CN115354274A - Dynamic microwave thermal shock method for modifying alloy surface layer, application and workpiece - Google Patents
Dynamic microwave thermal shock method for modifying alloy surface layer, application and workpiece Download PDFInfo
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- CN115354274A CN115354274A CN202210995675.9A CN202210995675A CN115354274A CN 115354274 A CN115354274 A CN 115354274A CN 202210995675 A CN202210995675 A CN 202210995675A CN 115354274 A CN115354274 A CN 115354274A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
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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
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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
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/30—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes using a layer of powder or paste on the surface
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Abstract
The invention discloses a dynamic microwave thermal shock method for modifying an alloy surface layer, application and a workpiece, belonging to the field of modification of alloy surface layer materials and comprising the following steps of: coating the alloy surface layer with the alloy elements to be infiltrated, and then carrying out dynamic microwave thermal shock at different adjustable thermal shock heating rates to infiltrate the external alloy elements into the alloy matrix so as to realize the modification of the alloy surface layer. The method infiltrates alloy elements in a dynamic microwave thermal shock mode to realize low-cost and high-efficiency modification of the alloy surface layer.
Description
Technical Field
The invention belongs to the field of modification of alloy surface layer materials, and particularly relates to a dynamic microwave thermal shock method for modifying an alloy surface layer, application and a workpiece.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
Surface modification techniques are a class of thermal treatment techniques that employ chemical or physical methods to alter the chemical composition or texture of a material or workpiece surface to improve the performance of a machine part or material. It includes chemical heat treatment, surface coating and non-metal coating technology. The techniques for strengthening the surface of the part or material endow the part with various new functional characteristics of corrosion resistance, wear resistance, fatigue resistance, radiation protection, electric conduction, magnetic conduction and the like, and have great economic significance and popularization value.
The surface modification method is a method for attaching a layer of new material on the surface layer, namely, the surface coating technology, such as low-pressure plasma spraying, low-pressure arc spraying, laser remelting compounding and other thin film coatings, physical vapor deposition, chemical vapor deposition and other non-metal coating technologies, can be used for realizing the surface modification of the material, endows the surface of the material with various new characteristics, and has great economic significance and popularization value. However, the surface modification of the additional material is prone to the problem of low layer-to-layer adhesion.
The other is to introduce external elements into the alloy matrix to change the chemical composition, phase composition, crystal structure, intercrystalline inclusion, pore space, grain size, lattice orientation, phase change and other factors of the surface layer of the material, thereby changing the physical and mechanical properties of the alloy material, namely chemical heat treatment, and finally realizing the surface modification of the material with different purposes and different degrees. For example, the modification of the alloy is realized by ion implantation, carburizing and nitriding, metallurgical smelting integral modification and other modes, but the modification basically needs precise and complex equipment, and has low efficiency and high cost;
in addition, the surface layer of the alloy is modified by adopting a vibration mode, on one hand, the vibration belongs to a pretreatment mode before heating, which is equivalent to that not only heating treatment but also vibration in advance is needed, the time consumption is 20 hours at most, and the whole time is too long by adding subsequent heat treatment for 24 hours at most; on the other hand, the vibration method is liable to cause the thickness of the modified layer to be uneven because the layer thickness is uneven, the particle diameters for vibration are different, and the sample cannot be uniformly impacted in every portion.
Disclosure of Invention
Aiming at the problems of low efficiency and high cost in the process of introducing external elements to change factors such as chemical compositions, crystal structures, intercrystalline inclusions, gaps, phase changes and the like of a material surface layer in the prior art, the invention aims to provide a dynamic microwave thermal shock method, application and a workpiece for modifying an alloy surface layer.
In order to achieve the purpose, the invention is realized by the following technical scheme:
in a first aspect, the present invention provides a dynamic microwave thermal shock method for modifying an alloy surface layer, comprising the steps of:
coating the alloy surface layer with the alloy elements to be infiltrated, and then carrying out dynamic microwave thermal shock at different adjustable thermal shock heating rates to infiltrate the external alloy elements into the alloy matrix so as to realize the modification of the alloy surface layer.
