CN113607606A - Preparation method of pure metal and easily-oxidized alloy diffusion couple - Google Patents
Preparation method of pure metal and easily-oxidized alloy diffusion couple Download PDFInfo
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- 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
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- 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
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
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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
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- 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
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N2013/003—Diffusion; diffusivity between liquids
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Abstract
The invention provides a preparation method of a pure metal and easily-oxidized alloy diffusion couple, which has the advantages of simple process, time saving and low cost, and can obtain the pure metal and easily-oxidized alloy diffusion couple on the premise that the easily-oxidized alloy is not oxidized and damaged. The method comprises the following steps of carrying out surface treatment of grinding, polishing and cleaning on a contact surface of an easily oxidized alloy test piece or a test block; embedding the easily oxidized alloy test piece or block after surface treatment in pure metal powder, and placing the easily oxidized alloy test piece or block and the pure metal powder together in a quartz tube with a sealed bottom; vacuumizing the quartz tube, filling inert gas, and sealing the top; and heating the sealed quartz tube at a set temperature, preserving heat according to test requirements, and then quenching and cooling to obtain a diffusion couple of the pure metal and the easily-oxidized alloy.
Description
Technical Field
The invention relates to a diffusion couple of an alloy system, in particular to a preparation method of a pure metal and easily-oxidized alloy diffusion couple.
Background
The diffusion couple method is the most efficient and reliable method for determining the current alloy system, especially for determining the solid state relationship, and is the most efficient and reliable method for determining the diffusion characteristics of carbon atoms in steel, and is applied to the fields of materials and metallurgical science research more and more widely along with the development of the preparation technology of the diffusion couple, such as measuring diffusion kinetics, researching the phase equilibrium relationship of a binary or multi-element metal system, interfacial reaction, bulk phase transition, metastable phase transition, determining the miscible gap region of a Spinodal decomposition type phase diagram, and the like.
The traditional method for preparing the diffusion couple comprises a binding method, a crucible method, a dipping method, a rolling method, an evaporation method, a deposition method, a diffusion welding method (vacuum hot pressing method), a powder sample pressing method, a clamp method and a rivet method; the novel diffusion couple preparation method comprises a laser forming method, a discharge plasma sintering method and a diffusion multi-element method. Different preparation methods are required to be selected according to different diffusion couple systems, for example, for two metal materials with larger difference of thermal expansion coefficients and better toughness, a rivet method can be adopted to prepare the diffusion couple. However, diffusion couples for many alloy systems do not have a suitable method of preparation, particularly for rare earth alloys. Because the rare earth metal has high activity and is easy to be oxidized; moreover, many rare earth alloys are prepared by powder metallurgy, and are relatively brittle, so that the method is not suitable.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a pure metal and easily-oxidizable alloy diffusion couple, which has the advantages of simple process, time saving and low cost, and can obtain the pure metal and easily-oxidizable alloy diffusion couple on the premise that the easily-oxidizable alloy is not oxidized or damaged.
The invention is realized by the following technical scheme:
a process for preparing the diffusion couple of pure metal and easily oxidized alloy includes such steps as preparing the alloy,
carrying out surface treatment of grinding, polishing and cleaning on the contact surface of the test piece or the test block of the easily oxidized alloy;
embedding the test piece or the test block of the easily oxidized alloy after surface treatment in pure metal powder, and placing the test piece or the test block and the pure metal powder together in a quartz tube with a sealed bottom;
vacuumizing the quartz tube, filling inert gas, and sealing the top;
and heating the sealed quartz tube at a set temperature, preserving heat according to test requirements, and then quenching and cooling to obtain a diffusion couple of the pure metal and the easily-oxidized alloy.
Further, the grinding and polishing, specifically including,
grinding a test piece or a test block of the easily oxidized alloy by using 80, 400, 800 and 1200-mesh SiC metallographic abrasive paper in sequence, and then using 8000-mesh Al2O3And polishing by using the polishing paste.
