CN114113181B - Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis - Google Patents
Original appearance analysis method for separating inclusions in non-aluminum weakly-deoxidized bearing steel through electrolysis Download PDFInfo
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Abstract
The invention provides an original appearance analysis method for electrolytically separating inclusions in non-aluminum weak deoxidation bearing steel, which realizes the accurate separation of the inclusions in the non-aluminum weak deoxidation bearing steel through the treatment of the electrolytic position of an electrolytic sample and the adjustment of the technological parameters of electrolysis, is not adhered to a matrix material, has high extraction rate and keeps the integrity of the three-dimensional appearance. According to the invention, the acrylate copolymer is added into the electrolyte in the electrolytic process, the sodium acrylate and acrylamide copolymer is added into the filtrate in the suction filtration, and the concentration and the air extraction amount of the filtrate are controlled through three-stage suction filtration, so that the unagglomerated silicate inclusions with good three-dimensional morphology are obtained through separation, and a basis is provided for the precise optimization of the production process.
Description
Technical Field
The invention belongs to the field of analysis and detection of inclusions in steel, and particularly relates to an original appearance analysis method for electrolytically separating inclusions in non-aluminum weakly-deoxidized bearing steel.
Background
With the development of various high-precision industries in China, such as aerospace, high-speed railways and the like, the quality requirement of the required bearing steel is higher and higher. Taking high-speed rail as an example, the bearings used by the high-speed rail with the speed of more than 300km/h at present completely depend on import, although the domestic bearing steel yield is high, the quality can not meet high requirements, and the domestic bearing steel production process needs to be further optimized.
One important factor affecting the quality of bearing steel is inclusions in the steel. Therefore, by adopting a proper process means, various inclusions in steel are removed to the greatest extent, and the realization of the clean purification of molten steel is very important for producing high-quality steel in the metallurgical industry. Because the whole process of traditional aluminum deoxidation smelting bearing steel adopts aluminum deoxidation, Al inevitably exists in molten steel2O3The inclusions are remained, the inclusions are hard in texture and do not deform during rolling,the method has great destructive effect on the continuity of a steel matrix, and magnesium aluminate spinel inclusions, even large-particle DS, can be generated by the reaction of aluminum with refining slag and refractory materials and can easily become crack sources to reduce the fatigue life of the bearing steel. Therefore, the prior method adopts a weak deoxidation mode to perform deoxidation, and uses Si deoxidation to replace the common Al deoxidation, so that the inclusion type in the steel is mainly silicate, and the content of calcium aluminate inclusions which have larger influence on the fatigue life is reduced; and the impurities are plasticized by refining and slagging and alkalinity control, so that D (coarse) and DS impurities are reduced; finally, the inclusions with the most content in the casting blank are silicates, spinels and calcium aluminates. The sizes of silicate and spinel inclusions in the weakly deoxidized bearing steel are mainly concentrated on less than 2 mu m, and a few inclusions are larger than 10 mu m. When the influence of impurities in non-aluminum weak deoxidized bearing steel is researched and the impurities in the steel are subjected to original appearance analysis by an electrolysis method, the small-particle silicate impurities are found to be obviously gathered and adhered to each other, so that the observation of the three-dimensional original appearance of the impurities is seriously influenced, and further, the production process cannot be accurately optimized.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide an original appearance analysis method for electrolytically separating inclusions in non-aluminum weakly-deoxidized bearing steel, which can clearly observe dispersed small-particle inclusions by controlling the components of electrolyte, electrolysis process parameters, the aperture of filter paper and the air extraction amount in the suction filtration process according to the physicochemical properties of the inclusions.
The specific technical scheme of the invention is as follows:
an original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis is characterized by comprising the following steps:
(1) processing a to-be-detected non-aluminum weak deoxidized bearing steel sample into a round rod-shaped electrolytic sample, polishing the surface of the round rod-shaped electrolytic sample to remove a surface oxide layer, and then cleaning the round rod-shaped electrolytic sample to remove oil stains;
(2) sealing the upper end of the round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with the positive electrode of a direct-current power supply through a metal lead, insulating and sealing the lower end of the round rod-shaped electrolytic sample, only leaving a middle cylindrical surface exposed, immersing the round rod-shaped electrolytic sample into electrolyte, and adding 100-plus 200mg/L acrylate copolymer into the electrolyte;
(3) connecting an electrolysis device for electrolysis, wherein a constant voltage control mode is adopted in the electrolysis process;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 200-400mg/L sodium acrylate-acrylamide copolymer, and pouring into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 2-3 times, wherein the suction capacity of a suction pump is 25L/min; then diluting the filtrate by 2 times, using a polycarbonate filter membrane with the aperture of 2 mu m, controlling the air suction amount of an air suction pump to be 50L/min, and repeatedly performing suction filtration for 2-3 times; then diluting the filtrate by 5 times, using a polycarbonate filter membrane with the aperture of 0.45 mu m, controlling the air suction amount of an air suction pump to be 100L/min, and repeatedly performing suction filtration for 2-3 times;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
Further, the diameter of the round rod-shaped electrolytic sample in the step (1) is 15-20mm, and the length of the round rod-shaped electrolytic sample is 50-70 mm.
