CN109986191A - A kind of surface treatment method applied to metal/high-molecular connection - Google Patents
A kind of surface treatment method applied to metal/high-molecular connection Download PDFInfo
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- CN109986191A CN109986191A CN201910298766.5A CN201910298766A CN109986191A CN 109986191 A CN109986191 A CN 109986191A CN 201910298766 A CN201910298766 A CN 201910298766A CN 109986191 A CN109986191 A CN 109986191A
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- metal
- treatment method
- surface treatment
- macromolecule
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Classifications
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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
-
- 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
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
-
- 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
- B23K20/24—Preliminary treatment
-
- 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
- B23K20/26—Auxiliary equipment
Abstract
The present invention relates to a kind of surface treatment methods applied to metal/high-molecular connection, after metal surface grinding and polishing is cleaned, metal surface is impregnated with corrosive liquids, its surface is set to form one layer of conversion zone, the conversion zone includes the compound particle of metallic substrates and dispersion on the metallic substrate, during being connect with macromolecule, the melting macromolecule that mobility is promoted under high temperature forms close microcosmic occlusion and is bonded after coming into full contact with wetting with metallic substrates and compound particle, connect metal surface effectively with macromolecule.Compared with prior art, process of surface treatment of the present invention is applied widely, easy to operate, effectively reliable, can satisfy the connection research of the metal/high-molecular of variety classes and size.
Description
Technical field
The present invention relates to metal/high-molecular connections, at a kind of surface applied to metal/high-molecular connection
Reason method.
Background technique
Metal and high molecular compound be combined have biggish need in fields such as auto industry, aerospace, biological medicines
It asks.But the difference of biggish mechanics, calorifics, chemical property makes metal/high-molecular connect difficulty with higher.In general,
Metal is connected with macromolecule frequently with the methods of Nian Jie, mechanical connection and new welding process.Wherein, mechanical connection is with bonding
More traditional storeroom connection method is respectively present easy stress concentration, rivet increases construction weight and extreme environment and uses the longevity
Order the shortcomings that short, connection needs the front and back of complex process to handle.New welding process such as laser welding, Friction Stir Welding, surpasses
Sound wave welds it is possible to prevente effectively from disadvantages mentioned above.In these processes, laser welding and Friction Stir Welding use laser respectively
The mode of heat and frictional heat generation heats metal/high-molecular interface, to melt macromolecule, forms it between metal preferably
Macroscopic view occlusion be bonded with microcosmic.And supersonic welding is then that interface is transferred to using the high-frequency vibration wave of pressure head, metal and height
Molecule is in the mutual frictional heat generation in interface, so that macromolecule be made to melt to form connection.These methods have proven effectively to realize
Connection between metal and macromolecule.
However, all lower using intensity of the above-mentioned Joining Technology to not surface treated metal/high-molecular jointing.
To find out its cause, being because its connection mechanism is mainly the micro interface bonding effect after macromolecule melts with metal, bonding strength
It is unstable.Effective macro/micromechanical occlusion can not be formed between the metal/high-molecular of no surface treatment, so that lifting sub is strong
Degree.Therefore, the process of surface treatment for developing suitable metal/high-molecular connection is to improve metal/high-molecular jointing intensity
Effective way.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind effectively, using model
Enclose the wide surface treatment method for being applied to metal/high-molecular connection.
The purpose of the present invention can be achieved through the following technical solutions: a kind of table applied to metal/high-molecular connection
Surface treatment method: the following steps are included:
1. be covered with finer and close oxide layer since common metal is exposed to the atmosphere, as aluminium alloy, titanium alloy, steel with
Copper, story first use sand paper to the grinding and polishing of metal blocks surface and clean, to remove the oxide layer and spot of metal surface.
2. after metal surface grinding and polishing is cleaned, impregnating metal surface with corrosive liquids, its surface is made to form one layer of reaction
Layer, which includes the compound particle of exposed metallic substrates and dispersion on the metallic substrate, what is connect with macromolecule
In the process, the melting macromolecule and metallic substrates that mobility is promoted under high temperature come into full contact with wetting, and are formed with compound particle
It is closely microcosmic to be engaged and be bonded, it connect metal effectively with macromolecule.
The length and width range of the compound particle are 1 μm -20 μm, and the projected area of compound particle occupies
The altitude range of the 5%-40% of the conversion zone gross area, the prominent metal surface of compound particle are 0.1 μm -10 μm.
