CN105537799A - Agcuti active brazing filler metal and preparation method thereof - Google Patents
Agcuti active brazing filler metal and preparation method thereof Download PDFInfo
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- CN105537799A CN105537799A CN201510988409.3A CN201510988409A CN105537799A CN 105537799 A CN105537799 A CN 105537799A CN 201510988409 A CN201510988409 A CN 201510988409A CN 105537799 A CN105537799 A CN 105537799A
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- active solder
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0227—Rods, wires
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses AgCuTi active brazing filler metal and a preparation method thereof. The AgCuTi active brazing filler metal is composed of, by mass, 60%-75% of Ag, 20%-35% of Cu and 1%-7% of Ti. In order to improve the dispersal uniformity of powder, main adopted measures are that AgCu28 powder, Cu powder and Ti powder of which the grain sizes are uniform (between 10 [mu]m and 30 [mu]m) are selected to be subjected to high energy ball milling (mechanical alloying) under the protection of Ar atmosphere. By means of a hot isostatic pressing process, the plastic processing performance is improved through a similar core-shell structure formed by atomic diffusion while the compactness of alloy ingots is improved. The defect of the simplex form of the AgCuTi active brazing filler metal in China is overcome, the problem that components of a single metal powder mixing method and a vacuum induction melting method are nonuniform is solved, and the competitiveness of Chinese active silver brazing filler metal in domestic and overseas markets is improved. Processing equipment required by the preparation method is simple and easy to operate, and large-batch preparation of active brazing filler metal alloy can be achieved quite easily.
Description
Technical field
The present invention relates to AgCuTi active solder and preparation method thereof.
Background technology
AgCuTi active solder has the performances such as suitable solid-liquid liquidus temperature, excellent wetability and higher soldering joint strength, is mainly used in the soldering between pottery and pottery, metal and pottery and material with carbon element, as Al
2o
3with CaF
2, Al
2o
3with Cu, SiC and TC4 and Cu-C composition metal and Al
2o
3between connection.According to existing document and relevant report, the active solder containing Ti has become the research emphasis of ceramic joining and popular direction, but perplexs technical bottleneck that AgCuTi active solder applies always and be that it lower shapes performance.
The main cause that AgCuTi active solder shapes performance poor is: Ti is easy to most metals reaction and generates brittle intermetallic thing, worsens its processing characteristics.The active solder that current domestic ceramic joining uses obtains generally through following three kinds of modes:
1, metal simple-substance powder mixing method: adopt metal simple-substance powder, according to the preparation of certain mass mark, is mixed by ball milling and other modes, then soldering.The advantage of this mode is simple to operation, but owing to being subject to the restriction of metal powder granularity and density, being difficult to simple substance powder is mixed, thus affecting the performance of ceramic soldered joint.
2, vacuum induction melting method: melt out AgCuTi alloy pig via Medium frequency induction in a vacuum, then reaches products application required size by the plastic deformation process such as rolling, wire drawing.The advantage of this technique is alloy density can be made to improve by the mode of melting, is conducive to next step plastic working.Shortcoming mainly contains: need high vacuum (<10
-3pa); Be limited to the intensity of Medium frequency induction, be difficult to the ingot casting obtaining uniform component; Because Ti activity is high, be easy to and conventional crucible reaction, while affecting alloy pig quality, be also difficult to realize active solder large-scale production.
3, import: domesticly at present mostly rely on import Germany or japanese product to demand that is thread, sheet-shaped Ag/Cu Ti active solder, is limited to purchase channel smooth, causes active solder product price too high, thus restrict its wider application.
Summary of the invention
A kind of AgCuTi active solder that object of the present invention is developed specially for the problem existing for above-mentioned prior art just and preparation method thereof, solder of the present invention has suitable fusing point, and preparation production technology efficiency is high, for the preparation of domestic AgCuTi active solder opens new way.
The object of the invention is to be achieved through the following technical solutions:
AgCuTi active solder of the present invention is made up of 60-75%Ag, 20-35%Cu and 1-7%Ti by mass percentage.For improving the uniformity of powder dispersion, the measure mainly taked be choose the AgCu28 powder of granularity consistent (between 10-30 μm), Cu powder and Ti powder carry out Ar atmosphere protection under high-energy ball milling (mechanical alloying).By heat and other static pressuring processes, while raising alloy pig density, form class " nucleocapsid structure " via atoms permeating promote plastic deformation ability.
