CN112593110B - Preparation method of nano-carbide reinforced aluminum matrix composite welding wire - Google Patents
Preparation method of nano-carbide reinforced aluminum matrix composite welding wire Download PDFInfo
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- 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
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- 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
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Abstract
The invention relates to a preparation method of a nano-carbide reinforced aluminum matrix composite welding wire, which has the following basic ideas: firstly, preparing sugar-carbon salt mixed solid, then melting pure aluminum, adding a proper amount of salt to protect aluminum, adding the prepared sugar-carbon salt mixed solid, and waiting for the reaction to be finished. The invention prepares sugar-carbon salt mixed solid by sugar bonding, and takes the mixed solid as a reaction speed control medium, so that the nucleation and growth speed of the nano-particles is reduced to a controllable range, and the growth of the nano-particles is inhibited without using a rapid cooling device. The method has simple production process, does not need special production equipment in the production process, can finish the production by the traditional aluminum alloy production equipment, has low equipment requirement, wide selection range of production raw materials and low comprehensive production cost, and provides possibility for large-scale application of the carbide nano-particle reinforced aluminum-based composite material welding wire.
Description
Technical Field
The invention relates to a preparation method of a nano-carbide reinforced aluminum-based composite welding wire, belonging to the technical field of aluminum alloy materials.
Background
The aluminum alloy has the advantages of high specific strength, specific stiffness, fatigue strength, excellent corrosion resistance and the like, is a preferred material for realizing light structure, and has wide application prospects in the fields of aerospace, automobile traffic and the like. During the use process, the aluminum alloy parts need to be connected with each other, and welding is the most common connection mode in the aluminum alloy field. Because part series of aluminum alloys have higher hot cracking sensitivity, welding wires with the same components as parent materials can not be used as filling materials in the welding process, and the mechanical property of a welding area is poor. For example, the welding of 6061 aluminum alloy mainly uses an ER4043(Al-5Si) or ER5356(Al-5Mg) welding wire as a filling material. Among them, when ER4043 welding wire is used, the strength and plasticity of the weld zone are poor, and when ER5356 welding wire is used, the corrosion resistance and high temperature stability of the weld zone are poor. In particular, for 2000-, 6000-and 7000-series high strength aluminum alloys, no welding wire is currently available that can be effectively welded. Therefore, these high strength aluminum alloys are typically joined using a large number of mechanical fasteners (e.g., rivets) in a practical application, which is labor intensive and time consuming, resulting in a dramatic increase in the cost of using these alloys. In addition, the strength at the riveted joint is also relatively low, where fatigue cracks often rapidly initiate. Therefore, this problem greatly limits the wide use of high strength aluminum alloys.
The nano particles are added into the aluminum alloy, so that the growth of crystal grains can be inhibited in the solidification process, and a fine crystal structure is formed, thereby improving the strength of the alloy. More importantly, the nanoparticles can inhibit dendrite formation and significantly refine the size of the second phase, thereby inhibiting thermal cracking due to feeding difficulties caused by coarse dendrite bridging or coarse second phase and dendrite bridging. Therefore, the welding wire made of the aluminum-based composite material containing the nanoparticles can effectively weld high-strength aluminum alloys having high hot crack sensitivity, such as 2000 series and 7000 series.
The nano carbide ceramic particles are commonly used reinforcing phases in aluminum alloy, have good wettability with an aluminum matrix, can effectively improve the microstructure of the aluminum alloy, such as refining grains and refining the second phase, and are excellent reinforcing phases for preparing the aluminum matrix composite welding wire. However, the existing method for preparing the aluminum-based composite material containing the nano-carbide ceramic particles has high cost and complex process, and the application of the welding wire of the aluminum-based composite material is severely limited.
Patent CN108796251A discloses a method for preparing metal-based nanocomposite, which is a method of adding high content, uniformly dispersed nanoparticle size to target metal by molten salt assistance. The method may incorporate a variety of nanoparticles, including carbide nanoparticles. With the help of molten salt, the combination of the nano particles and the matrix is good, the impurities are few, and the performance is excellent, but the method is an external method, is limited by the cost of the nano particles, and has high product price.
