CN108918220A - Carbide Phases low-temperature extraction method in ZGCr15 bearing steel - Google Patents
Carbide Phases low-temperature extraction method in ZGCr15 bearing steel Download PDFInfo
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Abstract
Carbide Phases low-temperature extraction method in ZGCr15 bearing steel, the present invention relates to Carbide Phases low-temperature extraction fields.The invention solves existing methods to extract ZGCr15 bearing steel carbide difficulty, and the technical problem that accuracy is low.Method:One, ZGCr15 bearing steel is processed into cylindrical coupon;Two, row insulation processing exposes effectively electrolysis area, obtains anode sample;Three, electrolyte is prepared;Four, anode sample is fitted into bearing steel in Carbide Phases low-temperature electrolytic extracting system, carries out low-temperature extraction.The method of the present invention can accurately extract carbide in the bearing steel quenched and be tempered state, and carry out quantitative analysis, using carbide in ZGCr15 bearing steel material as research object, it is separated by electrochemical means, the test of microphysics chemical property and characterization verifying to object phase, reach depth integration between profession to intersect, realize to the ingredient of material, tissue, structure, physical property Study on Integration.The present invention is for Carbide Phases in low-temperature extraction ZGCr15 bearing steel.
Description
Technical field
The present invention relates to Carbide Phases low-temperature extraction fields.
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- method, the Carbide Phases result extracted under different temperatures are also not quite similar, and need to find a good extracting process, come
It is good to obtain quality, the uniform Carbide Phases of form.
Common 8Cr4Mo4V (Cr4Mo4V), several bearings of 9Cr18, W9Cr4V2Mo, ZGCr15 and G13Cr4Mo4Ni4V
In steel, wherein ZGCr15 phosphorus content reaches as high as 1%, contains a large amount of carbide in tissue after heat treatment.Carbide conduct
The important component of bearing structure of steel, shape, size, quantity and distribution have a great impact to the performance of material.It is adopting
When measuring residual austenite content with national standard X-ray diffraction method, it is known that carbide content is accurate quantitative analysis residual austenite
Basis.Therefore, the influence and its quantitative approach research that carbide measures residual austenite content in control bearing steel to being carbonized
There are important directive significance in object content, Accurate Determining residual austenite content, raising bearing steel fatigue life.Meanwhile determining steel
Heat treatment, which is quenched, to be tempered in state GCr15 bearing, carbide particle pattern and structure, is conducive to optimize and treatment process.Currently,
The extraction of ZGCr15 bearing steel carbide there is no clearly unified extracting process, therefore it is accurate by carbide to explore a kind of extracting process
Carbide in quantitative ZGCr15 bearing steel, to solve practical problem in production.
Summary of the invention
The invention solves existing methods to extract ZGCr15 bearing steel carbide difficulty, and the technical problem that accuracy is low,
And provide Carbide Phases low-temperature extraction method in ZGCr15 bearing steel.
Carbide Phases low-temperature extraction method in ZGCr15 bearing steel, specifically carries out according to the following steps:
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.
Wherein according to GB/T18254 in step 1《High-carbon-chromium bearing steel》The evaluation of raw material chemical component test stone
Whether GCr15 bearing steel chemical composition is qualified.
The beneficial effects of the invention are as follows:Carbon in the bearing steel quenched and be tempered state can be accurately extracted using the method for the present invention
Compound, and quantitative analysis is carried out, using carbide in ZGCr15 bearing steel material as research object, separated by electrochemical means,
The test of microphysics chemical property and characterization verifying to object phase, reach depth integration between profession and intersect, realize to material
Ingredient, tissue, structure, physical property Study on Integration, micro-property and macro property, heat treatment process are connected, these letters
Breath is predicted the ingredient design of high temperature alloy, process system, macro property and assessment combines, from macroscopic arts to microcosmic neck
Domain extends.The size of carbide of the present invention reaches micron order.
The present invention is for Carbide Phases in low-temperature extraction ZGCr15 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 extraction method in present embodiment ZGCr15 bearing steel, it is specific by with
Lower step carries out:
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.
