CN104227008B - A kind of preparation method of titanium zirconium German silver solder powder - Google Patents
A kind of preparation method of titanium zirconium German silver solder powder Download PDFInfo
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- CN104227008B CN104227008B CN201410489744.4A CN201410489744A CN104227008B CN 104227008 B CN104227008 B CN 104227008B CN 201410489744 A CN201410489744 A CN 201410489744A CN 104227008 B CN104227008 B CN 104227008B
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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
- B23K35/02—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
-
- 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
- B23K35/0244—Powders, particles or spheres; Preforms made therefrom
-
- 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
- B23K35/0255—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in welding
-
- 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
-
- 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
-
- 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
- B23K35/22—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
- B23K35/302—Cu 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
- B23K35/22—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
- B23K35/3033—Ni 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
- B23K35/22—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
- B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
-
- 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
- B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
- B23K35/325—Ti 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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/38—Selection of media, e.g. special atmospheres for surrounding the working area
-
- 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
- B23K35/38—Selection of media, e.g. special atmospheres for surrounding the working area
- B23K35/383—Selection of media, e.g. special atmospheres for surrounding the working area mainly containing noble gases or nitrogen
Abstract
The preparation method who the invention provides a kind of titanium zirconium German silver solder powder, comprises the following steps: one, prepare yittrium oxide protective coating at the melting kettle inner surface of powder by atomization equipment; Two, titanium sponge, sponge zirconium, oxygen-free copper and electrolytic nickel are joined to melting in melting kettle, obtain aluminium alloy; Three, aluminium alloy is poured in the tundish of powder by atomization equipment, then proceeded in spray chamber and carry out atomization processing by mozzle, obtain titanium zirconium German silver solder powder. The present invention has overcome the excessive demand of traditional centrifugal atomizing technology to equipment, technique, the titanium zirconium German silver solder powder quality uniformity that adopts the present invention to prepare, chemical composition stability, total impurities and oxygen content are low, processing performance is superior, meets the requirement of various fields to high-quality titanium-base alloy solder powder completely.
Description
Technical field
The invention belongs to brazing material preparing technical field, be specifically related to a kind of titanium zirconium German silver solderThe preparation method of powder.
Background technology
At present, many for titanium alloy, titanium-Al series metal compounds, ceramic material and composite etc.Planting welding material multiselect money base active solder or the titanium base of advanced material soldering and diffusion welding (DW) connection livesProperty solder etc., and TiZrCuNi class alloy is the solder of thinking at present best, particularly for high temperatureJoint under operation and high corrosive environment. Because TiZrCuNi solder alloy itself is more crisp, processingPoor performance, solder foil preparation difficulty, is therefore generally used with pulverulence.
TiZrCuNi solder alloy powder adopts centrifugal atomizing powder process method or special gas atomization mostlyPowder process method is prepared from. The titanium zirconium German silver solder powder that for example Russia produces adopts centrifugal exactlyPrepared by atomization, but centrifugal atomizing method is very high to equipment precision requirement, at present domesticly there is no this type ofProcess equipment. Special gas atomization (as without crucible eddy-current heating gas atomization) need to first be madeStandby diameter 16mm～20mm, the pole of length 1500mm～3000mm, then eddy-current heating Cheng JinBelong to liquid, by the continuous molten metal flow nozzle without any contact, make powder by inert gas atomizer afterwardsEnd. But this method technique more complicated, and the larger alloy bar material of preparation fragility itself just comparesDifficulty, is unsuitable for large-scale industrialization and produces. And adopt traditional powder by gas-atomization technique, pass throughMetal material melting in common crucible is aluminium alloy, then aluminium alloy is poured into tundish, then executesBe prepared into powder with inert gas atomizer. Because the technology controlling and process of traditional powder by gas-atomization technique is thickRoughening, the activity of adding titanium, zirconium is larger, makes the solder powder chemical composition prepared unstable,Oxygen content is very high, and processing performance is very poor, cannot meet user demand.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, provides a kind ofThe simple preparation method of titanium zirconium German silver solder powder efficiently. The titanium zirconium copper that adopts the method to prepareNickel alloy solder powder, its quality uniformity, chemical composition stability, total impurities and oxygen content are low,Processing performance is superior, meets each application completely the technology of high-quality titanium-base alloy solder powder is wantedAsk.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of titanium zirconium corronilThe preparation method of solder powder, is characterized in that, the method comprises the following steps:
Step 1, by yittrium oxide, yttrium colloidal sol and deionized water in mass ratio 1: (1～1.2): (0.4～0.5)Mix, obtain glue, then glue is evenly coated on to the melting kettle of powder by atomization equipmentInner surface, obtains yittrium oxide protective coating at the inner surface of melting kettle after natural drying;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting under the condition of 840 DEG C～860 DEG C5min～8min, obtains aluminium alloy;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is that argon gas, atomizing pressure are 3MPa～3.5MPa at atomizing mediumCondition under carry out atomization processing, obtain titanium zirconium German silver solder powder after naturally cooling; Described titaniumIn zirconium German silver solder powder, the quality percentage composition of zirconium is 13%～40%, and the quality percentage of copper containsAmount is 15%～21%, and the quality percentage composition of nickel is 7%～20%, and surplus is titanium and inevitableImpurity.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 1Described in yttrium colloidal sol the quality percentage composition of yittrium oxide be 10%～15%.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 1Described in the material of melting kettle be magnesia.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 2Described in the trade mark of titanium sponge be MHT-100, the trade mark of described sponge zirconium is HZr-01, described nothingThe trade mark of oxygen copper is TU0, and the trade mark of described electrolytic nickel is Ni9999.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 3Described in the material of tundish be graphite.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 3Described in the internal diameter of mozzle be 3mm～4mm.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 3Described in titanium zirconium German silver solder powder the quality percentage composition of zirconium be 20%～37.5%, the matter of copperAmount percentage composition is 15%～20%, and the quality percentage composition of nickel is 10%～20%, and surplus is titanium and notEvitable impurity.
The preparation method of above-mentioned a kind of titanium zirconium German silver solder powder, is characterized in that step 3Described in titanium zirconium German silver solder powder the quality percentage composition of oxygen be not more than 0.25%.
The present invention compared with prior art has the following advantages:
1, first the present invention adopts the processing method of melting kettle being carried out to yttria-coating protective coating,Thereby having overcome melting kettle easy impurity of introducing in the time of melting titanium, zirconium isoreactivity element pollutes and oxygenThe problem of content overproof, has avoided again traditional centrifugal atomizing technique to wait for equipment, technique simultaneouslyHigh requirement.
2, the present invention adopts conventional equipment to prepare titanium zirconium German silver solder powder, and by meltingAnd the Precise control of atomization process, not only simplify and prepared titanium-base alloy solder powder for equipmentRequirement, has reduced manufacturing cost, and overcome that solder powder chemical composition is unstable, oxygen content is high,Cannot meet the technological deficiencies such as user demand. The present invention can not only prepare high-quality titanium zirconium copper nickel and closeGold brazing filler metal powder, applicable equally for the preparation of other various Ti-based active solder powder.
3, the titanium zirconium German silver solder powder that adopts the present invention to prepare, its quality uniformity, changesLearn stable components, total impurities is not more than 0.36%, and wherein oxygen content is not more than 0.25%, manufacturabilityCan be superior, meet the technical requirement of each application to high-quality titanium-base alloy solder powder completely.
The oxygen content of the titanium zirconium German silver solder powder that 4, prepared by employing the present invention is low, is not more than0.25wt%, alloying component uniformity, soldering spreadability and joint filling are very superior, completely satisfiedSoldering processes requirement.
5, the present invention can be used for multiple titanium alloy, titanium-Al series metal compounds, ceramic material, blackThe brazing of the material such as non-ferrous metal, composite; Can use vacuum brazing furnace, vacuum diffusion weldingStoves etc. carry out soldering, pricker is coated with and diffusion welding (DW), and technological requirement requires quite, also can with general vacuum brazingCarry out soldering and pricker painting, technological requirement and general sense with employing argon shield high-frequency induction brazing equipment etc.Answer soldering requirement suitable.
