CN110129792B - Method and device for preparing composite pipe/coating by full-liquid stirring and semi-solid stirring coating method - Google Patents
Method and device for preparing composite pipe/coating by full-liquid stirring and semi-solid stirring coating method Download PDFInfo
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- CN110129792B CN110129792B CN201910465558.XA CN201910465558A CN110129792B CN 110129792 B CN110129792 B CN 110129792B CN 201910465558 A CN201910465558 A CN 201910465558A CN 110129792 B CN110129792 B CN 110129792B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
- C23C26/02—Coating not provided for in groups C23C2/00 - C23C24/00 applying molten material to the substrate
Abstract
The invention discloses a method and a device for preparing a composite pipe/coating by a full-liquid stirring and semi-solid stirring coating method. In a full-liquid or semi-solid molten pool formed by a coating material, a liquid phase is pressed and stirred by a ceramic tool rotating at a high speed, on one hand, the liquid phase is stirred to be uniformly mixed and flow back along the pipe wall, on the other hand, the liquid phase is driven to rotate at a high speed by the rotating tool, so that the liquid phase is stirred, and high-speed relative motion is formed at a liquid/solid interface, thereby being beneficial to mechanical film removal and IMC growth inhibition. The invention can be used for preparing composite tubes and modifying the internal friction surfaces of small-sized tubes.
Description
Technical Field
The invention relates to preparation of a metal composite pipe/coating, in particular to a method and a device for preparing the composite pipe/coating by extruding and stirring coating in a full liquid state or a semi-solid state (liquid phase containing solid particles), namely a liquid phase stirring coating method (LPS coating or stirring brazing method).
Background
The aluminum composite on the surface of the steel can improve the high-temperature oxidation corrosion resistance of the steel, and the thickness of the corrosion-resistant layer of the composite pipe is thicker than that of the corrosion-resistant layer obtained by the hot dipping method and has strong durability (document 1). Meanwhile, compared with a coating corrosion-resistant layer, the coating has the advantages of high temperature resistance and erosion and wear resistance.
Currently, the main production methods of composite pipes include direct explosion cladding, hot extrusion, centrifugal casting, welding (explosion welding of plates + rolling + spiral forming + pipe welding), mechanical joining, and the like (document 2). Among the mechanical joining methods, the cold-forming tube expansion method can be used in which stainless steel is brought into close contact with the inner wall of carbon steel by drawing, spinning, rolling, or the like (document 2). The interface of the composite pipe obtained by the cold forming pipe expansion method and the hot extrusion method is mechanically combined, and when a medium with higher temperature passes through the interface, the composite pipe is easy to bubble, loosen or vibrate due to the difference of the thermal expansion coefficients of the inner layer and the outer layer of the composite pipe. The explosive cladding method mainly utilizes the deformation of an inner coating layer and high-speed impact to obtain metallurgical bonding under the combined action of heat and force of explosives, but has more problems in the aspects of 'environmental evaluation' and 'safety management', and is easy to cause quality fluctuation due to various external factors such as weather and the like.
In the centrifugal casting method, the inner pipe and the outer pipe are both formed by adopting a pouring mode, and metallurgical bonding can be obtained. The centrifugal casting method is characterized in that two layers of molten metal are sequentially poured into a rotating mold cylinder (pipe die) to form a hollow bimetallic pipe blank or a semi-finished product under the action of centrifugal force, and then a composite blank (the interface is metallurgically fused) is manufactured into a finished composite pipe through an extrusion process, and has the difficulty of easy melting and layering, wherein secondary pouring is not easy to control, and the outer layer is easy to crack (document 3). The adopted measures are as follows: a hot-melt agent with reducibility is placed between the interlayers, and an oxide film is melted, reduced and eliminated through a strong exothermic reaction, so that atomic bonding between the two layers is finally realized. Meanwhile, the inner surface temperature of the outer layer and the inner layer pouring temperature are well controlled; particularly, the secondary pouring time is strictly controlled.
In the centrifugal casting method, metallurgical bonding between the interfaces of the inner pipe and the outer pipe is easy to realize for large-caliber pipes and difficult for small-caliber pipes. In the case of a large-diameter pipe, because the heat input amount in the mold is large, the metals poured twice are easy to be metallurgically fused, and the field operation is also easy (document 4). For example, for
The composite pipe can realize the metallurgical bonding of most parts of the whole pipe as long as the temperature of twice pouring is well controlled. But for small calibers (e.g. for
) The composite pipe has thin wall and small heat input, so that the interlayer metallurgical bonding of the whole pipe is very difficult to realize. Before the second pouring, Al-Si powder is fed into the solidified inner wall of the tube by pressure wind at the cold end of the forming cylinder, and then the second pouring is carried out, so that the oxides such as ferric oxide formed on the inner wall of the layer 1 are reduced into lighter alumina. On the other hand, the slag inclusion on the inner surface is secondarily melted by utilizing the heat and other residual heat generated during the oxidation of the Al-Si powder, and the action of centrifugal force is fully utilized to float the lighter impurities on the surface of the innermost layer, so that the metallurgical bonding between the layers is realized as far as possible.
The phenomenon of metal liquid rain can occur at the excessively low rotating speed during centrifugal casting, and the defects of shrinkage porosity, slag inclusion, unevenness of the inner surface of the tube blank and the like can also occur in the tube blank; when the rotation speed is too high, the pipe blank is easy to have defects such as cracks, segregation and the like (document 5), and the phenomenon that the thickness of the bimetal lining layer is uneven is also caused by the fact that the rotation speed is too high, so that the prevention of the defects of uneven thickness of the pipe blank and the cracks of the base layer of the pipe blank is mainly focused on controlling the rotation speed.
In addition to the use of composite pipes, coatings to improve the corrosion resistance of metals, surface modification is another general method of improving the corrosion or wear resistance of substrates. The material surface modification method comprises various methods such as electroplating, thermal spraying, plasma spraying, physical vapor deposition, chemical vapor deposition and the like. The electroplating method has low surface bonding strength and certain pollution. The thermal spraying and deposition method is not suitable for preparing the protective layer on the inner wall of the small-diameter pipe.
