CN106840802A - A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion - Google Patents
A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion Download PDFInfo
- Publication number
- CN106840802A CN106840802A CN201710140516.XA CN201710140516A CN106840802A CN 106840802 A CN106840802 A CN 106840802A CN 201710140516 A CN201710140516 A CN 201710140516A CN 106840802 A CN106840802 A CN 106840802A
- Authority
- CN
- China
- Prior art keywords
- steel
- electrolysed
- suction filtration
- steel sample
- electrolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
Abstract
The present invention provides a kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion, it is described that first manufactured steel sample to be electrolysed is pre-processed in heating furnace, so as to the form and size of the carbide in control steel before electrolysis, reduce its influence to field trash observation, precise control electric current and electrolysis time during electrolysis, improve electrolytic efficiency, it is electrolysed steel sample after terminating, steel sample and wire connecting section, negative electrode etc. is rinsed, all flushing liquors and electrolyte are all collected and pours into bottle,suction, and it is that 2 μm of filter membranes with 0.45 μm are classified suction filtration to field trash that aperture is respectively adopted, filter membrane is put into drying box after suction filtration is complete is dried, and the field trash extracted using ESEM and energy spectrum analysis.The method is simple and reliable, efficiency high, shortens steel sample electrolysis time, and field trash loss is few, can effectively extract each type impurity in high-carbon steel, and effectively observation and accurate judgement are finally carried out to each type impurity pattern in high-carbon steel.
Description
Technical field
The invention belongs to steel inclusion electrolytic separation and three-dimensional appearance observation field, and in particular to a kind of electrolytic separation is high
The original appearance analysis method of carbon steel inclusion.
Background technology
With the development of each high-grade, precision and advanced industry of China, such as Aero-Space, high-speed railway etc., required high-carbon steel (such as bearing
Steel, pinion steel, spring steel etc.) quality requirement also more and more higher.By taking high ferro as an example, high ferro more than current 300km/h speed per hours
Bearing used also places one's entire reliance upon import, though domestic bearing output of steel is big, quality can not meet high request, and it is further right also to need
Domestic technique for manufacturing bearing steel is optimized.
A key factor for influenceing steel product quality is steel inclusion.Therefore, using suitable process meanses, maximum journey
Each type impurity in the removal steel of degree, realizes that molten steel is purifying most important to metallurgy industry production high-quality steel.By to electricity
Solution means carry out original appearance analysis to steel inclusion, grasp three-dimensional appearance, property and the formation condition of steel inclusion, are gone
Except the corresponding measure of steel inclusion, the important means as the efficient basic removal for realizing steel inclusion.
At present, the method for original appearance observation being carried out to steel inclusion using electrolysis mainly has two kinds, and one kind uses organic
Electrolyte is electrolysed, and one kind is electrolysed using inorganic electrolyte liquid.It is electrolysed using inorganic electrolyte liquid and is easily destroyed some types field trash
Primary morphology, is unfavorable for the accurate extraction of steel inclusion；But use organic electrolyte to be electrolysed in reservation steel that can be complete
The primary morphology of whole field trashes, but when carrying out the analysis of field trash original appearance using electrolysis for high-carbon steel, due to carbon in steel
Content is high, and inevitable generation carbide in electrolytic process, carbide can enter electricity with the carrying out of electrolysis together with field trash
In solution liquid, without being dissolved in electrolysis.And the usual particle of carbide is larger, when processing electrolysate using the means of suction filtration
It is difficult to be leached out, is mixed with the less field trash of size, the strong influence observation and extraction of field trash.
There are extraction and the analysis side of a kind of high-carbon steel field trash of Application No. CN201510239355.0 in the prior art
Method, the method still uses original organic solution electrolysis, it is impossible to be inherently eliminated carbide in high-carbon steel electrolytic process
Bring influence, the separative efficiency of extreme influence electrolysis high-carbon steel inclusion and effectively extraction.And process provides one kind
Brand-new method, overcomes the influence that a large amount of carbide are observed field trash in high-carbon steel after being electrolysed, and greatly reduces to height
The difficulty and workload of carbon steel inclusion original appearance analysis, by pretreatment before electrolysis to steel sample, in strict control steel
The size of carbide, makes most of carbide be separated with field trash during suction filtration, while strictly control electrical current, electrolysis
Time and steel sample ruler cun, realize more accurate quantitative electrolysis, and press chi to field trash using the filter paper of different pore size when suction filtration
Little progress row is classified suction filtration, finally realizes effective electrolytic separation of each type impurity in high-carbon steel, reaches the purpose for being easy to observation.And
And the method is simple and reliable, efficiency high shortens steel sample electrolysis time, and field trash loss is few, can effectively extract high-carbon steel
In each type impurity, effectively observation and accurate judgement are finally carried out to each type impurity pattern in high-carbon steel, be steel inclusion
The improvement and optimization for removing technique provide guidance.
