CN103454210A - Rotary dynamic metal corrosion testing device and using method thereof - Google Patents

Rotary dynamic metal corrosion testing device and using method thereof Download PDF

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CN103454210A
CN103454210A CN2013104132363A CN201310413236A CN103454210A CN 103454210 A CN103454210 A CN 103454210A CN 2013104132363 A CN2013104132363 A CN 2013104132363A CN 201310413236 A CN201310413236 A CN 201310413236A CN 103454210 A CN103454210 A CN 103454210A
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experiment
chamber
experiment chamber
upper cover
temperature
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CN103454210B (en
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王培�
叶中飞
董红
李殿中
李依依
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The invention relates to the field of high-temperature corrosion of liquid metal and particularly relates to a rotary dynamic metal corrosion testing device and a using method thereof. The device is provided with a gas path and sealing system, a temperature control and reactor system and a lifting and rotating system, wherein the gas path and sealing system mainly comprises a vacuum pump, a resistance type vacuum gauge, a gas mixing device and a gas flow controller; the temperature control and reactor system mainly comprises heating elements, a temperature measuring element, an artificial intelligent temperature controller, a heat resistant steel experiment cavity, an experiment cavity upper sealing cover and glass lining; the lifting and rotating system mainly comprises a stepping motor, a sliding slipway, a ball screw, limiting stoppers, a rotary rod and a sample holder. According to the device, the experiment environment atmosphere is controllable through the extrusion sealing mode of metal and a high-temperature rubber ring, the experiment temperature is accurate and controllable through intelligent temperature control, the relative movement of a sample and a corrosive medium (liquid metal) is realized through the mode that rotary motor drives an agitator arm to rotate, and high-temperature dynamic corrosion experiment is realized under the simple dynamic equipment composing condition.

Description

A kind of rotary dynamic metal corrosion device and using method thereof
Technical field
The present invention relates to liquid metal high temperature corrosion field, be specially a kind of rotary dynamic metal corrosion device and using method.Under the high temperature controlled atmosphere, adopt the mode of rotation to make structured material and liquid metal relative motion, realize the corrosion test of material in dynamic liquid metal, thereby, for the dynamic compatibility of research material and liquid metal provides possibility, simplified conventional pipelines formula Dynamic Corrosion device.
Background technology
Liquid metal has the density higher than water and thermal capacitance usually, and therefore, when using liquid metal as heat transfer medium, heat conduction efficiency is higher, simultaneously because its boiling point is high, can not worry the too high safety problem caused of vapour pressure in higher temperature use.So, use in recent years liquid metal to become study hotspot as heat transfer medium or cooling medium.
But the liquid metal under high temperature has usually than water or the higher corrosive power of water vapor, easily cause the corrosion of heat transfer medium to containment structure material or other structured material, so the compatibility of research structure material and liquid metal all has great importance for engineering application and scientific research.As heat transfer medium or cooling medium, liquid metal flows usually in certain container or pipeline.Therefore, the corrosion on common meaning, also can cause erosion to associated materials.So the corrosion that researching high-temperature current downflow liquid metal causes structured material or erosion are a kind of means of testing of more directly, more pressing close to true duty status.
At present, usually the mobile liquid metal corrosion proving installation adopted is the duct type device, be that thermal convection or external force drive (driving by mechanical pump or electromagnetic pump) that liquid metal is flowed in fixed-piping, specimen be placed on to the compatibility of research in pipeline itself and liquid metal.But in the duct type device that uses thermal convection to drive, the flow velocity of liquid metal is lower, is difficult to reach the flow velocity under true duty status, thereby causes test data inaccurate.And the duct type device that uses mechanical pump or electromagnetic pump to drive, device is complicated on the one hand, investment is larger, and liquid metal also can cause corrosion and the abrasion of mechanical pump and electromagnetic pump on the other hand, has both damaged pump and also can cause the pollution of liquid metal.Simultaneously, the duct type device is due to the restriction of pipe diameter, and the sample size that usually can put into is limited.So, design a kind of dynamic metal corrosion tester simple, that flowing velocity is adjustable and seem very necessary.
