CN103454210B - A kind of rotary dynamic metal corrosion device and using method thereof - Google Patents

A kind of rotary dynamic metal corrosion device and using method thereof Download PDF

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CN103454210B
CN103454210B CN201310413236.3A CN201310413236A CN103454210B CN 103454210 B CN103454210 B CN 103454210B CN 201310413236 A CN201310413236 A CN 201310413236A CN 103454210 B CN103454210 B CN 103454210B
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experiment chamber
experiment
chamber
upper cover
temperature
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CN103454210A (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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Abstract

The present invention relates to field of high-temperature corrosion of liquid metal, be specially a kind of rotary dynamic metal corrosion device and using method.This device has gas circuit and sealing system, temperature control and reactor assembly and lifting and rotary system, and gas circuit and sealing system mainly comprise vacuum pump, resistance manometer, gas mixing device, gas flow controller; Temperature control and reactor assembly mainly comprise heating element, temperature element, artificial intelligence temperature controller, heat-resisting steel are tested chamber, tested chamber upper cover, glass-lined; Lifting and rotary system mainly comprise stepper motor, are elevated slide unit, ball screw, stop, swingle, specimen mounting.This device is by metal and super heated rubber circle crush seal mode, realize experimental enviroment atmosphere controlled, test temperature controllable precise is realized by intelligent temperature control, the mode driving puddler to rotate by electric rotating machine realizes the relative motion of sample and corrosive medium (liquid metal), under simple equipment composition condition, realize high temperature dynamic corrosion test.

Description

A kind of rotary dynamic metal corrosion device and using method thereof
Technical field
The present invention relates to field of high-temperature corrosion of liquid metal, be specially a kind of rotary dynamic metal corrosion device and using method.Under 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, thus provide possibility for the dynamic compatibility of research material and liquid metal, simplify 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 use in higher temperature and not worry the too high safety problem caused of vapour pressure.So, use liquid metal to become study hotspot as heat transfer medium or cooling medium in recent years.
But the liquid metal under high temperature has than water or the higher corrosive power of water vapor usually, easily cause heat transfer medium to the corrosion of containment structure material or other structured material, therefore the compatibility of research structure material and liquid metal all has great importance for engineer applied and scientific research.As heat transfer medium or cooling medium, liquid metal flows usually in certain container or pipeline.Therefore, except the corrosion on common meaning, also erosion can be caused 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 more directly, more pressing close to true duty status.
At present, the flowing liquid metal corrosion proving installation of usual employing is duct type device, namely thermal convection or external force drive (being driven by mechanical pump or electromagnetic pump) that liquid metal is flowed in fixed-piping, and test sample is placed in pipeline the compatibility studying itself and liquid metal.But the flow velocity of liquid metal is lower in the duct type device using thermal convection to drive, is difficult to reach the flow velocity under true duty status, thus causes test data inaccurate.And using the duct type device that mechanical pump or electromagnetic pump drive, device is complicated on the one hand, investment is comparatively large, and liquid metal also can cause corrosion and the abrasion of mechanical pump and electromagnetic pump on the other hand, has both damaged the pollution that pump also can cause liquid metal.Meanwhile, duct type device is due to the restriction of pipe diameter, and the sample size usually can put into is limited.So, design a kind of simple, that flowing velocity is adjustable dynamic metal corrosion tester and seem very necessary.
