CN110823768A - Device and method for researching interface compatibility of solid material - Google Patents

Device and method for researching interface compatibility of solid material Download PDF

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Publication number
CN110823768A
CN110823768A CN201911149936.XA CN201911149936A CN110823768A CN 110823768 A CN110823768 A CN 110823768A CN 201911149936 A CN201911149936 A CN 201911149936A CN 110823768 A CN110823768 A CN 110823768A
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end plug
solid material
object bearing
solid
bearing cylinder
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CN110823768B (en
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张翔
潘小强
杨静
刘羽
曾强
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Nuclear Power Institute of China
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Nuclear Power Institute of China
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N2013/003—Diffusion; diffusivity between liquids

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention discloses a device for researching interface compatibility of a solid material, wherein a material for preparing a diffusion couple is contained in a material bearing cylinder, and an end plug is fixedly welded through girth welding after being connected with an open end at the top of the material bearing cylinder through threads; the end plugs are used for compressing the solid materials for preparing the diffusion couples, so that the interfaces of the materials for preparing the diffusion couples are always kept in compression fit; the end plug is provided with a micropore for vacuumizing the object bearing cylinder, and after vacuumizing is finished, micropore vacuum sealing is realized through hole plugging welding. The method for researching the interface compatibility of the solid material can obtain the thermal diffusion and interface reaction conditions of the solid interface under the vacuum condition, is simple and practical to operate, has wide applicability, and can be widely applied to the research of the interface compatibility of the solid material.