Below in conjunction with embodiment, the present invention is described in further detail.
Detailed description of the invention
The present invention adopts powder by gas-atomization technique to prepare titanium zirconium German silver solder powder, adoptsPowder by atomization equipment belongs to the commercially available common equipment being easy to get, comprise smelting furnace, tundish, mozzle,The parts such as spray chamber, gas protection system, powder gathering system, control system. Wherein, smelting furnaceInside be provided with melting kettle, tundish is positioned at spray chamber top and is connected with spray chamber by mozzleLogical, in spray chamber, be provided with the high pressure nozzle for aluminium alloy being atomized into a large amount of fine drop.
Embodiment 1
The nominal chemical composition of the present embodiment titanium zirconium to be prepared German silver solder powder is:Ti-37.5Zr-15Cu-10Ni. The preparation method of the present embodiment titanium zirconium German silver solder powder comprise withLower step:
Step 1, yittrium oxide, yttrium colloidal sol are mixed in mass ratio with deionized water at 1: 1.05: 0.45Evenly, obtain glue, then glue is evenly coated on to the interior table of the melting kettle of powder by atomization equipmentFace, obtains yittrium oxide protective coating at the inner surface of melting kettle after natural drying; Institute in the present embodimentThe yttrium colloidal sol adopting is preferably yittrium oxide quality percentage composition and accounts for 12% yttrium colloidal sol, and melting kettle is preferredFor the crucible of magnesia material;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting 6min under the condition of 850 DEG C,Obtain aluminium alloy; The titanium sponge adopting in the present embodiment is preferably MHT-100 titanium sponge and presses caking,Sponge zirconium is preferably HZr-01 atomic energy level sponge zirconium and presses caking, and oxygen-free copper is preferably TU0 oxygen-free copper,Electrolytic nickel is preferably Ni9999 electrolytic nickel;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is the bar that argon gas, atomizing pressure are 3.5MPa at atomizing mediumUnder part, carry out atomization processing, obtain adopting in titanium zirconium German silver solder powder the present embodiment after naturally coolingWith mozzle be preferably the mozzle of internal diameter 4mm, tundish is preferably the tundish of graphite material;
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by the present embodimentBe 37.29%, the quality percentage composition of copper is 15.05%, and the quality percentage composition of nickel is 10.10%,The quality percentage composition of titanium is 37.23%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by the present embodiment, carry out oxygen content detection, record the present embodimentIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.22%. Explanation is adopted thusThe titanium zirconium German silver solder powder of preparing with the present embodiment, its quality uniformity, total impurities andOxygen content is low, and processing performance is superior, meets each application completely to high-quality titanium-base alloy solder powderThe technical requirement at end.
Embodiment 2
The nominal chemical composition of the present embodiment titanium zirconium to be prepared German silver solder powder is:Ti-35Zr-15Cu-15Ni. The preparation method of the present embodiment titanium zirconium German silver solder powder comprises followingStep:
Step 1, yittrium oxide, yttrium colloidal sol are mixed all in mass ratio with deionized water at 1: 1.1: 0.4Even, obtain glue, then glue is evenly coated on to the inner surface of the melting kettle of powder by atomization equipment,After natural drying, obtain yittrium oxide protective coating at the inner surface of melting kettle; In the present embodiment, adoptYttrium colloidal sol be preferably yittrium oxide quality percentage composition and account for 13% yttrium colloidal sol, melting kettle is preferably oxygenChange the crucible of magnesium material;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting 8min under the condition of 840 DEG C,Obtain aluminium alloy; The titanium sponge adopting in the present embodiment is preferably MHT-100 titanium sponge and presses caking,Sponge zirconium is preferably HZr-01 atomic energy level sponge zirconium and presses caking, and oxygen-free copper is preferably TU0 oxygen-free copper,Electrolytic nickel is preferably Ni9999 electrolytic nickel;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is the condition that argon gas, atomizing pressure are 3MPa at atomizing mediumUnder carry out atomization processing, obtain adopting in titanium zirconium German silver solder powder the present embodiment after naturally coolingMozzle be preferably the mozzle of internal diameter 3.5mm, tundish is preferably the tundish of graphite material;
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by the present embodimentBe 34.78%, the quality percentage composition of copper is 15.07%, and the quality percentage composition of nickel is 15.10%,The quality percentage composition of titanium is 34.73%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by the present embodiment, carry out oxygen content detection, record the present embodimentIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.21%. Explanation is adopted thusThe titanium zirconium German silver solder powder of preparing with the present embodiment, its quality uniformity, total impurities andOxygen content is low, and processing performance is superior, meets each application completely to high-quality titanium-base alloy solder powderThe technical requirement at end.
