CN101745752B - Nanometer reinforced bismuth base lead-free high-temperature solder and preparation method thereof - Google Patents
Nanometer reinforced bismuth base lead-free high-temperature solder and preparation method thereof Download PDFInfo
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- CN101745752B CN101745752B CN2009102419485A CN200910241948A CN101745752B CN 101745752 B CN101745752 B CN 101745752B CN 2009102419485 A CN2009102419485 A CN 2009102419485A CN 200910241948 A CN200910241948 A CN 200910241948A CN 101745752 B CN101745752 B CN 101745752B
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 103
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 86
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000002360 preparation method Methods 0.000 title claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 107
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 30
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 29
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 27
- 150000001875 compounds Chemical class 0.000 claims abstract description 17
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052709 silver Inorganic materials 0.000 claims description 41
- 238000005303 weighing Methods 0.000 claims description 14
- -1 bismuthino Chemical group 0.000 claims description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 235000012054 meals Nutrition 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 229910052718 tin Inorganic materials 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 6
- 239000011858 nanopowder Substances 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 5
- 229910052738 indium Inorganic materials 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- 238000000889 atomisation Methods 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- 230000000536 complexating effect Effects 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 29
- 229910045601 alloy Inorganic materials 0.000 abstract description 28
- 238000003466 welding Methods 0.000 abstract description 11
- 229910016331 Bi—Ag Inorganic materials 0.000 abstract description 6
- 238000002844 melting Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 3
- 238000004100 electronic packaging Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 125000001475 halogen functional group Chemical group 0.000 abstract 1
- 238000009725 powder blending Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 47
- 238000005476 soldering Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 13
- 239000010949 copper Substances 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 239000012530 fluid Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 5
- 239000004744 fabric Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910020935 Sn-Sb Inorganic materials 0.000 description 3
- 229910008757 Sn—Sb Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 229910007570 Zn-Al Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 239000006023 eutectic alloy Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000010334 sieve classification Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 229910015363 Au—Sn Inorganic materials 0.000 description 1
- 229910001152 Bi alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 229910017802 Sb—Ag Inorganic materials 0.000 description 1
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910020836 Sn-Ag Inorganic materials 0.000 description 1
- 229910020922 Sn-Pb Inorganic materials 0.000 description 1
- 229910020988 Sn—Ag Inorganic materials 0.000 description 1
- 229910008783 Sn—Pb Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Abstract
The invention relates to a nanometer reinforced bismuth base lead-free high-temperature solder and a preparation method thereof, belonging to the technical field of lead-free solder manufacture. The nanometer reinforced bismuth base lead-free high-temperature solder comprises silver nanopowder and bismuth powder or powder blending bismuth and antimony or alloy powder, wherein the silver nanopowder accounts for 2-12wt%. The preparation method comprises: firstly, preparing bismuth powder (or bismuth/ antimony powder); evenly introducing bismuth powder (or bismuth/ antimony powder) with ration proportioning into silver nitrate solution provided with a stirring device; adding ammonia water to form silver-amino complex; reducing complex compound into the even compound of nano Ag powder and Bi powder (or bismuth/ antimony powder). The lead-free high-temperature solder can improve the problems of poor electric conduction and thermal conductivity of Bi-Ag (or Bi-Sb-AG) alloy solder and has the advantages of high strength, long service life, favourable tightness, light round halo of welding points and the like in the welding and using process. According to different compositions between powders, the nanometer reinforced bismuth base lead-free high-temperature solder can be prepared into high-temperature solder with any melting point at the temperature of 260-380 DEG C so as to replace high-Pb solder for electronic packaging.
Description
Technical field
The present invention relates to a kind of nanometer reinforced bismuth base lead-free high-temperature solder and preparation method thereof, this scolder is formed by chemically composited by metal bismuth meal (or mixed powder/alloyed powder of bismuth and antimony) and nanometer Ag powder, belongs to the manufacturing technology field of lead-free solder.
