CN104439956A - Method for connecting materials difficult to connect through ultrafast lasers - Google Patents
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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 ultrafast laser that utilizes and realize the method connected between difficult connecting material, belong to material connection area.
Background technology
Surface micronano structure is by specific processing method, at the regular texture with micron, nanometer or micro-nano compound yardstick prepared by material surface, common version has striped, projection (hemispherical, taper, bar-shaped) and pit etc., and the complex form of said structure.Surface micronano structure has the characteristics such as super-hydrophobic, super viscid, anti-light reflection, selective light absorption, all has broad application prospects in every field such as industry, military affairs, 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, very little with the heat affecting of material effects, can realize high accuracy materials processing, can process the material that high-melting-point, high rigidity etc. are nearly all, be a kind of high-energy-density, high-precision advanced manufacturing process.Ultrafast laser can prepare functionalization micron, nanoscale structures at material surface, and such as, laser ablation prepares imitative " lotus leaf " surface texture in metal surface, possesses superhydrophobic characteristic; Laser ablation prepares metal surface micro-nanostructure, possesses antireflective properties and ultra-wide bands of a spectrum absorption characteristic etc.
The connection of material is a kind of widely used materials processing technology, comprises the techniques such as riveted joint, welding, splicing.Compare with adhesive technology with riveted joint, welding procedure has the advantages such as bonding strength is high, joint tighness good, saving material, is widely used in the connection of various material.But very little for solid solubility under normal temperature, also do not form the foreign material of compound, as W/Cu, Mo/Cu, pottery/Al, owing to being difficult between bi-material form metallurgical binding, the connection of this type of material is very difficult, and bonding strength is extremely low.Consider the connector of this type of foreign material some special occasions application (as W/Cu connector as thermonuclear fusion reactor in facing plasma material), the bonding strength improving this type of difficult connecting material has important Research Significance and using value.
Summary of the invention
The object of this invention is to provide a kind of ultrafast laser that utilizes and realize the method connected between difficult connecting material, the present invention utilizes a kind of material of ultrafast pulsed laser ablation, micro nano structure is prepared on its surface, then be connected with another kind of material, achieve the bonding strength between two kinds of difficult connecting materials.
The ultrafast laser that utilizes provided by the present invention realizes the method connected between difficult connecting material, comprises the steps:
(1) use mechanism of ultrashort-pulse laser ablation materials A, remove portion of material through laser ablation, obtain micro nano structure on the surface of described materials A;
(2) impurity on the surface with described micro nano structure of described materials A is removed with corrosive liquid;
(3) in inert atmosphere or vacuum environment, material B is deformed and then occurs and flow to fill the described micro nano structure of described materials A, then by the mode of mechanical bond, described materials A and described material B are combined, namely realize the connection between bi-material;
The fusing point of described materials A and hardness are all higher than described material B.
In above-mentioned method, described materials A can be any one in tungsten, molybdenum, chromium, rhenium, high-speed steel and pottery;
Described material B can be any one in copper, aluminium, gold, silver and plastics.
In above-mentioned method, in step (1), described ultra-short pulse laser can be nanosecond laser, picosecond laser and/or femtosecond laser;
Described ultra-short pulse laser is visible ray (as 532nm) or infrared light (as 1030nm or 1064nm etc.), and beam energy is distributed as Gaussian mode or other distributions.
In above-mentioned method, the pulse width of described nanosecond laser can be for 10 nanoseconds, and repetition rate can be 1kHz ~ 30kHz, and mean power can be 1W ~ 20W;
The pulse width of described picosecond laser can be 15 psecs, and repetition rate can be 100kHz ~ 2MHz, and mean power can be 5W ~ 100W;
The pulse width of described femtosecond laser can be 800 femtoseconds, and repetition rate can be 200kHz ~ 800kHz, and as 400kHz ~ 800kHz, 400kHz or 800kHz, mean power is 2W ~ 40W, as 2W ~ 20W, 2W or 20W.