The content of the invention
In order to solve the above problems, a kind of separation high-carbon steel field trash of present invention offer is simple and reliable, loss is few, carbon
Compound is on the observation of field trash and separates the small field trash original appearance analytic approach of influence, methods described be first electrolysed before in heating furnace
Steel sample to be electrolysed to processing is pre-processed, and the size of carbide, makes most of carbide in suction filtration process in control steel
In separated with field trash, while control electrical current, electrolysis time and steel sample ruler cun, to carry out accurate quantitative electrolysis, and in
Using the filter paper of different pore size during suction filtration, classification suction filtration is carried out by size to field trash, finally realize all kinds of in high-carbon steel being mingled with
The electrolytic separation of thing, completes original appearance analysis；
Further, methods described includes：
S1：After steel sample is machined into desired size, the steel sample to be electrolysed that then will be processed be placed in heating furnace carry out it is pre-
Treatment, pretreating process is the annealing process after improvement；
S2：Connection electrolysis unit, power supply is dc source used in it, and after wiring connection, electrolytic process uses constant pressure
Control model；
S3：Be rinsed for steel sample, steel sample and wire connecting section, negative electrode etc. after terminating by electrolysis, all flushing liquors and electrolysis
Liquid is all collected, and pouring into bottle,suction carries out suction filtration, and first by the polycarbonate leaching film in 2 μm of aperture, suction filtration repeats suction filtration
2-4 times, reuse the filtrate that the polycarbonate leaching film in 0.45 μm of aperture will obtain after first time suction filtration and repeat suction filtration 2-4 again
Time；
S4：Different pore size filter membrane used by suction filtration twice is placed in drying box and is dried, then use filter membrane after drying
Conducting resinl is sticked on conducting base；
S5：Filter membrane to being fixed on conducting base carries out metal spraying or spray carbonaceous conductive treatment, uses ESEM and power spectrum
Analysis means carry out the observation of three-dimensional appearance to the field trash isolated on filter membrane；
Further, the annealing process described in S1 after improvement is：Steel sample in stove is placed on first is heated to 780
DEG C -820 DEG C, 3h-5h is incubated, then with stove with 30 DEG C/h slow cooling to 680 DEG C -720 DEG C, is incubated 2h-4h, then with 30 DEG C/h slow cooling
To 650 DEG C, taking-up is air cooled to room temperature, and steel sample section to be electrolysed is polished；
Further, the S1 is specifically included：
S11：First by steel sample be machined to the pole or (5-20) mm of φ (5-10) mm × (30-50) mm × (5-20) mm ×
The square of (5-20) mm is used as steel sample to be electrolysed；
S12：The steel sample to be electrolysed that will be processed is placed in heating furnace and is pre-processed, and handling process is the nodularization after improvement
Annealing process；
S13：The section to be electrolysed of the steel sample to be electrolysed after to treatment is polished, using the method for metallographic sample preparation, difference
Steel sample section to be electrolysed is carried out by grinding homogeneity using 200#, 400# and 600# sand paper；
Further, the S2 is specifically included：
S21：Negative electrode is immersed into electrolyte, electrolyte is AA solution, it is described for AA solution be absolute methanol/ethanol-(5~
15) % acetylacetone,2,4-pentanediones-(0.5~1.5) % tetramethyl ammonium chlorides, the negative electrode material is steel plate, and cathode shape is enclosed for closure, cloudy
Pole connects DC power cathode by plain conductor；
S22：Steel sample surrounding to be electrolysed is sealed using insulating tape, and DC power anode is connected by plain conductor,
Only remain electrolysis section exposed, electrolyte is immersed during electrolysis；
S23：After wiring connection, electrolytic process uses Isobarically Control pattern, and voltage is chosen
Fixed value control in the range of 120mV-160mV, and keep current control in the range of 0.04A-0.07A, during electrolysis
Between 2~5h；
Further, the S3 includes：
S31：The steel sample being electrolysed after terminating, the linkage section of steel sample and wire, negative electrode are rinsed, rinsing agents useful for same is
Absolute methanol/ethanol organic solution,
S32：All flushing liquors and electrolyte are all collected, pouring into bottle,suction carries out suction filtration, and suction filtration is first by aperture 2
μm polycarbonate leaching film, suction filtration repeats 2-4 times, reuses the polycarbonate leaching film in 0.45 μm of aperture by first time suction filtration
The filtrate for obtaining afterwards repeats suction filtration 2-4 times again；
Further, the S4 is specially to be placed in the different pore size filter membrane used by suction filtration twice in drying box and dries, and does
