CN105234547A - Connecting technology for metals without solid solubility - Google Patents
Connecting technology for metals without solid solubility Download PDFInfo
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- CN105234547A CN105234547A CN201510683322.5A CN201510683322A CN105234547A CN 105234547 A CN105234547 A CN 105234547A CN 201510683322 A CN201510683322 A CN 201510683322A CN 105234547 A CN105234547 A CN 105234547A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/02—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating by means of a press ; Diffusion bonding
- B23K20/023—Thermo-compression bonding
- B23K20/026—Thermo-compression bonding with diffusion of soldering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/16—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating with interposition of special material to facilitate connection of the parts, e.g. material for absorbing or producing gas
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/22—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded
- B23K20/233—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating taking account of the properties of the materials to be welded without ferrous layer
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/18—Dissimilar materials
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Abstract
The invention relates to a connecting technology for metals without solid solubility. The technology includes the steps that the first metal and the second metal to be connected are pretreated; powder of the second metal is pressed into a blank with the thickness of 2-5 mm; the first metal, the blank and the second metal are sequentially stacked; the first metal, the blank and the second metal which are sequentially stacked are fixed and pressed so that the first metal and the second metal can be tightly attached to the blank; and the first metal, the blank and the second metal which are fixed and pressed are subjected to annealing treatment, wherein the first metal is molybdenum or tungsten, the second metal is copper or silver, and the annealing temperature of the annealing treatment is 10-50 DEG C lower than the melting point of the second metal. According to the technical scheme, the technology is simple, and a uniform and continuous bonding interface and high bonding strength between the metals without solid solubility can be achieved.
Description
Technical field
The present invention relates to a kind of intermetallic interconnection technique, particularly relate to a kind of Joining Technology of not solid solution metal mutually.
Background technology
In some technical fields, especially in the technical fields such as nuclear fusion, often exist the interconnective demand of two metals of not solid solution mutually; A concrete example, molybdenum has the features such as higher fusing point, good thermal conductivity, low-steam pressure and low sputtering due to it and becomes excellent plasma in the face of material, and copper has the features such as good thermal conductivity due to it and becomes excellent heat sink material, because nuclear fusion technology needs plasma in the face of material and heat sink material couple together, therefore, not solid solution metal molybdenum and copper need to be joined together mutually.Here mutual not solid solution metal refers to that intermetallic solid solubility is less, is even zero.
At present, the existing interconnective method of not solid solution metal mutually comprises: using the metal or alloy with two kinds of equal solid solutions of material to be connected as intermediate layer, utilize intermediate layer to realize with the phase counterdiffusion of two kinds of materials to be connected the connection that two kinds are with connecting material; As BYJ.E.RAMIREZ delivered on WeldingJournal (welding magazine) in 2014 about stainless steel and the interconnective article of titanium, this paper describe nickel deposited and copper between stainless steel and titanium, by making nickel and copper form intermetallic compound with the stainless steel at two ends and titanium respectively, thus realize the connection between stainless steel and titanium.But, between two kinds of metals of two kinds of mutual not solid solutions, introduce the material composition that other materials not only can change connector, and be easy to produce harmful effect to the additional properties of material in specific application environment (as ferromagnetism).
In view of this, industry often wishes the metal straight of two kinds of mutual not solid solutions to connect to couple together, as at application number be 201310593854.0 patent application in, molybdenum and copper directly couple together by the technology such as ion implantation and plating that have employed.
But inventor is realizing finding in process of the present invention, existing two kinds of metal straights by mutually not solid solution are connecing the method coupled together and there is the uneven problem such as discontinuous of combination interface between the more loaded down with trivial details and two kinds of metals of technique.
Summary of the invention
One of the object of the invention is to, a kind of Joining Technology of not solid solution metal is mutually provided, technical problem to be solved is, while Simplified flowsheet, make the intermetallic combination interface of not solid solution mutually even and continuous, and make the intermetallic of not solid solution mutually have preferably bond strength, be very suitable for practicality.
Object of the present invention and solve its technical problem and can adopt following technical scheme to realize.
