrogen sulfide environment resistance-strain type load transducer - Google Patents

High pressure of hydrogen sulfide environment resistance-strain type load transducer Download PDF

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CN104062047B
CN104062047B CN201410203168.2A CN201410203168A CN104062047B CN 104062047 B CN104062047 B CN 104062047B CN 201410203168 A CN201410203168 A CN 201410203168A CN 104062047 B CN104062047 B CN 104062047B
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sensitive grid
high pressure
hydrogen sulfide
hydrogen
load transducer
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CN104062047A (en
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周成双
张�林
占生根
陈兴阳
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The invention discloses a kind of high pressure of hydrogen sulfide environment resistance-strain type load transducer, comprise sensor upper casing, sensor lower casing and elastomer, elastomer respectively with sensor upper casing, sensor lower casing is threaded, elastomer middle part is evenly equipped with foil gage, foil gage and elastomer are bonding, foil gage comprises sensitive grid, substrate, cover layer and lead-out wire, sensitive grid is bonded between substrate and cover layer by adhesive, lead-out wire connects sensitive grid, the making material of sensitive grid is ferrous alloy, sensitive grid surface is provided with one deck hydrogen and penetrates barrier film, described ferrous alloy is consisting of of each element by mass percentage: chromium 15-25%, nickel 2-7%, molybdenum 2-6%, aluminium 1-6%, iron surplus. the present invention has overcome existing load transducer self corrosion and damage and hydrogen under high pressure of hydrogen sulfide environment and has invaded the deficiency that produces larger null offset and creep, has ensured the Stability and veracity of measurement result, has extended the service life of sensor.

