CN113189127B - Method for preparing high-melting-point metal ternary diffusion couple - Google Patents
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Abstract
The invention discloses a method for preparing a high-melting-point metal ternary diffusion couple. The method is mainly used for preparing a diffusion couple consisting of three high-melting-point metals. The method comprises the following steps: firstly, laying a B metal block or sheet with the lowest melting point of three high-melting-point metals above an A metal block, then placing the A-B metal into a tube furnace protected by argon gas to be heated to be above the melting point of the B metal, so that the B metal is melted to form metallurgical bonding with the A, performing diffusion annealing to form an A-B diffusion couple, then coating a C metal sheet at the interface of the A-B diffusion couple, fixing the A-B diffusion couple by using a clamp, and performing diffusion annealing to obtain the A-B/C ternary diffusion couple. The method is simple, needs less metal, is easy to control the preparation process, has flexible and controllable diffusion couple combination, and has excellent effect and higher success rate. The method is suitable for preparing the diffusion couple of the metal material, in particular to the preparation of the diffusion couple of the noble metal and the high-temperature alloy material, and the prepared diffusion couple can be used for researching a phase diagram, diffusion dynamics and thermodynamics.
Description
Technical Field
The invention relates to a method for preparing a high-melting-point metal ternary diffusion couple, and belongs to the method for preparing diffusion couples in the fields of metal materials, phase diagram research, high-temperature alloy, brazing and the like. The method is mainly used for the related fields of preparing the high-melting-point metal ternary diffusion couple, and mainly comprises the fields of welding, brazing, phase diagram measurement, high-temperature alloy, diffusion data measurement and the like.
Background
Diffusion couple refers to a sample formed by diffusion bonding two or more materials. The diffusion is fully performed in the direction vertical to the welding surface, and the continuous diffusion from one phase diffusion layer to the other phase diffusion layer with a certain thickness is formed, and the thickness of the diffusion layer can meet the requirement of measuring component distribution by an electronic probe. This diffusion interface or phase interface is macroscopically a two-dimensional surface, but has a small dimension in the thickness direction, and is thus locally balanced. The local equilibrium state at the phase interface is the basis for determining the phase diagram using diffusion couple. Since the chemical potentials of each component at the phase interface are equal, the diffusion path proceeds along the equilibrium conjugate line in each two-phase region of the binary alloy phase diagram or the ternary alloy phase diagram during diffusion, and thus the phase composition at equilibrium of the two phases can be determined.
The diffusion couple method relies on the principle of local equilibrium, requiring only a local equilibrium at the phase interface and not a complete overall equilibrium of the sample. Compared with an alloy method, the method is simple, convenient and practical, has high experimental efficiency, and theoretically all relevant systems can appear in the diffusion couple if the mother alloy of the diffusion couple is properly selected. The method can greatly reduce the experimental workload, reduce the consumption of raw materials and accelerate the actual measurement progress of the phase diagram, thereby being widely applied to the equilibrium phase diagram experimental measurement of a multi-component system. The diffusion couple can avoid the supercooling effect because the diffusion couple method is used for measuring the equilibrium components in the rapidly-cooled sample after the sample is kept at a specific temperature for a long time and belongs to transverse measurement. Compared with a method for continuously measuring the transformation temperature of an alloy sample with a specific component (namely, longitudinal measurement), the method has no so-called supercooling effect which causes the transformation temperature to be measured inaccurately due to the excessively high cooling speed. The determination of phase boundaries and phase relationships is direct and not speculative.
The state of each component included in the diffusion couple is combined, and the diffusion couple is classified into a solid-solid diffusion method, a solid-liquid diffusion method, and a solid-gas diffusion method. According to the difference of the number of the diffusion couple components, the diffusion couple components can be divided into binary diffusion couples, ternary diffusion couples, quaternary diffusion couples and higher diffusion couples. The binary diffusion couple is generally prepared by a clamping method, a binding method, a rolling method, a solid-liquid dipping method and the like. The preparation method of the ternary diffusion couple mainly comprises a ' Chinese character ' pin ' shape combination method, a ' rivet method ' and the like.