Embodiment 3
The nominal chemical composition of the present embodiment titanium zirconium to be prepared German silver solder powder is:Ti-20Zr-20Cu-20Ni. The preparation method of the present embodiment titanium zirconium German silver solder powder comprises followingStep:
Step 1, yittrium oxide, yttrium colloidal sol are mixed all in mass ratio with deionized water at 1: 1.2: 0.5Even, obtain glue, then glue is evenly coated on to the inner surface of the melting kettle of powder by atomization equipment,After natural drying, obtain yittrium oxide protective coating at the inner surface of melting kettle; In the present embodiment, adoptYttrium colloidal sol be preferably yittrium oxide quality percentage composition and account for 15% yttrium colloidal sol, melting kettle is preferably oxygenChange the crucible of magnesium material;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting 5min under the condition of 860 DEG C,Obtain aluminium alloy; The titanium sponge adopting in the present embodiment is preferably MHT-100 titanium sponge and presses caking,Sponge zirconium is preferably HZr-01 atomic energy level sponge zirconium and presses caking, and oxygen-free copper is preferably TU0 oxygen-free copper,Electrolytic nickel is preferably Ni9999 electrolytic nickel;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is the bar that argon gas, atomizing pressure are 3.2MPa at atomizing mediumUnder part, carry out atomization processing, obtain adopting in titanium zirconium German silver solder powder the present embodiment after naturally coolingWith mozzle be preferably the mozzle of internal diameter 4mm, tundish is preferably the tundish of graphite material;
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by the present embodimentBe 19.66%, the quality percentage composition of copper is 20.11%, and the quality percentage composition of nickel is 20.09%,The quality percentage composition of titanium is 39.78%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by the present embodiment, carry out oxygen content detection, record the present embodimentIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.23%. Explanation is adopted thusThe titanium zirconium German silver solder powder of preparing with the present embodiment, its quality uniformity, total impurities andOxygen content is low, and processing performance is superior, meets each application completely to high-quality titanium-base alloy solder powderThe technical requirement at end.
Embodiment 4
The nominal chemical composition of the present embodiment titanium zirconium to be prepared German silver solder powder is:Ti-40Zr-21Cu-7Ni. The preparation method of the present embodiment titanium zirconium German silver solder powder comprises followingStep:
Step 1, yittrium oxide, yttrium colloidal sol are mixed in mass ratio with deionized water at 1: 1: 0.4,Obtain glue, then glue is evenly coated on to the inner surface of the melting kettle of powder by atomization equipment, fromAfter being so dried, obtain yittrium oxide protective coating at the inner surface of melting kettle; In the present embodiment, adoptYttrium colloidal sol is preferably yittrium oxide quality percentage composition and accounts for 10% yttrium colloidal sol, and melting kettle is preferably oxidationThe crucible of magnesium material;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting 5min under the condition of 860 DEG C,Obtain aluminium alloy; The titanium sponge adopting in the present embodiment is preferably MHT-100 titanium sponge and presses caking,Sponge zirconium is preferably HZr-01 atomic energy level sponge zirconium and presses caking, and oxygen-free copper is preferably TU0 oxygen-free copper,Electrolytic nickel is preferably Ni9999 electrolytic nickel;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is the bar that argon gas, atomizing pressure are 3.5MPa at atomizing mediumUnder part, carry out atomization processing, obtain adopting in titanium zirconium German silver solder powder the present embodiment after naturally coolingWith mozzle be preferably the mozzle of internal diameter 3mm, tundish is preferably the tundish of graphite material;
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by the present embodimentBe 38.92%, the quality percentage composition of copper is 21.25%, and the quality percentage composition of nickel is 7.29%,The quality percentage composition of titanium is 32.18%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by the present embodiment, carry out oxygen content detection, record the present embodimentIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.24%. Explanation is adopted thusThe titanium zirconium German silver solder powder of preparing with the present embodiment, its quality uniformity, total impurities andOxygen content is low, and processing performance is superior, meets each application completely to high-quality titanium-base alloy solder powderThe technical requirement at end.