As a further technical scheme, when the alloy is subjected to dynamic microwave thermal shock, the alloy with the surface coated with the alloy elements is placed in a cavity of dynamic microwave thermal shock equipment.
As a further technical scheme, the dynamic microwave thermal shock equipment is a microwave muffle furnace, the cavity is a ceramic fiber cavity, and the inner wall of the ceramic fiber cavity is coated with a wave-absorbing material.
As a further technical scheme, when the dynamic microwave thermal shock treatment is adopted, the thermal shock heating rate is between 25 ℃/min and 200 ℃/min.
As a further technical scheme, before coating, the modification thickness of the alloy surface layer and the dynamic microwave thermal shock heating rate of the alloy elements required to be infiltrated are determined.
As a further technical scheme, modification thickness and the amount of the alloy elements infiltrated are determined by calculating simulation software based on the first principle.
As a further technical scheme, in the dynamic microwave thermal shock process, the set modification thickness and the alloy element infiltration amount are obtained by optimizing dynamic shock process parameters; in the process, after the modification thickness and the amount of the alloy elements to be infiltrated are determined by first-principle calculation simulation software, the optimal process parameters are obtained through test data.
As a further technical scheme, after the modification is finished, the modified layer on the surface layer of the workpiece material is observed.
As a further technical scheme, the diffusion layer and the intermetallic compound are observed under a back scattering lens by adopting an electron microscope.
In a second aspect, the invention also provides an application of the dynamic microwave thermal shock method for modifying the alloy surface layer in regulating the alloy metal part compound and magnetism.
In a third aspect, the invention also provides a workpiece obtained by the dynamic microwave thermal shock method for modifying the alloy surface layer.
The beneficial effects of the invention are as follows:
the method of the invention treats the alloy surface layer coated with the alloy element to be infiltrated by a dynamic microwave thermal shock mode, can realize the controllable adjustment of the chemical composition, the crystal structure, the intercrystalline inclusion, the gap and the phase change of the material surface layer, has simple and high-efficiency treatment method and low cost, and does not need precise and expensive equipment.
According to the method, elements are infiltrated into the alloy surface layer under dynamic microwave thermal shock, an infiltration expanding layer is formed near the surface layer, an obvious intermetallic compound is formed at a crystal boundary, a new microstructure structure is endowed to a workpiece, and the modification of the workpiece surface layer is realized. The method can quantitatively control the thickness of the modified layer according to the temperature rise rate of the dynamic microwave thermal shock.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary 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 flow diagram of a dynamic microwave thermal shock method for alloy surface modification in accordance with one or more embodiments of the present invention;
fig. 2 is a schematic diagram of a mechanism of performing dynamic microwave thermal shock on a workpiece made of a nickel-based alloy Inconel 718 according to an embodiment of the present invention;
FIG. 3 is a diagram of atom migration and infiltration mechanism after dynamic microwave thermal shock is performed on a workpiece made of a nickel-based alloy Inconel 718 according to an embodiment of the present invention;
FIG. 4 is a microstructure diagram of a surface layer of a workpiece made of a nickel-based alloy Inconel 718 according to example 1 of the present invention after dynamic microwave thermal shock;
in the figure: the spacing or size between each other is exaggerated to show the location of the locations, and the illustration is for illustrative purposes only.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Research shows that for alloy materials, factors influencing element infiltration mainly include temperature, time, oxygen concentration in the environment and the like. For difficult-to-process materials such as plastic materials (nickel-based alloy and titanium alloy) and brittle materials (ceramics, semiconductors and single crystals), the prior art needs to adopt an ion-permeation technology to permeate other elements (such as sulfur element) into the alloy surface layer to change the surface layer structure of the material, and the ion-permeation technology has higher requirements on equipment, higher equipment investment cost and low efficiency.
