CN115852280B - Heat treatment method of coriolis force mass flowmeter for high-pressure hydrogen - Google Patents
Heat treatment method of coriolis force mass flowmeter for high-pressure hydrogen Download PDFInfo
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 104
- 239000001257 hydrogen Substances 0.000 title claims abstract description 81
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 81
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 87
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- 238000002955 isolation Methods 0.000 claims abstract description 10
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- 239000007789 gas Substances 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 86
- 229910052759 nickel Inorganic materials 0.000 claims description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- 239000010963 304 stainless steel Substances 0.000 claims description 3
- 229910000589 SAE 304 stainless steel Inorganic materials 0.000 claims description 3
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Abstract
The invention provides a heat treatment method of a coriolis force mass flowmeter for high-pressure hydrogen, which comprises the following steps: a) HC-22 is selected as a liquid receiving material of the Coriolis mass flowmeter; b) Assembling a heat treatment assembly of the coriolis force mass flowmeter; c) Respectively laying brazing solder BNi-5 on the vibration isolation sheet, the measuring tube and the shunt; d) Installing a wind scooper; e) Sending into a vacuum gas quenching furnace, vacuumizing, and executing a heat treatment process. According to the invention, a more proper material is selected, and a brand-new heat treatment overall process is adopted, so that the hydrogen removal thoroughness of the liquid receiving part is improved, the material uniformity of the liquid receiving part is improved, the material defects of the liquid receiving part are reduced, the stress concentration of the liquid receiving part is reduced, the hydrogen embrittlement sensitivity of the liquid receiving part is reduced, and the risk of hydrogen embrittlement of the liquid receiving part is reduced; the brazing is ensured to be firm, uniform and full, and the strength and consistency of the welded joint are improved; the stress of the liquid receiving part is thoroughly removed, and the accuracy and repeatability of the Coriolis mass flowmeter are improved.
Description
Technical Field
The invention relates to the technical field of heat treatment, in particular to a heat treatment method of a coriolis force mass flowmeter for high-pressure hydrogen.
Background
The prior Coriolis mass flowmeter adopts 316L stainless steel, the nickel content of the 316L stainless steel is 10-14%, the lower limit is 10% generally, the nickel equivalent is 25.188-31.468%, and when the national standard GB 50506-2010 requires austenitic stainless steel to be used for a hydrogen pipeline, the nickel content is more than 12%, and the nickel equivalent is more than 28.5%. In critical conditions, which are the requirements for hydrogen pipelines, the measuring tube for mass flow meters generally has a small wall thickness, and therefore, a material having a higher nickel content and nickel equivalent is required.
When the small-specification coriolis force mass flowmeter is used for carrying out braze welding heat treatment, the conditions of incomplete brazing parts, uneven brazing parts and insufficient strength often occur, and analysis is because the current coriolis force mass flowmeter assembly is directly placed into a vacuum gas quenching furnace for braze welding heat treatment after brazing filler metal is laid when the assembly is subjected to braze welding heat treatment, but after the highest temperature heat preservation is finished, a large amount of low-temperature nitrogen gas is required to be flushed for cooling, under the working condition, the brazing filler metal still becomes liquid phase, the high-pressure hydrogen flowmeter is usually small in specification, brazed parts are very small, the brazing filler metal is very little laid, the brazing filler metal still in the liquid phase can be blown away by instantaneous high-pressure air flow, so that the brazing is unstable and uneven, and the welding seam at the brazing part is not full. Meanwhile, when the current Coriolis mass flowmeter assembly is brazed, BNi-1 (BNi 74 CrSiB) brazing material is selected, and the brazing material contains too high iron and carbon components, and is low in chromium content and not suitable for being applied to nickel-based single-phase austenitic alloy of a high-pressure hydrogen flowmeter.
More importantly, the current coriolis force mass flowmeter for high-pressure hydrogen needs to be subjected to dehydrogenation heat treatment, brazing heat treatment, stress relief heat treatment and solution heat treatment, and the existing brazing and heat treatment process scheme is poor in process effect, and firstly hydrogen absorbed in the liquid receiving component cannot be thoroughly removed; secondly, the residual stress of the equipment is larger, so that the accuracy and repeatability of the coriolis force mass flowmeter for high-pressure hydrogen are poor, and the liquid metering accuracy can only reach 0.15%; thirdly, the problems of uneven materials, defects, stress concentration and martensitic transformation can not be effectively solved, the sensitivity of hydrogen embrittlement is high, and the phenomenon of hydrogen embrittlement is easy to occur under the working condition of high-pressure hydrogen-containing for a long time.
