CN115112547B - Static multi-sample lead-bismuth corrosion test device and test method - Google Patents
Static multi-sample lead-bismuth corrosion test device and test method Download PDFInfo
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- CN115112547B CN115112547B CN202210560493.9A CN202210560493A CN115112547B CN 115112547 B CN115112547 B CN 115112547B CN 202210560493 A CN202210560493 A CN 202210560493A CN 115112547 B CN115112547 B CN 115112547B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 58
- 230000007797 corrosion Effects 0.000 title claims abstract description 57
- 238000012360 testing method Methods 0.000 title claims abstract description 39
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 36
- 230000003068 static effect Effects 0.000 title claims abstract description 29
- 238000010998 test method Methods 0.000 title claims abstract description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000010453 quartz Substances 0.000 claims abstract description 105
- 125000006850 spacer group Chemical group 0.000 claims abstract description 28
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001152 Bi alloy Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims description 22
- 238000007789 sealing Methods 0.000 claims description 20
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- 239000002775 capsule Substances 0.000 claims description 10
- 229910001309 Ferromolybdenum Inorganic materials 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- QRRWWGNBSQSBAM-UHFFFAOYSA-N alumane;chromium Chemical compound [AlH3].[Cr] QRRWWGNBSQSBAM-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000007769 metal material Substances 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 4
- 230000007774 longterm Effects 0.000 description 4
- 238000005253 cladding Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 239000011253 protective coating Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009377 nuclear transmutation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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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
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Life Sciences & Earth Sciences (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention provides a static multi-sample lead bismuth corrosion test device and a test method, and belongs to the field of lead bismuth corrosion tests. Solves the problem that the prior static multi-sample lead bismuth corrosion test cannot be performed. The test device comprises a sample loading frame and a quartz tube, wherein the sample loading frame comprises a plurality of spacers and a plurality of supporting columns, the spacers are arranged at equal intervals, the spacers are connected with each other through the supporting columns, a corrosion sample is placed on the spacers, the sample loading frame is placed in the quartz tube, a lead-bismuth alloy is placed in the quartz tube, one end of the quartz tube is sealed, the other end of the quartz tube is open, and the open end of the quartz tube is sealed through the sealed quartz column. The method is mainly used for static multi-sample lead bismuth corrosion test.
Description
Technical Field
The invention belongs to the field of lead bismuth corrosion testing, and particularly relates to a static multi-sample lead bismuth corrosion testing device and a testing method.
Background
The pursuit of safe, stable, economical and sustainable power supply is a continuous pursuit of various countries, and nuclear power generation has the outstanding advantages of stable power output, safe, controllable and sustainable supply, and the like, and meets the requirement exactly. Currently, nuclear power generation technology has been developed to fourth generation nuclear reactor technology, and among six alternative fourth generation nuclear reactors, lead-cooled fast reactors are attracting attention from scientists due to their more excellent safety and stability.
The operating temperature of the lead cooled fast reactor is up to 450-550 ℃, and the long-term service performance and safety of the fuel cladding structure material are important considerations. The lead bismuth alloy is the first choice coolant for the lead cold fast reactor because of the outstanding advantages of low melting point, high boiling point, stable chemical property, strong transmutation capability, good neutron economy and the like. The fuel cladding metal material in a lead-cooled fast reactor is subject to the strong corrosion action of lead-bismuth alloy to cause the material to fail, so that the corrosion behavior of the fuel cladding structural material in a liquid lead-bismuth environment is necessary to be studied. The corrosion behavior of materials in the liquid lead bismuth alloy environment mainly includes dissolution corrosion, oxidation corrosion, abrasion corrosion and erosion corrosion, wherein dissolution corrosion is one of the most critical factors causing material failure. However, the related test technology is still not mature, and no adequate report on a lead-bismuth corrosion test method of multiple samples exists.
Disclosure of Invention
In view of the above, the invention aims to provide a static multi-sample lead-bismuth corrosion test device and a test method, which are used for solving the problem that the static multi-sample lead-bismuth corrosion test cannot be performed at present.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the utility model provides a static many samples plumbous bismuth corrosion test device, it includes dress appearance frame and quartz capsule, dress appearance frame includes a plurality of spacers and a plurality of support column, a plurality of spacers equidistant settings, link to each other through a plurality of support columns between a plurality of spacers, place the corrosion sample on the spacer, dress appearance frame is placed in the quartz capsule, place plumbous bismuth alloy in the quartz capsule, quartz capsule one end is sealed, and the other end opening, open end are sealed through sealed quartz capsule.
Furthermore, the spacers and the supporting columns are made of quartz, and the lead-bismuth alloy is in a columnar structure.
Further, the support columns are parallel to each other and the spacers are uniformly and symmetrically distributed along the circumferential direction.
