CN106271214B - A kind of preparation method being brazed stainless steel Ag-Cu/W nano-multilayer film solder - Google Patents
A kind of preparation method being brazed stainless steel Ag-Cu/W nano-multilayer film solder Download PDFInfo
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- CN106271214B CN106271214B CN201610851891.0A CN201610851891A CN106271214B CN 106271214 B CN106271214 B CN 106271214B CN 201610851891 A CN201610851891 A CN 201610851891A CN 106271214 B CN106271214 B CN 106271214B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/32—Selection of soldering or welding materials proper with the principal constituent melting at more than 1550 degrees C
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention relates to a kind of preparation methods for being brazed stainless steel Ag-Cu/W nano-multilayer film solder.Silver accounts for 16.7-37.5% in the multilayer film solder, and copper accounts for 12.5-33.3%, and tungsten accounts for 50%.Using magnetron sputtering method alternating sputtering silver-bearing copper layer and tungsten layer.Silver-bearing copper layer is sputtered simultaneously by two targets of silver-colored target and copper target, and tungsten target is individually sputtered with a target.Every layer of silver-colored copper layer thickness is 8nm-14nm, and every layer of W thickness degree is less than 10nm.The atomic ratio of Ag and Cu is between 0.5:1 to 3:1 in silver-bearing copper layer.Alternating deposit 200-400 period, final total 4 μm -8 μm of film thickness.It is irregular that the present invention not will cause solder, in addition, solder thickness can easily be controlled by sputtering the period.Using the reduction fusing point effect of nanoparticle, so that the fusing point of nanoparticle sharply declines.When soldering, conversion zone can form the eutectic or hypoeutectic structure of low melting point with matrix, and brazing temperature is effectively reduced.
Description
Technical field
The invention belongs to welding technology fields, are related to a kind of soldering stainless steel Ag-Cu/W nano-multilayer film solder.
Background technique
Stainless steel has stronger corrosion resistance, extensively because its surface forms one layer of thin and compact chromium oxide protective film
Applied to power station, chemical industry and paper-making process, and many commercial product such as building trades and automobile.The low-temperature welding of stainless steel
Common method is soldering, and the welding temperature of soldering is low, and the influence to stainless Steel Properties is minimum, and solder joint is beautiful, therefore to not
The research practical value with higher that the drill rod that becomes rusty welds.Stainless steel, which is brazed common solder, copper base solder, silver-base solder etc..Copper
When base solder vacuum brazing, a large amount of evaporations can pollute furnace wall, and furnace interior insulation is caused to fail, and thermocouple temperature control failure increases cleaning
The difficulty of work.The welding good fluidity of silver-base solder, intensity is also very high, but fusing point is also relatively high.Therefore, one is developed
The novel solder of kind stainless steel soldering, while solder is analyzed to the wetability of stainless steel, Interface Microstructure and joint bending stiffness
It influences, to have certain reference to the stainless steel soldering in engineer application, this work is extremely urgent.
Research hotspot one of of the nano-multilayer film as film applications, is constantly subjected to the extensive concern of researcher in recent years.
The significant changes for the thermal properties such as the fusing point of nano material reduces, sintering temperature reduces, crystallization temperature reduces derive from nanometer material
Table (boundary) face effect of material.Nano-multilayer film has the advantages that welding temperature is low as solder, can be improved efficiency, reduce at
This.Help to ensure that the performance of base material stainless steel.
The present invention is directed to study the Ag-Cu/W nano-multilayer film solder that a kind of fusion temperature is low, wettability is excellent, compare
Au base solder and Ni base solder have lower cost, and the pollution compared to fine copper solder is small, and the fusing point compared to Ag base solder is low.
The frangible compounds that soldered fitting generates are few, and can be applied to the soldering of a variety of occasions.Solder of the present invention is suitable for all kinds of stainless steels
Material itself and its soldering connection with ceramics or the dissimilar materials such as titanium alloy.