Disclosure of Invention
In view of this, in order to prevent the liquid-receiving material of the coriolis force mass flowmeter from generating hydrogen embrittlement in the high-pressure hydrogen environment, lead to the damage of liquid-receiving metal, hydrogen reveal, the coriolis force mass flowmeter of high-pressure hydrogen chooses the single-phase austenitic alloy with high nickel content and nickel equivalent to be regarded as the liquid-receiving material, on this basis, the invention chooses the more suitable material, and adopt the brand-new whole process of heat treatment, raise the thorough of dehydrogenation of the liquid-receiving component, raise the homogeneity of material of the liquid-receiving component, reduce the material defect of the liquid-receiving component, reduce the stress concentration of the liquid-receiving component, reduce the hydrogen embrittlement sensibility of the liquid-receiving component, reduce the danger that the liquid-receiving component generates hydrogen embrittlement; the brazing is ensured to be firm, uniform and full, and the strength and consistency of the welded joint are improved; the stress of the liquid receiving part is thoroughly removed, and the accuracy and repeatability of the Coriolis mass flowmeter are improved.
Hydrogen embrittlement: the hydrogen embrittlement of the metal material refers to the phenomenon that when the local hydrogen concentration reaches saturation after hydrogen enters the metal, metal plasticity is reduced, cracks are induced or delayed fracture is generated, the hydrogen embrittlement can be divided into internal hydrogen embrittlement and environmental hydrogen embrittlement, and the former refers to the phenomenon that the metal material absorbs excessive hydrogen in smelting and processing processes (such as acid washing, electroplating, cold processing and the like); the latter means that the metal is in a hydrogen-containing environment such as hydrogen, and hydrogen enters the metal to cause performance loss. The present invention mainly refers to the former for dehydrogenation. The hydrogen embrittlement prevention can reduce the material non-uniformity, defects, stress and martensitic transformation generated in the original material neutralization cold processing (such as bent pipe and the like) process by removing hydrogen and heat treatment, and reduce the sensitivity of hydrogen embrittlement.
The invention provides a heat treatment method of a coriolis force mass flowmeter for high-pressure hydrogen, which comprises the following steps:
a) HC-22 is selected as a liquid receiving material of the Coriolis mass flowmeter; b) Assembling a heat treatment assembly of the coriolis force mass flowmeter; c) Respectively laying brazing solder BNi-5 on the vibration isolation sheet, the measuring tube and the shunt; d) Installing a wind scooper; e) Sending into a vacuum gas quenching furnace, vacuumizing, and performing a heat treatment process:
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
h: heating to 1170 ℃ for 50min;
i: the time is 40min, and the temperature is kept at 1170 ℃;
j: filling low-temperature liquid nitrogen, and rapidly cooling to room temperature for 50min; and (5) finishing the heat treatment of the coriolis force mass flowmeter.
In the present invention, the nickel content of the HC-22 in the step A) is preferably 50% or more, and the nickel equivalent is preferably 77% or more. The HC-22 is adopted as the liquid receiving material, so that the technical problems existing in the prior art that 316L meeting the upper limit of the national standard or 904L stainless steel is selected can be solved, and specifically: the disadvantage of the 316L is that even if the 316L is made of materials according to the upper limits of national standards Ni, cr and Mo, the nickel content is 14%, the nickel equivalent is 31.5%, and the nickel equivalent is only a little higher than 12% and 28.5% of the national standards, but the nickel equivalent is the standard of the national standards for pipelines for hydrogen, and generally, the measuring tube used by the Coriolis mass flowmeter is a thin-walled tube for ensuring the Coriolis effect, so the requirements are more strict than the national standards, so the 316L is not suitable for serving as the liquid receiving material of the mass flowmeter for high-pressure hydrogen; while 904L (nickel content 23% -28%, nickel equivalent 50.5%) is superior to 316L in terms of material composition, but has two problems, namely, firstly, the nickel content and nickel equivalent are lower than HC-22 (nickel content is more than 50%, nickel equivalent is more than 77%), secondly, the yield strength and allowable stress of 904L are respectively 216MPa and 115MPa, and the yield strength and allowable stress of HC-22 are respectively 310MPa and 206MPa, and especially the allowable stress is almost twice as high as 904L, which means that the same pressure is required, the wall thickness of 904L measuring tube is twice as high as that of near HC-22, but the increase of the wall thickness greatly reduces the Coriolis force effect of the Coriolis force mass flowmeter, and the precision of equipment is reduced; 904L is also unsuitable.