Still further, the support column includes fixed support column and dismantles the support column, fixed support column links to each other with the spacer is fixed, dismantlement support column can dismantle with the spacer and be connected.
Furthermore, the opening end of the quartz tube is provided with a necking structure, and the sealed quartz column is arranged on the necking structure.
Further, the test device also comprises a vacuum tube sealing machine and a vertical box type furnace, wherein the vacuum tube sealing machine seals the quartz tube, and the sealed quartz tube is placed in the vertical box type furnace.
Furthermore, the vacuum tube sealing machine comprises a vacuumizing system and a heating and melting system, wherein the vacuumizing system vacuumizes the quartz tube, the heating and melting system heats and melts the sealed quartz column, the vacuumizing system is a high-vacuum molecular pump set, and the heating and melting system adopts hydrogen flame as a heating source.
Furthermore, the vertical box furnace uses a K-type thermocouple to control the temperature, and the heating element is doped with ferromolybdenum and chromium aluminum.
The invention also provides a test method of the static multi-sample lead bismuth corrosion test device, which comprises the following steps:
step 1: placing a sample loading frame with a corrosion sample into a quartz tube, placing a weighed lead-bismuth alloy into the quartz tube, and sealing the open end of the quartz tube by using a quartz column;
step 2: starting a vacuum tube sealing machine, vacuumizing the quartz tube and simultaneously burning and melting the quartz column and the quartz tube until the quartz column and the quartz tube are completely sealed;
step 3: and placing the sealed quartz tube into a quartz tube lofting frame, placing the quartz tube lofting frame into a vertical box-type furnace for heating until the set time is reached, and researching the corrosion behavior of the sample in a static environment.
Further, the oxygen concentration in the quartz tube is 10 -5 wt%, the quartz tube was heated to 550 ℃ in a vertical box furnace.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a corrosion testing device and a testing method in a high-temperature liquid lead bismuth environment, which are suitable for testing the dissolution corrosion of a sample in the liquid lead bismuth environment, can be used for developing the corrosion performance testing research of multiple samples of metal materials under a static working condition, and provide technical support for accelerating the lead-cooled fast reactor to commercial application. The corrosion behavior research of the multi-sample metal material or the surface protective coating in a static high-temperature liquid lead bismuth environment is realized, and the dissolution and corrosion resistance of the sample in the lead bismuth solution is evaluated.
The invention can study the corrosion behavior of the metal material or the surface protective coating in the high-temperature liquid lead bismuth environment and evaluate the corrosion resistance of the metal material at high temperature.
According to the invention, the quartz tube is matched with the sample loading frame, so that the number of samples for lead-bismuth corrosion test can be effectively increased, the occupied area is small, and the device for realizing the lead-bismuth corrosion test of multiple samples is less in current report.
The quartz tube and the quartz column are both made of quartz materials, the fusion bonding effect among the quartz tube and the quartz column is guaranteed, the sealing is performed in a mode of vacuumizing and fusing simultaneously, the cost is low, the operation is simple and easy to operate, the sealing effect is good, and the appearance is concise and elegant.
The quartz support column of the sample loading frame can be adjusted, and samples with different sizes can be put in, so that the requirements on the size of the samples are effectively reduced; meanwhile, the sample can be separated from each other by the sample holder interlayer, so that the mutual influence of different samples due to the fact that the samples are not used in a corrosion state is avoided.
The quartz tube and the quartz column used in the invention have good chemical stability at 450-550 ℃, can ensure long-term service and can not generate impurities to influence the corrosion state of the sample.
The test device has the advantages of simple structure, easy operation, and low cost; the appearance is simple and elegant, the inner wall of the quartz material ensures that the lead-bismuth corrosion can be effectively resisted at the high temperature of 450-550 ℃, and the method is suitable for static lead-bismuth corrosion test of multiple samples.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of a static multi-sample lead bismuth corrosion test device according to the present invention;
fig. 2 is a schematic structural diagram of a sample holder in the static multi-sample lead bismuth corrosion test device according to the present invention.
1-corrosion sample, 2-fixed support column, 3-spacer, 4-disassembly support column, 5-sample loading frame, 6-lead bismuth alloy, 7-quartz tube and 8-sealed quartz column.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It should be noted that, in the case of no conflict, embodiments of the present invention and features of the embodiments may be combined with each other, and the described embodiments are only some embodiments of the present invention, not all embodiments.
Referring to fig. 1-2 for describing the embodiment, a static multi-sample lead bismuth corrosion test device comprises a sample loading frame 5 and a quartz tube 7, wherein the sample loading frame 5 comprises a plurality of spacers 3 and a plurality of support columns, the spacers 3 are arranged at equal intervals, the spacers 3 are connected through the support columns, a corrosion sample 1 is placed on the spacers 3, the sample loading frame 5 is placed in the quartz tube 7, a lead bismuth alloy 6 is placed in the quartz tube 7, one end of the quartz tube 7 is sealed, the other end of the quartz tube is open, and the open end of the quartz tube is sealed through a sealed quartz column 8.
