CN102632347A - Aluminium matrix composite, brazing filler metal for aluminium alloy and brazing method - Google Patents
Aluminium matrix composite, brazing filler metal for aluminium alloy and brazing method Download PDFInfo
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Abstract
In order to improve the defect that the interface of a Zn-Al brazing filler metal and an Al matrix has no reaction or the reaction is not uniform (limited to a corrosion section and part crystal boundary), the invention discloses an aluminium matrix composite, a low-melting-point Zn-Al-Mg ternary active brazing filler metal (comprising 3-10% of Al, 2-7% of Mg and the balance of Zn, wherein the corresponding melting range is 337-475 DEG C) and a low-frequency low-amplitude reciprocating friction assistant low-temperature active soft brazing method. The low-temperature active soft brazing method is used as the other auxiliary method under the low-temperature working condition, when the low-frequency low-amplitude friction is applied, and the improvements on the liquid-phase liquidity, the striping effect and the wetting property are more notable. The low-frequency low-amplitude friction assistant low-temperature active soft brazing method comprises the following steps of: presetting brazing filler metal, then pressurizing and heating, canceling the pressure until the temperature is 330 DEG C, sequentially heating until the temperature is 400-550 DEG C, performing heat preservation and leading in the low-frequency low-amplitude friction. According to the method, a soldering flux is not needed, the brazing filler metal prematurity loss is avoided, and no obvious corrosion and/or ceramic grain prejudiced collection is caused; and the brazing filler metal uniformly infiltrate, the diffusion required time is shortened, and protected gas is not essential.
Description
Technical field:
The present invention relates to the Zn base low-melting solder prescription improvement of aluminum matrix composite and aluminium alloy and the improvement of soldering processes thereof; Having developed and having exempted from brazing flux low melting point Zn-Al-Mg is ternary active solder prescription, and the low frequency that is used for it rubs the active soldering method by a narrow margin auxiliary.
Background technology:
As everyone knows, the soldering of aluminum matrix composite and the aluminium alloy matter of utmost importance that all need solve is how effectively to remove the oxide-film on aluminum substrate surface.The method of abolishing the oxide-film of aluminium alloy or aluminum matrix composite matrix surface at present has three kinds: (1) chemical method, and clean in [2], the solder with chemical reagent like brazing flux [1], before welding and to add active element methods such as [3]; (2) physical method is like vacuum environment [4], utilize under the film liquefaction principle [5], plate surface modification [2,6] etc.; (3) mechanical means, as utilize mechanical scraping method [7], wire brush [2] and hyperacoustic cavitation (Ultrasonic cavitation effect) [8] etc.These methods are each has something to recommend him; Brazing flux striping soldering wherein commonly used, vacuum brazing, liquid-phase diffusion welding (additional or not attached supersonic vibration) need combined factors selections such as liquid phase viscosity and mobile quality after the activity, mother metal dissolving difficulty or ease, alloying according to composite mother metal, brazing filler metal alloy system, brazing temperature.
In the solder of having reported at present, the low-temperature brazing filler metal that is used for welding aluminum alloy and aluminum matrix composite can be divided three classes:
(1) the Al-Si-Cu brazing filler metal [4; 9; 10]; Like Al-28Cu-5Si [9], Al-20Cu-5Si-2Ni [10], Al-20Cu-3.3Ni-10Si [10], Al-28Cu-5Si-2Mg [4], Al-7Si-20Cu-2Sn-1Mg [4], Al-6Si-30Cu-20Zn solders such as [9], the fusing point of these solders is all between 450～550 ℃, and welding temperature is all more than 550 ℃; This just requires the alloy matrix aluminum fusing point higher, and high welding temperature also can be destroyed the interface between the ceramic phase and alloy matrix aluminum in the aluminum matrix composite; And need to use brazing flux or under vacuum environment, weld, then the corrosion resistance of welding point is poor if use brazing flux, then welding cost is high if need vacuum environment;
(2) Zn-Al system [1]; Zn-Al-Cu system [7] and Al-Ge system [11]; Like Zn-5Al [1], Zn-20Al [12], Zn-28Al [13], Al-4.5Si-40Zn [14], Zn-20Al-15Cu, Zn-4Al-3Cu-1Mg [7], Al-45Ge [11], Al-45Ge-2Si solders such as [11]; All between 370～450 ℃, welding temperature can be controlled at below 550 ℃ the fusing point of these solders, but these solders need use brazing flux or big pressure or ultrasonic wave to weld under auxiliary; This is just very high to the requirement of equipment, increases welding sequence or welding cost; And it is higher wherein to contain Cu, Ag or Ge solder cost;
(3) Sn-Zn system [15]; Sn-Pb is [6]; Sn-Ag-Ti system [16] and Zn-Cd system [17], like Sn-9Zn [15], Sn-37Pb [6], Sn-10Ag-4Ti [16], Zn-39Cd solders such as [17], its fusing point is all between 150 ℃～370 ℃; Welding temperature generally is no more than 450 ℃, must use the auxiliary oxide-film that goes to the aluminum substrate surface that breaks of brazing flux or ultrasonic wave when still welding; The poor corrosion resistance of Sn base solder welding point; Zn-Cd brazing filler metal to containing poisonous Elements C d can threaten personal safety and environment.