Further, the cleaning specifically comprises placing the grinded and polished test piece or test block of the easily oxidized alloy in acetone for ultrasonic cleaning.
Furthermore, the purity of the pure metal powder is 99.9-99.99%, and the particle size is 20-500 μm.
Further, the pure metal powder can be dissolved into the easily oxidizable alloy or can chemically react with the easily oxidizable alloy.
Further, when the test piece or the test block of the easily oxidized alloy after the surface treatment is embedded in the pure metal powder and is placed in the quartz tube with the sealed bottom, the volume of the pure metal powder is not less than 2 times of that of the easily oxidized alloy test piece or the test block, and the total volume of the pure metal powder and the easily oxidized alloy test piece or the test block is not more than 50% of that of the quartz tube.
Further, after the quartz tube is vacuumized and filled with inert gas, the top of the quartz tube is sealed, and the method specifically comprises the following steps,
the vacuum in the quartz tube is pumped to 10-2～10-5Pa or so, then filling argon to 8X 104～105And (4) carrying out closing-in sealing treatment by adopting acetylene flame after Pa, wherein the height of the closing-in position is not less than 2 times of the height of the upper edge of the metal powder.
Further, when the sealed quartz tube is heated at the set temperature, the set temperature is higher than the service temperature of the easily-oxidizable alloy and not higher than the melting points of the pure metal and the easily-oxidizable alloy.
Further, the easily-oxidizable alloy is a rare earth alloy.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the method, the whole easily-oxidizable alloy is coated with the pure metal powder and is placed in the inert environment, extremely low oxygen partial pressure is formed around the easily-oxidizable alloy, so that easily-oxidizable alloy elements with high activity are difficult to oxidize, an easily-oxidizable alloy interface cannot generate an oxidation film to block diffusion, the preparation process is simple, the success rate is high, and the method can be implemented in batches. The method is suitable for the rare earth alloy which is easy to oxidize, is particularly suitable for preparing the rare earth compound diffusion couple with larger brittleness, and the prepared diffusion couple can be used for researching diffusion kinetics, thermodynamics and a phase diagram.
Drawings
FIG. 1 is a schematic view of the manufacturing process of the present invention.
FIG. 2 is a SEM image of the Cu/Sm (Co, Fe) diffusion couple interface condition of the present invention.
FIG. 3 is a diagram showing the distribution of elements in the Cu/Sm (Co, Fe) diffusion couple interface region of the example of the present invention.
In the figure: the alloy comprises easily oxidized alloy 1, pure metal powder 2 and a quartz tube 3.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention discloses a preparation method of a pure metal and easily-oxidized alloy 1 diffusion couple, which comprises the following steps as shown in figure 1:
(1) grinding, polishing and cleaning a test piece or a test block of the easily oxidized alloy 1 to obtain a flat and smooth contact surface; in the preferred embodiment, the grinding and polishing treatment means that the test piece or block of the easily oxidizable alloy 1 is ground by using SiC metallographic abrasive paper of 80, 400, 800 and 1200 meshes in this order, and then, 8000 meshes of Al is used2O3Polishing the polishing paste; cleaning refers to ultrasonic cleaning in acetone to remove oil stains;
(2) embedding a test piece or a test block of the easily oxidized alloy 1 with a well-treated surface in the pure metal powder 2, and putting the test piece or the test block into a quartz tube 3 with one end open and the other end closed; in the preferred embodiment, the purity of the pure metal powder 2 is not less than 99.9% and the particle size is not more than 500. mu.m.
(3) Closing up and sealing the quartz tube 3 in which the pure metal powder 2 and the test piece or the test block of the easily-oxidized alloy 1 are placed by adopting high-temperature flame, and then cooling to room temperature; in the preferred embodiment, the volume of the pure metal powder 2 is not less than 2 times of the test piece or test block of the easily oxidized alloy 1, and the total volume of the pure metal powder 2 and the easily oxidized alloy 1 is not more than 50% of the volume of the quartz tube 3; before closing up and sealing the quartz tube 3, vacuumizing and then filling high-purity argon, and finally packaging the quartz tube 3 by adopting acetylene flame.
