CN202676528U - High-temperature high-pressure in situ high-speed scratching device - Google Patents

High-temperature high-pressure in situ high-speed scratching device Download PDF

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Publication number
CN202676528U
CN202676528U CN 201220352774 CN201220352774U CN202676528U CN 202676528 U CN202676528 U CN 202676528U CN 201220352774 CN201220352774 CN 201220352774 CN 201220352774 U CN201220352774 U CN 201220352774U CN 202676528 U CN202676528 U CN 202676528U
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pressure
autoclave
electrode
temperature
situ
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郦晓慧
王俭秋
韩恩厚
柯伟
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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 utility model relates to a scratching device, in particular to a high-temperature high-pressure in situ high-speed scratching device which solves a series of problems of the prior art of difficultly realizing in situ high-speed scratching, scratching sample fixing and insulating, signal wire lead-out, high-speed movement shaft pressure balancing, high-precision timing of sealing and scratching processes, and the like. The scratching device comprises a high-pressure kettle, an annular heater, a manual/hydraulic double-upright fixed bracket, a control box, a high-speed movement shaft, a scratching head, a sample fixing device, a cylinder, a reversing valve, magnetic steel, a Hall sensor and a precise timer. According to the scratching device, the in situ high-speed scratching research of the surface of a metal sample in a high-temperature and high-pressure environment can be realized, the time used by the high-speed scratching process can be precisely recorded, and signals of a process from damage to purification of a film of the sample in the scratching process can be detected out through a high-temperature high-pressure reference electrode, a high-temperature high-pressure working electrode and an auxiliary electrode by matching with an electrochemical workstation.

Description

A kind of high-temperature high-pressure in-situ scratches at a high speed device
Technical field
The utility model relates to corrosion-resistant material surface tear technology, is specially a kind of high-temperature high-pressure in-situ and scratches at a high speed device.
Background technology
Rely on that the surface forms fine and close passivating film and corrosion resistant alloy with corrosion resistance, when the passivating film on local surface exposes unsalted surface because of physical disturbance, then can aggravate the generation of unsalted surface corrosion, thereby form new passivating film in this position, and the generation of again passivation relies on the acting in conjunction of material itself and environmental factor.Therefore, metal material in specific environment again the in-situ characterization of passivation ability for the evaluation material have vital role at the decay resistance under the operating mode.
At present, material again the sign of passivation ability mainly realize by scratching the electrode method.Again the film forming on fresh material surface is a Fast Process in high temperature and high pressure environment, this just requires scuffing speed necessary fast so, otherwise will cause the scuffing of specimen surface limit, limit passivation, the signal that collects so also is a series of stacks of unsharp signal and the earlier scratch surface unsharp signal of unsalted surface, can not accurately reflect the again passivation ability of material in specific environment.Yet, because high-temperature high-pressure in-situ scratches at a high speed the device complexity, the original position that not only will realize material surface passivating film under the High Temperature High Pressure scratches at a high speed, also to consider pressure equilibrium, sealing, high-precision timing, sample and canister between realization, high-speed motion axle and the autoclave of lower stroke of head height of High Temperature High Pressure speed motion insulation, signal wire the series of problems such as draw.Exactly because the technical difficulty on these experimental facilitiess has limited the in-situ characterization to the corrosion-resistant material passivation ability that uses in the high temperature hyperbaric environments such as nuclear power and thermoelectricity.At present, relevant device yet there are no report.
The utility model content
The purpose of this utility model is to provide a kind of high-temperature high-pressure in-situ to scratch at a high speed device, solves to be difficult under the high temperature and high pressure environment in the prior art to realize that original position scratches at a high speed, scratches the problems such as the pressure equilibrium of the drawing of fixing, the insulation of sample, signal wire, high-speed motion axle and sealing.
The technical solution of the utility model is as follows:
A kind of high-temperature high-pressure in-situ scratches at a high speed device, this device is provided with: High Temperature High Pressure working electrode, High Temperature High Pressure auxiliary electrode, High Temperature High Pressure contrast electrode, up and down high pressure kettle cover, autoclave body, high-speed motion axle, draw head, ring heater, concrete structure is as follows:
Autoclave body and up and down two high pressure kettle covers consist of autoclaves, autoclave body is arranged at up and down between two high pressure kettle covers, autoclave body and two the high pressure kettle covers connections of being connected; Cover at upper autoclave thermopair, High Temperature High Pressure work/auxiliary electrical electrode seat and High Temperature High Pressure contrast electrode are set, auxiliary electrode is set in the autoclave body, draws head, working electrode, auxiliary electrode and working electrode pass High Temperature High Pressure work/auxiliary electrical electrode seat by wire respectively, and the catheter of High Temperature High Pressure contrast electrode extends in the autoclave body;
The high-speed motion axis hole at guide plate center is passed on high-speed motion axle top, be connected with guide plate, the guide plate periphery cooperates with cradling piece in the autoclave body by the hole, namely move up and down take cradling piece as guide rod, be provided with pressure balance mechanism between high-speed motion axle and the autoclave, and seal by O-ring seal, high-speed motion axle bottom is connected with the pneumatic piston connecting rod of pneumatic means, be equipped with on the high-speed motion axle and draw head, sample fixing is arranged on the stationary platform;
The arranged outside ring heater of autoclave body, autoclave arrange two column supports outward, two columns on two column supports: column I and column II are set in parallel in up and down the both sides of two high pressure kettle covers, autoclave body, ring heater; The slide block I is set on the column I, is hydraulic-driven, the slide block II is set on the column II, for the hand-operated lifting dish drives; The slide block I is connected with autoclave body and counterweight, and the autoclave body outside is provided with ring heater, and the slide block II is connected with the high pressure kettle cover.
