阅读说明：本技术 一种利用脉冲电流调控轴承钢中网状碳化物的方法 (Method for regulating and controlling network carbide in bearing steel by using pulse current ) 是由 张新房 郝剑桥 于 2021-08-18 设计创作，主要内容包括：本发明公开一种利用脉冲电流调控轴承钢中网状碳化物的方法,属于高质量轴承钢制造的技术领域。所述方法包括对存在粗大的网状碳化物的热轧态轴承钢取样、试样表面的打磨清洗、确定脉冲电流参数、在室温下进行脉冲电流处理、观察碳化物形貌及分布和碳化物量化表征。本发明的所述方法可显著改善轴承钢的显微组织均匀性,通过脉冲电流处理促进轴承钢轧后析出的网状碳化物优先固溶,实现晶界、晶内处碳原子的重新分配,从而达到提高轴承钢中碳化物分布均匀性,改善其产品质量的目的。该方法所需工况温度低、时间短,可直接通过外接电源对材料进行处理,操作简单,符合当前工业绿色发展规划的要求。(The invention discloses a method for regulating and controlling network carbide in bearing steel by using pulse current, and belongs to the technical field of high-quality bearing steel manufacturing. The method comprises the steps of sampling hot-rolled bearing steel with coarse reticular carbides, polishing and cleaning the surface of a sample, determining pulse current parameters, carrying out pulse current treatment at room temperature, observing the morphology and distribution of the carbides, and quantitatively characterizing the carbides. The method can obviously improve the microstructure uniformity of the bearing steel, promotes the prior solid solution of the reticular carbide precipitated after the bearing steel is rolled through the pulse current treatment, and realizes the redistribution of carbon atoms at the grain boundary and the crystal interior, thereby achieving the purposes of improving the distribution uniformity of the carbide in the bearing steel and improving the product quality. The method has the advantages of low required working condition temperature, short time, simple operation and accordance with the requirements of the current industrial green development planning, and can directly process the materials through an external power supply.)

1. A method for regulating and controlling network carbide in bearing steel by using pulse current is characterized in that the method carries out pulse current treatment on the hot-rolled bearing steel with coarse network carbide; the method obviously improves the carbide uniformity of the bearing steel and improves the product quality; the method specifically comprises the following steps:

s1: sampling hot-rolled bearing steel with coarse reticular carbide;

s2: polishing and cleaning the surface of the sample;

s3: determining a pulse current parameter;

s4: carrying out pulse current treatment at room temperature;

s5: observing the morphology and distribution of carbides;

s6: and (6) quantitatively characterizing carbides.

2. The method for efficiently regulating and controlling carbide in bearing steel by using pulse current according to claim 1, wherein the parameter range for determining the pulse current parameter in the step S3 is as follows: the frequency is 10-50000Hz, the pulse width is 10-500 mus, the current is 10-5000A, and the action time is 5min-10 h.

3. The method for efficiently controlling carbides in bearing steel according to claim 1, wherein the sampling of the hot rolled bearing steel in step S1 in which coarse network carbides exist comprises determination of the size and determination of the coarse network carbides.

4. The method for efficiently regulating and controlling carbide in bearing steel by using pulse current as claimed in claim 1, wherein the polishing and cleaning in step S2 comprises sequentially polishing the surface of the sample by 400-800 mesh, 1000-1400 mesh and 1800-2500 mesh sandpaper until no visible defects are detected, so as to ensure good contact with the pulse electrode.

5. The method for efficiently controlling carbides in bearing steel by using pulsed current according to claim 1, wherein argon gas is used for protection of surface oxidation during the pulsed current treatment in step S4.

6. The method for efficiently regulating and controlling the carbide in the bearing steel by using the pulse current according to claim 1, wherein the morphology and distribution of the carbide are observed in step S5 by polishing, mechanically polishing, chemically etching a sample treated by the pulse current and observing the sample by using a field emission electron scanning microscope.

