CN117554245B - Device and method for measuring hydrogen diffusion coefficient of nickel-based superalloy based on resistivity - Google Patents
Device and method for measuring hydrogen diffusion coefficient of nickel-based superalloy based on resistivity Download PDFInfo
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- CN117554245B CN117554245B CN202410040203.7A CN202410040203A CN117554245B CN 117554245 B CN117554245 B CN 117554245B CN 202410040203 A CN202410040203 A CN 202410040203A CN 117554245 B CN117554245 B CN 117554245B
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 217
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 217
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 238000009792 diffusion process Methods 0.000 title claims abstract description 55
- 229910000601 superalloy Inorganic materials 0.000 title claims abstract description 48
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 173
- 238000012360 testing method Methods 0.000 claims abstract description 135
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 124
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 90
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 62
- 150000002431 hydrogen Chemical class 0.000 claims abstract description 49
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 42
- 229910052751 metal Inorganic materials 0.000 claims abstract description 37
- 239000002184 metal Substances 0.000 claims abstract description 37
- 239000012466 permeate Substances 0.000 claims abstract description 4
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- 238000005498 polishing Methods 0.000 claims description 21
- 238000011084 recovery Methods 0.000 claims description 16
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- 239000000463 material Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
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- 238000013461 design Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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Abstract
The invention discloses a measuring device and a measuring method for a hydrogen diffusion coefficient of a nickel-based superalloy based on resistivity. The method comprises the following steps: mounting the test sample electroplated with the metal palladium layer between the outer gasket and the inner gasket; sequentially introducing nitrogen and hydrogen into the measuring device for purging; continuously introducing hydrogen into the measuring device to the target hydrogen pressure, then testing, recording the corresponding testing time when the resistivity is increased by 1% when the hydrogen permeates into the metal palladium layer, and calculating the hydrogen diffusion coefficient of the test sample; and repeatedly testing a plurality of samples, and averaging test results to obtain the nickel-based superalloy hydrogen diffusion coefficient based on resistivity. The invention adopts the palladium plating layer which is more sensitive to hydrogen element, the device is simple, the method is convenient and fast, and the cost is low.
Description
Technical Field
The invention belongs to the technical field of nickel-based superalloy hydrogen diffusion coefficient measurement, and particularly relates to a device and a method for measuring nickel-based superalloy hydrogen diffusion coefficient based on resistivity.
Background
It is well known that nickel-base superalloys are widely used for the preparation of hot end components for aircraft engines and ground gas turbines because of their excellent high temperature strength, creep resistance, fatigue resistance and oxidation resistance. In order to inhibit emission of greenhouse gases, development of hydrogen fuel engines is widely focused, and hydrogen is very easy to penetrate into nickel-based superalloy in the service process of hot end components in a hydrogen environment, so that alloy hydrogen embrittlement is caused. Hydrogen entering the alloy can be divided into two types according to diffusivity: diffusible hydrogen that is solid-dissolved in the matrix or reversible hydrogen traps and non-diffusible hydrogen that is adsorbed by the non-reversible hydrogen traps, wherein diffusible hydrogen is a major factor in causing hydrogen embrittlement failure of the alloy. In order to research the hydrogen embrittlement phenomenon in the service process of the hydrogen environment and reveal the hydrogen embrittlement failure mechanism of the nickel-based superalloy, the hydrogen diffusion coefficient in the nickel-based superalloy needs to be measured to assist in explaining the cracking process of the hydrogen-induced superalloy.
The current method for measuring the hydrogen diffusion coefficient in the nickel-based superalloy comprises an electrochemical method and a gas phase method, wherein the gas phase method adopts high-pressure hydrogen in a pressure kettle to charge hydrogen to a test sample, and the electrochemical method adopts electrochemical cathode electrolysis to charge hydrogen to the test sample. The same point of the two methods is that electrochemical methods are adopted to detect whether hydrogen diffuses to the hydrogen escape side, a constant potential is applied between a test sample and a corresponding auxiliary electrode, hydrogen atoms diffused from the hydrogen charging side are electrolyzed into hydrogen ions, a generated current can record a diffusion curve in real time, the diffusion curve reflects the diffusion characteristic of the hydrogen atoms in the test sample, and relevant information of diffusion of the hydrogen atoms in the material can be obtained by analyzing the diffusion curve. However, the test device used for detecting the hydrogen element by the electrochemical method is complex, the operation is very complicated, nickel needs to be plated on the hydrogen escaping side of the test sample when the hydrogen element is detected by the electrochemical method, the diffusion distance of the hydrogen element is increased, the test result is inaccurate, and the electrode corrosion is caused by continuously generating oxygen in the electrolytic cell in the hydrogen detection process, so that the repeatability and the reliability of the test result are reduced, and therefore, the development of the device and the method for measuring the hydrogen diffusion coefficient of the nickel-based superalloy based on the resistivity are urgent demands.