In the present invention, the assembled assembly in step B) preferably comprises:
the device comprises a supporting plate, a shunt, a measuring tube, vibration isolation sheets, brazing solder and a coil magnet bracket; the measuring tube is respectively contacted with the shunt and the vibration isolation sheet.
In the present invention, the BNi-5 in the step C) does not contain Fe, and the C content is preferably not more than 0.06, and the Cr content is preferably 18.5% to 19.5%. The invention adopts BNi-5 as brazing filler metal, can solve the technical problems existing in the prior art that BNi-2 is selected as brazing material, and specifically: BNi-2 is selected, and the components are as follows:
| Ni | Cr | B | Si | Fe | C | S | P | |
| BNi-2 | rest (about 82%) | 6～8 | 2.75～3.5 | 4.0～5.0 | 2.5～3.5 | ≤0.06 | ≤0.02 | ≤0.02 |
Compared with BNi-1, the alloy has greatly reduced Fe and C contents and increased Ni content, is more suitable for welding stainless steel, but has lower Cr content, and simultaneously has lower brazing temperature (1010-1177 ℃) and is not suitable for single-phase austenitic alloy with high nickel content and nickel equivalent.
In the present invention, the application of the brazing compound in step C) preferably requires the formation of an application width of 1mm to 1.5mm, requiring the application of a full weld 360.
In the present invention, in the step D), the material of the air guiding cover is preferably 304 stainless steel.
In the present invention, the process of installing the wind scooper in step D) is preferably specifically:
and each set of heat treatment assembly of the coriolis force mass flowmeter is provided with a wind scooper, and then the wind scooper is fixed on a fixed bottom plate, and a plurality of sets of heat treatment assemblies can be simultaneously arranged on the fixed bottom plate.
In the present invention, the air guiding hole arrangement principle of the air guiding cover in the step D) is preferably as follows:
(1) The arrangement of the air guide openings is required to be symmetrical at two sides according to the central line; (2) The total area of the air guide opening needs to account for 25% -35% of the area of the plane where the air guide opening is positioned; (3) The arrangement of the air guide opening must avoid the position where the brazing material is laid by at least 15mm; (4) a wind guide port is required to be arranged at the bent pipe of the measuring pipe; (5) the center must be provided with a wind guide port; (6) the bottom edge must be provided with a wind guide.
In the prior art, the components are cooled along with a furnace or are integrally wrapped, or a large amount of brazing material is smeared, so that the rest components can meet the strength requirement of the welded joint; in order to prevent wind formed by low-temperature nitrogen from blowing away the brazing filler metal still in a liquid phase, some manufacturers choose to cool the brazing filler metal to 850 ℃ along with the furnace; or directly furnace cooled to a lower temperature, such as 400 ℃; both methods increase the heat treatment time length, resulting in increased cost and reduced efficiency, especially by direct furnace cooling to lower temperatures; the sensitization temperature of the second stainless steel is 450-850 ℃, and the second stainless steel is in the temperature range for a long time, so that the stainless steel is subjected to intergranular corrosion, and the method is unsuitable; thirdly, the whole assembly is wrapped, so that air in the assembly cannot be completely separated out, oxidation occurs in the heat treatment process, meanwhile, as the whole assembly is wrapped, the temperature rise and heat dissipation of the whole assembly are greatly influenced, the heat treatment cannot be performed according to a designed temperature gradient, the temperature of the assembly is uneven, and the effects of solid solution and stress relief are influenced; insufficient melting of the brazing material affects the brazing effect, causes unstable and uneven brazing, is not full, and leaves welding slag; the temperature is slowly reduced, so that the temperature is in a sensitization temperature section for a long time, and the intergranular corrosion is caused. The adoption of the wind scooper ensures firm and full brazing.