In a typical embodiment of the present invention, as shown in fig. 1, a dynamic microwave thermal shock method for modifying an alloy surface layer is provided, in which an alloy surface layer is coated with an alloy element to be infiltrated, and then dynamic microwave thermal shock is performed at different adjustable thermal shock heating rates, so that an external alloy element is infiltrated into an alloy substrate, thereby modifying the alloy surface layer.
Pretreatment is not needed in the process of the scheme, so that the time and the cost are greatly saved; and the modified layer obtained by a thermal shock mode has high uniformity and consistent thickness.
When the alloy is subjected to dynamic microwave thermal shock, the alloy with the surface coated with the alloy elements is placed in a ceramic fiber cavity, and the inner wall of the ceramic fiber cavity is coated with a special wave-absorbing material.
In the embodiment, the wave-absorbing material is formed by superposing a composite wave-absorbing heat-conducting material with a carbon fiber heat-conducting gasket as an inner layer, and is mainly used for absorbing heat generated by microwaves so as to quickly raise the temperature in the cavity.
When the alloy is subjected to dynamic microwave thermal shock treatment, external alloy elements are infiltrated into the alloy matrix to form a diffusion layer, the size and orientation of crystal grains can be adjusted, and further surface layer modification is realized.
The dynamic microwave thermal shock in the method means that the thermal shock heating rate is controllable and can be randomly adjusted within the rate of 200 ℃/min, and meanwhile, the whole heating process is dynamic. The temperature raising stage is also a temperature raising stage which can be set to different rates and can be adjusted freely according to requirements.
In the whole process, the thermal shock heating rate is carried out at a high heating rate, and can be adjusted according to materials and requirements.
When the dynamic microwave thermal shock technology is adopted for treatment, the selectable thermal shock heating rate is between 25 ℃/min and 200 ℃/min, the surface layer modification can be quickly realized, the element infiltration, the new intercrystalline phase formation and the crystalline grain adjustment can be completed only in a short time, and the requirement on equipment is low.
The method comprises the following specific steps:
(1) Determining the modification thickness of the alloy surface layer and the dynamic microwave thermal shock heating rate of the alloy element required to be infiltrated according to the modification requirement of the alloy surface layer;
(2) Uniformly coating the element to be infiltrated on the surface of the alloy, then placing the alloy in a cavity of dynamic microwave thermal shock equipment, wherein the cavity is made of ceramic fiber, the inner layer is coated with a special wave-absorbing heating material, and the alloy is heated by absorbing microwaves while allowing the microwaves to pass through;
(3) Obtaining the set modification thickness and the alloy element infiltration capacity by adopting optimized dynamic impact process parameters;
(4) And observing the surface modified layer of the workpiece material.
In the step (1), the modification thickness and the thermal shock heating rate are determined by utilizing a first principle, an element diffusion kinetic theory and first principle calculation simulation software VASP or WIEN2k (or other software with similar simulation functions).
The alloy surface layer modification requirement refers to the thickness of the element required to be infiltrated, and the corresponding infiltration thickness can be obtained after calculation according to the diffusion activation energy and the element characteristics of each element and the first principle; the thermal shock heating rate is controlled by a PLC program of the device, thermocouple temperature measuring devices are distributed in the heating cavity, after the heating rate is set, the thermocouples feed back the temperature of the PLC controller in real time, and the controller adjusts the power of the microwave generator in due time, so that the control of the heating rate is realized.
In some embodiments, in step (2), the dynamic microwave thermal shock apparatus is a microwave muffle furnace.
In the step (3), the process parameters can be obtained by depending on test data, and the optimal infiltration thickness is obtained by testing different heating rates. Meanwhile, simulation means such as calculation based on a first principle and the like can predict the thickness of the modified layer and the required element infiltration amount which are possibly obtained by the corresponding process parameters to a certain extent, and then the optimal process parameters are obtained through a plurality of tests.
Under the combined action of microwave and heat, the element reacts with the alloy matrix by virtue of the electronegativity and the activation energy of the element, and diffuses into the matrix to form a modified layer.