Further, the insulation sealing used at the lower end part in the step (2) is wax sealing or plastic sealing.
Furthermore, the solvent of the electrolyte in the step (2) is (85-90) vol% of absolute methanol- (5-10) vol% of glycerol- (5-10) vol% of triethanolamine, and tetramethylammonium chloride accounting for 1.0-2.0 wt% of the total mass of the solvent is added.
Further, the voltage is controlled at 160mV for the first 1-2h in the step (3), and the current is controlled at 0.07-0.08A; then the voltage is adjusted to 120 mV and the current is 0.05-0.06A until the electrolysis is finished.
Further, the voltage is controlled to be 150mV and the current is controlled to be 0.08A 2h before the electrolysis process; the voltage was then adjusted to 130mV and the current 0.05A until the electrolysis was complete.
Further, the non-aluminum weak deoxidation bearing steel comprises, by mass, 0.96-1.05% of C, 0.15-0.35% of Si, 0.25-0.45% of Mn, 1.40-1.60% of Cr, less than 0.02% of P, less than 0.02% of S and less than 0.15% of Ti.
Further, the bearing steel comprises, by mass, 1.0% of C, 0.27% of Si, 0.35% of Mn, 1.45% of Cr, 0.015% of P, 0.0065% of S and 0.08% of Ti.
According to the invention, the acrylate copolymer is added in the electrolytic process, so that a wetting film can be formed on the surface of the inclusion generated by electrolysis, and the agglomeration of the inclusion can be reduced by controlling the addition amount without influencing the electrolytic process. In the suction filtration process, due to the influence of suction force of the suction pump and the collecting effect in the suction filtration process, aggregation and polyaddition of inclusions with different shapes can reduce the collecting effect when filtrate passes through a polycarbonate filter membrane by adding a copolymer of sodium acrylate and acrylamide and controlling the air extraction amount according to the concentration of electrolyte.
The present invention is preferably applied to an electrolytic sample having no edge or an unclear edge, but in order to control the uniformity of the electrolytic interface, an electrolytic sample having a diameter of phi (15-20) mm and a length of 50-70mm is preferably used as the dimension.
Since the electrolytic strength of the position with a distinct boundary such as an edge or an edge angle of the electrolytic sample is different from that of other positions, the electrolytic rate is not consistent under the same voltage and current, and the damage degree to the inclusion and the matrix is not the same, so that the three-dimensional morphology of the inclusion in the original form is difficult to be displayed uniformly and completely. The invention adopts a cylindrical electrolysis sample, and the lower end part immersed in the electrolyte is insulated and sealed, thereby avoiding overlarge electrolysis strength at the intersection line of the lower end surface and the cylindrical side surface; on the other hand, because the inclusions are often embedded and compounded with the matrix material, the electrolysis rate of the bottom end face of the electrolysis sample is too high, and when the electrolysis sample is electrolyzed to a certain extent to form a hollow shape, the composite of the inclusions and the matrix can fall off to the bottom of the electrolytic cell under the action of gravity and cannot be continuously electrolyzed, so that the original appearance cannot be separated.
In the electrolysis process, a sectional control mode is adopted for voltage and current, and in the initial stage of electrolysis, the surface of an electrolysis sample is smooth and uniform, and the electrolysis strength is weak; as the electrolysis proceeds, the specific surface area increases, and inclusions precipitate and are largely destroyed. Therefore, the invention adopts high-voltage high-current electrolysis in the early stage of electrolysis and low-voltage low-current electrolysis in the later stage.
