CN113373392A - Method for generating reverse gradient structure on metal surface - Google Patents
Method for generating reverse gradient structure on metal surface Download PDFInfo
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- CN113373392A CN113373392A CN202110626844.7A CN202110626844A CN113373392A CN 113373392 A CN113373392 A CN 113373392A CN 202110626844 A CN202110626844 A CN 202110626844A CN 113373392 A CN113373392 A CN 113373392A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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Abstract
The invention discloses a method for generating an inverse gradient structure on a metal surface, which comprises the steps of firstly carrying out mechanical rolling treatment (SMRT) on the metal surface, generating a deformation area with a certain width on the metal surface, and generating different deformation amounts and different deformation degrees at different depths from the rolling surface according to the magnitude of rolling reduction. And then carrying out vacuum annealing treatment on the metal sample. Through the control of the rolling reduction, the surface deformation of the rolled metal sample is controlled to be 2% -10%, and the abnormal growth of crystal grains can occur in the metal material in the deformation area, so that a reverse gradient structure with the size of the metal surface crystal grains more than ten times of the size of the original core crystal grains is obtained.
Description
Technical Field
The invention belongs to the technical field of metal material surface treatment, and particularly relates to a method for generating an inverse gradient structure on a metal surface, namely a structure that the surface layer of a metal material is coarse grains and the core part of the metal material is fine grains.
Background
Gradient nanostructuring refers to a material in which structural units (e.g., grain size) of the material exhibit a gradient distribution in a certain spatial range, increasing from nanometer size to macroscopic size, i.e., a part consisting of nanocrystals and a part consisting of coarse crystals. The essence of this texture is that there is a gradient in the density of grain boundaries within the material. Traditionally, in most cases, the nanocrystals exist in the surface layer of the material, and the coarse crystallites exist in the core of the material, and the material with such a structure can usually exhibit good overall properties, such as excellent plasticity of the coarse crystallites in the core and excellent strength of the fine crystallites in the surface layer, so that the overall material has a great improvement in fatigue properties. However, the corrosion resistance and creep resistance of such structures at high temperatures are not effectively improved. Firstly, the grain boundary is more sensitive to the corrosion environment at high temperature, and the increase of the density of the grain boundary increases corrosion points, thereby accelerating the corrosion speed of the material; secondly, the grain boundary at high temperature is used as a defect, the strength of the material is reduced more quickly along with the rise of the temperature, and the high-temperature creep resistance of the fine-grained material is not as good as that of the coarse-grained material. In order to improve the corrosion resistance and creep resistance of the material at high temperature, the original strength and plasticity of the material are combined, and the traditional gradient structure of thin surface layer and thick core is converted into an 'inverse' gradient structure form, so as to meet the requirements of corrosion resistance and creep resistance improvement required by people.
At present, a great deal of research has provided methods for preparing a Surface gradient structure from a Surface layer to a core layer by using a metal Surface mechanical nano-technology, such as Surface mechanical grinding treatment (Surface mechanical abrasion treatment), Surface mechanical grinding treatment (Surface mechanical grinding treatment), and Surface mechanical rolling treatment (Surface mechanical rolling treatment). These techniques can refine the grain deformation at the surface while the core retains a coarse grain morphology. However, after the machining, a large amount of residual stress is present on the surface of the sample.
Disclosure of Invention
The invention aims to provide a method for generating an inverse gradient structure on the surface of metal so as to overcome the defects of the prior art, and the method can improve the high-temperature corrosion resistance and the high-temperature creep resistance of the material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for generating a reverse gradient structure on a metal surface comprises the steps of carrying out forced deformation treatment on the metal surface by using a rolling cutter, and then carrying out vacuum annealing on a sample subjected to the forced deformation treatment to form a reverse gradient structure with a thick surface and a thin core;
the method specifically comprises the following steps:
1) rolling and forcibly deforming the surface of the metal sample by utilizing the downward pressure of a rolling cutter, and withdrawing the cutter after corresponding rolling passes to form a deformation area on the surface layer of the metal;
2) and (3) carrying out vacuum annealing treatment on the rolled sample, namely heating the sample to a preset temperature in vacuum for heat preservation, and cooling the sample to room temperature along with the furnace after the heat preservation is carried out for a set time.