The Joining Technology of a kind of not solid solution metal mutually proposed according to the present invention, described method comprises: carry out pretreatment to the first metal to be connected and the second metal; Bimetallic powder is pressed into the base that thickness is 2-5 millimeter; Stack according to the first metal, base and bimetallic order; The first metal, base and the second metal that order stacks are fixed and apply pressure, fits tightly to make the first metal and the second metal and base; Annealing in process is carried out to being in the first metal, base and the second metal of fixing also pressurized state; Wherein, the first metal comprises: molybdenum or tungsten, and the second metal comprises: copper or silver, and the annealing temperature of described annealing in process is lower than bimetallic fusing point 10-50 degree Celsius.
By technique scheme, the Joining Technology of not solid solution metal mutually of the present invention at least has following advantages and beneficial effect: the present invention by arranging the base be pressed into by bimetallic powder between the first metal and the second metal, and to the first metal stacked, base and the second metal are fixed pressurization and annealing in process, when annealing temperature is a little less than bimetallic fusing point, second metal can not deform melting phenomenon, again because the fusing point of the first metal is higher than bimetallic fusing point, therefore, only there is the base formed by bimetallic powder to deform melting phenomenon, thus generation Transient liquid phase, because the base of liquid phase fully can contact with the first metal joint face, and diffuse in the joint face of the first metal uniformly, therefore, the joint face of the first metal can form the alloying interface of uniformly continous, because base and the second metal are same metal, therefore, base and second metal of liquid phase can be linked together closely by atoms permeating, thus technical scheme provided by the invention is not when adding third party's material, utilize pressed compact, fixing pressurization and annealing process the first metal and the second metal straight to be connect to couple together, not only technique is simple, and the intermetallic combination interface of not solid solution mutually can be made even and continuous, and the intermetallic of not solid solution is mutually made to have preferably bond strength.
In sum, the present invention has significant progress technically, and has significantly positive technique effect, is really a new and innovative, progressive, practical new design.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, in order to technological means of the present invention can be better understood, and can be implemented according to the content of description, and can become apparent to allow above and other object of the present invention, feature and advantage, below especially exemplified by preferred embodiment, and coordinate accompanying drawing, be described in detail as follows.
Accompanying drawing explanation
Fig. 1 is the Joining Technology flow chart of not solid solution metal mutually of the present invention;
Fig. 2 is the schematic diagram of the metal bar for tension test of the present invention;
Fig. 3 is the schematic diagram pressurizeed to metal bar of the present invention;
Fig. 4 is the matrix pattern SEM observation figure in the intermediate layer of metal bar of the present invention;
Fig. 5 is the linkage interface pattern SEM observation figure of molybdenum of the present invention and copper;
Fig. 6 is that analysis chart swept by the linkage interface diffusion depth SEM line of molybdenum of the present invention and copper;
Fig. 7 is the hot strength schematic diagram of molybdenum of the present invention and copper;
Fig. 8 is the stretching fracture schematic diagram of molybdenum of the present invention and copper.
Detailed description of the invention
For further setting forth the present invention for the technological means reaching predetermined goal of the invention and take and effect, below in conjunction with accompanying drawing and preferred embodiment, to its detailed description of the invention of Joining Technology of mutual not solid solution metal proposed according to the present invention, structure, feature and effect thereof, be described in detail as follows.
The Joining Technology of embodiment one, mutually not solid solution metal.The flow process of the method as shown in Figure 1.
In Fig. 1, S100, pretreatment is carried out to the first metal to be connected and the second metal.
Concrete, the first metal in the present embodiment can be molybdenum, and the first metal can be also tungsten, and the second metal can be copper, and the second metal also can be silver.That is, molybdenum and copper can link together by the technical scheme of the present embodiment, also molybdenum and silver can be linked together, and also tungsten and copper can be linked together, and tungsten and silver can also be linked together.
The first metal in the present embodiment can be tabular, also bar-shaped (as pole or the square bar etc.) or bulk etc. of elongated shape can be become, and the second metal can be tabular, also can in bar-shaped (as pole or the square bar etc.) of elongated shape or bulk etc.
It should be noted that, interconnective first metal and bimetallic concrete shape should be arranged according to the actual requirements; Although the present embodiment is when carrying out bond strength experiment to the first metal interconnected and the second metal, the first metal of round bar shape and the second metal of round bar shape are selected, but this Joining Technology not representing the present embodiment is only applicable to the first metal of round bar shape and the second metal of round bar shape to interconnect.