Summary of the invention
The object 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, loading sample size be limited.For liquid metal Dynamic Corrosion testing requirement, provide a kind of simple, workable device.Use this device can facilitate the parameter such as speed of related movement, experiment atmosphere of Adjustment Tests temperature, sample and liquid metal, realize material and the convenience of liquid metal compatibility experiments data, reliable gather and analysis.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, 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, vacuumizes experiment chamber; 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 are tested chamber, tested chamber upper cover, glass-lined, and heating element is arranged at the outside in experiment chamber, heat experiment chamber; Artificial intelligence temperature controller is connected with heating element and temperature element respectively, and one end of temperature element extends in experiment chamber, by temperature element experiments of measuring cavity temperature, by the realization of artificial intelligence temperature controller to the setting of temperature and control; Glass-lined puts into heat-resisting steel experiment chamber, and liquid metal is isolated with experiment chamber; Experiment top of chamber installs experiment chamber upper cover, and experiment chamber upper cover is combined with experiment chamber by crush seal mode; Experiment chamber upper cover is hollow structure, and circulating water is passed through in inside; Swingle extends in experiment chamber through the center pit on the upper cover of experiment chamber, and one end that swingle extends in experiment chamber connects specimen mounting; Sealing is realized 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, lifting slide unit is the L-type lifting slide unit that facade and surface level are formed, 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 to slide up and down; The upper and lower of ball screw is separately installed with stop, and moving up and down of slide unit of lifting is limited by stop; Electric rotating machine is arranged on the surface level of L-type lifting slide unit, and the bottom of electric rotating machine connects one end of swingle, and electric rotating machine is rotated in experiment chamber by the specimen mounting of the swingle driven rotary bar other end; Swingle keeps coaxial with the hole in the middle part of the upper cover of experiment chamber, realizes dynamic seal (packing) between the two by metal and super heated rubber circle crush seal device.
Described rotary dynamic metal corrosion device, the outer setting artificial intelligence temperature controller of rotary dynamic metal corrosion device, the temperature element one end be connected with artificial intelligence temperature controller extends tests in chamber.
Described rotary dynamic metal corrosion device, metal and super heated rubber circle crush seal device are placed in tests chamber upper cover and experiment junction, chamber, and swingle and upper cover center pit junction, realizes Static and dynamic respectively and seals.
Described rotary dynamic metal corrosion device, rotary dynamic metal corrosion device uses electric rotating machine to drive specimen mounting to rotate, and causes the relative motion between sample and liquid metal, realizes Dynamic Corrosion experiment; Thus, by adjusting rotating speed and the position of sample on specimen mounting of electric rotating machine, the relative motion speed of adjustment sample and liquid metal further.
Described rotary dynamic metal corrosion device, the glass-lined that inside, experiment chamber has high purity quartz to make, is used for avoiding the contact between liquid metal and experiment chamber, reduces because the interference caused experimental result is corroded in experiment chamber; Use schmigel to tamp between glass-lined and experiment chamber, avoid rocking of glass-lined in experimentation.
Described rotary dynamic metal corrosion device, the center pit loading test chamber of swingle chamber upper cover is by experiment inner, and connects 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 the vacuum pump in gas circuit and sealing system to be evacuated in the experiment chamber of sealing and set below vacuum tightness, and then use temperature control and reactor assembly that experiment chamber is heated to design temperature; And pass into the mixed gas of setting in backward experiment chamber, and in whole experimentation in holding chamber atmosphere stablize; Drive specimen mounting to rotate by swingle in experimentation, realize the relative motion between sample and liquid metal, in experimentation, use lifting motor to promote or decline specimen mounting.
The using method of described rotary dynamic metal corrosion device, comprises the steps:
1) glass-lined is put into experiment chamber, and use schmigel to be tamped in the space between glass-lined and experiment chamber, and appropriate corrosive medium reguline metal is loaded in glass-lined;
2) in the upper cover center pit of experiment chamber, crush seal metal frame and super heated rubber circle is put into, by swingle through experiment chamber upper cover center pit;
3) be connected with through the swingle of testing chamber upper cover by specimen mounting, be installed sample simultaneously on specimen mounting, uses lifting motor, be promoted to by specimen mounting and exceed glass-lined position;
4) cover experiment chamber upper cover, use locking buckle locked experiment chamber upper cover, use vacuum pump that experiment chamber air pressure inside is evacuated to setting value;
5) use temperature control and reactor assembly to carry out heating and temperature control, Heating Experiment chamber, is fused into liquid by corrosive medium reguline metal, ensures that experiment cavity temperature runs according to setting program simultaneously, keeps vacuum tightness in experiment chamber in the process;
6) after experiment intraluminal fluid state metal reaches predetermined temperature and be in stable condition, use gas mixing device in experiment chamber, inject the mixed gas of design, gas flow is controlled by gas meter;
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor to be lowered by specimen mounting, in immersion 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, first stop the rotation motor, uses lifting motor to be promoted to by specimen mounting and depart from liquid metal liquid level, then stop heating, strengthen gas flow, make experiment cavity pressure 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 and specimen mounting is promoted to exceed with experiment chamber upper cover simultaneously test position, chamber, taking-up sample.
