CN116046608A - Device and method for measuring hydrogen content in aluminum and aluminum alloy - Google Patents
Device and method for measuring hydrogen content in aluminum and aluminum alloy Download PDFInfo
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- CN116046608A CN116046608A CN202211554830.XA CN202211554830A CN116046608A CN 116046608 A CN116046608 A CN 116046608A CN 202211554830 A CN202211554830 A CN 202211554830A CN 116046608 A CN116046608 A CN 116046608A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L21/00—Vacuum gauges
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
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Abstract
The invention discloses a device and a method for measuring hydrogen content in aluminum and aluminum alloy, and relates to the technical field of hydrogen measurement sensing; the device comprises: the device comprises a decompression container, a sampler, a first pressure transmitter, a first gas circuit, a first vacuum valve, a buffer cylinder, a second pressure transmitter, a second gas circuit, a second vacuum valve, a three-way valve, a vacuum pump, a controller, a sealing cover, a sealing ring and a heat insulation base; the vacuum degree of the decompression container is rapidly reduced to a target value through the buffer cylinder, so that interference is reduced; the vacuum degree of the decompression container is stably controlled at a target value through dynamic control of the buffer cylinder and the vacuum valve, and the testing accuracy is improved. The heat-insulating base is adopted to prolong the liquid solidification time in the sample, the hydrogen evolution time is long, the hydrogen content detection limit is lower, and the test result is accurate.
Description
Technical Field
The invention relates to the technical field of hydrogen measurement and sensing, in particular to a device and a method for measuring hydrogen content in aluminum and aluminum alloy.
Background
In the production process of high-performance aluminum and aluminum alloy materials, the quality control of an aluminum melt is one of key factors, and the hydrogen content is an important parameter of the quality of the aluminum melt.
The hydrogen saturation solubility of the liquid phase aluminum is far higher than that of the solid phase aluminum, hydrogen tends to be separated out from the aluminum melt in the solidification process of the aluminum melt, so that the inside of the aluminum alloy is loose, irregular air holes and pinholes appear, the aluminum alloy generates hydrogen induced defects, the mechanical property or the physical and chemical properties of the aluminum alloy are obviously reduced, and the compactness, the fatigue limit, the strength, the plasticity, the corrosion resistance, the electrical conductivity, the thermal conductivity and the like of the aluminum alloy are greatly influenced. Therefore, there is a need to rapidly test the hydrogen content of aluminum during the production process to control the quality of the product.
The method is that liquid aluminum is sampled and put into a sealed container, and after vacuum pumping, the liquid aluminum sample is gradually solidified under the condition of negative pressure. Due to the fact that the saturation solubility of hydrogen in solid-liquid phase aluminum is poor, negative pressure is driven to drive the hydrogen in the aluminum to separate out in the melt solidification process, a solidified aluminum sample generates air holes, and the porosity of a test sample can represent the hydrogen content in the aluminum. Therefore, a stable negative pressure/vacuum must be provided during the depressurization process to ensure test accuracy. In the general test process, the vacuum degree is required to be 2kPa, a rotary vane vacuum pump is usually adopted as a vacuum source, the ultimate vacuum degree is generally 2Pa, and in addition, factors such as an external power supply, vacuum oil quality, vacuum pump aging, vacuum pump sealing degree, pipeline sealing degree, vacuum container sealing degree and the like all influence the vacuum degree of the vacuum container. Because of the design defects of the existing method and device, large uncontrollable factors and the like, the vacuum degree of the decompression container cannot be controlled stably, so that the vacuum degree is very unstable in the solidification decompression process, and the test result is inaccurate.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art and provides a device and a method for measuring the hydrogen content in aluminum and aluminum alloy, which can rapidly and accurately measure the hydrogen content in aluminum and aluminum alloy.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
in one aspect, the present invention provides an apparatus for measuring hydrogen content in aluminum and aluminum alloys, the apparatus comprising: the device comprises a decompression container, a sampler, a first pressure transmitter, a first gas circuit, a first vacuum valve, a buffer cylinder, a second pressure transmitter, a second gas circuit, a second vacuum valve, a three-way valve, a vacuum pump, a controller, a sealing cover, a sealing ring and a heat insulation base; the sampler is placed in the heat-preserving base and is placed in a sealed decompression container together, and the top of the decompression container is provided with a sealing ring and covers an openable sealing cover; the vacuum degree of the decompression container and the buffer cylinder is tested respectively by the first pressure transmitter and the second pressure transmitter, and the controller is used for controlling the opening and closing of the first vacuum valve and the second vacuum valve, and adjusting and controlling the vacuum degree of the decompression container.
The material of the pressure reducing container is one of steel, copper and nickel and a plurality of alloys thereof.
The sampler is made of one or more of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel;
when the sampler is made of one or more of corundum, steel, copper and nickel, and alloys thereof, the surface of the sampler is required to be coated with a boron nitride release agent.