Described high-temperature high-pressure in-situ scratches at a high speed device, also comprise control box, heating power supply switch, burner on light, overtemperature alarm lamp, overpressure alarm lamp, timer reset button, temperature controller, heating voltage regulator, pressure display unit and timer are set in the control box; Wherein, timer is connected with the timer reset button, pressure display unit is connected with the overpressure alarm lamp, the overtemperature alarm lamp links to each other with temperature controller, the heating power supply switch is connected with the heating voltage regulator, the heating power supply switch is connected with burner on light, the heating voltage regulator is connected with temperature controller, pressure display unit and temperature controller are connected to the control box internal relay, the control box internal relay connects the electric furnace heating wire of ring heater by wire, form overtemperature outage heating arrangement and superpressure outage heating arrangement.
Described high-temperature high-pressure in-situ scratches at a high speed device, and the height of slide block I is regulated by hydraulic mechanism, and the bottom of column I is provided with hydraulic jack, and hydraulic jack adopts pedal-operated oil pump, is connected with pedal and spring reset mechanism in the hydraulic jack bottom outside; Adopt the governor motion of nut screw between slide block II and the column, the top of column II arranges the hand-operated lifting dish, by regulating the hand-operated lifting dish slide block II is moved up and down in the column II.
Described high-temperature high-pressure in-situ scratches at a high speed device, keep the balance of high-speed motion axle inside and outside autoclave by pressure balance mechanism, the high-speed motion axle adopts the mode of connection segment, covers at lower autoclave and is provided with high-speed motion axle axle sleeve, and the axle sleeve outside is provided with cooling jacket.
Described high-temperature high-pressure in-situ scratches at a high speed device, and the thermopair that upper autoclave covers stretches in the autoclave body, and the autoclave gas phase mouth divides three the tunnel, respectively Bonding pressure table, safety valve, pressure unit; Upper autoclave is covered with the exhaust passage that communicates with the autoclave body inner chamber, and the autoclave vent valve is equipped with in the outlet side of described exhaust passage; Lower autoclave covers and is provided with inlet channel and the feed pathway that communicates with the autoclave body inner chamber, and the inlet end of described inlet channel is equipped with gas admittance valve, and the liquid feeding end of described feed pathway is equipped with liquid feed valve, and feed pathway extends the top with the autoclave body inner chamber.
Described high-temperature high-pressure in-situ scratches at a high speed device, auxiliary electrode has the platinum filament of teflon heat-shrink tube to be welded in the platinized platinum back as tracerse point by outer cover, working electrode has the pure nickel wire of teflon heat-shrink tube or stainless steel wire to be welded on the test button as tracerse point by outer cover; Be provided with the high temperature plug in High Temperature High Pressure work/auxiliary electrical electrode seat, the wire on the auxiliary electrode and the wire on the working electrode are drawn from High Temperature High Pressure work/auxiliary electrical electrode seat.
Described high-temperature high-pressure in-situ scratches at a high speed device, also be provided with electrochemical workstation, the working electrode on the electrochemical workstation, auxiliary electrode and contrast electrode are connected wire clamp and are connected with High Temperature High Pressure working electrode wire, High Temperature High Pressure auxiliary electrode wire and High Temperature High Pressure contrast electrode wire respectively.
Described high-temperature high-pressure in-situ scratches at a high speed device, have the lifting platform hole on the platform, autoclave inner support bar is arranged in the lifting platform hole, platform is fixed on the autoclave inner support bar by the platform set bolt parallel with platform, autoclave inner support bar two ends are provided with screw thread, and autoclave inner support bar is fixed in lower autoclave by screw thread and covers.
Described high-temperature high-pressure in-situ scratches at a high speed device, draw back of head and be provided with spring, drawing a side setting stroke set bolt, sample is fixed in the sample fixing, be provided with the sample fastening bolt on sample fixing at the sample back, sample and fixedly adopt insulation system between the device of sample: teflon groove, the teflon groove is installed in the Baltimore groove of sample fixing, Baltimore groove is the closing in shape, its open top width is convenient to working electrode is fixed in the teflon groove less than bottom width.
Described high-temperature high-pressure in-situ scratches at a high speed device, one end of pneumatic piston connecting rod is connected with high-speed motion axle lower end, the other end of pneumatic piston connecting rod is provided with reciprocating piston in cylinder, air intake opening and exhausr port are communicated with two chambeies in the cylinder by reversal valve respectively, realize that by reversal valve the high speed of kinematic axis moves up and down; The pneumatic piston connecting rod junction of high-speed motion axle and pneumatic means is provided with magnet steel, and magnet steel is corresponding with Hall element, cooperates Hall element and timer with the accurate record of run duration of high-speed motion axle.