Summary of the invention
The purpose of this invention is to provide a kind of rotary dynamic metal corrosion device and using method thereof, solve the problems such as device complexity in prior art, liquid metal vulnerable to pollution, the sample size of packing into be limited.For liquid metal Dynamic Corrosion testing requirement, provide a kind of simple, workable device.Use this device can conveniently adjust the parameters such as the speed of related movement of test temperature, sample and liquid metal, experiment atmosphere, realize the convenience to material and liquid metal compatibility experimental data, reliable collection and analyze.In conjunction with invented rotary dynamic metal corrosion device, a kind of using method of rotary dynamic metal corrosion device is proposed.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A kind of rotary dynamic metal corrosion device, this device comprises gas circuit and sealing system, temperature control and reactor assembly and lifting and rotary system, concrete structure is as follows:
Gas circuit and sealing system comprise: vacuum pump, resistance manometer, gas mixing device, gas meter, one-way relief valves, gas cylinder, and vacuum pump is connected with experiment chamber upper cover by corrugated tube, and the experiment chamber is vacuumized; Resistance manometer is connected on the upper cover of experiment chamber, measurement and monitoring experiment chamber gaseous tension; The inlet end of gas mixing device connects gas cylinder by gas meter, and the outlet side of gas mixing device connects experiment chamber upper cover by solenoid valve, and one-way relief valves is arranged on the upper cover of experiment chamber;
Temperature control and reactor assembly comprise: heating element, temperature element, artificial intelligence temperature controller, heat-resisting steel experiment chamber, experiment chamber upper cover, glass-lined, and heating element is arranged at the outside in experiment chamber, and the experiment chamber is heated; The artificial intelligence temperature controller is connected with temperature element with heating element respectively, and an end of temperature element extends in the experiment chamber, by temperature element experiments of measuring cavity temperature, by the artificial intelligence temperature controller, realizes setting and the control to temperature; Glass-lined is put into heat-resisting steel experiment chamber, makes liquid metal and the isolation of experiment chamber; The experiment top of chamber is installed experiment chamber upper cover, and experiment chamber upper cover is combined with the experiment chamber by the crush seal mode; Experiment chamber upper cover is hollow structure, and circulating water is passed through in inside; The center pit that swingle sees through on the upper cover of experiment chamber extends in the experiment chamber, and the end that swingle extends in the experiment chamber connects specimen mounting; Realize sealing by fashion of extrusion between swingle and upper cover center pit;
Lifting and rotary system comprise: lifting motor, electric rotating machine, lifting slide unit, ball screw, stop, swingle, specimen mounting, the lifting slide unit is the L-type lifting slide unit that facade and surface level form, the facade of L-type lifting slide unit is threaded with ball screw, lifting motor is connected with ball screw, drives L-type lifting slide unit and slides up and down; The upper and lower of ball screw is separately installed with stop, and moving up and down by stop of lifting slide unit limits; Electric rotating machine is arranged on the surface level of L-type lifting slide unit, and the bottom of electric rotating machine connects an end of swingle, and electric rotating machine rotates in the experiment chamber by the specimen mounting of the swingle driven rotary bar other end; Swingle keeps coaxial with the hole at upper cover middle part, experiment chamber, realizes dynamic seal (packing) by metal and super heated rubber circle crush seal device between the two.
Described rotary dynamic metal corrosion device, the outer setting artificial intelligence temperature controller of rotary dynamic metal corrosion device, temperature element one end be connected with the artificial intelligence temperature controller extends in the experiment chamber.
Described rotary dynamic metal corrosion device, metal and super heated rubber circle crush seal device are placed in experiment chamber upper cover and experiment junction, chamber, and swingle and upper cover center pit junction, realize respectively the Static and dynamic sealing.
Described rotary dynamic metal corrosion device, rotary dynamic metal corrosion device is used electric rotating machine to drive the specimen mounting rotation, causes the relative motion between sample and liquid metal, realizes the Dynamic Corrosion experiment; Thereby, by adjusting rotating speed and the position of sample on specimen mounting of electric rotating machine, further adjust the relative motion speed of sample and liquid metal.
Described rotary dynamic metal corrosion device, the glass-lined that experiment inside, chamber has high purity quartz to make, be used for avoiding liquid metal and test contacting between chamber, reduces interference experimental result caused because of the corrosion of experiment chamber; Between glass-lined and experiment chamber, use schmigel to tamp, avoid rocking of glass-lined in experimentation.