Embodiment 5
The nominal chemical composition of the present embodiment titanium zirconium to be prepared German silver solder powder is:Ti-13Zr-15Cu-20Ni. The preparation method of the present embodiment titanium zirconium German silver solder powder comprises followingStep:
Step 1, yittrium oxide, yttrium colloidal sol are mixed all in mass ratio with deionized water at 1: 1.2: 0.5Even, obtain glue, then glue is evenly coated on to the inner surface of the melting kettle of powder by atomization equipment,After natural drying, obtain yittrium oxide protective coating at the inner surface of melting kettle; In the present embodiment, adoptYttrium colloidal sol be preferably yittrium oxide quality percentage composition and account for 15% yttrium colloidal sol, melting kettle is preferably oxygenChange the crucible of magnesium material;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting 8min under the condition of 840 DEG C,Obtain aluminium alloy; The titanium sponge adopting in the present embodiment is preferably MHT-100 titanium sponge and presses caking,Sponge zirconium is preferably HZr-01 atomic energy level sponge zirconium and presses caking, and oxygen-free copper is preferably TU0 oxygen-free copper,Electrolytic nickel is preferably Ni9999 electrolytic nickel;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is the condition that argon gas, atomizing pressure are 3MPa at atomizing mediumUnder carry out atomization processing, obtain adopting in titanium zirconium German silver solder powder the present embodiment after naturally coolingMozzle be preferably the mozzle of internal diameter 4mm, tundish is preferably the tundish of graphite material;
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by the present embodimentBe 12.85%, the quality percentage composition of copper is 15.10%, and the quality percentage composition of nickel is 20.04%,The quality percentage composition of titanium is 51.65%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by the present embodiment, carry out oxygen content detection, record the present embodimentIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.23%. Explanation is adopted thusThe titanium zirconium German silver solder powder of preparing with the present embodiment, its quality uniformity, total impurities andOxygen content is low, and processing performance is superior, meets each application completely to high-quality titanium-base alloy solder powderThe technical requirement at end.
Comparative example 1
The preparation method of this comparative example titanium zirconium German silver solder powder and the difference of embodiment 1 are onlyBe: do not apply and prepare yittrium oxide protective coating at the inner surface of melting kettle.
After testing, the quality percentage composition of zirconium in the titanium zirconium German silver solder powder that prepared by this comparative exampleBe 36.53%, the quality percentage composition of copper is 15.62%, and the quality percentage composition of nickel is 10.41%,The quality percentage composition of titanium is 35.87%, and surplus is impurity (comprising oxygen). In addition, right emphaticallyIn titanium zirconium German silver solder powder prepared by this comparative example, carry out oxygen content detection, record this comparative exampleIn the titanium zirconium German silver solder powder of preparation, the quality percentage composition of oxygen is 0.94%. Explanation thus,The present invention is applied and is prepared yittrium oxide protective coating by the inner surface at melting kettle, can effectively stopTitanium, zirconium isoreactivity element react with crucible, significantly reduce total impurities and the oxygen content of finished product powder.
The above, be only preferred embodiment of the present invention, not the present invention imposed any restrictions. AllThat any simple modification, change and the equivalence of above embodiment being done according to invention technical spirit becomesChange, all still belong in the protection domain of technical solution of the present invention.