The beneficial effects of the utility model are:
1, the utility model device has realized that sample original position under High Temperature High Pressure scratches at a high speed and passivation behavioral study again.By making insulation between sample and device, utilize the High Temperature High Pressure contrast electrode be installed on the autoclave and High Temperature High Pressure work, auxiliary electrode to cooperate the electrochemical workstation can be with sample surface film in the scuffing process by failure to the input of this process of passivation more out.
2, the utility model is connected by the piston rod with high-speed motion axle and outer inside casing, has the fireballing characteristics of scuffing, and adjustable pneumatic device inflow point air pressure changes the scuffing speed of high-speed motion axle.
3, the utility model is provided with magnet steel in the junction of high-speed motion axle and outer inside casing piston rod, cooperates Hall element and timer the run duration of high-speed motion axle accurately can be measured, and is convenient to scratch the quantification contrast of experimental result.
4, the utility model is by arranging spring drawing a back of head, can control dynamics size when drawing head and streaking specimen surface by regulating the distance of drawing between head and the sample.
5, the utility model can produce the cut of different in width and different depth by changing drawing head and regulating the distance of drawing between head and sample of different angles.
6, the utility model has solved the pressure equilibrium of high-speed motion axle and the problem of sealing by pressure balanced mode.
7, the axle of drawing in the utility model passes through connection segment, is easy to dismounting and maintenance.
8, the utility model is by at control section overtemperature auto-breaking and overvoltage automatic cutout being set respectively, and is more safe and reliable when making this device busy.
9, the utility model arranges standard interface outside autoclave, can by cutting ferrule and outside high-temperature high-pressure water circulation corrosion experiment system with automatic control function (referring to Chinese invention patent: 201010275276.2, the applying date: on 09 08th, 2010; Chinese utility model patent: 201020521040.8, the applying date: on 09 08th, 2010, authorize day: on 06 01st, 2011) connect, thus can accurately control the interior chemical environment of water of autoclave.
Description of drawings
Fig. 1 is that high-temperature high-pressure in-situ scratches at a high speed the apparatus structure schematic diagram.
Among the figure, 1 contrast electrode; 2 hand-operated lifting dishes; 3 cooling of electrode water inlets; 4 column II; 5 thermopairs; 6 slide block II; 7 guide plates; 8 working electrodes (sample); 9 ring heaters; 10 high-speed motion axles; 11 strokes of heads; 12 gas admittance valves; 13 high-speed motion axle cooling water inlets; 14 reversal valve switches; 15 reversal valves; 16 pneumatic piston connecting rods; 17 pistons; 18 air intake openings; 19 exhausr ports; 20 air releases; 21 pedals; 22 hydraulic jacks; 23 Hall elements; 24 high-speed motion axle coolant outlets; 25 liquid feed valves; 26 auxiliary electrodes; 27 counterweights; 28 slide block I; 29 autoclave vent valves; High pressure kettle cover on 30; 31 column I; 32 cooling of electrode water outs; 33 pressure units; 34 tensimeters; 35 safety valve; 36 magnet steel; 37 times high pressure kettle covers; 38 autoclave bodies; 39 High Temperature High Pressure work/auxiliary electrical electrode seat; 40 catheters; 41 cylinders; 42 cradling pieces; 62 axle sleeves; 63 cooling jackets.
Fig. 2 is Fig. 1 mesohigh kettle inner structure schematic diagram.
Among the figure, 11 strokes of heads; 38 autoclave bodies; 43 platforms; 44 lifting platform holes; 45 platform set bolts; 46 springs; 47 sample fixing; 49 sample fastening bolts; 50 teflon grooves; 51 strokes of set bolts.
Fig. 3 is guide board structure schematic diagram among Fig. 1.
Among the figure, 7 guide plates; 52 high-speed motion axis holes; 53 pilot holes.
Fig. 4 is that high-temperature high-pressure in-situ scratches at a high speed the device control box.
Among the figure, 48 burner on lights; 54 heating voltage regulators; 55 pressure display units; 56 timer; 57 timer reset button; 58 overpressure alarm lamps; 59 overtemperature alarm lamps; 60 heating power supply switches; 61 temperature controllers.