Since 2000, as an extension of the application of Friction Stir Welding (FSW) technology invented by british institute of welding 1991, surface remanufacturing repair and surface modification (friction coating) studies using "friction" have been carried out by foreign and foreign researchers, such as friction build-up welding (documents 6 and 7) and inner wall friction coating (document 8).
In 2011, japan has just proposed a method for modifying the surface by utilizing the friction phenomenon (document 8). The process for realizing surface modification by aiming at a friction inner surface coating (a coating is prepared on the inner wall of a cylinder body by utilizing a friction phenomenon) provided by an engine cylinder body comprises the following steps: (1) presetting the modified material at the bottom in the cylinder body (base material), and simultaneously rotating the non-consumable tool (rod); (2) pressing in the modified material while rotating the non-consumable tool to soften the modified material under the action of friction heat, so that the softened modified material generates plastic flow along with the pressing in of the tool and is pressed to the inner surface of the cylinder while flowing back along the gap between the tool and the cylinder; (3) when the rotating non-consumable tool is pulled out, an inner coating layer made of a modified material is obtained on the inner wall of the cylinder by friction. The process (stirring friction back extrusion method) is a method for preparing an inner coating layer by utilizing plastic flow in an all-solid state. Its main advantage has: (1) the modified material can form a thick film in a short time; (2) the obtained thick film is a forged structure, and has no defects of shrinkage porosity, nonuniform structure, coarse grains and the like in a cast structure; (3) the method is suitable for modifying the inner surface of the small-diameter cylinder body which cannot be constructed by thermal spraying and the like; (4) the method is suitable for materials with higher melting points of the inner layer, such as a layer of steel which is coated on the inner wall of an engine aluminum cylinder body in a friction mode.
However, the disadvantages of this process are: (1) pressure perpendicular to the interface cannot be applied to the backflow layer and the inner surface of the cylinder body directly along the radial direction of the cylinder body (the horizontal extrusion force is difficult to apply directly), and particularly in the stage of the plastic flowing metal flowing upwards vertically by bypassing the turning (chamfering) position of the bottom of the tool. This affects the stripping and densification during the all solid state bonding of the modified material/substrate interface. (2) In the preliminary study of the process, the applicant also found that the small pipe diameter can limit the diameter of the stirring tool in the substrate, and the linear velocity of the stirring tool is small, so that the friction heat generation and softening are insufficient, and the plastic flow of the modified material in a solid state is difficult, and the backward extrusion is difficult. (3) There are strict requirements on the size and shape of the original modified material (preferably, a cylindrical body with the same diameter as the inner diameter of the pipe) and, for example, when a powder modified material is used, the phenomenon of powder emission occurs, which results in metal powder loss and dust pollution.
Since 2012, some researchers in foreign countries proposed a technical solution for manufacturing seamless pipes by using a friction stir back extrusion (friction stir back extrusion) method, including AZ31B magnesium alloy pipes (documents 9 and 10), pure Cu pipes (document 11), aluminum pipes (document 12), and the like.
The modifying method based on friction stir also has a patent technology for preparing the bimetal composite plate by Friction Stir Brazing (FSB) which is proposed in 2009 by the subject group of the applicant, and the patent technology has succeeded in the aspect of plate compounding at present. From the EI web search results, the first english paper written by the applicant to introduce FSB has been cited 48 times between 11 months and 2019 months in 2011, and is cited 9 times by foreign authors in the united states, europe, and the day only in 2018. The applicant has recently conducted studies using friction stir brazing for the manufacture of composite tubes. However, experiments show that the technical difficulty of directly using the FSB technology for preparing the composite pipe is very high, and the main points are as follows: the inner tube has large radial deformation resistance and influences interface film removal and interface densification; complex tool design requirements, etc.
Reference to the literature
[1]H.D.Manesh,A.K.Taheri.Bond strength and formability of an aluminum-clad steel sheet,J.Alloy.Compd.,2003,361:138-143.
[2] Manufacturing technology of inner composite bimetallic tube in the middle of the Rabdosia, welded tube 2001,24(2):43-46.
[3] A technology for producing the metallurgical fused centrifugal blank extruded bimetal composite pipe by Guo Minghai, Pang Si, Liujunyou and casting, 2013,62(2): 118-.
[4] Huangjiayu, Yang Gui Lu, Liu Cheng Yuan, et al. development of a centrifugal casting composite tube [ J ]. hot working process, 2009,38(7):30-34.
[5] Wandonglin, wujinhui, cai, et al. centrifugal casting of bimetallic composite pipe defects and control [ J ] special casting and colored alloys, 2018,38 (3): .
[6] Zhang Yanhua, Hanhua, Liuxue plum, friction build-up welding technology and application, 2005,35(11):12-14.
[7] Chen Jia Qing, coke to east, round, Qiubue, Koelreuterian, New Material shaping processing technology-Friction stitch welding, journal of welding 2007,28(9): 108-.
[8] Tian 21083friction is achieved by による bonding method と surface modified lotus seeds, light metal welding 2011,49(1):7-12 Takeshi Shinoda.
[9]Abu F.A preliminary study on the feasibility of friction stir back extrusion[J].Scripta Materialia,2012,66(9):615-618.
[10]Baffari D,Buffa G,Fratini L.Influence of Process Parameters on the Product Integrity in Friction Stir Extrusion of Magnesium Alloys[J].Key Engineering Materials,2016,716:39-48.
[11]Dinaharan I,Sathiskumar R,Vijay S J,et al.Microstructural Characterization of Pure Copper Tubes Produced by a Novel Method Friction Stir Back Extrusion[J].Procedia Materials Science,2014,5:1502-1508.
[12]Mathew N,Dinaharan I,Vijay S J,et al.Microstructure and Mechanical Characterization of Aluminum Seamless Tubes Produced by Friction Stir Back Extrusion[J].Transactions of the Indian Institute of Metals,2016,69(10):1-8.
