CN115825371A - Device and method for measuring hydrogen content in metal - Google Patents
Device and method for measuring hydrogen content in metal Download PDFInfo
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- CN115825371A CN115825371A CN202211554776.9A CN202211554776A CN115825371A CN 115825371 A CN115825371 A CN 115825371A CN 202211554776 A CN202211554776 A CN 202211554776A CN 115825371 A CN115825371 A CN 115825371A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 108
- 239000002184 metal Substances 0.000 title claims abstract description 108
- 239000001257 hydrogen Substances 0.000 title claims abstract description 56
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 56
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000007789 sealing Methods 0.000 claims abstract description 31
- 238000012360 testing method Methods 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 10
- 238000002844 melting Methods 0.000 claims abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 32
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 22
- 229910052802 copper Inorganic materials 0.000 claims description 22
- 239000010949 copper Substances 0.000 claims description 22
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 229910000831 Steel Inorganic materials 0.000 claims description 13
- 239000010959 steel Substances 0.000 claims description 13
- 229910045601 alloy Inorganic materials 0.000 claims description 11
- 239000000956 alloy Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 229910052582 BN Inorganic materials 0.000 claims description 6
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 229920001971 elastomer Polymers 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002379 silicone rubber Polymers 0.000 claims description 3
- 229920001973 fluoroelastomer Polymers 0.000 claims description 2
- 239000004809 Teflon Substances 0.000 claims 2
- 229920006362 Teflon® Polymers 0.000 claims 2
- 238000005259 measurement Methods 0.000 abstract description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
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Abstract
The invention provides a device and a method for measuring hydrogen content in metal, and relates to the technical field of hydrogen measurement sensing; the device comprises a metal melt sampler, a sealed container, a thermocouple, a sealing ring, a sealing cover, a gas circuit, an electromagnetic valve, a pressure transmitter, a three-way valve, a vacuum pump and a controller; the metal melting point is firstly tested through the thermocouple, then the hydrogen content is calculated, the melting point and the hydrogen content of the metal can be simultaneously tested, and according to the tested melting point, after the metal generates a blank shell, the pressure is reduced, so that the hydrogen is prevented from being separated out and entering a gas phase, and the testing accuracy is improved.
Description
Technical Field
The invention relates to the technical field of hydrogen measurement sensing, in particular to a device and a method for measuring hydrogen content in metal.
Background
Hydrogen is a harmful impurity in metal, the hydrogen saturation solubility of liquid-phase metal is higher than that of solid phase, and in the process of metal melt solidification, hydrogen tends to be separated out from the metal melt, so that the metal is internally loosened, irregular pores are generated, and the metal generates hydrogen-induced defects, so that the mechanical property or the physicochemical property of the metal is remarkably reduced, and the characteristics of the metal in the aspects of compactness, fatigue limit, strength, plasticity, corrosion resistance, electrical conductivity, thermal conductivity and the like are greatly influenced. Therefore, there is a need to rapidly test the hydrogen content in aluminum during production to control product quality.
The decompression solidifying method is one hydrogen measuring method commonly used in metal material production, and includes sampling liquid metal, setting the sampled liquid metal inside sealed container, and vacuum pumping to solidify the liquid metal sample gradually under negative pressure. Due to the poor saturation solubility of hydrogen in solid-liquid phase metal and the driving of negative pressure, hydrogen in the metal is separated out in the process of melt solidification, so that a solidified metal sample generates pores, and the porosity of a test sample can represent the content of hydrogen in aluminum. However, before the metal solidifies, the hydrogen evolved can bubble into the gas phase, resulting in inaccurate testing.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a device and a method for measuring the hydrogen content in metal, so as to prevent hydrogen from entering into gas phase and accurately measure the hydrogen content in metal.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in one aspect, the present invention provides an apparatus for measuring the hydrogen content of a metal, the apparatus comprising:
the device comprises a metal melt sampler, a sealed container, a thermocouple, a sealing ring, a sealing cover, a gas circuit, an electromagnetic valve, a pressure transmitter, a three-way valve, a vacuum pump and a controller; wherein, the metal melt sampler is arranged in a sealed container, and the top of the sealed container is provided with a sealing ring and covers an openable sealing cover; the bottom of the metal melt sampler is provided with a groove which is tightly contacted with a thermocouple test point fixed at the bottom of the sealed container; the sealed container is connected with the vacuum pump through the gas circuit and the three-way valve, and is also connected with the pressure transmitter through the electromagnetic valve, and the controller is used for collecting thermoelectric even data, controlling the on-off of the electromagnetic valve and adjusting and controlling the vacuum degree of the decompression container.