Further, the rolling cutter comprises a shell, a ball is embedded in the shell, a bearing is arranged inside the shell, the bearing is connected with the ball in a matched mode, and a cutter handle matched with a lathe for clamping is connected to the outer side of the shell.
Further, the bearing is made of GCr15 bearing steel.
Further, a lubricating oil hole is formed in the shell.
Further, the ball is a hard alloy ball with the diameter of 9 mm.
Further, the vacuum annealing treatment adopts a vacuum quartz tube.
Further, the metal is a Zr-4 alloy.
Further, the method specifically comprises the following steps:
1) taking that the ball of the rolling cutter just contacts the surface of the metal sample as a reference, and then performing rolling cutter pressing down with the rolling cutter pressing down amount of 0, wherein the rolling cutter pressing down amount is 2-5 mu m, and performing 1-pass rolling on the metal surface by adopting continuous feed;
2) and (3) carrying out vacuum tube sealing treatment on the metal sample after rolling, putting the sealed tube into a heating furnace which is heated to 700-900 ℃ for heating and heat preservation for 30-60min, and then cooling the furnace to room temperature.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention focuses more on forming coarse grains on the surface of a metal material, and utilizes a mechanical rolling technology to carry out continuous feed on the surface of the metal material, so that a deformation area with a certain range is formed on the surface of the metal material, grains grow up after the area is subjected to vacuum annealing treatment, and accordingly, coarse grains are generated on the surface layer, and the core part still maintains the inverse gradient structure characteristic of original fine grains. The structure can improve the high temperature corrosion resistance and high temperature creep resistance of the metal material, and the method has lower operation and processing cost and is a suitable production method.
Furthermore, the cutter used in the invention has the advantages of detachability, easy replacement of internal parts, convenient use and the like.
Zr-4 alloy is used for nuclear fuel cladding tubes because of its good corrosion resistance. By utilizing the method of generating the reverse gradient structure on the surface, the surface layer of the Zr-4 alloy can have coarse grains, so that the Zr-4 alloy has better high-temperature corrosion resistance.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is a schematic view of a rolling tool used for mechanically rolling a metal surface. Wherein, 1 is the ball, 2 is the bearing, 3 is the lubrication hole, 4 is the shell, 5 is the handle of a knife.
FIG. 2 is a schematic view showing the processing of a bar-shaped metal sample by mechanical rolling.
FIG. 3 is a schematic view of the sample after the tube sealing process.
FIG. 4 is a metallographic structure photograph of a Zr-4 generated surface reverse gradient structure;
FIG. 5 is a graph showing weight gain comparison of a Zr-4 alloy original tissue sample and a reverse gradient tissue sample after high temperature and high pressure corrosion;
FIG. 6 is a plot of a rate fit for a second phase of reverse gradient microstructure creep for a Zr-4 alloy, with the slope being the steady state rate;
FIG. 7 is a plot of a rate fit for the second phase of creep for the original structure of a Zr-4 alloy, with the slope being the steady state rate.
Detailed Description
The invention is described in further detail below:
a method for generating a reverse gradient structure on a metal surface comprises the steps of carrying out forced deformation treatment on the metal surface by using a rolling cutter, and then carrying out vacuum annealing on a sample subjected to the forced deformation treatment to form a reverse gradient structure with a thick surface and a thin core; the method specifically comprises the following steps:
1) rolling and forcibly deforming the surface of the metal sample by using the pressing of a rolling cutter, retracting the cutter after rolling for a plurality of times, forming a layer of deformation area on the surface layer of the metal, and controlling the surface deformation of the rolled metal sample to be 2-10% by controlling the reduction;
2) and (3) carrying out vacuum annealing treatment on the rolled sample, namely heating the sample to a preset temperature in vacuum for heat preservation, and cooling the sample to room temperature along with the furnace after the heat preservation is carried out for a set time.