7. The method for efficiently regulating and controlling carbide in bearing steel by using pulse current as claimed in claim 1, wherein the step of polishing the sample after the pulse current treatment comprises polishing the surface by 400-800 mesh sand paper, 1000-1400 mesh sand paper and 1800-2500 mesh sand paper in sequence until only one-way scratches are formed.

8. The method for efficiently regulating and controlling carbide in bearing steel by using pulse current according to claim 6, wherein the chemical corrosion is performed at room temperature, the corrosion time is 28-32s, and the corrosion solution is composed of 3.5-4.5mL of nitric acid and 95-105mL of alcohol.

9. The method for efficiently regulating and controlling carbides in bearing steel by using pulsed current according to claim 1, wherein the quantitative characterization of carbides in the step S6 requires quantitative statistics on characteristic parameters of morphology, size and distribution of carbides of not less than 5000, and the tissue uniformity of a sample is evaluated.

10. The method for efficiently regulating and controlling carbide in bearing steel by using pulse current according to any one of claims 1 to 9, wherein the distribution uniformity of carbide in the sample after the pulse current treatment is improved by 2 to 5 times compared with that in the sample after the conventional heat treatment.

Technical Field

The invention belongs to the technical field of high-quality bearing steel manufacturing, and relates to a method for regulating and controlling network carbide in bearing steel by using pulse current.

Background

The bearing is a matched basic part which is widely used and has strict requirements in the mechanical industry. The high-carbon chromium bearing steel is used as a main material for preparing the bearing, accounts for more than 80% of the total production amount of bearing steel in the world, has higher carbon content (1 wt.%), obtains higher strength and hardness after heat treatment, and is beneficial to improving the rolling contact fatigue resistance and the wear resistance of the bearing due to the number density of carbides. However, with the increase of carbon content in steel, serious grain boundary network carbide can be precipitated, and the normal service life of the bearing is influenced.

The methods for removing the net carbide in the bearing steel comprise the following steps:

1) normalizing treatment

Removing it requires heating the steel material to A_cmThe above steps are carried out;

however, the normalizing process has a high heating temperature, which tends to cause problems such as coarse grain structure and surface decarburization. In addition, the cooling speed control after the normalizing treatment is very sensitive to the influence of the microstructure, and bainite and martensite can be formed due to too high cold degree; the cold degree is too slow, and the net-shaped carbide can be precipitated along the grain boundary again. The method not only adds extra complicated working procedures, but also easily causes the problem of uneven carbide granularity, so the technology is not generally adopted on site.

2) Controlling cooling rate

Comprises the steps of cooling the wire rod in an on-line manner by water bath isothermal quenching, wherein the highest quenching temperature is lower than A_cmAnd the carbide net is difficult to completely eliminate, the residual coarse carbide particles at the crystal boundary obviously destroy the uniformity of the bearing steel structure, and the mechanical property and the fatigue life of the bearing steel and the product thereof are reduced. This is the case for a method of controlled cooling of bearing steel wire after rolling as disclosed in patent CN 109402356A.

3) Adding rare earth elements

The rare earth elements are expensive and not beneficial to industrial mass production. For example, the patent CN104032221A discloses a niobium microalloyed high carbon chromium bearing steel and its hot rolling production method.

4) Spheroidizing annealing

The highest temperature of spheroidizing annealing is lower than A_cmAnd the carbide net is difficult to completely eliminate, the residual coarse carbide particles at the crystal boundary obviously destroy the uniformity of the bearing steel structure, and the mechanical property and the fatigue life of the bearing steel and the product thereof are reduced. For example, the patent CN103320583A discloses a GCr15 bearing steel spheroidizing annealing heat spotThis is true of the process.

Therefore, the existence of the reticular carbide is one of the main reasons for limiting the development of the bearing and the bearing steel, and if the size and the shape of the carbide in the steel can be effectively regulated and controlled by a certain means, the uniformity of the carbide in the steel can be improved, and great economic benefits can be generated for the field of steel manufacturing.

