CN103335937A - Simulation and accelerated testing device and method for oxidation performance of high-temperature-resisting water vapor - Google Patents
Simulation and accelerated testing device and method for oxidation performance of high-temperature-resisting water vapor Download PDFInfo
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- CN103335937A CN103335937A CN201310249884XA CN201310249884A CN103335937A CN 103335937 A CN103335937 A CN 103335937A CN 201310249884X A CN201310249884X A CN 201310249884XA CN 201310249884 A CN201310249884 A CN 201310249884A CN 103335937 A CN103335937 A CN 103335937A
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Abstract
The invention relates to a simulation and accelerated testing device for an oxidation performance of high-temperature-resisting water vapor. The simulation and accelerated testing device comprises a vapor generation mechanism and a high-temperature reaction furnace, wherein the vapor generation mechanism comprises a sealing container containing de-ionized water and a heating device for the sealing container; the sealing container is provided with an air inlet, an air outlet and a water inlet; the air inlet is connected with an argon bottle through an air inlet pipe and the air inlet pipe stretches to be below a liquid surface; the water inlet is connected with an automatic water supplementing mechanism, and the water outlet is connected with an inlet of the high-temperature reaction furnace through a pipeline. The invention further relates to a simulation and accelerated testing method for the oxidation performance of the high-temperature-resisting water vapor. The argon deoxidization and the generation of the water vapor in the device and the method disclosed by the invention are realized in one sealing container; a test of a metal test sample is only carried out in the high-temperature reaction furnace so that the aim of accurately experimenting is realized by adopting few laboratory equipment; the convenience of an experiment is greatly improved. The simulation and accelerated testing device and method disclosed by the invention can be applied to a high-temperature oxidization testing device.
Description
Technical field
The present invention relates to a kind of high temperature resistance steam oxidation performance simulation and accelerated test apparatus and method.
Background technology
Water or water vapor extensively are present in the industrial environment, as nuclear reactor, generating and space industry, petroleum and petrochemical industry field and solid fuel cell etc.And soft air has very big corrosivity to material, is having a strong impact on mechanical property and the life-span of alloy material, brings out industrial accident, and the harm personal safety causes enormous economic loss.How making metal material keep excellent performance under steam-laden high-temperature corrosion environment is an important problem that faces in the present industry.
Alleviating the global energy anxiety, reducing under an urgent demand of environmental pollution, development clean coal generation technology has become the task of top priority of countries in the world, utilizes further lifting boiler pressure and temperature parameter to reach exactly as the overcritical and ultra supercritical generation technology of one of clean coal generating major technique and improves unit efficiency and energy saving purposes.In view of the electric structure of China based on coal-fired fired power generating unit, so greatly develop and promote overcritical and the ultra supercritical generation technology not only very important but also very necessary.Summary operating experience in recent years as can be known, though the steel that superheater, reheater are selected for use develops into T22, T91, P91 and austenitic stainless steel TP304H, TP347H etc. from G102, but cause steam turbine solid particle erosion (SPE) accident still to happen occasionally owing to abominable Service Environment causes the serious steam oxidation corrosion of pipe material inner wall to cause the hard iron oxide particles that the inefficacy of boiler booster and superheater, reheater tube wall strip down, had a strong impact on security and economy that genset moves.
Therefore, the steam oxidation mechanism of this class material of necessary further investigation, in order to propose the effective measures that some are controlled oxide skin speeds of growth and peel off total amount from aspects such as boiler tube selection, operational factor control and material surface protection, for commercial production provides effective technical basis.But, if correlative study is based upon on the commercial production, required experimental period is long, the input human and material resources are big, maintenance cost is also higher, and that has particularly limited long experimental period experimental data exploitation is instructed to new material is ageing, can not satisfy the research and development demand, therefore, seek to reflect that the laboratory fast appraisement method of metal material high temperature resistance steam oxidation performance is very necessary.
Summary of the invention
In order to overcome above-mentioned technical matters, the object of the present invention is to provide a kind of high temperature resistance steam oxidation performance simulation and accelerated test apparatus and method, can in the laboratory, obtain the oxidation susceptibility of metal under high temperature, water vapor atmosphere fast, easily by these apparatus and method.