Embodiment
Such as Fig. 1-shown in Figure 4, the utility model high-temperature high-pressure in-situ scratches at a high speed device, this device is provided with: contrast electrode 1, hand-operated lifting dish 2, cooling of electrode water inlet 3, column II 4, thermopair 5, slide block II 6, guide plate 7, working electrode (sample) 8, ring heater 9, high-speed motion axle 10, draw 11, gas admittance valve 12, high-speed motion axle cooling water inlet 13, reversal valve switch 14, reversal valve 15, pneumatic piston connecting rod 16, piston 17, air intake opening 18, exhausr port 19, air release 20, pedal 21, hydraulic jack 22, Hall element 23, high-speed motion axle coolant outlet 24, liquid feed valve 25, auxiliary electrode 26, counterweight 27, slide block I 28, autoclave vent valve 29, upper high pressure kettle cover 30, column I 31, cooling of electrode water out 32, pressure unit 33, tensimeter 34, safety valve 35, magnet steel 36, lower high pressure kettle cover 37, autoclave body 38, High Temperature High Pressure work/auxiliary electrical electrode seat 39, catheter 40, cylinder 41, cradling piece 42, platform 43, lifting platform hole 44, platform set bolt 45, spring 46, sample fixing 47, burner on light 48, sample fastening bolt 49, teflon groove 50, draw a set bolt 51, high-speed motion axis hole 52, pilot hole 53, heating voltage regulator 54, pressure display unit 55, timer 56, timer reset button 57, overpressure alarm lamp 58, overtemperature alarm lamp 59, heating power supply switch 60, temperature controller 61, axle sleeve 62, cooling jacket 63 etc., concrete structure is as follows:
Autoclave body 38 and up and down two high pressure kettle covers (upper high pressure kettle cover 30, lower high pressure kettle cover 37) consist of autoclave, autoclave body 38 is arranged at up and down between two high pressure kettle covers, autoclave body 38 and two the high pressure kettle covers connections of being connected; At upper high pressure kettle cover 30 thermopair 5, High Temperature High Pressure work/auxiliary electrical electrode seat 39 and High Temperature High Pressure contrast electrode 1 are set, autoclave body 38 is interior to arrange auxiliary electrode 26, draw 11, working electrode (sample) 8, auxiliary electrode 26 and working electrode (sample) 8 passes High Temperature High Pressure work/auxiliary electrical electrode seat 39 by wire respectively, and the catheter 40 of High Temperature High Pressure contrast electrode 1 extends in the autoclave body 38; Between High Temperature High Pressure work/auxiliary electrical electrode seat 39 and the High Temperature High Pressure contrast electrode 1 the circulating cooling aquaporin is set, High Temperature High Pressure contrast electrode 1 is provided with cooling of electrode water inlet 3, and High Temperature High Pressure work/auxiliary electrical electrode seat 39 is provided with cooling of electrode water out 32.
The high-speed motion axis hole 52 at guide plate 7 centers is passed on high-speed motion axle 10 tops, be connected with guide plate 7 by nut, be respectively equipped with pilot hole 53(Fig. 3 around the guide plate 7), guide plate 7 cooperates by pilot hole 53 and autoclave body 38 interior cradling pieces 42, namely move up and down take cradling piece 42 as guide rod, be provided with pressure balance mechanism between high-speed motion axle 10 and the autoclave, and seal by O-ring seal, high-speed motion axle 10 bottoms are connected with the pneumatic piston connecting rod 16 of pneumatic means, are equipped with on the high-speed motion axle 10 to draw 11;
The arranged outside ring heater 9 of autoclave body 38, autoclave arrange two column supports outward, two columns on two column supports: column I 31, column II 4 are set in parallel in up and down the both sides of two high pressure kettle covers, autoclave body 38, ring heater 9; Slide block I 28 is set on the column I 31, is hydraulic-driven; Slide block II 6 is set, for the hand-operated lifting dish drives on the column II 4.Slide block I 28 is connected with autoclave body 38 and counterweight 27, and autoclave body 38 outsides are provided with ring heater 9, and slide block II 6 is connected with high pressure kettle cover 30.
In addition, as shown in Figure 4, also comprise control box, heating power supply switch 60, burner on light 48, overtemperature alarm lamp 59, overpressure alarm lamp 58, timer reset button 57, temperature controller 61, heating voltage regulator 54, pressure display unit 55 and timer 56 are set in the control box; Wherein, timer 56 is connected with timer reset button 57, and pressure display unit 55 is connected with overpressure alarm lamp 58, and overtemperature alarm lamp 59 links to each other with temperature controller 61.Heating power supply switch 60 is connected with heating voltage regulator 54, heating power supply switch 60 is connected with burner on light 48, heating voltage regulator 54 is connected with temperature controller 61, pressure display unit 55 and temperature controller 61 are connected to the control box internal relay, the control box internal relay connects the electric furnace heating wire of ring heater 9 by wire, form overtemperature outage heating arrangement and superpressure outage heating arrangement.
The height of slide block I 28 is regulated by hydraulic mechanism, the bottom of column I 31 is provided with hydraulic jack 22, hydraulic jack 22 adopts pedal-operated oil pump, be connected with pedal 21 and spring reset mechanism in hydraulic jack 22 bottom outside, hydraulic jack 22 by its bottom outside pedal 21 and cooperate the manually-operated gate at its middle part to start, realize that slide block I 28 moves up and down along column I 31; Adopt the governor motion of nut screw between slide block II 6 and the column II 4, the top of column II 4 arranges hand-operated lifting dish 2, by regulating hand-operated lifting dish 2 slide block II 6 is moved up and down in column II 4.
Keep the balance of high-speed motion axle inside and outside autoclave by pressure balance mechanism, high-speed motion axle 10 adopts the mode of connection segment, be provided with high-speed motion axle axle sleeve 62 at lower high pressure kettle cover 37, axle sleeve 62 outsides are provided with cooling jacket 63, are respectively equipped with high-speed motion axle cooling water inlet 13 and high-speed motion axle coolant outlet 24 on the cooling jacket 63.