Ton et al (Tong XC, Fan HS. Al-TiC compositions In Situ processed by ingot metal and vertical metal technology: Part I. Microstructural evaluation. Metal Mater Trans A.1998Mar 1; 29(3): 875-91.) produced a nano titanium carbide reinforced aluminum material by using a rapid cooling method. The basic method is that the aluminum melt added with the graphite powder and the titanium is rapidly cooled at the high temperature of 1200 ℃, so that the titanium carbide is rapidly nucleated and separated out in the cooling process, and titanium carbide particles with the size less than 100nm are obtained and can be uniformly dispersed in a matrix. However, the rapid cooling method has high requirements for equipment, low production efficiency and high comprehensive cost, and thus cannot realize industrial production.
In conclusion, if the carbide nanoparticles are prepared into the carbide nanoparticle reinforced aluminum alloy by an external addition method, the carbide nanoparticles are high in price, and the application range of the product is limited. The carbide nano-particles prepared by the rapid cooling method have the same disadvantages, and the rapid cooling method has high production equipment price and low production efficiency, and cannot be produced on a large scale.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the preparation method of the nano-carbide reinforced aluminum-based composite welding wire, the aluminum-based composite welding wire can obviously improve the mechanical property of a welding area, can be used for welding 2000 series, 6000 series and 7000 series high-strength aluminum alloys, and solves the problem of heat cracking in the welding process.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a nano-carbide reinforced aluminum-based composite welding wire comprises the following steps:
(1) mixing and heating salt, a carbon source, a cation source and sugar to melt the sugar to obtain a mixed solid; after being melted, the sugar can be used as a binder to bind salt, a carbon source and a cation source to form a mixed solid, sometimes the mixed carbon source is needed to be used for reaction control, or the mixed cation source is used for preparing multi-cation carbide;
(2) heating and melting pure aluminum to obtain molten aluminum;
(3) adding salt on the surface of the molten aluminum obtained in the step (2), and adding the mixed solid obtained in the step (1) after the salt is completely melted for reaction;
(4) after the reaction is finished, obtaining an aluminum melt containing the nano carbide particles, and casting the aluminum melt containing the nano carbide particles to obtain a nano carbide reinforced pure aluminum composite ingot;
(5) remelting the nano carbide reinforced pure aluminum composite ingot obtained in the step (4), preparing materials according to the components of the target aluminum alloy, and preserving heat to enable alloy elements to be uniformly distributed to obtain a melt;
(6) and (5) cooling the melt obtained in the step (5) to obtain a nano-carbide reinforced aluminum-based composite ingot, and extruding and drawing to obtain the nano-carbide reinforced aluminum-based composite welding wire.
The preparation process of the novel welding wire in the technology of the invention is mainly divided into two stages, firstly, the nanometer composite material ingot required by the welding wire is prepared, and secondly, the thermal deformation is carried out on the obtained composite material ingot to obtain the welding wire with the target size and shape. The preparation of the carbide reinforced aluminum matrix composite material is carried out in the atmosphere.
The basic thought of the preparation method of the invention is as follows: firstly, preparing sugar-carbon salt mixed solid, then melting pure aluminum, adding a proper amount of salt to protect aluminum, adding the prepared sugar-carbon salt mixed solid, and waiting for the reaction to be finished.
The shape of the carbide nano-particles obtained by the reaction is not strictly limited, and the carbide nano-particles can be spherical, polygonal, rod-shaped and lamellar, the size of the synthesized nano-particles is mostly below 100 nanometers, the partial size exceeds 100 nanometers, and the average size is below 100nm nanometers.
Preferably, the mass fraction of the nanoparticles in the carbide nanoparticle reinforced pure aluminum composite ingot is 0.5-50%, and the mass fraction of the carbide nanoparticles in the nano-carbide reinforced aluminum-based composite welding wire is 0.5-20%.