Description

High pressure of hydrogen sulfide environment resistance-strain type load transducer
Technical field
The present invention relates to a kind of load transducer, particularly a kind of high pressure of hydrogen sulfide environment resistance-strain type load transducer.
Background technology
Along with the increase gradually to petroleum resources demand, the exploitation quantity increasing year by year in acid-soluble oil gas field. In whole development process, have to face the threat of hydrogen sulfide corrosion. Hydrogen sulfide not only can be used as acid medium and causes corrosion of metal or perforation, and the hydrogen that hydrogen sulfide produces can make with metal reaction time keeps state of atom, hydrogen atom invades the hydrogen damage that metal inside can cause the various ways such as equipment generation hydrogen induced cracking (HIC), stress corrosion cracking, this greatly reduces the military service performance of material, and serious threat is to the safety in production in acid-soluble oil gas field.
Therefore under hydrogen-sulfide environmental, the stress-strain measurement of material is just essential. Wherein, strain gage testing is to use measuring method the most widely. But under hydrogen-sulfide environmental, common resistance-strain sector-meeting is due to hydrogen sulfide corrosion fracture or change because the intrusion of hydrogen causes resistivity, thereby causes foil gauge to lose efficacy or produce very large null offset. Therefore the adaptability that has influence on foil gauge, Stability and veracity that, hydrogen sulfide can be serious. This just causes common foil gauge to be not suitable for the stress-strain measurement under high pressure of hydrogen sulfide environment, need to develop special foil gauge under a kind of high pressure of hydrogen sulfide environment.
At present, the research of China aspect sensor is also in the relatively backward stage, especially high-precision pressure sensor. The high accuracy needing in Aero-Space, field of petrochemical industry, the pressure sensor of high stability rely on import for a long time. This badly influences need of production, the obstruction independent technological innovation of China.
But, China due to the exploitation of high-hydrogen sulfide oil gas field (with general phosgene Tian Wei representative) in the technology aspect high pressure of hydrogen sulfide oil-gas field development in world's higher level. And possesses perfect high-hydrogen sulfide production of hydrocarbons development ability. But, aspect the safety guarantee of China in high pressure of hydrogen sulfide environment, still need further reinforcement: lack material/complete machine durability testing equipment and technology in high pressure of hydrogen sulfide environment, do not there is the ability of the material in high pressure of hydrogen sulfide environment being carried out to direct safety detection. Therefore,, in order to ensure the service life of material in high pressure of hydrogen sulfide environment and operation safely and reliably, must strengthen the technical research aspect high pressure of hydrogen sulfide system security assurance. Wherein, under high pressure of hydrogen sulfide environment, stress-strain measurement is the key technology that realizes safety detection.
Summary of the invention
The object of the present invention is to provide a kind of load transducer of measuring material stress strain under high pressure of hydrogen sulfide environment that is specifically designed to, invade to overcome existing load transducer self corrosion and damage and hydrogen hydrogen under high pressure of hydrogen sulfide environment the deficiency that produces larger null offset and creep, ensure the Stability and veracity of measurement result, extended the service life of sensor.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of high pressure of hydrogen sulfide environment resistance-strain type load transducer, comprise sensor upper casing, sensor lower casing and elastomer, elastomer respectively with sensor upper casing, sensor lower casing is threaded, elastomer middle part is evenly equipped with foil gage, foil gage and elastomer are bonding, foil gage comprises sensitive grid, substrate, cover layer and lead-out wire, sensitive grid is bonded between substrate and cover layer by adhesive, lead-out wire connects sensitive grid, the making material of sensitive grid is ferrous alloy, sensitive grid surface is provided with one deck hydrogen and penetrates barrier film, described ferrous alloy is consisting of of each element by mass percentage: chromium 15-25%, nickel 2-7%, molybdenum 2-6%, aluminium 1-6%, iron surplus.
As preferably, the thickness of described sensitive grid is 5 μ m-20 μ m.
As preferably, described hydrogen penetrates barrier film and is made up of iron transition zone and alumin(i)um zinc alloy layer, hydrogen penetrates barrier film and adds that first to adopt magnetron sputtering technique man-hour be that 10-100nm metallic iron forms iron transition zone in sensitive grid surface deposition a layer thickness, and then depositing a layer thickness is the alumin(i)um zinc alloy formation alumin(i)um zinc alloy layer of 10-100nm again.
As preferably, described alumin(i)um zinc alloy is consisting of of each element by mass percentage: zinc 5%-30%, aluminium surplus.
