EP1740343A2 - Substances auxiliaires non corrosives, basees sur des alcalins de fluoroaluminate et contenant des metallates co-precipites, pour soudure a l'aluminium - Google Patents

Substances auxiliaires non corrosives, basees sur des alcalins de fluoroaluminate et contenant des metallates co-precipites, pour soudure a l'aluminium

Info

Publication number
EP1740343A2
EP1740343A2 EP05715974A EP05715974A EP1740343A2 EP 1740343 A2 EP1740343 A2 EP 1740343A2 EP 05715974 A EP05715974 A EP 05715974A EP 05715974 A EP05715974 A EP 05715974A EP 1740343 A2 EP1740343 A2 EP 1740343A2
Authority
EP
European Patent Office
Prior art keywords
compounds
alkali
auxiliaries
auxiliaries according
preparation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP05715974A
Other languages
German (de)
English (en)
Inventor
Ulrich Seseke-Koyro
Andreas Becker
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Solvay Fluor GmbH
Original Assignee
Solvay Fluor GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Solvay Fluor GmbH filed Critical Solvay Fluor GmbH
Publication of EP1740343A2 publication Critical patent/EP1740343A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings or fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • C22B21/062—Obtaining aluminium refining using salt or fluxing agents
    • 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
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings or fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/362—Selection of compositions of fluxes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/48—Halides, with or without other cations besides aluminium
    • C01F7/50—Fluorides
    • C01F7/54—Double compounds containing both aluminium and alkali metals or alkaline-earth metals

