CN112763524B - Three-dimensional corrosion method for carbide in GCr15 bearing steel - Google Patents
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Abstract
The invention discloses a three-dimensional corrosion method for carbides in GCr15 bearing steel, and belongs to the field of metal material detection. The method carries out current directional etching by configuring given etching liquid and setting different etching parameters under a specific etching method, so that the GCr15 steel matrix is partially dissolved, and the carbide is fully exposed on the premise of ensuring the complete morphology of the carbide. The method has the advantages that: under the corrosion etching solution provided by the invention, primary carbide and secondary carbide in steel can be respectively corroded and etched by changing the current density and the corrosion etching time, the whole process can be carried out at normal temperature, an extraction process is not needed, the operation is simple and convenient, the consumed time is short (less than or equal to 20 min), and in-situ electrolysis and in-situ analysis are carried out on a metal matrix. After the etching is finished, the scanning electron microscope can be used for completely observing the three-dimensional shapes of different carbides, so that the spatial distribution and morphological characteristics of the carbides are accurately mastered, and the further analysis of the carbides is deepened.
Description
Technical Field
The invention relates to the field of metal material detection, in particular to a three-dimensional corrosion method for carbides in GCr15 bearing steel
Background
GCr15 is high-carbon bearing steel with good performance, the most extensive application and the largest world output, and has high and uniform hardness, good wear resistance and higher contact fatigue performance after quenching and tempering. Because of its high carbon content (0.95-1.05%), its hardness and strength are high and it is often used for the manufacture of tools such as drills, reamers, etc. However, the high carbon content also causes a great amount of carbides to be precipitated during solidification and rolling, and these high-hardness and high-brittleness carbides not only serve as sources of fatigue cracks, but also cause severe phenomena such as product surface peeling.
The GCr15 bearing steel can generate serious dendritic segregation during solidification, so that the concentration of carbon and other metal elements in local areas is increased, and when the condition of forming eutectic components is reached, the carbon and other metal elements are segregated to form ledeburite eutectic carbide which is directly precipitated from a liquid phase. Such liquated carbides, also known as primary carbides, have a high chromium content, a high hardness and size, and are most detrimental in carbide defects.
However, if the concentration of carbon and other metal elements in a local region does not reach the precipitation condition during solidification, these regions are elongated into a segregation zone of high concentration after hot working deformation, and a large amount of carbide precipitates to form a band-shaped structure in the subsequent cooling process, and hence they are also called band-shaped carbide. In addition, during rolling, under the influence of liquated carbides and band-shaped carbides, the bearing steel precipitates proeutectoid carbides along grain boundaries during austenite cooling, and the carbides surround the austenite grains and are microscopically reticulated, so that the bearing steel is also called reticulated carbide. The band-like carbides and the network-like carbides are essentially carbides precipitated from austenite and are also collectively referred to as secondary carbides, and the presence of the secondary carbides weakens the intermetallic bonding force, lowers the mechanical properties of the steel, particularly lowers the impact toughness, and easily causes grain boundary cracking, thereby lowering the wear resistance of the bearing steel.
Therefore, how to control the precipitation of the carbide in the GCr15 bearing steel is of great significance for improving the quality of the bearing steel, and how to accurately and completely obtain the appearance of the carbide in the bearing steel is a more important field of research. Methods for extracting nonmetallic inclusions, which have been reported so far, are roughly two methods, acid dissolution and electrolysis. The acid dissolution method has been developed early and has wide application, and adopts HNO with various concentrations 3 、H 2 SO 4 The aqueous solution of HCl and HCl dissolves the metal matrix, while some stable inclusions not dissolved by the acid may remain. The acid dissolution method is described in the literature, "study of three-dimensional morphology of ultrafine oxide inclusions in steel by acid dissolution method" (journal of Steel research, 2007, (04) 85-89.)
The electrolysis method comprises the steps of aqueous solution electrolysis and non-aqueous solution electrolysis, wherein the impurities are separated from the steel through electrolysis, and then the impurities are filtered, extracted, weighed and analyzed for granularity and chemical composition, so that the information of the content, type and granularity of the non-metallic impurities in the steel can be given. The electrolyte adopted by the aqueous solution electrolysis method is an acidic aqueous solution, similar to the acid dissolution method, the acidic aqueous solution can destroy a plurality of inclusions in steel, and the electrolysis method can only completely retain the inclusions with larger sizes (more than or equal to 50 mu m), and can not accurately evaluate the inclusions with small sizes (2-20 mu m) with higher content in the steel, so the method also needs to be improved. In the book, "non-metallic inclusions in steel", 7 kinds of non-aqueous electrolytes are mentioned, but there are great limitations on the types of steel and inclusions that can be extracted by these electrolytes, either for one type of steel or for a type of inclusions.