Background technology
Pay attention to environmental protection, advocate the main trend that green product is the current world economy development, the unleaded of electronic product is exactly wherein major action.Unleaded alternative aspect at middle low temperature solder containing pb, progressively obtained reliability demonstration through nearly 10 years research, and be widely used, yet high kupper solder [w (Pb)＞85%] does not but also have suitable substitute so far, has therefore obtained temporary transient exemption in the RoHS instruction yet.But plan according to instruction: the RoHS of European Union instruction will be phased out exempt item, may all exemptions will be disengaged in July, 2014, to realize the unleaded comprehensively of electronics package system when the time comes, high kupper solder is also with replaced, therefore it is significant to prepare the well behaved lead-free product that can be used for substituting high kupper solder, and the research to high temperature lead-free solder at present mainly concentrates on 80Au-Sn alloy, Sn-Sb base alloy, Zn-Al base alloy and Bi base alloy.
1,80Au-Sn scolder: the fusing point of Au-Sn eutectic solder is 280 ℃, and is the most close with the fusing point of high kupper solder, compatible good, compares (about 217 ℃) with low-melting unleaded eutectic solder, has bigger stability and reliability.But this scolder is more crisp, and because w (Au) is that 80% cost is too high, thereby be mainly used in photoelectron encapsulation, high reliability (as the InP laser diode), high-power electronic device circuit level Hermetic Package and the chip encapsulation.
2, Sn-Sb alloy: because Sn-Sb[w (Sb)≤10%] alloy melting interval narrower (232～250 ℃), and it is compatible good with existing scolder, thereby as the candidate material of high temperature lead-free solder.But its fusing point is lower, particularly scolder unleaded since since the fusing point of existing lead-free solder than the height (general high 30-40 ℃) of Sn-Pb eutectic alloy, package temperature can promote to some extent, follow-up backflow or wave-soldering temperature can surpass its fusing point when causing multistage assembling, and then influence the reliability of packaging, even cause product rejection.
3, Zn-Al alloy: Rettenmayr etc. and Shimizu five equilibrium be you can well imagine and replaced the 95Pb-5Sn scolder with Zn base alloy and realize that chip is connected.But Zn base alloy poor in processability, and oxidation and cause moistening badness easily, and the greater activity of Zn base alloy also makes soldering reliability to be under suspicion, and therefore limited the application of such alloy to a great extent.
4, Bi base alloy: Bi base alloy is considered to replace unleaded candidate's scolder of traditional high Pb scolder owing to fusing point suitable (about 270 ℃), filling capacity are good, as the JP2001-205477 patent alloy of Japanese Murata Manufacturing Co. Ltd. announcement.Bi-Ag is that scolder is the Bi base alloy of studying at most, the mutual solubility of Bi and Ag is very little under the normal temperature, its eutectic alloy fusing point is 262.5 ℃, studies show that its percentage elongation is than SnAg25Sb10 (J alloy, 365 ℃ of fusing points) not bad, increase Ag content and can improve the intensity of Bi-Ag alloy, and can improve the fragility of its alloy, but littler than SnAg25Sb10 alloy generally, and increased cost of alloy.
The defective of Bi base alloy shows that also conduction, heat conductivility are poor except that mechanical property is relatively poor.The Bi base high-temperature leadless scolder (U.S. Patent number 6 that the Japan village announces in the field, 703,113), in matrix, add Ag or Cu, the Zn that is no more than 9.9wt%, and add the Sb of about 0.1-3wt% or Sn, In, Cu, Zn, Ge, P etc., this scolder is mainly used its temperature resistive properties, brittle bases such as glass for bonding.Bi-Ag solder (CN1507499A, the WO2002/097145) pyroconductivity that Honeywell Int Inc announces is not less than behind 9W/mK, the 1s that the wetting power to Ag reaches 0.2mN under the wettability equilibrium condition, and reached anti-oxidant purpose by one or more elements that add among Zn, Ni, Ge, the P, determine but the fragility problem of this alloy still is difficult to resolve, and its electrical and thermal conductivity is had a greatly reduced quality because of the complete alloying of Ag element.For improving the performance of Bi base high-temperature leadless scolder, the Takaku of northeastern Japan university etc. obtain the particular tissues pattern of Bi-Cu-X (X=Sb, Sn and Zn) high temperature lead-free solder by gas atomization and melt rotation method.Especially, the Bi base high-temperature leadless scolder (european patent number EP1952934A1) that Japan's thousand posts are announced has mixed second, third particle in the Bi matrix powder, and Yamada etc. has added the mechanical property that CuAlMn particle that atomization forms improves the Bi alloy in the Bi of fusion, all obtained result preferably, but the size of second particle that is mixed or enhancing particle is compared greatly, thereby the butt welding point performance improvement is still little.