Consider that (2024 and 475 ℃ 7075 aluminium alloys as solidus being respectively 500 ℃ need prevent alloy matrix aluminum fusing and overaging for the influence that reduces the mother metal tissue in the welding process as much as possible; To preventing alligatoring through violent crimp gained aluminum substrate crystal grain), this just needs research and development low melting point solder, and under alap temperature, welds.In the low temperature brazing field; Many at present with Zn base low-melting solder; As the fusing point of Zn-5Al that has reported [1] and Zn-5Al-3Cu [7] is respectively 360 ℃～430 ℃ and 385 ℃～400 ℃, simultaneously when low temperature brazing, for striping smoothly and improve wetability; The use report of the use, particularly ultrasonic vibration [7] of brazing flux [1] is more.Comparatively speaking; Although active element (Ti) has the effect that can quicken to abolish the aluminum substrate surface film oxide and is belonged to seminar by the applicant and confirm [18 in aluminum matrix composite high temperature active liquid-phase diffusion welding (610 ℃); 19]; But can active element realize the striping reaction and be still a research blank spot that its potentiality remain to be furtherd investigate smoothly in low temperature brazing.Particularly for the binary solder of using the Zn-Al class always; The applicant has confirmed in early-stage Study when not using brazing flux also not import ultrasonic vibration; Zn-5Al binary eutectic solder is difficult to homogeneous to mother metal dissolving to carry out, and causes film under liquefaction insufficient, inhomogeneous (only positions corrosion occurs) extremely individually; Though Zn can infiltrate matrices of composite material but interfacial gap is not eliminated yet, interface wet ability very poor [20] when the solder capacity.Based on above-mentioned analysis, the applicant attempts through in low melting point Zn-Al brazing filler metal, adding double mechanism acquisition to the aluminum substrate comparatively desirable wetability of active element (Mg) with the striping (physical mechanism) that liquefies under newly-increased reaction striping (chemical mechanism) and the reinforced film.
On the other hand, for there being another problem in the welding of aluminum matrix composite---how to avoid in the welding point ceramic enhancement phase to gather partially and dilution [21] and guarantee the compactness [3] between basal body interface, the ceramic phase/interface, braze metal of weld zone ceramic phase/on every side.The former is relevant with the dissolution degree of mother metal, promptly depends on the interaction of solder and aluminum substrate; The latter then depends on the improvement of the wetability between solder and the ceramic phase.The method of improving the wetability of brazed seam and ceramic phase has: preferred wild phase is separate, to the ceramic enhancement phase preliminary treatment, add active element, apply method such as ultrasonic vibration.But, choose back two kinds of methods only for set composite mother metal.The method of wherein utilizing the ultrasonic air cavitation by Yan Jiuchun, Xu Zhiwu people's successful use such as [8] in the welding of aluminum matrix composite, but its equipment cost is higher.
Can make aluminum matrix dissolves though be also pointed out that low welding temperature, and the liquid phase flow property that is not equal to after the alloying is good.Consider that low welding temperature is disadvantageous to the flowability of undercurrent under the film, so also need consider other improvement measures.
The present invention is directed to mother metal solubilizing reaction inhomogeneous (local corrosion) that above-mentioned low melting point Zn-Al binary solder exists, liquid phase flow property difference and oxide-film difficult broken and remove, problem such as the difficult removal of interfacial gap; And suitably take into account ceramic phase/braze metal wetability and improve, intend through adding new ternary active solder of active element (Mg) exploitation and the auxiliary process under the soldered.The applicant is according to the design principle [3] in active liquid-phase diffusion welding (A-TLP) intermediate layer; The thinking of utilizing active element reaction striping and film dive diffluence film to combine has successfully developed a kind of aluminium alloy and aluminum matrix composite is the ternary active solder with low melting point Zn-Al-Mg; And developed the active soldering method that the low-cost low frequency that can be used for this solder rubs auxiliary by a narrow margin, can further improve strength of joint (the joint coefficient of efficiency can reach 90%).
List of references:
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Summary of the invention:
It is reactionless and have interfacial gap that the object of the invention is to improve low melting point Zn-Al solder and Al basal body interface, perhaps react inhomogeneous (only limiting to) in corrosion place and part crystal boundary place and the reaction of Al matrix and cause the surface film oxide of crystal grain own abolish effect bad, see that wetability is still just obviously poor, empty drawback appears in the interface on a large scale.Technical scheme of the present invention is: at solder composition design aspect (aspect main), add active element Mg, can increase the solder activity, improve the interfacial reaction homogeneity and further reduce the solder fusing point; Aspect welding process (accidental), consider that welding temperature is low, Zn alloy fluid viscosity big, flowability is poor, when solder is about to melt; Promptly applying cheaply along the weld interface direction, low frequency rubs by a narrow margin; So that abolish the oxide-film of solder and Al and surface, impel the more contact of large tracts of land (surface of crystal grain itself particularly, and be not only the surface of crystal boundary) of fresh liquid solder and solid-state Al matrix with mechanical gimmick; Thereby further for to create favorable conditions through above-mentioned metallurgical approach striping; Like this, can further improve interface wet ability, improve strength of joint.
