CN115747576B - Preparation method of hydrogen embrittlement-resistant fatigue-resistant plate for hydrogen-contacting membrane of high-pressure hydrogen compressor - Google Patents
Preparation method of hydrogen embrittlement-resistant fatigue-resistant plate for hydrogen-contacting membrane of high-pressure hydrogen compressor Download PDFInfo
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 99
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 99
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000012528 membrane Substances 0.000 title claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 19
- 230000003746 surface roughness Effects 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005266 casting Methods 0.000 claims abstract description 10
- 230000033228 biological regulation Effects 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 5
- 239000011733 molybdenum Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000004321 preservation Methods 0.000 claims description 19
- 238000000137 annealing Methods 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 238000005097 cold rolling Methods 0.000 claims description 15
- 238000005242 forging Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000003303 reheating Methods 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 229910052717 sulfur Inorganic materials 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000011572 manganese Substances 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000004513 sizing Methods 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 238000005098 hot rolling Methods 0.000 claims description 2
- 229910052748 manganese Inorganic materials 0.000 claims description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- 239000006104 solid solution Substances 0.000 abstract description 3
- 229910001182 Mo alloy Inorganic materials 0.000 abstract description 2
- 229910052804 chromium Inorganic materials 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 abstract description 2
- 150000002431 hydrogen Chemical class 0.000 abstract description 2
- 238000005728 strengthening Methods 0.000 abstract description 2
- OGSYQYXYGXIQFH-UHFFFAOYSA-N chromium molybdenum nickel Chemical compound [Cr].[Ni].[Mo] OGSYQYXYGXIQFH-UHFFFAOYSA-N 0.000 abstract 1
- 229910045601 alloy Inorganic materials 0.000 description 24
- 239000000956 alloy Substances 0.000 description 24
- 239000000243 solution Substances 0.000 description 8
- 238000013461 design Methods 0.000 description 7
- 230000003009 desulfurizing effect Effects 0.000 description 6
- 239000007769 metal material Substances 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000009661 fatigue test Methods 0.000 description 5
- 238000005520 cutting process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 239000010752 BS 2869 Class D Substances 0.000 description 2
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001887 electron backscatter diffraction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005261 decarburization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention relates to the field of materials of key parts of hydrogen energy equipment, in particular to a preparation method of a hydrogen embrittlement-resistant and fatigue-resistant plate for a hydrogen membrane of a high-pressure hydrogen compressor. The invention is based on a nickel-chromium-molybdenum alloy system, ensures the high strength, fatigue resistance and hydrogen embrittlement resistance of the plate by utilizing solid solution strengthening and grain boundary regulation of chromium, molybdenum and iron, prepares the plate by adopting the method of ingot casting, strip blank preparation, finish rolling by a twenty-high roll mill, grain boundary regulation and leveling, wherein the width of the plate is not less than 400mm, the thickness is 0.45-0.55 mm, the length is not less than 1000mm, the surface roughness Ra of the plate is not more than 0.2 mu m, the unevenness is not more than 10mm/m, the thickness precision is +/-0.02 mm, the yield strength at room temperature and 200 ℃ can reach more than 350MPa and 300MPa respectively, the room temperature fatigue limit can reach more than 230MPa, and simultaneously, the plate has good plasticity and hydrogen embrittlement resistance, and can be used for preparing the hydrogen side diaphragm of a high-pressure (45 MPa and above) hydrogen diaphragm compressor.
Description
Technical Field
The invention relates to the field of materials of key parts of hydrogen energy equipment, in particular to a preparation method of a hydrogen embrittlement-resistant and fatigue-resistant plate for a hydrogen membrane of a high-pressure hydrogen compressor.
Background
Fossil fuels are the main body of energy consumption at present, but with the continuous increase of energy demand, the continuous exhaustion of fossil fuels is the serious problems of energy crisis, global warming, environmental pollution and the like. The development of related industries has been attracting attention in countries around the world due to the characteristics of clean, renewable, high energy density, high heat value, and the like. The hydrogen adding station is a key link in the hydrogen energy industry chain, wherein a high-pressure hydrogen diaphragm compressor (hereinafter referred to as a hydrogen compressor) is one of core equipment in the hydrogen adding station. The hydrogen compressor is equipment for realizing hydrogen pressurization by driving the membrane to reciprocate through hydraulic pressure, and three-layer membrane structural design is adopted at home and abroad in order to ensure safe and stable operation of the hydrogen compressor, but hydrogen-induced failure of the hydrogen-induced membrane still occurs, so that the safety problem of the hydrogen station is greatly challenged.