The mode that the middle temperature scolder (Chinese patent 01144487.8 and 200310116809.2) that Beijing Polytechnical University announces has adopted particle to strengthen equally, but the size restrictions that strengthens particle makes and uses limited in more and more littler microbonding point field.Compare, Chinese patent 02125594.6,200810112441.5 and 200510013430.8 has all adopted nanometer to strengthen particle, the mechanical property of scolder and wetability etc. have been improved, wherein Chinese patent 02125594.6 is sneaked into nano particle by the mechanical agitation mode in preparation tin cream process, and Chinese patent 200510013430.8 is by adding ZrO in fused solution Sn-Ag eutectic solder
2Nano particle, the introducing of Chinese patent 200810112441.5 novelties organic nanostructure material, but because its preparation method is the mechanical mixture mode, so its nanometer strengthens the difficult control of uniformity of particle, and warm scolder field in belonging to.
In order to overcome the technological deficiency that high temperature lead-free solder exists at present, solve problems such as intensity is low, service life short, sealing is poor, the bright difference of solder joint circle halation, provide a kind of high temperature lead-free solder that improves performance to become those skilled in the art's urgent problem.
Summary of the invention
One of purpose of the present invention provides a kind ofly has intensity height, service life length, good airproof performance, the bright high temperature lead-free solder of solder joint circle halation in welding and use, and the formation nanometer Ag strengthens the solder joint of Bi parent metal mutually.The present invention is for improving the mechanical property and the electric heating property of Bi base lead-free high-temperature solder, depend on the nano silver particles complex on Bi powder (or bismuth/antimony powder) top layer by the preparation of electronation Ag method in being mixed with the silver nitrate turbid solution of Bi based powders, and then reach the mixing of nano silver particles and base powder particles.Controls such as process window when passing through welding in welding is used and different component content proportioning realize that the part nanometer strengthens silver particles and matrix generation alloying reaction, reach in conjunction with perfect purpose.
For achieving the above object, the present invention takes following technical scheme:
A kind of nanometer reinforced bismuth base lead-free high-temperature solder is characterized in that: the mixed powder or the alloyed powder (hereinafter to be referred as bismuth/antimony powder) that comprise silver-colored nano powder and bismuth meal or bismuth, antimony; Wherein silver-colored nano powder accounts for 2～12wt%.
A kind of optimized technical scheme is characterized in that: in the mixed powder or alloyed powder of described bismuth, antimony, and bi content 〉=80wt%, antimony content≤20wt%.
A kind of optimized technical scheme is characterized in that: also comprise total amount and be no more than in 1% Sn, In, Cu, Zn, Ge, Au or the Ni element one or more.
A kind of optimized technical scheme is characterized in that: the mixed powder or the alloyed powder of described silver-colored nano powder and bismuth meal or bismuth, antimony form even complex.
Another object of the present invention provides the preparation method of above-mentioned high temperature lead-free solder, solve the mixing uniformity problem that nanometer strengthens scolder, utilize Yin Nami to strengthen to alleviate the fragility of Bi-Ag serial alloy welding material, improve its conduction, thermal conductivity, improve the wetability on its metal layer (copper, nickel, gold, silver, naked silicon etc.) common parts.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method of nanometer reinforced bismuth base lead-free high-temperature solder, its preparation process is as follows:
(1) takes by weighing the bismuthino powder, can adopt any known powder-making techniques such as Mechanical Crushing or medium atomization;
(2) the even importing of quantitative bismuthino powder had in the liquor argenti nitratis ophthalmicus of agitating device, make silver contained in the liquor argenti nitratis ophthalmicus be 2～12% of silver and bismuthino powder gross weight, constantly stirring makes solution become uniform turbid solution;
(3) take by weighing relative silver nitrate excess of ammonia water or other can with the material of silver-colored complexing, and it is added in the turbid solution of step (2) gained slowly, make silver ion be completed into complex compound or complex;
(4),, form the even complex of nano-silver powder and bismuthino powder with the complex compound reduction constantly slowly adding reducing agent under the stirring condition;
(5) filter, the gained filter cake is dried, dries up or is dried under guard mode, promptly gets nanometer reinforced bismuth base lead-free high-temperature solder.