In above-mentioned method, described micro nano structure is parallel groove, array of protrusions or pit array; Wherein said array of protrusions comprises hemispherical array, taper array or bar array etc.;
Micrometer structure in described micro nano structure is of a size of 30 ~ 300 μm, as 30 μm or 200 μm;
Nanostructured in described micro nano structure is of a size of 200 ~ 600nm, as the micron protrusion surface in W rod surface micronano structure prepared by embodiment 1 is dispersed with abundant micron/submicron striped and nano particle, its stereoscan photograph as shown in Figure 2, pit surface in W rod surface micronano structure prepared by embodiment 2 is dispersed with abundant micron/submicron striped and nano particle, and its stereoscan photograph as shown in Figure 5.
In above-mentioned method, in step (2), scanning galvanometer can be utilized to realize the preparation of described micro nano structure, can need according to the mechanical property of connector the micrometer structure preparing given shape like this, and go out abundant nanostructured at its spatial induction.
In above-mentioned method, in step (2), described corrosive liquid is watery hydrochloric acid, dust technology, ammonia spirit or hydrogen peroxide solution.
In above-mentioned method, in step (3), the mode that described tool combines is hot pressing, die casting, thermal spraying, plating or electric resistance welding etc.; The inventive method makes described material B (material that fusing point is lower) have good plasticity and mobility by techniques such as heating, pressurizations, abundant distortion, flow to fill the space in described micro nano structure, thus form good mechanical bond to obtain high material bonding strength.
In above-mentioned method, before step (1), described method also comprises the step processed the surface of described materials A and described material B, finally carries out ultrasonic cleaning by alcohol, acetone and other organic solvent, finally dries up with high pressure draught or dry;
The step of described process comprises step and the grinding and polishing of the removal impurity (oxide, greasy dirt etc.) carried out successively, described in go deimpurity step to comprise machining (turning, grinding etc.) or chemical attack.
" laser ablation removal portion of material " in preparation method provided by the invention refers to when pulsed laser energy density exceedes the ablation threshold of certain material, in laser action district there is Evaporation Phenomenon in material surface, form the removal of material, removal amount depends on laser parameter; The ablation threshold of material is as relevant in pulse width etc. with Pulsed Laser Parameters with material behavior, and as under 70 Femtosecond-Laser Pulse Excitations, the ablation threshold of the metals such as Cu, Al, Fe, Ni and Mo is respectively 0.25,0.25,0.28,0.20 and 0.40J/cm
2; Under 10 picosecond laser effects, the ablation threshold of H13 hot die steel is 0.9J/cm
2, and the ablation threshold of high-speed steel is 1.02J/cm
2.
The present invention is owing to taking above technical scheme, and tool has the following advantages:
(1) the present invention uses mechanism of ultrashort-pulse laser ablation material to prepare surface micronano structure; Ultra-short pulse laser has pulse width, feature that power density is large.Pulse width can shorten the action time of laser pulse and material, reduces the gross energy of input, suppresses heat accumulation, reduces the fusing of the material of adjacent area, substantially eliminates heat affected area, improves machining accuracy, reaches the effect being similar to " cold working "; Power density may be used for greatly processing the unmanageable materials of conventional method such as various high-melting-point, high rigidity, and improves working (machining) efficiency, is a kind of high accuracy, high efficiency, surface micronano structure preparation method applied widely.
(2) the present invention uses mechanism of ultrashort-pulse laser ablation material to prepare surface micronano structure, the repetition rate of laser is very high, for a few KHz is to a few megahertz, can induce at metal material surface that form is abundant, highdensity nanostructured, greatly improve the specific area of material, and then improve the bonding strength of material.
(3) the present invention uses mechanism of ultrashort-pulse laser ablation material to prepare surface micronano structure, coordinate scanning galvanometer, the micrometer structure preparing given shape can be needed according to the mechanical property of connector, and go out abundant nanostructured at its spatial induction, be a kind of flexibly, flexible method of attachment.
(4) the present invention uses mechanism of ultrashort-pulse laser ablation material to prepare surface micronano structure, then another kind of material is attached thereto, do not require to form metallurgical binding between bi-material, nested, mechanical snap by means of only the formation of bi-material surface just can realize the connection of two kinds of metal materials, are a kind of methods of attachment be extensively suitable for.