Upper high pressure kettle cover 30 is provided with thermopair 5 and stretches in the autoclave body 38, and upper high pressure kettle cover 30 is provided with the autoclave gas phase mouth, and the autoclave gas phase mouth divides three the tunnel, respectively Bonding pressure table 34, safety valve 35, pressure unit 33.
Upper high pressure kettle cover 30 is provided with the exhaust passage that communicates with autoclave body 38 inner chambers, and autoclave vent valve 29 is equipped with in the outlet side of described exhaust passage; Lower high pressure kettle cover 37 is provided with inlet channel and the feed pathway that communicates with autoclave body 38 inner chambers, the inlet end of described inlet channel is equipped with gas admittance valve 12, the liquid feeding end of described feed pathway is equipped with liquid feed valve 25, and feed pathway extends the top with autoclave body 38 inner chambers.
Auxiliary electrode 26 has the platinum filament of teflon heat-shrink tube to be welded in the platinized platinum back as tracerse point by outer cover, working electrode (sample) 8 has the pure nickel wire of teflon heat-shrink tube or stainless steel wire to be welded on the test button as tracerse point by outer cover; Be provided with four hole high temperature plugs in High Temperature High Pressure work/auxiliary electrical electrode seat 39, the wire on the wire on the auxiliary electrode 26 and the working electrode (sample) 8 is drawn from High Temperature High Pressure work/auxiliary electrical electrode seat 39.
In addition, also be provided with electrochemical workstation, the working electrode on the electrochemical workstation, auxiliary electrode and contrast electrode are connected wire clamp and are connected wire with the High Temperature High Pressure contrast electrode with High Temperature High Pressure working electrode (sample) 8 wires, High Temperature High Pressure auxiliary electrode 26 wires respectively and are connected.
As shown in Figure 2, have lifting platform hole 44 on the platform 43, autoclave inner support bar 42 is arranged in lifting platform hole 44, platform 43 is fixed on the autoclave inner support bar 42 by the four platforms set bolt 45 parallel with platform 43, autoclave inner support bar 42 two ends are provided with screw thread, and autoclave inner support bar 42 is fixed on the lower high pressure kettle cover 37 by screw thread.Draw 11 rear portion and be provided with spring 46, drawing a side setting stroke set bolt 51, sample fixing 47 is arranged on the platform 43, working electrode (sample) 8 is fixed in the sample fixing 47, be provided with sample fastening bolt 49 on sample fixing 47 at working electrode (sample) 8 backs, working electrode (sample) 8 and fixedly adopt insulation system between the device of sample: teflon groove 50, teflon groove 50 is installed in the Baltimore groove of sample fixing 47, Baltimore groove is the closing in shape, its open top width is convenient to working electrode (sample) 8 is fixed in the teflon groove 50 less than bottom width.
One end of pneumatic piston connecting rod 16 is connected with high-speed motion axle 10 lower ends, the other end of pneumatic piston connecting rod 16 is provided with reciprocating piston 17 in cylinder 41, air intake opening 18 and exhausr port 19 are communicated with two chambeies in the cylinder 41 by reversal valve 15 respectively, thus moving up and down by reversal valve realization kinematic axis.Cylinder 41 bottoms also are provided with air release 20, and its effect is further to accelerate the axially speed of lower motion of high-speed motion.
High-speed motion axle 10 and pneumatic means connecting rod 16 junctions are provided with magnet steel 36, and magnet steel 36 is corresponding with Hall element 23, cooperate Hall element 23 and timer 56 can be with the run duration of high-speed motion axle accurate record.
In the utility model, High Temperature High Pressure refers to: maximum operating temperature is 350 ℃, and maximum working pressure (MOP) is 20MPa.
In the utility model, the fastest motion speed that high-speed motion axle single moves downward is 4m/s.
In the utility model, the High Temperature High Pressure solution in the autoclave can produce a downward acting force to the high-speed motion axle, and the chamber inner high voltage liquid that high-speed motion axle axle sleeve bottom is connected with autoclave then can produce an acting force that makes progress to the high-speed motion axle.Pressure balance mechanism mainly refers to the balance between these two power.In addition, the high-speed motion axle also is subjected to friction force and the self gravitation effect between itself and the O-ring seal, and the high-speed motion shaft balancing mainly is this acting in conjunction that is subjected to these four power.
In the utility model, the timing resolution of timer is 0.1ms.
In the utility model, the maximum operating temperature of high temperature plug is 260 ℃.Because be connected with chilled water in High Temperature High Pressure work/auxiliary electrical electrode seat, so the high temperature plug is in the normal temperature state when normal operation.