In the scolder of gained, add quantitative scaling powder and stir into uniform fluid, promptly prepare the high-temp leadless soldering paste.
A kind of optimized technical scheme is characterized in that: described bismuthino powder packets contains the mixed powder or the alloyed powder of bismuth meal or bismuth, antimony.
A kind of optimized technical scheme is characterized in that: in the mixed powder or alloyed powder of described bismuth, antimony, and bi content 〉=80wt%, antimony content≤20wt%.
A kind of optimized technical scheme is characterized in that: also comprise total amount in the described bismuthino powder and be no more than in 1% Sn, In, Cu, Zn, Ge, Au or the Ni element one or more.
A kind of optimized technical scheme is characterized in that: in the step (3), take by weighing the ammoniacal liquor of relative silver nitrate excessive 5～20% or other can with the material of silver-colored complexing.
A kind of optimized technical scheme is characterized in that: the reducing agent described in the step (4) is hydrazine hydrate, glucose or formaldehyde etc.Described reducing agent can excessive 5～20%.
A kind of optimized technical scheme is characterized in that: in the step (5), the oven dry under vacuum state or hydrogen, inert gas shielding state of gained filter cake, dry up or dry.
Beneficial effect: nanometer reinforced bismuth base lead-free high-temperature solder of the present invention exists to have and compares the better conduction of alloy material, thermal conductivity and more excellent weld strength because of having complex nanometer Ag wild phase, has intensity height, service life length, good airproof performance, solder joint and justify characteristics such as halation is bright in welding and use; In addition, experiment shows that silver-colored nanometer reinforced bismuth base lead-free high-temperature solder of the present invention is controlled by welding procedure, can control the nanometer Ag proportion of home position alloying and the size and the distribution of Ag phase, and obtains best serviceability.
The composite powder of this method preparation efficiently solves the even mixed problem that nanometer strengthens particle and matrix powder, and can improve the problems such as conduction, poor thermal conductivity of Bi-Ag (or Bi-Sb-Ag) serial alloy welding material.Can make the high-temperature solder that is made into 260-380 ℃ of any fusing point according to the composition of the difference between powder, be used for substituting the high Pb scolder of used for electronic packaging.
The present invention is described in detail below by drawings and Examples.It should be understood that described embodiment only relates to the preferred embodiments of the invention, do not breaking away under the spirit and scope of the present invention situation that the changes and improvements of various components and content all are possible.
Description of drawings
Fig. 1 is the preparation facilities schematic diagram of nanometer reinforced bismuth base lead-free high-temperature solder of the present invention.
Fig. 2 is preparation technology's flow chart of preparation nanometer reinforced bismuth base lead-free high-temperature solder of the present invention.
Fig. 3 sprawls comparison diagram for the solder joint of typical nanometer reinforced bismuth base lead-free high-temperature solder and BiAg2.5, SnPb90 and SnPb95 solder among the present invention.
The specific embodiment
Fig. 1 is the preparation facilities schematic diagram of nanometer reinforced bismuth base lead-free high-temperature solder of the present invention.Wherein 1 is agitator; 2 is charge doors such as bismuthino powder, ammoniacal liquor (or other weak base), reducing agent; 3 is the turbid solution container.