Currently, 316L and 301 austenitic stainless steels are used for the hydrogen membrane in low pressure hydrogen presses (design pressure below 35 MPa). Engineering practice shows that the service life of the austenitic stainless steel hydrogen-contacting diaphragm is obviously reduced (even less than 1/5-1/10 of the service life of the 35MPa hydrogen compressor diaphragm) along with the increase of the hydrogenation pressure, and the service life of the austenitic stainless steel diaphragm is lower after the service hydrogen pressure is further increased to 90MPa (the design pressure of the 70MPa hydrogen compressor for the hydrogenation station is 90 MPa). The reason for this is that the high temperature strength and fatigue resistance of austenitic stainless steel in high hydrogen pressure environments limit its service life. The future construction of the hydrogen adding station in China is advancing towards a high pressure level, which puts higher demands on key equipment and components of the hydrogen adding station. It goes without saying that the development of the hydrogen embrittlement resistant austenitic alloy sheet material with higher strength grade meets the design and use requirements of the hydrogen press with the pressure grade of 45MPa and higher, and the requirements are urgent.
Disclosure of Invention
Aiming at the material requirement of key parts of hydrogen energy equipment, the invention aims to provide a preparation method of a hydrogen embrittlement-resistant and fatigue-resistant plate for a hydrogen-contacting diaphragm of a high-pressure hydrogen compressor, so as to meet the design and use requirements of the hydrogen-contacting diaphragm of the hydrogen compressor with the pressure of 45MPa and above.
The technical scheme of the invention is as follows:
a preparation method of a hydrogen embrittlement-resistant and fatigue-resistant plate for a hydrogen-contacting diaphragm of a high-pressure hydrogen compressor comprises the steps that the width of the plate is not less than 400mm, the thickness of the plate is 0.45-0.55 mm, the length of the plate is not less than 1000mm, the surface roughness Ra of the plate is not more than 0.2 mu m, the unevenness is not more than 10mm/m, and the thickness precision is +/-0.02 mm; the main components of the plate in percentage by weight are as follows:
cr:21.00 to 23.00, mo: 8.00-10.00, fe:10.00 to 15.00, ni and unavoidable residual elements: the balance; unavoidable residual elements include: aluminum, titanium, manganese, carbon, sulfur, phosphorus, silicon and nitrogen, wherein the aluminum content is controlled to be less than or equal to 0.050, the titanium content is controlled to be less than or equal to 0.030, the manganese content is controlled to be less than or equal to 0.030, the carbon content is controlled to be less than or equal to 0.030, the sulfur content is controlled to be less than or equal to 0.001, the phosphorus content is controlled to be less than or equal to 0.005, the silicon content is controlled to be less than or equal to 0.030, and the nitrogen content is controlled to be less than or equal to 0.010;
the preparation method of the fatigue-resistant hydrogen embrittlement-resistant plate for the high-pressure hydrogen compressor diaphragm comprises the following specific steps of:
(1) Ingot casting preparation: vacuum induction smelting and electroslag remelting are carried out by taking electrolytic nickel, metallic chromium, metallic molybdenum and metallic iron as raw materials to obtain an ingot;
(2) Preparing a belt blank: the cogging and forging temperature of the cast ingot is 1150-1170 ℃, the ingot is allowed to be returned to the furnace for reheating before being forged to the final specification, the temperature is kept for 1-4 hours at 1150-1170 ℃, and the final forging temperature is not lower than 950 ℃, so as to obtain a forged billet; the forging stock is subjected to hot rolling after heat preservation for 2-4 hours at 1130-1150 ℃, the cogging rolling temperature is 1100-1150 ℃, the reheating is allowed before the rolling to the final specification, the heat preservation is carried out for 0.5-3 hours at 1100-1150 ℃, and the final rolling temperature is not lower than 900 ℃, so that the hot rolled coiled material with the thickness of 4-6 mm is obtained; the hot rolled coiled material is pickled after uncoiling, cold rolling is carried out at room temperature, the deformation amount between every two annealing is 20-50%, the middle is subjected to stress relief annealing by adopting heat preservation for 15-60 min at 980-1030 ℃, and a strip blank with the thickness of 1-1.5 mm is obtained;
(3) Finish rolling by a twenty-high rolling mill: adopting a twenty-roller cold rolling unit with the roller surface roughness Ra less than or equal to 0.2 mu m to finish-roll the cold-rolled strip blank to obtain a finish-rolled plate with the thickness of 0.45-0.55 mm;
(4) Grain boundary regulation: the solution treatment temperature of the finish rolling plate is controlled at 1050-1150 ℃, the heat preservation time is 20-60 min, and the grain size is not lower than 7 grades; small-deformation cold rolling of the sheet, wherein the deformation amount of the cold rolling of the sheet is 3-7%; carrying out annealing heat treatment on the small-deformation plate at 980-1050 ℃ for 5-10 min;
(5) Leveling and sizing: the flattening pressing rate is 0.5-1.0%, and the roller surface roughness Ra is less than or equal to 0.2 mu m.