The preparation method of the invention prepares the composite material by generating the nano carbide particles in the aluminum alloy in situ and processes the nano carbide particles into the welding wire, and the welding wire can inhibit the generation of thermal cracks in the solidification process and improve the strength and plasticity of a welding area. Compared with the currently common addition method and rapid cooling method, the preparation process and equipment in the invention are simpler, thereby greatly reducing the production cost.
The present invention prepares sugar-carbon salt mixed solid by using sugar as binder and controls the reaction speed, so as to obtain nano carbide granules.
As a preferable embodiment of the preparation method of the present invention, in the step (1) and the step (2), the mass ratio of the total amount of the cation elements in the cation source to the pure aluminum is less than 0.4: 1; the total amount of the carbon source and the sugar is the carbon amount required by the cation element to form carbide (namely, the carbon amount required by the cation in the cation source to completely form carbide according to the chemical reaction equation), and 10 wt.% to 60 wt.% of the carbon element is additionally added; the mass ratio of the carbon source to the sugar is 0.5-1: 1; the mass ratio of the salt (namely the salt in the step (1)) to the pure aluminum (namely the pure aluminum in the step (2)) is 0.15-0.8: 1.
In a preferred embodiment of the preparation method of the present invention, in the step (1), the carbon source is at least one of activated carbon, carbon nanotubes, graphite, graphene oxide, graphene, pitch, diamond and wood, the sugar is at least one of white sugar, sucrose and glucose, the cation source is at least one of metal tungsten, a tungsten-containing compound, metal titanium, a titanium-containing compound, a silicon-containing compound, a boron-containing compound, metal zirconium, a zirconium-containing compound, metal chromium and a chromium-containing compound, and the salts in the step (1) and the step (3) are at least one of fluoride salt, fluoroaluminate, chloride salt and chloroaluminate, respectively. The salts in the step (1) and the step (3) may be the same or different, and are generally selected to be the same.
The raw material for preparing the aluminum-based nanocomposite is pure aluminum, and is used for providing a carbon source (activated carbon, carbon nanotubes, graphite, graphene oxide, graphene, asphalt, diamond, wood, other carbon-containing compounds and carbon simple substances) of carbon elements in carbide nanoparticles, and different carbon sources are suitable for preparing different carbide nanoparticles; sugar (white sugar, sucrose, glucose, etc.) for preparing sugar-carbon salt mixed solid; salts used for preparing sugar carbonate mixed solids (fluorine salts such as potassium tetrafluoroaluminate, sodium fluoroaluminate, potassium fluoride, sodium fluoride, etc., chlorine salts such as sodium chloride, potassium chloride, magnesium chloride, etc., or other salts having a high melting point and not reacting with the aluminum melt); a material of another element that reacts with carbon, namely a cation source, different cation sources are selected according to the target carbide, and the cation source and the selected carbon source are required to react at a high temperature; for example, tungsten carbide is prepared, and the cation source is tungsten-containing material such as metallic tungsten, tungsten oxide or tungsten chloride, and if titanium carbide is prepared, the cation source is titanium-containing material such as potassium fluotitanate, titanium dioxide powder, metallic titanium powder, aluminum titanium alloy, etc. Other carbides that may be prepared include, but are not limited to, titanium carbide, silicon carbide, boron carbide, zirconium carbide, chromium carbide, and the like.
In a preferred embodiment of the preparation method of the present invention, in the step (1), the heating temperature is 120 to 300 ℃.
In a preferred embodiment of the preparation method of the present invention, in the step (2), the heating temperature is 700 to 1200 ℃.
In a preferred embodiment of the production method of the present invention, the mass ratio of the salt to the aluminum in the step (3) (i.e., the mass of the aluminum in the step (2)) is 0.02 to 0.05: 1.
As a preferable embodiment of the preparation method, in the step (3), the reaction temperature is 750-1200 ℃ and the reaction time is 0.5-12 h.