The method utilizes a mode of carrying out vacuum annealing treatment after surface mechanical rolling to generate an inverse gradient structure on the surface of the zirconium alloy. The following will specifically describe the implementation process of the reverse gradient structure by taking the Zr-4 alloy as an example and combining with the accompanying drawings, and for other zirconium alloy series materials, the generation of the reverse gradient structure can be realized by changing the process parameters.
The rolling cutter shown in the attached figure 1 consists of 5 parts, and in the rolling process, the ball 1 realizes the contact rolling effect on a sample; the bearing 2 plays a role of supporting the ball 1 inside the housing 4; the shell 4 has a fixing function on the ball 1, and the top of the shell 4 is provided with a lubricating oil hole 3, so that the cutter can be supplied with oil in the working process; the rolling tool is held by the shank 5 on the lathe fixture during operation to support the operation of the rolling tool.
In the process of rolling the metal surface, the sample rotates along with the clamping end, the ball 1 contacts and presses the metal surface to also roll and feed along the axial direction of the sample, and the method ensures that the metal surface is mechanically rolled and improves the surface quality. The rolling cutter is lubricated to a certain extent through the lubricating oil hole while operating, and the jamming of the ball 1 is avoided.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
The method for mechanically rolling the metal surface by using the rolling cutter to form the deformation area comprises the following steps:
1) the annealed rod-shaped Zr-4 alloy having a diameter of 6.5mm was cut into small round rods having a length of 70mm to obtain original samples having an average crystal grain size of about 7 μm.
2) The small round bar sample shown in FIG. 2 was mounted on a common lathe and subjected to rolling treatment at room temperature under the following parameters: speed v of lathe1800 revolutions per minute, feed speed v210 mm/min. The amount of depression was 0 when the ball just contacted the sample, and on this basis, the cutter was depressed 3 μm using a dial gauge reading, and the sample surface was rolled 1 pass with continuous feed, and then withdrawn.
Performing tube sealing treatment on the rolled metal sample, as shown in FIG. 3, wherein the bottom of the vacuum quartz tube is arc-shaped, the outer diameter of the quartz tube is 11mm, the inner diameter of the quartz tube is 8.6mm, and the vacuum degree in the tube is pumped to 4.5 × 10-4And (6) sealing the pipe orifice after Pa, and putting the pipe orifice into a furnace for heating.
Annealing and heating the sealed sample, comprising the following steps:
1) heating an empty furnace of a common heating furnace to preheat, wherein the heating rate is 20 ℃/min, and the temperature is increased to 800 ℃.
2) And (3) putting the sealed sample into a heating furnace heated to 800 ℃, heating and preserving the temperature of the sample, closing a heating system of the heating furnace after 30 minutes to naturally reduce the temperature in the furnace, and taking out the sample after the sample is cooled to room temperature along with the furnace.
As shown in fig. 4, it is evident from the metallographic picture of the sample after vacuum annealing that a coarse grain region with a certain width is generated on the surface of the sample, which indicates that the grains in the region are annealed after rolling to generate recrystallization growth, and the growth degree is abnormally high. The grain size of the core is still comparable to the original grain size. The invention can generate a structure form of coarse grains with uniform structure on the surface of the metal, and the fine grains in the core part are combined to form an inverse gradient structure. The rolling parameters and the annealing parameters are test parameters of the Zr-4 alloy, and the parameters can be changed and adjusted according to the change of materials.
And (3) carrying out corrosion treatment on the sample after the reverse gradient tissue design and the original sample in a high-temperature and high-pressure water environment, wherein as shown in fig. 5, a black cylinder in the graph is the corrosion weight increase condition of the reverse gradient tissue sample, and the weight increase of the reverse gradient tissue sample after corrosion is smaller than that of the original tissue sample after corrosion. The performance of the high-temperature and high-pressure corrosion resistance of the reverse gradient structure is better than that of the original structure can be preliminarily judged.