Therefore, if the method is adopted to extract the inclusions in the steel, the time is consumed, the efficiency is low, the GCr15 bearing steel has weak conductivity and the corrosion resistance of the carbide is not high, so the existing electrolytic formula and parameters are not suitable for the steel, the limitation is large, and the further analysis of the carbide is limited.
Chinese patent CN 106840802A discloses an original appearance analysis method for separating inclusions in high-carbon steel by electrolysis, which is characterized in that a sample is preheated in a heating furnace, and an electrolyte is absolute methanol or ethanol- (5-15)% acetylacetone- (0.5-1.5)% tetramethylammonium chloride; the voltage control range during electrolysis is 120 mV-160 mV, and the holding current is 0.04A-0.07A cm 2 Within the range, the electrolysis time is 2-5 h; after electrolysis, collecting flushing liquid and electrolyte, pouring the flushing liquid and the electrolyte into a filter flask, carrying out graded suction filtration on the impurities by adopting filter membranes with the aperture of 2 mu m and 0.45 mu m, drying, and then analyzing the extracted impurities by utilizing a scanning electron microscope and energy spectrum. The present invention is different from the above inventions in that: the method adopts an in-situ electrolysis method, does not need extraction and collection processes, carries out in-situ electrolysis and in-situ analysis on the metal matrix, does not need preheating treatment, only needs 10-20 min for time consumption, and is simpler and more efficient to operate. And the carbide in the bearing steel is mainly (Fe, cr) 3 C, the complexing agent acetylacetone and Fe in the invention 2+ The complex reaction has strong capability, so that the carbide can be partially dissolved in the electrolytic process, thereby destroying the complete appearance of the carbide.
Chinese patent CN 110161066A discloses a method for extracting inclusions in steel by non-aqueous solution, which is characterized in that the components of the used electrolyte (mass percent) are: 10 percent of acetylacetone, 0.4 to 0.8 percent of tetramethylammonium chloride, 1 to 5 percent of ammonium thiocyanate and the balance of anhydrous methanol, the voltage is 2 to 5V, and the current is 0.04 to 0.05A cm 2 The electrolysis time is 2.5h; after electrolysis, the electricity is dischargedAnd (3) moving the electrolyte into a centrifugal tube to perform high-speed centrifugal motion, so that impurities in the electrolyte are adhered to the side wall of the centrifugal tube, pouring the electrolyte, adding absolute ethyl alcohol, fully mixing, dripping onto a monocrystalline silicon wafer, naturally drying by distillation, and observing the impurities on a scanning electron microscope. The present invention is different from the above inventions in that: the invention adopts the in-situ electrolysis method, does not need the extraction and collection processes, and carries out in-situ electrolysis and in-situ analysis on the metal matrix. In addition, in the invention, acetylacetone is also selected as a complexing agent, and the problem that the morphology of carbide is damaged due to damage in the electrolytic process still exists due to the strong complexing capability of the acetylacetone.
Chinese patent CN111596094A discloses a three-dimensional etching device and an etching method for nonmetallic inclusions in steel (9 electrolytic formulas are provided), wherein the etching operation is carried out according to the given method and etching parameters by a given etching device, current directional etching is carried out in etching liquid prepared by neutral solvent, complexing agent and conductive agent, the steel matrix is partially dissolved, the inclusions are not dissolved, the spatial morphology of the inclusions is exposed, the spatial position information of the inclusions is retained, the electrolysis temperature is-15-45 ℃, and the current density is 20-300 mA/cm 2 . The invention is different from the above invention in that: the corrosion etching liquid, the corrosion etching current density and the corresponding corrosion etching time are different from those of the corrosion etching liquid, the electrolyte in the invention is suitable for steel with a ferritic structure as an electrolytic matrix, is not suitable for weak-conductivity bearing steel with a structure of pearlite and cementite, and further limits corrosion to the bearing steel matrix due to the fact that the current density is smaller, so that carbides in the steel cannot be completely exposed.
Disclosure of Invention
In order to observe the three-dimensional appearance of carbide in GCr15 bearing steel, the invention provides a three-dimensional corrosion method of carbide in GCr15 bearing steel, which corrodes a steel matrix and exposes carbide by configuring specific electrolyte and setting different corrosion parameters, so that the three-dimensional appearance of different carbide in steel can be comprehensively and carefully observed, no toxic substance is generated in the whole electrolysis process, and the operation process is simple and efficient.