At 150 ± 2 DEG C, then filter membrane after drying is sticked at conducting base to dry case temperature control by drying time 1h-3h using conducting resinl
On, the conducting base material is metal material, and the metal material is bloom, copper coin or aluminium sheet；
Further, the high-carbon steel is steel grade of the carbon content in more than 0.5wt% in steel；
Further, the high-carbon steel includes high-carbon-chromium bearing steel, spring steel, pinion steel and hard wire steel；
Further, voltage chooses fixed value control in the range of (120-160) mV in electrolytic process described in S2, and keeps electricity
Flow control in the range of (0.04-0.07) A, 2~5h of electrolysis time；
Beneficial effects of the present invention are as follows：
1) there is provided a kind of effective original appearance analysis method for extracting high-carbon steel inclusion；
2) for high-carbon steel, by Technology for Heating Processing from electrolysis Sources controlling high-carbon steel in carbide size, greatly
Carbide when alleviating electrolysis to the field trash influence that brings of observation, reduce field trash observation difficulty；
3) electrolytic efficiency is improve, electrolysis time is foreshortened into 2~5h, there is provided effective acquisition is pressed from both sides with separating in high-carbon steel
The original appearance analysis method of debris；
4) by electrolysis size, the condition such as electricity parameters (electric current and voltage) and conduction time is improved precise control steel sample
Electrolysis precision, and using the filter membrane classification suction filtration of different pore size, field trash loss in operating process is reduced, realize being pressed from both sides in high-carbon steel
The full-scale separation of debris and extraction.
Brief description of the drawings
Fig. 1 is electrolysis unit connection diagram of the present invention；
Fig. 2 is Suction filtration device schematic diagram of the present invention；
Fig. 3 is the microstructure figure that Al-O type impurities are observed after being electrolysed in embodiment of the present invention 1；
Fig. 4 is the energy spectrum analysis component-part diagram that Al-O type impurities are observed after being electrolysed in embodiment of the present invention 1；
Fig. 5 is the microstructure figure that spinels field trash is observed after being electrolysed in embodiment of the present invention 1；
Fig. 6 is the energy spectrum analysis component-part diagram that spinels field trash is observed after being electrolysed in embodiment of the present invention 1；
Fig. 7 is the microstructure figure that MnS type impurities are observed after being electrolysed in embodiment of the present invention 1；
Fig. 8 is the energy spectrum analysis component-part diagram that MnS type impurities are observed after being electrolysed in embodiment of the present invention 1；
Fig. 9 is the microstructure figure that Al-Si-O type impurities are observed after being electrolysed in embodiment of the present invention 1；
Figure 10 is the energy spectrum analysis component-part diagram that Al-Si-O type impurities are observed after being electrolysed in embodiment of the present invention 1；
Figure 11 is the microstructure that Ca-Mg-Al-Si-O type impurities are observed after being electrolysed in embodiment of the present invention 1
Figure；
Figure 12 is the energy spectrum analysis that Ca-Mg-Al-Si-O type impurities are observed after being electrolysed in embodiment of the present invention 1
Component-part diagram.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.Conversely, the present invention cover it is any be defined by the claims done in spirit and scope of the invention
Replacement, modification, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to this
It is detailed to describe some specific detail sections in the detailed description of invention.It is thin without these for a person skilled in the art
The description for saving part can also completely understand the present invention.
The invention will be further described with specific embodiment below in conjunction with the accompanying drawings, but not as a limitation of the invention.
Below most preferred embodiment is enumerated for of the invention：
As shown in Fig. 1-Fig. 7, the present invention provides a kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion, described
High-carbon steel be steel in carbon content more than 0.5%wt steel grade, the high-carbon steel include high-carbon-chromium bearing steel, spring steel, gear
Steel and hard wire steel, steel sample to be electrolysed to processing in heating furnace is pre-processed before methods described is first electrolysed, and controls steel
The size of middle carbide, makes most of carbide be separated with field trash during suction filtration, while when controlling electrical current, electrolysis
Between and steel sample ruler cun, to carry out accurate quantitative electrolysis, and size is pressed to field trash using the filter paper of different pore size when suction filtration
Classification suction filtration is carried out, the electrolytic separation of each type impurity in high-carbon-chromium bearing steel is finally realized, original appearance analysis is completed.
