CN115856055A - Device and method for measuring hydrogen content in magnesium melt - Google Patents
Device and method for measuring hydrogen content in magnesium melt Download PDFInfo
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- CN115856055A CN115856055A CN202211554812.1A CN202211554812A CN115856055A CN 115856055 A CN115856055 A CN 115856055A CN 202211554812 A CN202211554812 A CN 202211554812A CN 115856055 A CN115856055 A CN 115856055A
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000011777 magnesium Substances 0.000 title claims abstract description 80
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 80
- 239000001257 hydrogen Substances 0.000 title claims abstract description 72
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 72
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 98
- 238000007789 sealing Methods 0.000 claims abstract description 31
- 239000004020 conductor Substances 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000010439 graphite Substances 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 24
- 239000000919 ceramic Substances 0.000 claims abstract description 23
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 22
- 239000011230 binding agent Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000010935 stainless steel Substances 0.000 claims description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 9
- 239000000155 melt Substances 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 6
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 5
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 3
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 238000003487 electrochemical reaction Methods 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 229910001120 nichrome Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 abstract description 6
- 239000000523 sample Substances 0.000 abstract description 5
- 238000004880 explosion Methods 0.000 abstract description 4
- 238000002485 combustion reaction Methods 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000011540 sensing material Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 241000695274 Processa Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000004678 hydrides Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229910001392 phosphorus oxide Inorganic materials 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- VSAISIQCTGDGPU-UHFFFAOYSA-N tetraphosphorus hexaoxide Chemical compound O1P(O2)OP3OP1OP2O3 VSAISIQCTGDGPU-UHFFFAOYSA-N 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Abstract
The invention discloses a device and a method for measuring hydrogen content in magnesium melt, and relates to the technical field of hydrogen measurement sensing; the device comprises a proton conductor solid electrolyte sheet, an electrode to be detected, a reference electrode, a ceramic tube, a binder, an electrode lead to be detected, a reference electrode lead, a reference gas outlet, a first sealing element, a reference gas tube, a reference gas inlet, porous graphite, an explosion-proof gas tube, a second sealing element, an explosion-proof gas inlet and a voltmeter; accurately testing the hydrogen content in the magnesium melt; meanwhile, the probe assembly comprising the binder, the support and the sensing material can be prevented from reacting with the magnesium melt; the reaction between air inside or on the surface of the test device and the magnesium melt is prevented, and the oxidation, combustion and explosion of the magnesium melt are prevented.
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 magnesium melt.
Background
Hydrogen is a harmful element of metal materials, if the content of hydrogen in magnesium and magnesium alloys is high, the performances of plasticity, strength, fatigue life and the like of the materials are seriously reduced, and the content of hydrogen must be accurately tested in the production process so as to efficiently control hydrogen and improve the product quality. The existing hydrogen measurement method mainly comprises a sampling analysis method, a first bubble method, a closed cycle method, an electrochemical sensing method and the like, wherein the sampling analysis method has long sampling, sample preparation and test time and cannot meet the requirement of rapid hydrogen measurement of a production line; the first bubble method is to sample the liquid state of the production line, seal and reduce the pressure, and the pressure for generating the first hydrogen bubble can be regarded as the hydrogen partial pressure, so as to calculate the hydrogen content, but the vapor pressure of magnesium is higher, and the bubble can be generated, so that reading error is easy to generate, and the test is inaccurate; the closed cycle method needs to introduce inert gas into the magnesium melt to carry out measurement after hydrogen in magnesium is carried out, but magnesium can also be carried out, and the magnesium reacts with hydrogen to generate hydride, so that the measurement is inaccurate; the electrochemical sensing method can accurately test the hydrogen content in magnesium, but the connection of the hydrogen sensitive material and the probe needs to adopt a binding agent, wherein the solvent is mostly water glass or phosphate, silicon oxide or phosphorus oxide generated by decomposition is easy to react with magnesium to generate explosion, and if the hydrogen sensitive material is separated from magnesium melt by a porous material, air in the porous material is easy to react with magnesium to combust and explode in an initial state.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art, and provides a device and a method for measuring the hydrogen content in magnesium melt, which can prevent combustion and explosion in the test process, thereby safely and accurately testing the hydrogen content in magnesium.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