A three-dimensional corrosion method for carbides in GCr15 bearing steel comprises the following steps:
a. aiming at GCr15 bearing steel, the method has the advantages that the chemical component mass percentages and the microscopic structures of the material both meet the following requirements: GB/T18254-2016;
b. the etching solution adopted by the method comprises the following components: tetramethylammonium chloride, potassium chloride, acetylacetone, sodium tripolyphosphate and methanol solution, wherein the components in percentage by volume are as follows: 10-15% (m/V) tetramethylammonium chloride, 8-15% (m/V) potassium chloride, 2-5% acetylacetone, 10-15% sodium tripolyphosphate and the balance methanol;
c. the method adopts the normal temperature condition that the initial electrolysis temperature is 10-30 ℃ and the etching current density is 500-800mA/cm 2 Controlling the etching time to be 10-20 min; the current density selected for different carbides is matched with etching time, and for primary carbides with the size of 50-200 μ M, namely M directly precipitated from liquid phase in the solidification process 7 C 3 The current density of the carbide is controlled to be 700-800 mA/cm 2 The etching time is controlled to be 16-20 min; for secondary carbides of size 5-30 μ M, i.e. M precipitated from the austenite grain boundaries during cooling 23 C 6 The current density of the type carbide is controlled between 500 and 600mA/cm 2 The etching time is controlled to be 10-15 min.
The preferred etching solution comprises the following components: 13% (m/V) tetramethylammonium chloride, 10% (m/V) potassium chloride, 3% acetylacetone, 13% sodium tripolyphosphate and the balance of methanol.
The corrosion current density and the corresponding corrosion time of different carbides are preferably as follows: primary carbide with current density of 780mA/cm 2 Etching for 19min; secondary carbide with current density of 530mA/cm 2 The etching time is 11min.
Preferably, the three-dimensional corrosion method for carbides in GCr15 bearing steel is not only suitable for GCr15 bearing steel, but also suitable for wear-resistant steel, cord steel or other high-carbon steel.
The method mainly comprises the steps of sample preparation, etching solution preparation, etching device connection, etching parameter setting, sample processing and observation. The specific operation process is as follows:
(1) Sample preparation
The shape of the sample has no special requirements, and the observation surface is polished by sand paper, washed by absolute ethyl alcohol after being polished and dried, and is opposite to the cathode.
(2) Etching solution configuration (volume ratio)
The etching solution is prepared by a neutral solvent, an electrolyte and a matrix element complexing agent according to a certain proportion. The electrolyte formula of the invention is as follows: 10 to 15 percent (m/V) tetramethylammonium chloride, 8 to 15 percent (m/V) potassium chloride, 2 to 5 percent acetylacetone, 10 to 15 percent sodium tripolyphosphate and the balance of methanol solution. The neutral solvent is high-purity methanol, has better solubility to inorganic salts and complexes than ethanol, and is a preferred solvent of the neutral electrolyte; as the bearing steel has weaker conductive capability, in order to enable the electrolyte to provide more conductive particles in the solution and enhance the conductive capability of the electrolyte, the electrolyte selected by the invention is 10-15% (m/V) tetramethylammonium chloride + 8-15% (m/V) potassium chloride; because the carbide in the bearing steel is (Fe, cr) x C y In order to slow down the strong complexing agents acetylacetone and Fe +2 The reaction of (2) and (5) is carried out to protect the complete morphology of carbide, the content of acetylacetone is controlled to be 2-5%, and Fe (OH) caused by too low content of complexing agent is prevented 3 The invention adds sodium tripolyphosphate with weak complexing ability, and the content of the sodium tripolyphosphate is controlled to be 10-15%.
(3) Connecting etching device
The anode rectangular steel sheet and the cathode clamp of the etching device are both made of stainless steel materials, so that good current stability can be kept, the anode rectangular steel sheet and the cathode clamp are respectively fixed by using insulating rubber, the distance between the cathode and the anode is 20-30 mm, and the bottom positions of the anode clamp and the cathode at the other end are ensured to be positioned on the same horizontal line, so that the anode and the cathode are prevented from touching the inner wall of the electrolytic etching groove.
(4) Etching parameter setting
(1) Etching temperature
The electrolytic corrosion temperature of the GCr15 bearing steel is controlled within the room temperature range of 10-30 ℃, but not too high or too low. Too high a temperature leads to a faster volatilization rate of the etching solution, which increases the resistivity and reduces the conductivity during the electrolysis process, thereby leading to a longer electrolysis time. If the temperature is too low, the ion diffusion in the etching solution is slowed down, and the etching solution crystallization phenomenon is formed, so that the steel matrix is not completely corroded, and the carbide cannot be completely exposed.