Compared with the prior art, the invention has the following beneficial effects:
under the condition of not adjusting the electrolysis process of the small sample too much, the invention realizes the accurate separation of the inclusions in the non-aluminum weak deoxidized bearing steel only by processing the electrolysis position of the electrolysis sample and adjusting the technological parameters of the electrolysis, and has the advantages of no adhesion with the matrix material, high extraction rate and complete three-dimensional appearance. The acrylate copolymer is added into the electrolyte in the electrolytic process, the sodium acrylate and acrylamide copolymer is added into the filtrate in the suction filtration, and the concentration and the air extraction amount of the filtrate are controlled through three-stage suction filtration, so that the silicate inclusions which are good in three-dimensional appearance and do not agglomerate are obtained through separation.
Drawings
FIG. 1 is a scanning electron microscope image of inclusions isolated in example 1 of the present invention under a first field of view;
FIG. 2 is a SEM image of inclusions separated in example 1 of the present invention under a second visual field;
FIG. 3 is a scanning electron micrograph of inclusions isolated in comparative example 2 of the present invention in a first field of view;
FIG. 4 is a SEM image of inclusions isolated in comparative example 2 of the present invention in a second visual field.
Detailed Description
In order to better explain the present invention and to facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below.
The steel type aiming at extracting the inclusions is non-aluminum weak deoxidation bearing steel, and the steel comprises, by mass, 0.96-1.05% of C, 0.15-0.35% of Si, 0.25-0.45% of Mn, 1.40-1.60% of Cr, less than 0.02% of P, less than 0.02% of S and less than 0.15% of Ti. In order to avoid the influence of the material on the electrolysis method, the electrolysis samples used in all the examples 1 to 5 of the invention aiming at the non-aluminum weak deoxidized bearing steel are taken from the same steel billet, and the specific components are 1.0% of C, 0.27% of Si, 0.35% of Mn, 1.45% of Cr, 0.015% of P, 0.0065% of S and 0.08% of Ti through component detection.
The following examples are merely illustrative of the present invention and do not represent or limit the scope of the present invention, which is defined by the claims.
Example 1
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, and immersing the round rod-shaped electrolytic sample into the electrolyte, wherein the electrolyte is a solvent of 90vol% of anhydrous methanol, 5vol% of glycerol and 5vol% of triethanolamine, and is prepared by adding 2wt% of tetramethylammonium chloride and 200mg/L of acrylate copolymer of the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 400mg/L of the copolymer of sodium acrylate and acrylamide, and pouring into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 25L/min; then diluting the filtrate by 2 times, using a polycarbonate filter membrane with the aperture of 2 mu m, controlling the air suction amount of an air suction pump to be 50L/min, and repeatedly performing suction filtration for 3 times; then diluting the filtrate by 5 times, using a polycarbonate filter membrane with the aperture of 0.45 mu m, controlling the suction capacity of a suction pump to be 100L/min, and repeatedly performing suction filtration for 3 times;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means. The inclusions observed were in a substantially dispersed state and were not agglomerated, and as shown in fig. 1 and 2, they were obtained by scanning electron microscopy under a first field of view and a second field of view, respectively, of the inclusions separated.
Example 2
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, and immersing the middle cylindrical surface into the electrolyte, wherein the electrolyte is a solvent of 85vol% of anhydrous methanol, 5vol% of glycerol and 10vol% of triethanolamine, and is prepared by adding 1.5wt% of tetramethylammonium chloride and 150mg/L of acrylate copolymer of the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 300mg/L of sodium acrylate and acrylamide copolymer, and pouring into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 25L/min; then diluting the filtrate by 2 times, using a polycarbonate filter membrane with the aperture of 2 mu m, controlling the air suction amount of an air suction pump to be 50L/min, and repeatedly performing suction filtration for 3 times; then diluting the filtrate by 5 times, using a polycarbonate filter membrane with the aperture of 0.45 mu m, controlling the suction capacity of a suction pump to be 100L/min, and repeatedly performing suction filtration for 3 times;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
Example 3
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, and immersing the round rod-shaped electrolytic sample into the electrolyte, wherein the electrolyte is a solvent of 88vol% of anhydrous methanol, 6vol% of glycerol and 6vol% of triethanolamine, and 1wt% of tetramethylammonium chloride and 100mg/L of acrylate copolymer are added in the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 200mg/L of sodium acrylate and acrylamide copolymer, and pouring into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 25L/min; then diluting the filtrate by 2 times, using a polycarbonate filter membrane with the aperture of 2 mu m, controlling the air suction amount of an air suction pump to be 50L/min, and repeatedly performing suction filtration for 3 times; then diluting the filtrate by 5 times, using a polycarbonate filter membrane with the aperture of 0.45 mu m, controlling the suction capacity of a suction pump to be 100L/min, and repeatedly performing suction filtration for 3 times;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
Comparative example 1
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, and immersing the middle cylindrical surface into the electrolyte, wherein the electrolyte is a solvent of 85vol% of anhydrous methanol, 5vol% of glycerol and 10vol% of triethanolamine, and is prepared by adding 1.5wt% of tetramethylammonium chloride and 150mg/L of acrylate copolymer of the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 300mg/L of sodium acrylate and acrylamide copolymer, and pouring into a filter flask; and (3) carrying out suction filtration repeatedly for 4 times by using a polycarbonate filter membrane with the aperture of 2 mu m, and carrying out suction filtration repeatedly for 4 times by using a polycarbonate filter membrane with the aperture of 0.45 mu m to obtain filtrate after the first suction filtration, wherein the suction capacity of a suction pump is controlled to be 50L/min in the suction filtration process.