The using method of described rotary dynamic metal corrosion device, swingle axis and experiment chamber center pit dead in line; Sample is symmetrical on specimen mounting to be placed, to ensure 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 is by rotary test sample, realizes the relative motion between test sample and liquid metal, thus avoids device complexity, liquid metal drive unit seriously corroded, the sample loading volume shortcoming such as less that use prior art to cause; Meanwhile, the present invention by simple adjustment specimen mounting rotational speed or the change position of sample on specimen mounting, can 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 experiment starts, use lifting motor to be lifted at above reaction vessel by sample, then by heating and melting corrosive medium (reguline metal), after thawing, by lifting motor, sample is immersed in liquid metal corrosion medium again, and start to rotate, at the end of experiment, use lifting motor that sample is proposed liquid metal, avoid operator in whole operating process to contact with the direct of liquid metals, guarantee operator's safety.
3, relative to prior art, the sample loading volume of spin etching proving installation of the present invention is large, simultaneously to several samples test, can improve conventional efficient.
In sum, spin etching proving installation of the present invention by gas meter and gas mixing device with the use of, realize experimental enviroment atmosphere controlled; By intelligent temperature control, realize test temperature controllable precise; By the mode that electric rotating machine drives puddler to rotate, realize the relative motion of sample and corrosive medium (liquid metal); Thus, under simple equipment composition condition, realize high temperature dynamic corrosion test, to research material and some liquid metal compatibility in a dynamic condition, there is important using value.
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;
Fig. 4 is the overall appearance structural representation of rotary dynamic metal corrosion device;
Fig. 5 is after loading sample, rotary dynamic metal corrosion device sectional view.
In figure, 1-vacuum pump; 2-vacuum meter; 3-gas mixing device; 4-gas meter; 5-crush seal device; 6-one-way relief valves; 7-tests chamber upper cover; 8-tests chamber; 9-gas cylinder; 10-swingle; 11-heating element; 12-temperature element; 13-artificial intelligence temperature controller; 14-glass-lined; 15-lifting motor; 16-electric rotating machine; 17-is elevated slide unit; 18-ball screw; 19-stop; 20-specimen mounting; 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, rotary dynamic metal corrosion device of the present invention, comprise gas circuit and sealing system A, temperature control and reactor assembly B and be elevated and rotary system C, 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, vacuumizes experiment chamber 8; 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: heating element 11, temperature element 12, artificial intelligence temperature controller 13, heat-resisting steel are tested chamber 8, tested the part such as chamber upper cover 7, glass-lined 14, heating element 11 is arranged at the outside in experiment chamber 8, heats experiment chamber 8; Artificial intelligence temperature controller 13 is connected with heating element 11 and temperature element 12 respectively, and one end of temperature element 12 extends in experiment chamber 8, by temperature element 12 experiments of measuring chamber 8 temperature, realizes setting to temperature and control by artificial intelligence temperature controller 13; Glass-lined 14 puts into heat-resisting steel experiment chamber 8, liquid metal and experiment chamber 8 is isolated; Experiment chamber upper cover 7 is installed at experiment top, chamber 8, and experiment chamber upper cover 7 is combined with experiment chamber 8 by crush seal mode; Experiment chamber upper cover 7 is hollow structure, and circulating water is passed through in inside; The center pit of swingle 10 by experiment on chamber upper cover 7 extends in experiment chamber 8, and specimen mounting 20 is equipped with in one end of swingle 10, and this end extends in experiment chamber 8.Metal and super heated rubber circle crush seal device 5 are placed in tests chamber upper cover 7 and experiment junction, chamber 8, and swingle 10 and upper cover 7 junction, realizes Static and dynamic sealing respectively.