The present embodiment carries out pretreated process to the first metal and generally includes: polish to the face to be connected of the first metal, then, alcohol washes process is carried out successively to the face to be connected after polishing, process of deoiling, washed with de-ionized water process, etching processing, washed with de-ionized water process and Ultrasonic Cleaning process.
The present embodiment carries out a pretreated concrete example to the first metal: use alcohol to clean (as cleaned the face to be connected of the first metal with alcohol) the first metal, then, the first metal crossed by alcohol washes is put into the liquid that deoils and is soaked (as soaked about 3 minutes, and to be connected of the first metal should fully immerse deoil in liquid), to remove the greasy dirt on to be connected of the first metal; The proportioning of the liquid that deoils in the present embodiment can be: the liquid that deoils of 1 liter is made up of the concentrated hydrochloric acid 50 milliliters of 37%, the concentrated sulfuric acid 50 milliliters of 98% and distilled water; Afterwards, first metal is taken out from the liquid that deoils and puts into deionized water (as soaked about 5 minutes, and to be connected of the first metal should fully immerse in deionized water), the present embodiment can utilize deionized water repeatedly to clean (cleaning three times to the first metal as utilized deionized water) the first metal; Then, first metal is immersed in etching liquid and carries out etching processing (as soaked about 10 minutes, and to be connected of the first metal should fully immerse in etching liquid), so that on to be connected of the first metal, form nano level etching hole, thus increase the surface area of to be connected of the first metal; The proportioning of the etching liquid in the present embodiment can be specially: the etching liquid of 1 liter is made up of concentrated hydrochloric acid 150 milliliters, the concentrated sulfuric acid 150 milliliters of 98%, 80 gram of three oxidation network and the distilled water of 37%; Afterwards, the first metal taken out from etching liquid and put into deionized water (as soaked about 15 minutes, and to be connected of the first metal should fully immerse in deionized water); Then, Ultrasonic Cleaning (as utilized supersonic frequency for 50Hz and temperature is that the ultrasonic wave of 30 degrees Celsius was to be connected of the first metal cleaning 20 minutes) is carried out to the first metal; After Ultrasonic Cleaning terminates, the first metal is dried stand-by.
The present embodiment carries out pretreated process to the second metal and generally includes: polish to bimetallic face to be connected, then, carries out alcohol washes process, washed with de-ionized water process and Ultrasonic Cleaning process successively to the face to be connected after polishing.
The present embodiment carries out a pretreated concrete example to the second metal: use alcohol to clean (as cleaned the face to be connected of the second metal with alcohol) the second metal, then, the second metal crossed by alcohol washes puts into deionized water (as soaked about 15 minutes, and the bimetallic to be connected should fully immerse in deionized water); Then, Ultrasonic Cleaning (as utilized supersonic frequency for 50Hz and temperature is that the ultrasonic wave of 30 degrees Celsius was to be connected of the first metal cleaning 20 minutes) is carried out to the second metal; After Ultrasonic Cleaning terminates, the second metal is dried stand-by.
The present embodiment is conducive to obtaining the first metal of high strength and bimetallic combination interface by carrying out pretreatment to the first metal and the second metal.
S110, bimetallic powder is pressed into the base that thickness is 2-5 millimeter.
Concrete, the granular size of the bimetallic powder in the present embodiment is no more than 5 microns usually, and granular size is generally 3-5 micron.
The present embodiment can utilize film laminator that bimetallic powder is pressed into base, as utilized film laminator to apply the pressure of 20-35MPa to a certain amount of bimetallic powder, and suppresses 5-10 minute, thus obtains the base that thickness is 2-5 millimeter.The shape of base depends on the shape of the first metal and the bimetallic to be connected usually, and the present embodiment can utilize the mould adapted to the first metal and bimetallic to be connected shape to have corresponding shape to make base.
The number of the bimetallic powder that the present embodiment uses depends on the first metal and the area of bimetallic to be connected and the thickness of base usually.
The present embodiment should ensure that the thickness of base is no less than 2 millimeters, and to ensure the intensity of the first metal and bimetallic combination interface, and this enforcement should ensure that the thickness of base is no more than 5 millimeters, to avoid unnecessary waste of material.
