CN115856055B - 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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- CN115856055B CN115856055B CN202211554812.1A CN202211554812A CN115856055B CN 115856055 B CN115856055 B CN 115856055B CN 202211554812 A CN202211554812 A CN 202211554812A CN 115856055 B CN115856055 B CN 115856055B
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000011777 magnesium Substances 0.000 title claims abstract description 82
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 82
- 239000001257 hydrogen Substances 0.000 title claims abstract description 74
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 74
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 91
- 238000007789 sealing Methods 0.000 claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004020 conductor Substances 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
- 238000012360 testing method Methods 0.000 claims abstract description 23
- 239000007784 solid electrolyte Substances 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 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
- 239000000853 adhesive Substances 0.000 claims description 7
- 230000001070 adhesive effect Effects 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 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
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 5
- 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
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 3
- 238000006243 chemical reaction 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
- 239000000395 magnesium oxide Substances 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
- 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
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 abstract description 6
- 238000005259 measurement Methods 0.000 abstract description 5
- 238000004880 explosion Methods 0.000 abstract description 4
- 238000002485 combustion reaction Methods 0.000 abstract description 3
- 239000000523 sample Substances 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
- 238000001816 cooling Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000009423 ventilation Methods 0.000 description 3
- 238000004458 analytical method Methods 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
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 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
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 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
- 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
Abstract
The invention discloses a device and a method for measuring the hydrogen content in a 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, a lead wire of the electrode to be detected, a lead wire of the reference electrode, a reference gas outlet, a first sealing piece, a reference gas pipe, a reference gas inlet, porous graphite, an explosion-proof gas pipe, a second sealing piece, an explosion-proof gas inlet and a voltmeter; to accurately test the hydrogen content in the magnesium melt; at the same time, the probe assembly including the binder, support and sensing material can be prevented from reacting with the magnesium melt; air remained in the testing device or on the surface is prevented from reacting with the magnesium melt, and 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 the hydrogen content in a magnesium melt.
Background
Hydrogen is a harmful element of metal materials, and in magnesium and magnesium alloy, if the hydrogen content is high, the properties of plasticity, strength, fatigue life and the like of the materials are seriously reduced, and the hydrogen content must be accurately tested in the production process so as to efficiently control the 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 is used for sampling, preparing samples and testing for a long time, and the rapid hydrogen measurement requirement of a production line cannot be met; the first bubble method is that the liquid state of the production line is sampled, sealed and decompressed, the pressure of the first hydrogen bubble generated can be regarded as hydrogen partial pressure, so that the hydrogen content is calculated, but the vapor pressure of magnesium is higher, bubbles can be generated, and the read error is easy to generate, so that the test is inaccurate; the closed cycle method needs to introduce inert gas into the magnesium melt to carry out the measurement of hydrogen in the magnesium, but the magnesium is carried out, and the magnesium reacts with the hydrogen to generate hydride, so that the test is inaccurate; the electrochemical sensing method can accurately test the hydrogen content in magnesium, but the hydrogen sensitive material and the probe are connected by adopting a binder, wherein the solvent is mostly water glass or phosphate, silicon oxide or phosphorus oxide generated by decomposition is extremely easy to react with magnesium to generate explosion, if the hydrogen sensitive material and a magnesium melt are separated by a porous material, air in the porous material is easy to react with magnesium to burn and explode in an initial state.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the device and the method for measuring the hydrogen content in the magnesium melt, which prevent the combustion and explosion in the test process, thereby safely and accurately testing the hydrogen content in the magnesium.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
In one aspect, the invention provides a device for measuring hydrogen content in magnesium melt, which comprises a proton conductor solid electrolyte sheet, a reference electrode, a ceramic tube, a binder, a to-be-measured electrode lead, a reference gas outlet, a first sealing element, a reference gas pipe, a reference gas inlet, porous graphite, an explosion-proof gas pipe, a second sealing element, an explosion-proof gas inlet and a voltmeter;
The two end surfaces of the proton conductor solid electrolyte sheet are respectively loaded with a to-be-measured electrode and a reference electrode, and the to-be-measured electrode and the reference electrode are respectively connected with a to-be-measured electrode lead and a reference electrode lead and then connected with a voltmeter; the proton conductor solid electrolyte sheet and one end of the ceramic tube seal the reference electrode in the middle by adopting an adhesive; the other end of the ceramic tube is sealed by a first sealing element with a reference gas outlet, the reference gas tube penetrates into the ceramic tube through the first sealing element, and the reference gas inlet is arranged outside the first sealing element; one end of the explosion-proof air pipe is connected with porous graphite, and the other end of the explosion-proof air pipe is connected with a second sealing piece with an explosion-proof air inlet; the combination of the proton conductor solid electrolyte sheet and the ceramic tube penetrates into the explosion-proof air tube through the second sealing piece, and the proton conductor solid electrolyte sheet is positioned above the porous graphite.