And (3) carrying out high-temperature creep test on the sample after the reverse gradient tissue design and the original sample, wherein fig. 6 shows the fitting condition of the slope of the curve after the reverse gradient tissue sample enters a creep steady-state stage, and the slope is 0.00125. FIG. 7 shows a curve slope 0.00151 as it is fitted to the initial tissue specimen after it has entered the steady-state phase of creep. The comparison shows that the slope of the reverse gradient structure is smaller, the creep rate is slower, and the creep resistance is better than that of the original structure.
Example 2
The method for mechanically rolling the metal surface by using the rolling cutter to form the deformation area comprises the following steps:
1) the annealed rod-shaped Zr-4 alloy having a diameter of 6.5mm was cut into small round rods having a length of 70mm to obtain original samples having an average crystal grain size of about 7 μm.
2) The small round bar sample shown in FIG. 2 was mounted on a common lathe and subjected to rolling treatment at room temperature under the following parameters: speed v of lathe1800 revolutions per minute, feed speed v210 mm/min. The ball just contacts the sampleThe amount of pressing was measured as 0, and on the basis of this, the cutter was pressed down by 2 μm by the dial gauge reading, and the surface of the sample was rolled by 1 pass of continuous feed, followed by withdrawal of the cutter.
Performing tube sealing treatment on the rolled metal sample, as shown in FIG. 3, wherein the bottom of the vacuum quartz tube is arc-shaped, the outer diameter of the quartz tube is 11mm, the inner diameter of the quartz tube is 8.6mm, and the vacuum degree in the tube is pumped to 4.5 × 10-4And (6) sealing the pipe orifice after Pa, and putting the pipe orifice into a furnace for heating.
Annealing and heating the sealed sample, comprising the following steps:
1) heating an empty furnace of a common heating furnace to preheat, wherein the heating rate is 20 ℃/min, and the temperature is raised to 700 ℃.
2) And (3) putting the sealed sample into a heating furnace heated to 700 ℃, heating and preserving the temperature of the sample, closing a heating system of the heating furnace after 45 minutes to naturally reduce the temperature in the furnace, and taking out the sample after the sample is cooled to room temperature along with the furnace.
Example 3
The method for mechanically rolling the metal surface by using the rolling cutter to form the deformation area comprises the following steps:
1) the annealed rod-shaped Zr-4 alloy having a diameter of 6.5mm was cut into small round rods having a length of 70mm to obtain original samples having an average crystal grain size of about 7 μm.
2) The small round bar sample shown in FIG. 2 was mounted on a common lathe and subjected to rolling treatment at room temperature under the following parameters: speed v of lathe1800 revolutions per minute, feed speed v210 mm/min. The amount of depression was 0 when the ball just contacted the sample, and on this basis, the cutter was depressed 5 μm by dial gauge reading, and the sample surface was rolled 1 pass by continuous feed, followed by retracting.
Performing tube sealing treatment on the rolled metal sample, as shown in FIG. 3, wherein the bottom of the vacuum quartz tube is arc-shaped, the outer diameter of the quartz tube is 11mm, the inner diameter of the quartz tube is 8.6mm, and the vacuum degree in the tube is pumped to 4.5 × 10-4And (6) sealing the pipe orifice after Pa, and putting the pipe orifice into a furnace for heating.
Annealing and heating the sealed sample, comprising the following steps:
1) heating the empty furnace of a common heating furnace to preheat, wherein the heating rate is 20 ℃/min, and the temperature is increased to 900 ℃.
2) And (3) putting the sealed sample into a heating furnace heated to 900 ℃, heating and preserving the temperature of the sample, closing a heating system of the heating furnace after 60 minutes to naturally reduce the temperature in the furnace, and taking out the sample after the sample is cooled to room temperature along with the furnace.
The embodiments described above are merely preferred embodiments of the present invention, and should not be considered as limitations of the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (8)
1. A method for generating a reverse gradient structure on a metal surface is characterized in that a rolling cutter is utilized to carry out forced deformation treatment on the metal surface, and then a sample after the forced deformation treatment is subjected to vacuum annealing to form a reverse gradient structure with a thick surface and a thin core;
the method specifically comprises the following steps:
1) rolling and forcibly deforming the surface of the metal sample by utilizing the downward pressure of a rolling cutter, and withdrawing the cutter after corresponding rolling passes to form a deformation area on the surface layer of the metal;
2) and (3) carrying out vacuum annealing treatment on the rolled sample, namely heating the sample to a preset temperature in vacuum for heat preservation, and cooling the sample to room temperature along with the furnace after the heat preservation is carried out for a set time.
