JP2024003804A - Inclusion evaluation method - Google Patents

Abstract

To provide an inclusion evaluation method which enables stable evaluation on a metal test piece having hardness less than HV400.SOLUTION: An inclusion evaluation method is provided, comprising: performing heat treatment on a metal test piece including nonmetallic inclusions of 10 μm or more in size to achieve hardness less than HV400; causing hydrogen to penetrate into the test piece with hardness less than HV400; performing a destructive test on the test piece penetrated with hydrogen to cause destruction of the test piece originating from the nonmetallic inclusions of 10 μm or more in size; and measuring dimensions of the nonmetallic inclusions that has originated the destruction.SELECTED DRAWING: Figure 5

Description

The present invention relates to an inclusion evaluation method for evaluating inclusions contained in a metal material.

It is known that non-metallic inclusions contained in metallic materials become the starting point of fatigue fracture. Therefore, it is important to evaluate nonmetallic inclusions contained in metallic materials.

As a conventional inclusion evaluation method, as in Patent Document 1, there is a method in which a tensile test as a destructive test is performed on a test piece made of a metal material into which hydrogen has penetrated. In this inclusion evaluation method, nonmetallic inclusions that are the origin of fracture are identified by a tensile test, and their dimensions are measured and evaluated.

In such conventional inclusion evaluation methods, hydrogen penetration tends to cause fractures originating from nonmetallic inclusions in a tensile test, and while it is possible to quickly evaluate nonmetallic inclusions, the stability of the evaluation is can also be secured.

However, test pieces made of metal materials with hardness of HV400 or higher are more likely to suffer fractures originating from non-metallic inclusions due to the intrusion of hydrogen. For this reason, the conventional inclusion evaluation method requires a large tensile machine for destructive tests such as tensile tests. For this reason, there has been a desire for a method that can easily perform destructive tests using smaller equipment.

Japanese Patent Application Publication No. 2009-65789

The problem to be solved is that a large testing machine was required for destructive testing.

The present invention provides a test piece made of a metal material containing non-metallic inclusions of 10 μm or more, heat-treated to have a hardness of less than HV400, hydrogen penetrated into the test piece having a hardness of less than HV400, and the hydrogen penetrated test piece. A method for evaluating inclusions, in which a destructive test is performed on the specimen, a fracture is caused in the test piece starting from the nonmetallic inclusion of 10 μm or more, and the size of the nonmetallic inclusion that is the origin of the fracture is measured. I will provide a.

In the present invention, since a destructive test is performed on a test piece made of a metal material having a hardness of less than HV400, the destructive test can be easily performed using a smaller testing machine.

FIG. 1 is a side view schematically showing a test piece used in an inclusion evaluation method according to an example of the present invention. FIG. 2 is a graph showing the relationship between the tempering temperature and the hardness of the test piece according to the example. FIG. 3 is a conceptual diagram showing hydrogen charging to a test piece according to an example. FIG. 4 is a conceptual diagram showing a tensile test on a test piece according to an example. FIG. 5 is a conceptual extreme value statistical graph of the dimensions of nonmetallic inclusions according to the example. FIG. 6 is a graph showing the distribution of equivalent circle diameters for test pieces with hardnesses of HV600, HV500, and HV370.

The purpose of the present invention is to easily perform a destructive test using a smaller testing machine, by heat treating a test piece made of a metal material containing non-metallic inclusions of 10 μm or more to a hardness of less than HV400, and by infiltrating hydrogen. This was achieved by conducting a destructive test.

That is, in the inclusion evaluation method, a test piece 3 made of a metal material containing a non-metallic inclusion 1 of 10 μm or more is heat-treated to have a hardness of less than HV400, and hydrogen is allowed to penetrate into the test piece 3 having a hardness of less than HV400. A destructive test is performed on the intruded test piece 3, a fracture is caused in the test piece 3 starting from a non-metallic inclusion 1 of 10 μm or more, and the size of the non-metallic inclusion 1 that is the origin of the fracture is measured. do.

In the inclusion evaluation method, the type of nonmetallic inclusion that is the origin of the fracture may be identified.

In addition, in the inclusion evaluation method, a distribution function of the dimensions of the non-metallic inclusion 1 that is the starting point of destruction may be determined, and the cleanliness of the metal material may be evaluated using this distribution function.

Moreover, the test piece 3 may have an unprocessed outer circumferential surface 3a that is cut out from a wire and constituted by the outer circumferential surface of the wire. In this case, the position of the nonmetallic inclusion 1, which is the starting point of the fracture, from the outer circumferential surface 3a of the test piece 3 is measured.