At present, the pulse current is used as a special treatment means with instantaneous high energy, which can effectively promote the dissolution and precipitation of second phase particles in the material, and realize the precise regulation and control of the morphology and distribution of the second phase particles, thereby improving the mechanical property of the material. The application of the pulse current in the preparation of the steel material particularly focuses on the following aspects:

1) pulse current for strengthening and toughening steel material

2) Pulse current refinement of non-net carbide size in M50 bearing matrix

In conclusion, the prior art does not provide that the pulse current is used for regulating and controlling and even completely eliminating the reticular carbide in the bearing steel, the subsequent spheroidizing annealing and quenching are difficult to completely eliminate the reticular carbide, and the residual coarse carbide particles at the grain boundary obviously destroy the uniformity of the bearing steel structure. Other purposes and technical effects such as pulse current treatment do not relate to the foregoing, and it is not particularly considered how to precisely control the morphology, size, distribution and the like of carbides in the bearing steel through pulse current, so as to improve the structural uniformity and improve the steel quality.

Disclosure of Invention

The invention solves the technical problems that the treatment mode of the net-shaped carbide in the existing hot-rolled high-carbon chromium bearing steel is realized by normalizing, annealing and controlling the cooling speed after quenching, and the problems of expensive equipment, complex operation, long period and the like exist.

In order to solve the technical problems, the invention provides the following technical scheme:

a method for regulating and controlling network carbides in bearing steel by using pulse current is used for carrying out pulse current treatment on hot-rolled bearing steel with coarse network carbides; the method obviously improves the carbide uniformity of the bearing steel and improves the product quality; the method specifically comprises the following steps:

s1: sampling hot-rolled bearing steel with coarse reticular carbide;

s2: polishing and cleaning the surface of the sample;

s3: determining a pulse current parameter;

s4: carrying out pulse current treatment at room temperature;

s5: observing the morphology and distribution of carbides;

s6: and (6) quantitatively characterizing carbides.

Preferably, the pulse current parameter range determined in step S3 is: the frequency is 10-50000Hz, the pulse width is 10-500 mus, the current is 10-5000A, and the action time is 5min-10 h.

Preferably, the sampling of the hot rolled bearing steel in which coarse network carbides exist in the step S1 includes determination of a size and determination of coarse network carbides.

Preferably, the polishing cleaning in step S2 includes polishing the surface of the sample with a plurality of sand papers from coarse to fine in sequence to have no visible defects, so as to ensure good contact with the pulse electrode.

Preferably, the polishing and cleaning in step S2 includes sequentially polishing the surface of the sample with 400-.

Preferably, an argon shield is used to prevent surface oxidation during the pulse current processing in step S4.

Preferably, in the step S5, the morphology and distribution of the carbide are observed by grinding, mechanically polishing, chemically etching the sample processed by the pulse current, and observing the sample by a field emission electron scanning microscope.

Preferably, the polishing of the sample after the pulse current treatment is performed by sequentially polishing a plurality of kinds of abrasive papers from coarse to fine until only one-direction scratches exist.

Preferably, the polishing of the sample after the pulse current treatment is to sequentially polish the surface with 400-.

Preferably, the chemical etching is carried out at room temperature, the etching time is 28-32s, and the etching solution consists of 3.5-4.5mL of nitric acid and 95-105mL of alcohol.

Preferably, the carbide quantitative characterization in the step S6 is to utilize ImageJ software to carry out quantitative statistics on characteristic parameters (morphology, size, distribution and the like) of not less than 5000 carbides, and to evaluate the distribution uniformity of the carbides in the sample.

Preferably, referring to the heat treatment process after rolling the industrial bearing steel, carrying out an industrial heat treatment contrast experiment on the high-carbon chromium bearing steel hot rolled bar by using a tubular vacuum furnace, wherein the treatment temperature is 780 ℃, the treatment time is 5 hours, and argon is used for protecting and preventing surface oxidation in the treatment process; the microstructure of the treated sample was also quantitatively analyzed.

Preferably, the distribution uniformity of the carbide in the sample after the pulse current treatment is improved by 2-5 times compared with the distribution uniformity of the carbide in the sample after the traditional heat treatment.