The corrosive liquids preferentially selects acid stronger corrosive agent, including in hydrofluoric acid, nitric acid, hydrochloric acid, sulfuric acid
One or more.In the selection of acid strength, for ensure acid solution to the intensity and corrosion efficiency of surface corrosion, hydrogen in acid solution
Ion concentration need to be greater than 0.1mol/L (i.e. pH value is lower than 1)；Excessive corruption for the compound particle for preventing acid solution from being formed to surface
It loses, hydrogen ion concentration need to be less than 10mol/L in acid solution (i.e. pH value is higher than -1).Therefore, hydrogen ion concentration need to be between in acid solution
Between 0.1mol/L -10mol/L.
The acid solution preferred concentration is the hydrofluoric acid of 0.5mol/L -10mol/L.
The time of the acid soak metal surface, according to different metal/high-molecular combinations and corrosive liquids
Selection, range are to differ for 5 seconds to 20 minutes.
The mode that the corrosive liquids impregnates metal is impregnated in ultrasonic wave, the power selection 10W-of ultrasonic wave
Between 200W.
The metal surface grinding and polishing is cleaned first be roughened after, then be immersed in acid solution, roughening treatment side
Method includes sandblasting, 3 D-printing or marking.The macro-asperity of certain method raising metal sheet surface can be used in roughening treatment,
To promote it to be engaged during the connection process with high molecular macro-mechanical.
The roughening treatment method is preferably blasting treatment, and sandblasting rear surface roughness range is 0.5 μm -100 μm.
Metal and macromolecule connection method after surface treatment include friction welding (FW), thermocompression bonding, Laser Welding or supersonic welding.
The conversion zone that the method for the present invention processing is formed has good auxiliary connection effect in metal/high-molecular connection procedure
Fruit:
1. the melting macromolecule that during the connection process, mobility is promoted under high temperature is contacted with fresh exposed metallic substrates
Afterwards, the compound particle of metal substrate surface is sufficiently soaked, form more close microcosmic occlusion and be bonded.Described is microcosmic
Occlusion with specific generation type be bonded is, passes through insertion metallic substrates after melting macromolecule wetting metal or compound particle
Micro-rough structure forms microcosmic occlusion, passes through the polar group (such as carbonyl, carboxyl and amino) and metallic substrates in macromolecule
Or compound particle forms chemical bonding.2. after connection, the compound particle of metal surface dense distribution is embossed can be with
Macromolecule forms effective pinning effect, with this effective lifting sub bonding strength.Effectively pin effect is specifically defined are as follows: on boundary
At face under the action of shear stress, the embossed crack propagation that can slow down and prevent metal/high-molecular interface of compound surface will
It is guided to macromolecule base material, to promote interface bonding strength.
Surface treatment method according to the present invention, because during the connection process without biggish volume under pressure and lower pressure
Auxiliary, therefore effective connection of metal/high-moleculars can be realized with many different connection methods, such as: friction welding (FW), thermocompression bonding,
Laser Welding, supersonic welding.Selection is illustrated using thermocompression bonding and friction welding (FW) in an embodiment of the present invention.
Compared with prior art, the invention has the following advantages:
1. this method is applied widely, applicable major part metal and high molecular connection, and Joining Technology can be a variety of
Multiplicity.General common metal (such as: steel, aluminium alloy, titanium alloy) and common macromolecule are (such as: polyethylene (PE), polyphenylene sulfide
(PPS), polyethylene terephthalate (PET), carbon fibre reinforced high-molecular material) it can be applicable at the surface in this method
Science and engineering skill promotes jointing performance.
2. the process of surface treatment that the present invention uses is more convenient effective.Required chemical solution is easier to obtain, surface
Treatment process time-consuming is short, operating cost is low, strength of joint is promoted significantly.
3. the process of surface treatment in the present invention is in the identical processing parameter of application, repeatable very high, table after processing
Face microscopic appearance is uniform, and bonding strength is stablized, and data are reliable.
Detailed description of the invention
Fig. 1 is the process schematic that the present invention is applied to thermocompression bonding；
Fig. 2 is that hydrofluoric acid treatment titanium alloy rear surface topography scan Electronic Speculum characterizes photo in embodiment 1；
Fig. 3 is that hydrofluoric acid+nitric acid mixed solution handles titanium alloy rear surface topography scan Electronic Speculum characterization photograph in embodiment 2
Piece；
Fig. 4 is the connection mechanism schematic diagram in the present invention after acid processing titanium alloy surface with PET.