It should be noted that, although the step S110 in the present embodiment is placed on being described of step S100 below, but, this does not represent that step S100 must be performed before step S110, the step S100 of the present embodiment and step S110 can perform simultaneously, in addition, the step S110 of the present embodiment also can perform prior to step S100.
S120, to stack according to the first metal, base and bimetallic order.
Concrete, the base in the present embodiment should be arranged between the first metal and the bimetallic to be connected; In addition, after bimetallic powder being pressed into thickness and being the base of 2-5 millimeter, and before being arranged at by base between the first metal and the bimetallic to be connected, preferably, the present embodiment can carry out pretreatment to base; The present embodiment carries out pretreated process to base and generally includes: carry out alcohol washes process, washed with de-ionized water process and Ultrasonic Cleaning process etc. successively to base.
The present embodiment carries out a pretreated concrete example to base: use alcohol to clean (as cleaned the whole outer surface of base with alcohol) base, then, deionized water (as soaked about 15 minutes, and base should submergence be in deionized water completely) put into by the base crossed by alcohol washes; Then, Ultrasonic Cleaning (as utilized supersonic frequency for 50Hz and the ultrasonic wave that temperature is 30 degrees Celsius cleans 20 minutes to whole base) is carried out to base; After Ultrasonic Cleaning terminates, base is dried stand-by.
S130, order the first metal, base and the second metal that stack be fixed and apply pressure, all fitting tightly with base to make to be connected and the bimetallic to be connected of the first metal.
Concrete, the present embodiment can utilize pressue device be fixed the first metal, base and the second metal that order stacks and apply pressure.Utilize pressue device to be fixed order the first metal, base and the second metal that stack and execute a stressed concrete example and be: stack one piece of quartz plate in the outside of the first metal, one piece of quartz plate is stacked in bimetallic outside, and stack one block of tungsten plate respectively in the outside of two pieces of quartz plates, the left and right sides of two blocks of tungsten plates is respectively arranged with bolt hole, two molybdenum pressurization bolt are each passed through the bolt hole of the left and right sides of two blocks of tungsten plates, and two blocks of tungsten plates are interconnected; Torque wrench (moment of torsion can be set to 30Nm) is used to rotate the molybdenum pressurizing nut of two pieces of tungsten plate left and right sides, thus the first metal, base and the second metal that order stacks are fixed and apply certain pressure (as applied the pressure of 3MPa-10MPa, and can be 3MPa usually).
In addition, the present embodiment is preferably after carrying out alcohol washes process (as cleaned the surface of two pieces of quartz plates and two blocks of tungsten plates respectively with alcohol) respectively to two pieces of quartz plates and two blocks of tungsten plates, and recycling quartz plate, tungsten plate, molybdenum pressurization bolt and molybdenum pressurizing nut are fixed the first metal, base and the second metal that order stacks and apply pressure.
S140, carry out annealing in process to being in the first metal of fixing and pressurized state, base and the second metal.
Concrete, the present embodiment to be in the first metal of fixing and pressurized state, base and the second metal carry out annealing in process time, should ensure that the first metal and the second metal all can not deform melting phenomenon, the annealing temperature namely in the present embodiment should respectively lower than fusing point and the bimetallic fusing point of the first metal; Because the fusing point of the first metal is higher than bimetallic fusing point; again because the base suppressed by the bimetallic powder to deform fusing and present Transient liquid phase prior to the second metal usually; therefore; the present embodiment is when carrying out annealing in process; annealing temperature should lower than bimetallic fusing point 10-50 degree Celsius; thus while making base produce Transient liquid phase, ensure that the first metal and the second metal are in solid phase respectively.When the second metal is copper, the annealing temperature in the present embodiment can be 1050 degrees centigrade; When the second metal is silver, the annealing temperature in the present embodiment can be 950 degrees centigrade.
The present embodiment to being in the example that the first metal of fixing and pressurized state, base and the second metal carry out of annealing in process concrete is: the first metal, base and the related pressue device of the second metal are put into atmosphere protection stove together, with the programming rate of 6 degrees Celsius per minute, temperature in atmosphere protection stove is increased to 250 degrees Celsius, and keeps about 10 minutes at the temperature of 250 degrees Celsius; With the programming rate of 6 degrees Celsius per minute, temperature in atmosphere protection stove is increased to annealing temperature (as 1050 degrees Celsius or 950 degrees Celsius) again; after annealing temperature keeps 3 hours-5 hours (being generally 4 hours); starting cooling, lowering the temperature with the stove type of cooling as adopted.