on one hand, the invention provides a device for measuring the hydrogen content in a magnesium melt, which comprises a proton conductor solid electrolyte sheet, a reference electrode, a ceramic tube, a binder, an electrode lead to be measured, a reference electrode lead, a reference gas outlet, a first sealing element, a reference gas tube, a reference gas inlet, porous graphite, an explosion-proof gas tube, a second sealing element, an explosion-proof gas inlet and a voltmeter;
the device comprises a proton conductor solid electrolyte sheet, a to-be-detected electrode, a reference electrode, a voltmeter and a power supply, wherein the to-be-detected electrode and the reference electrode are respectively loaded on two end faces of the proton conductor solid electrolyte sheet, and are respectively connected with a to-be-detected electrode lead and a reference electrode lead and then are connected to the voltmeter; a proton conductor solid electrolyte sheet and one end of a ceramic tube adopt a binder to seal a reference electrode in the middle; the other end of the ceramic tube is sealed by a first sealing piece with a reference gas outlet, the reference gas tube penetrates into the ceramic tube through the first sealing piece, and the reference gas inlet is arranged outside the first sealing piece; one end of the explosion-proof air pipe is connected with the porous graphite, and the other end of the explosion-proof air pipe is connected with a second sealing element with an explosion-proof air inlet; and the assembly of the proton conductor solid electrolyte sheet and the ceramic tube penetrates into the explosion-proof gas tube through the second sealing element, and the proton conductor solid electrolyte is positioned above the porous graphite.
The proton conductor solid electrolyte tube is made of a high-temperature perovskite type proton conductor.
The electrode to be detected and the reference electrode are one of porous Pt, au, ag, rh and Ni.
The lead of the electrode to be detected and the lead of the reference electrode are NiCr alloy or FeNiCr alloy.
The binder is Al 2 O 3 Based on an insulating ceramic binder.
The ceramic tube is made of one of corundum, magnesium oxide and zirconium dioxide.
The reference gas vent pipe is made of one of corundum, quartz and stainless steel.
The first sealing element and the second sealing element are made of one of polytetrafluoroethylene, nylon, copper and stainless steel.
The explosion-proof air pipe is made of stainless steel.
The porous graphite is graphite felt.
The voltmeter is a digital voltmeter.
The reference gas is hydrogen-argon standard gas or hydrogen-nitrogen standard gas.
The explosion-proof gas is carbon dioxide-sulfur fluoride mixed gas.
In another aspect, the present invention further provides a method for measuring hydrogen content in a magnesium melt, which is implemented by using the apparatus for measuring hydrogen content in a magnesium melt, and comprises the following steps:
s1: placing the device above the magnesium melt for preheating;
s2: the reference gas is introduced into the reference gas inlet, and the explosion-proof gas is introduced into the explosion-proof gas inlet;
s3: after aeration, the device is inserted into the magnesium melt, and the porous graphite is immersed into the melt;
s4: closing the explosion-proof gas, adopting a voltmeter to test the electromotive force of the device, and calculating the hydrogen content in the magnesium melt;
s5: after the test is finished, introducing the explosion-proof gas for the second time, pulling out the test device, closing the explosion-proof gas and the reference gas after the test device is naturally cooled to the set temperature,
the calculation of the hydrogen content in the magnesium melt comprises the following steps:
converting the concentration difference between the equilibrium hydrogen partial pressure of the magnesium melt and the hydrogen partial pressure of the reference gas into potential difference, wherein the electrochemical reaction is as shown in formula (1):
H 2 (reference) = H 2 (to be measured) (1)
Gibbs free energy of reaction Δ G is:
wherein R is a gas constant, T is a thermodynamic temperature,
for the partial pressure of hydrogen in the magnesium melt to be measured, is determined>
Is reference gas hydrogen partial pressure;
gibbs free energy Δ G, according to Nernst's equation, is shown in equation (2):
wherein E is concentration cell electromotive force, and F is Faraday constant;
according to the electromotive force, obtaining the hydrogen partial pressure of the magnesium melt
Calculation processAs shown in formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the specific law of Xihua as follows:
wherein S is 0 Is the saturated hydrogen content of the magnesium melt.