The first pressure transmitter and the second pressure transmitter are pressure transmitters.
The first air passage and the second air passage are made of one of stainless steel, copper and polytetrafluoroethylene.
The first vacuum valve and the second vacuum valve are electromagnetic valves.
The buffer cylinder is made of one of steel, copper and nickel and a plurality of alloys or polytetrafluoroethylene thereof.
The three-way valve is a three-way vacuum ball valve, and is made of one of stainless steel, copper and nylon.
The vacuum pump is a rotary vane vacuum pump.
The controller is an industrial personal computer.
The sealing cover is made of one of polytetrafluoroethylene, glass and quartz or one of steel, copper and nickel and a plurality of alloys thereof.
The sealing ring can be made of one of silicon rubber, fluororubber and polytetrafluoroethylene.
The shell of the heat-insulating base is made of stainless steel, and NaCl-KaCl mixed salt is arranged in the heat-insulating base.
On the other hand, the invention also provides a method for measuring the hydrogen content in aluminum and aluminum alloy, which is realized by adopting the device for measuring the hydrogen content in aluminum and aluminum alloy, and comprises the following steps:
s1: opening the sealing cover, taking out the sampler and the heat preservation base, and preheating together;
s2: the three-way valve is adjusted to be connected with the buffer cylinder through the vacuum pump, the first vacuum valve is closed, and the second vacuum valve is opened;
s3: starting a vacuum pump, and closing a second vacuum valve when the vacuum degree of the buffer cylinder measured by the second pressure transmitter reaches a preset threshold value; opening a second vacuum valve when the vacuum degree is higher than a preset threshold value;
s4: placing a sampler for taking an aluminum melt sample into a heat insulation base, placing the heat insulation base into a pressure reduction container, and closing a sealing cover;
s5: opening a first vacuum valve, closing the first vacuum valve when the vacuum degree reaches a preset threshold value, and opening the first vacuum valve when the vacuum degree is higher than 2 preset threshold values;
s6: after the aluminum sample is solidified, taking out the aluminum sample, testing the relative density of the aluminum sample, and calculating the porosity and the hydrogen content of the aluminum sample, wherein the calculation process is shown as the formula (1) and the formula (2):
L＝1-A (1)
wherein L is the porosity, A is the relative density, x is the hydrogen content in the aluminum, f (x) is the porosity of the solidified sample, M P For hydrogen solubility in aluminum, G C To increase the control constant, L P To test the minimum porosity, P, of the sample to be tested under a certain pressure I R is the maximum transition point of the relation between the porosity of the solidification sample and the hydrogen content, and r is the average transition point of the relation between the porosity of the solidification sample and the hydrogen content.
The preset threshold is 2.0kPa, and the error is +/-0.2 kPa;
the preheating is carried out to 600-700 ℃.
The beneficial effects of adopting above-mentioned technical scheme to produce lie in:
1. the invention provides a device and a method for rapidly measuring the hydrogen content in aluminum and aluminum alloy, which can rapidly reduce the vacuum degree of a decompression container to a target value through a buffer cylinder, reduce interference and improve test accuracy.
2. The invention provides a device and a method for rapidly measuring the hydrogen content in aluminum and aluminum alloy, which can stably control the vacuum degree of a decompression container at a target value through dynamic control of a buffer cylinder and a vacuum valve, and improve the test accuracy.
3. The invention provides a device and a method for rapidly measuring the hydrogen content in aluminum and aluminum alloy, which adopts a heat-insulating base to prolong the liquid solidification time in a sample, has long hydrogen evolution time, lower hydrogen content detection limit and accurate test result.
Drawings
FIG. 1 is a schematic diagram of an apparatus for measuring hydrogen content in aluminum and aluminum alloy according to an embodiment of the present invention;
FIG. 2 is a flow chart of a method for measuring hydrogen content in aluminum and aluminum alloys according to an embodiment of the present invention;
in the figure, 1, a decompression container, 2, a sampler, 3, an aluminum sample, 4, a first pressure transmitter, 5, a first gas circuit, 6, a first vacuum valve, 7, a buffer cylinder, 8, a second pressure transmitter, 9, a second gas circuit, 10, a second vacuum valve, 11, a three-way valve, 12, a vacuum pump, 13, a controller, 14, a sealing cover, 15, a sealing ring, 16 and a heat insulation base.
