CN104439956B - Method for connecting materials difficult to connect through ultrafast lasers - Google Patents
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- CN104439956B CN104439956B CN201410658225.6A CN201410658225A CN104439956B CN 104439956 B CN104439956 B CN 104439956B CN 201410658225 A CN201410658225 A CN 201410658225A CN 104439956 B CN104439956 B CN 104439956B
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Abstract
The invention discloses a method for connecting materials difficult to connect through ultrafast lasers. The method includes the following steps that firstly, a material A is ablated through ultrashort pulse lasers, removing is achieved through laser ablation, and a nano-micro-meter structure is obtained on the surface of the material A; secondly, impurities on the surface, with the nano-micro-meter structure, of the material A are removed through corrosive liquid; thirdly, in an inert gas or vacuum environment, a material B is deformed and flows to fill the nano-micro-meter structure of the material A, the material A and the material B are combined in a mechanical combination mode, and therefore the material A and the material B are connected, wherein the melting point and the hardness of the material A are higher than the melting point and the hardness of the material B. The method for connecting the materials difficult to connect through the ultrafast lasers is a new method which is flexible, high in efficiency and wide in application range and is used for improving the connecting strength of the materials, and the application of the method includes but is not limited to the development of a nuclear fusion reactor oriented to plasma materials, electric contact materials, heat sink materials, electronic packaging and advanced composite materials.
Description
Technical field
The present invention relates to a kind of utilization ultrafast laser realizes the method connected between difficult connecting material, belong to material connection neck
Domain.
Background technology
Surface micronano structure is by specific processing method, in material surface preparation with micron, nanometer or micro-
The regular texture of nano combined yardstick, common version has striped, projection (hemispherical, taper, bar-shaped) and pit etc., with
And the complex form of said structure.Surface micronano structure has super-hydrophobic, super viscid, anti-light reflection, selective light absorption etc.
Characteristic, all has broad application prospects in every field such as industry, military, Aeronautics and Astronautics and medical treatment.Conventional surface micronano
Structure preparation method has CVD, sol-gel process, masterplate method, self-assembly method, Electrospinning Method, laser ablation method etc..
Ultrafast laser has high peak energy denisty, extremely short pulse width, the heat affecting very little with material effects,
High accuracy materials processing can be realized, the almost all of material such as high-melting-point, high rigidity can be processed, be a kind of high-energy-density, height
The advanced manufacturing process of precision.Ultrafast laser can prepare functionalization micron, nanoscale structures in material surface, for example, swash
Light ablation prepares imitative " Folium Nelumbinis " surface texture in metal surface, possesses superhydrophobic characteristic；It is micro-nano that laser ablation prepares metal surface
Structure, possesses antireflective properties and ultra-wide spectrum band absorption characteristic etc..
The connection of material is a kind of widely used materials processing technology, including riveting, welding, be glued etc. technique.With riveting
Connect and compared with adhesive technology, welding procedure has the advantages such as bonding strength height, the good, material-saving of joint tighness, extensively application
In the connection of various materials.But for solid solubility very little under room temperature, do not form the foreign material of compound, such as W/Cu, Mo/ yet
Cu, ceramics/Al, due to being hardly formed metallurgical binding between bi-material, the connection of such material is very difficult, bonding strength pole
It is low.In view of such foreign material connector some special occasions application (as W/Cu connectors it is anti-as thermonuclear fusion
Answer facing plasma material in heap), the bonding strength for improving such difficult connecting material has important Research Significance and application
Value.
The content of the invention
It is an object of the invention to provide a kind of utilization ultrafast laser realizes the method connected between difficult connecting material, the present invention
Using a kind of material of ultrafast pulsed laser ablation, micro nano structure is prepared on its surface, is then attached with another kind of material,
Realize the bonding strength between two kinds of difficult connecting materials.
Utilization ultrafast laser provided by the present invention realizes the method connected between difficult connecting material, comprises the steps：
(1) mechanism of ultrashort-pulse laser ablation materials A is used, portion of material is removed through laser ablation, on the surface of the materials A
Obtain micro nano structure；
(2) impurity on the surface with the micro nano structure of the materials A is removed with corrosive liquid；
(3) in inert atmosphere or vacuum environment, material B is made to deform and then occur and the filling materials A that flows
The micro nano structure, the materials A is combined with the material B by way of mechanical bond, that is, realize
Connection between bi-material；
The fusing point and hardness of the materials A is above the material B.
In above-mentioned method, the materials A can be any one in tungsten, molybdenum, chromium, rhenium, high-speed steel and ceramics；
The material B can be any one in copper, aluminum, gold, silver and plastics.