Described rotary dynamic metal corrosion device, swingle is the inside, center pit loading test chamber of chamber upper cover by experiment, and connect specimen mounting, and swingle and experiment chamber upper cover center pit are by metal and the crush seal of super heated rubber circle.
The using method of described rotary dynamic metal corrosion device, before experiment starts, use gas circuit and the vacuum pump in sealing system that the experiment chamber of sealing is evacuated to and sets below vacuum tightness, and then use temperature control and reactor assembly will be tested chamber and be heated to design temperature; And pass into the mixed gas of setting in backward experiment chamber, and in whole experimentation in holding chamber atmosphere stable; Drive specimen mounting by swingle in experimentation and rotate, realize the relative motion between sample and liquid metal, in experimentation, use lifting motor to promote or the decline specimen mounting.
The using method of described rotary dynamic metal corrosion device, comprise the steps:
1) glass-lined is put into to the experiment chamber, and used schmigel that glass-lined and the space of testing between chamber are tamped, and packed in glass-lined in appropriate corrosive medium reguline metal;
2) put into crush seal metal frame and super heated rubber circle in the upper cover center pit of experiment chamber, swingle is passed to experiment chamber upper cover center pit;
3) specimen mounting is connected with the swingle through experiment chamber upper cover, the sample that has been installed on specimen mounting, used lifting motor, and specimen mounting is promoted to and exceeds the glass-lined position simultaneously;
4) cover experiment chamber upper cover, use the locked experiment of locking buckle chamber upper cover, use vacuum pump will test the chamber air pressure inside and be evacuated to setting value;
5) use temperature control and reactor assembly is heated and temperature control, the Heating Experiment chamber, be fused into liquid by the corrosive medium reguline metal, guarantees that the experiment cavity temperature moves according to setting program, keeps testing vacuum tightness in chamber in this process simultaneously;
6) experiment intraluminal fluid state metal reach predetermined temperature and in stable condition after, use gas mixing device to the mixed gas that injects design in the experiment chamber, gas flow is controlled by gas meter;
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor that specimen mounting is lowered, immerse in liquid metal, open electric rotating machine simultaneously, use arrangements for speed regulation to adjust its rotational speed to design load, start dynamic liquid metal corrosion test;
8), during off-test, the motor that at first stops the rotation, use lifting motor that specimen mounting is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow, makes to test cavity pressure and reach 1 standard atmospheric pressure;
9) after etc. sample is cooled to room temperature, open the locking buckle on the upper cover of experiment chamber, reuse lifting motor specimen mounting is promoted to simultaneously and exceeds experiment position, chamber with experiment chamber upper cover, take out sample.
The using method of described rotary dynamic metal corrosion device, the swingle axis overlaps with experiment chamber center pit axis; Sample is symmetrical the placement on specimen mounting, to guarantee sealing effectiveness in rotary course.
Corrosion tester of the present invention compared with prior art, has the following advantages and unique distinction:
1, the present invention by the rotary test sample, realizes the relative motion between specimen and liquid metal, thereby device complexity, liquid metal drive unit seriously corroded, the sample charging capacity having avoided using prior art to cause such as lack at the shortcoming; Simultaneously, the present invention can, by simple adjustment specimen mounting rotational speed or the change position of sample on specimen mounting, realize relative motion rate variation between sample and liquid metal.
2, simple, convenient, the safety of spin etching proving installation of the present invention, before starting, experiment use lifting motor sample to be lifted at above reaction vessel, then by heating and melting corrosive medium (reguline metal), after thawing, by lifting motor, sample is immersed in the liquid metal corrosion medium again, and start to rotate, when experiment finishes, use lifting motor that sample is proposed to liquid metal, in whole operating process, avoid operator and the direct of liquid metals to contact, guaranteed operator's safety.
3, with respect to prior art, the sample charging capacity of spin etching proving installation of the present invention is large, can, simultaneously to the several samples test, improve conventional efficient.
In sum, spin etching proving installation of the present invention is used in conjunction with by gas meter and gas mixing device, realizes that experimental enviroment atmosphere is controlled; By intelligent temperature control, realize that test temperature is accurately controlled; Drive the mode of puddler rotation by electric rotating machine, realize the relative motion of sample and corrosive medium (liquid metal); Thereby, realize the high temperature dynamic corrosion test under simple equipment composition condition, research material and some liquid metal are had to important using value in the compatibility under dynamic condition.
