WO2023015784A1 - Pâte de brasage pour brasage sans flux d'acier inoxydable et son procédé de préparation, matériau de brasage cuivre-manganèse-nickel-cobalt, et application - Google Patents

Pâte de brasage pour brasage sans flux d'acier inoxydable et son procédé de préparation, matériau de brasage cuivre-manganèse-nickel-cobalt, et application Download PDF

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Publication number
WO2023015784A1
WO2023015784A1 PCT/CN2021/135209 CN2021135209W WO2023015784A1 WO 2023015784 A1 WO2023015784 A1 WO 2023015784A1 CN 2021135209 W CN2021135209 W CN 2021135209W WO 2023015784 A1 WO2023015784 A1 WO 2023015784A1
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stainless steel
parts
copper
brazing
solder paste
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PCT/CN2021/135209
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English (en)
Chinese (zh)
Inventor
龙伟民
钟素娟
黄俊兰
裴夤崟
张冠星
薛行雁
聂孟杰
李文彬
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郑州机械研究所有限公司
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Publication of WO2023015784A1 publication Critical patent/WO2023015784A1/fr

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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
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries
    • 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
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/002—Soldering by means of induction heating
    • 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
    • B23K35/40—Making wire or rods for soldering or welding

Definitions

  • the invention belongs to the technical field of brazing materials, and in particular relates to a solder paste for stainless steel flux-free brazing, a preparation method thereof, a copper-manganese-nickel-cobalt solder and applications thereof.
  • stainless steel has superior high temperature performance and good corrosion resistance, and is widely used in the manufacture of heat exchanger piping.
  • stainless steel heat exchangers have become heat exchange devices commonly used in metallurgy, chemical industry, energy, transportation, light industry, food and other industrial sectors.
  • Brazing is a key link in the manufacture of stainless steel heat exchanger piping, which determines the service life of the heat exchanger. With the improvement of people's quality of life, the requirements for the welding quality of stainless steel heat exchangers are getting higher and higher. The welding quality of stainless steel heat exchangers is largely dependent on the brazing material used.
  • H1CuNi30-2-0.2 (Ni27 ⁇ 30; Si1.5 ⁇ 2.0; B0.2, Cu balance) widely used in the aviation industry has a melting temperature range of 1080 ⁇ 1200°C and a working temperature of up to 600°C (Zou Xi, Brazing Welding", high-temperature copper-based solder), has the advantages of good high-temperature performance, low cost, and good compatibility with stainless steel, and is often used for brazing stainless steel in protective atmosphere furnaces.
  • the existing H1CuNi30-2-0.2 solder does not have self-brazing properties. When brazing stainless steel in an atmosphere furnace, the dense oxide film on the surface of the stainless steel is difficult to remove when the brazing temperature is lower than 1000 ° C.
  • the purpose of the present invention is to provide a solder paste for stainless steel flux-free brazing, which can realize flux-free brazing of stainless steel in an atmospheric environment and improve joint strength.
  • the second object of the present invention is to provide a preparation method of the above-mentioned solder paste for stainless steel flux-free brazing.
  • the third object of the present invention is to provide a copper-manganese-nickel-cobalt solder for stainless steel brazing.
  • the fourth object of the present invention is to provide the application of the above solder paste in induction brazing stainless steel.
  • the technical scheme of the solder paste for stainless steel brazing without flux of the present invention is:
  • solder paste for stainless steel brazing without flux is mainly composed of water, sodium silicate, nano silicon dioxide and copper-based solder; the solder paste is made of the following raw materials in parts by weight : 70-80 parts of copper-based solder, 3-5 parts of nano silicon dioxide, 1-3 parts of sodium hydroxide, 10-15 parts of water; the copper-based solder is composed of the following components in mass percentage: Mn 26.0 ⁇ 30.0%, Ni 26.0 ⁇ 30.0%, Co 4.0 ⁇ 6.0%, B 0.1 ⁇ 0.5%, Li 0.1 ⁇ 0.6%, Na 0.1 ⁇ 0.2%, K 0.01 ⁇ 0.3%, Cu balance.
  • the solder paste of the present invention contains water, sodium silicate, and nano-silica paste, which is dehydrated at high temperature to form a thin film during brazing, and the nano-silica in it can build a three-dimensional network structure, which has a large surface area and a very large surface area.
