CN105609426B - A kind of nano pulp preparation method free of cleaning for low-temperature welding - Google Patents
A kind of nano pulp preparation method free of cleaning for low-temperature welding Download PDFInfo
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- CN105609426B CN105609426B CN201610040154.2A CN201610040154A CN105609426B CN 105609426 B CN105609426 B CN 105609426B CN 201610040154 A CN201610040154 A CN 201610040154A CN 105609426 B CN105609426 B CN 105609426B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
Abstract
The invention discloses a kind of preparation method of the nano pulp free of cleaning for low-temperature welding, comprise the following steps：1) organic thickening agent is added in the pyrrolidones of N methyl 2, solution A is formed through magnetic agitation；2) organic binder bond is added in the solution A, solution B is formed through magnetic agitation；3) m is taken1G nano metal powder and m2G solution B, stirred in vacuum defoamation mixer, obtain nano pulp.Nano pulp prepared by this method, not volatile under sealing state, storage stability is good.When preparing weld layer in substrate, coating, wetability are good, free of cleaning after welding, without post processing, suitable for low-temperature welding, interconnection and bonding.
Description
Technical field
The invention belongs to microelectronics Packaging field, more particularly, to a kind of nano pulp preparation method.
Background technology
Along with IC-3D integrated chips Electronic Encapsulating Technology in high speed development over the past thirty years, increasing technology
Bottleneck already slowly emerges, and Moore's Law can no longer represent the development trend of current IC electronic industries, and wherein IC-3D is integrated
Micro- interconnection material main flow in electronic chip package technology uses the lead-free solder based on tin.
When micro- interconnection interface size is less and less, the lead-free solder based on tin has just embodied many drawbacks, such as：Electricity
It is not high to flow bearing capacity；Tin element is also easy to produce whisker, further reduces current carrying capacity；It is on active service and is also easy to produce for a long time
Kirkendall holes, hinder electric transmission etc..But tin solder is there is also plurality of advantages, such as：Bonding temperature is low, during bonding not
Destructible chip performance and structure；Bond strength height etc..So scholars and scientist thirst for that military service performance can be developed
New solder stronger, current carrying capacity is higher but bonding temperature is low and bond strength is high.
In recent years, nano metal solder becomes the widely studied focus of scientists.Because the yardstick of nano material is imitated
Should, metal becomes hour (nanoscale) in yardstick, and fusing point can decrease, and the highly desirable current carrying capacity of people is more preferable, is on active service
Other stronger metal nano materials of stability can be widely applied in micro- interconnection.
But prepared and research process in solder, directly have shortcomings and not using commercial lead-free solder soldering fluid
Just part.Commercial lead-free solder soldering fluid is broadly divided into two classes：Colourless or faint yellow paste is presented in the first kind, and main component is
Rosin, and contain the additives such as some thickeners and binding agent.Although such scaling powder with fabulous adhesion property, due to
Its viscosity is too high, if in nano pulp proportion it is not high if be difficult to be well mixed nano metal powder, and welding
A large amount of impurity can be produced after connecing, it is difficult to clean, subsequently every test such as mechanics, electric property is an impediment to during theoretical research；
Second class is water-based type scaling powder free of cleaning, and such scaling powder volatilization temperature is relatively low, will not also produce a large amount of impurity after welding,
But its viscosity is relatively low, and adhesion property is also poor, it is difficult to metal nanoparticle is coated uniformly on substrate surface and closely ties
Close, experimental repeatability and reliability when having a strong impact on research.
In addition, there is many researchers to mix the higher organic solvent of one or several kinds of viscosityes, directly as receiving
The mixed slurry of rice metal material uses, such as terpinol, ethylene glycol, n-decane, isopropanol.Although such organic solvent can be with
Nano metal material is uniformly mixed, is volatilized completely when compared with low-temperature welding and be free of cleaning, but its adhesion property and water-based scaling powder
It is equally poor, it is difficult to possess good paintability.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of for the free of cleaning of low-temperature welding
Nano pulp preparation method, this method can uniformly mix nano metal material, and make nano material uniformly and be coated in securely
Substrate surface need to be welded, after welding organic solvent completely volatilization and it is free of cleaning, be particularly suitable for carry out low-temperature welding nanometer
Solder.
To achieve the above object, it is proposed, according to the invention, provide a kind of system of the nano pulp free of cleaning for low-temperature welding
Preparation Method, it is characterised in that comprise the following steps：
1) organic thickening agent is added in METHYLPYRROLIDONE and forms solution A through magnetic agitation, wherein, stirring temperature
Spend for 50 DEG C~70 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic thickening agent is 10g/L~20g/L；
2) organic binder bond is added in the solution A and forms solution B through magnetic agitation, wherein, whipping temp is 50 DEG C
~70 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic binder bond is 10g/L~20g/L；
3) m is taken1G nano metal powder and m2G solution B, with 2000 revs/min~3000 in vacuum defoamation mixer
Rev/min speed vacuum stirring 300s~800 second, then obtain nano pulp, wherein, 1：1≤m1：m2≤4：1.