Disclosure of Invention
The invention aims to solve the technical problem that the concept of 'stirring friction' is used for preparing a composite pipe or a coating, and provides a method and a device for preparing the composite pipe/coating by using a full-liquid stirring and semi-solid stirring coating method, which can fully exert the heat-force combined action advantage of 'stirring friction' in the aspect of interface joint and achieve the aim of preparing the composite pipe or the coating by using the stirring friction method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a metal composite tube/coating by liquid phase stirring, comprising the steps of:
pressing a rotating stirring tool into a full-liquid or semi-solid molten pool formed by a coating material in a pipe (for example, the diameter of the pipe is 12-30 mm), enabling a liquid phase coating formed on the inner wall of the pipe by extrusion and backflow of the stirring tool to move relative to the pipe at a liquid/solid interface, mechanically breaking an oxide film at the inner surface of the pipe contacted with the liquid phase coating through stirring friction, and inhibiting the growth of an intermetallic compound in the wetting and diffusion reaction of the liquid/solid interface, or inhibiting the growth of the intermetallic compound in the wetting and diffusion reaction of the liquid/solid interface through stirring friction; and after the stirring friction is finished, the stirring tool is pulled away from the pipe, and the liquid phase coating is solidified through cooling to form a coating for covering the inner wall of the pipe or form a coating (for example, the thickness of the coating is 1-5 mm) for covering the inner wall of the pipe along the axial direction within a certain length range, so that the composite pipe or the composite pipe section is obtained.
Preferably, during the friction stir, the pipe rotates in the direction opposite to the stirring tool; the stirring tool is drawn away from the pipe and kept rotating during the cooling and solidification of the liquid phase coating.
Preferably, the full liquid or semi-solid molten pool is formed by heating molten cladding material within the pipe or by pouring molten cladding material into the pipe.
Preferably, the friction stir process is performed in a plurality of periods, with the rotation of the stirring tool being stopped between each stirring period.
Preferably, the method further comprises the steps of: before the stirring tool is pressed into a full-liquid or semi-solid molten pool formed by the coating material in the pipe, the part of the inner wall of the pipe, which is positioned above the molten pool, is subjected to pre-stirring friction to break an oxide film on the inner surface of the pipe.
Preferably, the method further comprises the steps of: and performing friction tube expansion treatment on the composite tube.
Preferably, the composite pipe is formed by preparing a plurality of composite pipe sections with the coating extending along the inner wall of the pipe in a sectional stepping composite mode.
Preferably, the pipe is selected from steel pipe and the cladding material is selected from aluminium alloy.
Preferably, the friction stir conditions are: and (3) keeping the temperature of the stirring tool at the rotating speed of 300-600 rpm at the temperature of more than 660 ℃ for stirring for more than 5 minutes, wherein the upper limit of the heat preservation temperature refers to the condition that the pipe is not unstable and is not melted and selected.
The utility model provides a device through liquid phase stirring preparation metal composite pipe/coating, includes the motor, by a plurality of stirring tool of motor drive rotation and with stirring tool apart from adjustable base, be provided with the annular on the base and be located this annular and a plurality of tubular product mounting hole that each stirring tool's position is relative respectively, along with the adjustment of distance between base and stirring tool, stirring tool can be impressed in the tubular product that corresponds the setting of tubular product mounting hole department and contain the liquid phase cladding material (for example, the above-mentioned liquid state or semi-solid molten bath that form by the cladding material) in the rotatory while.
Preferably, the device still includes transmission assembly, and transmission assembly includes the shaft coupling that links to each other respectively with stirring instrument and motor, perhaps transmission assembly includes the multiaxis ware and links to each other with the output of multiaxis ware a plurality of shaft coupling, and each shaft coupling links to each other with corresponding stirring instrument, and the input of multiaxis ware links to each other with the motor.
Preferably, a rotating disc for driving the pipe to rotate in the direction opposite to the stirring tool is arranged in the pipe mounting hole.
Preferably, the annular groove is provided with a metal sleeve or a ceramic sleeve which is not easily wetted by the liquid phase coating material, and a gap for injecting the liquid phase coating material is reserved between the metal sleeve or the ceramic sleeve and the outer wall of the pipe.
Preferably, the stirring means is selected from metal or ceramic rods that are not readily wetted by the liquid phase coating material.
Preferably, a pipe protective cover into which inert gas is continuously introduced is arranged on the ring groove, and an induction coil used for heating the pipe and a coating material in the pipe is arranged in the pipe protective cover.
The invention has the beneficial effects that:
the problems of solid phase friction stir back extrusion (friction stir back extrusion) for preparing coating or composite tube are solved, for example: (1) the heating temperature is low (the linear velocity of the tool is low), the material softening is insufficient, so that the back extrusion deformation of the coating material is difficult to plastically flow in an all-solid state, and the stirring tool is required to have extremely high rotating speed and lower pressure; (2) acting force can not be directly applied to the reflowed part perpendicular to a welding interface, so that the film removal and dense welding of the interface are influenced; the invention provides a technical scheme of introducing a 'partial liquid phase' (namely, the coating material is in a semi-solid state) or 'the coating material is in a liquid phase completely' into the coating material.
The idea of the scheme is that the flow resistance of the coating material during backflow is remarkably reduced; and secondly, the stirring tool is utilized to stir the liquid phase coating to drive the liquid phase to rotate at a high speed, a large relative movement speed is formed at an interface with the fixed solid pipe, and a violent centrifugal washing (the centrifugal force is larger when the speed is higher), friction, shearing and other mechanical actions are formed on the surface of the solid pipe, so that the mechanical crushing and dispersing effects on the oxide film on the surface of the solid main pipe are enhanced, the wetting and diffusion reaction of a liquid/solid (L/S) interface can be promoted, the liquid/solid interface is ensured to be cleaned, densified and alloyed, the metallurgical bonding is achieved, and the problems that the interface between the internal coating modified material and the main pipe cannot be metallurgically bonded and even an interface is formed inside the internal coating due to the fact that the liquid modified material and the oxide film on the interface of the main pipe are difficult to break are solved. In addition, the high-speed rotation and scouring of the liquid phase can also avoid the growth of the intermetallic compound from being too thick.