(5) the present invention uses ultra-short pulse laser to prepare the bonding strength of material surface micro nano structure reinforcing material, can be used for the bonding strength strengthening multiple material method of attachment, comprising hot pressing, die casting, flame-spraying, plasma spraying, supersonic spray coating, plating, electric resistance welding etc., is a kind of method of attachment be extensively suitable for.
In sum, the invention provides a kind of flexibly, the new method of high efficiency, reinforcing material bonding strength applied widely.Application of the present invention includes but not limited to the exploitation of fusion reactor facing plasma material, contact material, heat sink material, Electronic Packaging and advanced composite material (ACM).
Accompanying drawing explanation
Fig. 1 is that the present invention utilizes ultrafast laser to realize the schematic diagram of the method connected between difficult connecting material.
Fig. 2 is the W surface array of protrusions (Fig. 2 (a)) of the embodiment of the present invention 1 preparation and the nanostructured (Fig. 2 (b)) of protrusion surface.
Fig. 3 is W/Cu connector pictorial diagram prepared by the invention process example 1.
Fig. 4 is the interface topography of W/Cu connector prepared by the invention process example 1.
Fig. 5 is the pit array (Fig. 5 (a)) of the invention process example 2 preparation and the nanostructured (Fig. 5 (b)) of pit surface.
Detailed description of the invention
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
The general principle that the present invention utilizes ultrafast laser to realize the method connected between difficult connecting material is the high-energy ablator utilizing ultra-short pulse laser, by controlling the scanning pattern of focal beam spot, in two kinds of materials to be connected, fusing point and the higher material surface of hardness prepare micro nano structure; Then material lower for wherein fusing point is connected to the material surface of micro nano structure, by technological measures such as heating, pressurizations, by the distortion of lower melting temperature materials, flow the space of filling fusing point higher material surface micronano structure, form mechanical snap structure mutually nested between bi-material, and promote the atoms permeating between bi-material, to strengthen the bonding strength between bi-material.
Be described in detail the present invention below in conjunction with accompanying drawing and enforcement example, it is to be noted that implementing example only sets forth for helping and understand the present invention, the scope of application of the present invention is not limited to following example.
Embodiment 1, fs laser are prepared W surface micron array of protrusions and are strengthened W/Cu bonding strength
The present embodiment uses fs laser to prepare W surface micron array of protrusions to strengthen the bonding strength of W/Cu hot pressing connector, and as shown in Figure 1, concrete steps are as follows for schematic flow sheet:
(1) oxide of W plane rod end is first removed by the method for machining, the oxide of Cu plane rod end is removed by the mode of chemical attack (corrosive agent: volume fraction is the watery hydrochloric acid of 5%), then with polished machine, grinding and polishing is carried out to W rod and Cu plane rod end, then carry out ultrasonic cleaning with alcohol to W is excellent and Cu is excellent, finally dry up with elevated pressure nitrogen air-flow.Wherein W rod is of a size of Φ 10mm × 5mm, and Cu rod is of a size of Φ 10mm × 30mm.
(2) prepare W plane rod end micro nano structure with fs laser instrument: average laser power is 20W, pulse frequency is 800kHz, and pulsewidth is 800fs, and single pulse energy is 25 μ J, and focal beam spot diameter is 30 μm; Control the scanning pattern of focal beam spot with scanning battle array mirror, sweep speed is 1500mm/s, and scanning pattern is the cross modal in horizontal, vertical direction, and distance between centers of tracks is 300 μm, live width about 100 μm, repeats 50 times.
The W rod surface micronano structure prepared is the square protrusions array of 200 μm × 200 μm, spacing about 100 μm, highly about 100 μm; Micron protrusion surface is dispersed with abundant micron/submicron striped and nano particle, and its stereoscan photograph as shown in Figure 2.