Methods described includes：
S1：After steel sample is machined into desired size, the steel sample to be electrolysed that then will be processed be placed in heating furnace carry out it is pre-
Treatment, pretreating process is the annealing process after improvement；
S2：Connection electrolysis unit, power supply is dc source used in it, and after wiring connection, electrolytic process uses constant pressure
Control model, voltage chooses fixed value control in the range of (120-160) mV, and keeps current control in (0.04-0.07) A scopes
It is interior, 2~5h of electrolysis time；
S3：Be rinsed for steel sample, steel sample and wire connecting section, negative electrode etc. after terminating by electrolysis, all flushing liquors and electrolysis
Liquid is all collected, and pouring into bottle,suction carries out suction filtration, and first by the polycarbonate leaching film in 2 μm of aperture, suction filtration repeats suction filtration
2-4 times, reuse the filtrate that the polycarbonate leaching film in 0.45 μm of aperture will obtain after first time suction filtration and repeat suction filtration 2-4 again
Time；
S4：Different pore size filter membrane used by suction filtration twice is placed in drying box and is dried, then use filter membrane after drying
Conducting resinl is sticked on conducting base；
S5：Filter membrane to being fixed on conducting base carries out metal spraying or spray carbonaceous conductive treatment, uses ESEM and power spectrum
Analysis means carry out the observation of three-dimensional appearance to the field trash isolated on filter membrane.
The S1 is specifically included：
S11：First by steel sample be machined to the pole or (5-20) mm of φ (5-10) mm × (30-50) mm × (5-20) mm ×
The square of (5-20) mm is used as steel sample to be electrolysed；
S12：The steel sample to be electrolysed that will be processed is placed in heating furnace and is pre-processed, and handling process is the nodularization after improvement
Annealing process；
S13：The section to be electrolysed of the steel sample to be electrolysed after to treatment is polished, using the method for metallographic sample preparation, difference
Steel sample section to be electrolysed is carried out by grinding homogeneity using 200#, 400# and 600# sand paper.Spheroidizing after being improved described in S1
Technique is：Be placed on steel sample in stove first and be heated to 780 DEG C -820 DEG C, be incubated 3h-5h, then with stove with 30 DEG C/h slow cooling extremely
680 DEG C -720 DEG C, 2h-4h is incubated, then with 30 DEG C/h slow cooling to 650 DEG C, taking-up is air cooled to room temperature, and to steel sample section to be electrolysed
Polished.
The S2 is specifically included：
S21：Negative electrode is immersed into electrolyte, electrolyte is AA solution, it is described for AA solution be absolute methanol/ethanol-(5~
15) % acetylacetone,2,4-pentanediones-(0.5~1.5) % tetramethyl ammonium chlorides, wherein, percentage is volume fraction, the negative electrode material in solution
Matter is steel plate, and cathode shape is enclosed for closure, and negative electrode connects DC power cathode by plain conductor；
S22：Steel sample surrounding to be electrolysed is sealed using insulating tape, and DC power anode is connected by plain conductor,
Only remain electrolysis section exposed, electrolyte is immersed during electrolysis；
S23：After wiring connection, electrolytic process uses Isobarically Control pattern, and voltage is chosen fixed in the range of 120mV-160mV
Value control, and keep current control in the range of 0.04A-0.07A, 2~5h of electrolysis time.
The S3 includes：
S31：The steel sample being electrolysed after terminating, the linkage section of steel sample and wire, negative electrode are rinsed, rinsing agents useful for same is
Absolute methanol/ethanol organic solution,
S32：All flushing liquors and electrolyte are all collected, pouring into bottle,suction carries out suction filtration, and suction filtration is first by aperture 2
μm polycarbonate leaching film, suction filtration repeats 2-4 times, reuses the polycarbonate leaching film in 0.45 μm of aperture by first time suction filtration
The filtrate for obtaining afterwards repeats suction filtration 2-4 times again, the S4 be specially the different pore size filter membrane used by suction filtration twice is placed in it is dry
Dried in dry case, at 150 ± 2 DEG C, then filter membrane after drying is used conducting resinl to drying box temperature control by drying time 1h-3h
Stick on conducting base, the conducting base material is metal material, the metal material is bloom, copper coin or aluminium sheet.