(5) And placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
Comparative example 2
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, immersing the middle cylindrical surface in the electrolyte, wherein the electrolyte is a solvent of 85vol% of anhydrous methanol, 5vol% of glycerol and 10vol% of triethanolamine, and adding 1.5wt% of tetramethylammonium chloride based on the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, and pouring the washing liquid and the electrolyte into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 25L/min; then diluting the filtrate by 2 times, using a polycarbonate filter membrane with the aperture of 2 mu m, controlling the air suction amount of an air suction pump to be 50L/min, and repeatedly performing suction filtration for 3 times; then diluting the filtrate by 5 times, using a polycarbonate filter membrane with the aperture of 0.45 mu m, controlling the suction capacity of a suction pump to be 100L/min, and repeatedly performing suction filtration for 3 times;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means. The observed small-particle inclusions were agglomerated, and as shown in fig. 3 and 4, the separated inclusions were observed in a first visual field and a second visual field, respectively, by scanning electron microscopy.
Comparative example 3
An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis comprises the following steps:
(1) sampling and processing a steel sample to be detected into a round rod-shaped electrolytic sample, wherein the diameter of the electrolytic sample is phi 20mm, the length of the electrolytic sample is 50mm, polishing the surface of the electrolytic sample by using sand paper to remove a surface oxide layer, and then cleaning the surface of the electrolytic sample by using acetone to remove oil stains;
(2) sealing the upper end of a round rod-shaped electrolytic sample by using an insulating tape, connecting the upper end of the round rod-shaped electrolytic sample with a positive electrode of a direct-current power supply through a metal wire, carrying out heat sealing by using wax within 10mm of the lower end of the round rod-shaped electrolytic sample, isolating electrolyte, only leaving a middle cylindrical surface exposed, immersing the middle cylindrical surface in the electrolyte, wherein the electrolyte is a solvent of 85vol% of anhydrous methanol, 5vol% of glycerol and 10vol% of triethanolamine, and adding 1.5wt% of tetramethylammonium chloride based on the total mass of the solvent;
(3) connecting an electrolysis device, wherein the electrolysis process adopts a constant voltage control mode; controlling the voltage to be 150mV and the current to be 0.08A in the first 2h in the electrolysis process; after 2h, controlling the voltage to be 130mV and controlling the current to be 0.05A until the electrolysis is finished;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 300mg/L of sodium acrylate and acrylamide copolymer, and pouring into a filter flask; using a polycarbonate filter membrane with the aperture of 5 mu m, repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 25L/min; then, a polycarbonate filter membrane with the aperture of 2 mu m is used, the air suction amount of an air suction pump is 50L/min, and the suction filtration is repeatedly carried out for 3 times; then using a polycarbonate filter membrane with the aperture of 0.45 mu m, and repeatedly performing suction filtration for 3 times, wherein the suction capacity of a suction pump is 100L/min;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
The inclusions separated in each example were observed under an electron microscope, and in each of examples 1 to 3 and comparative examples 1 to 3, the inclusions were observed, and as can be seen from the scanning electron microscope, the number of particles of the inclusions was 10 μm or less in many cases. The inclusions separated in each group of examples were statistically analyzed, 30 inclusions in different visual fields were randomly counted, and then the agglomeration of inclusions was counted, with the specific results shown in table 1.