It is worthy of note; In the improvement aspect above-mentioned two; Solder composition design improvement is even more important basic prerequisite; Because in fact,, the applicant also is starkly lower than the intensity (78MPa sees Fig. 6) that Zn-5Al-4Mg does not add auxiliary friction gained joint even applying the same gained of friction by a narrow margin strength of joint (70MPa) to Zn-Al binary solder in early-stage Study.Compare with Zn-Al solder and traditional method for welding; Can abolish the oxide-film on liquid solder and aluminum substrate surface at low temperatures preferably simultaneously through the double action of active element Mg and interface friction; And then, also created condition for the wetability between ceramic enhancement phase and fresh braze metal (P/M) interface in improvement fresh solder/aluminum substrate (M/M) interface and the composite.
The present invention seeks under above-mentioned thinking instructs, through following detailed, the series technical project realization:
1. brazing filler metal alloy is the aspect: at first, the alloy system of the determined Zn base low-melting of the present invention ternary active solder is a Zn-Al-Mg system.Mentality of designing is that interpolation active element Mg on the basis of Zn-Al binary eutectic to increase the solder activity, to improve interfacial reaction homogeneity and further reduction solder fusing point, is the ternary active solder thereby constitute low-melting Zn-Al-Mg.
Although as far as oxide-film and most ceramic enhancement phase of Al matrix surface, optional active element has Ti, Li, Mg, the applicant confirms that through early-stage Study Zn-Al-Ti system and Zn-Al-Li are that the ternary active solder is unsuccessful.Zn-Al-Ti is that the subject matter of ternary active solder is very difficulty of preparation, is in particular in three aspects: the one, and the volatilization of Zn liquid confirms that through test at 600 ℃, it is very obvious particularly just to become more than 650 ℃; The 2nd, below 600～650 ℃, dystectic Ti is difficult to fusing, even adopt intermediate alloy also very difficult; The 3rd, Ti is very obvious to the segregation of top melting piece in Zn liquid, the appearance of this problem and Ti be difficult to fusing smoothly and density relevant much smaller than Zn, at this moment, also It dones't help the situation even adopt chilling to get rid of band.Applicant's paper is seen in correlative study: Zhang Guifeng; Su Wei, Guo Yang, Liao Xianjin; Et al.Development of three kinds of active ternary filler metals of Al-Si-Ti; Zn-Al-Ti and Cu-Al-Ti systems for Al metal matrix composites.China Welding, 2011,20 (2): 73-80.
Although being ternary active solder macroscopic view, Zn-Al-Li sees solder/parent material interface fine and close (being superior to not containing the Zn-5Al solder of Li); Though just can be observed the solder infiltration but amplify about 200 times; The oxide-film at matrix/solder interface can only effectively be abolished at regional area, but the oxide-film at most of matrix/solder interface continued presence still.This and Li activity are greatly; Self is very easily oxidized (for example; The Zn-Al-Li brazing filler metal is positioned in the air after about 1 hour just can the oxidation blackout) and oxide-film is thickened rapidly; And then limited the active performance of Li, and the Li atomic radius makes the Li atom that has got into matrix spread relevant to the depth direction for a short time.Applicant's paper: Zhang Guifeng is seen in correlative study, Guo Yang, Zhang Jianxun, Zhang Linjie: Zn-Al-Li system and the wetability of Zn-Al brazing filler metal to the SiCp/ZL101 aluminum matrix composite. the China YouSe Acta Metallurgica Sinica, and 2012, employ, wait to deliver.
Positive and negative two aspect experimental results show (among the embodiment that sees below about implementing the introduction of result of implementation), the Zn-Al-Mg that the present invention proposes be the alloy system of ternary active solder aspect preparation, to improve aspect, joint microstructure and performance improvement aspect all be feasible to wetability.
2. solder composition range aspect: for set Zn-Al-Mg is the ternary active solder, from reducing solder fusing point angle, confirms that the mass fraction of each alloying element is: 3～10% Al, and 2～7% Mg, all the other are Zn; Corresponding fusion range is 337～475 ℃.
3. solder preparation method aspect: its subject matter is the oxidation and the volatilization that prevents Zn liquid that prevents Mg.Said low melting point Zn-Al-Mg is that the preparation method of ternary active solder is: 1) select materials: selecting raw material is pure Al, pure Zn, pure Mg piece (or grain, sheet); 2) batching: with pure Al, pure Zn, pure Mg is 3～10% Al according to mass percent, 2～7% Mg, all the other are Zn; Wherein let pure Zn in top of mixture and be positioned in the closed crucible; 3) melting: at first in the crucible of sealing, feed pure Ar, deaeration; Then, under the Ar protection, under high-frequency heating, after pure Zn melted rapidly earlier, partially liq was protected pure Mg and Mg is dissolved in the Zn liquid, and pure subsequently Al also is dissolved in rapidly in the Zn-Mg alloy liquid; Then; Alloy liquid is in 500 ℃～600 ℃ following meltings (when surpassing 600 ℃, particularly surpass 650 ℃, Zn can occur and volatilize in a large number) in the time of will continuing heating; Insulation 30min makes unreacted refractory metal in the liquid alloy of fusing in advance, continue dissolving, and makes alloy liquid homogenization of composition; Stop heating then, continuing under the protection of Ar, to leave standstill cooled and solidified is the brazing filler metal alloy piece.4) employing chilling belt-rejecting technology is prepared into the paper tinsel band or is prepared as solder sheet or solder rod through hot rolling technology.