The spacer 3 and the support columns are made of quartz, can withstand the high temperature of 550 ℃ for a long time, the lead bismuth alloy 6 is of a columnar structure, the support columns are parallel to each other and the spacer 3 is uniformly and symmetrically distributed along the circumferential direction, and the number of the support columns is preferably six. The support column includes fixed support column 2 and dismantles support column 4, fixed support column 2 links to each other with the spacer 3 is fixed, dismantlement support column 4 can dismantle with spacer 3 and be connected, and the quartz support column of dress appearance frame 5 same one side's three is for dismantling support column 4, the lofting of being convenient for.
The opening end of the quartz tube 7 is provided with a necking structure, the sealed quartz column 8 is arranged on the necking structure, and the necking structure can be used for fixing the sealed quartz column 8 and preventing the sealed quartz column 8 from sliding downwards; sealing is achieved by burning the fused silica tube 7 and sealing the silica column 8 using a vacuum tube sealer and then cooling.
The test device further comprises a vacuum tube sealing machine and a vertical box-type furnace, the vacuum tube sealing machine seals the quartz tube 7, and the sealed quartz tube 7 is placed in the vertical box-type furnace.
The vacuum tube sealing machine comprises a vacuum pumping system and a heating and melting system, wherein the vacuum pumping system is used for vacuumizing the quartz tube 7, the heating and melting system is used for heating and melting the sealed quartz column 8,the vacuumizing system is a high-vacuum molecular pump group, and can realize 10 at most -6 The heating and melting system adopts hydrogen flame as a heating source, and the vacuumizing system and the heating and melting system work cooperatively, and melt while vacuumizing, so as to realize the sealing of the quartz tube 7.
The vertical box-type furnace uses a K-type thermocouple to control the temperature, and the heating element is doped with ferromolybdenum and chromium aluminum. The sealed quartz tubes 7 are placed in a vertical box-type furnace surrounded by heating elements, and a long-term stable high-temperature environment is provided by the vertical box-type furnace. The temperature fluctuation range of the vertical box-type furnace is within +/-5 ℃, a K-type thermocouple is used, and the long-term working temperature is 1100 ℃.
The embodiment is a test method of a static multi-sample lead bismuth corrosion test device, which comprises the following steps:
step 1: placing the sample loading frame 5 with the corrosion sample 1 placed in a quartz tube 7, placing the weighed columnar lead bismuth alloy 6 in the quartz tube 7, and sealing the open end of the quartz tube 7 by using a quartz column 8;
step 2: starting a vacuum tube sealing machine, vacuumizing the quartz tube 7, and simultaneously fusing the quartz column 8 and the quartz tube 7, wherein the quartz is fused while vacuumizing, and the oxygen concentration pumped into the quartz tube 7 is 10 -5 The constant speed rate extraction can be kept at the weight percent until the quartz column 8 and the quartz tube 7 are completely sealed;
step 3: and sequentially placing the sealed quartz tubes 7 into a quartz tube lofting frame, sequentially placing the quartz tube lofting frames into a vertical box furnace for heating to 550 ℃, and placing the quartz tubes in the vertical box furnace for corresponding time according to the requirement to study the corrosion behavior of the sample in a static environment for a long time.
The embodiments of the invention disclosed above are intended only to help illustrate the invention. The examples are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention.
Claims (9)
1. A static multi-sample lead bismuth corrosion test device is characterized in that: it includes dress appearance frame (5) and quartz capsule (7), dress appearance frame (5) include a plurality of spacers (3) and a plurality of support column, equidistant setting of a plurality of spacers (3), link to each other through a plurality of support columns between a plurality of spacers (3), place corrosion sample (1) on spacer (3), dress appearance frame (5) are placed in quartz capsule (7), place plumbous bismuth alloy (6) in quartz capsule (7), quartz capsule (7) one end is sealed, and the other end opening, and the open end is sealed through sealed quartz capsule (8), spacer (3) and support column are quartz, plumbous bismuth alloy (6) are columnar structure.
2. The static multi-sample lead bismuth corrosion test apparatus according to claim 1, wherein: the support columns are parallel to each other, and the spacers (3) are uniformly and symmetrically distributed along the circumferential direction.
3. The static multi-sample lead bismuth corrosion test apparatus according to claim 1, wherein: the support column includes fixed support column (2) and dismantles support column (4), fixed support column (2) and spacer (3) are fixed to be connected, dismantlement support column (4) can dismantle with spacer (3) and be connected.