In the full-liquid or semi-solid molten pool formed by the coating material, a high-speed rotating tool is used for pressing and stirring the liquid phase, on one hand, the liquid phase is stirred to be uniformly mixed and flow back along the pipe wall, on the other hand, the liquid phase is driven to rotate at a high speed by the rotating tool, so that the stirring to the liquid phase is formed, and the stirring device has the significance of forming high-speed relative motion (forming interface friction and shearing action) at a liquid/solid (L/S) interface and is beneficial to mechanically removing a film and inhibiting the growth of IMC. Can be used for preparing composite tubes and friction modification of the inner wall surface of small-size tube barrels.
Compared with the stirring friction re-extrusion process, the liquid phase stirring coating method provided by the invention has the advantages that:
(1) the coating material has a low resistance to flow, which is mainly due to the use of liquid or semi-solid coating materials.
(2) The liquid/solid interface is good in membrane removal and compactness, which is mainly attributed to the scouring effect of the high-speed relative motion of the liquid phase and the solid phase on the interface, the mechanical membrane removal effect of the interface is improved, and the wettability is improved accordingly.
(3) The shape and the size of the coating material are not strictly required, and the coating material can be preset into the inner cavity of the mother pipe.
Compared with the composite method of centrifugal casting, the liquid phase stirring coating method provided by the invention has the advantages that:
(1) excellent interface wetting: in the process of preparing the composite pipe by centrifugal casting, the liquid phase rotates at high speed along with the pipe under the drive of the outer layer pipe, so that a larger centrifugal force is obtained, and the liquid phase flows towards the inner wall of the pipe favorably.
The invention not only keeps the larger centrifugal force of the high-speed rotating liquid phase, which is beneficial to the sealing of the liquid phase and the inner wall of the pipe (keeps the advantage of centrifugal casting), but also ensures the larger relative movement speed between the liquid phase and the inner wall of the pipe because the pipe does not rotate (or reversely rotates), and the relative movement speed between the liquid phase and the inner wall of the pipe is the linear speed of the rotation of the outer layer liquid phase. Greater relative movementThe dynamic speed strengthens the mechanical actions of friction, shearing, scouring and the like of a liquid-solid (L/S) interface, and the tangential friction force F of a rotating liquid to the surface of a static solid outer pipef＝fmω2r (in the formula, f is the friction coefficient of a liquid/solid interface, m is the liquid phase mass of a research part, omega is the angular velocity, r is the radius of an inner cavity of a static outer tube, and figure 16), the higher the rotating speed and the larger the inner diameter of the outer tube are, the larger the tangential friction force of the liquid-solid interface is, the more the mechanical stripping of the interface is favorably strengthened, the continuous dynamic scouring of the newly-generated intermetallic compound is strengthened, and the growth of the intermetallic compound (IMC) is favorably inhibited.
When the mother pipe rotates reversely to the stirring rod, the relative movement speed at the liquid/solid (L/S) interface is higher, the mechanical action (centrifugal impact and shearing) and the mechanical membrane breaking effect are stronger, and the interface welding quality can be further improved.
(2) The invention has the advantages in the preparation of the small-caliber composite pipe: the invention has the advantages that the relative speed of the liquid/solid interface is high, the mechanical film removing effect is better than that of centrifugal casting (the centrifugal casting is very difficult to realize the interlayer metallurgical bonding of the whole pipe because the heat radiation is fast and the heat input is small for a composite pipe blank with small caliber and thin wall thickness).
(3) The mother pipe is a ready-made pipe and is also heated synchronously, which is beneficial to activating the surface atoms of the solid mother pipe to alloy with the interface.
(4) And no casting process is carried out.
(5) There is no limitation on the shape of the tube: both square and round tubes are possible.
Drawings
FIG. 1 is a basic process flow demonstration of a liquid phase stirring coating method (braze coating method) for preparing a composite pipe: (a) pressing a stirring rod into the bottom layer melt, and stirring at a heat preservation state; (b) stopping heating and then drawing out the coating layer of the first section of brazing rod; (c) moving the heating coil upwards, pressing a stirring rod into the upper layer melt, and stirring at a heat preservation state; (d) after the heating is stopped, drawing out the composite pipe from the second section of the brazing coating layer to finish the brazing coating preparation of the whole section of the composite pipe; a + b, preparing a first section of composite pipe; c + d, preparing a second section of composite pipe.
FIG. 2 is a schematic view showing a liquid phase stirring coating method (brazing method) in which a stirring rod and an outer tube are rotated in opposite directions: (a) pressing a stirring rod into the bottom layer melt, and stirring at a heat preservation state; (b) stopping heating and then drawing out the coating layer of the first section of brazing rod; (c) moving the heating coil upwards, pressing a stirring rod into the upper layer melt, and stirring at a heat preservation state; (d) after the heating is stopped, drawing out the composite pipe from the second section of the brazing coating layer to finish the brazing coating preparation of the whole section of the composite pipe; a + b, preparing a first section of composite pipe; c + d, preparing a second section of composite pipe.
FIG. 3 is a schematic diagram of a liquid phase stirring coating method (braze coating method) with argon protection: (a) moving the heating coil upwards, pressing a stirring rod into the upper layer melt, and stirring at a heat preservation state; (b) and after the heating is stopped, drawing out the composite pipe from the second section of the brazing coating layer to finish the brazing coating preparation of the whole section of the composite pipe.
FIG. 4 is a schematic view of a horizontal liquid phase agitation coating process.
FIG. 5 is a schematic diagram of the preparation of a composite tube by simultaneous coating of the inside and outside of an outer tube: the inside of the outer tube was coated by a liquid phase stirring method (coating method).
FIG. 6 is a schematic diagram of a semisolid melt liquid phase stirring coating method (braze coating method): the squares in the coating material are solid particles.
FIG. 7 is a demonstration of a multi-axis liquid phase stirring coating method for preparing a composite tube.
