CN108918221A - Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel - Google Patents
Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel Download PDFInfo
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Abstract
Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel, the present invention relates to Carbide Phases low-temperature electrolytics to extract field.Carbide Phases are obtained using low-temperature electrolytic extraction the invention solves existing, since common water cooling mode temperature is not easy to control, the technical issues of influencing effect of extracting.System includes rectifier power source, magnetic stirring apparatus, stirring magneton, thermal insulation layer, stainless steel beaker, glass beaker, anode sample, spring clip, filtering iron net, crocodile clip, flange disk with holes and temperature sensor, wherein rectifier power source anode is connect by conducting wire with anode sample, rectifier power source cathode is connect by conducting wire with crocodile clip, and crocodile clip is clipped in the upper edge of glass beaker.The configuration of the present invention is simple, good heat dissipation effect can be good at the real time temperature for controlling electrolyte, guarantee that stable experiment carries out.The present invention is for Carbide Phases low-temperature electrolytic extraction in bearing steel.
Description
Technical field
The present invention relates to Carbide Phases low-temperature electrolytics to extract field.
Background technique
Bearing steel will form martensitic phase, retained austenite phase during heat treatment, while there are also Carbide Phases.It is remaining
Austenite is the tissue that martensite transfor mation does not occur in quenching process, and residual austenite content is Technology on Bearing Size Stability and fatigue
Service life important factor in order, when using X-ray diffraction method measurement residual austenite content, retained austenite phase and Carbide Phases
Diffraction overlap of peaks, testing result can not be corrected by analysis software, it is therefore necessary to will pass through electrochemical means Carbide Phases
Carry out quantitative collection correction result.Meanwhile the information such as ingredient, shape, structure, particle size of Carbide Phases determine the object of steel
Physicochemical property and mechanical performance, therefore the accurate quantitative analysis of Carbide Phases.To optimization heat treatment process, improving bearing life has
Great importance.
In order to obtain residual austenite content precise results, accurate evaluation bearing Steel Properties need to be by the carbonization in steel
The acquisition for mistake that object is mutually intact, the preparation method of Carbide Phases because material component and property difference there is no, mark by unified extraction at present
Quasi- cooling means, the Carbide Phases result extracted under different temperatures are also not quite similar, because opposite between electrolytic cell and sample
Position is not fixed, and caused test effect is also different.During electrolytic extraction, particle size of the electrolyte temperature to Carbide Phases
There is large effect with purity, it is therefore necessary to design a kind of cooling means with great heat radiation effect, want to meet experiment
It asks, obtains the preferable Carbide Phases of quality.
Carbide Phases are obtained using low-temperature electrolytic extraction at present, cryogenic conditions need to be maintained at 0 DEG C or so, cryogenic conditions it is cold
But ways and means there is no unified standard, and common water cooling mode temperature is not easy to control, and effect is bad.
Summary of the invention
Carbide Phases are obtained using low-temperature electrolytic extraction the invention solves existing, due to common water cooling mode temperature
It is not easy to control, the technical issues of influencing effect of extracting, and Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel is provided.
Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel, including rectifier power source, magnetic stirring apparatus, stirring magnetic
Son, thermal insulation layer, stainless steel beaker, glass beaker, anode sample, spring clip, filtering iron net, crocodile clip, flange disk with holes and
Temperature sensor, wherein rectifier power source anode is connect by conducting wire with anode sample, and rectifier power source cathode passes through conducting wire and crocodile
Folder connection, crocodile clip are clipped in the upper edge of glass beaker, and the open-mouth of glass beaker is arranged flange disk with holes, connect with crocodile clip
Conducting wire, anode sample and temperature sensor be each passed through and be fixed at three circular holes of flange disk with holes, anode sample
Protruded into glass beaker with temperature sensor, glass beaker is arranged in the inside of stainless steel beaker, the side wall of glass beaker with not
Spring clip, stainless steel beaker inside bottom setting filtering iron net is arranged in top between the side wall of rust steel beaker, while filtering iron
Net cover setting stirring magneton, stainless steel beaker outer wall in the lower part of glass beaker, the filtering iron net of stainless steel beaker bottom are set
Thermal insulation layer is set, bottom is sitting on magnetic stirring apparatus.
