CN113138137A - Silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method - Google Patents
Silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method Download PDFInfo
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- CN113138137A CN113138137A CN202010050912.5A CN202010050912A CN113138137A CN 113138137 A CN113138137 A CN 113138137A CN 202010050912 A CN202010050912 A CN 202010050912A CN 113138137 A CN113138137 A CN 113138137A
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- 238000001514 detection method Methods 0.000 title claims abstract description 36
- 239000000919 ceramic Substances 0.000 title claims abstract description 29
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 28
- 230000007797 corrosion Effects 0.000 title claims abstract description 27
- 238000005260 corrosion Methods 0.000 title claims abstract description 27
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 239000008188 pellet Substances 0.000 title claims abstract description 25
- 239000000758 substrate Substances 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 44
- 229910052786 argon Inorganic materials 0.000 claims description 22
- 229910052593 corundum Inorganic materials 0.000 claims description 17
- 239000010431 corundum Substances 0.000 claims description 17
- 230000002572 peristaltic effect Effects 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 2
- 230000002277 temperature effect Effects 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000009462 micro packaging Methods 0.000 description 1
- GALOTNBSUVEISR-UHFFFAOYSA-N molybdenum;silicon Chemical group [Mo]#[Si] GALOTNBSUVEISR-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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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
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- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Environmental & Geological Engineering (AREA)
- Environmental Sciences (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
Abstract
The invention relates to the technical field of high-temperature steam corrosion detection, and particularly discloses a silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and a method. The detection device provided by the invention has the advantages that the temperature change is small in the high-temperature test of the silicon carbide matrix ceramic core block, the influence of the introduced water vapor on the temperature of the equipment is small through the control of the gas flowmeter, the integral constant temperature effect is good, and the judgment of the oxidation resistance of the material through measuring the weight change and the color change of the sample before and after oxidation is realized.
Description
Technical Field
The invention belongs to the technical field of high-temperature steam corrosion detection, and particularly relates to a silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method.
Background
The water/steam corrosion test is currently performed primarily with reference to ASTM G2/G2M-06, U.S. Standard test method for corrosion testing of zirconium, hafnium and their alloys products in either steam at 750F. [400 ℃ C.) or water at 680F. [360 ℃ C.). ASTM practice requires a standard to be reviewed every five years to ensure sufficiency of its technical content.
Only two test conditions of 400 ℃, 10.3MPa steam neutralization and 360 ℃ and 18.7MPa water are specified in the standard, and the test time is 3 days in general. In practical application, various countries, departments and units can adjust the temperature, pressure, time, medium and the like of corrosion according to actual needs.
Because the corrosion temperature of the silicon carbide matrix ceramic core block is as high as 1500 ℃, and certain flow of water vapor is required to be continuously input under the constant temperature state, no special high-temperature steam corrosion detection device for the silicon carbide matrix ceramic core block exists at present.
Therefore, it is desirable to design a detection apparatus and a detection method to solve the above problems.
Disclosure of Invention
The invention aims to provide a silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and a method, which are used for realizing a high-temperature steam oxidation test on a silicon carbide ceramic matrix dispersion fuel pellet.
The technical scheme of the invention is as follows:
a silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device is sequentially connected with a peristaltic pump, a steam generator and a tubular furnace through a gas path pipeline, and a vacuum pump is further arranged at the inlet end of the tubular furnace;
the inlet end of the tube furnace is provided with a tube furnace inlet valve, and the outlet end of the tube furnace is provided with a tube furnace outlet valve;
the peristaltic pump is used for injecting deionized water into the steam generator;
the steam generator is used for generating steam and injecting the steam into the tubular furnace through the control of the inlet valve of the tubular furnace;
the vacuum pump is used for vacuumizing the tube furnace before injecting water vapor.
The tube furnace adopts a double-layer furnace shell structure, the hearth is integrated, and a fan is arranged between the double-layer furnace shells.
The silicon carbide substrate ceramic pellet sample to be detected is placed in the middle of a corundum tube of a tubular furnace to ensure that the sample is in a hearth constant-temperature area, and stainless steel end sockets are arranged at two ends of the corundum tube for sealing.
During detection, steam is introduced into the corundum tube of the tube furnace through the steam generator, a temperature rise curve in the tube furnace is set through the temperature control system, and the circuit automatically rises to a temperature range required by a test, so that the corundum tube of the tube furnace can achieve a test environment surrounded by high temperature and steam.
A silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method based on the detection device comprises the following steps:
step 1: placing the weighed samples on a sample boat, avoiding the contact between adjacent samples when placing, then slowly pushing the sample boat into a corundum tube of the tube furnace, and installing a heat insulation block and an outlet baffle of the tube furnace;
step 2: closing an outlet valve of the tube furnace, starting a vacuum pump, opening an inlet valve of the tube furnace, introducing argon into the tube furnace through an external argon bottle, then closing the inlet valve of the tube furnace and the argon, and opening the outlet valve of the tube furnace to realize vacuum pumping of the interior of the tube furnace;
closing the vacuum pump and disconnecting the vacuum pump from the tubular furnace, then closing an outlet valve of the tubular furnace, and connecting the outlet valve of the tubular furnace with a steam exhaust pipe to the outside;
and step 3: setting the target temperature and the heat preservation time of the tube furnace, and starting heating to enable the corundum tube of the tube furnace to reach a high-temperature test environment surrounded by water vapor;
and 4, step 4: when the heat preservation time reaches the set time, the temperature control system of the tube furnace automatically stops heating; closing the peristaltic pump, continuously introducing argon for 10-20 min, closing the argon, the inlet valve of the tube furnace and the outlet valve of the tube furnace, and naturally cooling;
and 5: and after the temperature in the tubular furnace is reduced to below 150 ℃, opening an outlet valve of the tubular furnace, detaching an outlet baffle of the tubular furnace, taking out the heat insulation block and the sample boat, and cooling the sample to room temperature for quality measurement.
In step 1, the samples are marked on the sample boat by marking or according to the placing sequence.
In the step 2, the pressure of introducing argon into the tube furnace is not more than 0.1 MPa.
In the step 3, the temperature of a heat tracing band of the steam generator and the steam output pipe is set to be 120 ℃, a heat tracing band heating switch is started, and after the steam generator is heated to 120 ℃, a peristaltic pump is started to inject deionized water into the steam generator;
and opening an inlet valve of the tube furnace, adjusting the flow of argon, opening an outlet valve of the tube furnace after the pressure in the tube furnace is positive pressure, and maintaining the normal pressure in the tube furnace.
In the step 3, the flow rate of the deionized water injected into the steam generator is set to be 0.5-1 mL/min.
In the step 3, the flow of argon gas is adjusted to be 20-30L/min.
The invention has the following remarkable effects:
(1) the invention realizes the steam oxidation test of the silicon carbide substrate ceramic pellet with the temperature not lower than 1500 ℃ by adding the devices such as the vacuum pump, the steam generator and the like to the common tube furnace in ingenious connection, not only meets the detection conditions of vacuumizing and injecting steam with the flow rate set to be 0.5-1 mL/min, but also establishes a reliable detection method.
(2) The detection device provided by the invention has the advantages that the temperature change is small in the high-temperature test of the silicon carbide matrix ceramic core block, the influence of the introduced water vapor on the temperature of the equipment is small through the control of the gas flowmeter, the integral constant temperature effect is good, and the judgment of the oxidation resistance of the material through measuring the weight change and the color change of the sample before and after oxidation is realized.
Drawings
FIG. 1 is a schematic view of a high-temperature steam corrosion detection apparatus according to the present invention.
In the figure: 1. a tube furnace; 2. a steam generator; 3. a peristaltic pump; 4. a vacuum pump.
Detailed Description
The invention is described in further detail below with reference to the figures and the embodiments.
As shown in figure 1, the silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device is sequentially connected with a peristaltic pump 3, a steam generator 2 and a tubular furnace 1 through a gas pipeline, and a vacuum pump 4 is further arranged at the inlet end of the tubular furnace 1, so that a high-temperature steam oxidation test of the fully ceramic micro-packaging pellets at a temperature not lower than 1500 ℃ can be completed.
The inlet end of the tube furnace 1 is provided with a tube furnace inlet valve, and the outlet end of the tube furnace 1 is provided with a tube furnace outlet valve.
The peristaltic pump 3 is used for injecting deionized water into the steam generator 2.
The steam generator 2 is used for generating steam, and the steam is injected into the tube furnace 1 through a tube furnace inlet valve control.
The vacuum pump 4 is used for vacuumizing the tube furnace 1 before injecting water vapor.
The tubular furnace 1 adopts a double-layer furnace shell structure, the hearth is integrated, the fan is arranged between the double-layer furnace shells, the temperature can be increased and decreased rapidly, and the surface temperature of the furnace shells is low.
The tubular furnace 1 is characterized in that a heating element is a silicon-molybdenum rod, a temperature measuring element is a B-type double-platinum cauterized thermocouple, a temperature control system adopts an artificial intelligence adjusting technology, the control precision of an instrument is +/-1 ℃, the instrument has PID adjusting, fuzzy control and self-adjusting capabilities, various temperature rising programs can be programmed, and the tubular furnace has an ultrahigh temperature alarm function, a thermocouple damage power-off function and a built-in parameter password control function.