Preferably, the organic thickening agent is ethyl cellulose or methylcellulose.
Preferably, the organic binder bond is polyvinyl acetate or Kynoar.
Preferably, the nano metal powder is one kind or more in copper powder, glass putty, aluminium powder, nickel powder, bronze or silver powder
Kind.
Preferably, the average grain diameter of the nano metal powder is 30nm~800nm.
In general, by the contemplated above technical scheme of the present invention compared with prior art, it can obtain down and show
Beneficial effect：
1) nano pulp prepared by this method, not volatile under sealing state, storage stability is good.Weldering is prepared in substrate
When connecing layer, coating, wetability are good, free of cleaning after welding, without post processing, suitable low-temperature welding, interconnection, bonding occasion；
After nanometer material is coated uniformly on smooth copper sheet by coated rod made from this method, then another smooth copper sheet covered, you can
Thermal compression welding is carried out immediately.
2) present invention has extraordinary stability at normal temperatures using NMP as the organic solvent in slurry, this solvent, no
Easily a large amount of volatilizations, are easy to long-time storage, and this solvent boiling point is 204 DEG C, can meet in low-temperature welding, interconnection research 200 DEG C~
The demand that organic solvent volatilizees completely at 300 DEG C, this solvent viscosity is higher, largely reduces the addition of thickener
Amount；
3) present invention is used as thickener using ethyl cellulose (EC) or methylcellulose (MC), and such thickener is food
Industry typical additives, basic nonhazardous, and very small amount, which use, just can reach preferably thickening purpose；
4) present invention is used as binding agent, such binding agent using polyvinyl acetate (PVAC) or Kynoar (PVDF)
Basic nonhazardous, it can preferably increase the adhesive property between nano-metal particle and can closely be glued between substrate in coating
It is attached；
5) present invention uses copper nanoparticle, glass putty, nickel powder, aluminium powder, bronze or silver powder as solid filling material, this eka-gold
Belong to the common used material in being studied for modern nanotube-solder, can well reflect performance of the welding material in this slurry；
6) present invention is using vacuum defoamation mixer as material mixer, and for such machinery without stirring rod, vacuum-pumping can be
Even mixing very small amount nano metal material, can effectively suppress the material oxidation in mixing process by the removal of bubbles in slurry.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in each embodiment of invention described below
Conflict can is not formed each other to be mutually combined.
Reference picture 1, the present invention propose a kind of nano pulp preparation method free of cleaning for low-temperature welding, and formation is received
Metal nano material, organic solvent, organic thickening agent and organic binder bond are included in Rice ＆ peanut milk material.In addition, the present invention also provides
The preparation process of above-mentioned slurry, mainly comprising following steps：1), by organic thickening agent (ethyl cellulose or first
Base cellulose) proportionally first carry out being thoroughly mixed to form solution A with organic solvent (METHYLPYRROLIDONE)；2), again will
Organic binder bond (polyvinyl acetate or Kynoar) is proportionally dissolved in solution A, forms solution B；3), mix simultaneously
After being uniformly dissolved, by solution B and nano metal material (one kind or more in copper powder, glass putty, aluminium powder, nickel powder, bronze or silver powder
Kind) be proportionally well mixed, used for coating.The present invention can uniformly mix nano metal material and form nano pulp, and make
Nano pulp material is uniformly and securely coated in that need to weld substrate surface, and (more than 205 DEG C are welded) organic solvent is complete after welding
Volatilize and free of cleaning, be particularly suitable for low-temperature welding.
Embodiment 1
A kind of preparation method of nano pulp free of cleaning for low-temperature welding, comprises the following steps：
1) organic thickening agent is added in METHYLPYRROLIDONE and forms solution A through magnetic agitation, wherein, stirring temperature
Spend for 60 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic thickening agent is 10g/L；The organic thickening agent is
Ethyl cellulose or methylcellulose.
2) organic binder bond is added in the solution A and forms solution B through magnetic agitation, wherein, whipping temp is 50 DEG C,
Mixing time is more than 1 hour, and the mass concentration of the organic binder bond is 10g/L；The organic binder bond is poly- acetic acid second
Alkene ester or Kynoar.
3) m is taken1G nano metal powder and m2G solution B, with 2000 revs/min of speed in vacuum defoamation mixer
It is stirred under vacuum 800 seconds, then obtains nano pulp, wherein, m1：m2=1：1.The nano metal powder is glass putty, aluminium powder or nickel powder
In the average grain diameters of one or more and described nano metal powders be 500nm.
Embodiment 2
A kind of preparation method of nano pulp free of cleaning for low-temperature welding, comprises the following steps：
1) organic thickening agent is added in METHYLPYRROLIDONE and forms solution A through magnetic agitation, wherein, stirring temperature
Spend for 50 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic thickening agent is 20g/L；The organic thickening agent is
Ethyl cellulose or methylcellulose.
2) organic binder bond is added in the solution A and forms solution B through magnetic agitation, wherein, whipping temp is 70 DEG C,
Mixing time is more than 1 hour, and the mass concentration of the organic binder bond is 13g/L；The organic binder bond is poly- acetic acid second
Alkene ester or Kynoar.