Fig. 8 is a photograph showing the appearance of a steel-clad aluminum composite pipe prepared by a liquid phase stirring coating method (braze coating method): (a) the thickness of the coating is 2 mm; (b) the thickness of the coating is 3 mm.
FIG. 9 is a macroscopic photograph of a longitudinal section of a ladle aluminum composite pipe prepared by a liquid phase stirring coating method (brazing method) (700 ℃ C.. times.5 min. times.400 rpm): the thickness of the coating is 2 mm.
FIG. 10 is a microscopic (200X) photograph of a longitudinal section (the square portion in FIG. 9) of a ladle aluminum composite pipe prepared by a liquid phase stirring coating method (brazing method) (700 ℃ C.. times.5 min. times.400 rpm): it can be seen that the aluminum/steel interface is compact, excellent in wetting, and free of significant intermetallic compounds.
Fig. 11 is a cross-sectional interface photograph of a steel ladle aluminum composite tube prepared by a liquid phase stirring coating method (braze coating method): (a) a macro graph; (b) an enlargement of the portion (a) at a lower magnification (50 ×), the adhesion at the aluminium/steel interface is visible.
FIG. 12 is a microstructure of a cross-sectional interface of a ladle aluminum composite tube prepared by a liquid phase stirring coating method (braze coating method) (700 ℃ C.. times.5 min. times.400 rpm): (a) the area 500 × enlarged view of the box in fig. 11 (b); (b) at a 2000 × magnification of the middle square area (a), it can be seen that an intermetallic layer about 2 μm thick is present at the aluminum/steel interface.
Fig. 13 is a macroscopic shearing photograph of a steel ladle aluminum composite pipe prepared by a liquid phase stirring coating method (braze coating method): (a) the aluminum side interface extruded by the shearing load is seen to be a wavy and non-smooth interface outside the aluminum layer; (b) the inside profile of the steel tube showed that aluminum had adhered to the inside surface of the steel.
FIG. 14 is a load-displacement curve of a steel ladle aluminum composite pipe shear test prepared by a liquid phase stirring coating method (braze coating method) (700 ℃ C.. times.5 min. times.400 rpm): the shear stress is about 5.2kN, and the shear strength is 34.5 MPa.
FIG. 15 is a pictorial view of a friction tube expander: diameter of cutting edge of friction tube expanding tool
Diameter of friction cylinder
FIG. 16 is a force analysis comparison of the inner surface infinitesimal of the outer tube: (a) the inner surface of the stirring and brazing coating outer pipe is stressed in a micro-element way, and the tangential friction force F of the rotating liquid relative to the inner wall of the static solid outer pipe in the stirring and brazing coating processfThe method has the functions of strengthening the interface mechanical stripping and inhibiting the growth of intermetallic compounds (IMC); (b) carrying out micro-element stress on the inner surface of the centrifugally cast outer pipe; fNIndicating the positive pressure of the rotating fluid relative to the outer tube.
In the above drawings: 1-ceramic stirring rod, 2-outer tube, 3-heating coil, 4-base, 5-protective cover, 6-coating, 7-ceramic sleeve, 8-coupling and 9-multi-shaft device.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Basic process of (I) method for preparing composite pipe/coating by full-liquid stirring or semi-solid stirring coating method (see figure 1 and figure 6)
(1) The inner wall cladding material is put into the mother pipe (namely the outer layer and the outer pipe of the composite pipe), protective gas is introduced according to needs, the inner wall cladding material and the outer pipe 2 are heated simultaneously by means of induction heating or radiation heating and the like (such as a heating coil 3) until the inner wall cladding material is heated to be in a full liquid state (such as pure metal or eutectic alloy) or a semi-solid state (such as hypoeutectic alloy or other alloys with larger difference between solidus and liquidus, and a liquid-phase molten pool can be formed in the outer pipe by additionally adding refractory metal particles and ceramic particles), so that the flowing resistance can be reduced, and the flow is easy.
(2) The ceramic stirring rod 1 is driven by a starting motor to rotate at a high speed, the ceramic stirring rod is pressed into the surface layer of the molten pool while rotating, the pressing is suspended, the in-situ stirring is carried out for a period of time, the oxide film between liquid phases is broken, and the liquid phases are rapidly and uniformly mixed (generally, the liquid phases can be uniformly mixed for more than 10 seconds).
(3) And continuously pressing the ceramic stirring rod into the outer pipe to extrude the liquid phase in depth, enabling the liquid phase to flow back upwards along the gap between the pipe wall and the ceramic stirring rod 1, simultaneously keeping the high-speed stirring liquid phase, and continuously carrying out induction heating through a heating coil. The liquid phase is driven to rotate at a high speed by a rotating tool (a ceramic stirring rod), so that 'stirring to the liquid phase' is formed, liquid/solid (L/S) interface (namely the inner surface of the outer pipe) is in high-speed relative motion at an interval, and the centrifugal impact and the tangential rotation of the liquid phase are utilized to form mechanical actions such as impact, friction, shearing and the like on the surface of the solid base metal, so that the mechanical action is facilitated to break an oxide film on the inner surface of the outer pipe, and the static growth of intermetallic compounds is inhibited by utilizing the high-speed scouring of the liquid phase.
(4) After the heating is stopped, when the temperature of the molten pool is lower than the melting point of the coating material of the inner wall (the temperature of the molten pool can be detected through a pre-test by a thermocouple, and the corresponding state change of the temperature or the color of the outer pipe and the like is determined), the stirring tool is drawn out while rotating, so that the smooth forming of the inner wall of the coating is ensured, and the stirring tool is drawn out smoothly.