The principle of regulating and controlling the network carbide in the bearing steel by utilizing the pulse current is as follows:

the material is high-carbon chromium bearing steel with a large amount of net-shaped carbide at grain boundaries, and the proposed pulse current treatment can not only spheroidize the pearlite in the grain boundaries, but also more importantly can reduce the dissolution temperature of the grain boundary net-shaped carbide by utilizing the crystal grain orientation difference at the two sides of the grain boundaries, the distortion energy caused by defect aggregation and the chemical energy caused by element segregation, so that the temperature node for eliminating the net-shaped carbide is advanced. The intragranular structure does not have many properties of grain boundaries, so the same effect cannot be achieved under the same electric field, and therefore, the pulse current treatment can enable the grain boundaries and the carbides in the intragranular part to be homogenized simultaneously in the treatment process of the material.

Specifically, during cooling after hot rolling, a coarse carbide network is formed along the grain boundaries, and the carbide network deteriorates the uniformity of the structure of the bearing steel, thereby deteriorating the mechanical properties thereof. The morphology and distribution of the carbide directly influence the mechanical properties of the material and the service life of the bearing parts. Based on electromagnetic thermodynamics/kinetics and Landau continuous medium electrodynamics theory, an electromagnetic field provides an additional electric free energy term based on current density distribution for an alloy matrix, when heterogeneous particles exist in the alloy matrix, the current density distribution is changed due to the difference of the conductivities of the particles and the matrix, so that the electric free energy of a system is changed, the electric free energy change has the tendency of reducing the overall resistivity of the system, and the electric free energy change is used as an additional driving force for particle dissolution to promote the dissolution of heterogeneous phases. The carbide serving as second-phase particles in the bearing steel material matrix has electric conductivity far lower than that of the matrix, so that the carbide can be regulated by using pulse current.

The electric field distortion caused by carbide particles with different sizes is different, the current density around the particles with larger sizes under the electric field is relatively higher, and the energy difference caused by the selective distribution of the current promotes coarse reticular carbides at the grain boundary to be dissolved in a solid solution preferentially, so that the redistribution of the grain boundary and carbon atoms in the grain is realized. Compared with the traditional annealing process, the pulse current serving as a special treatment means with instantaneous high energy can effectively break through the thermodynamic and kinetic limitations of carbide dissolution behavior in the traditional heat treatment process. Therefore, the required working condition is low in temperature and short in time, the material can be directly processed by an external power supply, and the operation is simple.

Based on the principle, the invention can realize the accurate control of the morphology and distribution of carbide in the bearing steel by accurately controlling the pulse current processing parameters, improve the distribution uniformity of the carbide and further improve the quality of the bearing steel product.

The technical scheme provided by the embodiment of the invention at least has the following beneficial effects:

in the scheme, the pulse current is utilized to regulate and control the network carbide in the bearing steel, particularly, the pulse current treatment is used for promoting the network carbide precipitated after the bearing steel is rolled to be dissolved in solid preferentially, and the redistribution of carbon atoms at crystal boundaries and crystal interiors is realized, so that the aims of improving the distribution uniformity of the carbide in the bearing steel and improving the product quality are fulfilled.

The scheme is that pulse current treatment is carried out at normal temperature, additional heat source assistance is not needed, and the method is easy to implement, high in efficiency, green and pollution-free and has a remarkable practical application value.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.

FIG. 1 is a JEOL scanning electron microscope image of the morphology and distribution of carbides in a bearing steel bar after the mesh carbides in the bearing steel bar are regulated and controlled by using pulse current in example 2 of the present invention;

FIG. 2 is a JEOL scanning electron microscope image of the morphology and distribution of carbides in a bearing steel bar after conventional heat treatment in comparative example 1 of the present invention;

FIG. 3 is a statistical chart showing the results of the size distribution of carbides in the steel bar for bearings according to example 2 and comparative example 1 of the present invention.

Detailed Description

In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.

The following is a test material of hot rolled bar of GCr15 bearing steel, which is taken in conjunction with the attached drawings, examples and comparative examples. Quantitative statistical analysis was performed on the microstructures of the examples and comparative examples.