FIG. 1 is a side view schematically showing a test piece used in an inclusion evaluation method according to an example of the present invention.

In the inclusion evaluation method of this example, a test piece 3 made of a metal material containing a nonmetallic inclusion 1 (FIG. 4) of 10 μm or more is heat-treated to have a hardness of less than HV400.

The test piece 3 of this example is cut from a spring steel as a metal material, for example, a SAE9254 wire. This test piece 3 has a round bar shape with a circular cross section in accordance with the shape of the wire rod, and the outer circumferential surface 3a is an unprocessed surface that is the same as the outer circumferential surface of the wire rod. Both sides of the test piece 3 in the axial direction constitute gripping portions 4 . The axial direction refers to the direction along the axis of the test piece 3.

In this example, the axial length of the test piece 3 is 150 mm, the diameter of the test piece 3 is 9.8 mm, and the distance between gauges and the axial length of the grip portion 4 are each 50 mm.

However, the shape and size of the test piece 3 are not limited to this. For example, it may be a JIS No. 4 test piece. Further, the metal material may be other than spring steel as long as it contains non-metallic inclusions 1 of 10 μm or more.

Although it is unclear before applying the inclusion evaluation method whether the test piece 3 contains non-metallic inclusions 1 with a diameter of 10 μm or more, the tensile test described below shows that fracture occurs starting from the non-metallic inclusions 1. If so, nonmetallic inclusions 1 of 10 μm or more are included.

Any heat treatment may be used as long as the hardness of the test piece 3 is less than HV400, and appropriate heat treatment such as tempering, annealing, normalizing, quenching, etc. may be adopted depending on the metal material. The heat treatment in this example is tempering, and the test piece 3 having a hardness of HV400 or more is made to have a hardness of less than HV400.

FIG. 2 is a graph showing the relationship between tempering temperature and hardness of a test piece.

As shown in FIG. 2, when the test piece 3 is tempered at 400 degrees, 455 degrees, 580 degrees, and 700 degrees, the hardness of the test piece 3 becomes HV600, HV500, HV370, and HV280, respectively. In this example, the hardness of the test piece 3 is set to HV370 by tempering at 580 degrees. Tempering time is approximately 30 minutes. Note that the tempering time is just an example, and can be set as appropriate depending on the material, tempering temperature, hardness, etc. of the test piece 3. In FIG. 2, the straight line is an approximate straight line.

Note that the hardness of the test piece 3 only needs to be less than HV400, so it may be set to HV280, or it may be tempered at about 570 degrees based on an approximate straight line to bring it closer to HV400.

After the hardness of the test piece 3 is reduced to less than HV400 by heat treatment, hydrogen is allowed to penetrate into the test piece 3. In the following, the intrusion of hydrogen will be referred to as "hydrogen charging."

FIG. 3 is a conceptual diagram showing hydrogen charging to the test piece 3.

Hydrogen charging is performed, for example, by immersing the test piece 3 in a solution 5 for hydrogen charging for a predetermined period of time, as shown in FIG. For example, the test piece 3 is immersed in a 20 mass% ammonium thiocyanate aqueous solution at 50° C. for 48 hours.

Note that the hydrogen charging method is not limited to this, for example, a method of exposing the test piece 3 to hydrogen gas, a method of immersing it in an electrolytic solution such as an aqueous solution of sodium chloride and ammonium thiocyanate, an aqueous solution of sulfuric acid and arsenite, etc. There is a method of applying current while

Alternatively, the test piece 3 may be formed after hydrogen charging the metal material. In this case, the metal material before hydrogen charging is tempered to have an HV of less than 400.

When such hydrogen charging and tempering are performed on the test piece 3 containing nonmetallic inclusions 1 of 10 μm or more, the largest nonmetallic inclusion 1 in the test piece 3 of 10 μm or more will be removed in the next tensile test. Destruction at the starting point is more likely to occur.

The tensile test is performed on the hydrogen-charged test piece 3, and the test piece 3 is caused to fracture starting from the nonmetallic inclusions 1 of 10 μm or more. Note that the tensile test is preferably conducted after hydrogen charging, but may be conducted during hydrogen charging. Further, instead of the tensile test, other destructive tests such as a fatigue test or an impact test may be performed.

FIG. 4 is a conceptual diagram showing a tensile test on the test piece 3.

In this example, in the tensile test, both sides of the test piece 3 are gripped and pulled at a tensile speed of 20 mm/min to cause a fracture starting from a nonmetallic inclusion 1 of 10 μm or more between the gauge marks of the test piece 3. . Note that the fracture originating from the nonmetallic inclusion 1 refers to a fracture in which the nonmetallic inclusion 1, which is the origin of the fracture, is exposed on the fracture surface 7 of the test piece 3.