Embodiment 1
Steel sample is machined to the pole or (5-20) mm of φ (5-10) mm × (30-50) mm × (5-20) mm × (5- first
20) square of mm is used as steel sample to be electrolysed；(2) the steel sample to be electrolysed that will be processed is placed in heating furnace and is pre-processed, treatment
Technique is the annealing process after improvement, and the technique concrete operation step is as follows：Steel sample in stove is placed on first to be heated to
(780-820) DEG C insulation (3-5) h, then with stove with 30 DEG C/h slow cooling to (680-720) DEG C, is incubated (2-4) h, then with 30 DEG C/h
To 650 DEG C, taking-up is air cooled to room temperature for slow cooling；(3) section to be electrolysed of the steel sample to be electrolysed after and to treatment is polished, and is used
The method of metallographic sample preparation, 200#, 400# and 600# sand paper is respectively adopted carries out grinding homogeneity by steel sample section to be electrolysed.
Electrolytic separation micro inclusions are carried out using this method for certain high-carbon-chromium bearing steel, the high-carbon-chromium bearing steel is main
Composition such as subordinate list 1.Specific implementation process is as follows：
(1) bearing steel is machined to 10mm × 10mm × 15mm squares as steel sample to be electrolysed first；
(2) the steel sample to be electrolysed that will be processed is placed in heating furnace and is pre-processed, and handling process is the nodularization after improvement
Annealing process, the technique concrete operation step is as follows：Be placed on steel sample in stove be heated to 800 DEG C insulation 5h, then with stove with
30 DEG C/h slow cooling is incubated 2h to 720 DEG C, then with 30 DEG C/h slow cooling to 650 DEG C, taking-up is air cooled to room temperature；
(3) section to be electrolysed (10mm × 10mm section) of the bearing steel sample to be electrolysed after and to treatment is beaten
Mill, using the method for metallographic sample preparation, 200#, 400# and 600# sand paper is respectively adopted to carry out steel sample section to be electrolysed to polish
It is even；
(4) electrolysis unit is connected by the wiring of accompanying drawing 1, it is dc source to use power supply.Negative electrode is immersed into electrolyte, is electrolysed
Liquid is the tetramethyl ammonium chloride of the acetylacetone,2,4-pentanedione of methyl alcohol -10% -1%, and negative electrode material is steel plate, and cathode shape is enclosed for closure, and negative electrode leads to
Cross plain conductor connection DC power cathode；Steel sample surrounding to be electrolysed is sealed using insulating tape, and is connected by plain conductor
Connect DC power anode, only remain electrolysis section it is exposed, electrolyte is immersed during electrolysis；After wiring connection, used in electrolytic process
Isobarically Control pattern, voltage chooses fixed value control in the range of 130mV, and keeps current control in (0.04-0.07) A scopes
It is interior, electrolysis time 2-5h；
(5) steel sample, steel sample and wire connecting section, negative electrode etc. are rinsed after electrolysis terminates, flushing agents useful for same is nothing
Water methanol or ethanol organic solution, all flushing liquors and electrolyte are all collected, and pouring into bottle,suction carries out suction filtration, and suction filtration is first
Using 2 μm of the polycarbonate leaching film in aperture, suction filtration repeats 2 times, reuses the polycarbonate leaching film in 0.45 μm of aperture by
The filtrate obtained after suction filtration repeats suction filtration 2 times again；
(6) the different pore size filter membrane used by suction filtration twice is placed in drying box and is dried, drying box temperature control is (150
± 2) DEG C, and drying time 1.5h, then filter membrane after drying is sticked on bloom using conducting resinl；
(7) metal spraying conductive processing is carried out to the filter membrane being fixed on bloom, uses ESEM and energy spectrum analysis means pair
The field trash isolated on filter membrane carries out the observation of three-dimensional appearance, all kinds of bearing steel inclusions in the observed high carbon chromium
Three-dimensional appearance is as shown in figs. 3-7.
The electrolysis high-carbon-chromium bearing steel of table 1 main component/wt%
Embodiment described above, simply one kind of the present invention more preferably specific embodiment, those skilled in the art
The usual variations and alternatives that member is carried out in the range of technical solution of the present invention all should be comprising within the scope of the present invention.
Claims (10)
1. a kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion, it is characterised in that before methods described is first electrolysed
The steel sample to be electrolysed for processing is pre-processed in heating furnace, the size of carbide, makes most of carbide in control steel
Separated with field trash during suction filtration, while electrical current, electrolysis time and steel sample ruler cun are controlled, it is accurately quantitative to carry out
Electrolysis, and carries out classification suction filtration to field trash using the filter paper of different pore size when suction filtration by size, in finally realizing high-carbon steel
The electrolytic separation of each type impurity, completes original appearance analysis.