4. utilizing above-mentioned low melting point Zn-Al-Mg is the low frequency of the ternary active solder auxiliary active soldering that rubs by a narrow margin, and its concrete technology is following: 1) with 100#, 400# sand paper welded piece surface grinding just; 2) utilize alcohol or acetone oil removing, scrubbing; 3) solder sheet or paper tinsel band are preset between the welded piece, and apply the pressure of 1MPa; 4) Ar that feeds 1～5L/min protects down or in air, after being heated to 330 ℃, pressure being reduced to 0.01～0.5MPa also continuing welded piece is heated to 400～550 ℃; 5) wait to be incubated 0～1min after, it is auxiliary that the bottom welded piece is applied the friction that is continuously 5～200s, its amplitude is 0.1～1mm, frequency is 10～50Hz; 6) the after-applied 0.05～2MPa pressure of vibration, insulation 0～10min can obtain good welding point.
5. the described low-cost low frequency composition and the operation principle of auxiliary friction mechanism transmission system by a narrow margin is a (see figure 2): with single-phase DC buncher or monopole asynchronous motor is power; Electric machine main shaft (14) drives eccentric wheel (10) through keyway; Eccentric throw between eccentric axis and electric machine main shaft axis is set to 0.05～1mm, and the amplitude that determined thus eccentric mechanism produces is 0.1～2mm, and frequency is determined by motor speed, is 10～50Hz mechanical oscillation; Wearing and tearing cause amplitude error to occur between parts in order to avoid, and eccentric wheel is through removable brass bearing drive link (11); Connecting rod is again through another bearing driving sliding block (12).Use this transmission system, realize the linear reciprocating motion of slide block, the final realization can replace artificial scraping along the auxiliary striping of the friction between weld interface.The photo in kind of this transmission system is seen Fig. 3.
6. a kind of in inverted T shape, dovetail groove or the directed guide rod of slide block guide rail (13, see Fig. 2).
The low melting point Zn-Al-Mg that the present invention researched and developed is that ternary active solder preparation is simple, cost is low, need not brazing flux, striping ability and wetability, to be much better than pure Zn be binary solder, strength of welded joint height with Zn-Al; The scope of application is extensive, is particularly suitable for the low melting point aluminium alloy and is the aluminum matrix composite of matrix with the low melting point aluminium alloy.
Description of drawings
(DSC: differential thermometric analysis appearance) result and chilling get rid of the band forming effect to the test of Fig. 1 Zn-5Al-4Mg solder fusing point;
Fig. 2 utilizes active soldering device sketch map that low frequency rubs auxiliary by a narrow margin and the low frequency schematic diagram of friction system a little;
Annotate: 1-body of heater heater; The 2-thermocouple; The 3-loading tool; The 4-fixed mount; 5-solder sheet or solder paper tinsel band;
The 6-welded piece; The 7-induction coil; 8-protective gas air inlet; 9-mechanical oscillation platform;
10-eccentric wheel (seeing Fig. 2 b and 2c) or cam (seeing Fig. 2 d and 2e); The 11-connecting rod; The 12-objective table;
13-base (guide rail (seeing Fig. 2 c and e) of band dovetail groove (seeing Fig. 2 b and d) or inverted T shape groove); The 14-line shaft
Fig. 3 low frequency is the auxiliary active brazing process parameter sketch map of reciprocating friction by a narrow margin;
The binary eutectic solder Zn-5Al that Fig. 4 does not have a Mg under 520 ℃ * 20min (a, b) and 520 ℃ * 30min (c, d) flow argon shield to the wettability test interface photo of SiCp/ZL101 (explain: no Mg solder striping weak effect, the interface is not fine and close, wetability is poor);
The Zn-5Al-4Mg low melting point ternary active solder paper tinsel band of Fig. 5 the present invention exploitation under the Ar atmosphere protection, under 520 ℃ to the wettability test interface photo of SiCp/ZL101: (a) with (b) 1min; (c) and (d) 3min; (e) and (f) 5min; (g) and (h) 20min (explain: this new solder and mother metal reaction are early and fully);
Fig. 6 Zn-5Al-4Mg ternary active of the present invention solder and Zn-5Al binary eutectic solder having/no low frequency by a narrow margin the auxiliary operating mode lower contact intensity contrast result of reciprocating friction (be not superior to the strength of joint after the Zn-5Al solder applies friction even Zn-5Al-4Mg ternary active solder of the present invention does not apply frictional behaviour yet; When apply friction auxiliary after, Zn-5Al-4Mg ternary active solder gained strength of joint is higher, can reach the composite mother metal 91%);
The active soldering joint microstructure photo that the low frequency of Fig. 7 contrast test Zn-5Al solder after the mechanical oscillation 20s time under 520 ℃ of welding temperature 0.06MPa pressure rubs auxiliary by a narrow margin (although auxiliary friction is described effectively, effect is far away from Zn-5Al-4Mg);
The A-TLP joint microstructure photo (explain even this new solder do not apply auxiliary friction can obtain preferably interface connection yet, but still have part interface have oxide-film) of Fig. 8 Zn-5Al-4Mg solder behind insulation 20min under 520 ℃ the welding temperature 1MPa pressure;
The active soldering joint microstructure photo that the low frequency of Fig. 9 Zn-5Al-4Mg solder after the mechanical oscillation 20s time under 520 ℃ of welding temperature 0.06MPa pressure rubs auxiliary by a narrow margin (explanation applies auxiliary friction back whole interface oxide-film and abolishes all better);
Figure 10 Zn-5Al-4Mg ternary active solder 520 ℃ down insulation 1min to 10vol.%SiC
pCeramic particle/braze metal (P/M) Interface Microstructure in the/ZL101 aluminum matrix composite wettability test tissue (explain that Mg also can promote the P/M interfacial reaction and eliminate the P/M interfacial gap).