In the existing preparation method of the ternary diffusion couple, wang Nie et al, named as 'measurement of Ni-Cr-Mo ternary system 1358K isothermal cross section' in rare metal materials and engineering (Vol.34, no. 9), discloses a 'pin' -shaped combined preparation method related to the Ni-Cr-Mo ternary diffusion couple, namely, mo and Ni with high melting point and low melting point are prepared into a binary diffusion couple through solid-solid diffusion, and then the binary diffusion couple and Cr with the melting point between Mo and Ni form a 'pin' -shaped diffusion couple.
Chinese patent 'a method for efficiently preparing a ternary diffusion couple' (CN 110340331A), discloses a method for preparing a ternary diffusion couple, which comprises the steps of firstly preparing a binary diffusion couple (solid-solid diffusion) by a clamp method, then putting the prepared binary diffusion couple into a grinding tool, adding another component to be diffused, heating to the melting point of the component, cooling to the heat treatment temperature, preserving heat, and performing water quenching to prepare the ternary diffusion couple.
In the ternary diffusion couple, if the melting point temperatures of three high-melting-point metals are respectively set as A, C and B from high to low, the first one in the preparation method is an A-B/C couple, and solid-solid diffusion is adopted; the second is A-C/B couple, and solid-solid diffusion and solid-liquid diffusion exist, so that no report related to the preparation of the A-B/C couple by adopting solid-liquid diffusion is found at present.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for flexibly preparing a high-melting-point metal ternary diffusion couple, which is easy to control the process flow, low in cost and suitable for preparing a high-temperature metal material diffusion couple, particularly a noble metal material diffusion couple and can be used for researching a phase diagram, diffusion dynamics and thermodynamics, aiming at the defects of the existing preparation technology of the high-melting-point metal diffusion couple.
The invention firstly combines high melting point and low melting point metals together through solid-liquid diffusion to prepare a binary diffusion couple (expressed as an A-B couple prepared by high-low melting point of three high melting point metals), and then prepares a ternary diffusion couple through solid-solid diffusion (namely the melting point is prepared according to high-low/medium and expressed as an A-B/C couple).
The technical scheme adopted by the invention is as follows:
a method for preparing a ternary diffusion couple of high-melting-point metals, wherein the three high-melting-point metals are respectively expressed as A metal, C metal and B metal according to relatively high, medium and low melting points; firstly, combining the metal A and the metal B together by a solid-liquid diffusion method to prepare an A-B binary diffusion couple; then preparing the ternary A-B/C diffusion couple by a solid-solid diffusion method.
Further, the invention specifically comprises the following steps:
(1) Firstly, overlapping and laying the blocks or the sheets of the metal B above the blocks of the metal A, and then horizontally placing the blocks or the sheets into a corundum boat;
(2) Putting the corundum boat into a high-temperature tube furnace, heating to a temperature higher than the melting point of the metal B and lower than the melting point of the metal A under the protection of argon, preserving the heat for more than 30 minutes to ensure that the metal B is uniformly melted and covered on the surface of the metal A block, then cooling to a temperature lower than the melting point of the metal B for diffusion annealing, and then cooling along with the furnace and taking out to obtain an A-B binary diffusion couple;
(3) Grinding and polishing the surface of the metal C sheet, wherein the length of the metal C sheet is based on the fact that the metal C sheet can cover the A-B binary diffusion couple, and the width of the metal C sheet is the same as the width of a bonding interface of the A-B binary diffusion couple; and bending and coating a C metal sheet at the joint interface of the A-B binary diffusion couple, fixing the C metal sheet by using a clamp, and performing diffusion annealing in a quartz tube in a vacuum packaging manner to prepare the A-B/C ternary diffusion couple.
(4) And after the annealing is finished, taking out the quartz tube, quickly cooling the quartz tube in cold water, taking out the prepared A-B/C ternary diffusion couple from the quartz tube, and polishing.
Preferably, the melting point of the A metal is 150 ℃ or higher than that of the B metal, and the heating is carried out until the temperature is 30-50 ℃ or higher than that of the B metal.
Preferably, the a metal, the B metal and the C metal are Pt, au and Ni, respectively. Heating to 1000-1120 ℃ under the protection of argon.
Preferably, the surface of the Ni metal sheet with the thickness of 0.4-0.5 mm is ground flat and polished, and then bent and coated at the Au-Pt combination interface.