(2) Current density and etching time
When GCr15 bearing steel is electrolyzed, a direct-current stabilized power supply is adopted. The GCr15 bearing steel has higher carbon content, the structure is cementite and pearlite, and the electrical conductivity is poorer than that of low-carbon steel, so that the steel matrix can be fully corroded by adopting higher current density, the carbide is easier to observe, and the current density is controlled to be 500-800mA/cm 2 (ii) a Because carbides in GCr15 bearing steel are metal carbides formed by carbon atom chains penetrating through a deformed metal structure and Cr, mn and Fe, the properties of the metal carbides are between ionic type and simple filling type, the corrosion resistance is not high, the electrolysis time is controlled to be 10-20 min, and if the electrolysis time is too long, the carbides are partially dissolved, so that the integrity is damaged, and the full appearance cannot be observed.
The current density chosen for the different carbides is matched to the etching time. In the case of primary carbides, which are directly precipitated from the liquid phase during solidification, the alloying elements Cr and Fe combine with C to form M 7 C 3 The size of the type carbide is larger and is between 50 and 200 mu M, and M is influenced by dendrite segregation 7 C 3 The Cr content of the carbide type is higher, and the carbide is shown as Cr-rich type carbide, so the content of Fe is lower, which causes M 7 C 3 The carbide has certain corrosion resistance, and can still keep complete morphology under high-density current and long-time etching. Thus for this large size M with a certain resistance to corrosion 7 C 3 The current density of the carbide is controlled to be 700-800 mA/cm 2 The etching time is controlled to be 16-20 min, and the steel substrate can be more sufficiently etched by the larger current density and the longer etching time, so that the large-size M is obtained 7 C 3 Type carbide completeAnd (5) exposing.
For secondary carbides, which precipitate from the austenite grain boundaries during cooling, M is already formed in the liquid phase with Fe, C due to the majority of Cr 7 C 3 Type carbide, so that the carbide precipitated from austenite is M with a low Cr content 23 C 6 Its size is smaller at 5-30 μ M, and its Fe content is higher, so that M is 23 C 6 The corrosion resistance of the type secondary carbide is relatively poor, and the secondary carbide needs to be selected to have relatively small current density and short etching time, and the current density is controlled to be 500-600 mA/cm 2 The etching time is controlled within 10-15 min to prevent the complete appearance of the electrolytic cell from being damaged in the electrolytic process.
(5) Sample processing and viewing
And after the etching is finished, spraying and washing the residual solvent on the surface by adopting absolute ethyl alcohol, and before the solvent is placed under a scanning electron microscope for observation, drying the solvent in a drying box to prevent the residual solvent from polluting the scanning electron microscope, wherein if the observation result is not to be managed, the etching process can be repeated by adjusting parameters.
Drawings
FIG. 1 shows a first embodiment: GCr15 bearing steel-780 mA/cm 2 And etching the carbide SEM picture for 19min once.
FIG. 2 example two: GCr15 bearing steel-780 mA/cm 2 And etching the 17min primary carbide SEM picture.
Fig. 3 example three: GCr15 bearing steel-720 mA/cm 2 Etching 19min primary carbide SEM picture.
FIG. 4 example four: GCr15 bearing steel-720 mA/cm 2 And etching the 17min primary carbide SEM picture.
Fig. 5 example five: GCr15 bearing steel-590 mA/cm 2 Etching 13min secondary carbide SEM picture.
Fig. 6 example six: GCr15 bearing steel-590 mA/cm 2 Etching 11min secondary carbide SEM picture.
Fig. 7 shows an embodiment: GCr15 bearing steel-530 mA/cm 2 Etching 13min secondary carbide SEM picture.
Fig. 8 example eight: GCr15 bearing steel-530 mA/cm 2 Etching 11min secondary carbide SEM picture.
Fig. 9 comparative example one: SEM picture of GCr15 bearing steel corrosion-etched carbide
Detailed Description
The following detailed description is made in conjunction with the accompanying drawings, examples and comparative patents.