In the step (4), an electron microscope is adopted under a back scattering lens, so that an obvious diffusion layer and an intermetallic compound can be observed.
In an alternative embodiment, the thermal shock ramp rate is 100 deg.C/min.
In some embodiments, the alloys include various types of alloys, such as iron-based alloys, cobalt-based alloys, nickel-based alloys, and the like.
In one or more embodiments, the nickel-based alloy is a nickel-based superalloy, inconel 718.
After the dynamic microwave thermal shock treatment, the crystal structure (including the grain size of the surface layer, intermetallic compounds, phase change and the like) of the surface layer of the sample is changed, so that the surface layer generates an diffusion layer, the original phase is converted into the intermetallic compounds, magnetism is generated, the magnetism conversion can be realized, and the surface layer modification of the material is realized.
In the present embodiment, the alloying element to be infiltrated may be a tellurium element.
The modification of the alloy surface layer can be effectively realized by adopting a dynamic microwave thermal shock technology. The microstructure of the alloy surface layer is obviously changed, the element infiltration phenomenon is obvious, and obvious intermetallic compounds are generated.
In the method, the method of infiltrating the alloy elements into the alloy surface layer by adopting microwave dynamic thermal shock has two main action mechanisms, namely, the temperature is quickly raised after the wave absorption of the inner cavity material, and the infiltration of the elements can be promoted by the internal high temperature; secondly, a part of the microwaves emitted by the microwave generator are absorbed by the wave-absorbing material in the inner cavity for heating, and the other part of the microwaves directly act on the alloy matrix and the elements to be infiltrated on the surface layer, so that the action of the microwaves is accelerated, the whole alloying element infiltration process is improved, and the alloying element infiltration process is more convenient, quicker and more effective.
In another exemplary embodiment of the present invention, the application of the above-mentioned dynamic microwave thermal shock method for alloy surface modification to adjust alloy metallic part composition and magnetism is provided.
In a further exemplary embodiment of the invention, a workpiece is provided, which is obtained by the dynamic microwave thermal shock method for modifying the surface layer of an alloy as described above.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
The alloy material adopted in the embodiment is nickel-based superalloy Inconel 718.
The thickness of the alloying layer is controlled to be 150 mu m, simulation software VASP is calculated by utilizing a first principle to carry out simulation, and the simulation result is as follows: tellurium element solid powder is selected as an alloy element to be infiltrated. Uniformly coating tellurium element solid powder on a high-temperature alloy material, placing the high-temperature alloy material in a microwave muffle furnace, heating to 1000 ℃ at the heating rate of 100 ℃/min, and then directly cooling by air, so that a 150-micron-thick diffusion layer, intermetallic compound distribution along a grain boundary and magnetic transformation can be realized.
The mechanism of this embodiment is shown in fig. 3, and fig. 3 shows that the element to be infiltrated and the original metal element in the matrix form a new intercrystalline compound and form an infiltration spreading layer.
The section of the sample of this example after the surface layer is permeated with tellurium element is shown in fig. 4, and the result is obtained under the condition of direct air cooling after the temperature is raised to 1000 ℃ under the dynamic microwave thermal shock of 100 ℃/min; wherein, the oxide layer is a surface oxide formed by direct air cooling after dynamic thermal shock, and the layer is easy to peel off; in the figure, white substances distributed along the grain boundary in the diffusion layer are newly generated intergranular compounds, and are formed by that the atoms which are permeated migrate along the grain boundary under the dynamic microwave thermal shock and are combined with the original metal atoms.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A dynamic microwave thermal shock method for modifying an alloy surface layer is characterized by comprising the following steps:
coating the alloy surface layer with the alloy elements to be infiltrated, and then carrying out dynamic microwave thermal shock at different adjustable thermal shock heating rates to infiltrate the external alloy elements into the alloy matrix so as to realize the modification of the alloy surface layer.
2. The dynamic microwave thermal shock method for modifying the surface of an alloy as claimed in claim 1, wherein the alloy with the surface coated with the alloy element is placed in a cavity of a dynamic microwave thermal shock device when the alloy is subjected to dynamic microwave thermal shock.