In the present invention, the degree of vacuum of the evacuated in step E) is preferably 1X 10 -2 Pa～3×10 -2 Pa, more preferably 2X 10 -2 Pa。
In the present invention, the vacuum is preferably maintained at 1X 10 throughout the heat treatment process in step E) -2 Pa～3×10 - 2 Pa, more preferably at 2X 10 -2 Pa。
Aiming at the heat treatment process, various heat treatment processes are formulated by various manufacturers, but the current heat treatment process is not ideal from the effect, and cannot meet the high-precision coriolis force mass flowmeter for the high-pressure hydrogen working condition; the current heat treatment process of coriolis force flowmeters generally has the following problems: the temperature gradient is unreasonably set, and the heat preservation time is not set at the temperature point, so that the flowmeter assembly cannot be heated uniformly; the temperature value and the heat preservation time of the highest temperature are unreasonable, so that the stress in the component cannot be effectively removed, the accuracy and the repeatability of the flowmeter are lower, and meanwhile, the nonuniformity, defects, stress concentration and martensitic transformation in the material cannot be effectively eliminated, so that hydrogen can enter a weak zone in the material more easily in the later use of high-pressure hydrogen, and the hydrogen embrittlement sensitivity of the material is increased; the last cooling section is unreasonable to set up, can make stainless steel be in sensitization temperature interval for a long time along with the stove cooling, leads to the stainless steel to appear intergranular corrosion to make the hydrogen embrittlement sensitivity of material increase, reduce equipment life, increase the damage of receiving liquid part, the risk of hydrogen leakage. The invention adopts an advanced heat treatment process, which comprises the following steps:
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
h: heating to 1170 ℃ for 50min;
i: the time is 40min, and the temperature is kept at 1170 ℃;
j: and (5) filling low-temperature liquid nitrogen, rapidly cooling to room temperature, and taking 50min.
Including a temperature section for dehydrogenation; a heat preservation section for homogenizing the temperature of the assembly; setting a temperature section avoiding a sensitization temperature zone; the high-temperature section setting is favorable for stress relief, brazing and solid solution effects, reducing the material unevenness, defects and stress concentration of the liquid receiving component, reducing the hydrogen embrittlement sensitivity of the liquid receiving component and reducing the danger of hydrogen embrittlement of the liquid receiving component; is favorable for avoiding sensitization temperature, improving solid solution effect and avoiding design of a cooling section for taking in hydrogen during cooling.
The invention provides a heat treatment method of a coriolis force mass flowmeter for high-pressure hydrogen, which comprises the following basic scheme: HC-22 is selected as a liquid receiving material of the flowmeter; BNi-5 is selected as nickel-based brazing filler metal for brazing; the bare pipe enters the vacuum gas quenching furnace and is provided with a solder protection cover; setting more reasonable heat treatment temperature gradient, heat preservation time and vacuum degree.
Has the following beneficial effects:
(1) HC-22 is selected as a raw material, the nickel content and the nickel equivalent of the HC-22 far exceed the national standard, and meanwhile, the HC-22 is also nickel-based single-phase austenitic alloy; the hydrogen embrittlement sensitivity of the material is reduced along with the increase of the nickel content and the nickel equivalent, the nickel content of more than 50% and the nickel equivalent of more than 77% of the HC-22 material are reduced along with the increase of the austenite proportion in the material, and the single-phase austenite composition ensures that the hydrogen embrittlement sensitivity of the material is extremely low and the hydrogen embrittlement resistance of the material is ensured; meanwhile, the yield strength of HC-22 is 310MPa, the allowable stress is 206MPa, and the allowable stress is far more than 172MPa and 115MPa of 316L, so that the wall thickness of the pipe can be reduced to the maximum extent while the bearing capacity is ensured, the Coriolis force effect is improved, and the precision and repeatability of equipment are improved.
(2) The design of the wind scooper ensures that the heat treatment can select low-temperature liquid nitrogen for rapid cooling, thereby avoiding weak brazing and uneven welding seams caused by blowing away liquid-phase brazing materials by the strong wind of the low-temperature liquid nitrogen and reducing the durability and the performance of equipment; the long-time sensitization temperature section and low production efficiency caused by furnace cooling are avoided; the uneven heating and slow heat dissipation caused by full wrapping are avoided; the novel use of the wind scooper in the heat treatment process can ensure the firmness and uniformity of brazing to the greatest extent and improve the destressing and solid solution effects of the assembly to the greatest extent.
(3) BNi-5 brazing material is selected, so that the brazing material can adapt to the heat treatment temperature of 1170 ℃, meanwhile, BNi-5 does not contain Fe, the C content is extremely low, the Cr content is high, the brazing material is more suitable for HC-22 brazing, and martensite is also prevented from being formed in the brazing process, so that the hydrogen embrittlement sensitivity is increased.