As shown in Figure 2, for preparing preparation technology's flow chart of nanometer reinforced bismuth base lead-free high-temperature solder of the present invention.The first step: take by weighing bismuth meal (or preparing bismuth/antimony powder in proportion), its preparation method can be any known powder-making techniques such as Mechanical Crushing or medium atomization; Second step: quantitative bismuth meal (or bismuth/antimony powder) is evenly imported the quantitative finite concentration liquor argenti nitratis ophthalmicus with agitating device, constantly stir, make solution become uniform turbid solution; The 3rd step: take by weighing quantitative ammoniacal liquor (compare silver nitrate will have excessive), and it constantly is added in the turbid solution, make silver nitrate be completed into silver ammonia complex; The 4th step: add reducing agent gradually (as, hydrazine hydrate (N
2H
4H
2O), glucose sugar, formaldehyde etc.), the complex compound reduction is formed the even composite powder-lead-free solder paste base-material of nanometer Ag powder and Bi powder (or bismuth/antimony powder); The 5th step: filter, and oven dry (drying up) under guard mode, add quantitative scaling powder, stir into uniform fluid, prepare the high-temp leadless soldering paste.
Adopt abrasive method to prepare bismuth meal 10kg, sieve is got-400 order powder 980g;
Pour the Bi powder that weighs up the AgNO3 solution of 0.185mol (31.5g solute) into, stir, make solution become uniform turbid solution, in case Bi powder precipitation;
Under stirring, in turbid solution, add ammoniacal liquor (1mol solute) gradually, make silver nitrate can be completed into complex compound (complex (Ag (NH3)
n +) solution);
In turbid solution, slowly add excessive hydrazine hydrate and continue stirring, the complex compound reduction is formed the even composite powder of nanometer Ag powder and Bi powder;
Pour solution into filter cloth and filter, and the powder after will filtering evenly completes and put into vacuum drying oven, drain moisture;
Take by weighing the 100g scaling powder, and put into the Bi+2.0%Ag nanometer reinforced bismuth base lead-free high-temperature solder powder of draining, fully stir, make it into uniform fluid, promptly prepared the high-temp leadless soldering paste.Soldering paste is poured in the solder paste cartridge, put into refrigerator and be in store for.
Embodiment 2 (Bi-10Sb)+2.5%Ag nanometer reinforced bismuth base lead-free high-temperature solder and preparation thereof:
Preparation Bi-10Sb solder 20kg, and utilize of the Bi-10Sb solder atomizing of ultrasonic atomizatio powder-making technique with fusing, and sieve classification, get 3# powder (25-45um) 975g;
Take by weighing the chip 25g of silver, pour nitric acid into and fully stir, Ag is dissolved fully;
Pour the Bi-10Sb alloyed powder that weighs up into AgNO that system prepares
3Solution stirs, and makes solution become uniform turbid solution, in case Bi-10Sb alloyed powder precipitation;
Under stirring, in turbid solution, add capacity ammoniacal liquor (1mol solute) gradually, make silver nitrate can be completed into complex compound (complex (Ag (NH3)
n +) solution);
In turbid solution, slowly splash into excessive formaldehyde and continue and stir, the complex compound reduction is formed the even composite powder of nanometer Ag powder and Bi-10Sb alloyed powder;
Pour solution into filter cloth and filter, and the powder after will filtering evenly completes and put into 100 ℃ of holding furnaces, logical hydrogen is dried moisture;
Take by weighing the 110g scaling powder, and put into (Bi-10Sb)+2.5%Ag nanometer reinforced bismuth base lead-free high-temperature solder powder of oven dry, fully stir, make it into uniform fluid, promptly prepared the high-temp leadless soldering paste.Soldering paste is poured in the solder paste cartridge, put into refrigerator and be in store for.