The technical solution adopted in the present invention is:
A kind of high temperature resistance steam oxidation performance simulation and accelerated test device, comprise that steam produces mechanism and high temperature reaction stove, described steam produces mechanism and comprises the airtight container that deionized water is housed and the heating arrangement that is used for airtight container, described airtight container is provided with air intake opening, gas outlet and water inlet, described air intake opening is connected to argon bottle by draft tube and described draft tube extends below the liquid level, described water inlet is connected to automatic water supplement mechanism, and described gas outlet is connected with the entrance of high temperature reaction stove by pipeline.
As further improvement in the technical proposal, the pipeline of described connection gas outlet and high temperature reaction stove is provided with for detection of the flowmeter that flows through gas.
As further improvement in the technical proposal, be provided with temperature monitoring mechanism in the described airtight container, described temperature monitoring mechanism comprise be positioned at liquid level above, be used for first thermometer of monitoring air outlet temperature and be positioned at second thermometer that liquid level is following, be used for monitoring deionized water temperature.
As further improvement in the technical proposal, the pipeline of described connection gas outlet and high temperature reaction stove is provided with for detection of the hygrometer that flows through gas and thermometer.
As further improvement in the technical proposal, described steam produces mechanism and comprises the ultrasound wave damping device that is arranged in the airtight container.
As further improvement in the technical proposal, described heating arrangement comprises the heating sheath that is coated on the airtight container outer wall.
As further improvement in the technical proposal, the outlet of described high temperature reaction stove is connected to vacuum pump.
The simulation of high temperature resistance steam oxidation performance and accelerated test method may further comprise the steps:
A. build experiment atmosphere: by steam produce mechanism make deionized water in the airtight container produce water vapor and with feed deionized water in after argon gas after the deoxidation mixes, feeding high temperature reaction stove 20～40min;
B. heating experiment: sample is put into high temperature reaction stove rear enclosed high temperature reaction stove and high temperature reaction stove is heated to working temperature, weighs through taking out sample behind the setting-up time;
C. repeating step a and b obtain the oxidation kinetics rule.
As further improvement in the technical proposal, among the described step a, the temperature of mixed gas is controlled at 80～90 ℃ by being installed in the thermometer that connects on airtight container gas outlet and the high temperature reaction stove inlet duct, and experiment atmosphere is by being installed in hygrometer and the flowmeter control that connects on airtight container gas outlet and the high temperature reaction stove inlet duct.
The invention has the beneficial effects as follows: the deionized water in the airtight container becomes behind the water vapor to mix with argon gas through the deionized water deoxidation and to feed in the high temperature reaction stove formation tests atmosphere, the test that test button can be carried out its oxidation susceptibility simulation and accelerate after being heated to suitable temperature and continuing the time of setting in high temperature reaction stove, because argon gas deoxidation in these apparatus and method, the formation of water vapor all realizes in an airtight container, and the test of test button is only in high temperature reaction stove, therefore adopt a spot of laboratory equipment can reach the purpose of accurate experiment, improved the convenience of experiment greatly.
Description of drawings
The present invention is further described below in conjunction with drawings and embodiments.
Fig. 1 is structural representation of the present invention;
Fig. 2 is T91 steel (Ar+10vol.%H under 650 ℃ ~ 800 ℃ temperature
2O) oxidation kinetics curve in the atmosphere.
Embodiment
As shown in Figure 1, a kind of high temperature resistance steam oxidation performance simulation and accelerated test device comprise that steam produces mechanism and high temperature reaction stove 1.Steam produces mechanism and comprises the airtight container 2 that deionized water is housed and the heating arrangement that is used for airtight container 2.Heating arrangement is the heating sheath 10 that is coated on airtight container 2 outer walls, on the one hand can be to airtight container 2 heating, also play a part heat insulationly on the other hand, and prevent the accidental injury to operating personnel.
Steam produces mechanism and also comprises the ultrasound wave damping device 9 that is arranged in the airtight container 2, according to the principle of ultrasound wave humidification, adopt ultrasound wave to produce water vapor, make that the water vapor generating capacity is controlled, and need not that water is heated to boiling point and also can produce water vapor, guaranteed required experimental temperature.