The preparation method of AgCuTi active solder of the present invention completes according to the following steps:
One, take by weight percentage: the Ti powder of the AgCu28 alloyed powder of 90-96%, the electrolysis Cu powder of 2-5%, 1-7%;
Two, mechanical alloying: powder ball milling ball and step one obtained loads in ball grinder, and be filled with Ar after vacuumizing, Ball-milling Time is 6-24 hour, rotating speed is 250-350r/min, ratio of grinding media to material is 6-15:1, filler ratio is 45-55%;
Three, high temperature insostatic pressing (HIP): ball milling powder step 2 obtained loads cylindrical stainless steel jacket and carries out high temperature insostatic pressing (HIP), pressure is at 150-300MPa, and holding temperature is 550-700 DEG C, and programming rate is 5-20 DEG C/min, and temperature retention time is 30-120min;
Four, hot extrusion: alloy pig step 3 obtained puts into resistance furnace insulation, and holding temperature is 500-700 DEG C, and temperature retention time is 60-180min; Put into heat extruder after insulation terminates and be squeezed into AgCuTi alloy slab (round bar);
Five, cold deformation: AgCuTi active solder slab step 4 obtained carries out multi-pass cold deformation (rolling and wire drawing), until solder product required size, pass deformation is 20-50%, annealing in process is carried out between every time deformation phases, annealing temperature is 300-700 DEG C, the temperature time is 30-180min, obtains active A gCuTi active solder finished product.
Advantage of the present invention:
1, overcome the shortcoming that China AgCuTi active solder form is single, solve metal simple-substance powder mixing method and the inhomogenous problem of vacuum induction melting method composition, add the competitiveness of the active silver solder of China at home and abroad on market.
2, this preparation method is by being formed so-called " nucleocapsid structure ", solves the difficulty that smelting process causes because brittle intermetallic thing exists in a large number and shapes problem.
3, the present invention is by the process means of high temperature insostatic pressing (HIP), in suitable holding temperature with under the time, improves the density of active solder alloy, and then improves the processing characteristics of sintered alloy ingot.
4, needed for this preparation method, process equipment is simple to operation, very easily realizes the large batch of preparation of active solder alloy.
Accompanying drawing explanation
Fig. 1 is the micro-organization chart of the AgCuTi active solder that embodiment five obtains;
Fig. 2 is the component distributing line sweep figure of the AgCuTi active solder that embodiment five obtains;
Fig. 3 is that embodiment five obtains the thick AgCuTi active solder photo of 0.05mm;
Fig. 4 is the AgCuTi active solder photo that embodiment nine obtains diameter phi 1.02mm;
Fig. 5 is the tensile stress-strain curve figure of the AgCuTi active solder that embodiment nine obtains;
Fig. 6 is the stretching fracture shape appearance figure of the AgCuTi active solder that embodiment nine obtains.
Detailed description of the invention
Embodiment one: the present embodiment is used for AgCuTi active solder, makes according to the Ti powder of percentage by weight by the AgCu28 alloyed powder of 90-96%, the electrolysis Cu powder of 2-5% and 1-7%.
Electrolysis Cu powder in the present embodiment, Ti powder quality purity are 99.9-99.99%
Embodiment two: the present embodiment and embodiment one unlike for AgCuTi active solder, according to percentage by the AgCu28 alloyed powder of 93.5%, the electrolysis Cu powder of 5% and 1.5% Ti powder make.Other is identical with embodiment one.
Embodiment three: the present embodiment and embodiment one unlike for AgCuTi active solder, according to percentage by the AgCu28 alloyed powder of 92%, the electrolysis Cu powder of 5% and 3% Ti powder make.Other is identical with embodiment one.
Embodiment four: the present embodiment and embodiment one unlike for AgCuTi active solder, according to percentage by the AgCu28 alloyed powder of 90%, the electrolysis Cu powder of 5% and 5% Ti powder make.Other is identical with embodiment one.
Embodiment five: the preparation method of the present embodiment AgCuTi active solder completes according to the following steps: one, according to the Ti powder of percentage by weight by the AgCu28 alloyed powder of 90-96%, the electrolysis Cu powder of 2-5% and 1-7%; Two, mechanical alloying: ball milling ball and powder are loaded in ball grinder, be filled with Ar after vacuumizing, Ball-milling Time is 6-24 hour, rotating speed is 250-350r/min, ratio of grinding media to material is 6-15:1, filler ratio is 45-55%; Three, high temperature insostatic pressing (HIP): ball milling powder step 2 obtained loads cylindrical stainless steel jacket and carries out high temperature insostatic pressing (HIP), pressure is at 150-300MPa, and holding temperature is 550-700 DEG C, and programming rate is 5-20 DEG C/min, and temperature retention time is 30-120min; Four, hot extrusion: alloy pig step 3 obtained puts into resistance furnace insulation, and holding temperature is 500-700 DEG C, and temperature retention time is 60-180min; Put into heat extruder after insulation terminates and squeeze out cross section for (80 × 10) mm
2alloy slab; Five, cold rolling: it is cold rolling that AgCuTi active solder slab step 4 obtained carries out multi-pass, until thickness is 0.05mm, pass deformation is 20-50%, annealing in process is carried out between every time deformation phases, annealing temperature is 300-700 DEG C, the temperature time is 30-180min, obtains active A gCuTi active solder finished product.