TABLE 1 agglomeration of inclusions in examples and comparative examples
| Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
| Agglomeration ratio of inclusions | 3.3% | 6.7% | 13.3% | 36.7% | 56.7% | 46.7% |
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. An original appearance analysis method for separating inclusions in non-aluminum weakly deoxidized bearing steel through electrolysis is characterized by comprising the following steps:
(1) processing a to-be-detected non-aluminum weak deoxidized bearing steel sample into a round rod-shaped electrolytic sample, polishing the surface of the round rod-shaped electrolytic sample to remove a surface oxide layer, and then cleaning the round rod-shaped electrolytic sample to remove oil stains;
(2) immersing the electrolytic sample into an electrolyte, and adding 100-200mg/L acrylate copolymer into the electrolyte;
(3) connecting an electrolysis device for electrolysis, wherein a constant voltage control mode is adopted in the electrolysis process;
(4) after the electrolysis is finished, washing the electrolysis sample, the connection section of the electrolysis sample and the lead and the cathode, collecting all washing liquid and electrolyte, adding 200-400mg/L sodium acrylate-acrylamide copolymer, and pouring into a filter flask; carrying out suction filtration with 25L/min of air suction by using a polycarbonate filter membrane with the aperture of 5 mu m; then diluting the filtrate by 2 times, and performing suction filtration by using a polycarbonate filter membrane with the aperture of 2 mu m at the air suction capacity of 50L/min; then diluting the filtrate by 5 times, and performing suction filtration by using a polycarbonate filter membrane with the aperture of 0.45 mu m at the air suction capacity of 100L/min;
(5) and placing filter membranes with different apertures for multiple suction filtration in a drying box for drying, adhering the dried filter membranes to a conductive substrate by using conductive adhesive, carrying out gold spraying or carbon spraying conductive treatment on the filter membranes fixed on the conductive substrate, and observing the three-dimensional morphology of inclusions separated from the filter membranes by using a scanning electron microscope and an energy spectrum analysis means.
2. A method for analyzing the original appearance of inclusions in bearing steel according to claim 1, wherein the solvent of the electrolyte in the step (2) is (85 to 90) vol% of anhydrous methanol- (5 to 10) vol% of glycerin- (5 to 10) vol% of triethanolamine, and tetramethylammonium chloride is added in an amount of 1.0 to 2.0 wt% based on the total mass of the solvent.
3. The method for analyzing the original appearance of inclusions in bearing steel as set forth in claim 1, wherein the voltage is controlled to be 150-160mV and the current is controlled to be 0.07-0.08A for the first 1-2 hours in the step (3); then the voltage is adjusted to 120 mV and the current is 0.05-0.06A until the electrolysis is finished.
4. The method for analyzing the original appearance of inclusions in bearing steel according to claim 3, wherein the control voltage is 150mV and the control current is 0.08A 2h before the electrolysis process; the voltage was then adjusted to 130mV and the current 0.05A until the electrolysis was complete.
5. The method for analyzing original appearance of inclusions in bearing steel according to claim 1, wherein the amount of the acrylate copolymer added during the electrolysis is 200mg/L, and the amount of the sodium acrylate-acrylamide copolymer added to the collected rinse solution and electrolyte after the completion of the suction filtration is 400 mg/L.
6. The method for analyzing the original appearance of inclusions in bearing steel according to claim 1, wherein the non-aluminum weakly deoxidized bearing steel comprises 0.96 to 1.05% by mass of C, 0.15 to 0.35% by mass of Si, 0.25 to 0.45% by mass of Mn, 1.40 to 1.60% by mass of Cr, less than 0.02% by mass of P, less than 0.02% by mass of S, and less than 0.15% by mass of Ti.
7. A method for analyzing the original appearance of inclusions in bearing steel according to claim 6, wherein the bearing steel comprises, by mass, 1.0% C, 0.27% Si, 0.35% Mn, 1.45% Cr, 0.015% P, 0.0065% S, and 0.08% Ti.
8. The method for analyzing the original appearance of inclusions in bearing steel according to claim 1, wherein the round-rod-shaped electrolytic sample in the step (1) has a diameter of 15 to 20mm and a length of 50 to 70 mm.
9. The method for analyzing the original appearance of inclusions in bearing steel according to claim 1, wherein, before the electrolytic sample is immersed in the electrolyte in the step (2), the upper end of the round rod-shaped electrolytic sample is sealed with an insulating tape, and is connected with the positive electrode of the direct current power supply through a metal wire, and the lower end is sealed in an insulating manner, leaving only the middle cylindrical surface exposed.
10. The method for analyzing the original appearance of inclusions in bearing steel according to claim 9, wherein the insulating seal used at the lower end portion in the step (2) is wax-sealed or plastic-sealed.
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