In the present invention, metal and super heated rubber circle crush seal device are equivalent to Wilson seal device, use high temperature spring will be squeezed on copper metal frame at super heated rubber circle, realize extrusion type sealed.
As shown in Figure 3-Figure 5, lifting comprises with rotary system: lifting motor 15, electric rotating machine 16, be elevated the parts such as 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 are formed, 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 to slide up and down; The upper and lower of ball screw 18 is separately installed with stop 19, and moving up and down of slide unit 17 of lifting is limited by stop 19; 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 one end of swingle 10, and electric rotating machine 16 is rotated in experiment chamber 8 by the specimen mounting 20 of swingle 10 driven rotary bar 10 other end; Swingle 10 keeps coaxial with the hole in the middle part of experiment chamber upper cover 7, realizes dynamic seal (packing) between the two by metal and super heated rubber circle crush seal device 5.In addition, the outer setting artificial intelligence temperature controller 13 of rotary dynamic metal corrosion device, can use buckle 21 to clamp between experiment chamber 8 and experiment chamber upper cover 7.
In the present invention, rotary dynamic metal corrosion device uses electric rotating machine 16 to drive specimen mounting 20 to rotate, and causes the relative motion between sample and liquid metal, realizes Dynamic Corrosion experiment.Thus, by adjusting rotating speed and the position of sample on specimen mounting 20 of electric rotating machine 16, the relative motion speed of adjustment sample and liquid metal further.
In the present invention, experiment chamber 8 material is heat-resisting steel, the glass-lined 14 that experiment inside, chamber 8 has high purity quartz (purity >=99.9wt%) to make, and is used for isolating the contact between liquid metal and experiment chamber 8, reduces because the interference caused experimental result is corroded in experiment chamber.Use schmigel to tamp between glass-lined 14 and experiment chamber 8, avoid rocking of glass-lined in experimentation.
In the present invention, the center pit loading test chamber 8 of swingle 10 chamber upper cover 7 is by experiment inner, and connects specimen mounting 20, and the sealing of swingle 10 and experiment chamber upper cover 7 center pit is by metal and the crush seal of super heated rubber circle.Wherein, swingle 10 axis and experiment chamber 8 center pit dead in line, sample is symmetrical on specimen mounting 20 to be placed, to ensure 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 the vacuum pump 1 in gas circuit and sealing system A to be evacuated in the experiment chamber 8 of sealing and set below vacuum tightness, and then use temperature control and reactor assembly B that experiment chamber 8 is 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 stablize; Drive specimen mounting 20 to rotate by swingle 10 in experimentation, realize the relative motion between sample and liquid metal, use lifting motor 15 to promote in experimentation or the specimen mounting 20 that declines, concrete steps are as follows:
1) glass-lined 14 is put into experiment chamber 8, and use schmigel to be tamped in the space between glass-lined 14 and experiment chamber 8, and appropriate reguline metal (corrosive medium) is loaded in glass-lined 14;
2) in upper cover 7 center pit of experiment chamber, metal frame and the super heated rubber circle of crush seal is put into, by swingle 10 through experiment chamber upper cover 7 center pit;
3) be connected with through the swingle 10 of testing chamber upper cover 7 by specimen mounting 20, be installed sample simultaneously on specimen mounting 20, uses lifting motor 15, be promoted to by specimen mounting 20 and exceed glass-lined 14 position.
4) cover experiment chamber upper cover 7, use locking buckle 21 locked experiment chamber upper cover 7, use vacuum pump 1 that experiment chamber 8 air pressure inside is evacuated to setting value (vacuum tightness is shown by electron vacuum gage 2).