Wherein, 1 is sheet metal, and 1a is titanium alloy plate used in embodiment；2 be the metal after surface treatment
Rough surface, in which: 2a is the titanium alloy surface that hydrofluoric acid treatment is used in embodiment 1, and 2b is that hydrogen fluorine is used in embodiment 2
Acid/nitric acid mixed solution processing metallic surface structures；3 be macromolecule block, and 3a is poly- terephthaldehyde used in embodiment
Sour second diester (PET) block；4 be conductive carbon brush；5 be pressure head；6 be load cell；7 (white is embossed) are after being surface-treated
The compound particle of metal surface, wherein 7a is embossed spot of the titanium alloy after hydrofluoric acid is surface-treated in embodiment, 7b
Be the surface relief spot thick by the processing of hydrofluoric acid/nitric acid mixed solution of titanium alloy in embodiment, 8 (dash-dotted gray lines) be without
Fracture path of the connector of surface treatment in extension test, 9 (dash-dotted gray lines) are that interface has the connector of compound particle to exist
Fracture path in extension test.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1:
It is connect applied to titanium alloy with the thermocompression bonding of polyethylene terephthalate (PET).First using sand paper by thickness 2~
The titanium alloy sheet surface grinding and polishing of 3mm, and ultrasound is cleaned in deionized water.The hydrofluoric acid for configuring 5wt%-10wt% concentration is molten
Liquid impregnates titanium alloy plate 5~20 seconds in ultrasonic wave.Titanium alloy surface scanning electron microscope after surface treated characterizes pattern
As shown in Figure 2.As it can be seen that the embossed spot 7a of a large amount of whites occurs in titanium alloy surface 2a in figure, spread out through power spectrum (EDS) with X-ray
It penetrates (XRD) and is detected as titanium oxide compounds particle, it is the titanium alloy surface of comparatively fresh, only that fast black base bottom, which is titanium alloy base material,
There is a small amount of oxygen element to be distributed.The area of the embossed oxide particle of white accounts for 15% or so of titanium alloy total surface, and after treatment
Titanium alloy surface be evenly distributed.
Using the installation way of Fig. 1, sheet metal 1 (titanium alloy) is fixed on the worktable using two conductive carbon brush 4.
Macromolecule block 3 is fixed on pressure head 5, and load cell 6 is integrated on pressure head 5.Conductive carbon brush 4 is connected with direct current generator, opens
Just pass through titanium alloy sheet using the electric current of 50~150A after dynamic motor to heat.Heat titanium alloy sheet to assigned temperature (200~
400 DEG C) after, control pressure head 5 pushes, and contacts macromolecule with titanium alloy sheet surface and keeps 10-50s, in lower pressure and high temperature
Connection is formed under collective effect.
Postwelding titanium alloy/PET connector shear tension intensity reaches 10MPa, is chemically treated compared to without titanium alloy surface
Connector (4.5MPa) strength enhancing be more than one times.Microscopic sdIBM-2+2q.p.approach discovery, the oxide particle of titanium alloy surface promoted metal/
It is acted in microcosmic occlusion between macromolecule significant.
Fig. 4 show titanium alloy surface and the connection mechanism schematic diagram of PET.When bearing shear stress, if without
Surface treatment, crackle 8 are extended readily along metal/high-molecular interface.And after titanium alloy surface acid etching, because of titanium alloy table
Face is throughout oxide particle 7, while to connect interface closer with high molecular chemical bonding on its fresh surface, and crackle 9 is difficult to
It is extended by interface, and needs to extend in macromolecule base material polyethylene terephthalate (PET) block 3a, to be promoted
Strength of joint.
Hydrofluoric acid treatment titanium alloy surface is used in the present embodiment, but according to different alloying components and applies needs,
It can choose different chemical solution processing metal surfaces in other embodiments.
In the present embodiment, the joint face between titanium alloy and macromolecule is plane, but in other embodiments can be any
Curved surface.