Preparation method of hydrogen embrittlement-resistant fatigue-resistant plate for hydrogen membrane of high-pressure hydrogen compressor, and sigma 3 of plate n The grain boundary proportion is not less than 55%, n=1, 2 or 3, and the sigma is not less than 29, the grain boundary proportion is not less than 60%.
The preparation method of the hydrogen embrittlement-resistant fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor comprises the following steps of: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 35%.
The preparation method of the hydrogen embrittlement-resistant fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor comprises the following steps of: the yield strength (Rp 0.2) is not lower than 300MPa, the tensile strength (Rm) is not lower than 650MPa, and the elongation (A) is not lower than 35%.
The preparation method of the hydrogen embrittlement-resistant fatigue-resistant plate for the high-pressure hydrogen compressor hydrogen-contacting membrane comprises the following steps of carrying out hydrogen charging treatment on the plate at 300 ℃ and 10MPa for 72 hours, wherein the mechanical properties of the plate at room temperature are as follows: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 25%.
According to the preparation method of the hydrogen embrittlement-resistant and fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor, the fatigue limit of the plate under the confidence coefficient of 50% is not lower than 230MPa.
In the step (4), the plate solid solution treatment is carried out in a gas protection heat treatment furnace, and the gas medium is argon or reducing gas.
In the step (4), the sheet annealing heat treatment adopts a vacuum or gas protection heat treatment furnace, and the protection gas is argon or reducing gas.
According to the preparation method of the hydrogen embrittlement-resistant fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor, the nonmetallic inclusion in the plate after annealing heat treatment in the step (4) meets the following requirements: fine system (m), A is less than or equal to 0.5 level, B is less than or equal to 0.5 level, D is less than or equal to 1.0 level, and the sum of the three types is less than or equal to 1.5 level; coarse system (m), A is less than or equal to 0.5 level, B is less than or equal to 0.5 level, D is less than or equal to 0.5 level, and the sum of the three types is less than or equal to 1.5 level; wherein A is sulfide, B is alumina, D is spherical oxide, and the sum of the three is A+B+D.
The design idea of the invention is as follows:
first, based on the design of single-phase austenitic alloy structure, by adding on the basis of Ni-Cr-Mo alloy systemAnd a proper amount of Fe is used for improving the alloy strength and controlling the cost so as to obtain higher temperature and high temperature strength of 200 ℃, wherein the room temperature yield strength (Rp 0.2) of the MP-4 alloy can reach more than 350MPa, the room temperature yield strength (Rp 0.2) of the MP-4 alloy can reach 300MPa, and meanwhile, the MP-4 alloy has good plasticity (the elongation at room temperature and 200 ℃ is higher than 35 percent and 35 percent respectively). First, by controlling the content of C, N nonmetallic elements, the precipitation of carbonitrides is reduced, and the fatigue life is improved. Second, by grain boundary regulation and control method, the number of free grain boundaries in the alloy is reduced, and special grain boundaries (low sigma 3 is promoted n (n=1, 2, 3) lattice grain boundaries at the coincident positions), and the hydrogen-induced crack initiation and propagation resistance along the grain boundaries of the plate alloy is obviously improved, so that the excellent hydrogen embrittlement resistance and fatigue resistance of the plate are obtained. Thirdly, the method for reducing the level of nonmetallic inclusion and regulating grain boundary through vacuum induction and electroslag remelting and smelting preparation reduces the number of strong hydrogen traps (also being a fatigue crack source) in the plate alloy, and can cooperatively improve the fatigue limit and hydrogen embrittlement resistance of the plate. Fourthly, finish rolling is carried out through a twenty-high rolling mill, so that the low-roughness plate is obtained, and the fatigue resistance of the plate is improved.
The invention has the advantages and beneficial effects that:
1. the hydrogen embrittlement-resistant fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor has low contents of carbon, nitrogen, sulfur and phosphorus impurity elements and nonmetallic inclusions, low surface roughness of the plate, high proportion of lattice grain boundaries at low sigma coincident positions, excellent high-temperature strength (nearly doubled compared with 316L) at the temperature of 200 ℃, excellent hydrogen embrittlement resistance and capability of being used under the complicated and severe working conditions of a hydrogen compressor of 45MPa or more.
2. The special plate has the width of not less than 400mm, the thickness of 0.45-0.55 mm, the length of not less than 1000mm, the surface roughness Ra of the plate is not more than 0.2 mu m, the unevenness is not more than 10mm/m, and the thickness precision is +/-0.02 mm.
3. Sigma 3 of the special plate of the invention n The proportion of special grain boundary is not less than 55%, and the proportion of sigma is not less than 29 grain boundary is not less than 60%.
