CN110369911A - A kind of copper nano-weld material and preparation method thereof - Google Patents
A kind of copper nano-weld material and preparation method thereof Download PDFInfo
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- CN110369911A CN110369911A CN201910569800.8A CN201910569800A CN110369911A CN 110369911 A CN110369911 A CN 110369911A CN 201910569800 A CN201910569800 A CN 201910569800A CN 110369911 A CN110369911 A CN 110369911A
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- nano particles
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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
- 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
- B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
- B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
-
- 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
- B23K35/40—Making wire or rods for soldering or welding
Abstract
The present invention relates to technical field of welding materials, more particularly, to a kind of copper nano-weld material and preparation method thereof.A kind of preparation method of copper nano-weld material includes the following steps: to mix copper nano particles into ultrasonic treatment with liquid organic acid, collects the copper nano particles after being ultrasonically treated, clean and remove liquid organic acid, dry.Under ultrasonication, copper organic acid clad that can be very thin in copper nano particles Surface Creation can be improved the inoxidizability of copper nano particles while avoiding nanoparticle agglomerates for copper nano particles and liquid organic acid of the present invention, improve electric conductivity；Also, the very thin copper organic acid clad generated will not influence subsequent welding process, and the high copper nano-weld material of the high welding efficiency of thermal conductivity height, conductivity can be prepared.
Description
Technical field
The present invention relates to technical field of welding materials, more particularly, to a kind of copper nano-weld material and preparation method thereof.
Background technique
Microelectronics Packaging copper-copper interconnection technology is current research hotspot, but copper-copper interconnection structure technology faces many skills
The problem of art, with the development of nanotechnology, Lockheed Martin's space system company aerospace system advanced technology center (ATC)
Advanced material and nanotechnology department developed a kind of revolutionary Nanometer Copper medium interconnection material in 2012.This dielectric material
The rule recognized extensively based on oneself: when metallic particles partial size is reduced to nanoscale, since specific surface area is significantly greatly increased, fusing point
It greatly reduces, blocky pure metal will be substantially less than.The pressure sintering nano particle experiment of Brien et al. is also used for for nano particle
Welding technique has established feasibility basis.The feasibility of stable sintering structure is formed by copper nano particles prepared by chemical method
Then it is verified by Kobayashi et al..There is document to point out when package temperature reaches a certain temperature, nanometer copper particle can be with
It is sintered, to realize copper-copper interconnection structure.Experiment shows copper-copper interconnection structure conductivity and thermal conductivity than tradition
Tin-based material improve 10 times or so, show that Nanometer Copper is a kind of novel welding material.But copper nano particles are being stored
It is easy to be oxidized in the process, is formed on its surface the oxide skin(coating) of copper, these oxide layers seriously hinder copper nano particles
Thermally conductive, conductive, switching performance.
In the prior art, have and Nanometer Copper and resin carrier etc. are mixed with Nanometer Copper welding material, while being added organic
Acid, reduces the oxidation of Nanometer Copper, but this method is likely to result in nano copper particle reunion, and obtained welding material be containing
The mixing material of resin carrier, organic acid and Nanometer Copper etc., nanometer copper content is low, and welding efficiency is low.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of preparation method of copper nano-weld material, to solve in the prior art
The Nanometer Copper reunion technical problem low with nanometer copper content in existing welding material.
The second object of the present invention is to provide a kind of copper nano-weld material, and in the welding material, copper content is high, welding
It is high-efficient, while copper nano particles are uniformly dispersed.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of preparation method of copper nano-weld material, includes the following steps:
Copper nano particles are mixed into ultrasonic treatment with liquid organic acid, the copper nano particles after collecting ultrasonic treatment, cleaning
Liquid organic acid is removed, it is dry.
The aerial surface oxidation of copper nano particles itself is inevitable, more or less all can be in copper nano particles
There are copper oxide, copper nano particles and liquid organic acid of the present invention, can be raw on copper nano particles surface under ultrasonication on surface
At very thin copper organic acid clad, while avoiding nanoparticle agglomerates, the inoxidizability of copper nano particles can be improved,
It avoids being further oxided, improves electric conductivity；Also, the very thin copper organic acid clad generated will not influence subsequent welding
Process.