2. original appearance analysis method according to claim 1, it is characterised in that methods described includes：
S1：After steel sample is machined into desired size, the steel sample to be electrolysed that then will be processed is placed in heating furnace and is pre-processed,
Pretreating process is the annealing process after improvement；
S2：Connection electrolysis unit, power supply is dc source used in it, and after wiring connection, electrolytic process uses Isobarically Control
Pattern；
S3：Be rinsed for steel sample, steel sample and wire connecting section, negative electrode etc. after terminating by electrolysis, and all flushing liquors and electrolyte are complete
Portion collects, and pouring into bottle,suction carries out suction filtration, and first by the polycarbonate leaching film in 2 μm of aperture, suction filtration repeats 2-4 to suction filtration
Time, reuse filtrate repeatedly suction filtration 2-4 times again that the polycarbonate leaching film in 0.45 μm of aperture will be obtained after first time suction filtration；
S4：Different pore size filter membrane used by suction filtration twice is placed in drying box and is dried, filter membrane uses conductive after then drying
It is gluing on conducting base；
S5：Filter membrane to being fixed on conducting base carries out metal spraying or spray carbonaceous conductive treatment, uses ESEM and energy spectrum analysis
Means carry out the observation of three-dimensional appearance to the field trash isolated on filter membrane.
3. original appearance analysis method according to claim 2, it is characterised in that the annealing process after being improved described in S1
For：Be placed on steel sample in stove first and be heated to 780 DEG C -820 DEG C, be incubated 3h-5h, then with stove with 30 DEG C/h slow cooling to 680 DEG C -
720 DEG C, 2h-4h is incubated, then with 30 DEG C/h slow cooling to 650 DEG C, taking-up is air cooled to room temperature, and steel sample section to be electrolysed is beaten
Mill.
4. original appearance analysis method according to claim 2, it is characterised in that the S1 is specifically included：
S11：Steel sample is machined to the pole or (5-20) mm of φ (5-10) mm × (30-50) mm × (5-20) mm × (5- first
20) square of mm is used as steel sample to be electrolysed；
S12：The steel sample to be electrolysed that will be processed is placed in heating furnace and is pre-processed, and handling process is the spheroidizing after improvement
Technique；
S13：The section to be electrolysed of the steel sample to be electrolysed after to treatment is polished, and using the method for metallographic sample preparation, is respectively adopted
Steel sample section to be electrolysed is carried out grinding homogeneity by 200#, 400# and 600# sand paper.
5. original appearance analysis method according to claim 2, it is characterised in that the S2 is specifically included：
S21：Negative electrode is immersed into electrolyte, electrolyte is AA solution, it is described for AA solution is absolute methanol/ethanol-(5~15) %
Acetylacetone,2,4-pentanedione-(0.5~1.5) % tetramethyl ammonium chlorides, the negative electrode material is steel plate, and cathode shape is enclosed for closure, and negative electrode leads to
Cross plain conductor connection DC power cathode；
S22：Steel sample surrounding to be electrolysed is sealed using insulating tape, and DC power anode is connected by plain conductor, only stayed
Section to be electrolysed is exposed, and electrolyte is immersed during electrolysis；
S23：After wiring connection, electrolytic process uses Isobarically Control pattern, and voltage chooses fixed value control in the range of 120mV-160mV
System, and keep current control in the range of 0.04A-0.07A, 2~5h of electrolysis time.
6. original appearance analysis method according to claim 2, it is characterised in that the S3 includes：
S31：The steel sample being electrolysed after terminating, the linkage section of steel sample and wire, negative electrode are rinsed, it is anhydrous to rinse agents useful for same
Methanol/ethanol organic solution；
S32：All flushing liquors and electrolyte are all collected, pouring into bottle,suction carries out suction filtration, suction filtration is first by 2 μm of aperture
Polycarbonate leaching film, suction filtration repeats 2-4 times, and the polycarbonate leaching film for reusing 0.45 μm of aperture will be obtained after first time suction filtration
The filtrate arrived repeats suction filtration 2-4 times again.
7. original appearance analysis method according to claim 2, it is characterised in that the S4 is specially used by suction filtration twice
Different pore size filter membrane is placed in drying box and dries, and at 150 ± 2 DEG C, then drying time 1h-3h will dry drying box temperature control
Filter membrane is sticked on conducting base using conducting resinl after dry, and the conducting base material is metal material, and the metal material is bloom,
Copper coin or aluminium sheet.
8. original appearance analysis method according to claim 1, it is characterised in that the high-carbon steel is that carbon content exists in steel
The steel grade of more than 0.5%wt.
9. original appearance analysis method according to claim 1, it is characterised in that the high-carbon steel include high-carbon-chromium bearing steel,
Spring steel, pinion steel and hard wire steel.