  • High activity will enhance the strength and high temperature resistance of the film and form a high temperature resistant film.
  • the film isolates the air, protects the surface to be brazed, and the molten solder is not oxidized, and realizes flux-free brazing of stainless steel in an atmospheric environment; at the same time, nano-silica particles are pinned in the brazing seam, which also helps to strengthen the stainless steel joint strength.
  • the above-mentioned improved copper-based solder is based on H1CuNi30-2-0.2 solder, adding Mn, Co, and reducing Cu, so that the melting temperature of the solder is between 930 and 970 ° C, which can reduce the brazing temperature .
  • a certain amount of B and Li elements are added to the solder, and the solder has self-brazing properties. This is because B and Li can reduce oxides on the surface of stainless steel, such as Cr 2 O 3 , and the melting point of the reduction product is lower than the brazing temperature, and it floats in the form of a liquid film on the surface of the base metal and the molten solder to protect it.
  • the viscosity of B oxide is very high, which will hinder the spreading of solder. For this reason, a small amount of Na and K elements are added.
  • the viscosity of Na and K oxides is small, which can reduce the viscosity of the reduction product, promote the wetting of the film and the spreading of the solder, and enhance the self-brazing performance of the solder.
  • the solder paste is made of the following raw materials in parts by weight: 74 to 80 parts of copper-based solder, 3 to 5 parts of nano silicon dioxide, 1 to 3 parts of sodium hydroxide, water 12 to 15 servings. More preferably, the copper-based solder is composed of the following components by mass percentage: Mn 28.0-30.0%, Ni 28.0-30.0%, Co 4.0-6.0%, B 0.3-0.5%, Li 0.4-0.6%, Na 0.1 ⁇ 0.2%, K 0.15 ⁇ 0.3%, Cu balance.
  • the particle size of the nano silicon dioxide is 30-50 nm.
  • the technical scheme of copper-manganese-nickel-cobalt solder for stainless steel brazing of the present invention is:
  • a copper-manganese-nickel-cobalt solder for stainless steel brazing which consists of the following components in mass percentage: Mn 26.0-30.0%, Ni 26.0-30.0%, Co 4.0-6.0%, B 0.1-0.5%, Li 0.1-0.6 %, Na 0.1-0.2%, K 0.01-0.3%, Cu balance.
  • the copper-manganese-nickel-cobalt brazing material for stainless steel brazing of the present invention has low brazing temperature (beneficial for suppressing the growth of stainless steel crystal grains), strong wetting and spreading ability, and is aimed at conventional matching In the case of using flux, the amount of flux can be reduced or no flux can be used.
  • the copper-manganese-nickel-cobalt solder for stainless steel brazing consists of the following components in mass percentage: Mn 28.0-30.0%, Ni 28.0-30.0%, Co 4.0-6.0%, B 0.3-0.5%, Li 0.4 ⁇ 0.6%, Na 0.1 ⁇ 0.2%, K 0.15 ⁇ 0.3%, Cu balance.
  • the technical scheme of the preparation method of the solder paste for stainless steel brazing without flux of the present invention is:
  • a preparation method of solder paste for stainless steel flux-free brazing comprising the following steps:
  • step 2) reacting the alkaline aqueous solution obtained in step 1) with nano silicon dioxide under conditions higher than normal pressure to obtain a suspension;
  • the preparation method of the solder paste for stainless steel brazing without flux has a simple preparation process, the obtained solder paste has high stability, and can effectively improve the brazing effect of stainless steel brazing.
  • the above-atmospheric pressure condition refers to a steam pressure of 0.3-0.5 MPa.
  • the reaction time is 3.0-5.0 hours.
  • the technical solution for the application of the above-mentioned solder paste is: the application of the above-mentioned solder paste in induction brazing stainless steel.
  • the stainless steel is brazed and connected in an atmospheric environment without flux.
  • the above-mentioned solder paste is used without brazing flux, which can realize rapid induction brazing of stainless steel in the atmospheric environment, does not pollute the environment, and is green and environmentally friendly.
  • Fig. 1 is the preparation schematic diagram of solder paste of the present invention
  • Fig. 2 is the spreading morphology when the existing H1CuNi30-2-0.2 brazing filler metal is carried out without flux spreading performance test under atmospheric environment;
  • Fig. 3 is the spreading morphology of the solder paste obtained in Example 5 of the present invention when the flux-free spreading performance test is performed in an atmospheric environment.
  • the amount of nano silicon dioxide is controlled to be relatively excessive, and the reaction with sodium hydroxide consumes a part of the nano silicon dioxide, and the other part remains in the liquid to form a suspension.