5) use temperature control and reactor assembly to carry out heating and temperature control, Heating Experiment chamber 8, is fused into liquid by reguline metal, ensures that in experiment chamber 8, temperature is run according to setting program, keeps vacuum tightness in experiment chamber 8 in the process simultaneously.
6) in experiment chamber 8 liquid metal melt complete and in stable condition after, use gas mixing device 3 to inject the mixed gas of design in experiment chamber 8, gas flow is controlled by gas meter 4.
7) after gaseous tension and composition are stablized in experiment chamber 8, use lifting motor 15 to be lowered by specimen mounting 20, in immersion liquid metal, open electric rotating machine 16 simultaneously, use arrangements for speed regulation to adjust its rotational speed to design load, start dynamic liquid metal corrosion test.
8) during off-test, first stop the rotation motor 16, uses lifting motor 15 to be promoted to by specimen mounting 20 and depart from liquid metal liquid level, then stop heating, strengthen gas flow, make experiment cavity pressure 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 and specimen mounting 20 is promoted to exceed with experiment chamber upper cover 7 simultaneously test position, chamber 8, taking-up sample.
In the present invention, sample can be the stainless steel of the various trade mark, heat-resisting steel, tool steel, straight carbon steel, grinding tool steel and the non-ferrous metal etc. of fusing point more than 600 DEG C.
Embodiment one:
Use the device mentioned in invention to carry out the corrosion behavior test of martensite heat-resistant steel P91 in 550 DEG C of dynamic plumbous bismuth (Pb-Bi) eutectic alloys, carry out as follows:
1) glass-lined is put into experiment chamber, and use schmigel to be tamped in the space between glass-lined and experiment chamber, and the Pb-Bi eutectic alloy of about 20kg is loaded in glass-lined;
2) in the upper cover center pit of experiment chamber, crush seal metal frame and super heated rubber circle is put into, by swingle through experiment chamber upper cover center pit;
3) specimen mounting is connected with through the swingle of testing chamber upper cover, the pole shape P91 sample of φ 5 × 10mm is installed on specimen mounting simultaneously, use lifting motor, specimen mounting and sample are promoted to and exceed glass-lined height.
4) cover experiment chamber upper cover, use locking buckle locked experiment chamber upper cover, use vacuum pump that experiment chamber air pressure inside is evacuated to below 10Pa.
5) use temperature control and reactor assembly to carry out heating and temperature control, with the rate of heat addition of 50 DEG C/h, experiment chamber is heated to 550 DEG C, insulation.
6) after testing block Pb-Bi eutectic alloy in chamber and be fused into liquid metal and stablizing, use gas mixing device by the blending ratio (volume) of 95% high-purity argon gas+5% oxygen, mixed gas is injected in experiment chamber, it is 5L/min that gas meter controls gas flow, make intracavity gas pressure be 1 standard atmospheric pressure, excessive 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 to be lowered by specimen mounting, immerse in liquid metal, open electric rotating machine simultaneously, arrangements for speed regulation adjustment is used to rotate to 90r/min(rev/min), start to carry out dynamic liquid metal corrosion test.
8) after 2000 hours, off-test.First stop the rotation motor, uses lifting motor to be promoted to by specimen mounting and depart from liquid metal liquid level, then stop heating, strengthens gas flow to 10L/min, get 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, and use lifting motor specimen mounting and upper cover to be promoted to higher than experiment chamber height, band gloves take out sample.After cleaning, carry out corrosion layer structure and component distributing research.
Embodiment two:
Use the device mentioned in invention to carry out the corrosion behavior test of martensite heat-resistant steel P91 in 600 DEG C dynamically plumbous (Pb) alloy, carry out as follows:
1) glass-lined is put into experiment chamber, and use schmigel to be tamped in the space between glass-lined and experiment chamber, and the Pb alloy of about 25kg is loaded in glass-lined;
2) in the upper cover center pit of experiment chamber, crush seal metal frame and super heated rubber circle is put into, by swingle through experiment chamber upper cover center pit;
3) specimen mounting is connected with through the swingle of testing chamber upper cover, the sheet P91 sample of 40mm × 20mm × 5mm is installed on specimen mounting simultaneously, use lifting motor, specimen mounting and sample are promoted to and exceed glass-lined height.