The accompanying drawing explanation
Fig. 1 is rotary dynamic metal corrosion device---gas circuit and sealing system structural representation;
Fig. 2 is rotary dynamic metal corrosion device---temperature control and reactor assembly structural representation;
Fig. 3 is rotary dynamic metal corrosion device---lifting and rotary system structural representation;
The overall appearance structural representation that Fig. 4 is rotary dynamic metal corrosion device;
Fig. 5 for the sample of packing into after, rotary dynamic metal corrosion device sectional view.
In figure, the 1-vacuum pump; The 2-vacuum meter; The 3-gas mixing device; The 4-gas meter; 5-crush seal device; The 6-one-way relief valves; 7-experiment chamber upper cover; 8-tests chamber; The 9-gas cylinder; The 10-swingle; The 11-heating element; The 12-temperature element; 13-artificial intelligence temperature controller; The 14-glass-lined; The 15-lifting motor; The 16-electric rotating machine; 17-lifting slide unit; The 18-ball screw; The 19-stop; The 20-specimen mounting; The 21-buckle; A-gas circuit and sealing system; B-temperature control and reactor assembly; C-lifting and rotary system.
Embodiment
As Figure 1-Figure 5, the rotary dynamic metal corrosion device of the present invention, comprise gas circuit and sealing system A, temperature control and reactor assembly B and lifting and rotary system C, and concrete structure is as follows:
As shown in Figure 1 and Figure 2, gas circuit and sealing system comprise: the parts such as vacuum pump 1, resistance manometer 2, gas mixing device 3, gas meter 4, one-way relief valves 6, gas cylinder 9, vacuum pump 1 is connected with experiment chamber upper cover 7 by corrugated tube, and experiment chamber 8 is vacuumized; Resistance manometer 2 is connected on experiment chamber upper cover 7, measurement and monitoring experiment chamber gaseous tension; The inlet end of gas mixing device 3 connects gas cylinder 9 by gas meter 4, and the outlet side of gas mixing device 3 connects experiment chamber upper cover 7 by solenoid valve; One-way relief valves 6 connects experiment chamber upper cover 7.
As shown in Fig. 2, Fig. 3, Fig. 5, temperature control and reactor assembly comprise: the parts such as heating element 11, temperature element 12, artificial intelligence temperature controller 13, heat-resisting steel experiment chamber 8, experiment chamber upper cover 7, glass-lined 14, heating element 11 is arranged at the outside in experiment chamber 8, and experiment chamber 8 is heated; Artificial intelligence temperature controller 13 is connected with temperature element 12 with heating element 11 respectively, and an end of temperature element 12 extends in experiment chamber 8, by temperature element 12 experiments of measuring chamber 8 temperature, and the setting and the control that by artificial intelligence temperature controller 13, realize temperature; Glass-lined 14 is put into heat-resisting steel experiment chamber 8, by liquid metal and 8 isolation of experiment chamber; Experiment chamber upper cover 7 is installed at 8 tops, experiment chamber, and experiment chamber upper cover 7 is by crush seal mode and experiment chamber 8 combinations; Experiment chamber upper cover 7 is hollow structure, and circulating water is passed through in inside; Swingle 10 center pit on chamber upper cover 7 by experiment extends in experiment chamber 8, and an end of swingle 10 is equipped with specimen mounting 20, and this end extends in experiment chamber 8.Metal and super heated rubber circle crush seal device 5 are placed in experiment chamber upper cover 7 and experiment 8 junctions, chamber, and swingle 10 and upper cover 7 junctions, realize respectively the Static and dynamic sealing.
In the present invention, metal and super heated rubber circle crush seal device are equivalent to the Wilson seal device, use high temperature spring to be squeezed on the copper metal frame at the super heated rubber circle, realize extrusion type sealed.