4. The static multi-sample lead bismuth corrosion test apparatus according to claim 1, wherein: the opening end of the quartz tube (7) is provided with a necking structure, and the sealed quartz column (8) is arranged on the necking structure.
5. The static multi-sample lead bismuth corrosion test apparatus according to claim 1, wherein: the test device further comprises a vacuum tube sealing machine and a vertical box-type furnace, the vacuum tube sealing machine seals the quartz tube (7), and the sealed quartz tube (7) is placed in the vertical box-type furnace.
6. The static multi-sample lead bismuth corrosion test apparatus according to claim 5, wherein: the vacuum tube sealing machine comprises a vacuumizing system and a heating and melting system, wherein the vacuumizing system vacuumizes the quartz tube (7), the heating and melting system heats and melts the sealed quartz column (8), the vacuumizing system is a high-vacuum molecular pump group, and the heating and melting system adopts hydrogen flame as a heating source.
7. The static multi-sample lead bismuth corrosion test apparatus according to claim 5, wherein: the vertical box-type furnace uses a K-type thermocouple to control the temperature, and the heating element is doped with ferromolybdenum and chromium aluminum.
8. A test method of the static multi-sample lead bismuth corrosion test apparatus as claimed in claim 1, wherein: it comprises the following steps:
step 1: placing a sample loading frame (5) with a corrosion sample (1) placed therein into a quartz tube (7), placing a weighed lead-bismuth alloy (6) into the quartz tube (7), and sealing the open end of the quartz tube (7) by using a quartz column (8);
step 2: starting a vacuum tube sealing machine, vacuumizing the quartz tube (7) and simultaneously burning the quartz column (8) and the quartz tube (7) until the quartz column (8) and the quartz tube (7) are completely sealed;
step 3: and (3) placing the sealed quartz tube (7) into a quartz tube lofting frame, placing the quartz tube lofting frame into a vertical box-type furnace for heating, and researching the corrosion behavior of the sample in a static environment until the set time is reached.
9. The test method of the static multi-sample lead bismuth corrosion test apparatus according to claim 8, wherein the test method comprises the steps of: the oxygen concentration in the quartz tube (7) is 10 -5 And (c) heating the quartz tube (7) to 550 ℃ in a vertical box furnace.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210560493.9A CN115112547B (en) | 2022-05-23 | 2022-05-23 | Static multi-sample lead-bismuth corrosion test device and test method |
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| CN202210560493.9A CN115112547B (en) | 2022-05-23 | 2022-05-23 | Static multi-sample lead-bismuth corrosion test device and test method |
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| CN115112547B true CN115112547B (en) | 2023-10-27 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010038719A (en) * | 2008-08-05 | 2010-02-18 | Miwa Seisakusho:Kk | Manufacturing method of sample housing container made of quartz and manufacturing apparatus of sample housing container made of quartz |
| CN103364332A (en) * | 2013-07-12 | 2013-10-23 | 中国核动力研究设计院 | Special sample rack for corrosion test outside nuclear material stack |
| CN103439227A (en) * | 2013-09-09 | 2013-12-11 | 中国原子能科学研究院 | Liquid lithium lead compatibility static testing device |
| CN209690141U (en) * | 2019-03-08 | 2019-11-26 | 华北电力大学 | Liquid metal static corrosion laboratory sample frame |
| CN112414927A (en) * | 2020-11-06 | 2021-02-26 | 中国科学院金属研究所 | Universal method for researching corrosion behavior of structural material in lead-bismuth alloy melt |
| CN214668468U (en) * | 2020-11-06 | 2021-11-09 | 中国科学院金属研究所 | Device for researching corrosion behavior of structural material in lead-bismuth alloy melt |
-
2022
- 2022-05-23 CN CN202210560493.9A patent/CN115112547B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010038719A (en) * | 2008-08-05 | 2010-02-18 | Miwa Seisakusho:Kk | Manufacturing method of sample housing container made of quartz and manufacturing apparatus of sample housing container made of quartz |
| CN103364332A (en) * | 2013-07-12 | 2013-10-23 | 中国核动力研究设计院 | Special sample rack for corrosion test outside nuclear material stack |
| CN103439227A (en) * | 2013-09-09 | 2013-12-11 | 中国原子能科学研究院 | Liquid lithium lead compatibility static testing device |
| CN209690141U (en) * | 2019-03-08 | 2019-11-26 | 华北电力大学 | Liquid metal static corrosion laboratory sample frame |
| CN112414927A (en) * | 2020-11-06 | 2021-02-26 | 中国科学院金属研究所 | Universal method for researching corrosion behavior of structural material in lead-bismuth alloy melt |
| CN214668468U (en) * | 2020-11-06 | 2021-11-09 | 中国科学院金属研究所 | Device for researching corrosion behavior of structural material in lead-bismuth alloy melt |
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