The invention patent with application publication number of CN116482013A discloses an experimental device for measuring gas or gas-liquid mixed state high-pressure hydrogen permeation behavior and a test method thereof, wherein the experimental device comprises an autoclave, a clamping sleeve connector, a pressure reducing valve, an exhaust valve, a high-pressure hydrogen cylinder, a connecting device of the autoclave and an electrolytic cell, the electrolytic cell, an experimental electrode, an electrochemical workstation and a strain gauge tester, two threaded through holes are arranged in the middle position of a kettle cover on the upper side of the autoclave, the two threaded through holes are respectively connected with the clamping sleeve connector, the clamping sleeve connector is connected with a guide pipe, the two guide pipes are respectively connected with the pressure reducing valve and the exhaust valve, the pressure reducing valve is connected with the high-pressure hydrogen cylinder through another guide pipe, and a circular channel is arranged in the middle of the kettle body of the autoclave. The invention patent with application publication number of CN115078183A discloses an experimental device and a method for detecting high-pressure hydrogen permeation behavior, the experimental device comprises a gas phase system, an autoclave and an electrolytic cell device which are connected, an electrochemical test system, an exhaust gas recovery system and a temperature control system, the gas phase system comprises an autoclave, a four-way valve, an exhaust valve, a high-purity hydrogen cylinder and a high-purity nitrogen cylinder, the electrochemical test system comprises an experimental electrode, an electrochemical workstation and a computer, the exhaust gas recovery system comprises an exhaust valve and a combustion system, the temperature control system comprises a tester and a water bath, grips are arranged at the left side and the right side of a cover of the autoclave, and gaskets are arranged at the upper side of the sample. According to the two technical schemes, the electrochemical method is adopted to detect the hydrogen element, nickel needs to be plated on the hydrogen escaping side of the test sample, the diffusion distance of the hydrogen element is increased, the test result is inaccurate, and the used test device is complex in structure and complex in operation.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a measuring device for the hydrogen diffusion coefficient of a nickel-based superalloy based on resistivity, which comprises a high-voltage component, a connecting component and a resistivity testing component which are sequentially connected from left to right, wherein a test sample is installed in the connecting component, and a metal palladium layer is electroplated on the hydrogen escaping surface of the test sample.
Preferably, the high-pressure component comprises an autoclave body, a hydrogen pipeline, a hydrogen valve, a first pressure gauge, a nitrogen pipeline, a nitrogen valve, a second pressure gauge, an exhaust pipeline and an exhaust valve; the left side of the autoclave body is provided with the hydrogen pipeline and the nitrogen pipeline, the hydrogen pipeline is provided with the hydrogen valve and the first pressure gauge, and the nitrogen pipeline is provided with the nitrogen valve and the second pressure gauge; the top of the autoclave body is provided with the exhaust pipeline, and the exhaust pipeline is provided with the exhaust valve; the hydrogen pipeline is connected with a high-pressure hydrogen cylinder, the nitrogen pipeline is connected with a high-pressure nitrogen cylinder, and the exhaust pipeline is connected with a gas recovery cylinder.
In any of the above aspects, preferably, the connection assembly includes a hydrogen passage, a sleeve, an inner flange, an outer flange, a fastening screw, an inner gasket, an outer gasket, and an annular gasket; the left end of the hydrogen channel is arranged on the right side of the autoclave body, and the right end of the hydrogen channel is embedded into the sleeve; the inner flange is arranged at the outer side of the hydrogen channel, the outer flange is arranged at the outer side of the sleeve, and the inner flange and the outer flange are fixedly connected through six fastening screws; the center part of the right end of the hydrogen channel, the center part of the inner gasket and the center part of the bottom of the sleeve are all provided with through holes, the diameters of the three through holes are equal, and the central axes of the three through holes are positioned on the same straight line; the outer gasket is symmetrically provided with two round holes at two sides of the center point of the outer gasket.
In any of the above schemes, preferably, the annular gasket is disposed between the outer wall of the hydrogen channel and the inner wall of the sleeve, the inner gasket and the outer gasket are sequentially disposed between the central part of the right end of the hydrogen channel and the central part of the bottom of the sleeve from left to right, the test sample is mounted between the inner gasket and the outer gasket, the metal palladium layer faces one side of the outer gasket, and the central axes of the inner gasket, the outer gasket and the test sample are on the same straight line.
In any of the above schemes, preferably, the resistivity testing assembly comprises a resistivity tester, two electrode wires, two testing chucks and two fixing springs; one end of the electrode wire is connected with the test chuck, the other end of the electrode wire is connected with the resistivity tester, and the test chuck is provided with the fixed spring; the two test chucks are respectively inserted into the two round holes and are contacted with the metal palladium layer; the resistivity tester is connected with a computer.