4) cover experiment chamber upper cover, use locking buckle locked experiment chamber upper cover.Use vacuum pump that experiment chamber air pressure inside is evacuated to below 10Pa.
5) use temperature control and reactor assembly to carry out heating and temperature control, with the rate of heat addition of 100 DEG C/h, experiment chamber is heated to 600 DEG C, insulation.
6) after in experiment chamber, block Pb alloy melting becomes liquid metal also to stablize, use gas mixing device by the blending ratio (volume) of 92% high-purity argon gas+2% hydrogen+6% water vapor, mixed gas is injected in experiment chamber, it is 5L/min that gas meter controls gas flow, make intracavity gas pressure be 1 standard atmospheric pressure, excessive 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 to be lowered by specimen mounting, in immersion liquid metal, open electric rotating machine simultaneously, use arrangements for speed regulation adjustment rotation to 60r/min, start to carry out dynamic liquid metal corrosion test.
8), after 2000 hours, test needs to change sample.First stop the rotation motor, uses lifting motor to be promoted to by specimen mounting and depart from liquid metal liquid level, then stop heating, strengthens gas flow to 10L/min, get rid of hot-air in chamber.
9) open the locking buckle on the upper cover of experiment chamber, use lifting motor specimen mounting and upper cover to be promoted to higher than experiment chamber height, band gloves take out sample.Meanwhile, new sample is installed on specimen mounting.
10) repeat step 7), after stable, gas flow is down to 5L/min, proceed test.
11) after 5000 hours, off-test.First stop the rotation motor, uses lifting motor to be promoted to by specimen mounting and depart from liquid metal liquid level, then stop heating, strengthens gas flow to 10L/min, get 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, and use lifting motor specimen mounting and upper cover to be promoted to higher than experiment chamber height, band gloves take out sample.After cleaning, carry out corrosion layer structure and component distributing research.
Embodiment result shows, use apparatus of the present invention can complete the experiment of dynamic liquid metal corrosion simply and effectively, speed of related movement between sample and liquid metal is adjustable, experimental temperature is adjustable, experiment atmosphere is adjustable, can realize the structured material under multiple etching condition and environment and liquid metal compatibility experiments.Meanwhile, this experimental provision is used also conveniently can to 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, vacuumizes experiment chamber; 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 are tested chamber, tested chamber upper cover, glass-lined, and heating element is arranged at the outside in experiment chamber, heat experiment chamber; Artificial intelligence temperature controller is connected with heating element and temperature element respectively, and one end of temperature element extends in experiment chamber, by temperature element experiments of measuring cavity temperature, by the realization of artificial intelligence temperature controller to the setting of temperature and control; Glass-lined puts into heat-resisting steel experiment chamber, and liquid metal is isolated with experiment chamber; Experiment top of chamber installs experiment chamber upper cover, and experiment chamber upper cover is combined with experiment chamber by crush seal mode; Experiment chamber upper cover is hollow structure, and circulating water is passed through in inside; Swingle extends in experiment chamber through the center pit on the upper cover of experiment chamber, and one end that swingle extends in experiment chamber connects specimen mounting; Sealing is realized 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, lifting slide unit is the L-type lifting slide unit that facade and surface level are formed, 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 to slide up and down; The upper and lower of ball screw is separately installed with stop, and moving up and down of slide unit of lifting is limited by stop; Electric rotating machine is arranged on the surface level of L-type lifting slide unit, and the bottom of electric rotating machine connects one end of swingle, and electric rotating machine is rotated in experiment chamber by the specimen mounting of the swingle driven rotary bar other end; Swingle keeps coaxial with the hole in the middle part of the upper cover of experiment chamber, realizes dynamic seal (packing) between the two by metal and super heated rubber circle crush seal device.