Principle
The present apparatus increases electromagnetic stirring function and metal mesh structure in outer layer beaker bottom, and metal grill is having a size of straight
Diameter 5mm is to enter stirring region in order to avoid ice cube to hinder magneton Effect of Rotation mixing effect, stirs to promote bottom of a cup and top
Water form stream field, to eliminate the temperature gradient of the water of vertical direction, make ice water in entire cup, ammonium nitrate mixture
Temperature is uniformly maintained at 0 DEG C or so.
When solid ammonium nitrate dissolves, since solute particle spreads absorbed heat into solvent greater than solute particle solvent
Change released heat, therefore show as solution temperature reduction, the solubility of ammonium nitrate is 119g/100mL at 0 DEG C, cooling to burn
The water of cup is about 300mL, therefore the quality for the ammonium nitrate being added is 357g, makes solution close to saturation, reaches dual refrigeration
Purpose.In order to keep the position of each device instrument in test relatively fixed, and corresponding positioning device is devised, to make entire
Extraction process carries out under an opposite smaller stable environment of interference.Insulating layer with a thickness of 8mm, in thermal insulation property and heat preservation
It is guaranteed in effect.
The beneficial effects of the invention are as follows：The configuration of the present invention is simple, good heat dissipation effect can be good at the reality for controlling electrolyte
Shi Wendu guarantees that stable experiment carries out.Present system utilizes the cooling characteristics of ice water and ammonium nitrate mixture simultaneously, will be electrolysed
The structure of slot carries out rationally connection configuration, and carries out magnetic agitation, to reach efficient cooling effect.
1. this system, using stainless beaker itself as cathode, sample is close in suitable electrolyte, electric current as anode
Under the conditions of degree, experimental temperature, the electrolysis precipitation extraction process of progress, main purpose is to obtain complete Carbide Phases.
2. design flange plug be in order to fix sample and thermometer and stainless steel beaker and keep relative static conditions, that is,
Saying orchid plug is fixed at stainless steel beaker mouth, and sample and thermometer are fixed at flange plug circular hole.Ring flange fastening with holes
At stainless steel beaker mouth, cathode sample and thermometer are fixed at ring flange circular hole, and sample, temperature sensor is made to become one
Whole, no matter the movement in which direction occurs for stainless steel beaker, and sample and thermometer also move therewith, guarantee that sample and temperature pass
It is constantly in opposing stationary between sensor and stainless steel beaker, electrolyte is full of in stainless steel beaker, guarantees that sample and temperature pass
It is constant always that sensor immerses solution position.
3. design filtering wire netting is that ice cube enters stirring area in order to prevent, while playing the work of fixed stainless steel beaker
With.Wire netting is filtered, there are two effects：First is that fixed stainless steel beaker bottom, prevents beaker radial direction vibration；Second is that preventing ice cube
Enter beaker bottom due to gravity, hinder magneton rotation, be fully rotatable stirring second son, increases flabellum at magneton both ends, be
In order to generate more vortex, guarantee good heat dissipation effect.
4. spring clip mainly positions stainless steel beaker, it is in the center location of the cooling beaker of outer layer, Bu Huishou always
The influence rolled to ice melting buoyancy bring, prevents vibration.
5. band flabellum magneton mainly increases vortex, electrolyte temperature is controlled.
6. thermal insulation layer reduces Ice-water coolant heat absorption rate, guarantee that electrolyte temperature is sufficiently low, slows down the dissolution speed of ice cube
Degree, slows down solution temperature rate of change.
7. using pH meter temperature sensor, electrolyte temperature is measured, smaller than glass-stem thermometer error, precision is high, Ke Yi
The real time temperature of PH meter display screen display electrolyte.
8. mixture of ice and water temperature is 0 DEG C, and ammonium nitrate is dissolved in water using ice water, ammonium nitrate mixture as cooling medium
It is the endothermic reaction, there is dual refrigeration effect.