As a preferred embodiment of the preparation method of the present invention, in the step (4), after the reaction is completed, the residual reactant, the molten salt and the surface impurities on the upper layer of the molten aluminum are removed to obtain the aluminum melt containing the nano carbide particles, and before the casting of the aluminum melt containing the nano carbide particles, refining and degassing are performed.
As a preferred embodiment of the preparation method of the invention, in the step (5), the remelting temperature is 690-900 ℃, and the heat preservation time is 10-30 min. It is noted that some alloying elements have melting points much higher than pure aluminum (e.g., copper), so that in the preparation of aluminum-based nanocomposites containing such elements, the temperature can be raised and the holding time can be extended appropriately, while the size of the raw materials added should be as small as possible to promote the melting of these pure metals.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention prepares sugar-carbon salt mixed solid, takes molten sugar as a binder, improves the traditional casting equipment, and synthesizes carbide nano-particles in situ in molten aluminum by using low-cost raw materials. The obtained nano particles have controllable sizes, and the aluminum matrix composite containing 20 mass percent of carbide nano particles can be prepared at most. The aluminum-based composite material is processed into the welding wire, can be applied to welding of high-strength aluminum alloy, and improves the strength and plasticity of a welding area.
(2) The invention prepares sugar-carbon salt mixed solid by sugar bonding, and takes the mixed solid as a reaction speed control medium, so that the nucleation and growth speed of the nano-particles is reduced to a controllable range, and the growth of the nano-particles is inhibited without using a rapid cooling device. The method has simple production process, does not need special production equipment in the production process, can finish the production by the traditional aluminum alloy production equipment, has low equipment requirement, wide selection range of production raw materials and low comprehensive production cost, and provides possibility for large-scale application of the carbide nano-particle reinforced aluminum-based composite material.
(3) The welding wire of the invention can be used for the same kind welding of high-strength aluminum alloys such as 2000 series, 6000 series and 7000 series and the like and the different kind welding of the alloy series and other series aluminum alloys (such as 5000 series and the like). The invention provides a new choice for the welding wire of the nano carbide ceramic particle reinforced aluminum matrix composite material which can be produced in a large scale.
Drawings
Fig. 1 is a photograph of a TiC nanoparticle reinforced 7075 aluminum matrix composite welding wire of example 1.
FIG. 2 is a photograph of a ZrC nanoparticle reinforced 2024 aluminum alloy wire as in example 2.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
In this embodiment, a novel welding wire made of a nano titanium carbide (TiC) ceramic particle reinforced aluminum matrix composite material comprises the following components in mass ratio: 7075 (5.1% -6.1% Zn, 2.1% -2.9% Mg, 1.2% -2.0% Cu, the balance Al, the content of each element is based on the total weight of each metal element), and 2% (the content of nanoparticles is based on the total weight of nanoparticles and a metal matrix) TiC nanoparticles with the diameter of 40-110nm (the average diameter is less than 100 nm). The production process comprises three parts, firstly synthesizing titanium carbide nano-particle reinforced pure aluminum composite material in situ, wherein the mass fraction of TiC nano-particles in the pure aluminum composite material is 10%, then preparing alloy by using the pure aluminum composite material, preparing cast ingot, and finally extruding and drawing the cast ingot to obtain the nano-carbide ceramic particle reinforced aluminum-based composite material welding wire.
The salt used in the synthesis process is sodium fluoroaluminate, the carbon source is carbon nano tube, the binder is sucrose, and the cation source is potassium fluotitanate.