As shown in Figure 3-Figure 5, lifting and rotary system comprise: the parts such as lifting motor 15, electric rotating machine 16, lifting slide unit 17, ball screw 18, stop 19, swingle 10, specimen mounting 20, lifting slide unit 17 is the L-type lifting slide unit that facade and surface level form, the facade of L-type lifting slide unit 17 is threaded with ball screw 18, lifting motor 15 is connected with ball screw 18, drives L-type lifting slide unit 17 and slides up and down; The upper and lower of ball screw 18 is separately installed with stop 19, and moving up and down by stop 19 of lifting slide unit 17 limits; Electric rotating machine 16 is arranged on the surface level of L-type lifting slide unit 17, and the bottom of electric rotating machine 16 connects an end of swingle 10, and electric rotating machine 16 is being tested the interior rotation in chamber 8 by the specimen mounting 20 of swingle 10 driven rotary bar 10 other ends; Swingle 10 keeps coaxial with the hole at experiment upper cover 7 middle parts, chamber, realizes dynamic seal (packing) by metal and super heated rubber circle crush seal device 5 between the two.In addition, the outer setting artificial intelligence temperature controller 13 of rotary dynamic metal corrosion device, can use buckle 21 chuckings between experiment chamber 8 and experiment chamber upper cover 7.
In the present invention, rotary dynamic metal corrosion device is used electric rotating machine 16 to drive specimen mounting 20 rotations, causes the relative motion between sample and liquid metal, realizes the Dynamic Corrosion experiment.Thereby, can, by adjusting rotating speed and the position of sample on specimen mounting 20 of electric rotating machine 16, further adjust the relative motion speed of sample and liquid metal.
In the present invention, experiment chamber 8 materials are heat-resisting steel, and the glass-lined 14 that experiment 8 inside, chamber have high purity quartz (purity >=99.9wt%) to make is used for isolating liquid metal and tests contacting between chamber 8, reduces interference experimental result caused because of the corrosion of experiment chamber.Between glass-lined 14 and experiment chamber 8, use schmigel to tamp, avoid rocking of glass-lined in experimentation.
In the present invention, swingle 10 is 8 inside, center pit loading test chamber of chamber upper cover 7 by experiment, and connect specimen mounting 20, and the sealing of swingle 10 and experiment chamber upper cover 7 center pits is by metal and the crush seal of super heated rubber circle.Wherein, swingle 10 axis overlap with experiment chamber 8 center pit axis, and sample is symmetrical the placement on specimen mounting 20, to guarantee sealing effectiveness in rotary course.
As Figure 1-5, the using method of rotary dynamic metal corrosion device provided by the invention, before experiment starts, use gas circuit and the vacuum pump 1 in sealing system A that the experiment chamber 8 of sealing is evacuated to and sets below vacuum tightness, and then use temperature control and reactor assembly B will test chamber 8 and be heated to design temperature; And pass into the mixed gas of setting in backward experiment chamber 8, and in whole experimentation in holding chamber atmosphere stable; Drive specimen mounting 20 by swingle 10 in experimentation and rotate, realize the relative motion between sample and liquid metal, in experimentation, use lifting motor 15 to promote or decline specimen mounting 20, concrete steps are as follows:
1) glass-lined 14 is put into to experiment chamber 8, and used schmigel that glass-lined 14 and the space of testing between chamber 8 are tamped, and appropriate reguline metal (corrosive medium) packed in glass-lined 14;
2) put into metal frame and the super heated rubber circle that crush seal is used in upper cover 7 center pits of experiment chamber, swingle 10 is passed to experiment chamber upper cover 7 center pits;
3) specimen mounting 20 is connected with the swingle 10 through experiment chamber upper cover 7, the sample that has been installed on specimen mounting 20, used lifting motor 15, and specimen mounting 20 is promoted to and exceeds glass-lined 14 positions simultaneously.
4) cover experiment chamber upper cover 7, use the locked experiment of locking buckle 21 chamber upper cover 7, use vacuum pump 1 will test chamber 8 air pressure inside and be evacuated to setting value (vacuum tightness shows by electron vacuum gage 2).
5) use temperature control and reactor assembly is heated and temperature control, Heating Experiment chamber 8, be fused into liquid by reguline metal, guarantees that the interior temperature in experiment chamber 8 moves according to setting program simultaneously, keeps testing the interior vacuum tightness in chamber 8 in this process.
6) the interior liquid metal in experiment chamber 8 melt complete and in stable condition after, use the mixed gas of gas mixing device 3 to the interior injection design in experiment chamber 8, gas flow is controlled by gas meter 4.
7) after the interior gaseous tension in experiment chamber 8 and composition are stablized, use lifting motor 15 that specimen mounting 20 is lowered, immerse in liquid metal, open electric rotating machine 16 simultaneously, the use arrangements for speed regulation are adjusted its rotational speed to design load, start dynamic liquid metal corrosion test.