The course of work that the utility model high-temperature high-pressure in-situ scratches at a high speed device is as follows:
One, scratch at a high speed device not when high-temperature high-pressure water circulation corrosion experiment system that the outside has an automatic control function links to each other when high-temperature high-pressure in-situ:
1, with pure nickel wire or stainless steel wire appearance surface cover one deck teflon heat-shrink tube, with after the heat gun pyrocondensation as wire bonds on working electrode (sample) 8 surfaces;
2, working electrode (sample) 8 is installed in the sample fixing 47 that is provided with teflon groove 50, and the sample fastening bolt 49 at working electrode (sample) 8 backs is tightened;
3, auxiliary electrode 26 is installed in the autoclave, and maintenance and sample over against;
4, will be installed on the upper high pressure kettle cover 30 after 1 demarcation of High Temperature High Pressure contrast electrode, and keep the liquid outlet on High Temperature High Pressure contrast electrode 1 top to close;
5, regulate to draw 11 and the distance of working electrode (sample) 8 and draw the spring 46 at a back, guarantee to draw 11 in the process of sliding, can contact with working electrode (sample) 8, and can not touch auxiliary electrode 26;
6, regulate hydraulicefficiency elevation structure (hydraulic jack 22), autoclave body 38 and lower high pressure kettle cover 37 are adjusted to suitable height, tighten the bolt on the lower high pressure kettle cover 37;
7, adding volume in the autoclave is the solution of autoclave volume 1/2 to 2/3, solution can be selected according to actual working environment, as simulate the aqueous solution etc. of nuclear power station one loop boronic acid containing and lithium hydroxide, and guarantee that the lower end of working electrode (sample) 8, auxiliary electrode 26 and High Temperature High Pressure contrast electrode catheter 40 can be immersed in the solution fully;
8, regulate hand-operated lifting dish 2, upper high pressure kettle cover 30 and autoclave body 38 are adjusted to suitable height, and working electrode (sample) 8 and auxiliary electrode 26 wires are drawn from the High Temperature High Pressure work of upper high pressure kettle cover/auxiliary electrical electrode seat 39, tighten the bolt on the high pressure kettle cover 30;
9, to autoclave body 38, pass into the nitrogen deoxygenation according to testing the air intake opening of needs from lower high pressure kettle cover 38, then from the autoclave vent valve 29 of upper high pressure kettle cover 30, discharge.Degasification is closed the gas admittance valve 12 of lower high pressure kettle cover 37 and the autoclave vent valve 29 of upper high pressure kettle cover 30 successively, and is opened the liquid outlet on High Temperature High Pressure contrast electrode 1 top after finishing;
10, the parameters such as upper pressure limit of the upper temperature limit of the target temperature on the design temperature controller 61, overtemperature auto-breaking, heat regulation voltage and overvoltage automatic cutout;
11, open cooling water switch, in the cooling jacket 63 of High Temperature High Pressure electrode cooling water inlet 3 and high-speed motion axle axle sleeve outside, pass into chilled water;
12, open heating power supply switch 60, after High Temperature High Pressure contrast electrode 1 liquid outlet continuous effluent, liquid outlet place valve tightened close;
13, treat that temperature reaches setting value, and after tending towards stability, utilize potentiostat to adding a constant potential on the sample according to the experiment needs, and stable a period of time makes it be in passive state.Press timer reset button 57, open the air release 20 of cylinder 41 bottoms.Then, press reversal valve switch 14, make cylinder 41 top fast aeration, so promote piston, the high-speed motion axle 10 that is connected with piston rod moves downward fast, drive to draw thus 11 and streak at a high speed from top to bottom working electrode (sample) 8 surfaces, destroy the specimen surface passivating film.By the curent change in electrochemical workstation Quick Acquisition and the record specimen surface passivating film again film forming procedure, just can know the again passivation ability of material.
14, finish single and scratch at a high speed after, close the air release 20 of pneumatic part, pull open reversal valve switch 14, make the inflation of cylinder 41 bottoms, and then promote piston, the high-speed motion axle 10 that is connected with piston rod moves upward, and makes stroke 11 location restore to initial position.After working electrode (sample) 8 surface tear positions regenerated passivating film, repeating step 13 can carry out Inactivation experiment research again again.