4. The room temperature mechanical properties of the special plate disclosed by the invention are as follows: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 35%.
5. The high-temperature mechanical properties at 200 ℃ of the special plate disclosed by the invention meet the following conditions: the yield strength (Rp 0.2) is not lower than 300MPa, the tensile strength (Rm) is not lower than 650MPa, and the elongation (A) is not lower than 35%.
6. The special plate provided by the invention is placed in high-purity hydrogen (volume purity is more than or equal to 99.999%) gas for 72 hours at 300 ℃ and 10MPa, and the room-temperature mechanical properties are as follows: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 25%.
7. The special plate has good plasticity, hydrogen embrittlement resistance and fatigue resistance, has a fatigue limit of not less than 230MPa under 50% confidence, and can be used for preparing hydrogen-contacting membranes of 45MPa and above hydrogen presses.
Drawings
Fig. 1 is an EBSD diagram of a grain boundary structure of a special plate.
FIG. 2 is a graph of special grain boundary statistics for a specialty sheet; in the figure, the abscissa Sigma-Value represents the grain boundary type, and the ordinate Fraction represents the specific grain boundary ratio (%).
Detailed Description
In the specific implementation process, the strength, fatigue resistance and hydrogen embrittlement resistance of the special plate are ensured based on Cr, mo and Fe element solid solution strengthening and grain boundary regulation, and the plate is prepared by a method of casting blank preparation, strip blank preparation, finish rolling by a twenty-high roll mill, grain boundary regulation and leveling. The special plate has the width of not less than 400mm, the thickness of 0.45-0.55 mm, the length of not less than 1000mm, the surface roughness Ra of the plate is not more than 0.2 mu m, the unevenness is not more than 10mm/m, and the thickness precision is +/-0.02 mm.
The invention is further illustrated by the following examples.
Example 1 sheet material with a specification of 1500 mm. Times.500 mm. Times.0.53 mm
Smelting alloy in a 1.0 ton vacuum induction furnace by adopting an aluminum magnesium spinel crucible, performing primary refining and primary refining desulfurization treatment in the smelting process, and then casting an ingot; the casting ingot is subjected to electroslag remelting after surface polishing treatment, the remelted casting ingot is subjected to polishing treatment to obtain a casting blank, the casting blank is prepared by a strip blank, finish rolling by a twenty-high roll mill, grain boundary regulation and control, and a special plate with 1500mm multiplied by 500mm multiplied by 0.53mm is prepared by flat sizing, wherein the chemical compositions are shown in Table 1, and the preparation process is as follows:
1. electrolytic nickel, metallic chromium, metallic molybdenum and metallic iron are taken as raw materials, ni, cr, mo, fe is put into a crucible before smelting, and a calcium desulfurizing agent is put into a hopper. Vacuum induction smelting is carried out by adopting an aluminum magnesium spinel crucible, refining is carried out for 10-15 minutes at 1530-1570 ℃ (10 minutes for the embodiment of 1530 ℃), then calcium desulfurizing agent is added for refining for 5-15 minutes (10 minutes for the embodiment of 10 minutes), better heat stability of the crucible and desulfurizing agent are utilized for desulfurizing, and cast ingots are cast at 1480-1520 ℃ (1500 ℃ for the embodiment of). The ingot is subjected to electroslag remelting, and the specification of the remelted ingot is phi 220-360 mm (phi 300mm in the embodiment).
2. The electroslag cast ingot is subjected to alloy forging (the heat preservation time is 6h at 1130 ℃ in the embodiment) after being subjected to heat preservation for 4-12 h at 1050-1150 ℃, the cogging forging temperature is 1050-1150 ℃ (1130 ℃ in the embodiment), and the final forging temperature is 850-950 ℃ (930 ℃ in the embodiment), so as to obtain a forging stock; the blank is allowed to be returned to the final gauge for reheating and then is held at 1050-1150 ℃ for 1-4 hours (this example is returned to the furnace for four times and held at 1130 ℃ for 1.5 hours), with the forged blank having a cross-sectional gauge of 400 x 60mm. The forging slab is rolled after heat preservation for 2-4 h at 1150-1170 ℃ (the heat preservation time of 1150 ℃ in the embodiment is 4 h), the cogging rolling temperature is 1150-1170 ℃ (1150 ℃ in the embodiment), the finishing rolling temperature is not lower than 900 ℃ (950 ℃ in the embodiment), the reheating is allowed before the rolling to the final specification, the heat preservation is carried out for 0.5-3 h at 1150-1170 ℃ (the heat preservation time of 1150 ℃ is 0.5h for three times in the embodiment), and the final hot rolled plate section specification is 530 multiplied by 5.0mm. The hot rolled coil is uncoiled, is subjected to cold rolling at room temperature after being pickled, and is subjected to stress relief annealing by adopting 980-1030 ℃ in the middle (1000 ℃ in the embodiment) for 15-60 min (30 min in the embodiment) with 20-50% of deformation between annealing every time (40-50% in the embodiment), so as to obtain a cold rolled sheet with the thickness of 1-1.5 mm (1 mm in the embodiment).