2. according to rotary dynamic metal corrosion device according to claim 1, it is characterized in that, the outer setting artificial intelligence temperature controller of rotary dynamic metal corrosion device, the temperature element one end be connected with artificial intelligence temperature controller extends tests in chamber.
3. according to rotary dynamic metal corrosion device according to claim 1, it is characterized in that, metal and super heated rubber circle crush seal device are placed in tests chamber upper cover and experiment junction, chamber, and swingle and upper cover center pit junction, realizes Static and dynamic respectively and seals.
4. according to rotary dynamic metal corrosion device according to claim 1, it is characterized in that, rotary dynamic metal corrosion device uses electric rotating machine to drive specimen mounting to rotate, and causes the relative motion between sample and liquid metal, realizes Dynamic Corrosion experiment; Thus, by adjusting rotating speed and the position of sample on specimen mounting of electric rotating machine, the relative motion speed of adjustment sample and liquid metal further.
5. according to rotary dynamic metal corrosion device according to claim 1, it is characterized in that, the glass-lined that inside, experiment chamber has high purity quartz to make, is used for avoiding the contact between liquid metal and experiment chamber, reduces because the interference caused experimental result is corroded in experiment chamber; Use schmigel to tamp between glass-lined and experiment chamber, avoid rocking of glass-lined in experimentation.
6. according to rotary dynamic metal corrosion device according to claim 1, it is characterized in that, the center pit loading test chamber of swingle chamber upper cover is by experiment inner, and connects 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 according to claim 1, it is characterized in that: before experiment starts, use the vacuum pump in gas circuit and sealing system to be evacuated in the experiment chamber of sealing and set below vacuum tightness, and then use temperature control and reactor assembly that experiment chamber is heated to design temperature; And pass into the mixed gas of setting in backward experiment chamber, and in whole experimentation in holding chamber atmosphere stablize; Drive specimen mounting to rotate by swingle in experimentation, realize the relative motion between sample and liquid metal, in experimentation, use lifting motor to promote or decline specimen mounting.
8., according to the using method of rotary dynamic metal corrosion device according to claim 7, it is characterized in that, comprise the steps:
1) glass-lined is put into experiment chamber, and use schmigel to be tamped in the space between glass-lined and experiment chamber, and appropriate corrosive medium reguline metal is loaded in glass-lined;
2) in the upper cover center pit of experiment chamber, crush seal metal frame and super heated rubber circle is put into, by swingle through experiment chamber upper cover center pit;
3) be connected with through the swingle of testing chamber upper cover by specimen mounting, be installed sample simultaneously on specimen mounting, uses lifting motor, be promoted to by specimen mounting and exceed glass-lined position;
4) cover experiment chamber upper cover, use locking buckle locked experiment chamber upper cover, use vacuum pump that experiment chamber air pressure inside is evacuated to setting value;
5) use temperature control and reactor assembly to carry out heating and temperature control, Heating Experiment chamber, is fused into liquid by corrosive medium reguline metal, ensures that experiment cavity temperature runs according to setting program simultaneously, keeps vacuum tightness in experiment chamber in the process;
6) after experiment intraluminal fluid state metal reaches predetermined temperature and be in stable condition, use gas mixing device in experiment chamber, inject the mixed gas of design, gas flow is controlled by gas meter;
7) after experiment intracavity gas pressure and composition are stablized, use lifting motor to be lowered by specimen mounting, in immersion 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, first stop the rotation motor, uses lifting motor to be promoted to by specimen mounting and depart from liquid metal liquid level, then stop heating, strengthen gas flow, make experiment cavity pressure 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 and specimen mounting is promoted to exceed with experiment chamber upper cover simultaneously test position, chamber, taking-up sample.
9. according to the using method of rotary dynamic metal corrosion device according to claim 7, it is characterized in that, swingle axis and experiment chamber center pit dead in line; Sample is symmetrical on specimen mounting to be placed, to ensure sealing effectiveness in rotary course.
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