The proton conductor solid electrolyte sheet is made of a high-temperature perovskite type proton conductor.
The electrode to be measured and the reference electrode are one of a plurality of holes Pt, au, ag, rh and Ni.
The electrode lead to be tested and the reference electrode lead are NiCr alloy or FeNiCr alloy.
The binder is an Al 2O3 -based insulating ceramic binder.
The ceramic tube is made of one of corundum, magnesia and zirconium dioxide.
The reference air 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.
On the other hand, the invention also provides a method for measuring the hydrogen content in the magnesium melt, which is realized by adopting the device for measuring the hydrogen content in the magnesium melt and comprises the following steps of:
s1: placing the device above a magnesium melt for preheating;
S2: the reference gas inlet is filled with reference gas, and the explosion-proof gas inlet is filled with explosion-proof gas;
S3: after aeration, inserting the device into the magnesium melt, immersing the porous graphite into the melt;
s4: closing the explosion-proof gas, testing the electromotive force of the device by adopting a voltmeter, and calculating the hydrogen content in the magnesium melt;
s5: after the test is completed, the explosion-proof gas is secondarily introduced, the testing device is pulled out, the explosion-proof gas and the reference gas are closed after the natural cooling is carried out to the set temperature,
The calculation of the hydrogen content in 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 a potential difference, wherein the electrochemical reaction is shown as a formula (1):
H 2 (reference) =h 2 (to be measured) (1)
The gibbs free energy of the reaction Δg is:
Wherein R is a gas constant, T is a thermodynamic temperature, For the hydrogen partial pressure of the magnesium melt to be measured,Is the partial pressure of hydrogen of the reference gas;
according to the Nernst equation, the Gibbs free energy ΔG is represented by formula (2):
wherein E is concentration battery electromotive force, F is Faraday constant;
Obtaining the hydrogen partial pressure of the magnesium melt according to the electromotive force The calculation process is shown as formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the law of Sihuatret:
Wherein S 0 is the saturated hydrogen content of the magnesium melt.
The device is placed above the magnesium melt for preheating, and specifically comprises: the device is placed at a position 2-10 cm above the magnesium melt for preheating.
The specific duration of ventilation is 10min.
The porous graphite is immersed into the melt, specifically 10-20 cm of the melt.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
1. the invention provides a device and a method for measuring the hydrogen content in a magnesium melt, which can accurately test the hydrogen content in the magnesium melt.
2. The invention provides a device and a method for measuring the hydrogen content in a 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 remained in or on the surface of a testing device from reacting with the magnesium melt and prevent oxidation, combustion and explosion of the magnesium melt.
Drawings
FIG. 1 is a schematic diagram of an apparatus for measuring hydrogen content in magnesium melt according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for measuring hydrogen content in magnesium melt according to an embodiment of the present invention;
The reference numerals are: 1. the proton conductor solid electrolyte sheet comprises 2 parts of a proton conductor solid electrolyte sheet, 2 parts of an electrode to be detected, 3 parts of a reference electrode, 4 parts of a ceramic tube, 5 parts of an adhesive, 6 parts of a lead wire of the electrode to be detected, 7 parts of a lead wire of a reference electrode, 8 parts of a reference gas outlet, 9 parts of a first sealing piece, 10 parts of a reference gas tube, 11 parts of a reference gas inlet, 12 parts of porous graphite, 13 parts of an explosion-proof gas tube, 14 parts of a second sealing piece, 15 parts of an explosion-proof gas inlet and 16 parts of a voltmeter.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples.