The device is arranged above the magnesium melt for preheating, and specifically comprises the following steps: the device is placed 2-10 cm above the magnesium melt for preheating.
And the specific time period of the ventilation is 10min.
The porous graphite is immersed into the melt, specifically at a position of 10-20 cm of the melt.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the invention provides a device and a method for measuring the hydrogen content in a magnesium melt, which can accurately measure the hydrogen content in the magnesium melt.
2. The invention provides a device and a method for measuring hydrogen content in magnesium melt, which can prevent a probe assembly comprising a binder, a support body and a sensing material from reacting with the magnesium melt.
3. The invention provides a device and a method for measuring the hydrogen content in a magnesium melt, which can prevent air reserved in the test device or on the surface from reacting with the magnesium melt and prevent the oxidation, combustion and explosion of the magnesium melt.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for measuring hydrogen content in a magnesium melt according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for measuring hydrogen content in a magnesium melt according to an embodiment of the present invention;
the reference signs are: 1. the device comprises a proton conductor solid electrolyte, 2 parts of an electrode to be detected, 3 parts of a reference electrode, 4 parts of a ceramic tube, 5 parts of a binder, 6 parts of a lead wire of the electrode to be detected, 7 parts of a lead wire of the reference electrode, 8 parts of a gas outlet of reference gas, 9 parts of sealing elements A,10 parts of a reference gas tube, 11 parts of a gas inlet of reference gas, 12 parts of porous graphite, 13 parts of an explosion-proof gas tube, 14 parts of a sealing element B,15 parts of an explosion-proof gas inlet and 16 parts of a voltmeter.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples.
On one hand, the embodiment provides a device for measuring hydrogen content in a magnesium melt, as shown in fig. 1, the device includes a proton conductor solid electrolyte sheet 1, an electrode to be measured 2, a reference electrode 3, a ceramic tube 4, a binder 5, an electrode lead 6 to be measured, a reference electrode lead 7, a reference gas outlet 8, a first sealing member 9, a reference gas tube 10, a reference gas inlet 11, porous graphite 12, an explosion-proof gas tube 13, a second sealing member 14, an explosion-proof gas inlet 15, and a voltmeter 16;
the two end faces of the proton conductor solid electrolyte sheet 1 are respectively loaded with a to-be-detected electrode 2 and a reference electrode 3, and the to-be-detected electrode 2 and the reference electrode 3 are respectively connected with a to-be-detected electrode lead 6 and a reference electrode lead 7 and then are connected to a voltmeter 16; a proton conductor solid electrolyte sheet 1 and one end of a ceramic tube 4 are sealed with a reference electrode 3 in the middle by a binder 5; the other end of the ceramic tube 4 is sealed by a first sealing element 9 with a reference gas outlet 8, a reference gas tube 10 penetrates into the ceramic tube 4 through the first sealing element 9, and a reference gas inlet 11 is arranged outside the first sealing element 9; one end of the explosion-proof air pipe 13 is connected with the porous graphite 12, and the other end is connected with a second sealing element 14 with an explosion-proof air inlet 15; the assembly of the proton conductor solid electrolyte 1 and the ceramic tube 4 penetrates into the explosion-proof gas tube 13 through the second sealing member 14, and the proton conductor solid electrolyte 1 is positioned above the porous graphite 12.
The proton conductor solid electrolyte tube 1 is made of a high-temperature perovskite type proton conductor.
The electrode to be measured 2 and the reference electrode 3 are one of porous Pt, au, ag, rh and Ni.
The lead 6 of the electrode to be measured and the lead 7 of the reference electrode are NiCr alloy or FeNiCr alloy.
The binder 5 is Al 2 O 3 Based on an insulating ceramic binder.
The ceramic tube 4 is made of one of corundum, magnesium oxide and zirconium dioxide.
The material of breather pipe is one of corundum, quartz and stainless steel.
The first sealing element 9 and the second sealing element 14 are made of one of polytetrafluoroethylene, nylon, copper and stainless steel.
The 13 explosion-proof air pipes are made of stainless steel.
The 12-hole graphite is graphite felt.
The 16 voltmeter is a digital voltmeter.