Meanwhile ultrasonic treatment can make copper nano particles further be uniformly dispersed, so that each copper nano particles surface is equal
Uniform copper organic acid clad can be formed.
Preferably, the liquid organic acid includes formic acid, acetic acid and any one or more of mixing of propionic acid.More preferably
, the liquid organic acid includes any one of formic acid and acetic acid or two kinds of mixing.It is further preferred that the liquid is organic
Acid is formic acid.
After formic acid and copper nano particles ultrasonic treatment, formic acid can be reacted with the copper oxide on copper nano particles surface generates formic acid
Layers of copper.
After acetic acid and copper nano particles ultrasonic treatment, acetic acid can be reacted with the copper oxide on copper nano particles surface generates acetic acid
Layers of copper.
Formic acid layers of copper and/or acetic acid layers of copper are coated on the surface of copper nano particles, have both avoided the reunion of copper nano particles,
The oxidation of copper nano particles is also avoided, inoxidizability and welding efficiency and switching performance are improved.
Meanwhile the content of copper in welding material can be further increased using formic acid, further increase welding efficiency.
Preferably, the mass ratio of the copper nano particles and liquid organic acid is 1 ﹕ (8-10).
As in different embodiments, by taking formic acid as an example, the mass ratio of copper nano particles and formic acid can be 1 ﹕ 8,1 ﹕
8.5,1 ﹕ 9,1 ﹕ 9.5,1 ﹕ 10 etc..
Within the above range by the mass ratio of regulation copper nano particles and liquid organic acid such as formic acid, make copper nano particles
The copper oxide on surface can sufficiently react to obtain formic acid layers of copper with formic acid, while guarantee that copper nano particles are uniformly dispersed.
Preferably, the diameter of the copper nano particles is 100-500nm, more preferably 150-300nm.
As in different embodiments, the average diameters of copper nano particles can for 100nm, 110nm, 120nm, 130nm,
140nm、150nm、160nm、170nm、180nm、190nm、200nm、210nm、220nm、230nm、240nm、250nm、
260nm, 270nm, 280nm, 290nm, 300nm etc..
Preferably, the time of the ultrasonic treatment is 2-8min, preferably 4-6min.
Preferably, the power of the ultrasonic treatment is 360-400W.
As in different embodiments, the power of ultrasonic treatment can for 360W, 365W, 370W, 375W, 380W, 385W,
390W, 395W, 400W etc..
In a specific embodiment of the invention, after ultrasonic treatment, it can isolate and collect by way of centrifuge separation
Copper nano particles after ultrasonic treatment.Optionally, the revolving speed of centrifugation is 1000-2000r/min.
As in different embodiments, the revolving speed of centrifugation can for 1000r/min, 1050r/min, 1100r/min,
1150r/min、1200r/min、1250r/min、1300r/min、1350r/min、1400r/min、1450r/min、1500r/
min、1550r/min、1600r/min、1650r/min、1700r/min、1750r/min、1800r/min、1850r/min、
1900r/min, 1950r/min, 2000r/min etc. can preferably be divided using the centrifugal speed of these above-mentioned revolving speeds
From effect.
Preferably, it is cleaned using ethyl alcohol and removes liquid organic acid.
Ethyl alcohol has suitable boiling point, and the ethyl alcohol on copper nano particles surface is remained in after cleaning removing liquid organic acid, can
To dry and remove at a lower temperature, and the organic acid layers of copper of formation will not be impacted.
Preferably, the method for the cleaning includes: to be cleaned 1-5 times, preferably 3-5 times using ethyl alcohol.
Preferably, every time in cleaning, the mass ratio of copper nano particles and ethyl alcohol is 1 ﹕ (6-8).
Using the method for above-mentioned cleaning, organic acid cleaning extra in the organic acid layers of copper of copper nano particles surface can be removed
It goes, and organic acid layers of copper will not be impacted.