In any of the above aspects, it is preferable that the autoclave body, the hydrogen line, the nitrogen line, the exhaust line, and the hydrogen passage are integrally formed and are each made of a stainless steel material; the length, width and height of the autoclave body are all 1m, and the wall thickness of the autoclave body is 5cm; the outer diameter of the hydrogen channel is 150mm, the thickness of the side wall is 5-10mm, and the wall thickness of the right end is 10-15mm; the diameters of the inner gasket and the outer gasket are 50mm, and the inner gasket, the outer gasket and the annular gasket are made of polytetrafluoroethylene materials; the diameter of the through hole is 30mm, the diameter of the round hole is 5mm, and the center-to-center distance between the two round holes is 20mm; the test sample is a nickel-based superalloy with a diameter of 50mm and a thickness of 0.1-0.2mm, and the metallic palladium layer has a thickness of 3-5 μm.
The invention also provides a measuring method of the nickel-base superalloy hydrogen diffusion coefficient based on resistivity, which uses the measuring device of the nickel-base superalloy hydrogen diffusion coefficient based on resistivity according to any one of the above, and comprises the following steps in sequence:
step one: cutting a nickel-based superalloy test sample according to design requirements, and polishing two surfaces of the test sample by sequentially using 400# abrasive paper, 800# abrasive paper and 2000# abrasive paper; after polishing is finished, respectively performing rough polishing and fine polishing on the two surfaces of the test sample by using diamond polishing liquid and silicon dioxide polishing liquid to the degree of mirror surface, so that the two surfaces are bright and have no scratches; after polishing is finished, placing the test sample into absolute ethyl alcohol for ultrasonic cleaning, and then electroplating a metal palladium layer on one surface of the test sample;
step two: sequentially placing the outer gasket, the test sample plated with the metal palladium layer and the inner gasket at the bottom of the sleeve, enabling the metal palladium layer to face one side of the outer gasket, simultaneously placing the annular gasket into the sleeve along the inner wall of the sleeve, sleeving the sleeve on the hydrogen channel, and screwing the inner flange and the outer flange by using fastening screws, wherein the central axes of the hydrogen channel, the inner gasket, the test sample, the outer gasket and the sleeve are positioned on the same straight line; respectively inserting two test chucks into two round holes on the outer gasket, and applying pretightening force through a fixed spring to enable the test chucks to be in close contact with the metal palladium layer; the hydrogen pipeline, the nitrogen pipeline and the exhaust pipeline are respectively connected to a high-pressure hydrogen cylinder, a high-pressure nitrogen cylinder and a gas recovery cylinder, and the resistivity tester is connected to a computer;
step three: opening a nitrogen valve and an exhaust valve, and introducing nitrogen into the measuring device to discharge air in the measuring device into the gas recovery bottle;
step four: keeping the exhaust valve in an open state, closing the nitrogen valve, opening the hydrogen valve, and introducing hydrogen into the measuring device to discharge the nitrogen in the measuring device into the gas recovery bottle; closing the exhaust valve, continuously introducing hydrogen into the measuring device to the target hydrogen pressure, and then closing the hydrogen valve, wherein the whole measuring device is in a sealing state;
step five: turning on a resistivity tester, adjusting the test current, resetting the measured data after the resistivity measured value is stable, and starting formal test, wherein a curve of test time and resistivity is recorded on a computer in real time; when hydrogen permeates into the metal palladium layer, the resistivity tends to increase rapidly, the corresponding test time when the resistivity increases by 1% is recorded, and the hydrogen diffusion coefficient of the test sample is obtained according to a calculation formula of the hydrogen diffusion coefficient;
step six: repeating the steps one to seven at least three times, and taking the average value of the test results of the plurality of times to obtain the nickel-based superalloy hydrogen diffusion coefficient based on resistivity.
Preferably, in the third step, the flow rate of the nitrogen gas introduced into the measuring device is 10-15L/min, and the time of introducing the nitrogen gas is 3-5min.
In any of the above schemes, preferably, in the fourth step, the flow rate of the hydrogen gas introduced into the measuring device is 10-15L/min, and the time of the hydrogen gas introduced is 3-5min; continuously introducing hydrogen into the measuring device at a flow rate of 10-15L/min and a target hydrogen pressure of 0.1-1MPa.
In any of the above schemes, preferably, in the fifth step, the test current is 1 μA-10mA; the calculation formula of the hydrogen diffusion coefficient isWherein:
-the test time corresponding to a 1% increase in resistivity, s;
-thickness of test sample, mm;
hydrogen diffusion coefficient of test sample, mm 2 /s。
The high-pressure hydrogen cylinder, the high-pressure nitrogen cylinder, the gas recovery cylinder, the valve, the pressure gauge, the resistivity tester and the like used in the invention can be selected from the existing test equipment and components according to actual conditions, and no special requirements are made on the type number. The invention electroplates a metal palladium layer on the surface of the test sample, the electroplating process and electroplating parameters can be adjusted according to the actual situation, and no special requirement is made for specific parameter values.