Summary of the invention
The purpose of the present invention be exactly directed to brazing temperature is low, the high performance demand of soldered fitting and above-mentioned Au base solder,
Deficiency present in Ni base solder, fine copper solder and Ag base solder concrete application and design a kind of soldering stainless steel Ag- is provided
Cu/W nano-multilayer film solder.The preparation method of the solder, follows the steps below:
Prepare the method that nano-multilayer film selects magnetron sputtering.Preparation before magnetron sputtering: the surface of stainless steel base material according to
It is secondary that 600#, 800# is used to be placed in ultrasonic washing instrument, after the polishing of 1000# sand paper with ethyl alcohol-ethanol-acetone-ethyl alcohol sequence
Cleaning 4 times, surface 5 minutes every time, is dried up, be placed on after cleaning with nitrogen gun in magnetron sputtering chamber, is sputtered by control
Period prepares required thickness, and solder is directly sputtered to base material surface.
A kind of preparation method being brazed stainless steel Ag-Cu/W nano-multilayer film solder, it is characterised in that: the nanometer
Multilayer film solder is made of three kinds of silver, copper and tungsten elements, and wherein silver accounts for 16.7-37.5%, and copper accounts for 12.5-33.3%, and tungsten accounts for
50%；Using magnetron sputtering method alternating sputtering silver-bearing copper layer and tungsten layer；Silver-bearing copper layer is sputtered simultaneously by two targets of silver-colored target and copper target, tungsten
Target is individually sputtered with a target；Every layer of silver-colored copper layer thickness is 8nm-14nm, and every layer of W thickness degree is less than 10nm；Ag in silver-bearing copper layer
Atomic ratio with Cu is between 0.5:1 to 3:1；Alternating deposit 200-400 period, final total 4 μm -8 μm of film thickness.Optimization
Scheme is that silver accounts for 16.7%, and copper accounts for 33.3%, and tungsten accounts for 50%.Or silver accounts for 25%, copper accounts for 25%, and tungsten accounts for 50%.Or silver accounts for
37.5%, copper accounts for 12.5%, and tungsten accounts for 50%.
The nano-multilayer film solder prepared is done into DTA test, easily learns the fusing point of the solder (usually from DTA figure
Between 820 DEG C -890 DEG C).Using the temperature for being higher than 50 DEG C of fusing point, in diffusion in vacuum furnace brazing stainless steel.
Soldering processes are as follows, open recirculated water, and stainless steel base material is placed in fixture and is fixed, the soldering of vacuum drying oven is arranged
Process curve, after brazing process, furnace cooling.
The advantages of technical solution of the present invention is: Ag-Cu/W nano-multilayer film solder of the present invention both can be used to be brazed not
Become rusty steel alloy and structural member, be also applied for ordinary carbon steel or Ni-based, ferrous alloy itself and with a kind of soldering of material such as ceramics.
The great advantage of Ag-Cu/W nano-multilayer film solder of the present invention is that practicability and brazing temperature are low.1, conventional solder is generally adopted
The modes such as foil or soldering paste are taken, the shortcomings that foil does not all help the thickness of solder and the control of holding time gap, soldering paste is
Be easy to smear it is irregular, and solder of the present invention take directly sputter at soldering base material surface to be welded mode, not will cause
Solder is irregular, in addition, the thickness of solder can easily be controlled by sputtering the period.2, often purely by addition drop in conventional solder
Element (Si or B etc.) is melted to reduce brazing temperature, but melting point depressant will cause the increase of soldered fitting brittleness, be unfavorable for certain pairs of prickers
The higher industrial application place of plumb joint strength demand.Solder of the present invention is using a kind of novel side for reducing fusing point
Formula, using the reduction fusing point effect of nanoparticle, compared with conventional powder material, since the particle of nanoparticle is small, surface
Energy is high, specific surface atomicity is more.These surface atom near neighboring coordinations are not complete, and activity is big and volume is much smaller than massive material
Required increased interior energy is much smaller when nanoparticle fusing, this fusing point for allowing for nanoparticle sharply declines.It is carried out in furnace
When soldering, conversion zone can form the eutectic or hypoeutectic structure of low melting point with matrix, and brazing temperature is effectively reduced, and reduce high temperature pricker
The weld metal zone brittle intermetallic thing generated is welded, connector crackle and stomata is reduced, improves the compactness and mechanical property of connector.This just keeps away
The disadvantage of increase melting point depressant is exempted from.3, widely applicable, which has good wellability to stainless steel, or even to other
Metal and ceramics also have good wellability.As long as solder ingredient, preparation process and Joining Technology are appropriate, which can be used for respectively
Kind stainless steel-ceramic, the connection of stainless steel-metal.Nano-multilayer film solder can be combined with a variety of soldering tech, such as titanium nickel
The soldering of active nano multilayer film laser, the soldering of ultrasonic sensing soldering connection, ultrasonic wave added laser etc..