Definitions

  • the invention relates to non-corrosive auxiliaries based on alkali fluoroaluminates for aluminum soldering and / or for refining aluminum alloys, the production of the auxiliaries and their use as a flux for soldering components made of aluminum and aluminum alloys or as an additive for introducing metals into aluminum alloys.
  • Assemblies of parts made of aluminum or aluminum alloys can be manufactured by soldering these parts.
  • a flux based on fluoroaluminate is used for this, which frees the surface of the components to be soldered to one another from oxidic buildup.
  • Fluxes based on potassium fluoroaluminate are particularly suitable for soldering aluminum or low-magnesium aluminum alloys. Such a method is disclosed in British Patent GB 1,438,955. The preparation of corresponding fluxes is described, for example, by Willenberg, US Pat. No. 4,428,920 and Meshri, US Pat. No. 5,318,764 and Kawase, US Pat. No. 4,579,605. Magnesium-containing aluminum alloys can be soldered with good results using a flux composition containing cesium. The addition of certain metal silicates in certain quantities can make the solder metal unnecessary.
  • the procedure is such that the flux and a solder metal are applied to the components to be connected.
  • the flux can be applied, for example, in the form of a slurry, as an aqueous suspension, as a paste or powder.
  • the components are assembled in the desired position and heated. First the flux melts and cleans the surface, then the solder melts. The parts are then allowed to cool.
  • the object of the invention is to provide non-corrosive auxiliaries which can be used as fluxes or for refining alloys, and to provide a process for the preparation of these novel non-corrosive auxiliaries based on alkali metal fluoroaluminates.
  • the new auxiliaries are said to improve solder flow and improve the surface, for example.
  • the non-corrosive auxiliaries according to the invention are characterized by a content of co-precipitated or admixed metallates.
  • auxiliaries based on alkali metal fluoroaluminates are produced by known manufacturing processes, in which the reactants hydrogen fluoride, aluminum hydroxide (alumina hydrate) and alkali compound, preferably alkali hydroxide and at least one metal compound, preferably in the form of their salts, e.g. Halides, nitrates, carbonates, sulfates, phosphates, borates or hexafluorosilicates and / or their oxides are brought into contact with one another.
  • the reactants hydrogen fluoride, aluminum hydroxide (alumina hydrate) and alkali compound, preferably alkali hydroxide and at least one metal compound, preferably in the form of their salts, e.g. Halides, nitrates, carbonates, sulfates, phosphates, borates or hexafluorosilicates and / or their oxides are brought into contact with one another.
  • the auxiliaries according to the invention are preferably used as a flux for soldering components made of aluminum and / or aluminum alloys, the composition of the surfaces of the components to be soldered functionalizing at the same time due to their composition.
  • the auxiliaries according to the invention are also suitable as an additive in aluminum production or as an additive for introducing metals into aluminum for the purpose of alloy refinement.
  • the base compound alkali fluoroaluminate is usually prepared by reacting alumina hydrate with hydrofluoric acid to fluoroaluminic acid in a first process step.
  • This fluoroaluminic acid reacts in a precipitation step with an aqueous alkali compound, whereupon the desired alkali salts of the complex fluorides of aluminum are precipitated.
  • the auxiliaries according to the invention based on alkali fluoroaluminates are prepared by reacting alumina hydrate (aluminum oxide thhydrate) with hydrogen fluoride in the presence of an alkali compound, in one embodiment according to the invention metal compounds of the 2nd to 5th main group of the periodic table of the elements, in particular compounds of strontium, indium, tin, antimony or bismuth, preferably in the form of their salts, in particular their halides, nitrates, carbonates or their oxides, are added to the reaction mixture.
  • alumina hydrate aluminum oxide thhydrate
  • hydrogen fluoride in the presence of an alkali compound
  • metal compounds of the 2nd to 5th main group of the periodic table of the elements in particular compounds of strontium, indium, tin, antimony or bismuth, preferably in the form of their salts, in particular their halides, nitrates, carbonates or their oxides, are added to the reaction mixture.
  • metal compounds of the subgroup elements are elements with atomic numbers 21 to 30 inclusive, atomic numbers 39 to 47 inclusive and / or atomic numbers 57 to 79 inclusive, preferably in the form of their salts, in particular their halides, nitrates, carbonates and / or oxides added to the reaction mixture.
  • Suitable compounds of the subgroup elements are, for example, compounds of zirconium, niobium, cerium, yttrium or lanthanum.
  • the metal compounds can be used both individually or in combination with one another, e.g. in the form of mixtures in the reaction system.
  • the use of complex metal compounds, e.g. ⁇ ZrF, ⁇ TiFß and / or mixtures of these with each other is also possible.
  • all metal compounds of the main and sub-group elements which are electrochemically more noble than the component to be soldered made of aluminum or aluminum alloys, are suitable for functionalizing the component surface.
  • the functionalization of the surface arises from the fact that, due to the electrochemical series of voltages, the metal ion contained in the flux reacts with the less noble surface of the component activated by the flux and is reduced to metal during the melting process. This redox reaction is probably not to be regarded as a priority when using metal compounds of the 2nd main group, since other effects, e.g. Lowering the surface energy.
  • the ionically bonded metal is reduced and "alloyed" during the melting process.
  • the time of addition of the main and / or subgroup compounds mentioned can be varied.
  • the addition to the hydrogen fluoride, which is advantageous when using poorly soluble metal compounds, or after the formation of the fluoroaluminic acid, is made here in the mixture of alumina hydrate and fluorine. Hydrogen. It is also possible to add the metal compound to the reaction mixture of hydrogen fluoride, alumina hydrate and alkali compound.
  • the metal compounds are introduced into the reaction mixture after the formation of the fluoroaluminic acid and before the addition of the alkali compound.
  • Alkali salts or alkali metal hydroxides are used as the alkali compound, as individual substances or as alkali salt or alkali hydroxide mixtures in the form of their solutions or as solids, alkali representing lithium, sodium, potassium, rubidium or cesium, preferably potassium.
  • the procedure is such that an aqueous hydrogen fluoride solution is initially introduced, alumina hydrate (aluminum oxide trihydrate) and main and / or subgroup metal compound are added, and then alkali metal hydroxide, preferably potassium hydroxide, is added.
  • alkali metal hydroxide preferably potassium hydroxide
  • alkali fluoroaluminate refers in particular to alkali tetrafluoroaluminate, alkali pentafluoroaluminate and alkali hexafluoroaluminate, and their hydrates.
  • Alkali stands for lithium, sodium, potassium, cesium or rubidium, preferably for potassium.
  • the properties of the alkali fluoroaluminates can be Flux can be changed, for example, by incorporating cesium into a potassium aluminum fluoride matrix, the magnesium tolerance of the flux can be increased.
  • Zirconium oxide, niobium oxide, lanthanum oxide, yttrium oxide or cerium oxide introduced. These oxides are mixed into the reaction mixture, preferably before adding the potassium hydroxide solution.
  • the metal compound is brought into contact with the hydrogen fluoride presented, that is to say introduced into the reaction mixture before the alumina is added.
  • the metal compounds are used in amounts of up to 30% by weight, preferably 0.01 to 20% by weight, based on the alkali metal fluorate.
  • the amount of metal compound added depends on the degree of functionalization of the surfaces, depending on the application.
  • the metals are chemically bound in the form of their metallates or are contained in the form of admixtures.
  • the metal ions are incorporated into the potassium aluminum fluoride crystal lattice if the metal compounds are introduced into the reaction system before the addition of the alkali compound, preferably alkali hydroxide, in particular potassium hydroxide solution.
  • the alkali compound preferably alkali hydroxide, in particular potassium hydroxide solution.
  • a mechanical mixture of the metal compounds with the alkali aluminum fluorides or alkali fluoroaluminates is also possible, but very inhomogeneous element-specific hygroscopic mixtures with indifferent solubilities are obtained.
  • the performance properties of the auxiliary according to the invention can be varied and controlled so that a specific property profile can be set.