2. The method for generating the inverse gradient structure on the metal surface according to the claim 1 is characterized in that the rolling tool comprises a shell (4), a ball (1) is embedded on the shell (4), a bearing (2) is arranged inside the shell (4), the bearing (2) is connected with the ball (1) in a matching way, and a tool shank (5) which is clamped by a lathe is connected to the outer side of the shell (4).
3. A method of generating an inverse gradient structure on a metal surface according to claim 2, characterized in that the bearing (2) is made of GCr15 bearing steel.
4. A method for generating an inverse gradient structure on a metal surface according to claim 2, characterized in that the housing (4) is provided with lubrication holes (3).
5. A method for creating an inverse gradient structure on a metal surface according to claim 2, characterized in that the rolling balls (1) are cemented carbide balls with a diameter of 9 mm.
6. The method of claim 2, wherein the vacuum annealing process is performed using a vacuum quartz tube.
7. The method of claim 6, wherein the metal is a Zr-4 alloy.
8. The method for generating an inverse gradient structure on a metal surface according to claim 7, comprising the following steps:
1) taking the fact that the ball (1) of the rolling cutter just contacts the surface of the metal sample as a reference, wherein the rolling reduction of the rolling cutter is 0, then performing rolling of the rolling cutter, wherein the rolling reduction is 2-5 mu m, and performing 1-pass rolling on the surface of the metal by adopting continuous feed;
2) and (3) carrying out vacuum tube sealing treatment on the metal sample after rolling, putting the sealed tube into a heating furnace which is heated to 700-900 ℃ for heating and heat preservation for 30-60min, and then cooling the furnace to room temperature.
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| CN202110626844.7A CN113373392A (en) | 2021-06-04 | 2021-06-04 | Method for generating reverse gradient structure on metal surface |
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| CN202110626844.7A CN113373392A (en) | 2021-06-04 | 2021-06-04 | Method for generating reverse gradient structure on metal surface |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166605A (en) * | 2021-12-07 | 2022-03-11 | 安徽林洪重工科技有限公司 | Method for simulating and predicting core structure performance of large-size CrMo steel component |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10249580A1 (en) * | 2002-10-24 | 2004-05-19 | Friedr. Gustav Theis Kaltwalzwerke Gmbh | Process for improving the surface quality of titanium and titanium alloys comprises hydrating the surface and oxidizing annealing |
| CN103305671A (en) * | 2013-05-17 | 2013-09-18 | 西安交通大学 | Method for performing gradient nano-crystallization on surface of metal |
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2021
- 2021-06-04 CN CN202110626844.7A patent/CN113373392A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10249580A1 (en) * | 2002-10-24 | 2004-05-19 | Friedr. Gustav Theis Kaltwalzwerke Gmbh | Process for improving the surface quality of titanium and titanium alloys comprises hydrating the surface and oxidizing annealing |
| CN103305671A (en) * | 2013-05-17 | 2013-09-18 | 西安交通大学 | Method for performing gradient nano-crystallization on surface of metal |
Non-Patent Citations (1)
| Title |
|---|
| CHAO XIN ET AL: ""Thermal stability of nanogradient microstructure produced by surface mechanical rolling treatment in Zircaloy-4"", 《J MATER SCI》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166605A (en) * | 2021-12-07 | 2022-03-11 | 安徽林洪重工科技有限公司 | Method for simulating and predicting core structure performance of large-size CrMo steel component |
| CN114166605B (en) * | 2021-12-07 | 2024-03-29 | 安徽林洪重工科技有限公司 | Method for simulating and predicting core tissue performance of large-size CrMo steel member |
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Application publication date: 20210910 |