(4) And heating the sealed quartz tube 3 at a set temperature, preserving heat according to test requirements, and quenching and cooling to complete the preparation of the pure metal and the easily-oxidized alloy 1 diffusion couple.
In practice, the specific steps of the preferred embodiment are as follows,
(1) processing the easily oxidized alloy 1 into a test block of 10 multiplied by 10mm or a test piece of 10 multiplied by 2mm by a wire cutting machine, grinding and polishing, and then ultrasonically cleaning in acetone to remove oil stains to obtain a smooth and clean contact surface;
(2) embedding a test piece or a test block of the easily oxidized alloy 1 with a well-treated surface into pure metal powder 2 with the purity of 99.9-99.99% and the particle size of 20-500 mu m, putting the test piece or the test block into the bottom of a quartz tube 3 with one end open and the other end closed and the inner diameter not less than 20mm, and ensuring that the volume of the quartz tube 3 is not more than 50%;
(3) the vacuum in the quartz tube 3 is pumped to 10 degree by using a vacuum tube sealing device-2～10-5Pa, then filling high-purity argon to 8X 104～105And Pa, finally carrying out closing-up sealing treatment by adopting acetylene flame, wherein the height of the closing-up position is not less than 2 times of the height of the upper edge of the metal powder.
(4) The sealing performance of the quartz tube 3 is checked, and if no gas is leaked, the sealed quartz tube 3 is put into a muffle furnace with a set temperature for heating, wherein the set temperature is not higher than the melting points of the pure metal and the oxidizable alloy 1 so as to prevent the occurrence of liquid phase. And preserving heat for a certain time according to test requirements, and finally quenching and cooling to obtain the diffusion couple of the pure metal and the easily oxidized alloy 1. The holding time is not particularly limited, and the diffusion distances of the pure metal elements at different times need to be observed, so that the holding time is adjusted according to requirements.
Example 1
In this example 1, pure Cu powder was used as the pure metal powder 2, and Sm was used as the oxidizable alloy 12(Co,Fe)17The invention is further illustrated by the diffusion couple preparation of the alloy.
Referring to FIG. 1, Sm prepared by powder metallurgy with a wire cutting machine2(Co,Fe)17Processing the alloy into a test block with the thickness of 10 multiplied by 10mm, grinding and polishing the test block, and then ultrasonically cleaning the test block in acetone to remove oil stains to obtain a flat and smooth contact surface;
sm with well treated surface2(Co,Fe)17The alloy test block is embedded in Cu powder with the purity of 99.99 percent and the average grain diameter of 100 mu m, and is placed at the bottom of a quartz tube 3 with one end opened and the other end closed and the inner diameter of 30 mm;
the vacuum in the quartz tube 3 is pumped to 5 x 10 by using a vacuum tube sealing device-3Pa, then filling high-purity argon to 105Pa, finally adopting acetylene flame to carry out closing-up sealing treatment, wherein the height of the closing-up position is above Cu powderAlong 2.5 times the height.
Checking the tightness of the quartz tube 3, putting the sealed quartz tube 3 into a muffle furnace with the set temperature of 700 ℃ for heat preservation for 20h, taking out the quartz tube and quenching and cooling to obtain Cu and Sm2(Co,Fe)17The diffusion couple of (2). Set temperature higher than Sm2(Co,Fe)17But below the melting point of the alloy and Cu; the time is not particularly limited, and in order to obtain a complete phase diagram, diffusion couple studies at continuous temperature and time are usually conducted, and the examples are explained by specific time and temperature.