8), during off-test, the motor 16 that at first stops the rotation, use lifting motor 15 that specimen mounting 20 is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow, makes to test cavity pressure and reach 1 standard atmospheric pressure.
9) after etc. sample is cooled to room temperature, open the locking buckle 21 on experiment chamber upper cover 7, reuse lifting motor 15 specimen mounting 20 is promoted to simultaneously and exceeds experiment 8 positions, chamber with experiment chamber upper cover 7, take out sample.
In the present invention, sample can be for stainless steel, heat-resisting steel, tool steel, straight carbon steel, grinding tool steel and the fusing point of the various trades mark at non-ferrous metal more than 600 ℃ etc.
Embodiment mono-:
Use the device of mentioning in invention to carry out the corrosion behavior test of martensite heat-resistant steel P91 in 550 ℃ of dynamic plumbous bismuths (Pb-Bi) eutectic alloy, carry out as follows:
1) glass-lined is put into to the experiment chamber, and used schmigel that glass-lined and the space of testing between chamber are tamped, and the Pb-Bi eutectic alloy of about 20kg is packed in glass-lined;
2) put into crush seal metal frame and super heated rubber circle in the upper cover center pit of experiment chamber, swingle is passed to experiment chamber upper cover center pit;
3) specimen mounting is connected with the swingle through experiment chamber upper cover, the pole shape P91 sample of φ 5 * 10mm is installed on specimen mounting simultaneously, the use lifting motor, be promoted to specimen mounting and sample to exceed the glass-lined height.
4) cover experiment chamber upper cover, use the locked experiment of locking buckle chamber upper cover, use vacuum pump will test the chamber air pressure inside and be evacuated to below 10Pa.
5) use temperature control and reactor assembly is heated and temperature control, will test chamber with the rate of heat addition of 50 ℃/h and be heated to 550 ℃, be incubated.
6) in the experiment chamber block Pb-Bi eutectic alloy be fused into liquid metal and stable after, use the blending ratio (volume) of gas mixing device by 95% high-purity argon gas+5% oxygen, inject mixed gas in the experiment chamber, it is 5L/min that gas meter is controlled gas flow, making intracavity gas pressure is 1 standard atmospheric pressure, and unnecessary gas is got rid of by the one way pressure-reducing valve be connected on the upper cover of experiment chamber.
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor that specimen mounting is lowered, immerse in liquid metal, open electric rotating machine simultaneously, use the arrangements for speed regulation adjustment to rotate to 90r/min(rev/min), start to carry out dynamic liquid metal corrosion test.
8) after 2000 hours, off-test.At first the motor that stops the rotation, use lifting motor that specimen mounting is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow to 10L/min, gets rid of hot-air in chamber.
9) after 10 hours, specimen temperature is down to room temperature, opens the locking buckle on the upper cover of experiment chamber, uses lifting motor that specimen mounting and upper cover are promoted to higher than experiment chamber height, and the band gloves take out sample.After cleaning, carry out corrosion layer structure and component distributing research.
Embodiment bis-:
Use the device of mentioning in invention to carry out the corrosion behavior test of martensite heat-resistant steel P91 in 600 ℃ of dynamically plumbous (Pb) alloys, carry out as follows:
1) glass-lined is put into to the experiment chamber, and used schmigel that glass-lined and the space of testing between chamber are tamped, and the Pb alloy of about 25kg is packed in glass-lined;
2) put into crush seal metal frame and super heated rubber circle in the upper cover center pit of experiment chamber, swingle is passed to experiment chamber upper cover center pit;
3) specimen mounting is connected with the swingle through experiment chamber upper cover, the sheet P91 sample of 40mm * 20mm * 5mm is installed on specimen mounting simultaneously, the use lifting motor, be promoted to specimen mounting and sample to exceed the glass-lined height.
4) cover experiment chamber upper cover, use the locked experiment of locking buckle chamber upper cover.Using vacuum pump will test the chamber air pressure inside is evacuated to below 10Pa.
5) use temperature control and reactor assembly is heated and temperature control, will test chamber with the rate of heat addition of 100 ℃/h and be heated to 600 ℃, be incubated.