The preparation process of the novel nano titanium carbide (TiC) ceramic particle reinforced aluminum matrix composite welding wire comprises the following steps:
1) weighing raw materials: according to the mass fraction of TiC in the pure aluminum composite material, potassium fluotitanate with corresponding weight is weighed, the total amount of carbon contained in the carbon nano tube and the cane sugar needs to consider the carbon amount required by all Ti ions to form TiC, 50% is additionally added on the basis, and the mass ratio of the carbon nano tube to the cane sugar is 0.5:1, uniformly mixing all weighed raw materials, wherein the mass ratio of sodium fluoroaluminate to aluminum (namely pure aluminum in the step (1)) is 0.5: 1;
2) heating at 200 deg.C for 1.5 hr, mixing, taking out, and cooling to obtain sugar-carbon salt mixed solid;
3) melting pure aluminum in a crucible and then heating to 1000 ℃;
4) after oxides on the surface of the pure aluminum are removed, adding sodium fluoroaluminate, waiting for the fluoride salt to be melted, and then stabilizing the temperature in the furnace at 1000 ℃, wherein the mass ratio of the sodium fluoroaluminate to the aluminum (namely the pure aluminum in the step (1)) is 0.05: 1;
5) adding sugar carbon salt mixed solid, and reacting for 5.5 hours;
6) after the reaction is finished, pouring out the residual reactant, molten salt and surface impurities on the upper layer, and carrying out deslagging and degassing treatment on the residual aluminum melt;
7) casting the obtained melt to obtain a nano TiC particle reinforced pure aluminum composite ingot;
8) weighing pure Al for dilution and pure Zn, pure Mg and pure Cu of other alloying elements;
9) remelting the prepared nanoparticle reinforced pure aluminum composite material at 800 ℃, adding alloy elements of pure Al, pure Cu, pure Zn and pure Mg into the remelted composite material melt, and preserving heat for 20min to uniformly diffuse the elements;
10) and refining and degassing the melt, casting to obtain a 7075 aluminum alloy ingot reinforced by nano titanium carbide (TiC) ceramic particles, and extruding and drawing the obtained ingot to obtain the 7075 aluminum alloy welding wire reinforced by the nano titanium carbide (TiC) ceramic particles with the diameter of 2.4mm, as shown in figure 1.
The obtained welding wire is used for welding 7075 aluminum alloy plates with the thickness of 3mm, no thermal crack is generated at a welding joint, the grain size of the welding joint is small, and the strength of a welding line reaches 550MPa after T6 treatment.
Example 2
In this embodiment, a novel welding wire made of a nano zirconium carbide (ZrC) ceramic particle reinforced aluminum matrix composite material comprises the following components in mass ratio: 2024 (3.8% -4.9% of Cu, 1.2% -1.8% of Mg and the balance of Al, the content of each element is based on the total weight of each metal element), and 2% (the content of the nanoparticles is based on the total weight of the nanoparticles and the metal matrix) ZrC nanoparticles with a diameter of 60-120nm (the average diameter is less than 100 nm).
The production process is divided into three parts, firstly, zirconium carbide nano-particle reinforced pure aluminum composite material is synthesized in situ, the mass fraction of ZrC nano-particles in the pure aluminum composite material is 15%, then, the pure aluminum composite material is used for preparing alloy, ingot casting is prepared, and finally, the ingot casting is extruded and drawn to obtain the nano-carbide ceramic particle reinforced aluminum-based composite material welding wire.
The salt used in the synthesis process is potassium fluoroaluminate, the carbon source is diamond powder, the binder is glucose, and the cation source is potassium fluorozirconate.