(5) The long composite pipe may be prepared in stepped compounding mode from the bottom of the outer pipe to the top. After the preparation of the first section of cladding at the bottom of the outer pipe is completed according to the steps (1) to (4), embedding a section of ceramic filler rod with the height lower than the interface height of the top of the cladding into the cladding, plugging the hollow part surrounded by the cladding, then using the top of the cladding as the bottom of a liquid-phase molten pool, preparing the second section of cladding of the outer pipe according to the steps (1) to (4), and so on until the preparation of each section of cladding of the whole long-size composite pipe is completed. Then cutting off the bottom dead end of the first section of cladding together with the corresponding part of the outer pipe, then ejecting out the ceramic filling rod in the outer pipe, and machining the inner wall of the formed cladding. When preparing the upper cladding layer, a stirring tool needs to be pressed below the top interface of the lower cladding layer so as to eliminate the interface; the back-squeezed liquid is tightly attached to the inner wall of the outer pipe under the action of centrifugal force, and the stirring tool is not contacted with the filling rod.
When the melting point of the inner wall cladding material is higher than that of the outer pipe (i.e. the inner wall cladding material in the outer pipe is not suitable to be heated by a heating coil arranged outside the outer pipe), on one hand, necessary cooling measures (such as water cooling or copper cooling) are taken for the outer pipe, and on the other hand, the inner wall cladding material is filled in an external melting casting mode, namely, the inner wall cladding material is melted in other crucibles or containers, and then the liquid inner wall cladding material is poured into the outer pipe to directly form a molten pool. The liquid phase agitation and other steps are referred to above in steps (2) to (5).
(II) design of stirring device for preparing composite pipe/coating by full-liquid stirring or semi-solid stirring coating method
Referring to fig. 1, 3,6 and 7, the stirring device includes the following parts: the stirring machine comprises a motor, a motor speed regulating assembly, a transmission assembly (used for connecting a motor spindle with a stirring tool, such as a coupler 8), a motor fixing clamp and a lifting part (comprising a base 4) of the stirring tool. The material of the stirring rod is selected from ceramics (such as corundum); other refractory metal rods or tubes (i.e., solid or hollow rods) which are not easily wetted by the liquid phase can also be adopted according to the working conditions to overcome the defects of brittleness and poor thermal shock resistance of the ceramic rod. Because the liquid phase flow resistance is small, a low-power single-phase motor can be selected; for the working conditions of low heat preservation temperature and large liquid phase flow resistance, a three-phase motor can be selected. In the transmission assembly, one end of a coupler 8 is connected with a motor by adopting a key (a motor shaft is provided with a key, and a key groove is arranged on the coupler); the ceramic stirring rod 1 is inserted into a clamping hole at the other end of the coupler 8, and the ceramic stirring rod 1 is fastened through threads. For raising the efficiency, can pass through multiaxis ware 9 with the motor and a plurality of shaft couplings 8 cooperation to drive a plurality of ceramic stirring rods 1 simultaneously with a motor, can prepare a plurality of compound pipes simultaneously. The lifting part is provided with a base 4 driven by a controllable lifting platform, the lower end face of the base 4 is arranged on the lifting platform (used for completing the extension, the retention and the separation of the stirring rod from the outer pipe), and the upper end face of the base is provided with a ring groove (used for installing a protective cover 5 and providing protective atmosphere for liquid phase stirring) and at least one outer pipe mounting hole (coaxial with a corresponding coupler) positioned in the ring groove. The outer tube mounting hole can be provided with a turntable, and the outer tube is driven to rotate according to needs.
(III) optimized application of process
Static tube type and moving tube type
Referring to fig. 1, the static pipe type means that the original pipe (outer pipe) is still. Referring to fig. 2, the tube type is that the rotation direction of the original tube (outer tube) is opposite to the rotation direction of the stirring rod in the liquid phase stirring, so as to further enhance the mechanical stripping action (through mechanical action such as friction, shearing, centrifugal impact and the like) of the liquid phase on the solid phase surface at the L/S interface.
Melting of liquid phase is divided into an internal melting type and an external melting pouring type:
referring to fig. 1, the internal melting mode is to melt a coating material inside an outer tube 2, so as to avoid a pouring step, and to heat a composite layer of the outer tube and an inner wall at the same time, which is suitable for preparing an internal coating with a lower melting point, and may also be called as a "brazing mode", but has higher requirements on interface cleanliness and wettability, and needs to perform necessary protection (for example, argon atmosphere protection, see fig. 3) on the surface of a solid base material (outer tube) to prevent an oxide film generated on the surface of the outer tube at a high temperature from affecting interface wettability.
The outer melt casting type is a method of melting a coating material in another container and then casting the melted coating material into an outer tube, is suitable for preparing an inner coating with a higher melting point, and reduces the requirement on surface protection of a solid base material because the surface of the solid base material (the outer tube) is partially liquefied and the wettability is easy to guarantee.
Thirdly, vertical and horizontal stirring is divided according to the length of the pipe and the melting point of the coating material
Referring to fig. 1, the vertical stirring is suitable for the working condition that the pipe size is short; referring to fig. 4, the horizontal stirring is suitable for the working condition that the pipe has a longer size and the cladding material has a higher melting point (even higher than that of the outer pipe) and needs external melting and pouring, so that the pouring is convenient, the device height is not limited, the coating of the inner wall of the long pipe is completed through one-time liquid phase stirring, and the preparation efficiency is higher than that of sectional compounding. When horizontal stirring is used, the outer tube should be properly inclined at a certain angle in order to prevent the high-temperature liquid phase from flowing down.
Simultaneous coating of inside and outside
Referring to fig. 5, a ceramic sleeve 7 is installed in the annular groove of the base 4 (tightly matched with the inner side wall surface of the annular groove), a gap is formed between the ceramic sleeve and the outer pipe, a liquid phase coating material can be added by adopting a pouring mode to form an L/S interface positioned on the inner surface and the outer surface of the outer pipe, and the stirring rod and the outer pipe both rotate but have opposite rotation directions.
Multi-pipe parallel combined type
Referring to fig. 7, in order to further improve the preparation efficiency, a plurality of stirring rods are driven by a motor through a multi-axis device 8 to rotate simultaneously, a plurality of composite tubes are prepared at one time, and the problem of poor precision of the composite tubes caused by the use of a plurality of motors is solved.