In such a tensile test, in this example, since the hardness of the test piece 3 before hydrogen charging is less than HV400, compared to the case where the hardness before hydrogen charging is HV400 or more, a tester (not shown) was used. The load on it is small. As a result, in cases where the hardness before hydrogen charging is HV400 or higher, the test can be easily performed using a smaller testing machine, or the testing machine can be protected.

After the test piece 3 is fractured, the type of nonmetallic inclusion 1 that caused the fracture is identified. The type of nonmetallic inclusions 1 in this example is Al--Ca--Si--Mg--O type. However, the type of nonmetallic inclusions 1 differs depending on the metal material.

Identification here refers to specifying the type of nonmetallic inclusion 1 with a certain degree of certainty. Therefore, in addition to direct identification by detecting the components of the nonmetallic inclusions 1, indirect identification is also possible.

In indirect identification, for example, a fatigue test is performed on a test piece 3 made from the same type of metal material in advance without hydrogen charging to identify the type of nonmetallic inclusion that was the origin of the fracture. The nonmetallic inclusions 1 obtained by the inclusion evaluation method of this example may be estimated to be the same type as the nonmetallic inclusions in the fatigue test.

In addition, when applying the inclusion evaluation method to multiple test pieces 3 of the same type, the components of nonmetallic inclusions 1 are detected for some of the test pieces 3, and the remaining test pieces 3 are detected as the starting point of fracture. It may be estimated that the nonmetallic inclusions 1 that have become the same as the nonmetallic inclusions 1 of some of the test pieces 3 whose components were detected.

Furthermore, when applying the inclusion evaluation method to multiple test pieces 3 of the same type, the distribution line 9 described later is obtained, the components of the nonmetallic inclusions 1 are detected for some of the test pieces 3, and the nonmetallic When the inclusion 1 is located in the confidence interval of the distribution straight line 9, the nonmetallic inclusions in the remaining test pieces 3 are of the same type as the nonmetallic inclusions 1 in some of the detected test pieces 3. It may be assumed that

Further, as long as the size of the nonmetallic inclusions 1 is 10 μm or more, it may be assumed that the nonmetallic inclusions 1 are of the same type. That is, in this example, it is also possible not to substantially identify the nonmetallic inclusions 1.

Before or after such identification, or instead of identification, after the test piece 3 is destroyed, the dimensions of the nonmetallic inclusions 1 are measured. In this example, the dimensions of the nonmetallic inclusions 1 are measured by observing the fracture surface using an electron microscope (SEM) and measuring the major axis, minor axis, and equivalent circle diameter.

The equivalent circle diameter refers to the diameter of a circle having the same area as the nonmetallic inclusion 1. Note that instead of the equivalent circle diameter, the average diameter of the major axis and the minor axis may be measured as the dimension of the nonmetallic inclusion 1.

In this way, in this example, it is possible to reliably measure the size of the largest non-metallic inclusion 1 in the test piece 3 that was the starting point of fracture, and it is possible to reliably measure the size of the largest non-metallic inclusion 1 in the test piece 3, which is the starting point of fracture. Stable evaluation can be performed.

Furthermore, in this example, the position of the largest nonmetallic inclusion 1 in the test piece 3, which was the starting point of fracture, from the outer circumferential surface 3a of the test piece 3 is measured. Note that this position is obtained as a distance in the radial direction. Here, the outer circumferential surface 3a of the test piece 3 is made of the outer circumferential surface of a wire rod. Therefore, in this embodiment, positional information of the nonmetallic inclusion 1 from the outer circumferential surface of the wire can be obtained. This positional information cannot be obtained by conventional methods of processing materials into test piece shapes that meet various standards.

In the evaluation of this example, a distribution function of the dimensions of the measured nonmetallic inclusions 1 is further determined, and the cleanliness of the metal material is evaluated using this distribution function. Specifically, a distribution straight line as a distribution function is determined using extreme value statistics.

In addition, when determining the distribution function, tempering, hydrogen charging, and tensile testing are performed on a plurality of test pieces 3, and the dimensions of the nonmetallic inclusions 1 that are the origin of fracture are measured. Then, as shown in Fig. 5, an extreme value statistical graph is generated in which the vertical axis is the cumulative probability and the horizontal axis is the equivalent circle diameter of the largest inclusion, and the dimensions of the nonmetallic inclusion 1 that is the origin of the fracture are plotted. . Note that FIG. 5 shows the extreme value statistical graph only conceptually.