Description

Device and method for researching interface compatibility of solid material
Technical Field
The invention relates to the technical field of material performance detection, in particular to a device and a method for researching interface compatibility of a solid material.
Background
The compatibility of two solid materials is generally determined by studying the thermal diffusion and chemical reaction conditions of diffusion couple interfaces of the two solid materials, and in the process of designing and selecting nuclear power materials, the two solid materials are often contacted with the conditions that the two materials are tightly attached and serve at a certain temperature, such as core block and cladding materials, coating and cladding materials and the like, the compatibility between the materials is a key factor which needs to be considered in material design and research, and the compatibility is usually required to be tested and verified in the prior period. To study the interfacial compatibility between materials, it is necessary to obtain an interface where two materials are tightly adhered, and perform heat treatment on the interface at a specific temperature and for a specific duration under a protective or vacuum condition to obtain the interfacial diffusion and reaction conditions.
At present, the preparation of the diffusion couple is carried out in a vacuum heat treatment furnace by a binding method, a riveting method, a mixed briquetting method, a coating method, a cladding hot pressing method and the like, or the vacuum heat treatment is carried out in a vacuum heat treatment furnace, or the atmosphere protection or vacuum condition is achieved through a quartz sealed tube, the preparation process is complex, and the control of the interface bonding of the diffusion couple is not accurate enough. According to the forming rule and mechanism of the Al/Mg diffusion layer, the Songhe strong and the like adopt an embedded diffusion couple, Al and Mg metals are embedded and processed together, and the interface diffusion condition is observed by an electron microscope after heat preservation at 580 ℃ for 60 hours of annealing treatment. The diffusion couple is prepared by putting metal and ceramic in contact with each other and then putting the metal and the ceramic in powder to be coated and hot-pressed.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the conventional diffusion couple preparation device is complex in structure and operation flow, and is particularly not suitable for scientific research in laboratories.
The invention is realized by the following technical scheme:
the device for researching the interface compatibility of the solid material comprises a material bearing barrel and an end plug, wherein the material for preparing the diffusion couple is contained in the material bearing barrel, and the end plug is fixedly connected with the top open end of the material bearing barrel through girth welding after being connected through threads; the end plugs are used for compressing the solid materials for preparing the diffusion couples, so that the interfaces of the materials for preparing the diffusion couples are compressed and attached; the end plug is provided with a micropore for vacuumizing the object bearing cylinder, and after vacuumizing is finished, micropore vacuum sealing is realized through hole plugging welding. The object bearing barrel with corresponding height can be selected according to the thickness of the diffusion couple; the solid material can adopt binary or ternary solid material according to the requirement.
Furthermore, one end of the end plug is provided with an external thread, an open top end of the object bearing barrel is provided with an internal thread, and one end of the end plug is screwed into the object bearing barrel through the internal thread and the external thread in a matching mode.
Further, the micropores comprise a small pore section and a large pore section, and the inner diameter of the large pore section is larger than that of the small pore section; one end of the big hole section is communicated with the object bearing cylinder, and the other end is communicated with the small hole section.
A method for researching the interfacial compatibility of solid materials is operated by the device for researching the interfacial compatibility of the solid materials, and comprises the following steps:
step 1, superposing a solid material I and a solid material II into a material bearing cylinder,
step 2, connecting the end plug with the open end of the object bearing barrel in a vacuum sealing manner;
step 3, vacuumizing the interior of the object bearing cylinder through the micro hole on the end plug;
step 4, after vacuumizing, vacuum sealing the micropores, and after nondestructive leakage detection, achieving a vacuum environment in the object bearing cylinder;
step 5, carrying out heat treatment on the whole device;
and 6, separating the end plug and the object bearing barrel, and taking out the diffusion couple for interface analysis and test.
Further, in the step 2, the end plug is screwed at the open end of the object bearing barrel through threaded connection, and the solid material I and the solid material II are compressed through the end face of the end plug, so that the interfaces of the solid material I and the solid material II are kept in positive pressure fit; and then the end plug is connected with the gap of the object bearing cylinder and the end plug through girth welding, so that the vacuum sealing connection of the end plug and the open end of the object bearing cylinder is realized.
Further, step 4, the vacuum sealing of the micropore is realized through hole plugging welding, and the vacuum environment is achieved in the object bearing cylinder after nondestructive leakage detection.
Further, in the step 3, the vacuum is pumped to ensure that the inner part of the object bearing cylinder reaches less than 1 multiplied by 10-2Pa, vacuum state.
Further, in the step 5, the whole device is placed in a heat treatment furnace for heat treatment.
The invention has the following advantages and beneficial effects:
1. the invention aims to provide a device for preparing a solid material diffusion couple, and the device is used for researching the interfacial compatibility and the diffusion condition of a solid material. The pressure fit of the diffusion couple interface of the solid material is obtained through the device, and the effective interface diffusion and reaction state among the materials are obtained through heat treatment at a specific temperature and for a specific duration after the interior of the device is vacuumized and sealed, so that the compatibility of the solid material at a certain temperature is judged.
2. The design of the invention realizes simple preparation of the solid material diffusion couple, quickly realizes pressure contact of the solid material attaching interface, ensures the effectiveness of interface diffusion and reaction of the solid material in a vacuum environment, can obtain the thermal diffusion and interface reaction conditions of the solid interface in a vacuum condition, has simple and practical operation, wide applicability and popularization value, and is mainly used in laboratory research in colleges, scientific research institutions and the like.
3. The invention provides a device for researching the interface compatibility of a solid material, which has the advantages of simple structure, lower cost and convenient operation, and can be repeatedly recycled after a diffusion couple is processed and taken out.
Patent CN201510664689, a method for preparing metal-ceramic diffusion couple this way of obtaining solid diffusion couple by hot pressing and powder coating requires hot pressing equipment and active powder, is not easy to implement, and powder easily enters into the interface during powder laying, causing separation of the diffusion couple interface or doping impurities, affecting the diffusion result. Patent CN201811254061, a metal solid diffusion device, is relatively complex, and its sample is put into a mold by smelting and suction casting, which has certain limitations for sample preparation.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the invention and together with the description serve to explain the principles of the invention. In the drawings:
fig. 1 is a front view of an apparatus for investigating interfacial compatibility of solid materials according to the present invention.
FIG. 2 is a diffusion couple interface diffusion electron microscope image obtained by the present invention.
Reference numbers and corresponding part names in the drawings: 1-micropore, 2-end plug, 3-end plug external thread, 4-object bearing barrel internal thread, 5-solid material I, 6-solid material II, 7-object bearing barrel.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example 1
The embodiment provides a device for researching interfacial compatibility of solid materials, which comprises a material bearing barrel 7 and an end plug 2, wherein the material of the material bearing barrel 7 and the material of the end plug 2 are stainless steel or high-temperature resistant materials, the material bearing barrel 7 with corresponding height can be selected according to the thickness of a diffusion couple, and the material bearing barrel 7 is of a cylinder structure with a closed bottom end and an open top end. The object bearing barrel 7 is used for containing a solid material I5 and a solid material II6 for preparing a diffusion couple, the end plug 2 is fixedly connected with the open top end of the object bearing barrel 7 through girth welding after being connected through threads, and the end plug 2 is used for compressing the solid material I5 and the solid material II6 and enabling the interface of the solid material I5 and the solid material II6 to be compressed and attached; the end plug 2 is provided with a micropore 1 for vacuumizing the interior of the object bearing barrel 7, and after vacuumizing is finished, vacuum sealing of the micropore 1 is realized through hole plugging welding.
Example 2
Further improve on embodiment 1's basis, end plug 2 includes horizontal segment and vertical section, and the horizontal segment is the external diameter and holds the plectane structure that thing section of thick bamboo 7 external diameter is the same, and the vertical section is cylinder straight-bar structure, and horizontal segment and vertical section mutually perpendicular set up are T type structure on vertical section axial cross-section. The free end of the vertical section of the end plug 2 is provided with an external thread, the open end at the top of the object bearing barrel 7 is provided with an internal thread, the free end of the vertical section of the end plug 2 is screwed into the object bearing barrel 7 through the internal thread and the external thread in a matching way until the end surface of the vertical section is in pressed contact with the solid material I5; set up the chamfer structure at the outer edge circumference of the vertical section of plectane structure orientation, hold the opening end of a thing section of thick bamboo 7 and set up the chamfer structure along circumference outward, when the vertical section complete screw in of end plug 2 holds in the thing section of thick bamboo 7, the lower face of plectane structure and the top terminal surface laminating that holds a thing section of thick bamboo 7 form the annular groove structure at chamfer position between them, and the welding is sealed in succession in annular groove department. And after the vacuumizing is finished, vacuum sealing is realized through hole plugging welding. The micropores 1 comprise a small pore section and a large pore section, and the inner diameter of the large pore section is larger than that of the small pore section; one end of the big hole section is communicated with the object bearing cylinder 1, and the other end is communicated with the small hole section.
Example 3
Based on the apparatus provided in example 2, this example provides a method for studying interfacial compatibility of a solid material, and the specific steps are as follows:
step 1, a solid material I to be researched and a solid material II are overlapped and placed in a material bearing cylinder,