In above-mentioned method, in step (1), the ultra-short pulse laser can be nanosecond laser, picosecond laser and/or femtosecond
Laser；
The ultra-short pulse laser is visible ray (such as 532nm) or infrared light (such as 1030nm or 1064nm), light beam energy
Amount is distributed as Gaussian mode or other distributions.
In above-mentioned method, the pulse width of the nanosecond laser can be 10 nanoseconds, repetition rate can for 1kHz～
30kHz, mean power can be 1W～20W；
The pulse width of the picosecond laser can be 15 psecs, and repetition rate can be 100kHz～2MHz, and mean power can
For 5W～100W；
The pulse width of the femtosecond laser can be 800 femtoseconds, and repetition rate can be 200kHz～800kHz, such as 400kHz
～800kHz, 400kHz or 800kHz, mean power is 2W～40W, such as 2W～20W, 2W or 20W.
In above-mentioned method, the micro nano structure is parallel groove, array of protrusions or pit array；Wherein described projection
Array includes hemispherical array, taper array or bar array etc.；
The size of the micrometer structure in the micro nano structure is 30～300 μm, such as 30 μm or 200 μm；
The size of the nanostructured in the micro nano structure is 200～600nm, and the W rods surface that such as prepared by embodiment 1 is micro-
Micron protrusion surface in nanostructured is dispersed with abundant micron/submicron striped and nano-particle, its stereoscan photograph
As shown in Fig. 2 the pit surface in the W rod surface micronano structures of the preparation of embodiment 2 is dispersed with abundant micron/submicron bar
Stricture of vagina and nano-particle, its stereoscan photograph is as shown in Figure 4.
In above-mentioned method, in step (2), the preparation of the micro nano structure is realized using scanning galvanometer, so may be used
Needed to prepare the micrometer structure of given shape according to the mechanical property of connector, and go out abundant nano junction in its spatial induction
Structure.
In above-mentioned method, in step (2), the corrosive liquid is that dilute hydrochloric acid, dust technology, ammonia spirit or dioxygen are water-soluble
Liquid.
In above-mentioned method, in step (3), the mode of the mechanical bond is hot pressing, die casting, thermal spraying, plating or electricity
Welding resistance etc.；The inventive method is to make the material B (the relatively low material of fusing point) have good modeling by techniques such as heating, pressurizations
Property and mobility, fully deformation, flow to fill the space in the micro nano structure, so as to form good mechanical bond with
Obtain high material bonding strength.
In above-mentioned method, before step (1), methods described also includes the surface to the materials A and the material B
The step of being processed, is finally cleaned by ultrasonic with ethanol, acetone and other organic solvent, is finally dried up with high pressure draught or is dried
It is dry；
The step of process, is described including carrying out successively the step of removing the removal of impurity (oxide, greasy dirt etc.) and grinding and polishing
The step of going the removal of impurity includes machining (turning, grinding etc.) or chemical attack.
" laser ablation removal portion of material " in the preparation method that the present invention is provided is referred to when pulsed laser energy density
More than certain material ablation threshold when, there is Evaporation Phenomenon in material surface in laser action area, forms the removal of material, removes
Amount depends on laser parameter；The ablation threshold of material is relevant with material behavior and Pulsed Laser Parameters such as pulse width etc., such as exists
Under 70 Femtosecond-Laser Pulse Excitations, the ablation threshold of the metal such as Cu, Al, Fe, Ni and Mo is respectively 0.25,0.25,0.28,0.20 and
0.40J/cm2；Under the effect of 10 picosecond lasers, the ablation threshold of H13 hot die steels is 0.9J/cm2, and the ablation of high-speed steel
Threshold value is 1.02J/cm2。
The present invention has the advantage that due to taking above technical scheme：
(1) present invention prepares surface micronano structure using mechanism of ultrashort-pulse laser ablation material；Ultra-short pulse laser has
The characteristics of pulse width, big power density.Pulse width can shorten the action time of laser pulse and material, reduce the total energy of input
Amount, suppresses heat accumulation, reduces the fusing of the material of adjacent area, substantially eliminates heat affected area, improves machining accuracy, reaches approximate
In the effect of " cold working "；It is unmanageable that power density is processed to greatly the traditional methods such as various high-melting-points, high rigidity
Material, and working (machining) efficiency is improved, it is a kind of high accuracy, high efficiency, surface micronano structure preparation method applied widely.