The tube furnace 1 is provided with an RS-485 communication interface and data management software, and has the functions of paperless recording of historical data, temperature rise curve and correction of temperature deviation.
The silicon carbide substrate ceramic pellet sample to be detected is placed in the middle of a corundum tube of the tubular furnace 1 to ensure that the sample is in a hearth constant-temperature area, and stainless steel end sockets are arranged at two ends of the corundum tube for sealing.
During detection, steam is introduced into the corundum tube of the tube furnace 1 through the steam generator 2, a temperature rise curve in the tube furnace 1 is set through the temperature control system, and the circuit automatically rises to a temperature range required by a test, so that the corundum tube of the tube furnace 1 reaches a test environment surrounded by high temperature and steam.
A silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method adopts the detection device for detection, and comprises the following steps:
step 1: placing the weighed samples on a sample boat, avoiding the contact between the two samples during placement, then slowly pushing the sample boat into a corundum tube of the tube furnace 1, and installing a heat insulation block and a tube furnace outlet baffle;
marking the samples by marking numbers on the sample boat or according to the placing sequence;
step 2: closing an outlet valve of the tube furnace, starting a vacuum pump 4, opening an inlet valve of the tube furnace, introducing argon gas into the tube furnace 1 through an external argon gas bottle, wherein the pressure is not more than 0.1MPa, then closing the inlet valve of the tube furnace and the argon gas, and opening the outlet valve of the tube furnace to realize vacuum pumping of the interior of the tube furnace 1;
closing the vacuum pump 4 and disconnecting the vacuum pump from the tubular furnace 1, then closing an outlet valve of the tubular furnace, and connecting the outlet valve of the tubular furnace with a steam exhaust pipe to the outside;
and step 3: setting the target temperature of the tube furnace 1 to be 1500 ℃, setting the heat preservation time to be 8h, and starting heating; setting the temperature of a heat tracing band of the steam generator 2 and a steam output pipe to be 120 ℃, starting a heat tracing band heating switch, after the steam generator 2 is heated to be 120 ℃, starting a peristaltic pump 3 to inject deionized water into the steam generator 2, and setting the flow rate to be 0.5-1 mL/min; opening an inlet valve of the tube furnace, adjusting the flow of argon gas to be 20-30L/min, opening an outlet valve of the tube furnace after the pressure in the tube furnace 1 is positive pressure, and maintaining the normal pressure in the tube furnace 1;
and 4, step 4: when the heat preservation time reaches the set time, the temperature control system of the tube furnace 1 automatically stops heating; closing the peristaltic pump 3, continuously introducing argon for 10-20 min, closing the argon, the inlet valve of the tube furnace and the outlet valve of the tube furnace, and naturally cooling;
and 5: and (3) after the temperature in the tube furnace 1 is reduced to below 150 ℃, opening an outlet valve of the tube furnace, detaching an outlet baffle of the tube furnace, taking out the heat insulation block and the sample boat, and cooling the sample to room temperature for mass measurement.
Claims (10)
1. The utility model provides a carborundum matrix ceramic pellet high temperature steam corrosion detection device which characterized in that: the peristaltic pump (3), the steam generator (2) and the tubular furnace (1) are sequentially connected through a gas pipeline, and a vacuum pump (4) is arranged at the inlet end of the tubular furnace (1);
the inlet end of the tube furnace (1) is provided with a tube furnace inlet valve, and the outlet end of the tube furnace (1) is provided with a tube furnace outlet valve;
the peristaltic pump (3) is used for injecting deionized water into the steam generator (2);
the steam generator (2) is used for generating steam and injecting the steam into the tubular furnace (1) through the control of a tubular furnace inlet valve;
the vacuum pump (4) is used for vacuumizing the tube furnace (1) before injecting water vapor.
2. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection device as claimed in claim 1, wherein: the tube furnace (1) adopts a double-layer furnace shell structure, the hearth is integrated, and a fan is arranged between the double-layer furnace shells.
3. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection device as claimed in claim 2, wherein: the silicon carbide substrate ceramic pellet sample to be detected is placed in the middle of a corundum tube of the tubular furnace (1) to ensure that the sample is in a hearth constant-temperature area, and stainless steel end sockets are arranged at two ends of the corundum tube for sealing.
4. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection device as claimed in any one of claims 1 to 3, wherein: during detection, steam is introduced into the corundum tube of the tube furnace (1) through the steam generator (2), a temperature rise curve in the tube furnace (1) is set through the temperature control system, the circuit automatically rises to a temperature range required by a test, and therefore the corundum tube of the tube furnace (1) achieves a test environment surrounded by high temperature and steam.