(4) The innovative heat treatment process flow has the characteristic functions of temperature gradient setting and time setting:
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
heating to 260 ℃ and preserving heat for 1 hour, wherein the hydrogen is greatly enhanced in activity above 200 ℃ and can be separated out from the metal material, so that the setting can maximally reduce the hydrogen content of the material summary; reducing the hydrogen embrittlement sensitivity of the liquid receiving component; meanwhile, the arrangement can fully volatilize the binder in the brazing material;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
the arrangement of the heat preservation section avoids the sensitization temperature section (450-850 ℃), and meanwhile, the heat preservation section is additionally arranged at a proper place, so that the temperature uniformity of the component can be improved, and the solid solution effect of heat treatment is improved;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
the temperature raising section is arranged in the sensitization temperature interval without a heat preservation section, so that intergranular corrosion is avoided; the temperature is raised to the temperature point and is kept warm, so that the internal stress of the part can be fully eliminated;
h: heating to 1170 ℃ for 50min;
i: the time is 40min, and the temperature is kept at 1170 ℃;
the setting of the temperature point and the setting of the heat preservation period 1 can eliminate residual stress in materials to the greatest extent, improve the consistency of materials, improve the consistency of the materials, and effectively improve the zero point stability of the mass flowmeter, thereby improving the precision of equipment; 2. fully ensures the effect of solid solution, enables austenite and martensite in a metastable state to be completely transformed into supersaturated austenite, and eliminates uneven structure and microscopic defects in the material; the reduction of stress in the material, the reduction of austenite and martensite in a metastable state, the improvement of the structural uniformity and the reduction of defects can reduce the hydrogen embrittlement sensitivity of the material; therefore, the process can furthest reduce the hydrogen embrittlement sensitivity of the material; 3. the melting temperature of the brazing material is considered, so that the brazing material can be melted and infiltrated fully, and firm welding is realized;
j: filling low-temperature liquid nitrogen, and rapidly cooling to room temperature for about 50min;
the rapid cooling section ensures that the heat treatment assembly is not in a sensitization temperature range, avoids intergranular corrosion, ensures the performance of the material, simultaneously directly pulls to room temperature, avoids hydrogen from entering the material again in the process, and furthest ensures the dehydrogenation effect of the material.
Drawings
FIG. 1 is an assembly view of a coriolis force mass flowmeter heat treatment assembly in accordance with an embodiment of the invention;
FIGS. 2-3 are schematic diagrams of brazing material laid at vibration isolation sheets and measurement tubes and at measurement tubes and flow splitters in an embodiment of the invention;
FIG. 4 is a schematic view of an embodiment of the present invention in which a wind scooper is installed;
FIG. 5 is a schematic view of an air guide arranged in an embodiment of the present invention;
FIG. 6 is a graph showing temperature profile of a heat treatment process according to an embodiment of the present invention;
fig. 7 is a process flow chart of a heat treatment method of the coriolis force mass flowmeter for high-pressure hydrogen provided by the invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
(1) HC-22 was used as the material for the liquid-receiving material of the flowmeter, and the composition thereof is shown in Table 1 below.
Table 1HC-22 material composition table (mass percent)
Wherein the nickel content is more than 50 percent, and the nickel equivalent is more than 77 percent.
(2) The coriolis force mass flowmeter completes the heat treatment assembly, as shown in fig. 1; fig. 1 is an assembly diagram of a coriolis force mass flowmeter heat treatment assembly in accordance with an embodiment of the present invention, wherein the support plate is 1-support plate, the shunt is 2-support plate, the measuring tube is 3-support plate, the vibration isolation sheet is 4-support plate, the brazing material is 5, and the coil magnet is 6.
(3) Laying brazing solder BNi-5 at the positions of the vibration isolation sheet, the measuring tube and the shunt, wherein the composition of the brazing solder BNi-5 is shown in the following table 2; laying plump, forming A:1 mm-1.5 mm; b: a laying width of 1mm to 1.5mm requires laying a full weld 360 deg., see figures 2 to 3.
TABLE 2 composition of BNi-5 materials (mass percent)
| Ni | Cr | B | Si | C | S | P | |
| BNi-5 | Remainder (about 71%) | 18.5～19.5 | ≤0.03 | 9.75～10.5 | ≤0.06 | ≤0.02 | ≤0.02 |
(4) Installing a wind scooper, wherein the wind scooper is made of 304 stainless steel, each set of flowmeter heat treatment assembly is provided with the wind scooper, then the wind scooper is fixed on a fixed bottom plate, and a plurality of sets of heat treatment assemblies can be installed on the fixed bottom plate at the same time; referring to fig. 4, fig. 4 is a schematic view of a wind scooper according to an embodiment of the present invention, wherein the wind scooper includes a 1-wind scooper, a 2-fixing base, 3-fixing bolts, and a 4-heat treatment module.