Embodiment six: the present embodiment and embodiment five unlike Ball-milling Time in step 2 12 hours, rotating speed 300r/min, ratio of grinding media to material 10:1, other steps and parameter identical with embodiment five.
Embodiment seven: the present embodiment and embodiment five are 650 DEG C unlike holding temperature in step 3, and temperature retention time is 90min, and pressure is 250MPa, other steps and parameter identical with embodiment five.
Embodiment eight: the present embodiment and embodiment five are 700 DEG C unlike annealing temperature in step 5, and temperature retention time is 10min, other steps and parameter identical with embodiment five.
Embodiment nine: it is 18mm alloy round bar that the present embodiment and embodiment five squeeze out diameter unlike heat extruder in step 4; And it is cold drawn in step 5, AgCuTi active solder round bar to be carried out multi-pass, until diameter is 1.02mm, pass deformation is 10-30%, and annealing temperature is 400-600 DEG C, and the temperature time is 60-120min, other steps and parameter identical with embodiment five.
Fig. 1 is the micro-organization chart of the AgCuTi active solder that embodiment five obtains; Fig. 2 is the component distributing line sweep figure of the AgCuTi active solder that embodiment five obtains; Fig. 3 is that embodiment five obtains the thick AgCuTi active solder photo of 0.05mm; As can be seen from Fig. 1 and Fig. 2, class " nucleocapsid structure " tissue topography formed in AgCuTi alloy after mechanical alloying and high temperature insostatic pressing (HIP), this structure can weaken the circumgranular pressure concentration effect of Ti in plastic history, thus improves the working ability of active solder.
Fig. 4 is the AgCuTi active solder photo that embodiment nine obtains diameter phi 1.02mm; Fig. 5 is the tensile stress-strain curve figure of the AgCuTi active solder that embodiment nine obtains; Following table 1 is the data of mechanical of AgCuTi active solder; Fig. 6 is the stretching fracture shape appearance figure of the AgCuTi active solder that embodiment nine obtains.As can be seen from Figure 6, the fracture mode of active solder is based on ductile rupture, and fracture origin should near fragility Ti particle.
Table 1
Claims (9)
1.AgCuTi active solder, is characterized in that AgCuTi active solder is made up of the Ti of Cu and 1-7% of Ag, 20-35% of 60-75% by mass percentage.
2.AgCuTi active solder, it is characterized in that AgCuTi active solder by mass percentage by the AgCu28 alloyed powder of 93.5%, the electrolysis Cu powder of 5% and 1.5% Ti powder make.
3.AgCuTi active solder, it is characterized in that AgCuTi active solder by mass percentage by the AgCu28 alloyed powder of 92%, the electrolysis Cu powder of 5% and 3% Ti powder make.
4.AgCuTi active solder, it is characterized in that AgCuTi active solder by mass percentage by the AgCu28 alloyed powder of 90%, the electrolysis Cu powder of 5% and 5% Ti powder make.
5. the preparation method of the AgCuTi active solder according to claim 1,2,3 or 4, is characterized in that the preparation method of AgCuTi active solder completes according to following steps:
One, according to the Ti powder of percentage by weight by the AgCu28 alloyed powder of 90-96%, the electrolysis Cu powder of 2-5% and 1-7%, batching;
Two, mechanical alloying: ball milling ball and powder are loaded in ball grinder, be filled with Ar after vacuumizing, Ball-milling Time is 6-24 hour, rotating speed is 250-350r/min, ratio of grinding media to material is 6-15:1, filler ratio is 45-55%;
Three, high temperature insostatic pressing (HIP): ball milling powder step 2 obtained loads cylindrical stainless steel jacket and carries out high temperature insostatic pressing (HIP), pressure is at 150-300MPa, and holding temperature is 550-700 DEG C, and programming rate is 5-20 DEG C/min, and temperature retention time is 30-120min;
Four, hot extrusion: alloy pig step 3 obtained puts into resistance furnace insulation, and holding temperature is 500-700 DEG C, and temperature retention time is 60-180min; Put into heat extruder after insulation terminates and squeeze out cross section for (80 × 10) mm
2alloy slab;
Five, cold rolling: it is cold rolling that AgCuTi active solder slab step 4 obtained carries out multi-pass, until thickness is 0.05mm, pass deformation is 20-50%, annealing in process is carried out between every time deformation phases, annealing temperature is 300-700 DEG C, the temperature time is 30-180min, obtains active A gCuTi active solder finished product.