As preferably, magnetron sputtering technique machined parameters is: be evacuated to 6.7 × 10-3Pa, is heated to 300 DEG C, and under 400V high pressure, after Ar Ion Cleaning, under 60V voltage, first deposition forms iron transition zone, and then deposition forms aluminium thin layer. Adopt such parameter, processing effect is good.
As preferably, described barrier film surface is gone back using plasma oxidation technology and is processed with the protective layer of alumina that a layer thickness is 1nm-10nm.
As preferably, plasma oxidation technology machined parameters is: the RF source frequencies of use is 10-15MHz, and radio frequency source power is 2W/cm2, source of the gas is the mist that the volume ratio according to 5-10:1 of argon gas and oxygen mixes, and gas flow is 49sccm, and reative cell air pressure is 1 × 104-8×104Pa, the control of sensitive grid temperature is 250 DEG C, oxidization time is 0.5-2.5h. Adopt such parameter, processing effect is good.
As preferably, sensor upper casing, sensor lower casing and elastomeric material all adopt C-276 Hastelloy. Because corrosion phenomenon under high pressure of hydrogen sulfide environment is serious, therefore, sensor upper casing, sensor lower casing and elastomeric material all adopt C-276 Hastelloy, significantly hydrogen sulfide corrosion-resistant.
Foil gage is the core component that the load transducer under high pressure of hydrogen sulfide environment is measured, and the core component that foil gauge is measured is sensitive grid, therefore, emphasis of the present invention has improved the material of sensitive grid, adopt the ferrous alloy of specific proportioning, because ferrous alloy is body-centered cubic structure, there is the saturated solid solubility of extremely low hydrogen, therefore sensitive grid internal hydrogen content is very low. So the load transducer preparing with this material has null offset, the little feature of creep under high pressure of hydrogen sulfide environment. In addition, the fill a prescription corrosivity of resistance to hydrogen sulfide of ferrous alloy of the present invention is good, especially adding of molybdenum element, has greatly improved the corrosivity of resistance to hydrogen sulfide.
Because content major part in sensitive grid material is iron, depositing of iron transition zone is beneficial to the adhesion that improves aluminium thin layer and matrix; The alumin(i)um zinc alloy of the specific proportioning of the present invention has extremely low hydrogen diffusion coefficient, can effectively stop the intrusion of hydrogen, and the corrosivity of the resistance to hydrogen sulfide of alumin(i)um zinc alloy is good simultaneously. Hydrogen with interstitial atom form diffusion, have very high penetrating power, and hydrogen mainly exists with molecular state in oxide in metal, and oxide can suppress hydrogen molecule and be dissociated into hydrogen atom, thereby stops hydrogen to spread to metallic matrix. Therefore preferred, the present invention utilizes plasma oxidation technology to prepare the ultra-thin compact aluminum oxide layer (1nm ~ 10nm) of one deck on barrier film surface, thereby has hindered again the intrusion of hydrogen, and the corrosivity of resistance to hydrogen sulfide is good simultaneously. Like this, extremely low at the hydrogen content that can invade sensitive grid after alumina layer and barrier film, simultaneously the corrosivity of resistance to hydrogen sulfide is good, and sensitive grid material itself also has the saturated solid solubility of lower hydrogen and hydrogen sulfide corrosion-resistant well. Finally, invade hydrogen content in sensitive grid material very low in environment, the corrosivity of resistance to hydrogen sulfide is good simultaneously, thereby invades by hydrogen the null offset and the creep that produce and will be suppressed, and the long service life of sensor.
Under high pressure of hydrogen sulfide environment, this novel sensitive grid of the present invention can effectively overcome under high pressure of hydrogen sulfide environment that self corrosion and damage and hydrogen are invaded and the null offset that causes and the problem of creep with respect to traditional sensitive grid, thereby ensure the Stability and veracity of the last measurement result of sensor, extended sensor service life.
The invention has the beneficial effects as follows: under high pressure of hydrogen sulfide environment, self corrosion and damage and hydrogen are invaded and the null offset that causes and the problem of creep, thereby ensured the Stability and veracity of the last measurement result of sensor, extended sensor service life.
Brief description of the drawings
Fig. 1 is the main TV structure schematic diagram of one of the present invention.
Fig. 2 is that the A-A of Fig. 1 is to diagram.
Fig. 3 is a kind of structural representation of foil gage of the present invention.
In figure: 1, sensor upper casing, 2, sensor lower casing, 3, elastomer, 4, foil gage, 41, sensitive grid, 42, substrate, 43, cover layer, 44, lead-out wire, 5, cable.
Detailed description of the invention
Below by specific embodiment, and by reference to the accompanying drawings, technical scheme of the present invention is described in further detail.
In the present invention, if not refer in particular to, raw material and the equipment etc. adopting all can be buied from market or this area is conventional. Method in following embodiment, if no special instructions, is the conventional method of this area.