Preferably, the temperature of the drying is 30-40 DEG C.It is furthermore preferred that the time of the drying is 20-22h.
Using above-mentioned drying condition, the alcohol solvent on copper nano particles surface can be removed, it is sufficiently dry, while will not be right
Organic acid layers of copper impacts.
Preferably, using vacuum drying mode.
Vacuum drying mode can further avoid the oxidation to copper nano particles.
Preferably, the copper nano particles obtained after drying are pressed into copper nano particles welding rod.It is furthermore preferred that using cold pressing
Method is suppressed.It is further preferred that the pressing pressure of the cold-press method is 15-30MPa.
It using cold-press method prepared by welding material and is formed, facilitate preservation.
The present invention also provides the copper nano-weld materials being prepared using above-mentioned preparation method.
Welding material of the invention is not limited to welding rod, and the welding material of other forms can also be made according to actual needs.
Compared with prior art, the invention has the benefit that
(1) preparation method of the invention, by copper nano particles and liquid organic acid under ultrasonication, generating very thin has
Machine acid copper-clad coating while avoiding nanoparticle agglomerates, can be improved the inoxidizability of copper nano particles, improve electric conductivity；
(2) the very thin copper organic acid clad of preparation method of the invention, generation will not influence subsequent welding process,
Improve electric conductivity and welding efficiency；Meanwhile preparation method of the invention is easy to operate, reproducible, cost of material is low, cost
It is low；
(3) copper nano-weld material of the invention, copper content is high, is free of other fillers, has high welding efficiency；Simultaneously
Conductivity, thermal conductivity are higher, and store conveniently.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
The XRD spectrum for the copper nano particles that the step of Fig. 1 is the embodiment of the present invention 1 (3) obtains；
Fig. 2 is the XRD spectrum of the untreated copper nano particles raw material of the embodiment of the present invention 1, wherein the position irised out is
Oxidation peak；
The XRD spectrum for the copper nano particles that the step of Fig. 3 is the embodiment of the present invention 3 (3) obtains；
Fig. 4 is the XRD spectrum of the untreated copper nano particles raw material of the embodiment of the present invention 3, wherein the position irised out is
Oxidation peak.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but
Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole
Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability
Domain those of ordinary skill every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same
Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
The preparation method for present embodiments providing a kind of copper nano-weld material, includes the following steps:
(1) at room temperature, ultrasonic disperse is put into after the copper nano particles that average diameter is 150nm being mixed with formic acid
It is ultrasonically treated in machine, the mass ratio of copper nano particles and formic acid is 1 ﹕ 8, and the time of ultrasonic treatment is 5min, and ultrasonic power is
360W；
(2) mixture after ultrasonic treatment in step (1) is placed in a centrifuge and is centrifugated out copper nano particles；Its
In, the centrifugal rotational speed of centrifuge is 1250r/min；
(3) copper nano particles being centrifugated out in step (2) are cleaned using dehydrated alcohol, cleaning 4 times, every time
The quality of the dehydrated alcohol used is 7 times of copper nano particles quality；After cleaning, the vacuum drying treatment under the conditions of 35 DEG C
20h obtains dry copper nano particles；
(4) copper nano particles dry obtained in step (3) are pressed into copper nano particles welding rod using cold-press method, it is cold
The pressure of pressure is 20MPa.
Fig. 1 is the XRD spectrum of copper nano particles dry obtained in the present embodiment step (3), it can be seen from the figure that
Treated, and copper nano particles welding body impurity is few, and purity is very high.Fig. 2 is the XRD diagram of untreated copper nano particles raw material, is had
Apparent oxidation peak.