(3) with corrosive liquid (NH
4oH:H
2o
2: H
2o=1:4:5, volume ratio) soak W rod about 1min, remove the oxide of W plane rod end, then with alcohol, ultrasonic cleaning is carried out to W rod, finally dry up with elevated pressure nitrogen air-flow.
(4) with protective atmosphere hot pressing furnace, W rod is carried out to hot pressing be connected with Cu is excellent, temperature is 1000 DEG C, and pressure is 80MPa, pressurize 2h, high-pure helium gas shielded, with stove cooling, namely realize W rod and Cu excellent between connection, obtain W rod/Cu rod connector.
The material object of W rod/Cu rod connector prepared by the present embodiment as shown in Figure 3.
The linkage interface pattern (optical microscope photograph) of W/Cu connector prepared by the present embodiment as shown in Figure 4, as known in the figure, Cu is fully out of shape, be filled with the micro nano structure on W rod surface, W rod/Cu rod clean interfaces, there is no impurity, define good connection.
The W rod that the surface micronano structure prepared by the present embodiment strengthens/Cu rod connector is lathed the pole of Φ 9mm, material mechanical performance testing machine is used to measure the tensile strength of this W rod/Cu rod connector (pole): to be clamped in by pole up and down between folder, loading velocity is 0.5mm/min, the elongation of continuous record load and pole, until pole fracture, obtains the tensile load of connector divided by the cross-sectional area of pole with breaking load.Measurement result is as follows:
Contrast connector: be prepared according to the method substantially identical with the present embodiment, difference is: the step preparing micro nano structure not included in W rod surface.
W rod/Cu rod connector the tensile strength of this enforcement preparation reaches about 40MPa;
The tensile strength of contrast connector is only about 20MPa;
From this contrast test, the inventive method enhances the bonding strength between difficult connecting material, is enhanced to about 2 times.
Embodiment 2, fs laser are prepared W surface micron pit array and are strengthened W/Cu bonding strength
The present embodiment uses fs laser to prepare W surface micron pit array to strengthen the bonding strength of W/Cu hot pressing connector, and as shown in Figure 1, concrete steps are as follows for schematic flow sheet:
(1) oxide of W plane rod end is first removed by the method for machining, the oxide of Cu plane rod end is removed by the mode of chemical attack (corrosive agent: volume fraction is the watery hydrochloric acid of 5%), then with polished machine, grinding and polishing is carried out to W rod and Cu plane rod end, then carry out ultrasonic cleaning with alcohol to W is excellent and Cu is excellent, finally dry up with elevated pressure nitrogen air-flow.Wherein W rod is of a size of Φ 10mm × 5mm, and Cu rod is of a size of Φ 10mm × 30mm.
(2) prepare W plane rod end micro nano structure with fs laser instrument: average laser power is 2W, pulse frequency is 400kHz, and pulsewidth is 800fs, and single pulse energy is 5 μ J, and focal beam spot diameter is 30 μm; Control the scanning pattern of focal beam spot with scanning galvanometer, scanning pattern is equilateral triangle dot matrix, and dot spacing is 30 μm, and each some dotting time is 0.4ms, repeats 20 times.
The W rod surface micronano structure prepared is the equilateral triangle dot matrix of dot spacing 30 μm, dot spacing 30 μm; Pit surface is dispersed with abundant micron/submicron striped and nano particle, and its stereoscan photograph as shown in Figure 5.
(3) with corrosive liquid (NH
4oH:H
2o
2: H
2o=1:4:5, volume ratio) soak W rod about 1min, remove the oxide of W plane rod end, then with alcohol, ultrasonic cleaning is carried out to W rod, finally dry up with elevated pressure nitrogen air-flow.
(4) with protective atmosphere hot pressing furnace, W rod is carried out to hot pressing be connected with Cu is excellent, temperature is 1050 DEG C, and pressure is 80MPa, pressurize 1.5h, high-pure helium gas shielded, with stove cooling, namely realize W rod and Cu excellent between connection, obtain W rod/Cu rod connector.