  • the suspension is dehydrated at high temperature to form a thin film, in which the excess nano-silica is a three-dimensional network structure with a large surface area and great activity, which will enhance the strength and high temperature resistance of the film and form a high temperature resistant film.
  • the film isolates the air, protects the surface to be brazed and the molten solder from being oxidized.
  • the nano-silica particles are pinned into the brazing joint and also help to strengthen the stainless steel joint.
  • the above-mentioned suspension can enhance the high temperature resistance of the film formed by mucus dehydration, and on the other hand, the nano-silica in it will be pinned to the brazing joint to enhance the strength of the joint.
  • the parts by weight of the raw materials used consist of: 70 parts of copper-based solder powder, 3 parts of nano silicon dioxide, 3 parts of sodium hydroxide, 10 parts of deionized water; the mass percent of each component in the copper-based solder powder is: Mn26.0%, Ni26.0%, Co4.0%, B0.1%, Li0.1%, Na0.1% , K0.01%, Cu balance.
  • step (2) Add nano-silica (30-50nm) into step (1) alkaline aqueous solution, put it in a high-pressure reactor, and react for 3.0 hours under 0.3MPa steam pressure to form a suspension (transparent colloidal liquid + a small amount of silicon dioxide); the reaction process schematic diagram is as shown in Figure 1;
  • step (3) Add copper-based solder powder into the suspension liquid in step (2), mix and stir to form a uniform paste, and obtain solder paste.
  • the preparation method of the solder paste for stainless steel flux-free brazing of the present embodiment the parts by weight of the raw materials used consist of: 72 parts of copper-based solder powder, 4 parts of nano silicon dioxide, 2 parts of sodium hydroxide, 11 parts of deionized water; the mass percent of each component in the copper-based solder powder is: Mn27.0%, Ni27.0%, Co5.0%, B0.2%, Li0.2%, Na0.1% , K0.1%, Cu balance.
  • the specific preparation method is basically the same as that of Example 1, except that in step (2), the steam pressure is 0.4 MPa, and the reaction time is 4.0 h.
  • the parts by weight of the raw materials used consist of: 74 parts of copper-based solder powder, 5 parts of nano silicon dioxide, 1 part of sodium hydroxide, 12 parts deionized water.
  • the mass percentage of each component in copper-based solder powder is: Mn28.0%, Ni28.0%, Co6.0%, B0.3%, Li0.4%, Na0.2%, K0.15%, Cu margin.
  • the specific preparation method is basically the same as that of Example 1, except that in step (2), the steam pressure is 0.5 MPa, and the reaction time is 5.0 h.
  • the preparation method of the solder paste for stainless steel flux-free brazing of the present embodiment the parts by weight of the raw materials used consist of: 76 parts of copper-based solder powder, 3 parts of nano silicon dioxide, 3 parts of sodium hydroxide, 14 parts deionized water.
  • the mass percentage of each component in copper-based solder powder is: Mn29.0%, Ni29.0%, Co4.0%, B0.4%, Li0.5%, Na0.1%, K0.2%, Cu margin.
  • Concrete preparation method is with embodiment 1.
  • the preparation method of the solder paste for stainless steel flux-free brazing of the present embodiment the parts by weight of the raw materials used consist of: 80 parts of copper-based solder powder, 5 parts of nano silicon dioxide, 2 parts of sodium hydroxide, 15 parts deionized water.
  • the mass percentage of each component in copper-based solder powder is: Mn30.0%, Ni30.0%, Co5.0%, B0.5%, Li0.6%, Na0.2%, K0.3%, Cu margin.
  • Concrete preparation method is with embodiment 1.
  • step (3) the reaction is controlled under a pressure of 0.3 to 0.5 MPa for 3.0 to 5.0 hours, for example, the reaction is carried out at 0.5 MPa for 3.0 hours. h, or under 0.4MPa to react for 5.0h, the reaction effect is basically equivalent to that of Example 1.
  • solder paste for stainless steel flux-free brazing of the present invention respectively correspond to the solder paste obtained by the preparation methods of the above-mentioned Examples 1-5, and will not be described in detail here.
  • the purpose of this experiment example is to compare the shear strength of brazing joints with different solders.
  • the base metal of the test is a stainless steel plate with a thickness of 3 mm, a width of 20 mm, and a length of 80 mm.
  • Brazing gas-shielded brazing temperature needs to be maintained between 1170 ° C ⁇ 1200 ° C), and then respectively adopt the solder paste of embodiments 1 to 5 to carry out the flux-free induction brazing of 304 stainless steel plates in the atmosphere (brazing The welding temperature is between 1050°C and 1100°C), and the six joints are processed into standard shear specimens (according to the provisions of GB/T 11364-2008), and the shear strength of the comparison joints is tested.
  • Table 1 The results are shown in Table 1.