6) after in the experiment chamber, block Pb alloy melting becomes liquid metal also to stablize, use the blending ratio (volume) of gas mixing device by 92% high-purity argon gas+2% hydrogen+6% water vapor, inject mixed gas in the experiment chamber, it is 5L/min that gas meter is controlled gas flow, making intracavity gas pressure is 1 standard atmospheric pressure, and unnecessary gas is got rid of by the one way pressure-reducing valve be connected on the upper cover of experiment chamber.
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor that specimen mounting is lowered, immerse in liquid metal, open electric rotating machine simultaneously, use the arrangements for speed regulation adjustment to rotate to 60r/min, start to carry out dynamic liquid metal corrosion test.
8), after 2000 hours, test needs to change sample.At first the motor that stops the rotation, use lifting motor that specimen mounting is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow to 10L/min, gets rid of hot-air in chamber.
9) open the locking buckle on the upper cover of experiment chamber, use lifting motor that specimen mounting and upper cover are promoted to higher than experiment chamber height, the band gloves take out sample.Simultaneously, new sample is installed on specimen mounting.
10) repeating step 7), after stablizing, gas flow is down to 5L/min, proceed test.
11) after 5000 hours, off-test.At first the motor that stops the rotation, use lifting motor that specimen mounting is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow to 10L/min, gets rid of hot-air in chamber.
12) after 12 hours, specimen temperature is down to room temperature, opens the locking buckle on the upper cover of experiment chamber, uses lifting motor that specimen mounting and upper cover are promoted to higher than experiment chamber height, and the band gloves take out sample.After cleaning, carry out corrosion layer structure and component distributing research.
The embodiment result shows, use apparatus of the present invention can complete simply and effectively dynamic liquid metal corrosion experiment, speed of related movement between sample and liquid metal is adjustable, experimental temperature is adjustable, experiment atmosphere is adjustable, can realize structured material and the experiment of liquid metal compatibility under multiple etching condition and environment.Simultaneously, use this experimental provision also can conveniently realize the replacing of long-term experiment middle sample.

Claims (9)

1. a rotary dynamic metal corrosion device, is characterized in that, this device comprises gas circuit and sealing system, temperature control and reactor assembly and lifting and rotary system, and concrete structure is as follows:
Gas circuit and sealing system comprise: vacuum pump, resistance manometer, gas mixing device, gas meter, one-way relief valves, gas cylinder, and vacuum pump is connected with experiment chamber upper cover by corrugated tube, and the experiment chamber is vacuumized; Resistance manometer is connected on the upper cover of experiment chamber, measurement and monitoring experiment chamber gaseous tension; The inlet end of gas mixing device connects gas cylinder by gas meter, and the outlet side of gas mixing device connects experiment chamber upper cover by solenoid valve, and one-way relief valves is arranged on the upper cover of experiment chamber;
Temperature control and reactor assembly comprise: heating element, temperature element, artificial intelligence temperature controller, heat-resisting steel experiment chamber, experiment chamber upper cover, glass-lined, and heating element is arranged at the outside in experiment chamber, and the experiment chamber is heated; The artificial intelligence temperature controller is connected with temperature element with heating element respectively, and an end of temperature element extends in the experiment chamber, by temperature element experiments of measuring cavity temperature, by the artificial intelligence temperature controller, realizes setting and the control to temperature; Glass-lined is put into heat-resisting steel experiment chamber, makes liquid metal and the isolation of experiment chamber; The experiment top of chamber is installed experiment chamber upper cover, and experiment chamber upper cover is combined with the experiment chamber by the crush seal mode; Experiment chamber upper cover is hollow structure, and circulating water is passed through in inside; The center pit that swingle sees through on the upper cover of experiment chamber extends in the experiment chamber, and the end that swingle extends in the experiment chamber connects specimen mounting; Realize sealing by fashion of extrusion between swingle and upper cover center pit;
Lifting and rotary system comprise: lifting motor, electric rotating machine, lifting slide unit, ball screw, stop, swingle, specimen mounting, the lifting slide unit is the L-type lifting slide unit that facade and surface level form, the facade of L-type lifting slide unit is threaded with ball screw, lifting motor is connected with ball screw, drives L-type lifting slide unit and slides up and down; The upper and lower of ball screw is separately installed with stop, and moving up and down by stop of lifting slide unit limits; Electric rotating machine is arranged on the surface level of L-type lifting slide unit, and the bottom of electric rotating machine connects an end of swingle, and electric rotating machine rotates in the experiment chamber by the specimen mounting of the swingle driven rotary bar other end; Swingle keeps coaxial with the hole at upper cover middle part, experiment chamber, realizes dynamic seal (packing) by metal and super heated rubber circle crush seal device between the two.