The present invention is for Carbide Phases low-temperature electrolytic extraction in bearing steel.
Detailed description of the invention
Fig. 1 is Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel described in embodiment one；
Fig. 2 is the XRD spectra that one ZGCr15 bearing steel of embodiment extracts Carbide Phases；
Fig. 3 is the SEM photograph that one ZGCr15 bearing steel of embodiment extracts Carbide Phases.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it
Between any combination.
Specific embodiment one：Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel of present embodiment, including it is whole
Galvanic electricity source 1, magnetic stirring apparatus 2, stirring magneton 3, thermal insulation layer 4, stainless steel beaker 5, glass beaker 6, anode sample 7, spring clip
8, iron net 9, crocodile clip 10, flange disk 11 with holes and temperature sensor 12 are filtered, wherein 1 anode of rectifier power source by conducting wire with
Anode sample 7 connects, and 1 cathode of rectifier power source is connect by conducting wire with crocodile clip 10, and crocodile clip 10 is clipped in the upper of glass beaker 6
Flange disk 11 with holes is arranged in edge, the open-mouth of glass beaker 6, and the conducting wire connecting with crocodile clip 10, anode sample 7 and temperature pass
Sensor 12 is each passed through and is fixed at three circular holes of flange disk 11 with holes, and anode sample 7 and temperature sensor 12 protrude into
In glass beaker 6, the inside of stainless steel beaker 5, the side wall of glass beaker 6 and the side of stainless steel beaker 5 is arranged in glass beaker 6
Spring clip 8,5 inside bottom of stainless steel beaker setting filtering iron net 9 is arranged in top between wall, while filtering 9 sets of iron net in glass
The lower part of glass beaker 6, setting stirring magneton 3 in the filtering iron net 9 of 5 bottom of stainless steel beaker, the setting of 5 outer wall of stainless steel beaker every
Thermosphere 4, bottom are sitting on magnetic stirring apparatus 2.
The configuration of the present invention is simple, good heat dissipation effect can be good at the real time temperature for controlling electrolyte, guarantee stable experiment
It carries out.Present system utilizes the cooling characteristics of ice water and ammonium nitrate mixture simultaneously, and the structure of electrolytic cell is rationally connected
Configuration is connect, and carries out magnetic agitation, to reach efficient cooling effect.
Specific embodiment two：The present embodiment is different from the first embodiment in that：Temperature sensor 12 is pH meter
Temperature sensor connects pH meter in the output end of sensor.It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that：Magnetic stirring apparatus 2 is sitting in
On the pedestal of experimental bench 13, fixing clamp is arranged in 13 side of experimental bench, and fixing clamp is clipped on the thermal insulation layer 4 in 5 outside of stainless steel beaker.
It is other the same as one or two specific embodiments.
Specific embodiment four：Unlike one of present embodiment and specific embodiment one to three：It is burnt in stainless steel
Ice water and ammonium nitrate mixed liquor are packed between cup 5 and glass beaker 6, medium floe is in 9 outside of filtering iron net.Other and specific reality
It is identical to apply one of mode one to three.
Specific embodiment five：Unlike one of present embodiment and specific embodiment one to four：Ice water and nitric acid
The volume of water is 300mL in ammonium mixed liquor, and the quality of ammonium nitrate is 357g.Other phases one of with specific embodiment one to four
Together.
Specific embodiment six：Unlike one of present embodiment and specific embodiment one to five：4 thickness of thermal insulation layer
For 8mm.It is other identical as one of specific embodiment one to five.
Specific embodiment seven：Unlike one of present embodiment and specific embodiment one to six：In glass beaker 6
The liquid of loading is electrolyte.It is other identical as one of specific embodiment one to six.
Specific embodiment eight：Unlike one of present embodiment and specific embodiment one to seven：Rectifier power source 1
Current density is 48~50mA/cm2.It is other identical as one of specific embodiment one to seven.
Specific embodiment nine：Unlike one of present embodiment and specific embodiment one to eight：Filter iron net 9
The diameter of grid is 5mm.It is other identical as one of specific embodiment one to eight.