Airtight container 2 is provided with air intake opening, gas outlet and water inlet.Air intake opening is connected to argon bottle 3 by draft tube, and air inlet adjustment valve 12 and charge flow rate meter also are installed on the draft tube, and the charge flow rate meter is used for the argon flow amount that statistics is used.Draft tube extends below the liquid level, makes argon gas enter in the deionized water and just enters next process procedure after the deoxidation.
The water inlet of airtight container 2 is connected to automatic water supplement mechanism.This automatic water supplement mechanism is made up of motorized valve 13, liquid level gauge 14, controller 15 and water tank 16.Wherein, motorized valve 13 is installed in the pipeline that connects water inlet and water tank 16, and liquid level gauge 14 is installed in the airtight container 2, and motorized valve 13, liquid level gauge 14 are electrically connected with controller 15 respectively.Its principle of work is, liquid level gauge 14 sends the instruction of opening motorized valve 13 by controller 15 after detecting the signal of water level deficiencies in the airtight container 2, and water tank 16 reaches setting value for airtight container 2 moisturizings detect water level up to liquid level gauge 14, and motorized valve 13 cuts out.
The gas outlet of airtight container 2 is connected by the entrance of pipeline with high temperature reaction stove 1.The mixed gas that produces in the airtight container 2 enters high temperature reaction stove 1 from above-mentioned pipeline, to build the experiment atmosphere of water vapor-argon gas.Simultaneously, before the experiment beginning, also can feed argon gas the air in the high temperature reaction stove 1 is discharged.
On the pipeline of connection gas outlet and high temperature reaction stove 1 reduction valve 17, mixed gas operation valve 18, thermometer 8, hygrometer 7 and flowmeter 4 are housed successively.Further accurately control the steam vapour amount that enters in the high temperature reaction stove 1 by flowmeter 4, and the detection of mixed gas makes required experiment condition precisely controlled in 8 pairs of pipes of hygrometer 7 and thermometer, thereby improve accuracy and the fiduciary level of experiment.The gas experiment condition can be regulated simultaneously by the aperture of airtight container 2 heating-up temperatures, water vapor generating capacity, argon gas supply and mixed gas operation valve 18 in the pipe.
Be provided with temperature monitoring mechanism in the airtight container 2, comprise being positioned at more than the liquid level, being used for first thermometer 5 of monitoring air outlet temperature and being positioned at second thermometer 6 that liquid level is following, be used for monitoring the deionized water temperature, be used for accuracy control over temperature.
High temperature silk hook 19 is housed in the high temperature reaction stove 1, and sample 20 is placed on the high temperature silk hook 19 and reacts.The outlet of high temperature reaction stove 1 is connected to vacuum pump 11, by vacuum pump 11 water vapor and argon gas is sucked high temperature reaction stove 1 back discharge.
The simulation of high temperature resistance steam oxidation performance and accelerated test method follow these steps to carry out:
At first with the sample machine cuts to given size, after sand papering, adopt the degreasing agent surface degreasing, anhydrous alcohol cleans the back and dries up sample with hair-dryer, adopt digimatic calipers to measure specimen size, standby with inserting in the drying basin preservation behind the electronic analytical balance weighing original weight;
Before the experiment beginning, start vacuum pump 11, use water tank 16 in airtight container 2, to add deionized water to the regulation liquid level, open air inlet adjustment valve 12, start ultrasound wave damping device 9, and the deionized water in the heated sealant container 2 is accurately controlled gas flow, temperature and humidity to reach experiment condition to working temperature by flowmeter 4, thermometer 8, hygrometer 7, guarantee the inner water vapor-argon gas experiment atmosphere that forms of device, continue about 30 minutes of ventilation.
Sample is hung on the high temperature silk hook 19, and good seal high temperature reaction stove 1, begin experiment after high temperature reaction stove 1 is heated to working temperature.Automatic water supplement mechanism controls the water level of deionized water in the airtight container 2 automatically, and experiment is taken out sample behind setting-up time point, weigh; Experiment obtains its oxidation kinetics rule after finishing, and adopts oxidation product analytical technology such as SED, XRD etc. that sample is carried out analysis-by-synthesis, obtains corresponding conclusion.