The specific embodiment
For example the present invention is done more below and describe in detail.Main contents comprise three aspects: the preparation of (1) low melting point Zn-5Al-4Mg ternary active solder; (2) two kinds of solders (promptly do not have the Zn-5Al of Mg and contain the Zn-5Al-4Mg ternary active solder of Mg) wetability contrast test; (3) two kinds of solders (having/no Mg) are in two kinds of operating modes (have/reciprocating friction is auxiliary by a narrow margin for no low frequency) contrast test of soldering processes down.Used aluminum matrix composite mother metal is 10Vol.%SiCp/ZL101 in wetability evaluation and the soldering processes test.
● the preparation test of Zn-5Al-4Mg ternary active solder of the present invention:
With preparation 30g low melting point Zn-5Al-4Mg ternary active solder is example, preparation method's concrete steps: 1) select materials: select raw material to be: pure Al piece, pure Zn piece, pure Mg piece; 2) batching: according to quality is the Al piece of 1.5g, the Mg of 1.2g, and all the other are Zn; Wherein pure Zn is placed on top of mixture and mixture is positioned in the closed crucible; 3) melting: at first in the crucible of sealing, feed the pure Ar of 3.5L/mind, deaeration; Then, under the Ar protection, under high-frequency heating, after pure Zn melted rapidly earlier, partially liq was protected pure Mg and Mg is dissolved in the Zn liquid, and pure subsequently Al also is dissolved in rapidly in the Zn-Mg alloy liquid; Then, alloy liquid stops heating 500 ℃ of following meltings behind the insulation 30min in the time of will continuing heating; Then, continuing under the protection of Ar, to leave standstill cooled and solidified is the brazing filler metal alloy piece.4) adopt the chilling belt-rejecting technology to be prepared into paper tinsel band (linear velocity is 12.65m/min for copper roller diameter 105mm, copper roller thickness 10mm).
● the wetability contrast test: test as a comparison, for the Zn-5Al solder paper tinsel band of no Mg, the wetability appreciation condition is 520 ℃ * 20min (for a long time); For the Zn-5Al-4Mg solder paper tinsel band of the present invention's exploitation, the wetability appreciation condition is 520 ℃ * 1min, 520 ℃ * 3min, 520 ℃ * 5min (short time).Used aluminum matrix composite mother metal is 10Vol.%SiC
p/ ZL101 aluminum matrix composite; Atmospheric condition is the Ar protection environment that flows.
● soldering processes contrast test: for checking the present invention designs (adding active element Mg) and novelty and the good result thereof of soldering processes (applying low frequency interface friction by a narrow margin) aspect two at the solder composition, with 10Vol.%SiC
p/ ZL101 aluminum matrix composite is a mother metal; Zn-5Al binary solder with no Mg is the contrast solder; Have, no low frequency is by a narrow margin under the auxiliary condition of reciprocating friction, carried out adopting the contrast test of the Zn-5Al-4Mg ternary active solder that contains Mg and the low temperature brazing technology of the Zn-5Al binary solder of no Mg respectively.
Apply the low frequency test method and the condition of the auxiliary active soldering welding procedure of reciprocating friction by a narrow margin: 1) with 100#, 400# sand paper welded piece surface grinding just; 2) utilize alcohol or acetone oil removing, scrubbing; 3) respectively two kinds of solder paper tinsel bands are preset at 10Vol.%SiC
pBetween/ZL101 the aluminum matrix composite, and apply the pressure of 1MPa; 4) the Ar protection that feeds 5L/min through after the high-frequency induction heating to 330 ℃, is reduced to pressure 0.05MPa and continues welded piece is heated to 520 ℃ down or in air; 5) wait to be incubated 1min after, it is auxiliary that the bottom welded piece is applied the friction that is continuously 20s, its amplitude is 0.25mm, frequency is 24Hz; 6) the friction continued applies 0.05MPa pressure, insulation 0min, cooling immediately.
The test method and the condition of the active soldering welding procedure that no low frequency rubs auxiliary by a narrow margin: 1) with 100#, 400# sand paper welded piece surface grinding just; 2) utilize alcohol or acetone oil removing, scrubbing; 3) respectively two kinds of solder paper tinsel bands are preset at by between the weldering aluminum matrix composite mother metal, and apply the pressure of 1MPa; 4) the Ar protection that feeds 5L/min through after the high-frequency induction heating to 330 ℃, is reduced to 0.05MPa with pressure, and continues welded piece is heated to 520 ℃ down or in air; 5) wait to be incubated 1min after, the bottom welded piece is applied 1MPa pressure; 6) cool off behind the insulation 20min.