The preparation process of the novel nano titanium carbide (ZrC) ceramic particle reinforced aluminum matrix composite welding wire comprises the following steps:
1) weighing raw materials: weighing potassium fluorozirconate with corresponding weight according to the mass fraction of ZrC in the pure aluminum composite material, wherein the total amount of carbon contained in diamond and glucose needs to consider the amount of carbon required by all Zr ions to form ZrC, and additionally adding 20 percent on the basis, wherein the mass ratio of diamond to sucrose is 1:1, uniformly mixing all weighed raw materials, wherein the mass ratio of potassium fluoroaluminate to aluminum (namely the pure aluminum in the step (1)) is 0.4: 1;
2) heating the mixture at 180 ℃, stirring for 2 hours, uniformly mixing, taking out and cooling to obtain a sugar-carbon salt mixed solid;
3) melting pure aluminum in a crucible and then heating to 1200 ℃;
4) after oxides on the surface of the pure aluminum are removed, adding potassium fluoroaluminate, waiting until the fluorine salt is melted, and then stabilizing the temperature in the furnace at 1200 ℃, wherein the mass ratio of the potassium fluoroaluminate to the aluminum (namely the pure aluminum in the step (1)) is 0.03: 1;
5) the sugar carbonate mixed solid is added, and the crucible can be covered by a cover, so that the possible oxidation reaction is reduced. The reaction process lasts for 4 hours;
6) after the reaction is finished, pouring out surface reaction residues, molten salt and surface impurities, removing slag from the remaining aluminum melt, and degassing;
7) casting the obtained melt to obtain a ZrC nano particle reinforced pure aluminum composite ingot;
8) weighing pure Al for dilution and pure Cu and pure Mg for alloying;
9) remelting the prepared nanoparticle reinforced pure aluminum composite material at 800 ℃, adding pure Al, pure Cu and pure Mg into the remelted composite material melt, and preserving heat for 20min to uniformly diffuse elements;
10) refining and degassing the melt, casting to obtain a 2% nano zirconium carbide (ZrC) ceramic particle reinforced 2024 aluminum alloy ingot, and extruding, drawing and coiling the obtained ingot to obtain the nano zirconium carbide (ZrC) particle reinforced 2024 aluminum alloy welding wire with the diameter of 1.2mm, as shown in figure 2.
Example 3
In this embodiment, a novel welding wire made of a nano zirconium carbide (ZrC) ceramic particle reinforced aluminum matrix composite material comprises the following components in mass ratio: 2024 (3.8% -4.9% of Cu, 1.2% -1.8% of Mg and the balance of Al, wherein the content of each element is based on the total weight of each metal element), and 2% (the content of the nanoparticles is based on the total weight of the nanoparticles and the metal matrix) of ZrC nanoparticles with a diameter of 40-100 nm.
The production process is divided into three parts, firstly, zirconium carbide nano-particle reinforced pure aluminum composite material is synthesized in situ, the mass fraction of ZrC nano-particles in the pure aluminum composite material is 20%, then, the pure aluminum composite material is used for preparing alloy, ingot casting is prepared, and finally, the ingot casting is extruded and drawn to obtain the nano-carbide ceramic particle reinforced aluminum-based composite material welding wire.
The salt used in the synthesis process is potassium fluoroaluminate, the carbon source is diamond powder, the binder is glucose, and the cation source is potassium fluorozirconate.
The preparation process of the novel nano titanium carbide (ZrC) ceramic particle reinforced aluminum matrix composite welding wire comprises the following steps:
1) weighing raw materials: weighing potassium fluorozirconate according to the mass fraction of ZrC in the pure aluminum composite material, wherein the total amount of carbon contained in diamond and glucose needs to consider the amount of carbon required by all Zr ions to form ZrC, and additionally adding 10 percent on the basis, wherein the mass ratio of diamond to sucrose is 0.5:1, uniformly mixing all weighed raw materials, wherein the mass ratio of potassium fluoroaluminate to aluminum (namely the pure aluminum in the step (1)) is 0.15: 1;
2) heating the mixture at 120 ℃, stirring for 2 hours, uniformly mixing, taking out and cooling to obtain a sugar-carbon salt mixed solid;
3) melting pure aluminum in a crucible and then heating to 900 ℃;
4) after oxides on the surface of the pure aluminum are removed, adding potassium fluoroaluminate, waiting until the fluorine salt is melted, and then stabilizing the temperature in the furnace at 900 ℃, wherein the mass ratio of the potassium fluoroaluminate to the aluminum (namely the pure aluminum in the step (1)) is 0.02: 1;
5) the sugar carbonate mixed solid is added, and the crucible can be covered by a cover, so that the possible oxidation reaction is reduced. The reaction process lasts for 8 hours, and the reaction temperature is 900 ℃;
6) after the reaction is finished, pouring out surface reaction residues, molten salt and surface impurities, removing slag from the remaining aluminum melt, and degassing;
7) casting the obtained melt to obtain a ZrC nano particle reinforced pure aluminum composite ingot;
8) weighing pure Al for dilution and pure Cu and pure Mg for alloying;
9) remelting the prepared nanoparticle reinforced pure aluminum composite material at 700 ℃, adding pure Al, pure Cu and pure Mg into the remelted composite material melt, and preserving heat for 30min to uniformly diffuse elements;
10) and refining and degassing the melt, casting to obtain a 2% nano zirconium carbide (ZrC) ceramic particle reinforced 2024 aluminum alloy ingot, and extruding, drawing and coiling the obtained ingot to obtain the nano zirconium carbide (ZrC) particle reinforced 2024 aluminum alloy welding wire with the diameter of 1.2 mm.