In the invention, a hydrogen pipeline is connected with a high-pressure hydrogen cylinder with a pressure reducing valve, hydrogen is controlled to be introduced into the high-pressure kettle body from the high-pressure hydrogen cylinder through a hydrogen valve, a nitrogen pipeline is connected with a high-pressure nitrogen cylinder with the pressure reducing valve, and nitrogen is controlled to be introduced into the high-pressure kettle body from the high-pressure nitrogen cylinder through a nitrogen valve for purging before testing. The first pressure gauge and the second pressure gauge are used for measuring the pressure inside the autoclave body and guaranteeing the accuracy of a hydrogen pressure measurement result. The inner gasket and the outer gasket are respectively arranged on two sides of the test sample, and the annular gasket is arranged on the inner wall of the sleeve for sealing and insulation. The center of the inner gasket is provided with a larger through hole, so that the hydrogen is ensured to be fully contacted with the hydrogen charging surface of the test sample, and the outer gasket is provided with two smaller round holes for the test chuck to contact with the metal palladium layer of the hydrogen escaping surface of the test sample, and the resistivity is measured.
The device and the method for measuring the hydrogen diffusion coefficient of the nickel-based superalloy based on resistivity have the following beneficial effects:
(1) The invention designs a brand new hydrogen diffusion coefficient measuring device and a measuring method based on resistivity, wherein the measuring principle is that the metal palladium has strong adsorption effect on hydrogen element, the resistivity of the metal palladium is greatly different from that of the nickel-based superalloy, the resistivity of the metal palladium is far lower than that of the nickel-based superalloy, the change of the resistivity of the metal palladium after adsorbing hydrogen element is sensitive, and the hydrogen diffusion coefficient of the nickel-based superalloy can be simply and efficiently measured.
(2) Compared with an electrochemical test method, the invention changes the nickel plating layer into the palladium plating layer which is more sensitive to hydrogen element, has simple measuring device, convenient measuring method and low cost. The nickel plating layer is mainly used for preventing the test sample from oxidizing, and the palladium plating layer is mainly used for adsorbing hydrogen element.
(3) The invention can rapidly determine the hydrogen diffusion coefficient after the hydrogen permeation is completed, and has the advantages of high response speed and reliable and accurate test result.
Drawings
FIG. 1 is a schematic structural view of a preferred embodiment of a device for measuring hydrogen diffusion coefficient of a nickel-base superalloy based on resistivity according to the present invention;
FIG. 2 is a front view of the measuring device of the embodiment shown in FIG. 1;
FIG. 3 is a schematic view of the connection assembly of the embodiment shown in FIG. 1;
fig. 4 is a cross-sectional view of the connection assembly of the embodiment of fig. 1.
The reference numerals in the drawings indicate:
1-high pressure assembly, 101-autoclave body, 102-hydrogen pipeline, 103-hydrogen valve, 104-first pressure gauge, 105-nitrogen pipeline, 106-nitrogen valve, 107-second pressure gauge, 108-exhaust pipeline, 109-exhaust valve;
2-connecting components, 201-hydrogen channels, 202-sleeves, 203-inner flanges, 204-outer flanges, 205-fastening screws, 206-inner gaskets, 207-outer gaskets, 208-annular gaskets, 209-through holes and 210-round holes;
3-resistivity testing components, 301-resistivity testers, 302-electrode wires, 303-testing chucks, 304-fixed springs;
4-test sample.
Detailed Description
For a further understanding of the present invention, the present invention will be described in detail with reference to the following examples.
Embodiment one:
as shown in fig. 1 to 4, a preferred embodiment of the measuring device for the hydrogen diffusion coefficient of the nickel-based superalloy based on the resistivity according to the present invention comprises a high voltage component 1, a connecting component 2 and a resistivity testing component 3 which are sequentially connected from left to right, wherein a test sample 4 is installed in the connecting component 2, and a hydrogen escaping surface of the test sample 4 is plated with a metallic palladium layer.
The high-pressure assembly 1 comprises an autoclave body 101, a hydrogen pipeline 102, a hydrogen valve 103, a first pressure gauge 104, a nitrogen pipeline 105, a nitrogen valve 106, a second pressure gauge 107, an exhaust pipeline 108 and an exhaust valve 109; the left side of the autoclave body 101 is provided with the hydrogen pipeline 102 and the nitrogen pipeline 105, the hydrogen pipeline 102 is provided with the hydrogen valve 103 and the first pressure gauge 104, and the nitrogen pipeline 105 is provided with the nitrogen valve 106 and the second pressure gauge 107; the top of the autoclave body 101 is provided with the exhaust pipeline 108, and the exhaust valve 109 is arranged on the exhaust pipeline 108; the hydrogen pipeline 102 is connected with a high-pressure hydrogen cylinder, the nitrogen pipeline 105 is connected with a high-pressure nitrogen cylinder, and the exhaust pipeline 108 is connected with a gas recovery cylinder.