The arrangement of the air guide openings follows the following principles: 1. the arrangement of the air guide openings is required to be symmetrical at two sides according to the central line; 2. the total area of the air guide opening needs to account for 25% -35% of the area of the plane where the air guide opening is positioned; 3. the arrangement of the air guide opening must avoid the position where the brazing material is laid by at least 15mm; 4. an air guide port is arranged at the bent pipe of the measuring pipe; 5. the center is provided with a wind guide port; 6. the bottom edge is provided with a wind guide port; a schematic diagram of the air guide hole is shown in fig. 5.
(5) After the air guide opening is arranged, the air guide opening is sent into a vacuum air quenching furnace for vacuumizing, and the vacuum degree is kept at 2.0 multiplied by 10 -2 Pa, performing a heat treatment process (see fig. 6):
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
h: heating to 1170 ℃ for 50min;
i: the temperature is kept at 1170 ℃ for 40 min.
j: and (5) filling low-temperature liquid nitrogen, rapidly cooling to room temperature, and taking 50min.
Ending the heat treatment process, and maintaining the vacuum degree at 2.0X10% in the whole process -2 Pa。
The process flow chart of the heat treatment method of the coriolis force mass flowmeter for high-pressure hydrogen provided by the invention is shown in fig. 7.
After the heat treatment process is finished, the performance of the flowmeter is greatly improved, the precision reaches 0.05 percent level, and the repeatability reaches 0.02 percent level. Optionally taking a set of samples subjected to the heat treatment process for 20: 1-range ratio, the flow rate range is (26.5-530) kg/h, the detection flow rate points and the detection times are set according to JJG1038-2008 'Coriolis mass flowmeter metering verification procedure', and verification is carried out at qmax, 0.5qmax, 0.2qmax, qmin and qmax respectively, and each flow rate point is verified for 6 times; the verification precision is 0.04%, and the repeatability is 0.02%; the advancement of the heat treatment process is embodied, and experimental data are shown in the following table 3.
Table 3 experimental data of experiments performed on the flowmeter after the heat treatment method provided by the present invention
In summary, the heat treatment method of the coriolis force mass flowmeter for high-pressure hydrogen provided by the invention has the following beneficial effects:
(1) HC-22 is selected as a raw material, the nickel content and the nickel equivalent of the HC-22 far exceed the national standard, and meanwhile, the HC-22 is also nickel-based single-phase austenitic alloy; the hydrogen embrittlement sensitivity of the material is reduced along with the increase of the nickel content and the nickel equivalent, the nickel content of more than 50% and the nickel equivalent of more than 77% of the HC-22 material are reduced along with the increase of the austenite proportion in the material, and the single-phase austenite composition ensures that the hydrogen embrittlement sensitivity of the material is extremely low and the hydrogen embrittlement resistance of the material is ensured; meanwhile, the yield strength of HC-22 is 310MPa, the allowable stress is 206MPa, and the allowable stress is far more than 172MPa and 115MPa of 316L, so that the wall thickness of the pipe can be reduced to the maximum extent while the bearing capacity is ensured, the Coriolis force effect is improved, and the precision and repeatability of equipment are improved.
(2) The design of the wind scooper ensures that the heat treatment can select low-temperature liquid nitrogen for rapid cooling, thereby avoiding weak brazing and uneven welding seams caused by blowing away liquid-phase brazing materials by the strong wind of the low-temperature liquid nitrogen and reducing the durability and the performance of equipment; the long-time sensitization temperature section and low production efficiency caused by furnace cooling are avoided; the uneven heating and slow heat dissipation caused by full wrapping are avoided; the novel use of the wind scooper in the heat treatment process can ensure the firmness and uniformity of brazing to the greatest extent and improve the destressing and solid solution effects of the assembly to the greatest extent.
(3) BNi-5 brazing material is selected, so that the brazing material can adapt to the heat treatment temperature of 1170 ℃, meanwhile, BNi-5 does not contain Fe, the C content is extremely low, the Cr content is high, the brazing material is more suitable for HC-22 brazing, and martensite is also prevented from being formed in the brazing process, so that the hydrogen embrittlement sensitivity is increased.