5. A silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method based on the detection device of claim 4 is characterized in that: the method comprises the following steps:
step 1: placing the weighed samples on a sample boat, avoiding the contact between adjacent samples when placing, then slowly pushing the sample boat into a corundum tube of the tube furnace (1), and installing a heat insulation block and a tube furnace outlet baffle;
step 2: closing an outlet valve of the tubular furnace, starting a vacuum pump (4), opening an inlet valve of the tubular furnace, introducing argon into the tubular furnace (1) through an external argon bottle, then closing the inlet valve of the tubular furnace and the argon, and opening the outlet valve of the tubular furnace to realize vacuum pumping of the interior of the tubular furnace (1);
the vacuum pump (4) is closed and disconnected with the tubular furnace (1), then the outlet valve of the tubular furnace is closed, and the outlet valve of the tubular furnace is connected with a steam exhaust pipe and communicated to the outside;
and step 3: setting the target temperature and the heat preservation time of the tubular furnace (1), and starting heating to enable the corundum tube of the tubular furnace (1) to reach a high-temperature test environment surrounded by water vapor;
and 4, step 4: when the heat preservation time reaches the set time, the temperature control system of the tube furnace (1) automatically stops heating; closing the peristaltic pump (3), continuously introducing argon for 10-20 min, then closing the argon, the inlet valve of the tube furnace and the outlet valve of the tube furnace, and naturally cooling;
and 5: and (3) after the temperature in the tube furnace (1) is reduced to below 150 ℃, opening an outlet valve of the tube furnace, detaching an outlet baffle of the tube furnace, taking out the heat insulation block and the sample boat, cooling the sample to room temperature, and measuring the mass.
6. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method as claimed in claim 5, wherein: in step 1, the samples are marked on the sample boat by marking or according to the placing sequence.
7. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method as claimed in claim 5, wherein: in the step 2, the pressure of introducing argon into the tube furnace (1) is not more than 0.1 MPa.
8. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method as claimed in claim 5, wherein: in the step 3, the temperature of a heat tracing band of the steam generator (2) and the steam output pipe is set to be 120 ℃, a heat tracing band heating switch is started, and after the steam generator (2) is heated to be 120 ℃, a peristaltic pump (3) is started to inject deionized water into the steam generator (2); and opening an inlet valve of the tube furnace, adjusting the flow of argon, opening an outlet valve of the tube furnace after the pressure in the tube furnace (1) is positive pressure, and maintaining the normal pressure in the tube furnace (1).
9. The silicon carbide matrix ceramic pellet high-temperature steam corrosion detection method according to claim 8, wherein the method comprises the following steps: in the step 3, the flow rate of the deionized water injected into the steam generator (2) is set to be 0.5-1 mL/min.
10. The silicon carbide matrix ceramic pellet high temperature steam corrosion detection method of claim 9, wherein: in the step 3, the flow of argon gas is adjusted to be 20-30L/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010050912.5A CN113138137A (en) | 2020-01-17 | 2020-01-17 | Silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010050912.5A CN113138137A (en) | 2020-01-17 | 2020-01-17 | Silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method |
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| CN113138137A true CN113138137A (en) | 2021-07-20 |
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| CN202010050912.5A Pending CN113138137A (en) | 2020-01-17 | 2020-01-17 | Silicon carbide substrate ceramic pellet high-temperature steam corrosion detection device and method |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204314199U (en) * | 2014-12-09 | 2015-05-06 | 华电电力科学研究院 | The metal material high temperature water vapor oxidation experiment device that a kind of laboratory uses |
| CN106769822A (en) * | 2017-01-11 | 2017-05-31 | 东南大学 | A kind of high-temperature corrosion testing system |
| CN109357993A (en) * | 2018-09-28 | 2019-02-19 | 中国人民解放军第五七九工厂 | Three temperature section water oxygen of carborundum based material couples corrosion device |
-
2020
- 2020-01-17 CN CN202010050912.5A patent/CN113138137A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204314199U (en) * | 2014-12-09 | 2015-05-06 | 华电电力科学研究院 | The metal material high temperature water vapor oxidation experiment device that a kind of laboratory uses |
| CN106769822A (en) * | 2017-01-11 | 2017-05-31 | 东南大学 | A kind of high-temperature corrosion testing system |
| CN109357993A (en) * | 2018-09-28 | 2019-02-19 | 中国人民解放军第五七九工厂 | Three temperature section water oxygen of carborundum based material couples corrosion device |
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Application publication date: 20210720 |