(2) present invention prepares surface micronano structure using mechanism of ultrashort-pulse laser ablation material, and the repetition rate of laser is very
Height, be several KHz to several megahertzs, can induce that form is abundant, highdensity nanostructured in metal material surface, greatly
Ground improves the specific surface area of material, and then improves the bonding strength of material.
(3) present invention prepares surface micronano structure using mechanism of ultrashort-pulse laser ablation material, coordinates scanning galvanometer, can root
Need to prepare the micrometer structure of given shape according to the mechanical property of connector, and go out abundant nanostructured in its spatial induction,
It is a kind of flexible, flexible method of attachment.
(4) present invention prepares surface micronano structure using mechanism of ultrashort-pulse laser ablation material, then by another kind of material
It is attached thereto, does not require to form metallurgical binding between bi-material, nesting, the mechanical snap for only being formed by bi-material surface is just
The connection of two kinds of metal materials can be realized, is a kind of generally applicable method of attachment.
(5) present invention prepares the bonding strength of material surface micro nano structure reinforcing material using ultra-short pulse laser, can
For strengthening the bonding strength of multiple material method of attachment, including hot pressing, die casting, flame-spraying, plasma spraying, supersonic speed spray
Painting, plating, electric resistance welding etc., are a kind of generally applicable methods of attachment.
In sum, the invention provides it is a kind of flexibly, high efficiency, reinforcing material bonding strength applied widely it is new
Method.Application including but not limited to fusion reactor facing plasma material, contact material, the heat sink material of the present invention
The exploitation of material, Electronic Packaging and advanced composite material (ACM).
Description of the drawings
Fig. 1 is the schematic diagram of the method that the present invention realizes connecting between difficult connecting material using ultrafast laser.
Fig. 2 is nanostructured (Fig. 2 of W surface array of protrusions (Fig. 2 (a)) prepared by the embodiment of the present invention 1 and protrusion surface
(b))。
Fig. 3 is the interface topography that the present invention implements W/Cu connectors prepared by example 1.
Fig. 4 is that the present invention implements the pit array (Fig. 4 (a)) of the preparation of example 2 and nanostructured (Fig. 4 of pit surface
(b))。
Specific embodiment
Experimental technique used in following embodiments if no special instructions, is conventional method.
Material used, reagent etc. in following embodiments, if no special instructions, commercially obtain.
The ultimate principle of the method that the present invention realizes connecting between difficult connecting material using ultrafast laser is using ultrashort arteries and veins
The high-energy ablator of impulse light, by the scanning pattern for controlling focal beam spot, the fusing point and hard in two kinds of materials to be connected
The higher material surface of degree prepares micro nano structure；Then the relatively low material of wherein fusing point is connected to into micro nano structure
Material surface, by technological measures such as heating, pressurizations, by the deformation of lower melting temperature materials, flows to fill the higher material of fusing point
The space of material surface micronano structure, forms mechanical snap structure mutually nested between bi-material, and promotes bi-material
Between atoms permeating, to strengthen the bonding strength between bi-material.
The present invention is described in detail below in conjunction with accompanying drawing and enforcement example, it is pointed out that implement example and only use
In helping illustrate and understand the present invention, the scope of application of the present invention is not limited to following example.
Embodiment 1, fs laser prepare W surface micron array of protrusions strengthens W/Cu bonding strengths
The present embodiment is strong using the connection that fs laser preparation W surface micron array of protrusions strengthens W/Cu hot pressing connects parts
Degree, schematic flow sheet is as shown in figure 1, comprise the following steps that：
(1) method being machined into first removes the oxide of W plane rod ends, with chemical attack (caustic：Volume fraction
Dilute hydrochloric acid for 5%) mode remove the oxide of Cu plane rod ends, then grinding and polishing is carried out to W rods and Cu plane rod ends with polished machine,
Then W rods and Cu rods are cleaned by ultrasonic with ethanol, are finally dried up with elevated pressure nitrogen air-flow.Wherein the size of W rods is Φ 10mm
The size of × 5mm, Cu rod is Φ 10mm × 30mm.
(2) W plane rod end micro nano structures are prepared with fs laser instrument：Average laser power is 20W, and pulse frequency is
800kHz, pulsewidth is 800fs, and single pulse energy is 25 μ J, and focal beam spot is a diameter of 30 μm；Focal beam spot is controlled with scanning array mirror
Scanning pattern, scanning speed is 1500mm/s, and scanning pattern is the cross modal in horizontal, vertical direction, and distance between centers of tracks is 300 μm, line
It is wide about 100 μm, repeat 50 times.