10. original appearance analysis method according to claim 2, it is characterised in that voltage is chosen in electrolytic process described in S2
Fixed value control in the range of (120-160) mV, and keep current control in the range of (0.04-0.07) A, 2~5h of electrolysis time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710140516.XA CN106840802A (en) | 2017-03-09 | 2017-03-09 | A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710140516.XA CN106840802A (en) | 2017-03-09 | 2017-03-09 | A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106840802A true CN106840802A (en) | 2017-06-13 |
Family
ID=59144908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710140516.XA Pending CN106840802A (en) | 2017-03-09 | 2017-03-09 | A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106840802A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576556A (en) * | 2017-08-15 | 2018-01-12 | 河钢股份有限公司邯郸分公司 | The method of superfine carbide in electroextraction steel |
| CN108535304A (en) * | 2018-04-27 | 2018-09-14 | 暨南大学 | Macroscopical metallographic detection method of fatiguability break bolt |
| CN109269965A (en) * | 2018-11-08 | 2019-01-25 | 马鞍山沐及信息科技有限公司 | A kind of metallic inclusion integrates extraction element and extracting method |
| CN109459294A (en) * | 2018-11-28 | 2019-03-12 | 邯郸钢铁集团有限责任公司 | The preparation method of bearing steel bulk sample electrolysis sample |
| CN109632856A (en) * | 2018-12-05 | 2019-04-16 | 敬业钢铁有限公司 | A kind of steel inclusion detection method |
| CN110161066A (en) * | 2019-06-09 | 2019-08-23 | 苏州大学 | A kind of method that nonaqueous solution electrolysis extracts steel inclusion |
| CN111238916A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Classified extraction and quantitative analysis method for nonmetallic inclusions in high-temperature alloy |
| CN111238915A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| CN112763296A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching method for chromium-manganese stainless steel inclusions |
| CN113466271A (en) * | 2021-07-30 | 2021-10-01 | 钢铁研究总院 | Method for accurately determining type, morphology and elemental composition of intermetallic compounds in steel |
| CN114113181A (en) * | 2022-01-27 | 2022-03-01 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
| CN114199169A (en) * | 2021-12-20 | 2022-03-18 | 北京科技大学 | Original appearance analysis method for separating TiN inclusions in IF steel through electrolysis |
| CN114323873A (en) * | 2022-01-14 | 2022-04-12 | 慈兴集团有限公司 | Method for detecting particle components on surface of bearing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN103014284A (en) * | 2012-12-19 | 2013-04-03 | 洛阳宜华滚动体有限公司 | Process for modifying GCr15 steel for manufacturing tapered roller |
| CN104807684A (en) * | 2015-05-12 | 2015-07-29 | 首钢总公司 | Method for extracting and analyzing high-carbon steel inclusions |
-
2017
- 2017-03-09 CN CN201710140516.XA patent/CN106840802A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101074907A (en) * | 2007-03-29 | 2007-11-21 | 上海大学 | Method for extracting steel superfine varia by electrolysis method |
| CN103014284A (en) * | 2012-12-19 | 2013-04-03 | 洛阳宜华滚动体有限公司 | Process for modifying GCr15 steel for manufacturing tapered roller |
| CN104807684A (en) * | 2015-05-12 | 2015-07-29 | 首钢总公司 | Method for extracting and analyzing high-carbon steel inclusions |
Non-Patent Citations (2)
| Title |
|---|
| 王顺兴等: "GCr15钢中碳化物尺寸统计分布规律的研究", 《理化检验.物理分册》 * |
| 马文俊等: "轴承钢 GCr15 铸坯夹杂物的分析研究", 《钢铁钒钛》 * |
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107576556A (en) * | 2017-08-15 | 2018-01-12 | 河钢股份有限公司邯郸分公司 | The method of superfine carbide in electroextraction steel |
| CN108535304B (en) * | 2018-04-27 | 2020-06-30 | 暨南大学 | Macroscopic metallographic detection method for bolts easy to fatigue fracture |
| CN108535304A (en) * | 2018-04-27 | 2018-09-14 | 暨南大学 | Macroscopical metallographic detection method of fatiguability break bolt |
| CN109269965A (en) * | 2018-11-08 | 2019-01-25 | 马鞍山沐及信息科技有限公司 | A kind of metallic inclusion integrates extraction element and extracting method |
| CN109459294A (en) * | 2018-11-28 | 2019-03-12 | 邯郸钢铁集团有限责任公司 | The preparation method of bearing steel bulk sample electrolysis sample |
| CN109632856A (en) * | 2018-12-05 | 2019-04-16 | 敬业钢铁有限公司 | A kind of steel inclusion detection method |
| CN109632856B (en) * | 2018-12-05 | 2021-12-31 | 敬业钢铁有限公司 | Method for detecting inclusions in steel |