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 provides an apparatus for measuring hydrogen content in aluminum and aluminum alloy, as shown in fig. 1, the apparatus includes: the vacuum sampler comprises a pressure reducing container 1, a sampler 2, an aluminum sample 3, a first pressure transmitter 4, a first gas circuit 5, a first vacuum valve 6, a buffer cylinder 7, a second pressure transmitter 8, a second gas circuit 9, a second vacuum valve 10, a three-way valve 11, a vacuum pump 12, a controller 13, a sealing cover 14, a sealing ring 15 and a heat insulation base 16; the sampler 2 with the aluminum sample 3 is placed in a heat-preserving base 16 and is placed in a sealed decompression container 1 together, and a sealing ring 15 is arranged at the top of the decompression container 1 and covers an openable sealing cover 14; the decompression container is connected with a buffer cylinder 7 through a first air path 5 and a first vacuum valve 6, the buffer cylinder is connected with a vacuum pump 12 through an air path B and a second vacuum valve 10, the first pressure transmitter 3 and the second pressure transmitter 9 respectively test the vacuum degree of the decompression container 1 and the buffer cylinder 7, and a controller 13 is adopted to control the opening and closing of the first vacuum valve 6 and the second vacuum valve 10 and adjust and control the vacuum degree of the decompression container 1.
The material of the pressure reducing container 1 is one of steel, copper and nickel and a plurality of alloys thereof.
The sampler 2 is made of one or more of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel;
when the sampler 2 is made of corundum, steel, copper, nickel or alloys of a plurality of the corundum, steel, copper and nickel, the surface of the sampler needs to be coated with a boron nitride release agent.
The first pressure transmitter 4 and the second pressure transmitter 8 are pressure transmitters, and in this embodiment, pressure transmitters with a measuring range of 0kPa to 100kPa and an accuracy of 0.2% fs are used.
The first air channel 5 and the second air channel 9 are made of one of stainless steel, copper and polytetrafluoroethylene.
The first vacuum valve 6 and the second vacuum valve 10 are normally closed electromagnetic valves, and in this embodiment, normally closed electromagnetic valves with the pressure range of 0-0.5 Mpa are adopted.
The buffer cylinder 7 is made of one of steel, copper and nickel, and a plurality of alloys or polytetrafluoroethylene.
The three-way valve 11 is a three-way vacuum ball valve, and is made of one of stainless steel, copper and nylon.
The vacuum pump 12 is a rotary vane vacuum pump.
The controller 13 is an industrial personal computer.
The sealing cover 14 is made of one of polytetrafluoroethylene, glass and quartz or one or more of steel, copper and nickel and the alloy thereof.
The sealing ring 15 may be made of one of silicone rubber, fluororubber and polytetrafluoroethylene.
The shell of the heat-insulating base 16 is made of stainless steel, and the interior of the heat-insulating base is NaCl-KaCl mixed salt.
On the other hand, the embodiment also provides a method for measuring the hydrogen content in aluminum and aluminum alloy, which is realized by adopting the device for measuring the hydrogen content in aluminum and aluminum alloy, as shown in fig. 2, and comprises the following steps:
s1: opening a sealing cover, taking out the sampler and the heat preservation base, and preheating to 600-700 ℃;
s2: the three-way valve is adjusted to be connected with the buffer cylinder through the vacuum pump, the first vacuum valve is closed, and the second vacuum valve is opened;
s3: starting a vacuum pump, and closing a second vacuum valve when the vacuum degree of the buffer cylinder measured by the second pressure transmitter reaches a preset threshold value; opening a second vacuum valve when the vacuum degree is higher than a preset threshold value;
in the embodiment, the preset threshold is 2.0kPa, and the error is +/-0.2 kPa;
s4: placing a sampler for taking an aluminum melt sample into a heat insulation base, placing the heat insulation base into a pressure reduction container, and closing a sealing cover;
s5: opening a first vacuum valve, closing the first vacuum valve when the vacuum degree reaches a preset threshold value, and opening the first vacuum valve when the vacuum degree is higher than the preset threshold value;
s6: after the aluminum sample is solidified, taking out the aluminum sample, testing the relative density of the aluminum sample, and calculating the porosity and the hydrogen content of the aluminum sample, wherein the calculation process is shown as the formula (1) and the formula (2):
L＝1-A (1)
wherein L is the porosity, A is the relative density, x is the hydrogen content in the aluminum, f (x) is the porosity of the solidified sample, M P For hydrogen solubility in aluminum, G C To increase the control constant, L P To test the minimum porosity, P, of the sample to be tested under a certain pressure I R is the maximum transition point of the relation between the porosity of the solidification sample and the hydrogen content, and r is the average transition point of the relation between the porosity of the solidification sample and the hydrogen content.
Claims (10)
1. An apparatus for measuring hydrogen content in aluminum and aluminum alloys, the apparatus comprising: the device comprises a decompression container, a sampler, a first pressure transmitter, a first gas circuit, a first vacuum valve, a buffer cylinder, a second pressure transmitter, a second gas circuit, a second vacuum valve, a three-way valve, a vacuum pump, a controller, a sealing cover, a sealing ring and a heat insulation base; the sampler is placed in the heat-preserving base and is placed in a sealed decompression container together, and the top of the decompression container is provided with a sealing ring and covers an openable sealing cover; the vacuum degree of the decompression container and the buffer cylinder is tested respectively by the first pressure transmitter and the second pressure transmitter, and the controller is used for controlling the opening and closing of the first vacuum valve and the second vacuum valve, and adjusting and controlling the vacuum degree of the decompression container.