Embodiment 1:
Load transducer under a kind of high pressure of hydrogen sulfide environment is (as Fig. 1, shown in 2), comprise sensor upper casing 1, sensor lower casing 2 and elastomer 3, sensor upper casing 1, the making material of sensor lower casing 2 and elastomer 3 all adopts C-276 Hastelloy (commercially available), elastomer 3 respectively with sensor upper casing 1, sensor lower casing 2 is threaded, elastomer 3 middle parts are evenly equipped with foil gage 4, there is a slice foil gage 4 each the centre of four faces at elastomer 3 middle parts, before elastomer 3 middle parts, foil gage 4 lateral arrangement (with reference to accompanying drawing 3) on rear surface, elastomer 3 left sides, middle part, foil gage 4 at right surface is longitudinally arranged, foil gage 4 is bonding with elastomer 3, foil gage 4 comprises sensitive grid 41, substrate 42(can adopt conventional glass fabric), cover layer 43(can adopt conventional polytetrafluoroethylene film) and lead-out wire 44(is as shown in Figure 3), thereby lead-out wire 44 is connected on cable 5 data is exported, the thickness of sensitive grid 41 is 3 μ m, sensitive grid 41 is bonded between substrate 42 and cover layer 43 by adhesive, lead-out wire 44 connects sensitive grid 41 two ends, the making material of sensitive grid is ferrous alloy, ferrous alloy is consisting of of each element by mass percentage: chromium 15%, nickel 7%, molybdenum 6%, aluminium 6%, iron 66%.
When sensitive grid is made, first ferrous alloy is pressed into the paillon foil that thickness is 5 μ m, then the figure that adopts conventional optical etching technology to produce design in foil surfaces obtains sensitive grid, then penetrate barrier film at sensitive grid Surface Machining one deck hydrogen, hydrogen penetrates barrier film and is made up of iron transition zone and alumin(i)um zinc alloy layer, hydrogen penetrates barrier film and adds that first to adopt magnetron sputtering technique man-hour be that 10nm metallic iron forms iron transition zone in sensitive grid surface deposition a layer thickness, and then depositing a layer thickness is the alumin(i)um zinc alloy formation alumin(i)um zinc alloy layer of 10nm again. Alumin(i)um zinc alloy is consisting of of each element by mass percentage: zinc 30%, aluminium 70%.
Magnetron sputtering technique machined parameters is: be evacuated to 6.7 × 10-3Pa, is heated to 300 DEG C, and under 400V high pressure, after Ar Ion Cleaning, under 60V voltage, first deposition forms iron transition zone, and then deposition forms aluminium thin layer.
Barrier film surface is gone back using plasma oxidation technology and is processed with the protective layer of alumina that a layer thickness is 1nm. Plasma oxidation technology machined parameters is: the RF source frequencies of use is 10MHz, and radio frequency source power is 2W/cm2, source of the gas is the mist that the volume ratio according to 5:1 of argon gas and oxygen mixes, and gas flow is 49sccm, and reative cell air pressure is 1 × 104Pa, the control of sensitive grid temperature is 250 DEG C, oxidization time is 0.5h.
Embodiment 2:
The difference of the present embodiment and embodiment 1 is: the thickness of sensitive grid is 20 μ m, and ferrous alloy is consisting of of each element by mass percentage: ferrous alloy is consisting of of each element by mass percentage: chromium 25%, nickel 2%, molybdenum 2%, aluminium 1%, iron 70%; Iron transition region thickness is 100nm, and alumin(i)um zinc alloy layer thickness is 100nm. Alumin(i)um zinc alloy is consisting of of each element by mass percentage: zinc 5%, aluminium 95%.
Protective layer of alumina thickness is 10nm, and plasma oxidation technology machined parameters is: the RF source frequencies of use is 15MHz, and radio frequency source power is 2W/cm2, source of the gas is the mist that the volume ratio according to 10:1 of argon gas and oxygen mixes, and gas flow is 49sccm, and reative cell air pressure is 8 × 104Pa, the control of sensitive grid temperature is 250 DEG C, oxidization time is 2.5h.
The other the same as in Example 1.
Embodiment 3:
The difference of the present embodiment and embodiment 1 is: the thickness of sensitive grid is 15 μ m, and ferrous alloy is consisting of of each element by mass percentage: chromium 10%, nickel 5%, molybdenum 4%, aluminium 4%, iron 77%; Iron transition region thickness is 100nm, and alumin(i)um zinc alloy layer thickness is 100nm. Alumin(i)um zinc alloy is consisting of of each element by mass percentage: zinc 20%, aluminium 80%.
Protective layer of alumina thickness is 5nm, and plasma oxidation technology machined parameters is: the RF source frequencies of use is 12MHz, and radio frequency source power is 2W/cm2, source of the gas is the mist that the volume ratio according to 7:1 of argon gas and oxygen mixes, and gas flow is 49sccm, and reative cell air pressure is 5 × 104Pa, the control of sensitive grid temperature is 250 DEG C, oxidization time is 1.5h.
The other the same as in Example 1.
Load transducer of the present invention is placed the null offset≤100 μ m/m of 20h under 120Mpa high pressure of hydrogen sulfide environment, and creep≤100 μ m/m, has ensured the Stability and veracity of measurement result, and extended service life.
Above-described embodiment is preferably scheme of one of the present invention, not the present invention is done to any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim records.