Example 1

This example applied pulsed current treatment to a small size GCr15 bearing steel hot rolled bar. The method comprises the following steps:

s1: a hot rolled bearing steel containing coarse network carbides was sampled. A bearing steel hot rolled bar material of 60mm multiplied by 10mm multiplied by 1.5m is taken.

S2: and (5) polishing and cleaning the surface of the sample. The surface was sequentially sanded with 600, 1200, 2000 mesh sandpaper until no visible defects were observed to ensure good contact with the pulse electrode.

S3: pulse processing parameters are determined. Setting the parameter range of the pulse current, and determining the parameters of the pulse current to be 50Hz, 20 mus, 3000A and the action time to be 10 h;

s4: the pulsed current treatment was performed at room temperature. Fixing the polished bearing steel hot rolled bar at the output end of a pulse power supply by using a clamp, carrying out 10-hour pulse current treatment on the polished bearing steel hot rolled bar at room temperature, and using argon for protection to prevent surface oxidation in the treatment process;

s5: and observing the morphology and distribution of the carbide. For the sample after pulse treatment, the surface was polished with 600 mesh, 1200 mesh, 2000 mesh sandpaper in sequence until only one-way scratches were present. After mechanically polishing a sample, chemically etching the sample for about 30 seconds at room temperature, wherein the etching solution consists of 4mL of nitric acid and 100mL of alcohol; observing the morphology and distribution of carbides in the sample after the pulse current treatment by using a field emission electron scanning microscope;

s6: and (6) quantitatively characterizing carbides. And the ImageJ software is utilized to carry out quantitative statistics on the characteristic parameters of the morphology, the size, the distribution and the like of the carbides of which the carbon number is not less than 5000, so as to evaluate the tissue uniformity of the sample.

Example 2

This example applied pulsed current treatment to a small size GCr15 bearing steel hot rolled bar. The method comprises the following steps:

s1: a hot rolled bearing steel containing coarse network carbides was sampled. A bearing steel hot rolled bar material of 60mm multiplied by 10mm multiplied by 1.5m is taken.

S2: and (5) polishing and cleaning the surface of the sample. The surface was sequentially sanded with 600, 1200, 2000 mesh sandpaper until no visible defects were observed to ensure good contact with the pulse electrode.

S3: pulse processing parameters are determined. The parameter range of the pulse current is set, the pulse current parameter is determined to be 30000Hz, 75 mus and 150A, and the action time is 30 min.

S4: the pulsed current treatment was performed at room temperature. Fixing the polished bearing steel hot rolled bar at the output end of a pulse power supply by using a clamp, carrying out 30-min pulse current treatment on the polished bearing steel hot rolled bar at room temperature, and using argon for protection to prevent surface oxidation in the treatment process.

S5: and observing the morphology and distribution of the carbide. For the sample after pulse treatment, the surface was polished with 600 mesh, 1200 mesh, 2000 mesh sandpaper in sequence until only one-way scratches were present. After mechanical polishing, chemical etching was performed at room temperature for about 30 seconds, and the etching solution consisted of 4mL of nitric acid and 100mL of alcohol. The morphology and distribution of carbides in the sample after pulsed current treatment was observed using a field emission electron scanning microscope, as shown in fig. 1.

S6: and (6) quantitatively characterizing carbides. And the ImageJ software is utilized to carry out quantitative statistics on the characteristic parameters of the morphology, the size, the distribution and the like of the carbides of which the carbon number is not less than 5000, so as to evaluate the tissue uniformity of the sample.

Example 3

This example applied pulsed current treatment to a small size GCr15 bearing steel hot rolled bar. The method comprises the following steps:

s1: a hot rolled bearing steel containing coarse network carbides was sampled. A bearing steel hot rolled bar material of 60mm multiplied by 10mm multiplied by 1.5m is taken.

S2: and (5) polishing and cleaning the surface of the sample. The surface was sequentially sanded with 600, 1200, 2000 mesh sandpaper until no visible defects were observed to ensure good contact with the pulse electrode.