(4) The innovative heat treatment process flow has the characteristic functions of temperature gradient setting and time setting:
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
heating to 260 ℃ and preserving heat for 1 hour, wherein the hydrogen is greatly enhanced in activity above 200 ℃ and can be separated out from the metal material, so that the setting can maximally reduce the hydrogen content of the material summary; reducing the hydrogen embrittlement sensitivity of the liquid receiving component; meanwhile, the arrangement can fully volatilize the binder in the brazing material;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
the arrangement of the heat preservation section avoids the sensitization temperature section (450-850 ℃), and meanwhile, the heat preservation section is additionally arranged at a proper place, so that the temperature uniformity of the component can be improved, and the solid solution effect of heat treatment is improved;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
the temperature raising section is arranged in the sensitization temperature interval without a heat preservation section, so that intergranular corrosion is avoided; the temperature is raised to the temperature point and is kept warm, so that the internal stress of the part can be fully eliminated;
h: heating to 1170 ℃ for 50min;
i: the time is 40min, and the temperature is kept at 1170 ℃;
the setting of the temperature point and the setting of the heat preservation period 1 can eliminate residual stress in materials to the greatest extent, improve the consistency of materials, improve the consistency of the materials, and effectively improve the zero point stability of the mass flowmeter, thereby improving the precision of equipment; 2. fully ensures the effect of solid solution, enables austenite and martensite in a metastable state to be completely transformed into supersaturated austenite, and eliminates uneven structure and microscopic defects in the material; the reduction of stress in the material, the reduction of austenite and martensite in a metastable state, the improvement of the structural uniformity and the reduction of defects can reduce the hydrogen embrittlement sensitivity of the material; therefore, the process can furthest reduce the hydrogen embrittlement sensitivity of the material; 3. the melting temperature of the brazing material is considered, so that the brazing material can be melted and infiltrated fully, and firm welding is realized;
j: filling low-temperature liquid nitrogen, and rapidly cooling to room temperature for about 50min;
the rapid cooling section ensures that the heat treatment assembly is not in a sensitization temperature range, avoids intergranular corrosion, ensures the performance of the material, simultaneously directly pulls to room temperature, avoids hydrogen from entering the material again in the process, and furthest ensures the dehydrogenation effect of the material.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A heat treatment method of a Coriolis mass flowmeter for high-pressure hydrogen comprises the following steps:
a) HC-22 is selected as a liquid receiving material of the Coriolis mass flowmeter; b) Assembling a heat treatment assembly of the coriolis force mass flowmeter; c) Respectively laying brazing solder BNi-5 on the vibration isolation sheet, the measuring tube and the shunt; d) Installing a wind scooper; the process of installing the wind scooper specifically comprises the following steps:
the heat treatment components of each set of coriolis force mass flowmeter are provided with a wind scooper, then the wind scooper is fixed on a fixed bottom plate, and a plurality of sets of heat treatment components can be simultaneously arranged on the fixed bottom plate; the air guide opening arrangement principle of the air guide cover is as follows:
(1) The arrangement of the air guide openings is required to be symmetrical at two sides according to the central line; (2) The total area of the air guide opening needs to account for 25% -35% of the area of the plane where the air guide opening is positioned; (3) The arrangement of the air guide opening must avoid the position where the brazing material is laid by at least 15mm; (4) a wind guide port is required to be arranged at the bent pipe of the measuring pipe; (5) the center must be provided with a wind guide port; (6) the bottom edge is provided with a wind guide port;
e) Sending into a vacuum gas quenching furnace, vacuumizing, and performing a heat treatment process:
a: firstly, the time is 30min, and the temperature is raised to 260 ℃;
b: the time is 60min, and the temperature is kept at 260 ℃;
c: heating to 420 deg.C for 30 min;
d: the time is 20min, and the temperature is kept at 420 ℃;
e: heating to 600deg.C for 30 min;
f: heating to 1030 deg.C for 50min;
g: the time is 25min, and the temperature is kept at 1030 ℃;
h: heating to 1170 ℃ for 50min;
i: the time is 40min, and the temperature is kept at 1170 ℃;
j: filling low-temperature liquid nitrogen, and rapidly cooling to room temperature for 50min; and (5) finishing the heat treatment of the coriolis force mass flowmeter.
2. The heat treatment method of a coriolis force mass flowmeter for high-pressure hydrogen of claim 1 wherein said HC-22 in step a) has a nickel content of 50% or more and a nickel equivalent of 77% or more.