3. The cold-rolled sheet was cold-rolled at room temperature using a twenty-roller cold-rolling mill having a roller surface roughness Ra of 0.2 μm or less (ra=0.1 μm in this example) to obtain a finish-rolled sheet having a thickness of 0.45 to 0.55mm (0.53 mm in this example).
4. The fine plate rolled material is subjected to solution treatment, the plate solution treatment is performed in a gas protection heat treatment furnace, and the gas medium is argon. The solution treatment temperature is controlled to 1050-1150 ℃ (1100 ℃ in the embodiment), the heat preservation time is 20-60 min (30 min in the embodiment), and the air cooling is performed; taking the sheet subjected to solution treatment, cutting a metallographic specimen perpendicular to the rolling direction of the sheet, preparing the specimen according to a standard metallographic test method, and evaluating the grain size according to the specification of GB/T9394 metal average grain size determination method, wherein the evaluation result shows that the average grain size of the alloy sheet is 7 grade; the solution-treated sheet was cold rolled to a final sheet thickness of 0.50mm with a deformation of 3 to 7% (5% in this example), and then subjected to an annealing heat treatment of 980 to 1050 ℃ for 5 to 10 minutes (9 minutes in this example). The annealing heat treatment of the plate adopts a gas protection heat treatment furnace, and the protection gas is argon.
5. The annealed finish rolled plate is flattened by a twenty-roller cold rolling mill with the roller surface roughness Ra less than or equal to 0.2 mu m (Ra=0.1 mu m in the embodiment), and the pressing rate is 0.5-1% (0.5% in the embodiment); and then cutting to length.
6. Taking the hot rolled plate in the step 2, cutting a metallographic specimen along the longitudinal section in the rolling direction, preparing the specimen according to a standard metallographic test method, and carrying out inclusion assessment according to GB/T10561 'microscopic assessment method of nonmetallic inclusion in steel', wherein the result is shown in Table 2.
7. The flat plate in the step 5 is taken for size and surface quality detection, and the result shows that the width of the plate is not less than 530mm (500 mm in the embodiment), the thickness is not less than 0.45-0.55 mm (0.50 mm in the embodiment), the length is not less than 1000mm (1500 mm in the embodiment), the surface roughness Ra is less than or equal to 0.2 mu m (Ra=0.16 mu m in the embodiment), the unevenness is not more than 10mm/m (3 mm/m in the embodiment), and the thickness precision is +/-0.02 mm (0.02-0.02 mm in the embodiment).
8. Taking the plate flattened in the step 5, and processing the plate into corresponding specificationsSample, EBSD analysis of plate alloy grain boundary, shows Sigma 3 in plate alloy n The proportion of special grain boundary is 68.36%, the proportion of sigma less than or equal to 29 grain boundary is 70.42%, the grain boundary structure and sigma 3 n The statistics of the proportion of the special grain boundary are shown in fig. 1 and fig. 2 respectively.
9. And (3) taking the plate flattened in the step (5), processing a plate-shaped tensile sample, and detecting room temperature mechanical properties according to GB/T228.1 section 1 room temperature test method of metal material tensile test, wherein the results are shown in Table 3.
10. And (3) taking the plate flattened in the step (5), processing a tensile sample, and detecting the mechanical property at 200 ℃ according to GB/T4338 high temperature tensile test method of metal materials, wherein the result is shown in Table 4.
11. And (3) taking the plate flattened in the step (5), processing a tensile sample, then carrying out hydrogen charging treatment on the plate at 300 ℃ and 10MPa for 72 hours, and carrying out mechanical property detection according to GB/T228.1, wherein the volume purity is more than or equal to 99.999%, and the results are shown in Table 5.
12. And (3) taking the flattened plate in the step (5), processing a fatigue test sample, and carrying out fatigue performance test by referring to GB/T3075-2008 'axial force control method for metal material fatigue test' and GB/T24176-2009 'statistical scheme and analysis method for metal material fatigue test data', wherein the result shows that the fatigue limit under the 50% confidence coefficient is 250MPa.