| CN110161066A (en) * | 2019-06-09 | 2019-08-23 | 苏州大学 | A kind of method that nonaqueous solution electrolysis extracts steel inclusion |
| CN110161066B (en) * | 2019-06-09 | 2022-03-15 | 苏州大学 | Method for extracting inclusions in steel through non-aqueous solution electrolysis |
| CN111238915A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| CN111238916A (en) * | 2020-02-12 | 2020-06-05 | 北京科技大学 | Classified extraction and quantitative analysis method for nonmetallic inclusions in high-temperature alloy |
| CN111238915B (en) * | 2020-02-12 | 2021-05-07 | 北京科技大学 | Method for extracting non-metallic inclusions in high-temperature alloy |
| CN112763296A (en) * | 2020-12-30 | 2021-05-07 | 上海大学 | Three-dimensional etching method for chromium-manganese stainless steel inclusions |
| CN112763296B (en) * | 2020-12-30 | 2022-11-18 | 上海大学 | Three-dimensional etching method for chromium-manganese stainless steel inclusions |
| CN113466271A (en) * | 2021-07-30 | 2021-10-01 | 钢铁研究总院 | Method for accurately determining type, morphology and elemental composition of intermetallic compounds in steel |
| CN114199169A (en) * | 2021-12-20 | 2022-03-18 | 北京科技大学 | Original appearance analysis method for separating TiN inclusions in IF steel through electrolysis |
| CN114323873A (en) * | 2022-01-14 | 2022-04-12 | 慈兴集团有限公司 | Method for detecting particle components on surface of bearing |
| CN114113181A (en) * | 2022-01-27 | 2022-03-01 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
| CN114113181B (en) * | 2022-01-27 | 2022-04-08 | 北京科技大学 | Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106840802A (en) | A kind of original appearance analysis method of electrolytic separation high-carbon steel inclusion | |
| CN105738188B (en) | The separation method of non-metallic inclusion in Inconel625 series of high temperature alloys | |
| CN107235485A (en) | The preparation method of graphene | |
| CN107604168A (en) | The method of recovering copper, nickel, cobalt from the sludge containing non-ferrous metal | |
| CN105648472A (en) | Recycling method and system for tin in tin stripping waste liquid and tin stripping waste liquid | |
| CN105018971B (en) | A kind of method by the dendritic α Fe sills of iron standby functional micro-nano structure | |
| CN104841691A (en) | Repair method of heavy metal nickel contaminated soil | |
| CN104674299B (en) | The recovery method of a small amount of fine copper of corrosion resistant plate attachment in copper electrolyzing refining | |
| CN102367527A (en) | Highly-ordered single-piece copper-based porous material and preparation method thereof | |
| CN115184393A (en) | Integrated device and method for extracting second-phase particles in steel through electrolysis | |
| CN102492848A (en) | Method for recovering NdFeB waste material by cold crucible induction smelting technology | |
| CN105399423A (en) | Method for preparing nanopore graphene filter film through arc discharge method | |
| CN212426234U (en) | Novel energy-concerving and environment-protective device that can improve electroplating homogeneity | |
| CN101230475A (en) | Aluminum alloy differential arc oxidation batch production technique | |
| CN102295330A (en) | Method for synchronous treatment of waste liquid and waste acid of heavy metal | |
| CN104550991B (en) | A kind of preparation method of titanium-aluminium alloy superfines | |
| CN103884550B (en) | A kind of method that oxide in steel is analyzed by electroextraction | |
| CN108871924A (en) | A method of extracting carbide from rich chromium cast iron | |
| CN110342525A (en) | A kind of method of low cost removal boron impurities in metallurgical silicon | |
| CN106854768A (en) | electrodeposition preparation method of superfine copper powder | |
| CN105567981A (en) | Method for extracting nickel from waste nickel-metal hydride batteries and preparing electrolytic nickel | |
| CN105648479B (en) | A kind of twin cathode rotates micro-electroforming apparatus vertically | |
| CN105063660B (en) | A kind of method that nano-silicon powder is directly prepared in electrorefining processes | |
| CN111223657B (en) | Recovery of Nd from bulk sintered Nd-Fe-B magnets and/or magnet scrap by electrochemical etching 2 Fe 14 Method of B-grain | |
| CN204509430U (en) | The retrieving arrangement of metallic copper in a kind of aluminium-containing sludge waste residue |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170613 |
|
| RJ01 | Rejection of invention patent application after publication |