step 2, one end of the end plug is screwed into the object bearing barrel from the open end of the object bearing barrel through threaded connection, the solid material I and the solid material II are compressed through the end face of the end part of the end plug extending into the object bearing barrel, and the solid material I and the solid material II are compressed between the lower end face of the end plug and the inner bottom face of the object bearing barrel, so that the interfaces of the solid material I and the solid material II are kept to be attached under positive pressure; then, a circumferential gap between the object bearing cylinder and the end plug is connected through girth welding, so that the end plug is connected with the open end of the object bearing cylinder in a vacuum sealing manner;
step 3, vacuumizing the interior of the object bearing cylinder through the micro hole on the end plug, and vacuumizing to enable the interior of the object bearing cylinder to be lower than 1x10-2A vacuum state of Pa;
step 4, after vacuumizing, realizing vacuum sealing at the micropore through hole plugging welding, and after nondestructive leakage detection, achieving a vacuum environment in the object bearing cylinder;
step 5, putting the whole device into a heat treatment furnace for heat treatment, and performing heat treatment under specific temperature and duration conditions according to material characteristics and service conditions, for example, keeping the temperature at 600 ℃ for 200 h;
and 6, processing and taking down the end plug after cooling, taking out the diffusion couple, cutting out a diffusion couple interface, and analyzing and testing the diffusion couple interface to judge the compatibility of the diffusion couple interface.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. An apparatus for studying interfacial compatibility of solid materials, which comprises a bearing barrel (7) and an end plug (2), wherein the bearing barrel (7) is used for accommodating the solid materials for preparing a diffusion couple, and the end plug (2) is connected with the top open end of the bearing barrel (7) through a screw thread and then fixed through girth welding; the end plug (2) is used for compressing the material for preparing the diffusion couple, so that the interface of the material for preparing the diffusion couple is compressed and attached; the end plug (2) is provided with a micropore (1) for vacuumizing the interior of the object bearing barrel (7), and after vacuumizing is finished, vacuum sealing of the micropore (2) is realized through hole plugging welding.
2. The device for studying the interfacial compatibility of solid materials as claimed in claim 1, wherein one end of the end plug (2) is provided with an external thread, the top open end of the receiver (7) is provided with an internal thread, and one end of the end plug (2) is screwed into the receiver (7) by the internal thread and the external thread.
3. The device for studying the interfacial compatibility of solid materials according to claim 1, wherein the micropores (1) comprise a small pore section and a large pore section, and the inner diameter of the large pore section is larger than that of the small pore section; one end of the big hole section is communicated with the object bearing cylinder (1), and the other end is communicated with the small hole section.
4. A method for investigating interfacial compatibility of solid materials, which is performed using the apparatus for investigating interfacial compatibility of solid materials according to any one of claims 1 to 3, comprising the steps of:
step 1, superposing a solid material I and a solid material II into a material bearing cylinder,
step 2, connecting the end plug with the open end of the object bearing barrel in a vacuum sealing manner;
step 3, vacuumizing the interior of the object bearing cylinder through the micro hole on the end plug;
step 4, after vacuumizing, vacuum sealing the micropores, and after nondestructive leakage detection, achieving a vacuum environment in the object bearing cylinder;
step 5, carrying out heat treatment on the whole device;
and 6, separating the end plug and the object bearing barrel, and taking out the diffusion couple for interface analysis and test.
5. The method for researching the interfacial compatibility of the solid material according to claim 4, wherein in the step 2, the end plug is screwed to the open end of the object bearing barrel through the threaded connection, and the solid material I and the solid material II are pressed through the end face of the end plug, so that the interface of the solid material I and the interface of the solid material II are kept attached in a positive pressure manner; and then the end plug is connected with the gap of the object bearing cylinder and the end plug through girth welding, so that the vacuum sealing connection of the end plug and the open end of the object bearing cylinder is realized.
6. The method for studying interfacial compatibility of solid materials as claimed in claim 4, wherein step 4, the vacuum sealing at the micro-holes is realized by plugging hole welding, and the vacuum environment is achieved in the object bearing cylinder after nondestructive leakage detection.
7. The method of claim 4, wherein the method further comprises a step of measuring the interfacial compatibility of the solid materialIn the step 3, the interior of the object bearing cylinder is vacuumized to be less than 1 multiplied by 10-2Pa, vacuum state.
8. The method for studying interfacial compatibility of solid materials according to claim 4, wherein in the step 5, the whole device is placed in a heat treatment furnace for heat treatment.
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CN111398010A (en) * 2020-03-16 2020-07-10 中广核研究院有限公司 Irradiation device for studying chemical diffusion between materials
CN112557136A (en) * 2020-11-16 2021-03-26 上海大学 Multi-element alloy diffusion couple device and multi-element alloy diffusion coefficient determination experimental method

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CN112557136A (en) * 2020-11-16 2021-03-26 上海大学 Multi-element alloy diffusion couple device and multi-element alloy diffusion coefficient determination experimental method
CN112557136B (en) * 2020-11-16 2023-05-23 上海大学 Multi-element alloy diffusion couple device and multi-element alloy diffusion coefficient determination experiment method

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