  • the flux in addition to its known effect, namely cleaning the surface by removing the oxide layer, is capable of the flux activity, for example by influencing the viscosity and influencing the surface tension of the solder metal, positively to change.
  • the smoothness of the surface can be improved.
  • This effect can probably be explained by the fact that the metallates built into the alkali fluoroaluminate undergo an electro-chemical reaction with the cleaned or activated surface of the aluminum components to be soldered during the soldering process, so that a surface change (functionalization) is brought about.
  • This functionalized surface can in turn lead to an improvement in the solder flow (increased solder activity), a reduced roughness of the solidified flux after the soldering process, or even a surface coating, which make a subsequent “conversion coating” unnecessary.
  • the flux can be applied to the aluminum or aluminum alloy components to be connected in a manner known per se, e.g. by spraying, brushing or dipping, in the form of aqueous or organic suspensions.
  • the flux can also be applied to the components to be soldered using modern technologies, such as plasma or high-speed spray coating.
  • Dry application using electrostatic spray technology is also possible.
  • the flux can also be applied in the form of aqueous or organic suspensions, as a varnish or as a paste to the components to be connected.
  • Aqueous or organic slurries advantageously contain 10 to 75% by weight of the flux.
  • the substances normally used as organic solvents such as alcohols, in particular methanol, ethanol, propanol or isopropanol and polyols, can be used as organic liquids.
  • suitable organic liquids are e.g. pyrrolidones or ethers, e.g. Diethylene glycol monobutyl ether, or ketones such as acetone, or esters of alcohols, diols or polyols.
  • binders are added to the flux e.g. Ethyl cellulose added.
  • film formers usually polymers, which are soluble in organic solvents, for example acetone, if necessary, solder metal or solder metal precursors can be applied to the workpiece simultaneously with the flux.
  • Suitable polymers are, for example Acrylates, polyvinyls, polyamines, polyenes, polyisoprenes or similar compounds with correspondingly functionalized organic radicals. Most of these organic compounds, known as film formers, evaporate during the soldering process.
  • soldering temperature depends on the solder used or the solder-forming metal. Soldering is preferably carried out above the melting point of the solder or the conversion phases of the flux or its mixtures.
  • solder metal liquidus temperature 450 ° C
  • soft soldering moreover of "hard soldering”.
  • high melting solders e.g. Zinc-aluminum solders that melt from 390 ° C or pure zinc solder that can be used from 420 ° C for soldering. It is preferred to solder at 390 to 620 ° C, with ambient pressure.
  • Flame soldering or furnace soldering, especially under an inert atmosphere are suitable process processes.
  • the auxiliary according to the invention is suitable as a flux for soldering components made of aluminum or aluminum alloys both in the presence of solder and without the addition of solder if the corresponding solder metal precursor is added.
  • the auxiliary according to the invention can also be used to alloy the corresponding metals in aluminum melts or aluminum alloys.
  • the auxiliary according to the invention can also be used to alloy the corresponding metals in aluminum melts or aluminum alloys.
  • it is reduced to the metal and thus made available to the aluminum as an alloying agent.
  • Example 1 Production of a functional flux, here: NOCOLOK®-lanthanum
  • Hydrofluoric acid was placed in a suitable container which can be thermostatted from the outside, provided with a stirrer and dropping funnel and appropriate protection against loss of evaporation of hydrogen fluoride, and diluted with 100 g of water.
  • the appropriate amount of Al (OH) 3 and additional water to control the exotherm were added to this acid solution with stirring using the dropping funnel.
  • the lanthanum oxide was added in portions, followed by the addition of the potassium hydroxide solution.
  • This reaction solution was stirred for a further 30 minutes and then filtered.
  • the filter residue after drying at 200 ° C gave a white powder with a weight of 71 grams with 0.73% lanthanum.
  • the differential thermal analysis (DTA), the X-ray diffraction spectrum (XRD) and also a scanning electron microscope (SEM) surface analysis were used for the analytical characterization of the new flux. The values were compared with the values of the well-known NOCOLOK® fluxes.
  • the XRD analysis primarily showed the presence of the potassium aluminum phases, KAIF4 and the so-called phase 1, which are also known from the NOCOLOK®. Comments on the DTA:
  • the DAT for NOCOLOK-lanthanum showed an endothermicity (melting range) known for NOCOLOK® and a characteristic curve that allows conclusions to be drawn about the analogous melting behavior and solderability.
  • Example 2 Production of a functional flux, here: NOCOLOK® zirconium
  • Hydrofluoric acid was weighed into a suitable vessel and diluted with 135.4 ml of deionized water. 39 g of Al (OH) 3 were then carefully metered into the dilute HF solution with stirring at about 170 rpm under temperature control. The KOH solution was then metered in via a dropping funnel. After a reaction time of about 30 minutes, the K 2 ZrF 6 was added in portions and the mixture was stirred for a further 30 minutes. The precipitated solid was filtered off.
  • this XRD evaluation primarily showed the presence of the potassium aluminum phases, KAIF4 and the so-called phase 1, which are known as the NOCOLOK® phase.
  • the DAT for NOCOLOK zirconium also showed an endothermicity (melting range) known for NOCOLOK®.
  • Example 3 Production of a functional flux, here: NOCOLOK® bismuth
  • This XRD evaluation also primarily showed the presence of the potassium aluminum phases, KAIF4 and the so-called phase 1, which are known as the NOCOLOK® phase.
  • the DAT for NOCOLOK®-bismuth also showed an endothermia (melting range) known for NOCOLOK®.
  • Comparative surface analysis which was carried out after soldering, showed that less roughness and crystallite formation occurred when using NOCOLOK®-lanthanum or also NOCOLOK®-zirconium than with parts soldered with standardized NOCOLOK®.
  • auxiliaries according to the invention when used as fluxes (NOCOLOK® metallates), produce a smoother surface and thus cause a reduced microorganism attack on, for example, soldered capacitors.
  • the formation of nest structures accumulation of microorganisms
  • the growth of the microorganisms is additionally inhibited or suppressed by the intrinsically cytokinetic effect of the transition metal ions. All in all, this can result in improved hygiene in air-conditioning operation.
  • Comparative spreading test activity test:
  • the fluxes according to the invention clearly showed a quantitatively larger spreading area, which can be interpreted with an improved flux activity (lower surface tension).
  • this enlargement of the spreading area means that smaller amounts of the flux according to the invention are required, with additional functionalization of the surface to be soldered being achieved, for example in the form of a metallization of the surface.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Nonmetallic Welding Materials (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne des substances auxiliaires non corrosives utilisées pour la soudure à l'aluminium et pour la purification d'alliages d'aluminium à base de fluoroaluminates alcalins, leur préparation et leur utilisation. L'invention a également pour objet des métallates contenant des substances auxiliaires non corrosives de l'invention. Afin de former des métallates, sont utilisés en tant que partenaires réactionnels, des composés métalliques des éléments du 2ème au 5ème groupe principal du tableau périodique des éléments ou des éléments des sous-groupes, sous la forme de leurs sels ou de leurs oxydes. Notamment, les composés utilisés sont par ex. leurs halogénures, nitrates, carbonates, sulfates, phosphates, borates, hexafluorosilicates ou oxydes. Selon l'invention, les composés métalliques sont introduits dans le mélange réactionnel comprenant de l'acide fluorhydrique et/ou de l'hydrate d'alumine et/ou un composé alcalin, l'instant d'adjonction du composé métallique pouvant varier en fonction du degré de fonctionnalisation souhaité de la surface.
EP05715974A 2004-03-20 2005-03-11 Substances auxiliaires non corrosives, basees sur des alcalins de fluoroaluminate et contenant des metallates co-precipites, pour soudure a l'aluminium Withdrawn EP1740343A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE102004013841 2004-03-20
DE102004028093A DE102004028093A1 (de) 2004-03-20 2004-06-09 Nichtkorrosive Hilfsstoffe zum Aluminiumlöten
PCT/EP2005/002609 WO2005092563A2 (fr) 2004-03-20 2005-03-11 Substances auxiliaires non corrosives pour soudure a l'aluminium