Example 4
In this embodiment, a novel welding wire made of a nano tungsten carbide (WC) ceramic particle reinforced aluminum matrix composite material includes the following components by mass: 6061 (0.4% -0.8% Si, 0.8% -1.2% Mg, 0.04% -0.35% Cu, the balance Al, the content of each element is based on the total weight of each metal element), 0.5% (the content of the nano-particles is based on the total weight of the nano-particles and the metal matrix) WC nano-particles with the diameter of 50-110nm (the average diameter is less than 100 nm).
The production process is divided into three parts, firstly, tungsten carbide nano-particle reinforced pure aluminum composite material is synthesized in situ, the mass fraction of WC nano-particles in the pure aluminum composite material is 50%, then, the pure aluminum composite material is used for preparing alloy, ingot casting is prepared, and finally, the ingot casting is extruded and drawn to obtain the nano-carbide ceramic particle reinforced aluminum-based composite material welding wire.
The salt used in the synthesis process is potassium fluoroaluminate, the carbon source is diamond powder, the binder is glucose, and the cation source is tungsten oxide.
The preparation process of the novel nano titanium carbide (WC) ceramic particle reinforced aluminum-based composite welding wire comprises the following steps:
1) weighing raw materials: according to the mass fraction of WC in the pure aluminum composite material, tungsten oxide with corresponding weight is weighed, the total amount of carbon contained in diamond and glucose needs to consider the carbon amount required by all W ions to form WC, 60% is additionally added on the basis, and the mass ratio of diamond to sucrose is 0.8:1, uniformly mixing all weighed raw materials, wherein the mass ratio of potassium fluoroaluminate to aluminum (namely the pure aluminum in the step (1)) is 0.8: 1;
2) heating the mixture at 300 ℃, stirring for 2 hours, uniformly mixing, taking out and cooling to obtain a sugar-carbon salt mixed solid;
3) melting pure aluminum in a crucible and then heating to 1000 ℃;
4) after oxides on the surface of the pure aluminum are removed, adding potassium fluoroaluminate, waiting until the temperature in the furnace is stabilized at 1200 ℃ after the villiaumite is melted, wherein the mass ratio of the potassium fluoroaluminate to the aluminum (namely the pure aluminum in the step (1)) is 0.05: 1;
5) the sugar carbonate mixed solid is added, and the crucible can be covered by a cover, so that the possible oxidation reaction is reduced. The reaction process lasts for 12h, and the reaction temperature is 1200 ℃;
6) after the reaction is finished, pouring out surface reaction residues, molten salt and surface impurities, removing slag from the remaining aluminum melt, and degassing;
7) casting the obtained melt to obtain a WC nano particle reinforced pure aluminum composite ingot;
8) weighing pure Al for dilution, pure Cu for alloying, pure Mg and Al-Si intermediate alloy;
9) remelting the prepared nanoparticle reinforced pure aluminum composite material at 700 ℃, adding pure Al, pure Cu and pure Mg into the remelted composite material melt, and preserving heat for 10min to uniformly diffuse elements;
10) and refining and degassing the melt, casting to obtain a 0.5% nano tungsten carbide (WC) ceramic particle reinforced 2024 aluminum alloy ingot, and extruding and drawing the obtained ingot to obtain the nano tungsten carbide (WC) particle reinforced 6061 aluminum alloy welding wire with the diameter of 3.0 mm.