Claims (6)
1. a preparation method for titanium zirconium German silver solder powder, is characterized in that, the method bagDraw together following steps:
Step 1, by yittrium oxide, yttrium colloidal sol and deionized water in mass ratio 1: (1～1.2): (0.4～0.5)Mix, obtain glue, then glue is evenly coated on to the melting kettle of powder by atomization equipmentInner surface, obtains yittrium oxide protective coating at the inner surface of melting kettle after natural drying; Described yttrium is moltenIn glue, the quality percentage composition of yittrium oxide is 10%～15%; The material of described melting kettle is magnesia;
Step 2, according to the Composition Design requirement of titanium zirconium German silver solder powder to be prepared, willTitanium sponge, sponge zirconium, oxygen-free copper join and in step 1, are coated with yittrium oxide protection together with electrolytic nickelIn the melting kettle of coating, in argon gas atmosphere protection, temperature is melting under the condition of 840 DEG C～860 DEG C5min～8min, obtains aluminium alloy;
Step 3, aluminium alloy described in step 2 is poured in the tundish of powder by atomization equipment, thenProceeding in spray chamber by mozzle, is that argon gas, atomizing pressure are 3MPa～3.5MPa at atomizing mediumCondition under carry out atomization processing, obtain titanium zirconium German silver solder powder after naturally cooling; Described titaniumIn zirconium German silver solder powder, the quality percentage composition of zirconium is 13%～40%, and the quality percentage of copper containsAmount is 15%～21%, and the quality percentage composition of nickel is 7%～20%, and surplus is titanium and inevitableImpurity.
2. the preparation method of a kind of titanium zirconium German silver solder powder according to claim 1,It is characterized in that, the trade mark of titanium sponge described in step 2 is MHT-100, the trade mark of described sponge zirconiumFor HZr-01, the trade mark of described oxygen-free copper is TU0, and the trade mark of described electrolytic nickel is Ni9999.
3. the preparation method of a kind of titanium zirconium German silver solder powder according to claim 1,It is characterized in that, the material of tundish described in step 3 is graphite.
4. the preparation method of a kind of titanium zirconium German silver solder powder according to claim 1,It is characterized in that, the internal diameter of mozzle described in step 3 is 3mm～4mm.
5. the preparation method of a kind of titanium zirconium German silver solder powder according to claim 1,It is characterized in that, in the zirconium of titanium described in step 3 German silver solder powder, the quality percentage composition of zirconium is20%～37.5%, the quality percentage composition of copper is 15%～20%, and the quality percentage composition of nickel is10%～20%, surplus is titanium and inevitable impurity.
6. a kind of preparation side of titanium zirconium German silver solder powder according to claim 1 or 5Method, is characterized in that, in the zirconium of titanium described in step 3 German silver solder powder, the quality percentage of oxygen containsAmount is not more than 0.25%.
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| CN104772578B (en) * | 2015-04-10 | 2018-01-09 | 北京航空航天大学 | A kind of solder for including titanium zirconium cupro-nickel |
| CN105033504A (en) * | 2015-08-28 | 2015-11-11 | 河南科技大学 | Brazing filler metal containing lanthanum and neodymium elements for titanium alloy brazing and preparation method thereof |
| CN106001587B (en) * | 2016-06-30 | 2019-09-10 | 安泰（霸州）特种粉业有限公司 | Prepare iron-based water atomised soft-magnetic alloy powder tundish and its manufacturing method |
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| CN110625127A (en) * | 2019-11-05 | 2019-12-31 | 西北有色金属研究院 | Preparation method of cobalt-chromium-nickel-tungsten alloy brazing filler metal powder |
| CN110625128A (en) * | 2019-11-05 | 2019-12-31 | 西北有色金属研究院 | Preparation method of titanium-copper-nickel-chromium alloy brazing filler metal powder |
| CN111872594A (en) * | 2020-07-22 | 2020-11-03 | 郑州机械研究所有限公司 | Titanium-based brazing filler metal and preparation method and application thereof |
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