Publications (1)

Publication Number Publication Date
EP1740343A2 true EP1740343A2 (fr) 2007-01-10

Family

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Application Number Title Priority Date Filing Date
EP05715974A Withdrawn EP1740343A2 (fr) 2004-03-20 2005-03-11 Substances auxiliaires non corrosives, basees sur des alcalins de fluoroaluminate et contenant des metallates co-precipites, pour soudure a l'aluminium

Country Status (9)

Country Link
US (1) US20070277908A1 (fr)
EP (1) EP1740343A2 (fr)
JP (1) JP2007529322A (fr)
KR (1) KR20060132004A (fr)
BR (1) BRPI0508978A (fr)
DE (1) DE102004028093A1 (fr)
MX (1) MXPA06010750A (fr)
RU (1) RU2006137081A (fr)
WO (1) WO2005092563A2 (fr)

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Also Published As

Publication number Publication date
KR20060132004A (ko) 2006-12-20
WO2005092563A2 (fr) 2005-10-06
RU2006137081A (ru) 2008-04-27
DE102004028093A1 (de) 2005-10-06
WO2005092563A3 (fr) 2005-11-24
BRPI0508978A (pt) 2007-08-28
US20070277908A1 (en) 2007-12-06
MXPA06010750A (es) 2007-04-19
JP2007529322A (ja) 2007-10-25

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