Embodiment 2
The preparation method for present embodiments providing a kind of copper nano-weld material, includes the following steps:
(1) at room temperature, ultrasonic disperse is put into after the copper nano particles that average diameter is 150nm being mixed with acetic acid
It is ultrasonically treated in machine, the mass ratio of copper nano particles and acetic acid is 1 ﹕ 9, and the time of ultrasonic treatment is 5min, and ultrasonic power is
380W；
(2) mixture after ultrasonic treatment in step (1) is placed in a centrifuge and is centrifugated out copper nano particles；Its
In, the centrifugal rotational speed of centrifuge is 1500r/min；
(3) copper nano particles being centrifugated out in step (2) are cleaned using dehydrated alcohol, cleaning 4 times, every time
The quality of the dehydrated alcohol used is 7 times of copper nano particles quality；After cleaning, under the conditions of 35 DEG C at vacuum drying
Reason, obtains dry copper nano particles；
(4) copper nano particles dry obtained in step (3) are pressed into copper nano particles welding rod using cold-press method, it is cold
The pressure of pressure is 30MPa.
Embodiment 3
The preparation method for present embodiments providing a kind of copper nano-weld material, includes the following steps:
(1) at room temperature, ultrasonic disperse is put into after the copper nano particles that average diameter is 300nm being mixed with formic acid
It is ultrasonically treated in machine, the mass ratio of copper nano particles and propionic acid is 1 ﹕ 8, and the time of ultrasonic treatment is 5min, and ultrasonic power is
400W；
(2) mixture after ultrasonic treatment in step (1) is placed in a centrifuge and is centrifugated out copper nano particles；Its
In, the centrifugal rotational speed of centrifuge is 1750r/min；
(3) copper nano particles being centrifugated out in step (2) are cleaned using dehydrated alcohol, cleaning 4 times, every time
The quality of the dehydrated alcohol used is 7 times of copper nano particles quality；After cleaning, under the conditions of 35 DEG C at vacuum drying
Reason, obtains dry copper nano particles；
(4) copper nano particles dry obtained in step (3) are pressed into copper nano particles welding rod using cold-press method, it is cold
The pressure of pressure is 20MPa.
Fig. 3 is the XRD spectrum of copper nano particles dry obtained in the present embodiment step (3), it can be seen from the figure that
Copper nano particles welding body impurity after purification processes is few, and purity is very high.Fig. 4 is the XRD of untreated copper nano particles raw material
Figure, there is apparent oxidation peak.
Embodiment 4
The preparation method for present embodiments providing a kind of copper nano-weld material, includes the following steps:
(1) at room temperature, ultrasonic disperse is put into after the copper nano particles that average diameter is 300nm being mixed with propionic acid
It is ultrasonically treated in machine, the mass ratio of copper nano particles and propionic acid is 1 ﹕ 9, and the time of ultrasonic treatment is 5min, and ultrasonic power is
400W；
(2) mixture after ultrasonic treatment in step (1) is placed in a centrifuge and is centrifugated out copper nano particles；Its
In, the centrifugal rotational speed of centrifuge is 2000r/min；
(3) copper nano particles being centrifugated out in step (2) are cleaned using dehydrated alcohol, cleaning 4 times, every time
The quality of the dehydrated alcohol used is 7 times of copper nano particles quality；After cleaning, under the conditions of 35 DEG C at vacuum drying
Reason, obtains dry copper nano particles；
(4) copper nano particles dry obtained in step (3) are pressed into copper nano particles welding rod using cold-press method, it is cold
The pressure of pressure is 30MPa.
Embodiment 5
The preparation method for present embodiments providing a kind of copper nano-weld material, includes the following steps:
(1) at room temperature, ultrasonic disperse is put into after the copper nano particles that average diameter is 300nm being mixed with propionic acid
It is ultrasonically treated in machine, the mass ratio of copper nano particles and propionic acid is 1 ﹕ 8, and the time of ultrasonic treatment is 5min, and ultrasonic power is
400W；
(2) mixture after ultrasonic treatment in step (1) is placed in a centrifuge and is centrifugated out copper nano particles；Its
In, the centrifugal rotational speed of centrifuge is 1750r/min；
(3) copper nano particles being centrifugated out in step (2) are cleaned using dehydrated alcohol, cleaning 4 times, every time
The quality of the dehydrated alcohol used is 7 times of copper nano particles quality；After cleaning, under the conditions of 35 DEG C at vacuum drying
Reason, obtains dry copper nano particles；
(4) copper nano particles dry obtained in step (3) are pressed into copper nano particles welding rod using cold-press method, it is cold
The pressure of pressure is 20MPa.