Result of implementation of the present invention is following:
Fig. 1 is that a kind of low melting point ternary active solder Zn-5Al-4Mg solder fusing point test among the present invention (adopts that differential thermometric analysis appearance---DSC) result and chilling get rid of the band forming effect.But because when doing heat and analyze with differential thermometric analysis appearance, when promptly measuring fusion curve, programming rate is 10 ℃/min under argon gas atmosphere is protected, this balanced reaction with phasor is different, belongs to non-equilibrium fusing.Finding has two endothermic peaks in the curve, first endothermic peak be since in the solder paper tinsel band tissue fusing of Zn-Al-Mg ternary four phase eutectic compositions absorb heat and cause; Second endothermic peak is because the intermetallic compound Mg Zn in the solder
2Dissolving caused.Shown in the DSC fusion curve of Fig. 1, the fusing point of Zn-5Al-4Mg solder paper tinsel band is 344.9 ℃～356.9 ℃.
Get rid of band through the homemade belting chilling under the linear velocity of 12.65m/min that gets rid of, gained Zn-5Al-4Mg solder paper tinsel band outward appearance is more smooth; And solder paper tinsel band is very peripheral neat, and its tapability is fine.But this solder paper tinsel band is more crisp relatively, frangible.
Fig. 2 is the low frequency device sketch map of the auxiliary active soldering method of reciprocating friction by a narrow margin; Wherein Fig. 2 a is low frequency a kind of in the device sketch map of the auxiliary active soldering method of reciprocating friction by a narrow margin, and Fig. 2 b, 2c, 2d and 2e are the mechanical transmission structure sketch map in this soldering.Its basic principle is: a. heating system: the alternating magnetic field that produces through induction coil (7) through the high frequency alternating current is in body of heater heater (1); With welded piece (6) and solder (5) heating, record the temperature of welded piece (6) through thermocouple (2) through radiant heat simultaneously; B. welding surroundings system: if in the indignant welding down of protection, then protective gas gets into furnace chamber through gas inlet (8); C. reciprocating friction system a little: mechanical oscillation produce mechanisms (10,11,12,13,14) and import mechanical oscillation through shaking platform (9) in welding process; D. compression system: the on-load pressure in welding process through loading tool (3) to welded piece (6) and solder (5) pressurization.
Fig. 3 is the active brazing process parameter sketch map that low frequency rubs auxiliary by a narrow margin.Can find out by figure, near specimen temperature does not rise to the solder solidus temperature before, apply big pressure, do not apply low frequency and rub auxiliary by a narrow margin; When temperature rises to solidus temperature, pressure is reduced to certain value; Continue heating sample and after welding temperature, be incubated a period of time; The low frequency that applies the certain frequency amplitude that continues necessarily the to apply assistant brazing that rubs by a narrow margin keeps or intensified pressure subsequently, cooling or be incubated a period of time after lower the temperature.
Fig. 4 be the binary eutectic solder Zn-5Al that tests as a comparison under 520 ℃ of mobile argon shields at the temperature retention time of 20min and 30min wettability test photo to SiCp/ZL101.Can find out that by Fig. 4 a and b the Zn-5Al solder with SiCp/ZL101 any effect does not take place, promptly under the help that does not have brazing flux, can't wetting mother metal when 520 ℃ of insulation 20min.Though and can find that in Fig. 4 c and d Zn separates out along crystal boundary in the SiCp/ZL101 mother metal; But interfacial gap, oxide-film between residual solder and the SiCp/ZL101 mother metal still exist, and this shows that Zn makes under the SiCp/ZL101 matrix surface film occurrence degree of liquefaction and undercurrent be not enough to the continuity of broken oxide-film.So Zn can not abolish the oxide-film that matrix shows having no under the situation of other subsidiary conditions.
Fig. 5 be Zn-5Al-4Mg solder paper tinsel band under the Ar atmosphere protection, be respectively under 1min, 3min, 5min and the 20min at 10Vol.%SiC 520 ℃ of following temperature retention times
pWettability test on the/ZL101 mother metal is organized photo.Can find out by Fig. 5 a and b; In time, solder has occurred in the subregion effectively being connected with mother metal, and liquefaction phenomenon has appearred in the mother metal surf zone at insulation 1min; Promptly begin to abolish through the mode that film dissolves down the oxide-film of matrix surface, the part has begun wetting mother metal; And it is more in Fig. 5 c and d, to occur effective join domain between solder and mother metal, and solder can wetting well 10Vol.%SiC in the time at 3min
p/ ZL101 mother metal; In Fig. 5 e and f, can find out that the living column crystal of growing of couplet at original interface has taken place to cross over mother metal residual solder; In Fig. 5 g and h, solder is realized complete solder bond with mother metal; The SiC particle gathers in the top layer partially, and the remaining quantity of Zn is few, and this shows dissolving and diffusion fully, and isothermal solidification is realized basically.