Table 1 chemical composition, mass percent, of the sheet alloy
| Element(s) | C | S | N | Cr | Mo | Fe | Al | Ti | Mn | P | Si | Ni |
| Content of | 0.026 | 0.001 | 0.002 | 21.2 | 9.8 | 10.5 | 0.021 | 0.01 | 0.02 | 0.001 | 0.038 | Allowance of |
TABLE 2 nonmetallic inclusion of sheet alloy
Table 3 mechanical properties of the sheet at room temperature
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 484 | 797 | 38.5 |
| 2 | 482 | 784 | 40.0 |
| 3 | 488 | 799 | 36.0 |
Table 4 mechanical Properties of the sheet at 200 ℃
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 422 | 720 | 36.0 |
| 2 | 429 | 733 | 35.5 |
| 3 | 428 | 737 | 36.0 |
TABLE 5 mechanical Properties at Room temperature of the plate after thermal Hydrogen charging
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 486 | 793 | 29.2 |
| 2 | 490 | 796 | 28.0 |
| 3 | 474 | 794 | 27.5 |
Experimental results show that the prepared plate with the specification of 1500mm multiplied by 500mm multiplied by 0.50mm has the surface roughness Ra less than or equal to 0.2 mu m and the unevenness not more than 3mm/m; only class-D nonmetallic inclusions of 0.5 grade exist in the plate; sigma 3 in plate alloy n The proportion of special grain boundary is higher than 68 percent, and the proportion of the grain boundary with the sigma less than or equal to 29 percent is higher than 70 percent; the mechanical properties of the plate at room temperature are as follows: yield strength (Rp) 0.2 ) Higher than 480MPa, tensile strength (Rm) higher than 780MPa, and elongation higher than 35%; the mechanical properties of the plate at 200 ℃ are as follows: yield strength (Rp) 0.2 ) Higher than 420MPa, tensile strength (Rm) higher than 720MPa, and elongation higher than 35%; after being left for 72 hours in a high-purity hydrogen atmosphere at 300 ℃ and 10MPa, the product has a yield strength (Rp 0.2 ) More than 470MPa, tensile strength (Rm) more than 790MPa, and elongation more than 25%; the fatigue limit of the plate at the 50% confidence level is not lower than 250MPa.
Example 2: sheet material with specification of 1000mm x 450mm x 0.52mm
The difference from example 1 is that the sheet prepared has a length of 1000mm, a width of 450mm and a thickness of 0.52mm.
Smelting alloy in a vacuum induction furnace of 500Kg by adopting a CaO crucible, and smelting alloy by taking electrolytic nickel, metallic chromium, metallic molybdenum and metallic iron as raw materials. In the smelting process, firstly refining treatment is carried out for 10 minutes at 1550 ℃, then calcium desulfurizing agent is added for refining for 10 minutes, decarburization and desulfurization treatment are carried out by utilizing the heat stability of a CaO crucible and the desulfurizing agent, and cast ingots are cast at 1510 ℃. Casting ingotElectroslag remelting was carried out, the specification of remelted ingot was phi 230mm, and the chemical composition is shown in table 6. Alloy forging is carried out after heat preservation is carried out for 4 hours at 1150 ℃, the cogging forging temperature is 1150 ℃, the final forging temperature is 950 ℃, the furnace is returned to heat for two times before forging to the final specification, the reheating temperature is 1150 ℃, the heat preservation time is 1 hour, and the section specification of the forged slab is 300 multiplied by 70mm. And (3) rolling after the heat preservation time is 2h at 1130 ℃, the cogging rolling temperature is 1130 ℃, the final rolling temperature is 920 ℃, the hot rolled plate is returned to the furnace and heated three times before being rolled to the final specification, the reheating temperature is 1130 ℃, the heat preservation time is 0.5h, and the final specification of the section of the hot rolled plate is 450 multiplied by 3.0mm. The cold-rolled sheet with the thickness of 1.1mm is prepared by carrying out multi-pass cold-rolling annealing processing of stress-relief annealing heat treatment with the deformation of 40-50% + and the temperature of 1000 ℃ for 30min, the cold-rolled sheet is subjected to cold finish rolling by adopting a twenty-roller cold-rolling mill with the roller surface roughness Ra=0.1 mu m, the cold-rolled sheet with the thickness of 0.55mm is prepared, the cold-rolled sheet is subjected to solution treatment of 1000 ℃ for 30min air cooling, the solution treatment of the sheet is carried out in a gas protection heat treatment furnace, and the gas medium is argon. Subsequently, 5% cold rolling was performed to obtain a sheet having a thickness of 0.52mm. And then carrying out annealing heat treatment on the plate at 980 ℃ for 10min, wherein the annealing heat treatment adopts a gas protection heat treatment furnace, and the protection gas is argon. Flattening the annealed finish rolled plate by adopting a twenty-roller cold rolling mill with roller surface roughness Ra=0.1 mu m, wherein the pressing rate is 0.5%; and then cutting to length. The dimensions and surface quality measurements showed that the sheet surface roughness ra=0.2 μm and the unevenness was 4mm/m. Sigma 3 in plate alloy n The proportion of special grain boundary is 66.7%, the proportion of sigma is less than or equal to 29 grain boundary is 68.5%, the evaluation result of nonmetallic inclusion is shown in table 7, the mechanical properties at room temperature are shown in table 8, the mechanical properties at 200 ℃ are shown in table 9, the mechanical properties at 300 ℃ are shown in table 10, and the mechanical properties after the hydrogen charging treatment of high-purity hydrogen (volume purity is more than or equal to 99.999%) and 72 hours are shown in table 10. The fatigue performance test is carried out by referring to GB/T3075-2008 axial force control method for metal material fatigue test and GB/T24176-2009 statistical scheme and analysis method for metal material fatigue test, and the result shows that the fatigue limit of the plate under the 50% confidence level is 243MPa.