In one aspect, the present embodiment proposes a device for measuring hydrogen content in 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, an adhesive 5, a lead wire to be measured 6, a lead wire to be reference electrode 7, a reference gas outlet 8, a first sealing member 9, a reference gas pipe 10, a reference gas inlet 11, porous graphite 12, an explosion-proof gas pipe 13, a second sealing member 14, an explosion-proof gas inlet 15, and a voltmeter 16;
The two end surfaces of the proton conductor solid electrolyte sheet 1 are respectively loaded with an electrode 2 to be detected and a reference electrode 3, and the electrode 2 to be detected and the reference electrode 3 are respectively connected with a lead 6 of the electrode to be detected and a lead 7 of the reference electrode and then connected to a voltmeter 16; the proton conductor solid electrolyte sheet 1 and one end of the ceramic tube 4 seal the reference electrode 3 in the middle by adopting an adhesive 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 pipe 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 piece 14 with an explosion-proof air inlet 15; the combination of the proton conductor solid electrolyte sheet 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 sheet 1 is positioned above the porous graphite 12.
The proton conductor solid electrolyte sheet 1 is made of a high-temperature perovskite type proton conductor.
The electrode 2 to be measured and the reference electrode 3 are one of a plurality of holes Pt, au, ag, rh and Ni.
The electrode lead 6 to be tested and the reference electrode lead 7 are made of NiCr alloy or FeNiCr alloy.
The adhesive 5 is an Al 2O3 -based insulating ceramic adhesive.
The ceramic tube 4 is made of one of corundum, magnesia and zirconia.
The breather pipe is made of 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 pipe is 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 realized by adopting the device for measuring the hydrogen content in the magnesium melt, as shown in fig. 2, and comprises the following steps:
S1: preheating the device at a position 2-10 cm above the magnesium melt;
S2: the reference gas inlet is filled with reference gas, and the explosion-proof gas inlet is filled with explosion-proof gas;
S3: after ventilation for 10min, inserting the device into a magnesium melt, and immersing porous graphite into the melt for 10-20 cm;
s4: closing the explosion-proof gas, testing the electromotive force of the device by adopting a voltmeter, and calculating the hydrogen content in the magnesium melt;
s5: after the test is completed, the explosion-proof gas is secondarily introduced, the testing device is pulled out, the explosion-proof gas and the reference gas are closed after the natural cooling is carried out to the set temperature,
The calculation of the hydrogen content in 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 a potential difference, wherein the electrochemical reaction is shown as a formula (1):
h 2 (reference) =h 2 (to be measured) (1)
The gibbs free energy of the reaction Δg is:
Wherein R is a gas constant, T is a thermodynamic temperature, For the hydrogen partial pressure of the magnesium melt to be measured,Is the partial pressure of hydrogen of the reference gas;
according to the Nernst equation, the Gibbs free energy ΔG is represented by formula (2):
wherein E is concentration battery electromotive force, F is Faraday constant;
Obtaining the hydrogen partial pressure of the magnesium melt according to the electromotive force The calculation process is shown as formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the law of Sihuatret:
Wherein S 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 shown in fig. 1 is adopted for measurement, and the device is placed above the magnesium melt for preheating at a position of 5cm; the reference gas inlet is filled with hydrogen-argon standard gas with the hydrogen content of 3 percent, and the explosion-proof gas inlet is filled with carbon dioxide-sulfur fluoride mixed gas; after ventilation for 10min, the device is inserted into a magnesium melt, and the porous graphite is immersed into the melt for 15cm; the explosion-proof gas is closed, the electromotive force of a voltmeter testing device is 0.0427V, and the hydrogen content in the magnesium melt is calculated to be 8.02ml/100gMg. After the test is finished, the explosion-proof gas is introduced again, the testing device is pulled out, natural cooling is carried out, and then the explosion-proof gas and the reference gas are closed.
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, a to-be-measured electrode lead, a reference gas outlet, a first sealing element, a reference gas pipe, a reference gas inlet, porous graphite, an explosion-proof gas pipe, a second sealing element, an explosion-proof gas inlet and a voltmeter;
The two end surfaces of the proton conductor solid electrolyte sheet are respectively loaded with a to-be-measured electrode and a reference electrode, and the to-be-measured electrode and the reference electrode are respectively connected with a to-be-measured electrode lead and a reference electrode lead and then connected with a voltmeter; the proton conductor solid electrolyte sheet and one end of the ceramic tube seal the reference electrode in the middle by adopting an adhesive; the other end of the ceramic tube is sealed by a first sealing element with a reference gas outlet, the reference gas tube penetrates into the ceramic tube through the first sealing element, and the reference gas inlet is arranged outside the first sealing element; one end of the explosion-proof air pipe is connected with porous graphite, and the other end of the explosion-proof air pipe is connected with a second sealing piece with an explosion-proof air inlet; the combination of the proton conductor solid electrolyte sheet and the ceramic tube penetrates into the explosion-proof air tube through the second sealing piece, and the proton conductor solid electrolyte sheet is positioned above the porous graphite.