Wherein, the temperature of water vapor-argon gas is controlled at 80～90 ℃ by thermometer 8.
Embodiment 1:650 ℃ ~ 800 ℃, Ar+10vol.%H
2The high temperature resistance steam oxidation performance of T91 steel detects under the O condition.
Be detected object with the T91 steel, tested the high temperature resistance steam oxidation performance of T91 steel under 650 ℃, 700 ℃, 750 ℃, 800 ℃.
At first with sample to be evaluated by machine cuts to 10mm * 10mm * 2mm, surperficial ungrease treatment, standby with drying up after the alcohol wash at last.
Concrete operations are as follows:
1) starts vacuum pump 11;
2) open motorized valve 13 and in airtight container 2, add deionized water to the regulation liquid level, close motorized valve 13;
3) open air inlet adjustment valve 12, start ultrasound wave damping device 9, and the deionized water of heated sealant container 2 is to working temperature;
4) check thermometer 8, first thermometer 5 and second thermometer 6, control water vapor-temperature of argon gas is at 85 ℃; Check hygrometer 7, flowmeter 4, control experiment atmosphere is Ar+10vol.%H
2O continues about 30 minutes of ventilation.
5) sample 20 is hung on the high temperature silk hook 19, and good seal high temperature reaction stove 1, begin experiment after high temperature reaction stove 1 is heated to 650 ℃, 700 ℃, 750 ℃, 800 ℃.
6) take out sample 20 every 10h and weigh once, oxidation T.T. is 160h, obtains its oxidation kinetics rule.
As can be seen from Figure 2, in 650 ℃ ~ 800 ℃ temperature ranges, the high-temperature vapor oxidation kinetics of T91 steel is obeyed parabola rule substantially.
Embodiment 2:650 ℃, Ar+5vol.%H
2O/Ar and Ar+10vol.%H
2The high temperature resistance steam oxidation performance of T91 steel detects under the O condition.
As evaluation object, oxidizing temperature is 650 ℃ with the T91 steel, and comparative steel is at Ar+5vol.%H
2O, Ar+10vol.%H
2High temperature resistance steam oxidation performance under the O.
At first with sample to be evaluated by machine cuts to 10mm * 10mm * 2mm, surperficial ungrease treatment, standby with drying up after the alcohol wash at last.
Concrete operations are as follows:
1) starts vacuum pump 11;
2) open motorized valve 13 and in airtight container 2, add deionized water to the regulation liquid level, close motorized valve 13;
3) open air inlet adjustment valve 12, start ultrasound wave damping device 9, and the deionized water of heated sealant container 2 is to working temperature;
4) check thermometer 8, first thermometer 5 and second thermometer 6, control water vapor-temperature of argon gas is at 85 ℃; Check hygrometer 7, flowmeter 4, control experiment atmosphere is Ar+10vol.%H
2O and Ar+5vol.%H
2O continues about 30 minutes of ventilation.
5) sample 20 is hung on the high temperature silk hook 19, and good seal high temperature reaction stove 1, begin experiment after high temperature reaction stove 1 is heated to 650 ℃.
6) take out sample 20 every 2h and weigh once, oxidation T.T. 10h obtains its oxidation kinetics rule.
The result shows that the T91 steel is at 650 ℃ of following Ar+5vol.%H
2During oxidation, dynamics meets parabola rule substantially, at Ar+10vol.%H in the O atmosphere
2Meet the sectional parabola rule in the O atmosphere.
The above is the preferred embodiment of the present invention, and it does not constitute limiting the scope of the invention.
Claims (9)
1. a high temperature resistance steam oxidation performance is simulated and the accelerated test device, it is characterized in that: comprise that steam produces mechanism and high temperature reaction stove (1), described steam produces mechanism and comprises the airtight container (2) that deionized water is housed and the heating arrangement that is used for airtight container (2), described airtight container (2) is provided with air intake opening, gas outlet and water inlet, described air intake opening is connected to argon bottle (3) by draft tube and described draft tube extends below the liquid level, described water inlet is connected to automatic water supplement mechanism, and described gas outlet is connected by the entrance of pipeline with high temperature reaction stove (1).