Cu/Sm pair using scanning electron microscope and X-ray diffractometer with attached energy spectrum2(Co,Fe)17The interfacial bonding of the diffusion couple, the diffusion of the Cu element, and the interface phase were measured. Referring to FIGS. 2 and 3, the observation of Sm on a scanning electron microscope is shown2(Co,Fe)17The interface of the alloy and the Cu powder does not form oxides, and only a remarkable diffusion layer and a phase change region are formed. I.e. Cu to Sm2(Co,Fe)17Diffusion occurs in the process, resulting in Cu and Sm2(Co,Fe)17Sm at the interface2(Co,Fe)17Completely degenerates into a (Co, Fe) solid solution of bcc structure, and the excess Sm is discharged and enters into the Sm at a deeper position2(Co,Fe)17In the alloy. Sm in the matrix adjacent to the diffusion couple interface under the combined action of supersaturated Sm and Cu2(Co,Fe)17Becomes unstable and turns into Sm (Cu, Co)7And (Co, Fe) solid solution. This is to perfect Sm-Co-Fe-Cu quaternary phase diagram and understand Cu in Sm2(Co,Fe)17The dissolution and diffusion of (b) provide an assistance force.
The pure metal of the present invention should be soluble in the easily oxidizable alloy 1 or chemically reactive with the easily oxidizable alloy 1, and neither the pure metal nor the easily oxidizable alloy 1 react with the quartz tube 3.
Example 2
In this example 2, pure Al powder was used as the pure metal powder 2, and the easily oxidizable alloy 1 was prepared by a diffusion couple of Cu-50Ni alloy, which further illustrates the present invention.
Processing Cu-50Ni alloy into a test block with the thickness of 10 multiplied by 10mm by a wire cutting machine, grinding and polishing the test block, and then ultrasonically cleaning the test block in acetone to remove oil stains to obtain a flat and smooth contact surface;
embedding the Cu-50Ni alloy test block with the well-processed surface into Al powder with the purity of 99.9 percent and the average grain diameter of 200 mu m, and putting the Al powder and the Al powder together into the bottom of a quartz tube 3 with an opening at one end and a closed opening at the other end and the inner diameter of 35 mm;
the vacuum in the quartz tube 3 is pumped to 3 x 10 by using a vacuum tube sealing device-4Pa, then filling high-purity argon to 9X 104And Pa, finally carrying out closing-in sealing treatment by adopting acetylene flame, wherein the height of the closing-in position is 3 times of the height of the upper edge of the Al powder.
And (3) checking the sealing performance of the quartz tube 3, putting the sealed quartz tube 3 into a muffle furnace with the set temperature of 600 ℃ for heat preservation for 10h, taking out the quartz tube, and quenching and cooling to obtain the diffusion couple of Al and Cu-50 Ni. The set temperature is slightly below the melting point of Al.
Example 3
In this example 3, pure Zr powder is used as the pure metal powder 2, and NbFeB alloy is used as the oxidizable alloy 1, and the present invention will be further described.
Processing NbFeB alloy into a test block with the thickness of 10 multiplied by 10mm by a wire cutting machine, grinding and polishing the test block, and then ultrasonically cleaning the test block in acetone to remove oil stains to obtain a flat and smooth contact surface;
embedding the surface-treated NbFeB alloy test block in Zr powder with the purity of 99.95 percent and the average grain diameter of 100 mu m, and putting the Zr powder and the Zr powder together into the bottom of a quartz tube 3 with an opening at one end and a closing-in at the other end and the inner diameter of 40 mm;
the vacuum in the quartz tube 3 is pumped to 4 x 10 by using a vacuum tube sealing device-5Pa, then filling high-purity argon to 8X 104And Pa, finally carrying out closing-up sealing treatment by adopting acetylene flame, wherein the height of the closing-up position is 3 times of the height of the upper edge of the Zr powder.