Embodiment 2:
It is connect applied to titanium alloy with the thermocompression bonding of polyethylene terephthalate (PET).First according to described in embodiment 1
Titanium alloy surface grinding and polishing is cleaned, and uses the mixed solution of 3wt% hydrofluoric acid and 30wt% nitric acid by titanium alloy sheet in ultrasound
It is impregnated 15 minutes in wave.Titanium alloy surface scanning electron microscope characterization pattern after surface treated is as shown in Figure 3.As it can be seen that making in figure
With the metallic surface structures 2b of hydrofluoric acid/nitric acid mixed solution processing throughout embossed spot 7b, but titanium in this embodiment
For alloy surface oxidation particle (embossed spot 7b) quantity than significantly reducing in embodiment 1, accounting for total surface area is only 5% left side
The right side is evenly distributed.
Using the installation way of Fig. 1, sheet metal 1 (titanium alloy) is fixed on the worktable using two conductive carbon brush 4.
Macromolecule block 3 is fixed on pressure head 5.Conductive carbon brush 4 is connected with direct current generator, and the electricity of 50~150A is just used after starting motor
Stream is by titanium alloy sheet to heat.After heating titanium alloy sheet to assigned temperature (200~400 DEG C), control pressure head is pushed, and makes high score
Son is contacted with titanium alloy sheet surface, is formed and is connected under lower pressure and high temperature collective effect.
Postwelding titanium alloy/PET connector shear tension intensity reaches 7MPa, chemically treated compared to without titanium alloy surface
Connector (4.5MPa) strength enhancing amplitude is 60%.
In the present embodiment, the joint face between titanium alloy and macromolecule is plane, but in other embodiments can be any
Curved surface.
Embodiment 3:
Thermocompression bonding applied to titanium alloy and PET connects, and first washes the grinding and polishing of titanium alloy sheet surface according to described in embodiment 1
Only, titanium alloy surface and using the alumina grits of 100~500 μm of particle diameters is impacted under 500~1000MPa air pressure, is held
It is 5~20 seconds continuous.Titanium alloy surface macro-asperity by sandblasting reaches 10~20 μm, there is stronger mechanical snap ability.It
Ultrasound is cleaned in deionized water afterwards.The hydrofluoric acid solution for configuring 5%~10% concentration impregnates titanium alloy plate 5~20 seconds.
After surface treatment, the connection of titanium alloy and PET is realized according to the hot pressing soldering method of embodiment 2.Postwelding titanium closes
Gold/PET connector shear tension intensity has reached 14MPa, and more not surface treated connector (4.5MPa) strength enhancing is more than
Twice.The visible a large amount of macromolecules of titanium alloy section part are remaining after extension test.This shows the microcosmic connection mechanism caused by acid etching
Except (Fig. 4), the macroscopic view sandblasting also improves titanium alloy/macromolecule to the promotion of titanium alloy surface macro-asperity is engaged,
To further improve strength of joint.
In the present embodiment, the joint face between titanium alloy and macromolecule is plane, but in other embodiments can be any
Curved surface.
Embodiment 4:
Applied to the friction spot welding connection between aluminium alloy and high density polyethylene (HDPE) (HDPE).It will be with a thickness of the conjunction of the aluminium of 3mm
Gold surface according to rub described in embodiment 1 throw clean after, aluminium alloy table is impregnated in ultrasonic wave using the dilute sulfuric acid of 10% concentration
Face 60 seconds.After surface treated, occurred using metallographic microscope substrate aluminum alloy surface visible with scanning electron microscope obvious
Coarse particles, particle main component be aluminium oxide.
It by the aluminium alloy and the placement of HDPE plate overlap joint after surface treatment and is fixed on the workbench of friction spot welding, using straight
The needleless that diameter is 10-15mm rotates tool in aluminium alloy upper surface with 1000-2000 revs/min of speed rotation and with 1mm/min
Speed slowly push, continue 30 seconds.During the connection process, the frictional heat generation of rotation tool and aluminium alloy upper surface is conducted to boundary
At face, make macromolecule melting and selective oxidation.Macromolecule surface generates polar group (carbonyl and carboxyl) after oxidation, metal surface
Preferable microcosmic occlusion and chemical bonding are formed by the contact under larger lower pressure.
Joints shear tensile strength after molding has reached 18MPa, close to the intensity (20MPa) of macromolecule base material.It stretches
Aluminum alloy surface afterwards has the trace of more macromolecule remnants.And fail to be formed with HDPE without the aluminium alloy of surface treatment
Effect connection (intensity is lower than 5MPa).The facilitation that visible surface handles butt joint intensity is huge.
In the present embodiment, the joint face between aluminium alloy and macromolecule is plane, but in other embodiments can be any
Curved surface.