After above-mentioned steps S100-S140, first metal and the second metal are linked together closely, in order to verify uniformity and the continuity of the combination interface between the first metal and the second metal, and in order to measure the bond strength between the first metal and the second metal, invention has been following experiment:
Experimental procedure A, choose copper metal bar 1 and molybdenum rod 3 (as shown in Figure 2) that diameter is 10mm.
Experimental procedure B, the surface of molybdenum rod 3 deoiled and cleans; As first cleaned the outer surface of molybdenum rod 3 with alcohol, then, being immersed to be connected one end of molybdenum rod 3 deoils in liquid (proportioning of the liquid that deoils can be: the liquid that deoils of 1 liter is made up of 37% concentrated hydrochloric acid 50mL+98% concentrated sulfuric acid 50mL+ distilled water), the length immersing the molybdenum rod 3 deoiled in liquid can be 5mm, molybdenum rod 3 soaks after 3 minutes deoiling in liquid, molybdenum rod 3 is taken out from the liquid that deoils, and immerse in deionized water soak 5 minutes, to clean molybdenum rod 3, deionized water can be utilized repeatedly to clean 3 times molybdenum rod 3.
Experimental procedure C, the surface of copper metal bar 1 to be cleaned; As first cleaned the outer surface (as face to be connected) of copper metal bar 1 with alcohol, then, the copper metal bar 1 of scrub is immersed in deionized water to soak after 15 minutes and take out, utilize supersonic frequency for 50Hz and the ultrasonic wave that temperature is 30 DEG C carries out Ultrasonic Cleaning 20 minutes to copper metal bar 1, then, copper metal bar 1 is dried stand-by.
Experimental procedure D, etching processing is carried out to the face to be connected of molybdenum rod 3; As to be connected one end of the molybdenum rod 3 through washed with de-ionized water is immersed in etching liquid (proportioning of etching liquid can be: the etching liquid of 1 liter is made up of 37% concentrated hydrochloric acid 150mL+98% concentrated sulfuric acid 150mL+ distilled water+80g chromium trioxide), etch 10 minutes, molybdenum rod 3 is taken out from etching liquid, and immerse in deionized water soak 15 minutes, then, utilize supersonic frequency for 50Hz and the ultrasonic wave that temperature is 30 DEG C carries out Ultrasonic Cleaning after 20 minutes to molybdenum rod 3, molybdenum rod 3 is dried stand-by.
Experimental procedure E, pressed compact and cleaning treatment are carried out to copper powder, the copper powder 5 grams that granular size is 5 microns as got, 5 grams of copper powders are poured in the mould for press mold, and the mould that copper powder is housed is put into film laminator, under the pressure of 30MPa, copper powder is suppressed 5-10 minute, copper powder is become there is 3-5 height and diameter is the round base 2 of 10mm, circle base 2 is cleaned with alcohol, and complete for circle base 2 submergence is soaked 15 minutes in deionized water, then, circle base 2 is taken out from deionized water, and utilize supersonic frequency for 50Hz and the ultrasonic wave that temperature is 30 DEG C carries out Ultrasonic Cleaning after 20 minutes to molybdenum rod 3, circle base 2 is dried stand-by.
Experimental procedure F, copper metal bar 1, circle base 2 and molybdenum rod 3 to be stacked, and to be fixed and pressurized treatments; As copper metal bar 1, circle base 2 and molybdenum rod 3 superpose (as shown in Figure 2) successively, form sample 7 (as shown in Figure 3), the quartz plate 6 (as shown in Figure 3) crossed of placement alcohol washes respectively up and down of sample 7, and the tungsten plate 4 (as shown in Figure 3) that specification is 150mm × 150mm × 2mm is placed respectively in the outside of two pieces of quartz plates 6, the both sides of tungsten plate 4 are respectively arranged with two molybdenum pressurization bolt 5, then, the torque wrench adopting moment of torsion to be set to 30Nm rotates the molybdenum pressurizing nut that specification is M8, to be fixed sample 7 and to pressurize.