Fig. 6 be utilize Zn-5Al solder and Zn-5Al-4Mg solder under 520 ℃ under 0.06MPa pressure the soldering 10Vol.%SiC of low frequency auxiliary by a narrow margin friction continuing 5s and 20s
pThe shearing strength of joint of/ZL101 mother metal and in the shear strength contrast of the auxiliary by a narrow margin friction braze welding joint of no low frequency of insulation 20min under 1MPa pressure under 520 ℃.Can find out by Fig. 6; The shear strength of mother metal is 130MPa; And be 97MPa (reach mother metal shear strength 74.6%) in the shear strength of the soldered fitting of the auxiliary by a narrow margin friction of low frequency 5s, be 119MPa (reach mother metal shear strength 91.5%) in rub the by a narrow margin shear strength of the soldered fitting that continues 20s of low frequency; The shear strength of auxiliary joint also reaches 78MPa (reach mother metal shear strength 60%) and the no low frequency that utilizes this solder rubs by a narrow margin; But utilize the tradition Zn-5Al solder that comes to exist, the soldered fitting intensity that rubs auxiliary by a narrow margin at no low frequency is merely 13MPa; The shear strength of auxiliary soldered fitting is 70MPa (reaches mother metal shear strength 53.8%) and the low frequency that the Zn-5Al solder is continuously 20s in fraction time rubs by a narrow margin.
Fig. 7 is that the soldered fitting of Zn-5Al solder paper tinsel band behind the auxiliary by a narrow margin friction 20s of low frequency under 520 ℃ of welding temperature 0.06MPa pressure organized photo.As can be seen from Figure 7, there is not interfacial gap in the welding point tissue, and do not occur the defectives such as cavity that ceramic phase particles is gathered partially or ceramic phase occurs because wetability is bad on every side; But still there is 10Vol.%SiC in most of zone
pThe original interface of/ZL101 mother metal.The auxiliary soldering of this explanation friction can broken its matrix surface oxide-film because the Zn-5Al solder can not effectively be removed oxide-film, so there is discontinuous oxide-film.
Fig. 8 is the auxiliary by a narrow margin friction welding 10Vol.%SiC of the no low frequency of Zn-5Al-4Mg solder paper tinsel band behind insulation 20min under 520 ℃ the welding temperature 1MPa pressure
p/ ZL101 mother metal joint microstructure photo.As can be seen from Figure 8, there is not oxide-film in most zone in the welding point tissue, and joint microstructure is fine and close evenly, does not occur that ceramic phase particles is gathered partially or defective such as cavity; Have only regional area to have interrupted oxide-film, this explanation solder can be removed the oxide-film of its matrix surface, but property is bad because the molten metal of the liquefaction on mother metal surface flows, so can not fully remove the oxide-film of its matrix surface.
Fig. 9 is the soldering 10Vol.%SiC of Zn-5Al-4Mg solder after the auxiliary by a narrow margin friction of low frequency under 520 ℃ of welding temperature 0.06MPa pressure continues 20s
pThe soldered fitting of/ZL101 mother metal is organized photo.Can find out by Fig. 9 a and b, not occur the cavity in the brazed seam, not have oxide-film; Simultaneously, have a spot of SiC ceramic phase particles in the brazed seam, and the interface is fine and close between these particles and the braze metal; Crossed over the column crystal of the adhesion growth at original interface between brazed seam and the mother metal, this can think that solder is realized complete solder bond with mother metal.
Figure 10 be Zn-5Al-4Mg ternary active solder 520 ℃ down insulation 1min to 10vol.%SiC
pP/M Interface Microstructure in the/ZL101 aluminum matrix composite wettability test tissue.Can find out by Figure 10 a and b; The SiC particle and the metal interface (P/M interface) that distribute in Zn-5Al-4Mg ternary active solder diffusion region do not have interfacial gap; But having formed one deck and the thick thin layer of 1 μ m near the SiC particle, the power spectrum point analysis of this thin layer is whether Zn-Mg-Si-C alloy or this thin layer of intermetallic compound are that the cenotype that reaction generates awaits further to confirm; But can confirm that the P/M interface is fine and close.
Summarize said; Wetability qualification test and soldering test all show; Low melting point Zn-Al-Mg of the present invention is that ternary active solder and the reaction of Al matrix can be carried out ahead of time, reaction profile is even, the extent of reaction is abundant; Continuity that can fast and effeciently broken aluminum substrate surface film oxide, thus good to aluminium alloy and aluminum matrix composite wetability; (brazing temperature is low to consider the particularity of Zn base solder; Eutectic reaction is arranged in rich Zn side and makes the solution restricted etc. to the dissolution degree of Al), when being aided with low frequency reciprocal interface friction machinery striping by a narrow margin again, can abolish Al matrix surface oxide-film better effectively, improve strength of joint.In addition, Mg also helps to improve the wetability (see figure 10) at ceramic particle and molten metal (P/M) interface.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Though the present invention discloses as above with preferred embodiment; Yet be not in order to limiting the present invention, anyly be familiar with the professional and technical personnel, in not breaking away from technical scheme scope of the present invention; When the method for above-mentioned announcement capable of using and technology contents are made a little change or be modified to the equivalent embodiment of equivalent variations; In every case be the content that does not break away from technical scheme of the present invention, to any simple modification, equivalent variations and modification that above embodiment did, still belong in the scope of technical scheme of the present invention according to technical spirit of the present invention.