Sixthly, intermittent stirring
For example, in the liquid phase stirring, a mode of continuous circulation of stirring-standing-stirring-standing is adopted, and the standing can prolong the static contact reaction time of a liquid/solid (L/S) interface after stirring and removing a membrane, properly strengthen the interface reaction and improve the interface bonding strength. The total duration of the heat preservation stirring is consistent with the continuous stirring.
Seventh post-weld heat treatment
Considering that the temperature required by stirring is higher, the intermetallic compound is easy to grow too thick when the temperature is kept at high temperature for a long time, therefore, the interface can be stirred for a short time at the temperature higher than the melting temperature of the coating material to realize the basic interface wetting and the sealing, and then the interface is timely diffused in the solid state of the coating material to strengthen the interface bonding.
Wall-touching type and non-wall-touching type
The wall-touching type is to divide the stirring process into two steps: in the early stage (a molten pool is formed), the rotating tool is enabled to be tightly attached to the inner wall of the outer pipe for rotating and stirring by moving the base, so that the aim of mechanically breaking the oxide film on the inner wall of the pipe is fulfilled; and the rotating tool moves to the center of the pipe (namely does not contact the outer pipe) for rotating and stirring during stirring at the later stage (the stage of pressing into the molten pool), so that the uniform distribution of the thickness of the coating is ensured. The contact wall type is suitable for the occasion that the oxide film in the pipe is difficult to clean in advance.
Referring to fig. 1, the non-contact wall type means that the stirring tool always rotates in the center of the pipe (i.e. does not contact the outer pipe), and the implementation is easy.
Ninthly coating expansion composite (first coating and then expansion)
The friction stir coating is firstly carried out, the friction expansion is carried out on the formed composite pipe from the inner coating side, the interface of the coating layer/base material is further densified, and the coating structure is improved from a casting structure to an extrusion structure. The structure of the friction tube expanding tool is shown in fig. 15, and the cutting edge, the table conical surface, the columnar friction surface (cylindrical surface) and the handle part which is slightly thinner than the columnar friction surface are arranged in sequence from the front end to the back end.
The principle of friction tube expansion is as follows: starting the friction tube expanding tool to rotate and simultaneously pressing the friction tube expanding tool into the stirring coating composite tube along the axial direction; guiding and rubbing by using a cone surface to preheat; expanding the pipe and expanding the diameter (expanding along the radial direction) while heating and softening the inner-layer pipe by using the cylindrical surface friction of a tool, and vertically applying acting force to a welding surface; the chips are discharged downwards, and the diameter of the handle part is slightly smaller than that of the columnar part, so that the friction pipe expanding tool can be pulled out conveniently.
(IV) Process examples
To be provided with
Q235 steel pipe (diameter 19mm, wall thickness 2.5mm) was used as an outer pipe, and the length was 120 mm. With 6061 aluminum alloy rod
Taking a 60-70 mm long 6061 aluminum alloy bar as an inner wall coating material for later use. The pretreatment step comprises the steps of sanding the inner wall of the Q235 steel pipe and the outer surface of the 6061 aluminum alloy rod by using sand paper, and then carrying out ultrasonic cleaning by using absolute ethyl alcohol. Mounting the pretreated Q235 steel pipe in the mounting hole of the base, uniformly distributing heating coils outside the steel pipe, and mounting protection in the ring grooveAnd the cover is used for determining the lifting and stopping positions of the base according to the length of the steel pipe. And putting the pretreated 6061 aluminum alloy rod into the Q235 steel pipe, enabling the interior of the Q235 steel pipe to be in a protective atmosphere formed by Ar gas introduced into the protective cover by using the protective cover, and heating the heating coil to 700 ℃ by using an induction power supply to ensure that the 6061 aluminum alloy rod is melted into 6061 aluminum alloy melt to form an aluminum molten pool.
Starting the motor, the drive being connected to the motor via a coupling
The solid corundum rod was rotated (400rpm) by raising the base so that it slowly passed through the protective shield into the outer tube and was pressed into the aluminum bath (without touching the base). Firstly, stirring in situ for 10s through a shallow surface layer to break an oxide film on the surface of liquid aluminum; then continuing to press the solid corundum rod downwards, and applying pressure to the inside of the depth of the 6061 aluminum alloy melt so that the liquid metal flows back upwards along the inner wall of the steel pipe to form a liquid-phase inner coating layer; meanwhile, the solid corundum rod which keeps rotating is utilized to keep the temperature continuously and stir the liquid phase which flows back for 5 min. The stirring tool drives the liquid phase to rotate at a high speed, so that high-speed relative motion of a liquid/solid (L/S) interface is formed, the high-speed rotating liquid phase forms mechanical actions such as friction, shearing, centrifugal impact and the like on the surface of a solid-phase pipe, and the rotating liquid phase has a mechanical film removing function through the mechanical actions, so that the interface is cleaned favorably (experiments show that Al/Fe compounding can be realized even if protective gas is not applied, and the high-speed rotating liquid phase has strong mechanical film removing capability); in addition, the liquid phase rotating at high speed can scour and shear intermetallic compounds just formed on the interface, and the in-situ continuous growth of the IMC can be effectively inhibited. Thus, the preparation of the aluminum/steel composite pipe (the composite pipe with the inner surface of the steel base material coated with the aluminum alloy) can be completed, the stirring drill rod coated aluminum/steel composite pipe, the ladle aluminum composite pipe for short, is also equivalent to the modification of the friction surface in the small-size (inner diameter) pipe.
The composite tube prepared in this example was tested for effectiveness as follows:
(1) and (3) appearance forming: the appearance of the stirring braze-coated aluminum/steel composite pipe is shown in figures 8 and 9, the ladle aluminum composite pipe with the length of 110mm (10 mm is cut off at the blind end), the coating thickness of 2mm and 3mm and good appearance is prepared under the adopted preparation process conditions (700 ℃ multiplied by 5min multiplied by 400rpm), and the longitudinal section macroscopic interface is dense and has no gap and hollow defects. The cross-sectional area micrograph (fig. 11) shows: the stirring drill coated aluminum/steel composite pipe has compact cross section interface and no gap and cavity defects.