6. the preparation method of AgCuTi active solder according to claim 5, to is characterized in that in step 2 Ball-milling Time 12 hours, rotating speed 300r/min, ratio of grinding media to material 10:1.
7. the preparation method of AgCuTi active solder according to claim 5, it is characterized in that in step 3, holding temperature is 650 DEG C, temperature retention time is 90min, and pressure is 250MPa.
8. the preparation method of AgCuTi active solder according to claim 5, it is characterized in that in step 5, annealing temperature is 700 DEG C, temperature retention time is 10min.
9. the preparation method of AgCuTi active solder according to claim 5, it is characterized in that in step 4 that heat extruder squeezes out diameter is 18mm alloy round bar; And it is cold drawn in step 5, AgCuTi active solder round bar to be carried out multi-pass, until diameter is 1.02mm, pass deformation is 10-30%, and annealing temperature is 400-600 DEG C, and the temperature time is 60-120min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106493485A (en) * | 2016-11-15 | 2017-03-15 | 张金水 | Welding material containing tungsten, molybdenum, titanium, nickel, nobelium and constantan and preparation method thereof |
| CN106521203A (en) * | 2016-11-14 | 2017-03-22 | 中国工程物理研究院材料研究所 | Preparation method of AgCuTi alloy, preparation method of foil strip brazing filler of AgCuTi alloy, and products of AgCuTi alloy |
| CN108213771A (en) * | 2018-01-15 | 2018-06-29 | 合肥工业大学 | A kind of composite soldering and its soldering processes for soldering silicon carbide ceramics in vacuum |
| CN109622938A (en) * | 2018-12-12 | 2019-04-16 | 江苏阳明船舶装备制造技术有限公司 | It is a kind of to prepare copper alloy surface wear-resistant coating and preparation method with AgCuTi |
| CN113084392A (en) * | 2021-03-29 | 2021-07-09 | 华南理工大学 | Ag-Cu-Ti-Sn-Ni active alloy solder and preparation method thereof |
| WO2023051410A1 (en) * | 2021-09-29 | 2023-04-06 | 比亚迪股份有限公司 | Active metal solder paste composition, solder paste, and method for soldering ceramic and metal |
| CN115922147A (en) * | 2022-12-27 | 2023-04-07 | 云南大学 | Is suitable for Al 2 O 3 High-strength active brazing filler metal for ceramic welding and preparation method thereof |
| CN115958329A (en) * | 2022-12-30 | 2023-04-14 | 无锡日月合金材料有限公司 | Active brazing solder and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106521203A (en) * | 2016-11-14 | 2017-03-22 | 中国工程物理研究院材料研究所 | Preparation method of AgCuTi alloy, preparation method of foil strip brazing filler of AgCuTi alloy, and products of AgCuTi alloy |
| CN106493485A (en) * | 2016-11-15 | 2017-03-15 | 张金水 | Welding material containing tungsten, molybdenum, titanium, nickel, nobelium and constantan and preparation method thereof |
| CN108213771A (en) * | 2018-01-15 | 2018-06-29 | 合肥工业大学 | A kind of composite soldering and its soldering processes for soldering silicon carbide ceramics in vacuum |
| CN108213771B (en) * | 2018-01-15 | 2020-05-22 | 合肥工业大学 | Composite brazing filler metal for brazing silicon carbide ceramic in vacuum and brazing process thereof |
| CN109622938A (en) * | 2018-12-12 | 2019-04-16 | 江苏阳明船舶装备制造技术有限公司 | It is a kind of to prepare copper alloy surface wear-resistant coating and preparation method with AgCuTi |
| CN113084392A (en) * | 2021-03-29 | 2021-07-09 | 华南理工大学 | Ag-Cu-Ti-Sn-Ni active alloy solder and preparation method thereof |
| WO2023051410A1 (en) * | 2021-09-29 | 2023-04-06 | 比亚迪股份有限公司 | Active metal solder paste composition, solder paste, and method for soldering ceramic and metal |
| CN115922147A (en) * | 2022-12-27 | 2023-04-07 | 云南大学 | Is suitable for Al 2 O 3 High-strength active brazing filler metal for ceramic welding and preparation method thereof |
| CN115958329A (en) * | 2022-12-30 | 2023-04-14 | 无锡日月合金材料有限公司 | Active brazing solder and preparation method thereof |
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