The W rod surface micronano structures for preparing are the square protrusions array of 200 μm of 200 μ m, the μ of spacing about 100
M, about 100 μm of height；Micron protrusion surface is dispersed with abundant micron/submicron striped and nano-particle, and its scanning electron microscope shines
Piece is as shown in Figure 2.
(3) with corrosive liquid (NH4·OH:H2O2:H2O=1:4:5, volume ratio) immersion W rod about 1min, remove W plane rod ends
Oxide, is then cleaned by ultrasonic with ethanol to W rods, is finally dried up with elevated pressure nitrogen air-flow.
(4) hot pressing connects are carried out to W rods and Cu rods with protective atmosphere hot pressing furnace, temperature is 1000 DEG C, and pressure is 80MPa,
Pressurize 2h, high-purity helium protection, furnace cooling realizes the connection between W rods and Cu rods, obtains W rods/Cu rod connectors.
The linkage interface pattern (optical microscope photograph) of W/Cu connectors manufactured in the present embodiment is as shown in figure 3, by this
Figure understands that Cu fully deforms, is filled with the micro nano structure on W rods surface, and W rods/Cu rod clean interfaces, without impurity, are defined
Good connection.
The enhanced W rods of surface micronano structure manufactured in the present embodiment/Cu rod connectors are lathed into the pole of Φ 9mm,
The tensile strength of the W rods/Cu rod connectors (pole) is measured using material mechanical performance testing machine：Pole is clamped in and is pressed from both sides up and down
Between, loading velocity is 0.5mm/min, and the elongation of continuous record load and pole is removed until pole fracture with breaking load
With the tensile load that the cross-sectional area of pole obtains connector.Measurement result is as follows：
Contrast connector：It is prepared according to the method essentially identical with the present embodiment, difference is：Not included in
The step of W rods surface prepares micro nano structure.
W rods/Cu rod connector tensile strength prepared by this enforcement has reached about 40MPa；
The tensile strength of contrast connector is only for about 20MPa；
From the contrast test, the inventive method enhances the bonding strength between difficult connecting material, is enhanced to about 2
Times.
Embodiment 2, fs laser prepare W surface micron pit array strengthens W/Cu bonding strengths
The present embodiment is strong using the connection that fs laser preparation W surface micron pit array strengthens W/Cu hot pressing connects parts
Degree, schematic flow sheet is as shown in figure 1, comprise the following steps that：
(1) method being machined into first removes the oxide of W plane rod ends, with chemical attack (caustic：Volume fraction
Dilute hydrochloric acid for 5%) mode remove the oxide of Cu plane rod ends, then grinding and polishing is carried out to W rods and Cu plane rod ends with polished machine,
Then W rods and Cu rods are cleaned by ultrasonic with ethanol, are finally dried up with elevated pressure nitrogen air-flow.Wherein the size of W rods is Φ 10mm
The size of × 5mm, Cu rod is Φ 10mm × 30mm.
(2) W plane rod end micro nano structures are prepared with fs laser instrument：Average laser power is 2W, and pulse frequency is 400kHz,
Pulsewidth is 800fs, and single pulse energy is 5 μ J, and focal beam spot is a diameter of 30 μm；The scanning road of focal beam spot is controlled with scanning galvanometer
Footpath, scanning pattern is equilateral triangle dot matrix, and dot spacing is 30 μm, and each point dotting time is 0.4ms, is repeated 20 times.
The W rods surface micronano structure for preparing for 30 μm of dot spacing equilateral triangle dot matrix, 30 μm of dot spacing；Pit
Surface distributed abundant micron/submicron striped and nano-particle, and its stereoscan photograph is as shown in Figure 4.
(3) with corrosive liquid (NH4·OH:H2O2:H2O=1:4:5, volume ratio) immersion W rod about 1min, remove W plane rod ends
Oxide, is then cleaned by ultrasonic with ethanol to W rods, is finally dried up with elevated pressure nitrogen air-flow.
(4) hot pressing connects are carried out to W rods and Cu rods with protective atmosphere hot pressing furnace, temperature is 1050 DEG C, and pressure is 80MPa,
Pressurize 1.5h, high-purity helium protection, furnace cooling realizes the connection between W rods and Cu rods, obtains W rods/Cu rod connectors.
The enhanced W rods of surface micronano structure manufactured in the present embodiment/Cu rod connectors are lathed into the pole of Φ 9mm,
The tensile strength (during method of testing is with embodiment 1) of the W rods/Cu rod connectors is measured using material mechanical performance testing machine, is surveyed
Amount result is as follows：
Contrast connector：It is prepared according to the method essentially identical with the present embodiment, difference is：Not included in
The step of W rods surface prepares micro nano structure.