2. The apparatus for measuring hydrogen content in aluminum and aluminum alloys according to claim 1, wherein the material of the pressure reducing container is one or more of steel, copper and nickel.
3. The apparatus for measuring hydrogen content in aluminum and aluminum alloys according to claim 1, wherein the material of the sampler is one or more of boron nitride, graphite, silicon carbide, corundum, steel, copper and nickel, and alloys thereof.
4. The apparatus for measuring hydrogen content in aluminum and aluminum alloy as claimed in claim 3, wherein the surface of the sampler is coated with boron nitride release agent when the sampler is made of one or more of corundum, steel, copper and nickel.
5. The apparatus for measuring hydrogen content in aluminum and aluminum alloy as recited in claim 1, wherein the first gas path and the second gas path are made of one of stainless steel, copper and polytetrafluoroethylene.
6. The apparatus for measuring hydrogen content in aluminum and aluminum alloys according to claim 1, wherein the first vacuum valve and the second vacuum valve are solenoid valves;
the buffer cylinder is made of one of steel, copper and nickel and a plurality of alloys or polytetrafluoroethylene thereof;
the three-way valve is a three-way vacuum ball valve, and is made of one of stainless steel, copper and nylon;
the vacuum pump is a rotary vane vacuum pump;
the controller is an industrial personal computer.
7. The apparatus for measuring hydrogen content in aluminum and aluminum alloy as claimed in claim 1, wherein the sealing cover is made of one of polytetrafluoroethylene, glass and quartz or one of steel, copper and nickel and their alloys;
the sealing ring is made of one of silicon rubber, fluororubber and polytetrafluoroethylene;
the shell of the heat-insulating base is made of stainless steel, and NaCl-KaCl mixed salt is arranged in the heat-insulating base.
8. The method for measuring the hydrogen content in the aluminum and the aluminum alloy is realized by adopting the device for measuring the hydrogen content in the aluminum and the aluminum alloy and comprises the following steps of:
s1: opening the sealing cover, taking out the sampler and the heat preservation base, and preheating together;
s2: the three-way valve is adjusted to be connected with the buffer cylinder through the vacuum pump, the first vacuum valve is closed, and the second vacuum valve is opened;
s3: starting a vacuum pump, and closing a second vacuum valve when the vacuum degree of the buffer cylinder measured by the second pressure transmitter reaches a preset threshold value; opening a second vacuum valve when the vacuum degree is higher than a preset threshold value;
s4: placing a sampler for taking an aluminum melt sample into a heat insulation base, placing the heat insulation base into a pressure reduction container, and closing a sealing cover;
s5: opening a first vacuum valve, closing the first vacuum valve when the vacuum degree reaches a preset threshold value, and opening the first vacuum valve when the vacuum degree is higher than the preset threshold value;
s6: after the aluminum sample is solidified, taking out the aluminum sample, testing the relative density of the aluminum sample, and calculating the porosity and the hydrogen content of the aluminum sample, wherein the calculation process is shown as the formula (1) and the formula (2):
L＝1-A(1)
wherein L is the porosity, A is the relative density, x is the hydrogen content in the aluminum, f (x) is the porosity of the solidified sample, M P For hydrogen solubility in aluminum, G C To increase the control constant, L P To test the minimum porosity, P, of the sample to be tested under a certain pressure I R is the maximum transition point of the relation between the porosity of the solidification sample and the hydrogen content, and r is the average transition point of the relation between the porosity of the solidification sample and the hydrogen content.
9. The apparatus for measuring hydrogen content in aluminum and aluminum alloys according to claim 8, wherein the preheating is performed to 600 to 700 ℃.
10. The apparatus for measuring hydrogen content in aluminum and aluminum alloy as claimed in claim 8, wherein the preset threshold is 2.0kPa, error ± 0.2kPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211554830.XA CN116046608A (en) | 2022-12-06 | 2022-12-06 | Device and method for measuring hydrogen content in aluminum and aluminum alloy |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211554830.XA CN116046608A (en) | 2022-12-06 | 2022-12-06 | Device and method for measuring hydrogen content in aluminum and aluminum alloy |
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| CN116046608A true CN116046608A (en) | 2023-05-02 |
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| CN202211554830.XA Pending CN116046608A (en) | 2022-12-06 | 2022-12-06 | Device and method for measuring hydrogen content in aluminum and aluminum alloy |
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- 2022-12-06 CN CN202211554830.XA patent/CN116046608A/en active Pending
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