The material of the metal melt sampler is one of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel and alloys of a plurality of the copper and the nickel.
When the metal melt sampler is one or more of corundum, steel, copper and nickel and alloy thereof, the surface of the metal melt sampler is coated with a boron nitride release agent.
The material of the sealed container is one of steel, copper and nickel and the alloy of a plurality of the steel, the copper and the nickel.
The material of the sealing rubber ring is one of silicon rubber, fluorine rubber and polytetrafluoroethylene.
The thermocouple is a K-type thermocouple with a contact test point exposed and leaked.
The sealing cover is made of one of steel, copper and nickel and alloy thereof, polytetrafluoroethylene, glass and quartz.
The air path is made of one of stainless steel, copper and polytetrafluoroethylene.
The three-way valve is a three-way vacuum ball valve and is made of one of stainless steel, copper and nylon.
In another aspect, the present invention provides a method for measuring hydrogen content in a metal, which is implemented by using the apparatus for measuring hydrogen content in a metal, and includes the following steps:
s1: opening the sealing cover, and preheating the metal melt sampler;
s2: adjusting the three-way valve to a state that the vacuum pump is connected with the sealed container, closing the electromagnetic valve and opening the vacuum valve;
s3: placing a metal melt sampler for containing a metal melt sample into a sealed container, wherein the bottom of the metal melt sampler is tightly contacted with a thermocouple, and closing a sealing cover;
s4: acquiring a thermocouple temperature signal by using a controller, recording the temperature when the change of the temperature along with time is less than or equal to a first set threshold, and determining the temperature as the melting point of the metal to be measured;
s5: taking out the metal melt sampler, pouring out a metal sample, and carrying out secondary preheating on the metal melt sampler;
s6: adopting a preheated metal melt sampler to contain a metal melt sample, placing the sampled sampler into a sealed container, enabling the bottom of the sampler to be in close contact with a thermocouple, and closing a sealing cover;
s7: acquiring a thermocouple temperature signal by using a controller;
s8: after the temperature of the metal melt sample is reduced to the melting point, starting a vacuum pump, and closing the electromagnetic valve when the vacuum degree measured by the pressure transmitter is lower than a second set threshold value; when the vacuum degree is higher than a second set threshold value, the electromagnetic valve is opened;
s9: after the sample is solidified, taking out the sample, testing the relative density of the sample, and calculating the porosity and the hydrogen content of the metal sample, wherein the calculation process is as shown in the formula (1) and the formula (2):
L＝1-A (1)
wherein L is porosity, A is relative density, x is hydrogen content in metal, f (x) is porosity of solidified sample, M P Is the solubility of hydrogen in the metal, G C To increase the control constant, L P For testing the minimum porosity, P, of a sample to be tested under a certain pressure I The maximum transition point of the relationship between the porosity and the hydrogen content of the solidified sample, and r is the average transition point of the relationship between the porosity and the hydrogen content of the solidified sample.
Preheating the metal melt sampler to 600-900 ℃.
The first set threshold is 0.2 ℃/sec.
The second set threshold is 2.0kPa with a tolerance of + -0.2 kPa.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the invention provides a device and a method for measuring hydrogen content in metal.
2. The invention provides a device and a method for measuring hydrogen content in metal, which can test the temperature of the metal through a thermocouple, and start decompression after the metal generates a blank shell according to the tested melting point, thereby avoiding hydrogen from being separated out and entering a gas phase and improving the test accuracy.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for measuring hydrogen content in metal according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for measuring hydrogen content in a metal according to an embodiment of the present invention;
the reference signs are: 1. the device comprises a metal melt sampler, 2, a metal sample, 3, a sealed container, 4, a thermocouple, 5, a sealing ring, 6, a sealing cover, 7, a gas circuit, 8, an electromagnetic valve, 9, a pressure transmitter, 10, a three-way valve, 11, a vacuum pump, 12 and a controller.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples.