Claims (7)

1. a high pressure of hydrogen sulfide environment resistance-strain type load transducer, comprise sensor upper casing, sensor lower casing and elastomer, elastomer respectively with sensor upper casing, sensor lower casing is threaded, it is characterized in that: elastomer middle part is evenly equipped with foil gage, foil gage and elastomer are bonding, foil gage comprises sensitive grid, substrate, cover layer and lead-out wire, sensitive grid is bonded between substrate and cover layer by adhesive, lead-out wire connects sensitive grid, the making material of sensitive grid is ferrous alloy, sensitive grid surface is provided with one deck hydrogen and penetrates barrier film, described ferrous alloy is consisting of of each element by mass percentage: chromium 15-25%, nickel 2-7%, molybdenum 2-6%, aluminium 1-6%, iron surplus, described hydrogen penetrates barrier film and is made up of iron transition zone and alumin(i)um zinc alloy layer, hydrogen penetrates barrier film and adds that first to adopt magnetron sputtering technique man-hour be that 10-100nm metallic iron forms iron transition zone in sensitive grid surface deposition a layer thickness, and then depositing a layer thickness is the alumin(i)um zinc alloy formation alumin(i)um zinc alloy layer of 10-100nm again.
2. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 1, is characterized in that: the thickness of described sensitive grid is 5 μ m-20 μ m.
3. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 1, is characterized in that: described alumin(i)um zinc alloy is consisting of of each element by mass percentage: zinc 5%-30%, aluminium surplus.
4. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 1, is characterized in that: magnetron sputtering technique machined parameters is: be evacuated to 6.7 × 10-3Pa, is heated to 300 DEG C, and under 400V high pressure, after Ar Ion Cleaning, under 60V voltage, first deposition forms iron transition zone, and then deposition forms alumin(i)um zinc alloy layer.
5. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 1 and 2, is characterized in that: described barrier film surface is gone back using plasma oxidation technology and is processed with the protective layer of alumina that a layer thickness is 1nm-10nm.
6. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 5, is characterized in that: plasma oxidation technology machined parameters is: the RF source frequencies of use is 10-15MHz, radio frequency source power is 2W/cm2, source of the gas is the mist that the volume ratio according to 5:1 ~ 10:1 of argon gas and oxygen mixes, and gas flow is 49sccm, and reative cell air pressure is 1 × 104-8×104Pa, the control of sensitive grid temperature is 250 DEG C, oxidization time is 0.5-2.5h.
7. high pressure of hydrogen sulfide environment resistance-strain type load transducer according to claim 1 and 2, is characterized in that: sensor upper casing, sensor lower casing and elastomeric material all adopt C-276 Hastelloy.
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CN104880206B (en) * 2015-06-09 2018-03-06 中国科学院深圳先进技术研究院 Resistance strain gage and resistance strain type sensor
CN105067166A (en) * 2015-07-28 2015-11-18 北京工业大学 Sleeve type force transducer for support structures
US20220307968A1 (en) * 2021-03-23 2022-09-29 Saudi Arabian Oil Company Laboratory apparatus for hydrogen permeation electrochemicalmeasurements under high pressure, temperature and tensile stress

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CN1094454A (en) * 1993-04-26 1994-11-02 重庆特殊钢厂 A kind of iron-base anti-corrosion alloy
CN1360081A (en) * 2001-07-17 2002-07-24 束润涛 Low-alloy rare-earth steel resisting corrosion of hydrogen sulfide
CN1584528A (en) * 2004-05-24 2005-02-23 西北工业大学 Apparatus for measuring composite stress
CN1672022A (en) * 2002-07-25 2005-09-21 梅特勒-托莱多有限公司 Moisture protection for an electromechanical transducer
CN102023179A (en) * 2010-11-04 2011-04-20 中南大学 Foil type sensor with function of automatically accumulating resistance

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Publication number Priority date Publication date Assignee Title
CN1094454A (en) * 1993-04-26 1994-11-02 重庆特殊钢厂 A kind of iron-base anti-corrosion alloy
CN1360081A (en) * 2001-07-17 2002-07-24 束润涛 Low-alloy rare-earth steel resisting corrosion of hydrogen sulfide
CN1672022A (en) * 2002-07-25 2005-09-21 梅特勒-托莱多有限公司 Moisture protection for an electromechanical transducer
CN1584528A (en) * 2004-05-24 2005-02-23 西北工业大学 Apparatus for measuring composite stress
CN102023179A (en) * 2010-11-04 2011-04-20 中南大学 Foil type sensor with function of automatically accumulating resistance

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