The embodiment is as follows:
carrying out electrolytic corrosion on GCr15 bearing steel (chemical components are 1.0 percent of C, 0.25 percent of Si, 0.34 percent of Mn, 0.013 percent of P, 0.002 percent of S and 1.48 percent of Cr);
etching is carried out according to the steps in the invention content, the size of a sample is 10 x 10mm, and etching parameters are as follows:
the etching liquid volume percentage is as follows: 13% (m/V) tetramethylammonium chloride, 10% (m/V) potassium chloride, 3% acetylacetone, 13% sodium tripolyphosphate and the balance of methanol;
etching temperature: 24-26 ℃;
the current densities and corresponding etch times in the examples are tabulated:
as can be seen from the attached drawings 1-4, along with the increase of the current density and the increase of the etching time, the large-sized secondary carbide is gradually etched from the iron matrix, and the three-dimensional appearance of the secondary carbide is more and more complete, so that in order to accurately observe the three-dimensional appearance of the secondary carbide in GCr15 bearing steel, the current density is 780mA/cm 2 Etching time is 19min; as can be seen from the attached figures 5 to 8, for small-size non-corrosion-resistant secondary carbides, the three-dimensional morphology of the small-size non-corrosion-resistant secondary carbides can be clearly observed under the conditions of lower current and shorter etching time, but with the increase of current density and etching time, the secondary carbides begin to be partially dissolved and are fused with surrounding carbides and tissues, so that a certain influence is caused on the observation of the real morphology of the carbides, and therefore, in order to accurately observe the three-dimensional morphology of the secondary carbides in GCr15 bearing steelThe current density should be 530mA/cm 2 The etching time is 11min.
The above-mentioned embodiments are only intended to illustrate the technical solutions of the present invention, and not to limit the present invention, and the contents of the present invention are given in the claims.
Comparative example one:
the procedure of performing electrolytic etching on GCr15 bearing steel (chemical components: 1.0% of C, 0.25% of Si, 0.34% of Mn, 0.013% of P, 0.002% of S and 1.48% of Cr) is the same as that described in example 2 of Chinese patent CN 111596094A; etching parameters are as follows:
sample size: 10 × 10mm;
etching solution (volume percent): 6% (m/V) tetramethylammonium chloride, 18% acetylacetone and the balance of methanol;
etching temperature: 5 ℃;
current density: 300mA/cm 2 ；
Etching time: 45-80min.
The implementation effect is shown in fig. 9, and it can be seen from the figure that under the electrolytic etching condition, the large-sized primary carbides are not completely exposed, so that the overall morphology is blurred and cannot be accurately observed, and the secondary carbides are not completely electrolyzed, so that the electrolytic etching effect is far inferior to that of the embodiment.
Claims (3)
1. A three-dimensional corrosion method for carbide in GCr15 bearing steel is characterized by comprising the following steps:
a. aiming at GCr15 bearing steel, the method has the advantages that the chemical component mass percentages and the microscopic structures of the material both meet the following requirements: GB/T18254-2016;
b. the etching solution adopted by the method comprises the following components: tetramethylammonium chloride, potassium chloride, acetylacetone, sodium tripolyphosphate and methanol solution, wherein the components in percentage by volume are as follows: 10-15% (m/V) tetramethylammonium chloride, 8-15% (m/V) potassium chloride, 2-5% acetylacetone, 10-15% sodium tripolyphosphate and the balance methanol;
c. the method adopts the normal temperature condition that the initial electrolysis temperature is 10-30 ℃ and the etching current density is 500-800mA/cm 2 Etching time is controlled at 10 ℃20min; the current density selected for different carbides is matched with the etching time, and for the primary carbides with the size of 50-200 μ M, namely M directly precipitated from the liquid phase in the solidification process 7 C 3 The current density of the type carbide is controlled between 700 and 800mA/cm 2 The etching time is controlled to be 16-20 min; for secondary carbides of size 5-30 μ M, i.e. M precipitated from the austenite grain boundaries during cooling 23 C 6 The current density of the carbide is controlled between 500 and 600mA/cm 2 The etching time is controlled to be 10-15 min;
the three-dimensional etching method for carbides in GCr15 bearing steel is not only suitable for GCr15 bearing steel, but also suitable for wear-resistant steel, cord steel or other high-carbon steel.
2. The three-dimensional etching method for carbides in GCr15 bearing steel according to claim 1, wherein: the etching solution comprises the following components: 13% (m/V) tetramethylammonium chloride, 10% (m/V) potassium chloride, 3% acetylacetone, 13% sodium tripolyphosphate and the balance of methanol.
3. The three-dimensional etching method for carbides in GCr15 bearing steel according to any one of claims 1-2, wherein: the etching current density and the corresponding etching time of different carbides are as follows: primary carbide with current density of 780mA/cm 2 Etching time is 19min; secondary carbide with current density of 530mA/cm 2 The etching time is 11min.
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