In one aspect, the present embodiment provides an apparatus for measuring hydrogen content in metal, as shown in fig. 1, the apparatus comprising:
the device comprises a metal melt sampler 1, a metal sample 2, a sealed container 3, a thermocouple 4, a sealing ring 5, a sealing cover 6, a gas path 7, an electromagnetic valve 8, a pressure transmitter 9, a three-way valve 10, a vacuum pump 11 and a controller 12; wherein, the metal melt sampler 1 containing the metal sample 2 is arranged in a sealed container 3, and the top of the sealed container is provided with a 5 sealing ring 5 and covers an openable sealing cover 6; the bottom of the cover metal melt sampler 1 is provided with a groove which is tightly contacted with a test point of a thermocouple 4 fixed at the bottom of the sealed container 3; the sealed container 3 is connected with a vacuum pump 11 through a gas circuit 7 and a three-way valve 10, the sealed container 3 is also connected with a pressure transmitter 9 through an electromagnetic valve 8, and an application controller 12 collects thermoelectric even data, controls the on-off of the electromagnetic valve 8 and adjusts and controls the vacuum degree of the decompression container.
The material of the metal melt sampler 1 is one of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel and alloys of a plurality of the copper and the nickel.
When the metal melt sampler 1 is one or more of corundum, steel, copper and nickel and alloy thereof, the surface of the metal melt sampler is coated with a boron nitride release agent.
The material of the sealed container 3 is one of steel, copper and nickel and the alloy of a plurality of the copper and the nickel.
The thermocouple is a K-type thermocouple with a contact test point exposed and leaked.
The sealing ring 5 is made of one of silicon rubber, fluororubber and polytetrafluoroethylene.
The material of the sealing cover 6 is one of steel, copper, nickel and alloy thereof, polytetrafluoroethylene, glass and quartz.
The material of the gas circuit 7 is one of stainless steel, copper and polytetrafluoroethylene.
The electromagnetic valve 8 is a normally closed electromagnetic valve, and in this embodiment, a normally closed electromagnetic valve with a pressure range of 0 to 0.5Mpa is adopted.
The pressure transmitter 9 is a pressure transmitter, and in the present embodiment, a pressure transmitter having a range of 0 to 100kPa and an accuracy of 0.2% fs is used.
The three-way valve 10 is a three-way vacuum ball valve made of one of stainless steel, copper and nylon.
The vacuum pump 11 is a rotary vane vacuum pump.
The controller 12 is an industrial personal computer.
In another aspect, the present invention provides a method for measuring hydrogen content in metal, which is implemented by using the apparatus for measuring hydrogen content in metal, as shown in fig. 2, and includes the following steps:
s1: opening a sealing cover, and preheating a metal melt sampler to 600-900 ℃;
s2: adjusting the three-way valve to a state that the vacuum pump is connected with the sealed container, closing the electromagnetic valve and opening the vacuum valve;
s3: placing a metal melt sampler for containing a metal melt sample into a sealed container, wherein the bottom of the metal melt sampler is tightly contacted with a thermocouple, and closing a sealing cover;
s4: collecting a thermocouple temperature signal by using a controller, recording the temperature when the temperature changes less than or equal to 0.2 ℃/second along with the time, and determining the temperature as the melting point of the metal to be measured;
s5: taking out the metal melt sampler, pouring out a metal sample, and carrying out secondary preheating on the metal melt sampler;
s6: adopting a preheated metal melt sampler to contain a metal melt sample, placing the sampled sampler into a sealed container, enabling the bottom of the sampler to be in close contact with a thermocouple, and closing a sealing cover;
s7: acquiring a thermocouple temperature signal by using a controller;
s8: after the temperature of the metal melt sample is reduced to the melting point, starting a vacuum pump, and closing an electromagnetic valve when the vacuum degree measured by a pressure transmitter is lower than 2.0kPa +/-0.2 kPa; when the vacuum degree is higher than 2.0kPa +/-0.2 kPa, opening the electromagnetic valve;
s9: after the sample is solidified, taking out the sample, testing the relative density of the sample, and calculating the porosity and the hydrogen content of the metal sample, wherein the calculation process is shown as the formula (1) and the formula (2):
L＝1-A (1)
wherein L is porosity, A is relative density, x is hydrogen content in metal, f (x) is porosity of solidified sample, M P Is the solubility of hydrogen in the metal, G C To increase the control constant, L P For testing the minimum porosity, P, of a sample to be tested under a certain pressure I The maximum transition point of the relationship between the porosity and the hydrogen content of the solidified sample, and r is the average transition point of the relationship between the porosity and the hydrogen content of the solidified sample.