W rods manufactured in the present embodiment/Cu rod connector tensile strength has reached about 60MPa；
The tensile strength of contrast connector is only for about 20MPa；
From the contrast test, the inventive method enhances the bonding strength between difficult connecting material, is enhanced to about 3
Times.
In sum, the present invention prepares material surface micro nano structure using ultra-short pulse laser, with high efficiency, high-precision
The advantages of degree, micro nano structure pattern enrich, can process the material of high-melting-point, high rigidity；The present invention can be used to strengthen various materials
The bonding strength of material method of attachment (hot pressing, die casting, spraying, plating, electric resistance welding etc.), is a kind of flexible, flexible, generally applicable
Method.
Claims (4)
1. a kind of utilization ultrafast laser realizes the method connected between difficult connecting material, comprises the steps：
(1) mechanism of ultrashort-pulse laser ablation materials A is used, is removed through laser ablation, on the surface of the materials A micro-nano knot is obtained
Structure；
The preparation of the micro nano structure is realized using scanning galvanometer；
The materials A is any one in tungsten, molybdenum, chromium, rhenium, high-speed steel and ceramics；
The ultra-short pulse laser is nanosecond laser, picosecond laser or femtosecond laser；
The ultra-short pulse laser is visible or infrared light；
The pulse width of the nanosecond laser was 10 nanoseconds, and repetition rate is 1kHz～30kHz, and mean power is 1W～20W；
The pulse width of the picosecond laser is 15 psecs, and repetition rate is 100kHz～2MHz, and mean power is 5W～100W；
The pulse width of the femtosecond laser be 800 femtoseconds, repetition rate be 200kHz～800kHz, mean power be 2W～
40W；
The micro nano structure is parallel groove, array of protrusions or pit array；
The size of the micrometer structure in the micro nano structure is 30～300 μm；
The size of the nanostructured in the micro nano structure is 200～600nm；
(2) impurity on the surface with the micro nano structure of the materials A is removed with corrosive liquid；
(3) in inert atmosphere or vacuum environment, make material B deform and then flow to fill the micro-nano of the materials A
Rice structure, the materials A is combined with the material B by way of mechanical bond, that is, realize bi-material it
Between connection；
The material B is any one in copper, aluminum, gold, silver and plastics；
The fusing point and hardness of the materials A is above the material B.
2. method according to claim 1, it is characterised in that：In step (2), the corrosive liquid be dilute hydrochloric acid, dust technology,
Ammonia spirit or hydrogen peroxide solution.
3. method according to claim 1 and 2, it is characterised in that：In step (3), the mode of the mechanical bond is heat
Pressure, die casting, thermal spraying, plating or electric resistance welding.
4. method according to claim 3, it is characterised in that：Before step (1), methods described is also included to the material
The step of surface of the material A and material B is processed；
The step of process, is described to include machine the step of go the removal of impurity including carrying out successively the step of going the removal of impurity and grinding and polishing
Tool is processed or chemical attack.
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| TWI637805B (en) * | 2016-10-25 | 2018-10-11 | 財團法人工業技術研究院 | Laser processing system and method for metallic surface |
| CN107069070A (en) * | 2017-04-14 | 2017-08-18 | 重庆创元新能源科技有限责任公司 | A kind of nanosecond laser is welded on the application process in soft package lithium battery |
| CN107511586A (en) * | 2017-10-09 | 2017-12-26 | 有研亿金新材料有限公司 | A kind of method of laser assisted welding target and backboard |
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| CN110640307B (en) * | 2019-09-18 | 2020-12-01 | 清华大学 | Functional ceramic welding device based on time domain shaping femtosecond laser |
| CN111574238A (en) * | 2020-04-29 | 2020-08-25 | 南京理工大学 | Ultrafast laser welding method applied to ceramics |
| CN112894143B (en) * | 2021-01-25 | 2022-06-24 | 北京理工大学 | Method for regulating and controlling surface wettability of stainless steel based on femtosecond laser direct writing scanning |
| CN113996942A (en) * | 2021-05-18 | 2022-02-01 | 中国人民解放军陆军装甲兵学院 | Method for fine processing surgical instruments |
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| CN101012052A (en) * | 2007-01-30 | 2007-08-08 | 中山大学 | Micro and nano structure assembling method welded by energy beam |
| CN101736214B (en) * | 2010-01-08 | 2012-07-25 | 清华大学 | Light metal surface laser impact micronano particle injection reinforcing method |
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