The W rod that the surface micronano structure prepared by the present embodiment strengthens/Cu rod connector is lathed the pole of Φ 9mm, use material mechanical performance testing machine to measure the tensile strength (method of testing is with in embodiment 1) of this W rod/Cu rod connector, measurement result is as follows:
Contrast connector: be prepared according to the method substantially identical with the present embodiment, difference is: the step preparing micro nano structure not included in W rod surface.
W rod/Cu rod connector tensile strength prepared by the present embodiment reaches about 60MPa;
The tensile strength of contrast connector is only about 20MPa;
From this contrast test, the inventive method enhances the bonding strength between difficult connecting material, is enhanced to about 3 times.
In sum, the present invention uses ultra-short pulse laser to prepare material surface micro nano structure, has high efficiency, high accuracy, micro nano structure pattern enrich, can process high-melting-point, the advantage such as the material of high rigidity; The present invention can be used for the bonding strength strengthening various material joining methods (hot pressing, die casting, spraying, plating, electric resistance welding etc.), is a kind of method that is flexible, flexible, that be extensively suitable for.
Claims (10)
1. utilize ultrafast laser to realize the method connected between difficult connecting material, comprise the steps:
(1) use mechanism of ultrashort-pulse laser ablation materials A, remove through laser ablation, obtain micro nano structure on the surface of described materials A;
(2) impurity on the surface with described micro nano structure of described materials A is removed with corrosive liquid;
(3) in inert atmosphere or vacuum environment, material B is deformed and then occurs and flow to fill the described micro nano structure of described materials A, then by the mode of mechanical bond, described materials A and described material B are combined, namely realize the connection between bi-material;
The fusing point of described materials A and hardness are all higher than described material B.
2. method according to claim 1, is characterized in that: described materials A is any one in tungsten, molybdenum, chromium, rhenium, high-speed steel and pottery;
Described material B is any one in copper, aluminium, gold, silver and plastics.
3. method according to claim 1 and 2, is characterized in that: in step (1), and described ultra-short pulse laser is nanosecond laser, picosecond laser and/or femtosecond laser;
Described ultra-short pulse laser is visible or infrared light.
4. method according to claim 3, is characterized in that: the pulse width of described nanosecond laser was 10 nanoseconds, and repetition rate is 1kHz ~ 30kHz, and mean power is 1W ~ 20W;
The pulse width of described picosecond laser is 15 psecs, and repetition rate is 100kHz ~ 2MHz, and mean power is 5W ~ 100W;
The pulse width of described femtosecond laser is 800 femtoseconds, and repetition rate is 200kHz ~ 800kHz, and mean power is 2W ~ 40W.
5. the method according to any one of claim 1-4, is characterized in that: described micro nano structure is parallel groove, array of protrusions or pit array;
Micrometer structure in described micro nano structure is of a size of 30 ~ 300 μm;
Nanostructured in described micro nano structure is of a size of 200 ~ 600nm.
6. the method according to any one of claim 1-5, is characterized in that: in step (1), utilizes scanning galvanometer to realize the preparation of described micro nano structure.
7. the method according to any one of claim 1-6, is characterized in that: in step (2), and described corrosive liquid is watery hydrochloric acid, dust technology, ammonia spirit or hydrogen peroxide solution.
8. the method according to any one of claim 1-7, is characterized in that: in step (3), and the mode that described tool combines is hot pressing, die casting, thermal spraying, plating or electric resistance welding.
9. the method according to any one of claim 1-8, is characterized in that: before step (1), and described method also comprises the step processed the surface of described materials A and described material B;
The step of described process comprise carry out successively go deimpurity step and grinding and polishing, described in go deimpurity step to comprise machining or chemical attack.
10. ultrafast pulsed laser is improving the application between difficult connecting material in bonding strength.
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| WO2022242270A1 (en) * | 2021-05-18 | 2022-11-24 | 中国人民解放军陆军装甲兵学院 | Method for fine machining of surgical instrument |
| CN114260576A (en) * | 2021-12-31 | 2022-04-01 | 东北电力大学 | Ultrasonic-assisted hollow tungsten electrode GTA-laser coaxial hybrid welding system |
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