The reference gas is hydrogen-argon standard gas or hydrogen-nitrogen standard gas.
The explosion-proof gas is carbon dioxide-sulfur fluoride mixed gas.
On the other hand, the embodiment also provides a method for measuring the hydrogen content in the magnesium melt, which is implemented by using the device for measuring the hydrogen content in the magnesium melt, and as shown in fig. 2, the method comprises the following steps:
s1: placing the device above the magnesium melt for preheating at a position of 2-10 cm;
s2: the reference gas is introduced into the reference gas inlet, and the explosion-proof gas is introduced into the explosion-proof gas inlet;
s3: after ventilating for 10min, inserting the device into the magnesium melt, and immersing the porous graphite into the melt by 10-20 cm;
s4: closing the explosion-proof gas, adopting a voltmeter to test the electromotive force of the device, and calculating the hydrogen content in the magnesium melt;
s5: after the test is finished, the explosion-proof gas is introduced for the second time, the test device is pulled out, the explosion-proof gas and the reference gas are closed after the natural cooling to the set temperature,
the calculation of the hydrogen content in the magnesium melt comprises the following steps:
converting the concentration difference between the equilibrium hydrogen partial pressure of the magnesium melt and the hydrogen partial pressure of the reference gas into potential difference, wherein the electrochemical reaction is as shown in formula (1):
H 2 (reference) = H 2 (to be measured) (1)
Gibbs free energy of reaction Δ G is:
wherein R is a gas constant, T is a thermodynamic temperature,
for the partial pressure of hydrogen in the magnesium melt to be measured, is determined>
Is reference gas hydrogen partial pressure;
gibbs free energy Δ G, according to Nernst's equation, is shown in equation (2):
wherein E is concentration cell electromotive force, and F is Faraday constant;
according to the electromotive force, obtaining the hydrogen partial pressure of the magnesium melt
The calculation process is shown in formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the specific law of Xihua as follows:
wherein S is 0 Is the saturated hydrogen content of the magnesium melt.
In the embodiment, the device for measuring the hydrogen content in the AZ91 magnesium melt in the invention in the figure 1 is adopted for measurement, and the device is placed above the magnesium melt for preheating at a position 5cm; a reference gas inlet is filled with hydrogen-argon standard gas with 3 percent of hydrogen content, and an explosion-proof gas inlet is filled with carbon dioxide-sulfur fluoride mixed gas; after ventilating for 10min, inserting the device into the magnesium melt, and immersing the porous graphite into the melt by 15cm; and (4) closing the explosion-proof gas, adopting a voltmeter to test the electromotive force of the device to be 0.0427V, and calculating the hydrogen content in the magnesium melt to be 8.02ml/100gMg. And after the test is finished, introducing the explosion-proof gas again, pulling out the test device, naturally cooling, and then closing the explosion-proof gas and the reference gas.
Claims (10)
1. The device for measuring the hydrogen content in the magnesium melt is characterized by comprising a proton conductor solid electrolyte sheet, a reference electrode, a ceramic tube, a binder, an electrode lead to be measured, a reference electrode lead, a reference gas outlet, a first sealing element, a reference gas tube, a reference gas inlet, porous graphite, an explosion-proof gas tube, a second sealing element, an explosion-proof gas inlet and a voltmeter;
the device comprises a proton conductor solid electrolyte sheet, a to-be-detected electrode, a reference electrode, a voltmeter and a power supply, wherein the to-be-detected electrode and the reference electrode are respectively loaded on two end faces of the proton conductor solid electrolyte sheet, and are respectively connected with a to-be-detected electrode lead and a reference electrode lead and then are connected to the voltmeter; a proton conductor solid electrolyte sheet and one end of a ceramic tube adopt a binder to seal a reference electrode in the middle; the other end of the ceramic tube is sealed by a first sealing piece with a reference gas outlet, the reference gas tube penetrates into the ceramic tube through the first sealing piece, and the reference gas inlet is arranged outside the first sealing piece; one end of the explosion-proof air pipe is connected with the porous graphite, and the other end of the explosion-proof air pipe is connected with a second sealing element with an explosion-proof air inlet; and the assembly of the proton conductor solid electrolyte sheet and the ceramic tube penetrates into the explosion-proof gas tube through the second sealing piece, and the proton conductor solid electrolyte is positioned above the porous graphite.