(2) The interface microstructure is as follows: referring to fig. 10, the longitudinal section of the stirring braze-coated aluminum/steel composite pipe prepared under the conditions of 700 ℃ x 5min x 400rpm has a microscopic (200 x) interface, is compact, has excellent wetting, and has no obvious intermetallic compounds; FIG. 12(a) shows the microscopic (500X) interface densification at the cross-sectional interface of the stirring braze-coated aluminum/steel composite pipe, and FIG. 12(b) shows the presence of an intermetallic layer about 2 μm thick at the microscopic interface of aluminum/steel at 2000X.
(3) And (3) testing the shearing performance: a macroscopic photograph of a shear sample of the stirring brazing coated aluminum/steel composite pipe prepared under the conditions of 700 ℃ multiplied by 5min multiplied by 400rpm shows that, referring to fig. 13(a), the aluminum side of the outer side of the aluminum layer extruded by the shear load is a wavy interface instead of a smooth interface, which indicates that the aluminum-steel interface is well wetted, and referring to fig. 13(b), the aluminum/steel interface is metallurgically bonded; cutting a 4 mm-long small section of the composite pipe for testing shear strength, and stirring drill coating the composite pipe for shear test (outer pipe)
Cladding 6061
) Referring to fig. 14, the shear stress is measured to be about 5.2kN, and the shear strength is measured to be 34.5MPa, which indicates that the aluminum/steel composite pipe prepared by the stirring brazing process has a compact metallurgical bonding interface and higher shear strength.
In a word, the invention discloses a method and a device for preparing a composite pipe/coating by a full-liquid stirring and semi-solid stirring coating method. In a full-liquid or semi-solid molten pool formed by a coating material, a liquid phase is pressed and stirred by a ceramic tool rotating at a high speed, on one hand, the liquid phase is stirred to be uniformly mixed and flow back along the pipe wall, on the other hand, the liquid phase is driven to rotate at a high speed by the rotating tool, so that the liquid phase is stirred, and high-speed relative motion (interface friction and shearing action) is formed at a liquid/solid (L/S) interface, thereby being beneficial to mechanical film removal and IMC growth inhibition. The invention can be used for preparing composite tubes and modifying the internal friction surfaces of small-sized tubes.
Claims (10)
1. A method for preparing a metal composite pipe/coating by liquid phase stirring is characterized in that: the method comprises the following steps:
pressing a rotating stirring tool into a full-liquid or semi-solid molten pool formed by a coating material in the pipe, enabling a liquid phase coating formed on the inner wall of the pipe by extrusion and backflow of the stirring tool to move relative to the pipe at a liquid/solid interface, realizing mechanical breaking of an oxide film on the inner surface of the pipe, which is in contact with the liquid phase coating, through stirring friction, and inhibiting growth of intermetallic compounds in wetting and diffusion reactions of the liquid/solid interface, or realizing inhibition of growth of the intermetallic compounds in the wetting and diffusion reactions of the liquid/solid interface through stirring friction; after the stirring and rubbing are finished, the stirring tool is pulled out of the pipe and the liquid phase coating is solidified through cooling, so that a coating covering the inner wall of the pipe or a coating covering the inner wall of the pipe in a certain length range along the axial direction is formed, and a composite pipe or a composite pipe section is obtained;
in a full-liquid or semi-solid molten pool formed by a coating material, a high-speed rotating tool is used for pressing and stirring a liquid phase, on one hand, the liquid phase is stirred to be uniformly mixed and flow back along a pipe wall, on the other hand, the liquid phase is driven to rotate at a high speed by the rotating tool, and a large relative movement speed is formed at an interface with a fixed solid pipe, so that the liquid phase is stirred, high-speed relative movement is formed at a liquid/solid (L/S) interface, interface friction and shearing effects are formed, and mechanical film removal and IMC growth inhibition are facilitated.
2. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: in the process of stirring and rubbing, the pipe rotates in the direction opposite to the stirring tool; the stirring tool is drawn away from the pipe and kept rotating during the cooling and solidification of the liquid phase coating.
3. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the full liquid or semi-solid melt pool is formed by heating molten cladding material within the pipe or by pouring molten cladding material into the pipe.
4. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the friction stir process is completed in a plurality of time periods, with the rotation of the stirring tool being stopped between each time period.
5. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the method further comprises the steps of: before the stirring tool is pressed into a full-liquid or semi-solid molten pool formed by the coating material in the pipe, the part of the inner wall of the pipe, which is positioned above the molten pool, is subjected to pre-stirring friction to break an oxide film on the inner surface of the pipe.
6. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the method further comprises the steps of: and performing friction tube expansion treatment on the composite tube.
7. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the composite pipe is formed by preparing a plurality of composite pipe sections with coatings extending along the inner wall of the pipe in a sectional stepping composite mode.
8. A method of producing metal composite pipes/coatings by liquid phase stirring according to claim 1, characterized in that: the pipe is selected from a steel pipe, and the coating material is selected from an aluminum alloy.
9. A method for producing a metal composite pipe/coating by liquid phase stirring according to claim 1 or 8, characterized in that: the friction stir conditions are as follows: the stirring tool is used for stirring at the rotating speed of 300-600 rpm for more than 5 minutes at the temperature of more than 660 ℃.
10. An apparatus for manufacturing a metal composite pipe/coating by the method for manufacturing a metal composite pipe/coating by liquid phase stirring according to claim 1, wherein: the device includes the motor, by a plurality of stirring tool that motor drive is rotatory and with stirring tool apart from adjustable base (4), be provided with the annular on base (4) and be located this annular and a plurality of tubular product fixed mounting hole relative respectively with the position of each stirring tool, along with the adjustment of distance between base (4) and stirring tool, stirring tool can be when rotatory impress in the tubular product that contains liquid phase coating material that corresponds the setting of tubular product mounting hole department, the device is still including the induction coil who is used for heating the coating material in tubular product and the tubular product.
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