And (3) checking the sealing performance of the quartz tube 3, putting the sealed quartz tube 3 into a muffle furnace with the set temperature of 750 ℃ for heat preservation for 24h, taking out the quartz tube, and quenching and cooling to obtain the diffusion couple of NbFeB and Zr.
While specific embodiments of the present invention have been described with reference to examples, the description is not to be construed as limiting the scope of the invention, which is defined by the appended claims, as any variation thereof is encompassed by the present claims.
Claims (9)
1. A method for preparing a pure metal and easily-oxidized alloy diffusion couple is characterized by comprising the following steps of,
carrying out surface treatment of grinding, polishing and cleaning on the contact surface of the test piece or the test block of the easily oxidized alloy (1);
embedding a test piece or a test block of the easily oxidized alloy (1) after surface treatment in pure metal powder (2), and placing the test piece or the test block and the pure metal powder together in a quartz tube (3) with a sealed bottom;
vacuumizing the quartz tube (3) and filling inert gas, and sealing the top;
and heating the sealed quartz tube (3) at a set temperature, preserving heat according to test requirements, and then quenching and cooling to obtain a diffusion couple of the pure metal and the easily-oxidized alloy (1).
2. The method of claim 1, wherein the grinding and polishing comprises,
grinding a test piece or a test block of the easily oxidized alloy (1) by using 80, 400, 800 and 1200-mesh SiC metallographic abrasive paper in sequence, and then using 8000-mesh Al2O3And polishing by using the polishing paste.
3. The method for preparing a diffusion couple of a pure metal and an easily oxidizable alloy according to claim 1, wherein the cleaning specifically comprises placing a test piece or a test block of the easily oxidizable alloy (1) after grinding and polishing in acetone for ultrasonic cleaning.
4. The method for preparing a pure metal and easily oxidizable alloy diffusion couple according to claim 1, wherein said pure metal powder (2) has a purity of 99.9-99.99% and a particle size of 20-500 μm.
5. The method for preparing a diffusion couple of a pure metal and an easily oxidizable alloy according to claim 1, wherein said pure metal powder (2) is soluble in said easily oxidizable alloy (1) or chemically reactive with said easily oxidizable alloy (1).
6. The method for preparing a pure metal and easily oxidizable alloy diffusion couple according to claim 1, wherein when the test piece or block of the easily oxidizable alloy (1) after surface treatment is embedded in the pure metal powder (2) and is placed together in the quartz tube (3) with a sealed bottom, the volume of the pure metal powder (2) is not less than 2 times that of the test piece or block of the easily oxidizable alloy (1), and the total volume of the test piece or block of the pure metal powder (2) and the easily oxidizable alloy (1) is not more than 50% of the volume of the quartz tube (3).
7. The method for preparing a diffusion couple of a pure metal and an easily oxidizable alloy according to claim 1, wherein the top is sealed after the quartz tube (3) is evacuated and filled with an inert gas, and comprises,
the vacuum in the quartz tube (3) is pumped to 10-2～10-5Pa or so, then filling argon to 8X 104～105And (4) carrying out closing-in sealing treatment by adopting acetylene flame after Pa, wherein the height of the closing-in position is not less than 2 times of the height of the upper edge of the metal powder.
8. The method for preparing a diffusion couple of a pure metal and an easily oxidizable alloy according to claim 1, wherein the sealed quartz tube (3) is heated at a set temperature which is higher than the service temperature of the easily oxidizable alloy (1) and not higher than the melting points of the pure metal and the easily oxidizable alloy (1).
9. The method of claim 1, wherein the oxidizable alloy (1) is a rare earth alloy.
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| CN110608931A (en) * | 2019-09-11 | 2019-12-24 | 贵研铂业股份有限公司 | High-flux preparation method for preparing metal diffusion couples with large melting point difference |
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| CN110608931A (en) * | 2019-09-11 | 2019-12-24 | 贵研铂业股份有限公司 | High-flux preparation method for preparing metal diffusion couples with large melting point difference |
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