Experimental example 1
For the performance for the copper nano particles welding rod that comparative illustration various embodiments of the present invention and comparative example obtain, to each implementation
The copper nano particles welding rod that example and comparative example obtain is tested as follows, wherein the test method of thermal conductivity is heat-pole method；Conductance
The test method of rate is four probe method；Test result is shown in Table 1.
The performance test results of the different copper nano particles welding rods of table 1
Note: wherein it is untreated refer to copper nano particles are handled without the preparation method of corresponding embodiment, by copper
Nanoparticle raw materials directly adopt step (4) compacting and obtain welding rod
It is found that preparation method of the invention can be improved the electric conductivity and thermal conductivity of copper nano-weld material from upper table,
Improve welding efficiency.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of preparation method of copper nano-weld material, which comprises the steps of:
Copper nano particles are mixed into ultrasonic treatment with liquid organic acid, the copper nano particles after collecting ultrasonic treatment, cleaning removes
Liquid organic acid, it is dry.
2. the preparation method of copper nano-weld material according to claim 1, which is characterized in that the copper nano particles
Diameter is 100-500nm；
Preferably, the diameter of the copper nano particles is 150-300nm.
3. the preparation method of copper nano-weld material according to claim 1 or 2, which is characterized in that the liquid is organic
Acid includes any one or two kinds of mixing of formic acid and acetic acid；
Preferably, the liquid organic acid is formic acid.
4. the preparation method of copper nano-weld material according to claim 3, which is characterized in that the copper nano particles with
The mass ratio of liquid organic acid is 1 ﹕ (8-10).
5. the preparation method of copper nano-weld material according to claim 1 or 4, which is characterized in that the ultrasonic treatment
Time be 2-8min；
Preferably, the time of the ultrasonic treatment is 4-6min；
Preferably, the power of the ultrasonic treatment is 360-400W.
6. the according to claim 1, preparation method of 2,4 described in any item copper nano-weld materials, which is characterized in that by from
The mode of heart separation, the copper nano particles after collecting ultrasonic treatment；
Preferably, the revolving speed of the centrifugation is 1000-2000r/min.
7. the according to claim 1, preparation method of 2,4 described in any item copper nano-weld materials, which is characterized in that use second
Alcohol cleaning removes liquid organic acid；
Preferably, the method for the cleaning includes: to be cleaned 1-5 times using ethyl alcohol；
It is furthermore preferred that being cleaned 3-5 times using ethyl alcohol；
Preferably, every time in cleaning, the mass ratio of the copper nano particles and ethyl alcohol is 1 ﹕ (6-8).
8. the according to claim 1, preparation method of 2,4 described in any item copper nano-weld materials, which is characterized in that described dry
Dry temperature is 30-40 DEG C；
Preferably, the time of the drying is 20-22h；
Preferably, using vacuum drying mode.
9. the according to claim 1, preparation method of 2,4 described in any item copper nano-weld materials, which is characterized in that will dry
The copper nano particles obtained afterwards are pressed into copper nano particles welding rod；
Preferably, it is suppressed using cold-press method；
It is furthermore preferred that the pressing pressure of the cold-press method is 15-30MPa.
10. the copper nanometer weldering being prepared using the preparation method of the described in any item copper nano-weld materials of claim 1-9
Connect material.
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| CN111843169A (en) * | 2020-06-29 | 2020-10-30 | 华北水利水电大学 | Method for ultrasonically welding copper thin plate and nickel thin plate |
| CN111843167A (en) * | 2020-06-29 | 2020-10-30 | 华北水利水电大学 | Method for ultrasonically welding nickel-titanium shape memory alloy thin plate |
| CN112904625A (en) * | 2021-01-25 | 2021-06-04 | 北海惠科光电技术有限公司 | Preparation method of conductive frame glue, conductive frame glue and display panel |
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