2. The apparatus for measuring hydrogen content in magnesium melt according to claim 1, wherein the proton conductor solid electrolyte sheet is made of high temperature perovskite proton conductor.
3. The apparatus for measuring hydrogen content in magnesium melt according to claim 1, wherein the electrode to be measured and the reference electrode are one of a porous Pt, au, ag, rh and Ni;
The electrode lead to be tested and the reference electrode lead are NiCr alloy or FeNiCr alloy;
The binder is an Al 2O3 -based insulating ceramic binder.
4. The device for measuring the hydrogen content in the magnesium melt according to claim 1, wherein the ceramic tube is made of one of corundum, magnesia and zirconia;
The reference air 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 device for measuring the hydrogen content in the magnesium melt according to claim 1, wherein the explosion-proof air 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 a magnesium melt using the apparatus for measuring the hydrogen content in a magnesium melt according to claim 1, comprising the steps of:
s1: placing the device above a magnesium melt for preheating;
S2: the reference gas inlet is filled with reference gas, and the explosion-proof gas inlet is filled with explosion-proof gas;
S3: after aeration, inserting the device into the magnesium melt, immersing the porous graphite into the melt;
s4: closing the explosion-proof gas, testing the electromotive force of the device by adopting a voltmeter, and calculating the hydrogen content in the magnesium melt;
S5: after the test is completed, the explosion-proof gas is introduced for the second time, the testing device is pulled out, the explosion-proof gas and the reference gas are closed after the test device is naturally cooled to the set temperature, and the hydrogen content in the magnesium melt is calculated.
8. The method of measuring the hydrogen content of a magnesium melt according to 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 a potential difference, wherein the electrochemical reaction is shown as a formula (1):
H 2 (reference) =h 2 (to be measured) (1)
The gibbs free energy of the reaction Δg is:
Wherein R is a gas constant, T is a thermodynamic temperature, For the hydrogen partial pressure of the magnesium melt to be measured,Is the partial pressure of hydrogen of the reference gas;
according to the Nernst equation, the Gibbs free energy ΔG is represented by formula (2):
wherein E is concentration battery electromotive force, F is Faraday constant;
Obtaining the hydrogen partial pressure of the magnesium melt according to the electromotive force The calculation process is shown as formula (4):
the hydrogen content S of the magnesium melt can be calculated according to the law of Sihuatret:
Wherein S 0 is the saturated hydrogen content of the magnesium melt.
9. The method for measuring the hydrogen content in a magnesium melt according to claim 7, characterized in that the device is preheated at a position above the magnesium melt, in particular: the device is placed at a position 2-10 cm above the magnesium melt for preheating.
10. The method for measuring the hydrogen content in a magnesium melt according to claim 7, wherein the aeration period is 10min;
The porous graphite is immersed into the melt, and specifically comprises the following components: the porous graphite is immersed into the melt at a position of 10-20 cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211554812.1A CN115856055B (en) | 2022-12-06 | Device and method for measuring hydrogen content in magnesium melt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211554812.1A CN115856055B (en) | 2022-12-06 | Device and method for measuring hydrogen content in magnesium melt |
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| Publication Number | Publication Date |
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| CN115856055A CN115856055A (en) | 2023-03-28 |
| CN115856055B true CN115856055B (en) | 2024-07-16 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980009A (en) * | 2010-09-10 | 2011-02-23 | 清华大学 | Solid oxide electrolytic cell testing bracket |
| CN114324535A (en) * | 2022-01-05 | 2022-04-12 | 东北大学 | Detachable metal melt hydrogen measuring sensor device |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101980009A (en) * | 2010-09-10 | 2011-02-23 | 清华大学 | Solid oxide electrolytic cell testing bracket |
| CN114324535A (en) * | 2022-01-05 | 2022-04-12 | 东北大学 | Detachable metal melt hydrogen measuring sensor device |
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