Preferably, the diffusion annealing is performed at a temperature of 750 to 900 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) The preparation method is simple, the required metal amount is less, the preparation process is easy to control, the diffusion couple combination is very flexible and controllable, the effect is excellent, and the success rate is higher.
(2) In the Pt-Au/Ni diffusion couple prepared in the embodiment 1 of the invention, at a diffusion interface, three elements of Pt, au and Ni are well diffused, au and Ni are diffused into Pt, and Pt and Ni are also diffused into Au, wherein the content of Ni at the interface is higher.
(3) The invention is especially suitable for the preparation of noble metal and high-temperature alloy material diffusion couples, and the prepared diffusion couples can be used for the research of phase diagrams, diffusion dynamics and thermodynamics.
Drawings
FIG. 1: SEM scanning image of diffusion interface of Pt-Au/Ni diffusion couple, wherein the dotted line represents the position of line scanning.
FIG. 2: line scan of the Pt-Au/Ni diffusion couple at the dashed line position in FIG. 1.
Detailed Description
Example 1
(1) Firstly, among three high-melting-point metals of Pt, au and Ni, an Au metal block or sheet with the lowest melting point is overlapped and laid above a Pt metal block with the highest melting point, and is horizontally placed in a corundum boat;
(2) Putting the corundum boat into a high-temperature tube furnace, heating to 1100 ℃ under the protection of argon, preserving heat for 30 minutes to enable Au to be uniformly molten and cover the surface of the Pt block, then cooling to 900 ℃, preserving heat for 120 hours, then cooling to room temperature along with the furnace, and taking out;
(3) Grinding and polishing the surface of a Ni metal sheet with the thickness of 0.4mm, bending and wrapping the Ni metal sheet at an Au-Pt combination interface, fixing the Ni metal sheet by using a clamp, packaging the Ni metal sheet in a quartz tube in a vacuum manner, and carrying out annealing heat treatment at 900 ℃;
(4) And after the heat treatment is finished, taking the quartz tube out, rapidly cooling in cold water, taking the prepared diffusion couple out of the quartz tube, and polishing to directly use for phase diagram measurement and diffusion experiments.
The diffusion interface of the PtAu/Ni diffusion couple prepared in the embodiment is shown in FIG. 1, and it can be seen from the figure that at the diffusion interface, three metal elements are well diffused, au and Ni are diffused into Pt, and Pt and Ni are also diffused into Au, wherein the content of Ni at the interface is high.
Example 2
(1) Firstly, overlapping and laying a Cu metal block or sheet with the lowest melting point among three high-melting-point metals of Pt, pd and Cu above a Pt metal block with the highest melting point, and horizontally putting the Cu metal block or sheet above a corundum boat;
(2) Putting the corundum boat into a high-temperature tube furnace, heating to 1120 ℃ under the protection of argon, preserving heat for 30 minutes, enabling Cu to be uniformly melted and cover the surface of the Pt block, then cooling to 800 ℃, preserving heat for 120 hours, and then cooling along with the furnace and taking out;
(3) Grinding and polishing the surface of a Pd metal sheet with the thickness of 0.5mm, bending and coating the surface at a Pt-Cu combination interface, fixing the surface by using a clamp, packaging the surface in a quartz tube in vacuum, and performing diffusion annealing at 800 ℃;
(4) And after the annealing is finished, taking out the quartz tube, rapidly cooling in cold water, taking out the prepared diffusion couple from the quartz tube, and polishing to directly use the diffusion couple for phase diagram measurement and diffusion experiments.
Example 3
(1) Firstly, among three high-melting-point metals of Pd, ag and Pt, an Ag metal block or sheet with the lowest melting point is overlapped and laid above a Pt metal block with the highest melting point, and is horizontally placed in a corundum boat;
(2) Putting the corundum boat into a high-temperature tube furnace, heating to 1000 ℃ under the protection of argon, preserving heat for 30 minutes to enable Ag to be uniformly melted and cover the surface of the Pt block, then cooling to 750 ℃, preserving heat for 120 hours, and then cooling along with the furnace and taking out;
(3) Grinding and polishing the surface of a Pd metal sheet with the thickness of 0.5mm, bending and wrapping the surface at an Ag-Pt combination interface, fixing the surface by using a clamp, packaging the surface in a quartz tube in a vacuum manner, and performing diffusion annealing at 750 ℃;
(4) And after the annealing is finished, taking out the quartz tube, rapidly cooling in cold water, taking out the prepared diffusion couple from the quartz tube, and polishing to directly use the diffusion couple for phase diagram measurement and diffusion experiments.