Detailed description of the invention
Fig. 1 is the DTA image of solder of the present invention (number 2), and Cong Tuzhong endothermic peak can be seen that fusing point is 842 DEG C.General pricker
Material takes brazing temperature to be higher than 50 DEG C -70 DEG C of fusing point, and both the brazing temperature of No. 2 solders can be determined as 900 DEG C with the method.
Fig. 2 is High Speed Photography Images when solder of the present invention (number 3) heats, and solder is melted and moistened at 820 DEG C
Wet, fine in stainless steel surface spreadability, wetting areas is about 5.33mm2, the intensity of soldered fitting with solder layer diffusion
It disappears and is gradually increased.a)800℃b)810℃c)820℃d)830℃e)840℃f)850℃g)860℃h)870℃i)880
DEG C j) 890 DEG C k) are enlarged drawing.
Fig. 3 is the structural schematic diagram of solder of the present invention (number 3) under transmission electron microscope, and nano-multilayer film is clear in structure, side
Boundary is obvious.
Specific embodiment
Technical solution of the present invention is further described below with reference to embodiment；It prepares nano-multilayer film and selects magnetic control
The method of sputtering.Preparation before magnetron sputtering: 600#, 800# are successively used in the surface of stainless steel base material, after the polishing of 1000# sand paper,
It is placed in ultrasonic washing instrument, is cleaned 4 times with ethyl alcohol-ethanol-acetone-ethyl alcohol sequence, 5 minutes every time, nitrogen is used after cleaning
Rifle dries up surface, is placed in magnetron sputtering chamber, prepares required thickness by the control sputtering period, and solder is straight
It connects and sputters at base material surface.Alternating sputtering silver-bearing copper and tungsten.Silver-bearing copper layer is sputtered simultaneously by two targets of silver-colored target and copper target, using radio frequency
Power supply, tungsten target is individually sputtered with a target, using DC power supply.Ag-Cu layers are less than with a thickness of 8nm-14nm, W thickness degree
10nm.Ag-Cu layers are solder layers, and the atomic ratio of Ag and Cu is between 0.5:1 to 3:1 in silver-bearing copper layer.W layers are diffusion barriers
Layer avoids agglomerating and aoxidize, do not play solder.Alternating deposit 200-400 period, final total 4 μm -8 μm of film thickness, vacuum
It is sealed.
Table 1 gives in 15 embodiments and each embodiment of nano-multilayer film solder described in technical solution of the present invention
Chemical analysis and atomic percent composition.
Nano-multilayer film solder described in above-described embodiment is prepared by following process route:
(1) Ag-Cu/W nano-multilayer film is prepared with high vacuum magnetron sputtering apparatus, and disc-shaped target diameter 80mm, W target is pure
It spends 99.95%, Ag target purity and is higher than 99.97%, anaerobic Cu target purity is higher than 99.97%.Substrate is 304 stainless steel to be welded.
First stainless steel base material to be welded ethyl alcohol-ethanol-acetone-ethyl alcohol sequence is cleaned by ultrasonic 4 times, 5 minutes every time, deposition was preceding again
1min is impacted with nitrogen gun, surface to be welded is placed in deposit cavity upward.Modulation period, λ (was defined as Ag-Cu molecular layers thick hAg-Cu
With W molecular layers thick hWThe sum of) it is 20nm, modulation ratio η (is defined as Ag-Cu molecular layers thick hAg-CuWith W molecular layers thick hWThe ratio between) be
1, the sputtering power of setting Ag target, Cu target and W target splashes so that the ratio of Ag and Cu is 0.5:1,1:1 and 3:1 in Ag-Cu sublayer
Firing rate rate is about 1nm/min.Nano-multilayer film solder is deposited directly on base material, first deposited W layer, alternating deposit Ag-Cu and
W, final stainless steel base material superficial layer to be welded are Ag-Cu.