The connection assembly 2 comprises a hydrogen channel 201, a sleeve 202, an inner flange 203, an outer flange 204, fastening screws 205, an inner gasket 206, an outer gasket 207 and an annular gasket 208; the left end of the hydrogen channel 201 is arranged on the right side of the autoclave body 101, and the right end of the hydrogen channel 201 is embedded into the sleeve 202; the inner flange 203 is arranged on the outer side of the hydrogen channel 201, the outer flange 204 is arranged on the outer side of the sleeve 202, and the inner flange 203 and the outer flange 204 are fixedly connected through six fastening screws 205; the center part of the right end of the hydrogen channel 201, the center part of the inner gasket 206 and the center part of the bottom of the sleeve 202 are all provided with through holes 209, the diameters of the three through holes 209 are equal, and the central axes of the three through holes 209 are on the same straight line; the outer washer 207 is symmetrically provided with two round holes 210 at both sides of the center point thereof.
The annular gasket 208 is arranged between the outer wall of the hydrogen channel 201 and the inner wall of the sleeve 202, the inner gasket 206 and the outer gasket 207 are sequentially arranged between the central part of the right end of the hydrogen channel 201 and the central part of the bottom of the sleeve 202 from left to right, the test sample 4 is arranged between the inner gasket 206 and the outer gasket 207, the metal palladium layer faces one side of the outer gasket 207, and the central axes of the inner gasket 206, the outer gasket 207 and the test sample 4 are positioned on the same straight line.
The resistivity testing assembly 3 comprises a resistivity tester 301, two electrode wires 302, two testing chucks 303 and two fixing springs 304; one end of the electrode wire 302 is connected with the test chuck 303, the other end of the electrode wire 302 is connected with the resistivity tester 301, and the test chuck 303 is provided with the fixed spring 304; the two test chucks 303 are respectively inserted into the two round holes 210 and are contacted with the metal palladium layer; the resistivity tester 301 is connected with a computer.
The autoclave body 101, the hydrogen line 102, the nitrogen line 105, the exhaust line 108 and the hydrogen passage 201 are integrally formed and are made of stainless steel materials; the length, width and height of the autoclave body 101 are all 1m, and the wall thickness of the autoclave body 101 is 5cm; the outer diameter of the hydrogen channel 201 is 150mm, the thickness of the side wall is 8mm, and the wall thickness of the right end is 12mm; the diameters of the inner gasket 206 and the outer gasket 207 are 50mm, and the inner gasket 206, the outer gasket 207 and the annular gasket 208 are all made of polytetrafluoroethylene materials; the diameter of the through hole 209 is 30mm, the diameter of the round hole 210 is 5mm, and the center-to-center distance between the two round holes 210 is 20mm; the test sample 4 is a nickel-based superalloy with a diameter of 50mm and a thickness of 0.15mm, and the metallic palladium layer has a thickness of 4 μm.
The embodiment also provides a method for measuring the hydrogen diffusion coefficient of the nickel-base superalloy based on resistivity, which comprises the following steps in sequence:
step one: cutting a nickel-based superalloy test sample according to design requirements, and polishing two surfaces of the test sample by sequentially using 400# abrasive paper, 800# abrasive paper and 2000# abrasive paper; after polishing is finished, respectively performing rough polishing and fine polishing on the two surfaces of the test sample by using diamond polishing liquid and silicon dioxide polishing liquid to the degree of mirror surface, so that the two surfaces are bright and have no scratches; after polishing is finished, placing the test sample into absolute ethyl alcohol for ultrasonic cleaning, and then electroplating a metal palladium layer on one surface of the test sample;
step two: sequentially placing the outer gasket, the test sample plated with the metal palladium layer and the inner gasket at the bottom of the sleeve, enabling the metal palladium layer to face one side of the outer gasket, simultaneously placing the annular gasket into the sleeve along the inner wall of the sleeve, sleeving the sleeve on the hydrogen channel, and screwing the inner flange and the outer flange by using fastening screws, wherein the central axes of the hydrogen channel, the inner gasket, the test sample, the outer gasket and the sleeve are positioned on the same straight line; respectively inserting two test chucks into two round holes on the outer gasket, and applying pretightening force through a fixed spring to enable the test chucks to be in close contact with the metal palladium layer; the hydrogen pipeline, the nitrogen pipeline and the exhaust pipeline are respectively connected to a high-pressure hydrogen cylinder, a high-pressure nitrogen cylinder and a gas recovery cylinder, and the resistivity tester is connected to a computer;
step three: opening a nitrogen valve and an exhaust valve, and introducing nitrogen into the measuring device to discharge air in the measuring device into the gas recovery bottle;
step four: keeping the exhaust valve in an open state, closing the nitrogen valve, opening the hydrogen valve, and introducing hydrogen into the measuring device to discharge the nitrogen in the measuring device into the gas recovery bottle; closing the exhaust valve, continuously introducing hydrogen into the measuring device to the target hydrogen pressure, and then closing the hydrogen valve, wherein the whole measuring device is in a sealing state;
step five: turning on a resistivity tester, adjusting the test current, resetting the measured data after the resistivity measured value is stable, and starting formal test, wherein a curve of test time and resistivity is recorded on a computer in real time; when hydrogen permeates into the metal palladium layer, the resistivity tends to increase rapidly, the corresponding test time when the resistivity increases by 1% is recorded, and the hydrogen diffusion coefficient of the test sample is obtained according to a calculation formula of the hydrogen diffusion coefficient;
step six: repeating the steps one to seven at least three times, and taking the average value of the test results of the plurality of times to obtain the nickel-based superalloy hydrogen diffusion coefficient based on resistivity.