Claims (7)
1. A method for preparing a ternary diffusion couple of high-melting-point metal is characterized by comprising the following steps:
three kinds of high-melting point metals are respectively expressed as metal A, metal C and metal B according to the relative high, medium and low melting points; firstly, combining the metal A and the metal B together by a solid-liquid diffusion method to prepare an A-B binary diffusion couple; then preparing a ternary A-B/C diffusion couple by a solid-solid diffusion method;
the method specifically comprises the following steps:
(1) Firstly, overlapping and laying the block or sheet of the metal B above the block of the metal A, and then horizontally placing the block or sheet of the metal B into a corundum boat;
(2) Putting the corundum boat into a high-temperature tube furnace, heating to a temperature higher than the melting point of the metal B and lower than the melting point of the metal A under the protection of argon, preserving the heat for more than 30 minutes to ensure that the metal B is uniformly melted and covered on the surface of the metal A block, then cooling to a temperature lower than the melting point of the metal B for diffusion annealing, and then cooling along with the furnace and taking out to obtain an A-B binary diffusion couple;
(3) Grinding and polishing the surface of the metal C sheet, wherein the length of the metal C sheet is based on the fact that the metal C sheet can cover the A-B binary diffusion couple, and the width of the metal C sheet is the same as the width of a bonding interface of the A-B binary diffusion couple; and bending and coating a C metal sheet at the joint interface of the A-B binary diffusion couple, fixing the C metal sheet by using a clamp, and performing diffusion annealing in a quartz tube in a vacuum packaging manner to prepare the A-B/C ternary diffusion couple.
2. The method of preparing a refractory metal ternary diffusion couple as in claim 1, further comprising the steps of:
(4) And after the annealing is finished, taking the quartz tube out, rapidly cooling in cold water, taking the prepared A-B/C ternary diffusion couple out of the quartz tube, and polishing.
3. The method of preparing a refractory metal ternary diffusion couple as defined in claim 1, wherein:
the melting point of the metal A is higher than that of the metal B by more than 150 ℃, and the temperature is raised to be 30-50 ℃ higher than that of the metal B.
4. The method for producing a high melting point metal ternary diffusion couple according to any one of claims 1 to 3, characterized in that:
the metal A, the metal B and the metal C are respectively Pt, au and Ni.
5. The method of making a refractory metal ternary diffusion couple of claim 4, wherein:
heating to 1000-1120 ℃ under the protection of argon.
6. The method of making a refractory metal ternary diffusion couple of claim 4, wherein:
and grinding and polishing the surface of a Ni metal sheet with the thickness of 0.4-0.5 mm, and bending and cladding the Ni metal sheet at the Au-Pt combination interface.
7. The method of making a refractory metal ternary diffusion couple of claim 4, wherein:
the diffusion annealing is carried out at a temperature of 750-900 ℃.
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| CN108240926A (en) * | 2016-12-27 | 2018-07-03 | 北京有色金属研究总院 | The preparation method of one Albatra metal multi-component diffusion idol |
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| US7392927B2 (en) * | 2003-04-17 | 2008-07-01 | General Electric Company | Combinatorial production of material compositions from a single sample |
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| CN108240926A (en) * | 2016-12-27 | 2018-07-03 | 北京有色金属研究总院 | The preparation method of one Albatra metal multi-component diffusion idol |
| CN110340331A (en) * | 2019-07-31 | 2019-10-18 | 贵研铂业股份有限公司 | A kind of method of efficient preparation ternary diffusion idol |
| CN110523776A (en) * | 2019-08-27 | 2019-12-03 | 贵研铂业股份有限公司 | A kind of even high-throughput preparation of ternary diffusion and heat treatment method |
| CN110514498A (en) * | 2019-09-11 | 2019-11-29 | 贵研铂业股份有限公司 | A kind of method that centrifugal process prepares metal expansion idol |
| 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 |
| CN110595955A (en) * | 2019-09-27 | 2019-12-20 | 贵研铂业股份有限公司 | Method for preparing easily oxidized metal diffusion couple |
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