Embodiment 3 (Bi-10Sb-0.5Sn)+5%Ag nanometer reinforced bismuth base lead-free high-temperature solder and preparation thereof:
Preparation Bi-10Sb-0.5Sn solder 50kg, and utilize of the Bi-10Sb-0.5Sn solder atomizing of centrifugal atomizing powder-making technique with fusing, and sieve classification, get 3# powder (25-45um) 950g;
The Bi-10Sb-0.5Sn powder that weighs up is poured into the AgNO of 0.463mol (78.7g solute)
3Solution stirs, and makes solution become uniform turbid solution, in case Bi-10Sb-0.5Sn alloyed powder precipitation;
The mixed solution that adds rare NaOH and ammoniacal liquor under stirring in turbid solution gradually makes silver nitrate can be completed into complex compound (complex (Ag (NH3)
n +) solution);
Under stirring condition, in turbid solution, slowly add excessive glucose solution, the complex compound reduction is formed the even composite powder of nanometer Ag powder and Bi-10Sb-0.5Sn alloyed powder;
Pour solution into filter cloth and filter, and the powder after will filtering evenly completes and put into 60 ℃ vacuum drying oven, dry moisture;
Take by weighing the 110g scaling powder, and put into (Bi-10Sb-0.5Sn)+5.0%Ag nanometer reinforced bismuth base lead-free high-temperature solder powder of oven dry, fully stir, make it into uniform fluid, promptly prepared the high-temp leadless soldering paste.Soldering paste is poured in the solder paste cartridge, put into refrigerator and be in store for.
Embodiment 4 (Bi-0.1Ge)+10%Sb+5%Ag nanometer reinforced bismuth base lead-free high-temperature solder and preparation thereof:
Preparation Bi-0.1Ge solder 900g, pure Sb100g, two canisters putting into the star ball grinder after smashing respectively carry out ball milling 6h, get Bi-0.1Ge alloyed powder 855g, Sb powder 95g;
The AgNO that pours the Bi-0.1Ge alloyed powder that weighs up and Sb powder into 0.463mol (78.7g solute) synchronously
3Solution stirs, and makes solution become uniform turbid solution, in case Bi-0.1Ge alloyed powder and Sb powder precipitation;
Under stirring, in this turbid solution, add ammoniacal liquor gradually, make silver nitrate can be completed into complex compound (complex (Ag (NH3)
n +) solution);
Under stirring condition, in turbid solution, slowly add excessive hydrazine hydrate solution, the complex compound reduction is formed the even composite powder of nanometer Ag powder+Bi-0.1Ge alloyed powder+Sb powder;
Pour turbid solution into filter cloth and filter, and the powder after will filtering evenly completes with nitrogen and dry, carry out air-dry processing;
Take by weighing the 110g scaling powder, and put into air-dry (Bi-0.1Ge)+10%Sb+5.0%Ag nanometer reinforced bismuth base lead-free high-temperature solder powder, fully stir, make it into uniform fluid, promptly prepared the high-temp leadless soldering paste.Soldering paste is poured in the solder paste cartridge, put into refrigerator and be in store for.
Embodiment 5 (Bi-0.1Cu)+1% (Sn-10Sb-0.5Ge)+12%Ag nanometer reinforced bismuth base lead-free high-temperature solder and preparation thereof:
Preparation Bi-0.1Cu solder 2kg, sieve is got the 870g powder behind the mechanical ball milling; The preparation of melting simultaneously Sn-10Sb-0.5Ge solder 5kg, sieve is got the 10g powder behind the employing ultrasonic atomizatio legal system powder;
Take by weighing the chip 120g of silver, pour capacity nitric acid into and fully stir, Ag is dissolved fully;
Pour the Bi-0.1Cu alloyed powder and the Sn-10Sb-0.5Ge alloy powder that weigh up into AgNO that system prepares synchronously
3In the solution, stir, make solution become uniform turbid solution, in case mix uneven between Bi-0.1Cu and Sn-10Sb-0.5Ge alloy powder and the generation precipitation;
Under stirring, in this turbid solution, add capacity ammoniacal liquor gradually, make silver nitrate can be completed into complex compound (complex (Ag (NH3)
n +) solution);
Under stirring condition, in turbid solution, slowly add excessive hydrazine hydrate solution,, form the even composite powder of the simple substance nanometer Ag that depends on Bi-0.1Cu powder and Sn-10Sb-0.5Ge powder surface the complex compound reduction;
Pour turbid solution into filter cloth and filter, and the filter cake after will filtering evenly completes with nitrogen and dry, carry out air-dry processing;
Take by weighing the 110g scaling powder, and put into air-dry (Bi-0.1Cu)+1% (Sn-10Sb-0.5Ge)+12%Ag solder powder, fully stir, make it into uniform fluid, promptly prepared the high-temp leadless soldering paste.Soldering paste is poured in the solder paste cartridge, put into refrigerator and be in store for.