The specific deposition process parameters for preparing multilayer film are as shown in table 2.In experimentation when the opening of strict control baffle
Between regulate and control thicknesses of layers, rotate sample turntable alternating deposit multilayer film.
It is using the method that nano-multilayer film solder of the present invention is brazed:
Sputtering is had to the stainless steel base material to be welded of nano-multilayer film solder, is assembled according to the requirement of jointing,
It is placed in vacuum drying oven (or induction furnace etc.)；Heating process curve is set, starts to be brazed, is cooled to the furnace after soldering heat preservation
Room temperature.
Embodiment one: solder vacuum brazing stainless steel of the present invention, size 30*10*1mm, using overlapping mode, overlap joint are used
Length 10mm, solder can full filling pricker cutting edge of a knife or a sword, soldering is preferable, and soldered fitting shear strength can reach 30-60MPa, fracture point
Analysis display fracture position is at solder.
Embodiment two: solder induction brazing stainless steel of the present invention and zirconia ceramics are used, stainless steel and xenogenesis are realized
The connection of the especially difficult welding ceramics material of material.
Embodiment three: using solder brazing stainless steel of the present invention and Ti-6Al-4V, is able to achieve high-quality connection, titanium alloy tool
There are excellent performances, the aero titanium alloys such as specific strength is high, corrosion resistance and fatigue resistance are good often to need different with ceramics, aluminium, stainless steel etc.
Kind material is attached.During being brazed titanium alloy, it is often found that there is a phenomenon where diffusion reactions for solder and base material, it is this
Adverse reaction, which will lead to, generates brittle intermetallic compound in interface, and weld seam will be caused there are biggish tearing tendency, made
Joint performance deteriorates.It can be to avoid causing to damage and improve welding to base material performance using nano-multilayer film solder of the present invention
The performance of connector, this in addition to the application of electricity, optics and magnetics etc., opens up new nano-multilayer film in soldering direction
Application direction has important practical significance.
Claims (4)
1. a kind of preparation method for being brazed stainless steel Ag-Cu/W nano-multilayer film solder, it is characterised in that: the nanometer is more
Tunic solder is made of three kinds of silver, copper and tungsten elements, and according to atomic percent, wherein silver accounts for 16.7-37.5%, and copper accounts for 12.5-
33.3%, tungsten accounts for 50%, and the sum of silver and copper account for 50%；Using magnetron sputtering method alternating sputtering silver-bearing copper layer and tungsten layer；Silver-bearing copper layer by
Two targets of silver-colored target and copper target sputter simultaneously, and tungsten target is individually sputtered with a target；Every layer of silver-colored copper layer thickness is 8nm-14nm, often
Layer W thickness degree is less than 10nm；Alternating deposit 200-400 period, final total 4 μm -8 μm of film thickness.
2. according to the method described in claim 1, copper accounts for 33.3%, and tungsten accounts for 50% it is characterized by: silver accounts for 16.7%.
3. according to the method described in claim 1, copper accounts for 25%, and tungsten accounts for 50% it is characterized by: silver accounts for 25%.
4. according to the method described in claim 1, copper accounts for 12.5%, and tungsten accounts for 50% it is characterized by: silver accounts for 37.5%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110699656A (en) * | 2019-11-07 | 2020-01-17 | 昆明理工大学 | Sn-Zn-Ag solder film and preparation method thereof |
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| CN106676490B (en) * | 2017-01-09 | 2019-04-12 | 北京工业大学 | A kind of preparation of titanium/nickel composite membrane and the method for connecting titanium or titanium alloy |
| CN106695141B (en) * | 2017-01-21 | 2019-08-09 | 北京工业大学 | A method of utilizing nano-multilayer film self-propagating reaction auxiliary laser high temperature brazing |
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| CN109317864A (en) * | 2018-12-06 | 2019-02-12 | 衢州学院 | A kind of preparation method and applications technique of nickel base powder brazing material |
| CN110280926B (en) * | 2019-06-25 | 2021-11-09 | 上海大学 | High-flux preparation method of Sn-Zn-Cu solder |
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