3) m is taken1G nano metal powder and m2G solution B, with 3000 revs/min of speed in vacuum defoamation mixer
It is stirred under vacuum 600 seconds, then obtains nano pulp, wherein, m1：m2=2.3：1.The nano metal powder is in bronze or silver powder
The average grain diameters of one or more and described nano metal powders be 30nm.
Embodiment 3
A kind of preparation method of nano pulp free of cleaning for low-temperature welding, comprises the following steps：
1) organic thickening agent is added in METHYLPYRROLIDONE and forms solution A through magnetic agitation, wherein, stirring temperature
Spend for 70 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic thickening agent is 13g/L；The organic thickening agent is
Ethyl cellulose or methylcellulose.
2) organic binder bond is added in the solution A and forms solution B through magnetic agitation, wherein, whipping temp is 60 DEG C,
Mixing time is more than 1 hour, and the mass concentration of the organic binder bond is 20g/L；The organic binder bond is poly- acetic acid second
Alkene ester or Kynoar.
3) m is taken1G nano metal powder and m2G solution B, with 2500 revs/min of speed in vacuum defoamation mixer
It is stirred under vacuum 300 seconds, then obtains nano pulp, wherein, m1：m2=4：1.The nano metal powder is copper powder, bronze or silver powder
In the average grain diameters of one or more and described nano metal powders be 800nm.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (3)
1. the preparation method of a kind of nano pulp free of cleaning for low-temperature welding, it is characterised in that comprise the following steps：
1) organic thickening agent is added in METHYLPYRROLIDONE and forms solution A through magnetic agitation, wherein, whipping temp is
50 DEG C~70 DEG C, mixing time is more than 1 hour, and the mass concentration of the organic thickening agent is 10g/L~20g/L, described to have
Machine thickener is ethyl cellulose or methylcellulose；
2) organic binder bond is added in the solution A and forms solution B through magnetic agitation, wherein, whipping temp is 50 DEG C~70
DEG C, mixing time is more than 1 hour, and the mass concentration of the organic binder bond is 10g/L~20g/L, the organic binder bond
For polyvinyl acetate or Kynoar；
3) m is taken1G nano metal powder and m2G solution B, with 2000 revs/min~3000 revs/min in vacuum defoamation mixer
Speed vacuum stirring 300s~800 second, then obtain nano pulp, wherein, 1：1≤m1：m2≤4：1.
2. a kind of preparation method of nano pulp free of cleaning for low-temperature welding according to claim 1, its feature exist
In the nano metal powder is the one or more in copper powder, glass putty, aluminium powder, nickel powder, bronze or silver powder.
3. a kind of preparation method of nano pulp free of cleaning for low-temperature welding according to claim 1, its feature exist
In the average grain diameter of the nano metal powder is 30nm~800nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610040154.2A CN105609426B (en) | 2016-01-21 | 2016-01-21 | A kind of nano pulp preparation method free of cleaning for low-temperature welding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610040154.2A CN105609426B (en) | 2016-01-21 | 2016-01-21 | A kind of nano pulp preparation method free of cleaning for low-temperature welding |
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| Publication Number | Publication Date |
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| CN105609426A CN105609426A (en) | 2016-05-25 |
| CN105609426B true CN105609426B (en) | 2018-01-05 |
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| CN201610040154.2A Expired - Fee Related CN105609426B (en) | 2016-01-21 | 2016-01-21 | A kind of nano pulp preparation method free of cleaning for low-temperature welding |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108098191B (en) * | 2017-12-17 | 2020-02-14 | 华中科技大学 | Preparation method of copper nanoparticle soldering paste and product thereof |
| CN111916344B (en) * | 2020-09-09 | 2022-10-04 | 合肥工业大学 | Copper-copper low-temperature bonding method based on graphene/tin modified copper nanoparticles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000094179A (en) * | 1998-09-22 | 2000-04-04 | Harima Chem Inc | Solder paste and manufacture of the same and method for solder precoating |
| CN101156236A (en) * | 2005-04-06 | 2008-04-02 | 松下电器产业株式会社 | Flip chip mounting method and bump forming method |
| CN101224525A (en) * | 2008-01-21 | 2008-07-23 | 广州瀚源电子科技有限公司 | Lead-free pasty solder and preparing method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100409423C (en) * | 2003-02-05 | 2008-08-06 | 千住金属工业株式会社 | Method for interconnecting terminals and method for mounting semiconductor device |
-
2016
- 2016-01-21 CN CN201610040154.2A patent/CN105609426B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000094179A (en) * | 1998-09-22 | 2000-04-04 | Harima Chem Inc | Solder paste and manufacture of the same and method for solder precoating |
| CN101156236A (en) * | 2005-04-06 | 2008-04-02 | 松下电器产业株式会社 | Flip chip mounting method and bump forming method |
| CN101224525A (en) * | 2008-01-21 | 2008-07-23 | 广州瀚源电子科技有限公司 | Lead-free pasty solder and preparing method thereof |
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