According to GB/T18254 in present embodiment step 1《High-carbon-chromium bearing steel》Raw material chemical component test stone is commented
Whether qualified determine GCr15 bearing steel chemical composition.
Carbide in the bearing steel quenched and be tempered state can be accurately extracted using the method for the present invention, and is quantitatively divided
Analysis, using carbide in ZGCr15 bearing steel material as research object, is separated by electrochemical means, to the microphysics of object phase
Performance test and characterization verifying are learned, reaches depth integration between profession and intersects, realize to the ingredient of material, tissue, structure, physical property
Study on Integration connects micro-property and macro property, heat treatment process, these information are to high temperature alloy at setting up separately
Meter, process system, macro property prediction and assessment combine, and extend from macroscopic arts to microscopic fields.
Specific embodiment two:The present embodiment is different from the first embodiment in that:Coupon diameter phi in step 1
12.4mm, long 80mm.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:Insulation position in step 2
Coupon both ends are specifically sealed processing using insulating tape by reason.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 will in step 3
25mL density is 1.19g/mL hydrochloric acid, the methanol solution of citric acid and the mixing of 50mL glycerin solution, is then diluted to 500mL,
Electrolyte is obtained, wherein citric acid is 10g.It is other identical as one of specific embodiment one to three.
Specific embodiment five:Unlike one of present embodiment and specific embodiment one to four:Step 4 axis
Holding Carbide Phases low-temperature electrolytic extracting system in steel includes rectifier power source 1, magnetic stirring apparatus 2, stirring magneton 3, thermal insulation layer 4, no
Rust steel beaker 5, glass beaker 6, anode sample 7, spring clip 8, filtering iron net 9, crocodile clip 10, flange disk 11 with holes and temperature
Sensor 12, wherein 1 anode of rectifier power source is connect by conducting wire with anode sample 7, and 1 cathode of rectifier power source passes through conducting wire and crocodile
10 connection of folder, crocodile clip 10 are 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
Conducting wire, anode sample 7 and the temperature sensor 12 of 10 connection of fish folder are each passed through and are fixed on three of flange disk 11 with holes
At circular hole, anode sample 7 and temperature sensor 12 are protruded into glass beaker 6, and glass beaker 6 is arranged in stainless steel beaker 5
Spring clip 8,5 inside bottom of stainless steel beaker is arranged in portion, the top between the side wall of glass beaker 6 and the side wall of stainless steel beaker 5
Portion's setting filtering iron net 9, while 9 sets of the iron net lower parts in glass beaker 6 are filtered, in the filtering iron net 9 of 5 bottom of stainless steel beaker
Thermal insulation layer 4 is arranged in setting stirring magneton 3,5 outer wall of stainless steel beaker, and bottom is sitting on magnetic stirring apparatus 2.Other and specific implementation
One of mode one to four is identical.
Specific embodiment six:Unlike one of present embodiment and specific embodiment one to five:It is electric in step 4
Current density is 0.048~0.050A/cm2.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:Step 4 middle-jiao yang, function of the spleen and stomach
The length of pole sample leaching in the electrolytic solution is 47mm.It is other identical as one of specific embodiment one to six.
Effectively electrolysis area is 18.3cm for it2。
Specific embodiment eight:Unlike one of present embodiment and specific embodiment one to seven:Ice in step 4
The mixture of water and ammonium nitrate is packed between stainless steel beaker 5 and glass beaker 6.One of other and specific embodiment one to seven
It is identical.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
Carbide Phases low-temperature extraction method in the present embodiment ZGCr15 bearing steel, specifically carries out according to the following steps:
One, GCr15 bearing steel is processed into cylindrical coupon;Coupon diameter phi 12.4mm, long 80mm;
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.