Table 6 chemical composition, mass percent, of the sheet alloy
| Element(s) | C | S | N | Cr | Mo | Fe | Al | Ti | Mn | P | Si | Ni |
| Content of | 0.024 | 0.001 | 0.002 | 22.3 | 9.5 | 12.5 | 0.014 | 0.01 | 0.03 | 0.004 | 0.02 | Allowance of |
TABLE 7 nonmetallic inclusion of sheet alloy
Table 8 mechanical properties of the sheet at room temperature
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 463 | 787 | 42.0 |
| 2 | 466 | 792 | 44.5 |
| 3 | 457 | 791 | 40.0 |
Table 9 mechanical Properties of the sheet at 200 ℃
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 437 | 735 | 38.0 |
| 2 | 430 | 729 | 40.5 |
| 3 | 433 | 730 | 39.0 |
Table 10 room temperature mechanical properties of the sheet after thermal charging
| Numbering device | Rp 0.2 /MPa | R m /MPa | A/％ |
| 1 | 458 | 784 | 33.0 |
| 2 | 461 | 795 | 29.5 |
| 3 | 464 | 789 | 32.0 |
Experimental results show that the prepared plate with the specification of 1000mm multiplied by 450mm multiplied by 0.52mm has the surface roughness Ra less than or equal to 0.2 mu m and the flatness not exceeding 4mm/m; only class-D nonmetallic inclusions of 0.5 grade exist in the plate; sigma 3 in plate alloy n The proportion of special grain boundary is higher than 66%, and the proportion of the grain boundary with the sigma less than or equal to 29 is higher than 68%; the mechanical properties of the plate at room temperature are as follows: yield strength (Rp) 0.2 ) A tensile strength (Rm) higher than 455MPa, 785MPa, and an elongation higher than 40%; the mechanical properties of the plate at 200 ℃ are as follows: yield strength (Rp) 0.2 ) Higher than 430MPa, tensile strength (Rm) higher than 725MPa, and elongation higher than 38%; after being left for 72 hours in a high-purity hydrogen atmosphere at 300 ℃ and 10MPa, the product has a yield strength (Rp 0.2 ) Is higher than 455MPa and has high tensile strengthThe degree (Rm) is higher than 780MPa, and the elongation is higher than 29%; the fatigue limit of the plate at 50% confidence is higher than 240MPa.
Claims (9)
1. A preparation method of a hydrogen embrittlement-resistant and fatigue-resistant plate for a hydrogen-contacting diaphragm of a high-pressure hydrogen compressor is characterized in that the width of the plate is not less than 400mm, the thickness of the plate is 0.45-0.55 mm, the length of the plate is not less than 1000mm, the surface roughness Ra of the plate is not more than 0.2 mu m, the unevenness is not more than 10mm/m, and the thickness precision is +/-0.02 mm; the plate comprises the following components in percentage by weight:
cr:21.00 to 23.00, mo: 8.00-10.00, fe:10.00 to 15.00, ni and unavoidable residual elements: the balance; unavoidable residual elements include: aluminum, titanium, manganese, carbon, sulfur, phosphorus, silicon and nitrogen, wherein the aluminum content is controlled to be less than or equal to 0.050, the titanium content is controlled to be less than or equal to 0.030, the manganese content is controlled to be less than or equal to 0.030, the carbon content is controlled to be less than or equal to 0.030, the sulfur content is controlled to be less than or equal to 0.001, the phosphorus content is controlled to be less than or equal to 0.005, the silicon content is controlled to be less than or equal to 0.030, and the nitrogen content is controlled to be less than or equal to 0.010;
the preparation method of the fatigue-resistant and hydrogen-embrittlement-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor comprises the following specific steps of:
(1) Ingot casting preparation: vacuum induction smelting and electroslag remelting are carried out by taking electrolytic nickel, metallic chromium, metallic molybdenum and metallic iron as raw materials to obtain an ingot;
(2) Preparing a belt blank: the cogging and forging temperature of the cast ingot is 1150-1170 ℃, the ingot is allowed to be returned to the furnace for reheating before being forged to the final specification, the temperature is kept for 1-4 hours at 1150-1170 ℃, and the final forging temperature is not lower than 950 ℃, so as to obtain a forged billet; the forging stock is subjected to hot rolling after heat preservation for 2-4 hours at 1130-1150 ℃, the cogging rolling temperature is 1100-1150 ℃, the reheating is allowed before the rolling to the final specification, the heat preservation is carried out for 0.5-3 hours at 1100-1150 ℃, and the final rolling temperature is not lower than 900 ℃, so that the hot rolled coiled material with the thickness of 4-6 mm is obtained; the hot rolled coiled material is pickled after uncoiling, cold rolling is carried out at room temperature, the deformation amount between every two annealing is 20-50%, the middle is subjected to stress relief annealing by adopting heat preservation for 15-60 min at 980-1030 ℃, and a strip blank with the thickness of 1-1.5 mm is obtained;