Based on this extreme value statistical graph, a distribution line 9 as a regression line can be determined. By using this distribution straight line 9, the size of the largest nonmetallic inclusion 1 in the metal material can be predicted. In other words, the cleanliness of metal materials can be evaluated. The cleanliness refers to the degree of non-metallic inclusions 1 contained in the metal material. In this example, the cleanliness is determined based on the size of the largest nonmetallic inclusion 1 in the metal material.

In this manner, the inclusion evaluation method of this example allows accurate prediction of the largest nonmetallic inclusion 1, similar to the fatigue test. That is, in the inclusion evaluation method, a test piece 3 made of a metal material having a hardness of less than HV400 can be destroyed starting from the largest non-metallic inclusion 1 in the test piece 3. Then, by measuring the dimensions of the nonmetallic inclusions 1 that are the origin of the fracture, it becomes possible to perform stable evaluation.

FIG. 6 is a graph showing the distribution of equivalent circle diameters for test pieces 3 having hardnesses of HV600, HV500, and HV370.

FIG. 6 is a graph of the equivalent circular diameters of nonmetallic inclusions 1 measured by tempering, hydrogen charging, and tensile testing a plurality of test pieces 3 with hardnesses of HV600, HV500, and HV370. It is something. Note that the numbers of samples for HV600, HV500, and HV370 are 45, 15, and 10, respectively.

The vertical axis of FIG. 6 is the equivalent circle diameter, the horizontal axis is the hardness of the test piece 3, and the numerical values in the graph indicate the average value of the equivalent circle diameter. Furthermore, the error range in the graph indicates the range between the maximum value and the minimum value.

As shown in Fig. 6, the maximum value, minimum value, and average value of the dimensions of nonmetallic inclusions 1 are approximately the same in all of HV600, HV500, and HV370, and even under HV400, the maximum value in specimen 3 The measurement of non-metallic inclusions 1 is as stable as in the case of HV400 or higher.

In addition, in HV370, the maximum value of the dimension of the nonmetallic inclusion 1 is 43 μm, and the minimum value is 13 μm. If the size of the nonmetallic inclusion 1 is 13 μm to 43 μm, as in this HV370, even if the hardness of the test piece 3 is less than HV400, the fracture will be stable starting from the largest nonmetallic inclusion 1. It is possible to measure the dimensions of the non-metallic inclusion 1 which is the starting point.

This tendency can be seen in a range where the size of the nonmetallic inclusions 1 is 10 μm or more. There is no upper limit to the size of the non-metallic inclusions 1 as long as the non-metallic inclusions 1 can be included in the test piece 3, and although not shown, even if the size of the non-metallic inclusions 1 is 500 μm, the same A trend can be seen.

1 Nonmetallic inclusions 3 Test piece

However , positional information from the outer peripheral surface of the wire of the nonmetallic inclusion that was the origin of the fracture could not be obtained by conventional methods of processing materials into test piece shapes that meet various standards.

The problem to be solved is that positional information from the outer peripheral surface of the wire of nonmetallic inclusions that are the origin of fracture cannot be obtained by conventional methods of processing materials into test piece shapes that meet various standards.

The present invention involves infiltrating hydrogen into a test piece made of a metal material that is cut out from a wire rod containing non-metallic inclusions and having an outer peripheral surface made of the outer peripheral surface of the wire rod , and destroying the test piece into which the hydrogen has penetrated. Inclusion evaluation, in which a test is performed to cause fracture in the test piece starting from the non-metallic inclusion, and the position of the non-metallic inclusion that is the origin of the fracture from the outer circumferential surface of the test piece is measured. provide a method.

The present invention can obtain positional information from the outer circumferential surface of the wire of the nonmetallic inclusion that is the origin of the fracture .

Claims (4)

Hydrogen is introduced into a test piece made of a metallic material that is cut from a wire containing non-metallic inclusions and has an outer circumferential surface formed from the outer circumferential surface of the wire;
A destructive test is performed on the test piece into which the hydrogen has penetrated, and the test piece is caused to fracture starting from the non-metallic inclusion,
An inclusion evaluation method, comprising: measuring the position of a nonmetallic inclusion that is the origin of the fracture from the outer peripheral surface of the test piece. The inclusion evaluation method according to claim 1,
measuring the dimensions of the nonmetallic inclusion that became the origin of the destruction;
Inclusion evaluation method. The inclusion evaluation method according to claim 1,
identifying the type of nonmetallic inclusion that was the origin of the fracture;
Inclusion evaluation method. The inclusion evaluation method according to claim 2,
determining a distribution function of the dimensions of the nonmetallic inclusion that was the origin of the fracture, and evaluating the cleanliness of the metal material based on this distribution function;
Inclusion evaluation method.

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