It wherein, is that 1.19g/mL hydrochloric acid, the methanol solution of citric acid and 50mL glycerine are molten by 25mL density in step 3
Liquid mixing, is then diluted to 500mL, and wherein citric acid is 10g;
Carbide Phases low-temperature electrolytic extracting system includes rectifier power source 1, magnetic stirring apparatus 2, stirs in step 4 middle (center) bearing steel
Mix 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 10, band
Hole flange disk 11 and temperature sensor 12, wherein 1 anode of rectifier power source is connect by conducting wire with anode sample 7, rectifier power source 1
Cathode 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 setting of glass beaker 6
Flange disk 11 with holes, the conducting wire connecting with crocodile clip 10, anode sample 7 and temperature sensor 12 are each passed through and are fixed on band
At three circular holes of hole flange disk 11, anode sample 7 and temperature sensor 12 are protruded into glass beaker 6, and glass beaker 6 is arranged
In the inside of stainless steel beaker 5, spring clip 8 is arranged in the top between the side wall of glass beaker 6 and the side wall of stainless steel beaker 5,
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 beaker 5
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 bottom, and bottom is sitting in magnetic stirring apparatus 2
On;
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.
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。
Carbide Phases low-temperature electrolytic extracting system is as shown in Figure 1 in bearing steel described in the present embodiment.
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.
Carbide in the bearing steel quenched and be tempered state can be accurately extracted using this method, and carries out quantitative analysis, with
Carbide is research object in ZGCr15 bearing steel material, is separated by electrochemical means, chemically to the microphysics of object phase
Verifying can be tested and be characterized, reaches depth integration between profession and intersects, is realized to the ingredient of material, tissue, structure, physical property one
Change research, micro-property and macro property, heat treatment process are connected, these information design the ingredient of high temperature alloy,
Process system, macro property prediction and assessment combine, and extend from macroscopic arts to microscopic fields.
Claims (8)
- Carbide Phases low-temperature extraction method in 1.ZGCr15 bearing steel, it is characterised in that this method specifically carries out according to the following steps: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 by step Three obtained electrolyte pour into bearing steel in the glass beaker of Carbide Phases low-temperature electrolytic extracting system, regulate and control carbon in bearing steel The current density of compound phase low-temperature electrolytic extracting system, and protected using the temperature of the mixture of ice water and ammonium nitrate control electrolyte It holds at 0 DEG C, while carrying out real-time monitoring using temperature sensor;Complete Carbide Phases low-temperature extraction side in ZGCr15 bearing steel Method.
- 2. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 1 Middle coupon diameter phi 12.4mm, long 80mm.
- 3. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 2 Middle insulation processing specifically uses insulating tape that coupon both ends are sealed processing.
- 4. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 3 Middle by 25mL density is that 1.19g/mL hydrochloric acid, the methanol solution of citric acid and 50mL glycerin solution mix, and is then diluted to 500mL obtains electrolyte, and wherein citric acid is 10g.
- 5. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 4 In middle (center) bearing steel Carbide Phases low-temperature electrolytic extracting 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), spring clip (8), filtering iron net (9), crocodile clip (10), flange disk (11) with holes and temperature sensor (12), wherein rectifier power source (1) anode passes through conducting wire and anode sample (7) it connects, rectifier power source (1) cathode 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, the conducting wire connecting with crocodile clip (10), anode sample (7) is arranged in the open-mouth on edge, glass beaker (6) It is each passed through and is fixed at three circular holes of flange disk (11) with holes with temperature sensor (12), anode sample (7) and temperature Degree sensor (12) protrudes into glass beaker (6), and glass beaker (6) is arranged in the inside of stainless steel beaker (5), glass beaker (6) spring clip (8) are arranged in the top between the side wall of side wall and stainless steel beaker (5), and stainless steel beaker (5) inside bottom is set Filtering iron net (9) is set, while filtering iron net (9) and covering in the lower part of glass beaker (6), the filtering iron of stainless steel beaker (5) bottom Thermal insulation layer (4) are arranged in setting stirring magneton (3) in net (9), stainless steel beaker (5) outer wall, and bottom is sitting in magnetic stirring apparatus (2) On.
- 6. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 4 Middle current density is 0.048~0.050A/cm2。
- 7. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 4 The length of Anodic sample leaching in the electrolytic solution is 47mm.
- 8. Carbide Phases low-temperature extraction method in ZGCr15 bearing steel according to claim 1, it is characterised in that step 4 The mixture of middle ice water and ammonium nitrate is packed between stainless steel beaker (5) and glass beaker (6).
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