3. The method of heat treating a coriolis force mass flowmeter for high-pressure hydrogen of claim 1 wherein said assembled assembly of step B) comprises:
the device comprises a supporting plate, a shunt, a measuring tube, vibration isolation sheets, brazing solder and a coil magnet bracket; the measuring tube is respectively contacted with the shunt and the vibration isolation sheet.
4. The method for heat treatment of coriolis force mass flowmeter for high-pressure hydrogen of claim 1 wherein said BNi-5 in step C) contains no Fe, C content is 0.06 or less, and Cr content is 18.5% to 19.5%.
5. The method of heat treatment of coriolis force mass flowmeter for high-pressure hydrogen of claim 1 characterized in that said laying braze in step C) requires a laying width of 1mm to 1.5mm and a full weld bead of 360 ° to be laid.
6. The method for heat treatment of coriolis force mass flowmeter for high-pressure hydrogen of claim 1 wherein said material of said hood in step D) is 304 stainless steel.
7. The method for heat treatment of coriolis force mass flowmeter for high-pressure hydrogen of claim 1 wherein said vacuum degree of said vacuum pumping in step E) is 1 x 10 -2 Pa～3×10 -2 Pa。
8. Coriolis force for high pressure hydrogen of claim 1A heat treatment method of a flowmeter, characterized in that the whole heat treatment process in the step E) maintains the vacuum degree at 1X 10 -2 Pa～3×10 -2 Pa。
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2222466A1 (en) * | 1997-11-25 | 1999-05-25 | Jacques Montagnon | Nickel-chrome-iron-based alloy compound |
| JP2008144237A (en) * | 2006-12-12 | 2008-06-26 | Hitachi Ltd | gamma' PHASE STRENGTHENED FeNi BASED ALLOY |
| WO2016131702A1 (en) * | 2015-02-17 | 2016-08-25 | Höganäs Ab (Publ) | Nickel based alloy with high melting range suitable for brazing super austenitic steel |
| JP2018104793A (en) * | 2016-12-28 | 2018-07-05 | 新日鐵住金株式会社 | Ni steel for liquid hydrogen |
| TW201901809A (en) * | 2017-05-17 | 2019-01-01 | 日商斯庫林集團股份有限公司 | Heat treatment device and heat treatment method |
| CN113637929A (en) * | 2021-07-14 | 2021-11-12 | 北京科技大学 | Heat treatment process for improving room temperature strength of nickel-based high-temperature alloy |
| CN113681103A (en) * | 2021-07-16 | 2021-11-23 | 北京科技大学 | Multi-brazing and heat treatment process for maintaining strength of nickel-based high-temperature alloy |
| CN114107630A (en) * | 2021-11-19 | 2022-03-01 | 北京科技大学 | Heat treatment method for improving hydrogen embrittlement resistance of martensitic stainless steel, stainless steel and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6544362B2 (en) * | 2001-06-28 | 2003-04-08 | Haynes International, Inc. | Two step aging treatment for Ni-Cr-Mo alloys |
-
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Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2222466A1 (en) * | 1997-11-25 | 1999-05-25 | Jacques Montagnon | Nickel-chrome-iron-based alloy compound |
| JP2008144237A (en) * | 2006-12-12 | 2008-06-26 | Hitachi Ltd | gamma' PHASE STRENGTHENED FeNi BASED ALLOY |
| WO2016131702A1 (en) * | 2015-02-17 | 2016-08-25 | Höganäs Ab (Publ) | Nickel based alloy with high melting range suitable for brazing super austenitic steel |
| JP2018104793A (en) * | 2016-12-28 | 2018-07-05 | 新日鐵住金株式会社 | Ni steel for liquid hydrogen |
| TW201901809A (en) * | 2017-05-17 | 2019-01-01 | 日商斯庫林集團股份有限公司 | Heat treatment device and heat treatment method |
| CN113637929A (en) * | 2021-07-14 | 2021-11-12 | 北京科技大学 | Heat treatment process for improving room temperature strength of nickel-based high-temperature alloy |
| CN113681103A (en) * | 2021-07-16 | 2021-11-23 | 北京科技大学 | Multi-brazing and heat treatment process for maintaining strength of nickel-based high-temperature alloy |
| CN114107630A (en) * | 2021-11-19 | 2022-03-01 | 北京科技大学 | Heat treatment method for improving hydrogen embrittlement resistance of martensitic stainless steel, stainless steel and application |
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