And thirdly, introducing nitrogen into the measuring device for 4min at a flow rate of 12L/min.
In the fourth step, the flow rate of the hydrogen gas introduced into the measuring device is 12L/min, and the time of the hydrogen gas introduced is 4min; continuously introducing hydrogen into the measuring device at a flow rate of 12L/min and a target hydrogen pressure of 0.5MPa.
In the fifth step, the test current is 5mA; the calculation formula of the hydrogen diffusion coefficient isWherein:
-the test time corresponding to a 1% increase in resistivity, s;
-thickness of test sample, mm;
hydrogen diffusion coefficient of test sample, mm 2 /s。
The high-pressure hydrogen cylinder, the high-pressure nitrogen cylinder, the gas recovery cylinder, the valve, the pressure gauge, the resistivity tester and the like used in the embodiment can be selected from the existing test equipment and components according to actual conditions, and no special requirements are made on type numbers. In this embodiment, a metal palladium layer is electroplated on the surface of the test sample, and the electroplating process and electroplating parameters used can be adjusted according to actual conditions, so that no special requirement is made on specific parameter values.
In this embodiment, the hydrogen pipeline is connected with the high-pressure hydrogen bottle that has the relief pressure valve, passes through the hydrogen valve and controls hydrogen and lets in the autoclave body by the high-pressure hydrogen bottle, and the nitrogen pipeline is connected with the high-pressure nitrogen bottle that has the relief pressure valve, passes through the nitrogen valve and controls nitrogen and lets in the autoclave body by the high-pressure nitrogen bottle for the sweep before the test. The first pressure gauge and the second pressure gauge are used for measuring the pressure inside the autoclave body and guaranteeing the accuracy of a hydrogen pressure measurement result. The inner gasket and the outer gasket are respectively arranged on two sides of the test sample, and the annular gasket is arranged on the inner wall of the sleeve for sealing and insulation. The center of the inner gasket is provided with a larger through hole, so that the hydrogen is ensured to be fully contacted with the hydrogen charging surface of the test sample, and the outer gasket is provided with two smaller round holes for the test chuck to contact with the metal palladium layer of the hydrogen escaping surface of the test sample, and the resistivity is measured.
The device and the method for measuring the hydrogen diffusion coefficient of the nickel-based superalloy based on resistivity have the following beneficial effects:
(1) The measurement principle is that the metal palladium has strong adsorption effect on hydrogen element, the resistivity of the metal palladium is greatly different from that of the nickel-based superalloy, the resistivity of the metal palladium is far lower than that of the nickel-based superalloy, the change of the resistivity of the metal palladium after adsorbing hydrogen element is sensitive, and the hydrogen diffusion coefficient of the nickel-based superalloy can be simply and efficiently measured; (2) The nickel plating layer is changed into the palladium plating layer which is more sensitive to hydrogen, the measuring device is simple, the measuring method is convenient and quick, and the cost is low. The nickel plating layer is mainly used for preventing the test sample from oxidizing, and the palladium plating layer is mainly used for adsorbing hydrogen element; (3) The hydrogen diffusion coefficient can be rapidly measured after the hydrogen permeation is completed, the response speed is high, and the test result is reliable and accurate.
Embodiment two:
according to another preferred embodiment of the device and method for measuring hydrogen diffusion coefficient of nickel-base superalloy based on resistivity of the present invention, the structure, measuring steps, used equipment, technical principle and beneficial effects of the measuring device are basically the same as those of the first embodiment, except that:
the outer diameter of the hydrogen channel is 150mm, the thickness of the side wall is 5mm, and the wall thickness of the right end is 10mm; the test sample is a nickel-based superalloy with a diameter of 50mm and a thickness of 0.1mm, and the metallic palladium layer has a thickness of 3 μm.
And thirdly, introducing nitrogen into the measuring device for 5min at a flow rate of 10L/min.