Experimental procedure G, annealing in process is carried out to pressue device and sample 7; As pressue device fixed with pressurized device and putting into atmosphere protection stove together with the sample 7 pressurizeed; the temperature in atmosphere protection stove is made to be increased to 250 DEG C with the heating rate of 6 DEG C per minute; and keep 10 minutes at the temperature of 250 DEG C; then; 1050 DEG C are increased to the heating rate of 6 DEG C per minute; and keep 4 hours at the temperature of 1050 DEG C, then, to start cooling with the stove type of cooling.
After experimental procedure H, annealing in process terminate, open pressue device, copper metal bar 1 and molybdenum rod 3 are joined together.
Experimental procedure I, the intermediate layer matrix pattern of SEM (SEM) to sample 7 is utilized to observe.
Fig. 4 is the SEM observation figure of the intermediate layer matrix pattern of sample 7, as can be seen from Figure 4 the copper particle in round base 2 matrix there occurs a large amount of fusings, this can ensure in sintering process, circle base 2 produces micro-deformation due to fusing thus is filled in the gap of to be connected of molybdenum rod 3, thus expand the physical contact of to be connected, by having carried out the pressure heat-preserving of certain hour in annealing process, spread between atom, interpenetrate, finally achieve the metallurgical binding between molybdenum and copper.
Experimental procedure J, the combination interface pattern of SEM to sample 7 is utilized to carry out observation analysis.
Fig. 5 is the result utilizing SEM to observe sample 7 combination interface pattern, and the molybdenum layer 8 in Fig. 5 is connected combination interface closely with the diffusion of layers of copper 9, and the two becomes an entirety.
Experimental procedure K, utilize the combination interface diffusion depth of SEM to sample 7 to carry out line to sweep analysis.
Fig. 6 utilizes SEM to carry out to sample 7 combination interface diffusion depth the schematic diagram that line sweep obtains, as can be seen from Figure 6: successfully achieve between molybdenum atom and copper atom mutually evenly and continuous print diffusion, obtain metallurgical binding.
Experimental procedure L, hot strength test is carried out to sample 7; As utilized electronic universal tester (model is CSS-44100, and Changchun testing machine produced), hot strength test is carried out to sample 7; The draw speed of electronic universal tester is 1mm/min, until be stretched to copper and the fracture of molybdenum combination interface of sample 7, record maximum load amount (being labeled as F), stress strain curve as shown in Figure 7.
Experimental procedure M, the fracture of sample 7 to be observed.
With the stereomicroscope observation stretching fracture also lower fracture apperance photo (as shown in Figure 8) of shooting; As can be seen from Figure 8: the fracture area of the intermediate layer circle base of sample 7 is black, other regions are white, this mainly due in sample 7 drawing process the copper on top layer, intermediate layer taken away from matrix by molybdenum bar, the binding ability also describing the molybdenum of the sample 7 of the present embodiment and copper is thus better.
Experimental procedure N, fracture to be calculated.
Image-ProPlus software (MediaCybernetics company of U.S. image analysis software) is utilized to calculate, to obtain area of fracture (being labeled as A), the area in the region that the side to the right as the circle of calculating chart 8 is surrounded by black silhouette line; By maximum load amount F divided by area of fracture A, can obtain interface bond strength between molybdenum and copper laminar metal matrix composite layer, the test result of this interface bond strength is as shown in table 1.
Table 1: molybdenum and copper metal layer shape composite extension test result
From above-mentioned table 1, the copper metal bar 3 of the present embodiment and molybdenum rod 1, after being joined together, have preferably bond strength.