Embodiment 5:
Applied to the friction spot welding connection between steel and fibre reinforced polyphenylene sulfide (CFR-PPS).It will be with a thickness of 2mm's
Steel surface according to rub described in embodiment 1 throw clean after, using the hydrofluoric acid of 10% concentration in ultrasonic wave and 60 DEG C of constant temperature baths
It impregnates steel surface 30 seconds.After surface treated, occurred using the visible substrate steel surface of scanning electron microscope some comparatively fine
Compound particle.It by the steel and the placement of CFR-PPS plate overlap joint after surface treatment and is fixed on the workbench of friction spot welding, makes
The wolfram steel needleless for being 10-15mm with diameter rotates tool in the upper surface of steel with 2000 revs/min of speed rotation and with 1mm/
The speed of min slowly pushes, and continues 60 seconds.During the connection process, the frictional heat generation of the upper surface of rotation tool and steel conduct to
Interface, when accumulate heat it is enough after, polyphenylene sulfide (PPS) matrix melting in CFR-PPS, under larger lower pressure with metal
Surface contacts to form microcosmic occlusion and chemical bonding.Meanwhile the fibre reinforced in macromolecule is mutually inserted into the coarse of metal surface
Structure further promotes the mechanical snap at interface.
Joints shear tensile strength after molding has reached 33MPa, compares not surface treated strength of joint (20MPa)
It is lifted beyond 60%.Steel surface after stretching has some macromolecule leftover traces.
In the present embodiment, the joint face between steel and macromolecule is plane, but in other embodiments can be arbitrary surface.
Five kinds of embodiments of the invention are described in detail above, list five kinds of different metal surface chemical treatment sides
Method, and detail its facilitation to metal/high-molecular jointing intensity.The present invention do not limit metal with it is high molecular
Type, the size of metal surface rough morphology, connection method and Joining Technology parameter etc., those skilled in the art can basis
The present invention makes many modifications and variation.Therefore, all those skilled in the art design according to the invention passes through
The technical solution that logic analysis, reasoning or experiment obtain, within the protection scope being defined in the patent claims.
Claims (10)
1. a kind of surface treatment method applied to metal/high-molecular connection, which is characterized in that clean metal surface grinding and polishing
Afterwards, metal surface is impregnated with corrosive liquids, its surface is made to form one layer of conversion zone, which includes metallic substrates and dispersion
Compound particle on the metallic substrate, during being connect with macromolecule, the melting macromolecule of mobility promotion under high temperature
After being contacted with metallic substrates, close microcosmic occlusion is formed with compound particle and is bonded, connect metal effectively with macromolecule.
2. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
The length and width range of the compound particle are 1 μm -20 μm, and the projected area of compound particle occupies the conversion zone
The 5% -40% of the gross area.
3. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
The altitude range of the prominent metal surface of compound particle is 0.1-10 μm.
4. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
The corrosive liquids is that can generate the liquid of corrosive effect, preferably acidic liquid, including hydrofluoric acid, nitre in metal surface
One or more of acid, hydrochloric acid, sulfuric acid, and hydrogen ion concentration is between 0.1mol/L -10mol/L in acid solution, i.e. acid solution
PH value between -1 and 1.
5. a kind of surface treatment method applied to metal/high-molecular connection according to claim 4, which is characterized in that
The acid solution is the hydrofluoric acid that concentration is 0.5mol/L -10mol/L.
6. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
According to different metal/high-molecular combinations and the selection of different acid solutions, the corrosive liquids impregnates the time of metal surface
Range is -20 minutes 5 seconds.
7. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
The mode that the corrosive liquids impregnates metal is impregnated in ultrasonic wave, and the power of ultrasonic wave is 10W -200W.
8. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
The metal surface grinding and polishing is cleaned first be roughened after, then be immersed in acid solution, roughening treatment method includes spray
Sand, 3 D-printing or marking.
9. a kind of surface treatment method applied to metal/high-molecular connection according to claim 8, which is characterized in that
The roughening treatment method is preferably blasting treatment, and sandblasting rear surface roughness reaches 0.5 μm -100 μm.
10. a kind of surface treatment method applied to metal/high-molecular connection according to claim 1, which is characterized in that
Metal and macromolecule connection method after surface treatment include friction welding (FW), thermocompression bonding, Laser Welding or supersonic welding.
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