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Abstract

Une pâte de brasage destinée à un brasage sans flux d'acier inoxydable est divulguée. La pâte de brasage est principalement composée d'eau, de silicate de sodium, de dioxyde de silicium nanométrique et d'un matériau de brasage à base de cuivre. La pâte de brasage est préparée à partir des matières premières suivantes en parties en poids : 70 à 80 parties d'un matériau de brasage à base de cuivre, 3 à 5 parties de dioxyde de silicium nanométrique, 1 à 3 parties d'hydroxyde de sodium et 10 à 15 parties d'eau. Selon la pâte de brasage, la pâte comprenant de l'eau, du silicate de sodium et du dioxyde de silicium nanométrique est déshydratée à une température élevée pendant le brasage pour former un film mince, le dioxyde de silicium nanométrique pouvant construire une structure de réseau tridimensionnel qui présente une grande surface et une grande activité et qui augmenterait la solidité et la résistance à haute température du film mince, de telle sorte qu'un film mince résistant aux hautes températures est formé. Le film mince isole l'air, empêche une surface à braser et un matériau de brasage fondu d'être oxydés, et réalise un brasage sans flux d'acier inoxydable dans un environnement atmosphérique ; de plus, des particules de dioxyde de silicium nanométrique sont fixées dans une soudure et facilitent également l'amélioration de la résistance d'un joint en acier inoxydable. Un procédé de préparation d'une pâte de brasage, une application et un matériau de brasage cuivre-manganèse-nickel-cobalt sont également divulgués.
PCT/CN2021/135209 2021-08-12 2021-12-03 Pâte de brasage pour brasage sans flux d'acier inoxydable et son procédé de préparation, matériau de brasage cuivre-manganèse-nickel-cobalt, et application WO2023015784A1 (fr)

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