The obtained welding wire is used for welding 6061 aluminum alloy plates, the quality of a welding joint is good, no hot crack occurs, the structure of the welding joint is uniform and fine and is isometric crystal, and the tensile strength of the joint is 300MPa after the joint is treated by T6.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The preparation method of the nano-carbide reinforced aluminum-based composite welding wire is characterized by comprising the following steps of:
(1) mixing and heating salt, a carbon source, a cation source and sugar to melt the sugar to obtain a mixed solid;
(2) heating and melting pure aluminum to obtain molten aluminum;
(3) adding salt on the surface of the molten aluminum obtained in the step (2), and adding the mixed solid obtained in the step (1) after the salt is completely melted for reaction;
(4) after the reaction is finished, obtaining an aluminum melt containing the nano carbide particles, and casting the aluminum melt containing the nano carbide particles to obtain a nano carbide reinforced pure aluminum composite ingot;
(5) remelting the nano carbide reinforced pure aluminum composite ingot obtained in the step (4), preparing materials according to the components of the target aluminum alloy, and preserving heat to obtain a melt;
(6) and (5) cooling the melt obtained in the step (5) to obtain a nano-carbide reinforced aluminum-based composite ingot, and extruding and drawing to obtain the nano-carbide reinforced aluminum-based composite welding wire.
2. The method of claim 1, wherein the mass fraction of nanoparticles in the carbide nanoparticle reinforced pure aluminum composite ingot is 0.5-50%; the mass fraction of carbide nano particles in the nano carbide reinforced aluminum matrix composite welding wire is 0.5-20%, and the average particle size of the carbide nano particles is less than 100 nm.
3. The method according to claim 1, wherein in the steps (1) and (2), the mass ratio of the total amount of the cation elements in the cation source to the pure aluminum is less than 0.4: 1; the total consumption of the carbon source and the sugar is that 10 wt.% to 60 wt.% of carbon element is additionally added on the basis of the carbon amount required by the cation element to form carbide; the mass ratio of the carbon source to the sugar is 0.5-1: 1; the mass ratio of the salt to the pure aluminum is 0.15-0.8: 1.
4. The preparation method according to claim 1, wherein in the step (1), the carbon source is at least one of activated carbon, carbon nanotubes, graphite, graphene oxide, graphene, pitch, diamond and wood, the sugar is at least one of white sugar, sucrose and glucose, the cation source is at least one of metal tungsten, a tungsten-containing compound, metal titanium, a titanium-containing compound, a silicon-containing compound, a boron-containing compound, metal zirconium, a zirconium-containing compound, metal chromium and a chromium-containing compound, and the salts in the step (1) and the step (3) are at least one of fluoride salt, fluoroaluminate salt, chloride salt and chloroaluminate salt, respectively.
5. The method according to claim 1, wherein the heating temperature in the step (1) is 120 to 300 ℃.
6. The method according to claim 1, wherein the heating temperature in the step (2) is 700 to 1200 ℃.
7. The method according to claim 1, wherein in the step (3), the mass ratio of the salt to the aluminum is 0.02 to 0.05: 1.
8. The method according to claim 1, wherein in the step (3), the reaction temperature is 750 to 1200 ℃ and the reaction time is 0.5 to 12 hours.
9. The method according to claim 1, wherein in the step (4), after the reaction is finished, residual reactants, molten salt and surface impurities on the upper layer of the molten aluminum are removed to obtain the aluminum melt containing the nano carbide particles, and refining degassing is performed before the aluminum melt containing the nano carbide particles is cast.
10. The method according to claim 1, wherein in the step (5), the remelting temperature is 690-900 ℃ and the holding time is 10-30 min.
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