The above is only preferred embodiment of the present invention, not any pro forma restriction is done to the present invention, although the present invention discloses as above with preferred embodiment, but, above-described embodiment is also not used to limit the present invention, any those skilled in the art are not departing within the scope of technical solution of the present invention, make a little change when the technology contents of above-mentioned announcement can be utilized or be modified to the Equivalent embodiments of equivalent variations, in every case be the content not departing from technical solution of the present invention, according to any simple modification that technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (10)
1. a Joining Technology for mutual not solid solution metal, is characterized in that, comprising:
Pretreatment is carried out to the first metal to be connected and the second metal;
Bimetallic powder is pressed into the base that thickness is 2-5 millimeter;
Stack according to the first metal, base and bimetallic order;
The first metal, base and the second metal that order stacks are fixed and apply pressure, all fits tightly with base to make to be connected and the bimetallic to be connected of the first metal;
Annealing in process is carried out to being in the first metal, base and the second metal of fixing also pressurized state;
Wherein, the first metal comprises: molybdenum or tungsten, and the second metal comprises: copper or silver, and the annealing temperature of described annealing in process is lower than bimetallic fusing point 10-50 degree Celsius.
2. the method for claim 1, is characterized in that, describedly carries out pretreated step to the first metal to be connected and the second metal and comprises:
Described first metal and the bimetallic to be connected are polished respectively;
Alcohol washes process is carried out successively to the face to be connected of described first metal, process of deoiling, washed with de-ionized water process, etching processing, washed with de-ionized water process and Ultrasonic Cleaning process;
Alcohol washes process, washed with de-ionized water process and Ultrasonic Cleaning process are carried out successively to described bimetallic face to be connected.
3. the method for claim 1, is characterized in that, the step of described etching processing comprises:
The joint face of the first metal is immersed in etching liquid.
The proportioning of described etching liquid is: the etching liquid of 1 liter comprises: the concentrated hydrochloric acid 150 milliliters of 37%, the concentrated sulfuric acid 150 milliliters of 98%, 80 gram of three oxidation network and distilled water.
4. the method for claim 1, is characterized in that, described bimetallic powder comprises: granular size is no more than the bimetallic powder of 5 microns.
5. the method for claim 1, is characterized in that, the described thickness that is pressed into by bimetallic powder is that the base of 2-5 millimeter comprises:
Utilize film laminator to apply the pressure of 20-35MPa to bimetallic powder, and suppress 5-10 minute, to obtain the base of thickness for 2-5 millimeter.
6. the method for claim 1, is characterized in that, described method also comprises:
Alcohol washes process, washed with de-ionized water process and Ultrasonic Cleaning process are carried out successively to described base.
7. the method as described in claim arbitrary in claim 1 to 6, is characterized in that, described the first metal, base and the second metal stacked order is fixed and executes stressed step and comprise:
Quartz plate is stacked respectively in the outside of the first metal and bimetallic outside;
Tungsten plate is stacked respectively in the outside of two pieces of quartz plates;
The molybdenum pressurizing nut that the left and right sides rotating two blocks of tungsten plates by torque wrench is arranged respectively, is fixed with the first metal, base and the second metal that stack order and applies the pressure of 3MPa-10MPa.
8. method as claimed in claim 7, it is characterized in that, described method also comprises:
Respectively alcohol washes process is carried out to described quartz plate and tungsten plate.
9. the method as described in claim arbitrary in claim 1 to 6, is characterized in that, the described step to being in the first metal of pressurized state, base and the second metal and carrying out annealing in process comprises:
With the programming rate of 6 degrees Celsius per minute, temperature is risen to 250 degrees Celsius;
Keep 10 minutes at the temperature of 250 degrees Celsius;
With the programming rate of 6 degrees Celsius per minute, temperature is risen to annealing temperature;
After annealing temperature keeps 3 hours-5 hours, start cooling.
10. the method as described in claim arbitrary in claim 1 to 6, is characterized in that:
When described second metal is copper, described annealing temperature is 1050 degrees Celsius;
When described second metal is silver, described annealing temperature is 950 degrees Celsius.
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| CN105537751A (en) * | 2016-02-05 | 2016-05-04 | 兰微悦美（天津）科技有限公司 | Connection process for metal silver and tantalum not capable of being dissolved in each other in solid mode |
| CN105537750A (en) * | 2016-01-20 | 2016-05-04 | 天津大学 | High-strength connection process for copper-niobium rodlike metals under non-vacuum low-pressure condition |
| CN107398630A (en) * | 2017-06-26 | 2017-11-28 | 天津大学 | The high intensity of tungsten and copper is directly connected to technique |
| TWI791432B (en) * | 2016-04-01 | 2023-02-11 | 美商哈尼威爾國際公司 | Sputtering target assembly having a graded interlayer and methods of making |
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