Table 1 is that silver-colored nanometer reinforced bismuth base lead-free high-temperature solder compares with the contrast solder performance among the embodiment.
Table 2 is the component and the fusing point of the nanometer reinforced bismuth base lead-free high-temperature solder of representative instance of the present invention.
Fig. 3 sprawls comparison diagram for the solder joint of typical nanometer reinforced bismuth base lead-free high-temperature solder and BiAg2.5, SnPb90 and SnPb95 solder among the present invention, and 12 is the Bi-2.5Ag solder joint among the figure; 13 are Bi+2.5%Ag solder joint of the present invention; 14 is the Sn-90Pb solder joint; 15 is the Sn-95Pb solder joint; 16 is the Bi-2.5Ag solder joint; 17 are Bi+2.5%Ag solder joint of the present invention; 18 is the Sn-90Pb solder joint; 19 is the Sn-95Pb solder joint.Figure a is that Cu substrate, figure b are the Ni substrate, and it is on 99.9% the copper plate and pure Ni plate that experimentation is placed on purity according to Japanese JIS standard respectively with the various soldering paste of 0.22+0.001g, is incubated 90s on 350 ℃ of thermostatic electrothermal plates, takes with digital camera behind the air cooling.Before the experiment, copper coin and the sand paper fine grinding of nickel plate are cleaned with acetone and are removed greasy dirt, and dip 5s and remove surface film oxide in 10%HCl, fully wash with deionized water again.From figure as can be seen: no matter on Cu substrate and Ni substrate, it is a little that the spreadability of BiAg2.5 solder is compared nanometer reinforced bismuth base composite powder of the present invention (Bi+2.5%Ag) the scolder inequality of same component, and the spreadability of embodiments of the invention (Bi+2.5%Ag) lead-free high-temperature solder can be compared with SnPb95 with SnPb90, and solder joint appearance rounding, full.This explanation nanometer reinforced bismuth base lead-free high-temperature solder of the present invention has better solderability than the solder with component, thus the generation of defectives such as short circuit can reduce the welding of Bi base lead-free high-temperature solder time the, hole, and can promote bond strength.
Nanometer reinforced bismuth base lead-free high-temperature solder and contrast solder performance among table 1 embodiment
Typical nanometer reinforced bismuth base lead-free high-temperature solder component of table 2 and fusing point
| Sample number into spectrum | Alloy compositions | Fusing point ℃ |
| 1# | 98％Bi+2.0％Ag | ～270 |
| 2# | 97.5％Bi+2.5％Ag | ～270 |
| 3# | 88％Bi+12％Ag | 270～360 |
| 4# | 90％(Bi-5.0Sb)+10％Ag | 270～340 |
| 5# | 97.5％(Bi-10Sb)+2.5％Ag | 270～320 |
| 6# | 98％(Bi-20Sb)+2.0％Ag | 300～380 |
| 7# | 95％(Bi-10Sb-0.5Sn)+5％Ag | 270～330 |
| 8# | 95％(Bi-10Sb-0.5Zn)+5％Ag | 270～330 |
| 9# | 90％(Bi-10Sb-1.0In)+10％Ag | 270～350 |
| 10# | 95％(Bi-10Sb-0.5Cu)+5％Ag | 270～330 |
| 11# | 98％(Bi-10Sb-0.1Au)+2％Ag | 270～320 |
| 12# | 97.5％(Bi-5Sb-0.2Zn-0.1Ge)+2.5％Ag | 280～300 |
| 13# | 85％(Bi-0.1Ge)+10％Sb+5％Ag | 270～380 |
| 14# | 92％(Bi-0.1Ge)+5％(Sb-10Sn)+3％Ag | 270～380 |
| 15# | 95％Bi+2.5％(Sb-5Ni)+2.5％Ag | 270～380 |
| 16# | 96％Bi+1％(Sb-95Sn)+3％Ag | 270～360 |
| 17# | (Bi-0.1Cu)+1％(Sn-10Sb-0.5Ge)+12％Ag | 270～380 |
Claims (9)
1. nanometer reinforced bismuth base lead-free high-temperature solder is characterized in that: comprise the alloyed powder of the mixed powder of silver-colored nano powder and bismuth meal or bismuth, antimony or bismuth, antimony, wherein silver-colored nano powder accounts for 2～12wt%; The alloyed powder of the mixed powder of described silver-colored nano powder and bismuth meal or bismuth, antimony or bismuth, antimony forms even composite powder.