Specific embodiment ten：Unlike one of present embodiment and specific embodiment one to nine：Experimental bench 13
The hole of upper table surface setting and flange disk 11 with holes cooperation.It is other identical as one of specific embodiment one to nine.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment one：
Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel of the present embodiment, including rectifier power source 1, magnetic stirring apparatus
2, magneton 3, thermal insulation layer 4, stainless steel beaker 5, glass beaker 6, anode sample 7, spring clip 8, filtering iron net 9, crocodile clip are stirred
10, flange disk 11 and temperature sensor 12 with holes, wherein 1 anode of rectifier power source is connect by conducting wire with anode sample 7, is rectified
1 cathode of power supply is connect by conducting wire with crocodile clip 10, and crocodile clip 10 is clipped in the upper edge of glass beaker 6, the open-mouth of glass beaker 6
Flange disk 11 with holes is set, and the conducting wire connecting with crocodile clip 10, anode sample 7 and temperature sensor 12 are each passed through and fix
At three circular holes of flange disk 11 with holes, anode sample 7 and temperature sensor 12 are protruded into glass beaker 6, glass beaker 6
The inside of stainless steel beaker 5 is set, and spring is arranged in the top between the side wall of glass beaker 6 and the side wall of stainless steel beaker 5
Folder 8,5 inside bottom of stainless steel beaker setting filtering iron net 9, while filtering 9 sets of the iron net lower parts in glass beaker 6, stainless steel
Thermal insulation layer 4 is arranged in setting stirring magneton 3,5 outer wall of stainless steel beaker in the filtering iron net 9 of 5 bottom of beaker, and bottom is sitting in magnetic force and stirs
It mixes on device 2.
Wherein, temperature sensor 12 is pH meter temperature sensor, connects pH meter in the output end of sensor；Magnetic stirring apparatus
2 are sitting on the pedestal of experimental bench 13, and fixing clamp is arranged in 13 side of experimental bench, and fixing clamp is clipped in the heat-insulated of 5 outside of stainless steel beaker
On layer 4；Ice water and ammonium nitrate mixed liquor are packed between stainless steel beaker 5 and glass beaker 6, medium floe is in filtering iron net 9
Outside；The volume of water is 300mL in ice water and ammonium nitrate mixed liquor, and the quality of ammonium nitrate is 357g；Thermal insulation layer 4 is with a thickness of 8mm；
The liquid being packed into glass beaker 6 is electrolyte；The current density of rectifier power source 1 is 49mA/cm2；Filter the grid of iron net 9
Diameter is 5mm；The hole of the upper table surface setting and flange disk 11 with holes cooperation of experimental bench 13.
Carbide Phases low-temperature electrolytic extracting process in ZGCr15 bearing steel is carried out using the present embodiment：
One, GCr15 bearing steel is processed into cylindrical coupon；
Two, the coupon both ends by step 1 preparation carry out insulation processing, expose effectively electrolysis area, obtain anode sample；
Three, hydrochloric acid, the methanol solution of citric acid and glycerin solution are mixed, then dilutes, obtains electrolyte；
Four, the anode sample that step 2 obtains is fitted into bearing steel in Carbide Phases low-temperature electrolytic extracting system, and will
The electrolyte that step 3 obtains pours into bearing steel in the glass beaker of Carbide Phases low-temperature electrolytic extracting system, regulates and controls bearing steel
The current density of middle Carbide Phases low-temperature electrolytic extracting system, and using the temperature of the mixture of ice water and ammonium nitrate control electrolyte
Degree is maintained at 0 DEG C, while carrying out real-time monitoring using temperature sensor；Complete Carbide Phases low-temperature extraction in ZGCr15 bearing steel
Method.