(3) Finish rolling by a twenty-high rolling mill: adopting a twenty-roller cold rolling unit with the roller surface roughness Ra less than or equal to 0.2 mu m to finish-roll the cold-rolled strip blank to obtain a finish-rolled plate with the thickness of 0.45-0.55 mm;
(4) Grain boundary regulation: the solution treatment temperature of the finish rolling plate is controlled at 1050-1150 ℃, the heat preservation time is 20-60 min, and the grain size is not lower than 7 grades; small-deformation cold rolling of the sheet, wherein the deformation amount of the cold rolling of the sheet is 3-7%; carrying out annealing heat treatment on the small-deformation plate at 980-1050 ℃ for 5-10 min;
(5) Leveling and sizing: the flattening pressing rate is 0.5-1.0%, and the roller surface roughness Ra is less than or equal to 0.2 mu m.
2. The method for producing a hydrogen embrittlement and fatigue resistant sheet material for a hydrogen-contacting membrane of a high pressure hydrogen compressor according to claim 1, wherein Σ3 of the sheet material n The grain boundary proportion is not less than 55%, n=1, 2 or 3, and the sigma is not less than 29, the grain boundary proportion is not less than 60%.
3. The method for preparing the hydrogen embrittlement-resistant fatigue-resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor according to claim 1, wherein the plate has the following room-temperature mechanical properties: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 35%.
4. The method for preparing the hydrogen embrittlement and fatigue resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor according to claim 1, wherein the plate has the following mechanical properties at a high temperature of 200 ℃: the yield strength (Rp 0.2) is not lower than 300MPa, the tensile strength (Rm) is not lower than 650MPa, and the elongation (A) is not lower than 35%.
5. The method for preparing the hydrogen embrittlement and fatigue resistant plate for the hydrogen membrane of the high-pressure hydrogen compressor, according to claim 1, is characterized in that after the hydrogen charging treatment for 72 hours at 300 ℃ under 10MPa with high purity of more than or equal to 99.999 percent, the room temperature mechanical properties of the plate are as follows: the yield strength (Rp 0.2) is not lower than 350MPa, the tensile strength (Rm) is not lower than 700MPa, and the elongation (A) is not lower than 25%.
6. The method for producing a hydrogen embrittlement and fatigue resistant sheet material for a hydrogen-contacting membrane of a high pressure hydrogen compressor according to claim 1, wherein the sheet material has a fatigue limit of not less than 230MPa at a confidence level of 50%.
7. The method for producing a hydrogen embrittlement and fatigue resistant sheet material for a hydrogen-bearing membrane for a high-pressure hydrogen compressor according to claim 1, wherein in the step (4), the sheet material solution treatment is performed in a gas-shielded heat treatment furnace, and the gaseous medium is argon or a reducing gas.
8. The method for producing a hydrogen embrittlement and fatigue resistant sheet material for a hydrogen-contacting membrane of a high pressure hydrogen compressor according to claim 1, wherein in the step (4), a vacuum or gas-shielded heat treatment furnace is used for the sheet material annealing heat treatment, and the shielding gas is argon or a reducing gas.
9. The method for preparing the hydrogen embrittlement and fatigue resistant plate for the hydrogen-contacting diaphragm of the high-pressure hydrogen compressor, according to claim 1, wherein the nonmetallic inclusion in the plate after the annealing heat treatment in the step (4) meets the following requirements: fine system (m), A is less than or equal to 0.5 level, B is less than or equal to 0.5 level, D is less than or equal to 1.0 level, and the sum of the three types is less than or equal to 1.5 level; coarse system (m), A is less than or equal to 0.5 level, B is less than or equal to 0.5 level, D is less than or equal to 0.5 level, and the sum of the three types is less than or equal to 1.5 level; wherein A is sulfide, B is alumina, D is spherical oxide, and the sum of the three is A+B+D.
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