Two, when high-temperature high-pressure in-situ scratches at a high speed high-temperature high-pressure water circulation corrosion experiment system that device and outside have automatic control function and links to each other:
1, with pure nickel wire or stainless steel wire appearance surface cover one deck teflon heat-shrink tube, with after the heat gun pyrocondensation as wire bonds on working electrode (sample) 8 surfaces;
2, working electrode (sample) 8 is installed in the sample fixing that is provided with teflon groove 50, and the sample fastening bolt 49 at working electrode (sample) 8 backs is tightened;
3, auxiliary electrode 26 is installed in the autoclave, and maintenance and sample over against;
4, will be installed on the upper high pressure kettle cover 30 after 1 demarcation of High Temperature High Pressure contrast electrode, and keep the liquid outlet on High Temperature High Pressure contrast electrode 1 top to open;
5, regulate to draw 11 and the distance of working electrode (sample) 8 and draw the spring 46 at a back, guarantee to draw 11 in the process of sliding, can contact with working electrode (sample) 8, and can not touch auxiliary electrode 26;
6, regulate hydraulicefficiency elevation structure (hydraulic jack 22), autoclave body 38 and lower high pressure kettle cover 37 are adjusted to suitable height, tighten the bolt on the lower high pressure kettle cover 37;
7, regulate hand-operated lifting dish 2, upper high pressure kettle cover 30 and autoclave body 38 are adjusted to suitable height, and working electrode (sample) 8 and auxiliary electrode 26 wires are drawn from the High Temperature High Pressure work of upper high pressure kettle cover/auxiliary electrical electrode seat 39, tighten the bolt on the high pressure kettle cover 30;
8, by cutting ferrule the inlet on the lower high pressure kettle cover 37 is linked to each other with the high-temperature high-pressure water circulation corrosion experiment system that the outside has automatic control function with air intake opening place pipeline, solution can be selected according to actual working environment, such as the aqueous solution of simulation nuclear power station one loop boronic acid containing and lithium hydroxide etc.;
9, after the every water chemistry parameter in whole high-temperature high-pressure water circulation corrosion experiment system reaches setting value, open liquid feed valve 25 on the lower high pressure kettle cover 37 and the autoclave vent valve 29 on the upper high pressure kettle cover 30, after the autoclave vent valve 29 place's continuous effluent on the upper high pressure kettle cover 30 with exhaust valve closure, after High Temperature High Pressure contrast electrode 1 liquid outlet continuous effluent, contrast electrode 1 liquid outlet place valve tightened close.Then open the gas admittance valve 12 on the lower high pressure kettle cover 37;
10, the interlock adjusting by high-pressure pump and counterbalance valve makes the pressure of system high pressure part reach preset value;
11, observe whole system various piece normal operation, after leaking, the parameters such as upper pressure limit of the upper temperature limit of the target temperature on the design temperature controller 61, overtemperature auto-breaking, heat regulation voltage and overvoltage automatic cutout;
12, open cooling water switch, in the cooling jacket 63 of High Temperature High Pressure electrode cooling water inlet 3 and high-speed motion axle axle sleeve outside, pass into chilled water, then open primary heater in the high-temperature high-pressure water circulation corrosion experiment system and the heating power supply switch 60 of autoclave;
13, treat that temperature reaches setting value, and after tending towards stability, utilize potentiostat to adding a constant potential on the sample according to the experiment needs, and stable a period of time makes it be in passive state.Press the timer reset button, open the air release 20 of cylinder 41 bottoms.Then, press reversal valve switch 14, make cylinder 41 top fast aeration, so promote piston, the high-speed motion axle 10 that is connected with piston rod moves downward fast, drive to draw thus 11 and streak at a high speed from top to bottom working electrode (sample) 8 surfaces, destroy the specimen surface passivating film.By the curent change in electrochemical workstation Quick Acquisition and the record specimen surface passivating film again film forming procedure, just can know the again passivation ability of material.
14, finish single and scratch at a high speed after, close the air release 20 of pneumatic part, pull open reversal valve switch 14, make the inflation of cylinder 41 bottoms, and then promote piston, the high-speed motion axle 10 that is connected with piston rod moves upward, and makes stroke 11 location restore to initial position.After working electrode (sample) 8 surface tear positions regenerated passivating film, repeating step 13 can carry out Inactivation experiment research again again.

Claims (10)

1. a high-temperature high-pressure in-situ scratches at a high speed device, it is characterized in that, this device is provided with: High Temperature High Pressure working electrode, High Temperature High Pressure auxiliary electrode, High Temperature High Pressure contrast electrode, up and down high pressure kettle cover, autoclave body, high-speed motion axle, draw head, ring heater, concrete structure is as follows:
Autoclave body and up and down two high pressure kettle covers consist of autoclaves, autoclave body is arranged at up and down between two high pressure kettle covers, autoclave body and two the high pressure kettle covers connections of being connected; Cover at upper autoclave thermopair, High Temperature High Pressure work/auxiliary electrical electrode seat and High Temperature High Pressure contrast electrode are set, auxiliary electrode is set in the autoclave body, draws head, working electrode, auxiliary electrode and working electrode pass High Temperature High Pressure work/auxiliary electrical electrode seat by wire respectively, and the catheter of High Temperature High Pressure contrast electrode extends in the autoclave body;
The high-speed motion axis hole at guide plate center is passed on high-speed motion axle top, be connected with guide plate, the guide plate periphery cooperates with cradling piece in the autoclave body by the hole, namely move up and down take cradling piece as guide rod, be provided with pressure balance mechanism between high-speed motion axle and the autoclave, and seal by O-ring seal, high-speed motion axle bottom is connected with the pneumatic piston connecting rod of pneumatic means, be equipped with on the high-speed motion axle and draw head, sample fixing is arranged on the stationary platform;
The arranged outside ring heater of autoclave body, autoclave arrange two column supports outward, two columns on two column supports: column I and column II are set in parallel in up and down the both sides of two high pressure kettle covers, autoclave body, ring heater; The slide block I is set on the column I, is hydraulic-driven, the slide block II is set on the column II, for the hand-operated lifting dish drives; The slide block I is connected with autoclave body and counterweight, and the autoclave body outside is provided with ring heater, and the slide block II is connected with the high pressure kettle cover.
2. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: also comprise control box, heating power supply switch, burner on light, overtemperature alarm lamp, overpressure alarm lamp, timer reset button, temperature controller, heating voltage regulator, pressure display unit and timer are set in the control box; Wherein, timer is connected with the timer reset button, pressure display unit is connected with the overpressure alarm lamp, the overtemperature alarm lamp links to each other with temperature controller, the heating power supply switch is connected with the heating voltage regulator, the heating power supply switch is connected with burner on light, the heating voltage regulator is connected with temperature controller, pressure display unit and temperature controller are connected to the control box internal relay, the control box internal relay connects the electric furnace heating wire of ring heater by wire, form overtemperature outage heating arrangement and superpressure outage heating arrangement.
3. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: the height of slide block I is regulated by hydraulic mechanism, the bottom of column I is provided with hydraulic jack, and hydraulic jack adopts pedal-operated oil pump, is connected with pedal and spring reset mechanism in the hydraulic jack bottom outside; Adopt the governor motion of nut screw between slide block II and the column, the top of column II arranges the hand-operated lifting dish, by regulating the hand-operated lifting dish slide block II is moved up and down in the column II.
4. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: keep the balance of high-speed motion axle inside and outside autoclave by pressure balance mechanism, the high-speed motion axle adopts the mode of connection segment, cover at lower autoclave and to be provided with high-speed motion axle axle sleeve, the axle sleeve outside is provided with cooling jacket.
5. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: the thermopair that upper autoclave covers stretches in the autoclave body, and the autoclave gas phase mouth divides three the tunnel, respectively Bonding pressure table, safety valve, pressure unit; Upper autoclave is covered with the exhaust passage that communicates with the autoclave body inner chamber, and the autoclave vent valve is equipped with in the outlet side of described exhaust passage; Lower autoclave covers and is provided with inlet channel and the feed pathway that communicates with the autoclave body inner chamber, and the inlet end of described inlet channel is equipped with gas admittance valve, and the liquid feeding end of described feed pathway is equipped with liquid feed valve, and feed pathway extends the top with the autoclave body inner chamber.
6. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: auxiliary electrode has the platinum filament of teflon heat-shrink tube to be welded in the platinized platinum back as tracerse point by outer cover, and working electrode has the pure nickel wire of teflon heat-shrink tube or stainless steel wire to be welded on the test button as tracerse point by outer cover; Be provided with the high temperature plug in High Temperature High Pressure work/auxiliary electrical electrode seat, the wire on the auxiliary electrode and the wire on the working electrode are drawn from High Temperature High Pressure work/auxiliary electrical electrode seat.
7. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: also be provided with electrochemical workstation, the working electrode on the electrochemical workstation, auxiliary electrode and contrast electrode are connected wire clamp and are connected with High Temperature High Pressure working electrode wire, High Temperature High Pressure auxiliary electrode wire and High Temperature High Pressure contrast electrode wire respectively.
8. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: have the lifting platform hole on the platform, autoclave inner support bar is arranged in the lifting platform hole, platform is fixed on the autoclave inner support bar by the platform set bolt parallel with platform, autoclave inner support bar two ends are provided with screw thread, and autoclave inner support bar is fixed in lower autoclave by screw thread and covers.
9. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: draw back of head and be provided with spring, drawing a side setting stroke set bolt, sample is fixed in the sample fixing, be provided with the sample fastening bolt on sample fixing at the sample back, sample and fixedly adopt insulation system between the device of sample: teflon groove, the teflon groove is installed in the Baltimore groove of sample fixing, Baltimore groove is the closing in shape, its open top width is convenient to working electrode is fixed in the teflon groove less than bottom width.
10. scratch at a high speed device according to high-temperature high-pressure in-situ claimed in claim 1, it is characterized in that: an end of pneumatic piston connecting rod is connected with high-speed motion axle lower end, the other end of pneumatic piston connecting rod is provided with reciprocating piston in cylinder, air intake opening and exhausr port are communicated with two chambeies in the cylinder by reversal valve respectively, realize that by reversal valve the high speed of kinematic axis moves up and down; The pneumatic piston connecting rod junction of high-speed motion axle and pneumatic means is provided with magnet steel, and magnet steel is corresponding with Hall element, cooperates Hall element and timer with the accurate record of run duration of high-speed motion axle.
CN 201220352774 2012-07-19 2012-07-19 High-temperature high-pressure in situ high-speed scratching device Expired - Lifetime CN202676528U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768133A (en) * 2012-07-19 2012-11-07 中国科学院金属研究所 High-temperature high-pressure in-situ high-speed scratching device
CN107267181A (en) * 2017-07-20 2017-10-20 孙振轩 Horizontal rotary damaged tire pyrocrack furnace

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102768133A (en) * 2012-07-19 2012-11-07 中国科学院金属研究所 High-temperature high-pressure in-situ high-speed scratching device
CN102768133B (en) * 2012-07-19 2014-04-09 中国科学院金属研究所 High-temperature high-pressure in-situ high-speed scratching device
CN107267181A (en) * 2017-07-20 2017-10-20 孙振轩 Horizontal rotary damaged tire pyrocrack furnace

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