2. nanometer reinforced bismuth base lead-free high-temperature solder according to claim 1 is characterized in that: in the alloyed powder of the mixed powder of described bismuth, antimony or bismuth, antimony, and bi content 〉=80wt%, antimony content≤20wt%.
3. nanometer reinforced bismuth base lead-free high-temperature solder according to claim 1 and 2 is characterized in that: also comprise gross weight and be no more than in 1% Sn, In, Cu, Zn, Ge, Au or the Ni element one or more.
4. the preparation method of a nanometer reinforced bismuth base lead-free high-temperature solder comprises the following steps:
(1) takes by weighing the bismuthino powder, can adopt any known powder-making techniques such as Mechanical Crushing or medium atomization;
(2) the even importing of quantitative bismuthino powder had in the liquor argenti nitratis ophthalmicus of agitating device, make silver contained in the liquor argenti nitratis ophthalmicus be 2～12% of silver and bismuthino powder gross weight, constantly stirring obtains uniform turbid solution;
(3) take by weighing relative silver nitrate excess of ammonia water or other can with the material of silver-colored complexing, and it is added in the turbid solution of step (2) gained slowly, make silver ion be completed into complex compound or complex;
(4),, form the even composite powder of nano-silver powder and bismuthino powder with the complex compound reduction constantly slowly adding reducing agent under the stirring condition;
(5) filter, the gained filter cake is dried, dries up or is dried under guard mode, promptly gets nanometer reinforced bismuth base lead-free high-temperature solder.
5. the preparation method of nanometer reinforced bismuth base lead-free high-temperature solder according to claim 4 is characterized in that: described bismuthino powder packets contains the alloyed powder of the mixed powder of bismuth meal or bismuth, antimony or bismuth, antimony.
6. the preparation method of nanometer reinforced bismuth base lead-free high-temperature solder according to claim 5 is characterized in that: in the alloyed powder of the mixed powder of described bismuth, antimony or bismuth, antimony, and bi content 〉=80wt%, antimony content≤20wt%.
7. the preparation method of nanometer reinforced bismuth base lead-free high-temperature solder according to claim 6 is characterized in that: also comprise gross weight in the described bismuthino powder and be no more than in 1% Sn, In, Cu, Zn, Ge, Au or the Ni element one or more.
8. the preparation method of nanometer reinforced bismuth base lead-free high-temperature solder according to claim 4, it is characterized in that: the reducing agent described in the step (4) is hydrazine hydrate, glucose or formaldehyde.
9. the preparation method of nanometer reinforced bismuth base lead-free high-temperature solder according to claim 4 is characterized in that: in the step (5), the oven dry under vacuum state or hydrogen, inert gas shielding state of gained filter cake, dry up or dry.
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| KR101073440B1 (en) * | 2011-05-16 | 2011-10-17 | 강수향 | Card manufactured by priming powder and method for manufacturing thereof |
| CN105935845B (en) * | 2016-06-08 | 2018-06-19 | 上海无线电设备研究所 | A kind of bismuth telluride reinforced by nanoparticles tin-silver-copper solder and its application method |
| CN106392366B (en) * | 2016-12-02 | 2019-07-19 | 北京康普锡威科技有限公司 | A kind of BiSbAg system high temperature lead-free solder and preparation method thereof |
| KR102187085B1 (en) * | 2019-01-24 | 2020-12-04 | 주식회사 경동엠텍 | lead-free solder composition for high-temperature and vibrational circumstance and manufacturing method thereof |
| CN110102934A (en) * | 2019-04-30 | 2019-08-09 | 周轻轩 | A kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material |
| CN115635212B (en) * | 2022-12-26 | 2023-03-10 | 广州汉源微电子封装材料有限公司 | Silver soldering paste and preparation method and application thereof |
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