In the fourth step, the flow rate of the hydrogen gas introduced into the measuring device is 10L/min, and the time of the hydrogen gas introduced is 5min; continuously introducing hydrogen into the measuring device at a flow rate of 10L/min and a target hydrogen pressure of 1MPa.
In step five, the test current was 1. Mu.A.
Embodiment III:
according to another preferred embodiment of the device and method for measuring hydrogen diffusion coefficient of nickel-base superalloy based on resistivity of the present invention, the structure, measuring steps, used equipment, technical principle and beneficial effects of the measuring device are basically the same as those of the first embodiment, except that:
the outer diameter of the hydrogen channel is 150mm, the thickness of the side wall is 10mm, and the wall thickness of the right end is 15mm; the test sample is a nickel-based superalloy with a diameter of 50mm and a thickness of 0.2mm, and the metallic palladium layer has a thickness of 5 μm.
And thirdly, introducing nitrogen into the measuring device for 3min at a flow rate of 15L/min.
In the fourth step, the flow rate of the hydrogen gas introduced into the measuring device is 15L/min, and the time of the hydrogen gas introduced is 3min; the flow rate of the hydrogen continuously introduced into the measuring device was 15L/min, and the target hydrogen pressure was 0.1MPa.
In the fifth step, the test current was 10mA.
The specific description is as follows: the technical scheme of the invention relates to a plurality of parameters, and the beneficial effects and remarkable progress of the invention can be obtained by comprehensively considering the synergistic effect among the parameters. In addition, the value ranges of all the parameters in the technical scheme are obtained through a large number of tests, and aiming at each parameter and the mutual combination of all the parameters, the inventor records a large number of test data, and the specific test data are not disclosed herein for a long period of time.
It will be appreciated by those skilled in the art that the resistivity-based nickel-base superalloy hydrogen diffusion coefficient determination apparatus and method of the present invention includes any combination of the above-described aspects of the present invention and the detailed description of the invention and the various components shown in the drawings, and is limited in length and does not describe each of these combinations for simplicity of the description. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The utility model provides a measuring device based on nickel base superalloy hydrogen diffusion coefficient of resistivity which characterized in that: the device comprises a high-voltage assembly, a connecting assembly and a resistivity testing assembly which are sequentially connected from left to right, wherein a test sample is installed in the connecting assembly, and a metal palladium layer is electroplated on the hydrogen escaping surface of the test sample;
the high-pressure assembly comprises an autoclave body, a hydrogen pipeline, a hydrogen valve, a first pressure gauge, a nitrogen pipeline, a nitrogen valve, a second pressure gauge, an exhaust pipeline and an exhaust valve; the left side of the autoclave body is provided with the hydrogen pipeline and the nitrogen pipeline, the hydrogen pipeline is provided with the hydrogen valve and the first pressure gauge, and the nitrogen pipeline is provided with the nitrogen valve and the second pressure gauge; the top of the autoclave body is provided with the exhaust pipeline, and the exhaust pipeline is provided with the exhaust valve; the hydrogen pipeline is connected with a high-pressure hydrogen cylinder, the nitrogen pipeline is connected with a high-pressure nitrogen cylinder, and the exhaust pipeline is connected with a gas recovery cylinder;
the connecting component comprises a hydrogen channel, a sleeve, an inner flange, an outer flange, fastening screws, an inner gasket, an outer gasket and an annular gasket; the left end of the hydrogen channel is arranged on the right side of the autoclave body, and the right end of the hydrogen channel is embedded into the sleeve; the inner flange is arranged at the outer side of the hydrogen channel, the outer flange is arranged at the outer side of the sleeve, and the inner flange and the outer flange are fixedly connected through six fastening screws; the center part of the right end of the hydrogen channel, the center part of the inner gasket and the center part of the bottom of the sleeve are all provided with through holes, the diameters of the three through holes are equal, and the central axes of the three through holes are positioned on the same straight line; two circular holes are symmetrically formed in the two sides of the center point of the outer gasket;
the resistivity testing assembly comprises a resistivity tester, two electrode wires, two testing chucks and two fixing springs; one end of the electrode wire is connected with the test chuck, the other end of the electrode wire is connected with the resistivity tester, and the test chuck is provided with the fixed spring; the two test chucks are respectively inserted into the two round holes and are contacted with the metal palladium layer; the resistivity tester is connected with a computer;
the method for measuring the hydrogen diffusion coefficient of the nickel-based superalloy based on resistivity comprises the following steps in sequence:
step one: cutting a nickel-based superalloy test sample according to design requirements, and polishing two surfaces of the test sample by sequentially using 400# abrasive paper, 800# abrasive paper and 2000# abrasive paper; after polishing is finished, respectively performing rough polishing and fine polishing on the two surfaces of the test sample by using diamond polishing liquid and silicon dioxide polishing liquid to the degree of mirror surface, so that the two surfaces are bright and have no scratches; after polishing is finished, placing the test sample into absolute ethyl alcohol for ultrasonic cleaning, and then electroplating a metal palladium layer on one surface of the test sample;
step two: sequentially placing the outer gasket, the test sample plated with the metal palladium layer and the inner gasket at the bottom of the sleeve, enabling the metal palladium layer to face one side of the outer gasket, simultaneously placing the annular gasket into the sleeve along the inner wall of the sleeve, sleeving the sleeve on the hydrogen channel, and screwing the inner flange and the outer flange by using fastening screws, wherein the central axes of the hydrogen channel, the inner gasket, the test sample, the outer gasket and the sleeve are positioned on the same straight line; respectively inserting two test chucks into two round holes on the outer gasket, and applying pretightening force through a fixed spring to enable the test chucks to be in close contact with the metal palladium layer; the hydrogen pipeline, the nitrogen pipeline and the exhaust pipeline are respectively connected to a high-pressure hydrogen cylinder, a high-pressure nitrogen cylinder and a gas recovery cylinder, and the resistivity tester is connected to a computer;
step three: opening a nitrogen valve and an exhaust valve, and introducing nitrogen into the measuring device to discharge air in the measuring device into the gas recovery bottle;
step four: keeping the exhaust valve in an open state, closing the nitrogen valve, opening the hydrogen valve, and introducing hydrogen into the measuring device to discharge the nitrogen in the measuring device into the gas recovery bottle; closing the exhaust valve, continuously introducing hydrogen into the measuring device to the target hydrogen pressure, and then closing the hydrogen valve, wherein the whole measuring device is in a sealing state;
step five: turning on a resistivity tester, adjusting the test current, resetting the measured data after the resistivity measured value is stable, and starting formal test, wherein a curve of test time and resistivity is recorded on a computer in real time; when hydrogen permeates into the metal palladium layer, the resistivity tends to increase rapidly, the corresponding test time when the resistivity increases by 1% is recorded, and the hydrogen diffusion coefficient of the test sample is obtained according to a calculation formula of the hydrogen diffusion coefficient;
step six: repeating the steps one to five for at least three times, and taking the average value of the test results of the plurality of times to obtain the nickel-based superalloy hydrogen diffusion coefficient based on resistivity.
2. The device for measuring hydrogen diffusion coefficient of a nickel-base superalloy based on resistivity according to claim 1, wherein: the annular gasket is arranged between the outer wall of the hydrogen channel and the inner wall of the sleeve, the inner gasket and the outer gasket are sequentially arranged between the central part of the right end of the hydrogen channel and the central part of the bottom of the sleeve from left to right, the test sample is installed between the inner gasket and the outer gasket, the metal palladium layer faces one side of the outer gasket, and the central axes of the inner gasket, the outer gasket and the test sample are positioned on the same straight line.
3. The device for measuring hydrogen diffusion coefficient of a nickel-base superalloy based on resistivity according to claim 2, wherein: the autoclave body, the hydrogen pipeline, the nitrogen pipeline, the exhaust pipeline and the hydrogen channel are integrally formed and are made of stainless steel materials; the length, width and height of the autoclave body are all 1m, and the wall thickness of the autoclave body is 5cm; the outer diameter of the hydrogen channel is 150mm, the thickness of the side wall is 5-10mm, and the wall thickness of the right end is 10-15mm; the diameters of the inner gasket and the outer gasket are 50mm, and the inner gasket, the outer gasket and the annular gasket are made of polytetrafluoroethylene materials; the diameter of the through hole is 30mm, the diameter of the round hole is 5mm, and the center-to-center distance between the two round holes is 20mm; the test sample is a nickel-based superalloy with a diameter of 50mm and a thickness of 0.1-0.2mm, and the metallic palladium layer has a thickness of 3-5 μm.
4. The apparatus for measuring hydrogen diffusion coefficient of a nickel-base superalloy based on resistivity according to claim 3, wherein: and thirdly, introducing nitrogen into the measuring device at a flow rate of 10-15L/min for 3-5min.
5. The device for measuring hydrogen diffusion coefficient of a nickel-base superalloy based on resistivity according to claim 4, wherein: in the fourth step, the flow rate of the hydrogen gas introduced into the measuring device is 10-15L/min, and the time of the hydrogen gas introduced is 3-5min; continuously introducing hydrogen into the measuring device at a flow rate of 10-15L/min and a target hydrogen pressure of 0.1-1MPa.
6. The electrical-based of claim 5The device for measuring the hydrogen diffusion coefficient of the nickel-based superalloy with the resistivity is characterized in that: in the fifth step, the test current is 1 mu A-10mA; the calculation formula of the hydrogen diffusion coefficient isIn which, in the process,
-the test time corresponding to a 1% increase in resistivity, s;
-thickness of test sample, mm;
hydrogen diffusion coefficient of test sample, mm 2 /s。
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