Claims (10)
1. An apparatus for measuring the hydrogen content of a metal, the apparatus comprising: the device comprises a metal melt sampler, a sealed container, a thermocouple, a sealing ring, a sealing cover, a gas circuit, an electromagnetic valve, a pressure transmitter, a three-way valve, a vacuum pump and a controller; wherein, the metal melt sampler is arranged in a sealed container, and the top of the sealed container is provided with a sealing ring and covers an openable sealing cover; the bottom of the metal melt sampler is provided with a groove which is in contact with a thermocouple test point fixed at the bottom of the sealed container; the sealed container is connected with the vacuum pump through the gas circuit and the three-way valve, and is also connected with the pressure transmitter through the electromagnetic valve, and the controller is used for collecting thermoelectric even data, controlling the on-off of the electromagnetic valve and adjusting and controlling the vacuum degree of the decompression container.
2. The apparatus of claim 1, wherein the metal melt sampler is made of one or more of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel.
3. The apparatus for measuring the hydrogen content in a metal according to claim 2, wherein the surface of the metal melt sampler is coated with a boron nitride release agent when the metal melt sampler is one of corundum, steel, copper and nickel, and alloys thereof.
4. The apparatus for measuring hydrogen content in metal according to claim 1, wherein the material of the hermetic container is one of steel, copper and nickel, and an alloy of a plurality thereof;
the sealing rubber ring is made of one of silicon rubber, fluororubber and polytetrafluoroethylene.
5. The apparatus for measuring hydrogen content in a metal according to claim 1, wherein said thermocouple is a type K thermocouple with a contact test point exposed.
6. The apparatus for measuring hydrogen content in metal according to claim 1, wherein the material of the sealing cap is one of steel, copper and nickel and their alloys, teflon, glass, and quartz.
7. The apparatus of claim 1, wherein the gas path is made of one of stainless steel, copper and teflon;
the three-way valve is a three-way vacuum ball valve and is made of one of stainless steel, copper and nylon.
8. A method for measuring the hydrogen content in a metal, which is implemented by using the apparatus for measuring the hydrogen content in a metal according to claim 1, comprising the steps of:
s1: opening a sealing cover, and preheating a metal melt sampler to 600-900 ℃;
s2: adjusting the three-way valve to a state that the vacuum pump is connected with the sealed container, closing the electromagnetic valve and opening the vacuum valve;
s3: placing a metal melt sampler for containing a metal melt sample into a sealed container, wherein the bottom of the metal melt sampler is tightly contacted with a thermocouple, and closing a sealing cover;
s4: acquiring a thermocouple temperature signal by using a controller, recording the temperature when the change of the temperature along with time is less than or equal to a first set threshold, and determining the temperature as the melting point of the metal to be measured;
s5: taking out the metal melt sampler, pouring out a metal sample, and carrying out secondary preheating on the metal melt sampler;
s6: adopting a preheated metal melt sampler to contain a metal melt sample, placing the sampled sampler into a sealed container, enabling the bottom of the sampler to be in close contact with a thermocouple, and closing a sealing cover;
s7: acquiring a thermocouple temperature signal by using a controller;
s8: after the temperature of the metal melt sample is reduced to the melting point, starting a vacuum pump, and closing an electromagnetic valve when the vacuum degree measured by a pressure transmitter is lower than a second set threshold value; when the vacuum degree is higher than a second set threshold value, the electromagnetic valve is opened;
s9: after the sample is solidified, taking out the sample, testing the relative density of the sample, and calculating the porosity and the hydrogen content of the metal sample, wherein the calculation process is as shown in the formula (1) and the formula (2):
L＝1-A(1)
wherein L is porosity, A is relative density, x is hydrogen content in metal, f (x) is porosity of solidified sample, M P Is the solubility of hydrogen in the metal, and is,G C to increase the control constant, L P For testing the minimum porosity, P, of a sample to be tested under a certain pressure I The maximum transition point of the relationship between the porosity and the hydrogen content of the solidified sample, and r is the average transition point of the relationship between the porosity and the hydrogen content of the solidified sample.
9. The apparatus according to claim 8, wherein the metal melt sampler is preheated to 600-900 ℃ and the first threshold is 0.2 ℃/sec.
10. The apparatus for measuring hydrogen content in a metal according to claim 8, wherein said second set threshold is 2.0kPa with a tolerance of ± 0.2kPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211554776.9A CN115825371A (en) | 2022-12-06 | 2022-12-06 | Device and method for measuring hydrogen content in metal |
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| CN202211554776.9A CN115825371A (en) | 2022-12-06 | 2022-12-06 | Device and method for measuring hydrogen content in metal |
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