Current density is 0.049A/cm in step 42。
The length of step 4 Anodic sample leaching in the electrolytic solution is 47mm；Effectively electrolysis area is 18.3cm for it2。
Using suction filtration machine, to treated, electrolyte is filtered, and the quality that blank filter membrane is weighed before suction filtration is M1, is filtered
(filter membrane+filtrate quality) is weighed after drying as M2, carbide quality M=M2-M1, carbide accounts for the quality of sample electrolysis total amount
Score w%=M/ (mQuality before being electrolysed-mQuality after electrolysis) × 100%
Three GCr15 bearing steels are taken, numbers, is operated respectively according to embodiment, the data result obtained is arranged and is divided
Analysis such as following table：
By the XRD spectra of Carbide Phases in ZGCr15 bearing steel, as shown in Fig. 2, quench is tempered state as can be seen from Figure
Carbide structure is Fe3C。
By the SEM photograph of Carbide Phases in ZGCr15 bearing steel, as shown in figure 3, present invention carbonization as can be seen from Figure
The size of object reaches micron order.
The configuration of the present invention is simple, good heat dissipation effect can be good at the real time temperature for controlling electrolyte, guarantee stable experiment
It carries out.Present system utilizes the cooling characteristics of ice water and ammonium nitrate mixture simultaneously, and the structure of electrolytic cell is rationally connected
Configuration is connect, and carries out magnetic agitation, to reach efficient cooling effect.
Claims (10)
1. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel, it is characterised in that：The system include rectifier power source (1),
Magnetic stirring apparatus (2), stirring magneton (3), thermal insulation layer (4), stainless steel beaker (5), glass beaker (6), anode sample (7), bullet
Spring presss from both sides (8), filtering iron net (9), crocodile clip (10), flange disk with holes (11) and temperature sensor (12), wherein rectifier power source
(1) anode is connect by conducting wire with anode sample (7), and rectifier power source (1) cathode is connect by conducting wire with crocodile clip (10), crocodile
Folder (10) is clipped in the upper edge of glass beaker (6), and flange disk (11) with holes is arranged in the open-mouth of glass beaker (6), with crocodile clip
(10) conducting wire, anode sample (7) and the temperature sensor (12) connected is each passed through and is fixed on flange disk (11) with holes
At three circular holes, anode sample (7) and temperature sensor (12) are protruded into glass beaker (6), and glass beaker (6) is arranged stainless
Spring clip is arranged in the inside of steel beaker (5), the top between the side wall of glass beaker (6) and the side wall of stainless steel beaker (5)
(8), stainless steel beaker (5) inside bottom setting filtering iron net (9), while filtering iron net (9) and covering under glass beaker (6)
Portion, interior setting stirring magneton (3) of the filtering iron net (9) of stainless steel beaker (5) bottom, the setting of stainless steel beaker (5) outer wall are heat-insulated
Layer (4), bottom is sitting on magnetic stirring apparatus (2).
2. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Temperature
Sensor (12) is pH meter temperature sensor, connects pH meter (14) in the output end of sensor.
3. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Magnetic force
Blender (2) is sitting on the pedestal of experimental bench (13), and fixing clamp is arranged in experimental bench (13) side, and fixing clamp is clipped in stainless steel beaker
(5) on the thermal insulation layer (4) on the outside of.
4. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Not
It becomes rusty steel beaker (5) and is packed into ice water and ammonium nitrate mixed liquor between glass beaker (6), medium floe is on the outside of filtering iron net (9).
5. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 4, it is characterised in that：Ice water
Volume with water in ammonium nitrate mixed liquor is 300mL, and the quality of ammonium nitrate is 357g.
6. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：It is heat-insulated
Layer (4) is with a thickness of 8mm.
7. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Glass
The liquid being packed into beaker (6) is electrolyte.
8. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Rectification
The current density of power supply (1) is 48~50mA/cm2。
9. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：Filtering
The Mesh Diameter of iron net (9) is 5mm.
10. Carbide Phases low-temperature electrolytic extracting system in a kind of bearing steel according to claim 1, it is characterised in that：It is real
Test the hole of the upper table surface setting and flange disk (11) with holes cooperation of platform (13).
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115090001A (en) * | 2022-07-04 | 2022-09-23 | 昆明理工大学 | Extraction device suitable for stirring and extracting granular materials and use method thereof |
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Application publication date: 20181130 |