2. high temperature resistance steam oxidation performance according to claim 1 is simulated and the accelerated test device, and it is characterized in that: the pipeline of described connection gas outlet and high temperature reaction stove (1) is provided with for detection of the flowmeter that flows through gas (4).
3. high temperature resistance steam oxidation performance according to claim 1 and 2 is simulated and the accelerated test device, it is characterized in that: described airtight container is provided with temperature monitoring mechanism in (2), described temperature monitoring mechanism comprise be positioned at liquid level above, be used for first thermometer (5) of monitoring air outlet temperature and be positioned at second thermometer (6) that liquid level is following, be used for monitoring the deionized water temperature.
4. high temperature resistance steam oxidation performance according to claim 1 and 2 is simulated and the accelerated test device, and it is characterized in that: the pipeline of described connection gas outlet and high temperature reaction stove (1) is provided with for detection of the hygrometer that flows through gas (7) and thermometer (8).
5. high temperature resistance steam oxidation performance according to claim 1 is simulated and the accelerated test device, it is characterized in that: described steam produces mechanism and comprises the ultrasound wave damping device (9) that is arranged in the airtight container (2).
6. high temperature resistance steam oxidation performance is simulated and the accelerated test device according to claim 1 or 5, and it is characterized in that: described heating arrangement comprises the heating sheath (10) that is coated on airtight container (2) outer wall.
7. high temperature resistance steam oxidation performance according to claim 1 is simulated and the accelerated test device, and it is characterized in that: the outlet of described high temperature reaction stove (1) is connected to vacuum pump (11).
8. utilize in the claim 1 to 7 each described device to carry out the simulation of high temperature resistance steam oxidation performance and accelerated test method, it is characterized in that, may further comprise the steps:
A. build experiment atmosphere: by steam produce mechanism make deionized water in the airtight container (2) produce water vapor and with feed deionized water in after argon gas after the deoxidation mixes, feeding high temperature reaction stove (1) 20～40min;
B. heating experiment: sample is put into high temperature reaction stove (1) rear enclosed high temperature reaction stove (1) and high temperature reaction stove (1) is heated to working temperature, weighs through taking out sample behind the setting-up time;
C. repeating step a and b obtain the oxidation kinetics rule.
9. high temperature resistance steam oxidation performance according to claim 8 is simulated and accelerated test apparatus and method and monitoring method, it is characterized in that: among the described step a, the temperature of mixed gas is controlled at 80～90 ℃ by being installed in the thermometer (8) that connects on airtight container (2) gas outlet and high temperature reaction stove (1) inlet duct, and experiment atmosphere is by being installed in hygrometer (7) and flowmeter (4) control that connects on airtight container (2) gas outlet and high temperature reaction stove (1) inlet duct.
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| CN105203448A (en) * | 2014-06-27 | 2015-12-30 | 宝山钢铁股份有限公司 | Testing device and method for simulating solar water heater inner barrel accelerated corrosion |
| CN111307704A (en) * | 2020-04-25 | 2020-06-19 | 中昊清远(北京)科技有限公司 | Novel salt solution week soaks test device |
| CN112326713A (en) * | 2020-10-20 | 2021-02-05 | 北京航空航天大学 | Simplified method for simulating high-temperature water-oxygen environment of silicon carbide fiber by utilizing quartz sealed tube |
| CN112557292A (en) * | 2020-11-30 | 2021-03-26 | 西北有色金属研究院 | Device and method for evaluating ultrahigh-temperature water vapor oxidation corrosion of zirconium alloy coating |
| CN116087261A (en) * | 2023-04-11 | 2023-05-09 | 中国石油大学(华东) | Foam heat-resistant stability evaluation device and method |
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Address after: 510663 Guangzhou Province, Whampoa District, No. research road, No. 9 Applicant after: The extraordinary bearing device in Guangzhou detects research institute Address before: 510663 Luogang District Science City, Guangdong Province, research road, No. 9, No. Applicant before: Guangzhou Special Pressure Equipment Inspection and Research Institute |
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Application publication date: 20131002 |