2. according to rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that, the outer setting artificial intelligence temperature controller of rotary dynamic metal corrosion device, temperature element one end be connected with the artificial intelligence temperature controller extends in the experiment chamber.
3. according to rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that, metal and super heated rubber circle crush seal device are placed in experiment chamber upper cover and experiment junction, chamber, and swingle and upper cover center pit junction, realize respectively the Static and dynamic sealing.
4. according to rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that, rotary dynamic metal corrosion device is used electric rotating machine to drive the specimen mounting rotation, causes the relative motion between sample and liquid metal, realizes the Dynamic Corrosion experiment; Thereby, by adjusting rotating speed and the position of sample on specimen mounting of electric rotating machine, further adjust the relative motion speed of sample and liquid metal.
5. according to rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that, the glass-lined that experiment inside, chamber has high purity quartz to make, be used for avoiding liquid metal and test contacting between chamber, reduces interference experimental result caused because of the corrosion of experiment chamber; Between glass-lined and experiment chamber, use schmigel to tamp, avoid rocking of glass-lined in experimentation.
6. according to rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that, swingle is the inside, center pit loading test chamber of chamber upper cover by experiment, and connect specimen mounting, and swingle and experiment chamber upper cover center pit are by metal and the crush seal of super heated rubber circle.
7. the using method of a rotary dynamic metal corrosion device claimed in claim 1, it is characterized in that: before experiment starts, use gas circuit and the vacuum pump in sealing system that the experiment chamber of sealing is evacuated to and sets below vacuum tightness, and then use temperature control and reactor assembly will be tested chamber and be heated to design temperature; And pass into the mixed gas of setting in backward experiment chamber, and in whole experimentation in holding chamber atmosphere stable; Drive specimen mounting by swingle in experimentation and rotate, realize the relative motion between sample and liquid metal, in experimentation, use lifting motor to promote or the decline specimen mounting.
8. according to the using method of rotary dynamic metal corrosion device claimed in claim 7, it is characterized in that, comprise the steps:
1) glass-lined is put into to the experiment chamber, and used schmigel that glass-lined and the space of testing between chamber are tamped, and packed in glass-lined in appropriate corrosive medium reguline metal;
2) put into crush seal metal frame and super heated rubber circle in the upper cover center pit of experiment chamber, swingle is passed to experiment chamber upper cover center pit;
3) specimen mounting is connected with the swingle through experiment chamber upper cover, the sample that has been installed on specimen mounting, used lifting motor, and specimen mounting is promoted to and exceeds the glass-lined position simultaneously;
4) cover experiment chamber upper cover, use the locked experiment of locking buckle chamber upper cover, use vacuum pump will test the chamber air pressure inside and be evacuated to setting value;
5) use temperature control and reactor assembly is heated and temperature control, the Heating Experiment chamber, be fused into liquid by the corrosive medium reguline metal, guarantees that the experiment cavity temperature moves according to setting program, keeps testing vacuum tightness in chamber in this process simultaneously;
6) experiment intraluminal fluid state metal reach predetermined temperature and in stable condition after, use gas mixing device to the mixed gas that injects design in the experiment chamber, gas flow is controlled by gas meter;
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor that specimen mounting is lowered, immerse in liquid metal, open electric rotating machine simultaneously, use arrangements for speed regulation to adjust its rotational speed to design load, start dynamic liquid metal corrosion test;
8), during off-test, the motor that at first stops the rotation, use lifting motor that specimen mounting is promoted to and breaks away from the liquid metal liquid level, then stops heating, strengthens gas flow, makes to test cavity pressure and reach 1 standard atmospheric pressure;
9) after etc. sample is cooled to room temperature, open the locking buckle on the upper cover of experiment chamber, reuse lifting motor specimen mounting is promoted to simultaneously and exceeds experiment position, chamber with experiment chamber upper cover, take out sample.
9. according to the using method of rotary dynamic metal corrosion device claimed in claim 7, it is characterized in that, the swingle axis overlaps with experiment chamber center pit axis; Sample is symmetrical the placement on specimen mounting, to guarantee sealing effectiveness in rotary course.
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