Claims (6)
1. aluminum matrix composite and aluminium alloy are the ternary active solder with low melting point Zn-Al-Mg; It is characterized in that: on the basis of Zn-Al binary eutectic, add active element Mg; Thereby constituting low-melting, as to improve interfacial reaction homogeneity Zn-Al-Mg is the ternary active solder; Wherein the mass fraction content of each alloying element is: 3～10%Al, and 2～7%Mg, all the other are Zn.
2. low melting point Zn-Al-Mg is the ternary active solder according to claim 1; It is characterized in that: said low melting point Zn-Al-Mg is that the fusion range of ternary active solder is 337 ℃～475 ℃, and wherein the fusion range of typical activity solder composition Zn-5Al-4Mg is 344.9～356.9 ℃.
3. low melting point Zn-Al-Mg is the preparation method of ternary active solder according to claim 1 or claim 2, it is characterized in that, operation is:
1) selects materials: select raw material to be: pure Al piece, pure Zn piece, pure Mg piece;
2) batching: with pure Al, pure Zn, pure Mg according to mass percent be 3～10% Al, 2～7% Mg, all the other prepare burden for Zn;
3) charging: above-mentioned Al, Mg, three kinds of original materials of Zn are positioned in the closed crucible, and pure Zn wherein that fusing point is low, that density is big, inertia is strong places top of mixture so that with the active Mg of Zn liquid protection;
4) melting: at first in the crucible of sealing, feed pure Ar, deaeration; Continuation under Ar protection, high-frequency heating melting, dissolving; For preventing the evaporation of Zn liquid, alloy liquid is continued to be heated to 500 ℃, be incubated 30min then, continue melting, dissolving, make the liquid phase ingredient homogenising; Then, continuing under the protection of Ar, to leave standstill cooled and solidified is the brazing filler metal alloy piece;
5) moulding: gravity segregation in Zn, occurs for preventing Al, Mg light metal alloy atom, adopt the chilling belt-rejecting technology to be prepared into the paper tinsel band brazing filler metal alloy piece; Perhaps be prepared as solder sheet or solder rod so that preset through insulation, hot rolling technology.
4. the preparation method of solder according to claim 3; It is characterized in that: 1), mid-term first in melting; Utilize Zn liquid to prevent the further oxidation of Mg, promptly after the minimum pure Zn of fusing point melted rapidly earlier, partially liq was protected pure Mg and Mg is dissolved in the Zn liquid; 2) subsequently in the fusion process of pure Al, the same dissolving thinking of utilizing makes the higher relatively Al of fusing point dissolving and liquefying in the Zn-Mg alloy liquid that forms in advance, thereby can reduce smelting temperature, to prevent the evaporation of Zn liquid; 3) continue insulation and make the liquid phase ingredient homogenising; 4) having benefited from determined composition range tapability can be good and not cataclasm, adopts the chilling belt-rejecting technology to be prepared into the banded solder of the uniform paper tinsel of composition.
5. the low frequency auxiliary active soldering method of reciprocating friction by a narrow margin is characterized in that: adopted " shape of a saddle " pressurization programme-control; Said " shape of a saddle " pressurization program is: 1) solder sheet or paper tinsel band are preset between the welded piece, and apply the pressure of 1MPa, so that the interface driving fit, import little distortion and anti-oxidation; 2) be heated near the solder solidus 330 ℃ after, for avoiding solder to extrude pressure is reduced to 0.01～0.5MPa, and continues welded piece is heated to 400～550 ℃; 3) wait to be incubated 0～1min after, one of welded piece is applied the auxiliary friction in interface of 5～200s, its amplitude is 0.1～2mm, frequency is 10～50Hz; 4) vibration stops after-applied 0.05～2MPa pressure, insulation 0～10min, cooling.
6. low frequency according to claim 5 is the auxiliary active soldering method of reciprocating friction by a narrow margin; It is characterized in that; The auxiliary friction system in its low-cost interface is that eccentric wheel transmission mechanism, the slide block guide rail of 0.05～1mm formed by single-phase DC buncher or monopole asynchronous motor, eccentric throw; The interface friction amplitude of its generation is 0.1～2mm, and frequency is 10～50Hz; Its slide block guide rail is a kind of in inverted T shape, dovetail groove or the directed guide rod.
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| CN103934590A (en) * | 2014-04-13 | 2014-07-23 | 北京工业大学 | ZnAlMgIn high temperature lead-free solder |
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| CN105458547A (en) * | 2015-12-28 | 2016-04-06 | 西安交通大学 | Active brazing filler metal suitable for cast aluminum-based composite material reinforced through high-volume-fraction SiC and preparation method of active brazing filler metal |
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| CN106944698A (en) * | 2017-05-12 | 2017-07-14 | 哈尔滨工业大学 | The SiC ceramic and the direct method for welding of SiC ceramic reinforced aluminum matrix composites ultrasonic cryogenic being modified based on thermal oxide surface |
| CN106944698B (en) * | 2017-05-12 | 2019-12-10 | 哈尔滨工业大学 | SiC ceramic or SiC ceramic reinforced aluminum matrix composite material ultrasonic low-temperature direct brazing method based on thermal oxidation surface modification |
| CN113732422A (en) * | 2021-09-23 | 2021-12-03 | 郑州机械研究所有限公司 | Brazing flux-free brazing method and brazing filler metal paste for aluminum alloy |
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