3. The method of claim 1, wherein the dynamic microwave thermal shock device is a microwave muffle furnace, the chamber is a ceramic fiber chamber, and the inner wall of the ceramic fiber chamber is coated with a wave absorbing material.
4. The dynamic microwave thermal shock method for alloy surface modification according to claim 1, wherein the thermal shock heating rate is between 25 ℃/min and 200 ℃/min when the dynamic microwave thermal shock treatment is adopted.
5. The dynamic microwave thermal shock method for modifying an alloy surface layer according to claim 1, wherein before coating, the modification thickness of the alloy surface layer and the temperature rise rate of the dynamic microwave thermal shock required to be infiltrated with the alloy element are determined.
6. The dynamic microwave thermal shock method for alloy surface modification of claim 5 where the modification thickness and the amount of alloying elements that penetrate are determined based on first-order-principle computational simulation software.
7. The dynamic microwave thermal shock method for modifying the surface layer of the alloy as claimed in claim 1, wherein in the dynamic microwave thermal shock process, the set modification thickness and the infiltration amount of the alloy element are obtained by optimizing the technological parameters of dynamic shock; in the process, after the modification thickness and the amount of the alloy elements to be infiltrated are determined by first-principle calculation simulation software, the optimal process parameters are obtained through test data.
8. The dynamic microwave thermal shock method for alloy surface modification of claim 1 where after modification is completed, the workpiece material surface modification layer is observed.
9. Use of a dynamic microwave thermal shock method for modifying the surface of an alloy according to any one of claims 1 to 8 for modifying the composition and magnetic properties of alloy-metal parts.
10. Workpiece obtained by the dynamic microwave thermal shock method for the modification of the surface layer of an alloy according to any one of claims 1 to 8.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5154779A (en) * | 1990-04-20 | 1992-10-13 | Martin Marietta Energy Systems, Inc. | Method of nitriding, carburizing, or oxidizing refractory metal articles using microwaves |
| CN101565810A (en) * | 2009-06-09 | 2009-10-28 | 天津大学 | Preparation method and device for industrial microwave heating diffusion coating |
| CN101565811A (en) * | 2009-06-09 | 2009-10-28 | 天津大学 | Processing method of fast slurry zinc impregnation and zinc/aluminum common impregnation coating |
| CN108581057A (en) * | 2018-05-04 | 2018-09-28 | 山东大学 | A kind of surface layer alloying Weakening treatment assistance processing method for difficult-to-machine material high-efficient cutting |
| CN112239842A (en) * | 2020-10-12 | 2021-01-19 | 山东大学 | Surface layer tellurium infiltration weakening auxiliary processing method for nickel and chromium alloy cutting |
-
2022
- 2022-08-18 CN CN202210995675.9A patent/CN115354274A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5154779A (en) * | 1990-04-20 | 1992-10-13 | Martin Marietta Energy Systems, Inc. | Method of nitriding, carburizing, or oxidizing refractory metal articles using microwaves |
| CN101565810A (en) * | 2009-06-09 | 2009-10-28 | 天津大学 | Preparation method and device for industrial microwave heating diffusion coating |
| CN101565811A (en) * | 2009-06-09 | 2009-10-28 | 天津大学 | Processing method of fast slurry zinc impregnation and zinc/aluminum common impregnation coating |
| CN108581057A (en) * | 2018-05-04 | 2018-09-28 | 山东大学 | A kind of surface layer alloying Weakening treatment assistance processing method for difficult-to-machine material high-efficient cutting |
| CN112239842A (en) * | 2020-10-12 | 2021-01-19 | 山东大学 | Surface layer tellurium infiltration weakening auxiliary processing method for nickel and chromium alloy cutting |
Non-Patent Citations (1)
| Title |
|---|
| GUOYING LI: "Enhancement of Te infiltration into Inconel 718 surface layer through dynamic microwave thermal shock", APPLIED SURFACE SCIENCE, pages 2 - 7 * |
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