2. The apparatus for measuring the hydrogen content in a magnesium melt according to claim 1, wherein the proton conductor solid electrolyte tube is made of a high temperature perovskite type proton conductor.
3. The apparatus according to claim 1, wherein the electrode to be measured and the reference electrode are one of porous Pt, au, ag, rh and Ni;
the lead of the electrode to be detected and the lead of the reference electrode are NiCr alloy or FeNiCr alloy;
the binder is Al 2 O 3 Based on an insulating ceramic binder.
4. The apparatus according to claim 1, wherein the ceramic tube is made of one of corundum, magnesium oxide and zirconium dioxide;
the reference gas vent pipe is made of one of corundum, quartz and stainless steel;
the first sealing element and the second sealing element are made of one of polytetrafluoroethylene, nylon, copper and stainless steel.
5. The apparatus for measuring the hydrogen content in the magnesium melt according to claim 1, wherein the explosion-proof gas pipe is made of stainless steel;
the porous graphite is graphite felt.
6. The apparatus for measuring the hydrogen content in a magnesium melt according to claim 1, wherein the reference gas is a hydrogen-argon standard gas or a hydrogen-nitrogen standard gas;
the explosion-proof gas is carbon dioxide-sulfur fluoride mixed gas.
7. A method for measuring the hydrogen content in magnesium melt, which is realized by the device for measuring the hydrogen content in the magnesium melt according to claim 1, and comprises the following steps:
s1: placing the device above the magnesium melt for preheating;
s2: the reference gas is introduced into the reference gas inlet, and the explosion-proof gas is introduced into the explosion-proof gas inlet;
s3: after aeration, the device is inserted into the magnesium melt, and the porous graphite is immersed into the melt;
s4: closing the explosion-proof gas, adopting a voltmeter to test the electromotive force of the device, and calculating the hydrogen content in the magnesium melt;
s5: and after the test is finished, introducing explosion-proof gas for the second time, pulling out the test device, closing the explosion-proof gas and the reference gas after the test device is naturally cooled to the set temperature, and calculating the hydrogen content in the magnesium melt.
8. The method of measuring the hydrogen content of a magnesium melt of claim 7, wherein said calculating the hydrogen content of the magnesium melt comprises:
converting the concentration difference between the equilibrium hydrogen partial pressure of the magnesium melt and the hydrogen partial pressure of the reference gas into potential difference, wherein the electrochemical reaction is as shown in formula (1):
H 2 (reference) = H 2 (to be measured) (1)
Gibbs free energy of reaction Δ G is:
wherein R is a gas constant, T is a thermodynamic temperature,
for the partial pressure of hydrogen in the magnesium melt to be measured, is determined>
Is reference gas hydrogen partial pressure;
gibbs free energy Δ G, according to the Nernst equation, is shown in equation (2):
wherein E is concentration cell electromotive force, and F is Faraday constant;
according to the electromotive force, obtaining the hydrogen partial pressure of the magnesium melt
The calculation process is shown in formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the specific law of Xihua as follows:
wherein S is 0 Is the saturated hydrogen content of the magnesium melt.
9. The method for measuring the hydrogen content in the magnesium melt according to claim 7, wherein the device is placed above the magnesium melt for preheating, and specifically comprises: the device is placed 2-10 cm above the magnesium melt for preheating.
10. The method of measuring the hydrogen content of a magnesium melt according to claim 7, wherein said aeration, optionally for a period of 10min;
the porous graphite is immersed into the melt, and specifically comprises the following steps: the porous graphite is immersed into the melt at a position of 10-20 cm.
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| 李大勇;肖鹏;马旭梁;王利华;: "铝镁合金熔体氢含量快速定量检测技术研究进展", 机械工程学报, no. 20, 10 September 2013 (2013-09-10) * |
| 王东;刘春明;华千慧;张慧玲;杨博威;: "铝熔体定量测氢技术的研究进展", 特种铸造及有色合金, no. 10, 20 October 2016 (2016-10-20) * |
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