S3: pulse processing parameters are determined. The parameter range of the pulse current is set, the parameters of the pulse current are determined to be 30000Hz, 100 mus and 100A, and the action time is 5 min.

S4: the pulsed current treatment was performed at room temperature. Fixing the polished bearing steel hot rolled bar at the output end of a pulse power supply by using a clamp, carrying out 5min pulse current treatment on the polished bearing steel hot rolled bar at room temperature, and using argon gas for protection to prevent surface oxidation in the treatment process.

S5: and observing the morphology and distribution of the carbide. For the sample after pulse treatment, the surface was polished with 600 mesh, 1200 mesh, 2000 mesh sandpaper in sequence until only one-way scratches were present. After mechanical polishing, chemical etching was performed at room temperature for about 30 seconds, and the etching solution consisted of 4mL of nitric acid and 100mL of alcohol. And observing the morphology and distribution of carbides in the sample after the pulse current treatment by using a field emission electron scanning microscope.

S6: and (6) quantitatively characterizing carbides. And the ImageJ software is utilized to carry out quantitative statistics on the characteristic parameters of the morphology, the size, the distribution and the like of the carbides of which the carbon number is not less than 5000, so as to evaluate the tissue uniformity of the sample.

Comparative example 1

In the embodiment, the small-size GCr15 bearing steel hot-rolled bar is subjected to comparative heat treatment by referring to a traditional annealing process. The method comprises the following steps:

s1: a hot rolled bearing steel containing coarse network carbides was sampled. Taking a bearing steel hot rolled bar material with the thickness of 60mm multiplied by 10mm multiplied by 1.5 m.

S2: and determining heat treatment parameters. The pulse current parameter is determined to be 780 ℃ and the action time is 5 h.

S3: and (6) heat treatment. The bearing steel hot-rolled bar material is placed in a vacuum tube furnace, heat treatment is carried out on the bearing steel hot-rolled bar material for 5 hours at the temperature of 780 ℃, and argon is used for protecting the surface during the treatment process to prevent surface oxidation.

S4: and observing the morphology and distribution of the carbide. For the sample after pulse treatment, the surface was polished with 600 mesh, 1200 mesh, 2000 mesh sandpaper in sequence until only one-way scratches were present. After mechanical polishing, chemical etching was performed at room temperature for about 30 seconds, and the etching solution consisted of 4mL of nitric acid and 100mL of alcohol. The morphology and distribution of carbides in the sample after pulsed current treatment was observed using a field emission electron scanning microscope, as shown in fig. 2.

S5: and (6) quantitatively characterizing carbides. And the ImageJ software is utilized to carry out quantitative statistics on the characteristic parameters of the morphology, the size, the distribution and the like of the carbides of which the carbon number is not less than 5000, so as to evaluate the tissue uniformity of the sample.

As shown in figure 3, the statistical results of the size distribution of the carbides in the bearing steel bar in the pulse treatment state shown in figure 1 and the equivalent heat treatment state shown in figure 2 show that the carbides in the sample after pulse treatment are smaller and dispersed in size, no obvious grain boundary net-shaped carbide residue exists, and the structure uniformity is better.

It was found from the comparison of the carbide size and distribution in the samples of examples 1-3 and comparative example 1 that the uniformity of the carbide distribution in the samples of examples 1-3 after pulse treatment was 2-5 times improved over the heat treated sample of comparative example 1.

In the scheme, the pulse current is utilized to regulate and control the network carbide in the bearing steel, specifically, the pulse current treatment is utilized to promote the network carbide precipitated after the bearing steel is rolled to be dissolved in solution preferentially, and the redistribution of carbon atoms in crystal boundaries and crystal interiors is realized, so that the aims of improving the distribution uniformity of the carbide in the bearing steel and improving the product quality are fulfilled.

The method is used for pulse current treatment at normal temperature, does not need additional heat source assistance, is easy to implement, high in efficiency, green and pollution-free, and has obvious practical application value.

While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.