CN102909362B - Sub-micron solder alloy powder and preparation method thereof - Google Patents
Sub-micron solder alloy powder and preparation method thereof Download PDFInfo
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- CN102909362B CN102909362B CN201210389898.7A CN201210389898A CN102909362B CN 102909362 B CN102909362 B CN 102909362B CN 201210389898 A CN201210389898 A CN 201210389898A CN 102909362 B CN102909362 B CN 102909362B
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- 239000000843 powder Substances 0.000 title claims abstract description 72
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 41
- 239000000956 alloy Substances 0.000 title claims abstract description 41
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 46
- 229910052709 silver Inorganic materials 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000005476 soldering Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 239000010949 copper Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000010944 silver (metal) Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910002065 alloy metal Inorganic materials 0.000 claims description 4
- 239000010946 fine silver Substances 0.000 claims description 4
- 229910017944 Ag—Cu Inorganic materials 0.000 claims description 3
- 229910016331 Bi—Ag Inorganic materials 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 239000003595 mist Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004781 supercooling Methods 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- -1 when feeding intake Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000008020 evaporation Effects 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 238000009835 boiling Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000005275 alloying Methods 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000004100 electronic packaging Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910000521 B alloy Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 230000007306 turnover Effects 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010027439 Metal poisoning Diseases 0.000 description 1
- 229910020816 Sn Pb Inorganic materials 0.000 description 1
- 229910020922 Sn-Pb Inorganic materials 0.000 description 1
- 229910008783 Sn—Pb Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- YCKOAAUKSGOOJH-UHFFFAOYSA-N copper silver Chemical compound [Cu].[Ag].[Ag] YCKOAAUKSGOOJH-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006023 eutectic alloy Substances 0.000 description 1
- 235000021050 feed intake Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 208000008127 lead poisoning Diseases 0.000 description 1
- 235000021180 meal component Nutrition 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Abstract
The present invention discloses a kind of sub-micron solder alloy powder, and this alloyed powder is made up of each metallic element of following percentage by weight: Sn:94.9 ~ 99.8%, Ag:0.1 ~ 4.2%, Cu:0.1 ~ 0.9%; And the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns; Or this alloyed powder is made up of each metallic element of following percentage by weight: Sn:25.8 ~ 74.9%, Bi:25 ~ 70%, Ag:0.1 ~ 4.2%, and the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns.A kind of preparation method of above-mentioned alloyed powder is also disclosed.The present invention has fine size, narrowly distributing, advantage that oxygen content is low.
Description
Technical field
The present invention relates to solder powder technical field used for electronic packaging, be specifically related to a kind of submicron order (1.0 ~ 3.0 microns) soldering alloy powder and preparation method thereof.
Background technology
Sn-Pb series solder powder has the application of decades in Electronic Packaging, and the fusing point of its eutectic alloy is low, cheap, and properties is excellent, is widely used.But, along with electronic product more New Alternate speed accelerate, leaded material in many scrap can not reclaim completely, cause the severe contamination of environment, when lead is entered in human body by food chain, just easily enter blood and accumulate, causing lead poisoning, irreversible harm is caused to human body.Therefore, the development & application of lead-free solder becomes inevitable.
At present, most widely used Pb-free coating glass putty, general is all obtain by spray-on process, the solder powder that spray-on process is obtained, and particle diameter distributes in the width range of 1-100 micron (μm), and, wherein the product of particle diameter below 3 μm accounts for insufficient total amount 10%, and the solder(ing) paste that the solder powder produced in this way is made, fine circuitry can not be formed and effectively fill tiny pin hole, therefore, the requirement that electronic product becomes more meticulous can not be met.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art, the sub-micron solder alloy powder that a kind of fine size, narrowly distributing, oxygen content are low is provided.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of sub-micron solder alloy powder, and this alloyed powder is made up of each metallic element of following percentage by weight: Sn:94.9 ~ 99.8%, Ag:0.1 ~ 4.2%, Cu:0.1 ~ 0.9%; And the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns;
Or
This alloyed powder is made up of each metallic element of following percentage by weight: Sn:25.8 ~ 74.9%, Bi:25 ~ 70%, Ag:0.1 ~ 4.2%, and the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns.
Above-mentioned sub-micron solder alloy powder is by the standby soldering alloy powder of physical vapor legal system, and the shape of particle of alloyed powder is spherical or class is spherical.
The present invention also provides a kind of granularity narrow respectively, and particle diameter is thin, effectively can meet the preparation method of the above-mentioned sub-micron solder alloy powder of the requirement that electronic product becomes more meticulous: preparation process comprises:
(1) the soldering alloy metal (commercially available prod) of formula rate and simple metal are put into the crucible of high-temperature metal evaporimeter as raw material, after the air-tightness of inspection machine is qualified, by the plasma transferred arc that produces between crucible and plasma torch as heating source, above-mentioned raw material are fused into metal liquid;
(2) to continuous feed in crucible, feed rate is 5.5 ~ 20Kg/h, and the pressure of the working gas of plasma transferred arc is 0.3 ~ 0.8MPa, and the voltage of plasma transferred arc is 60 ~ 200V, under the effect of plasma transferred arc, metal liquid is heated to form metal mixed steam;
(3) the metal mixed steam be evaporated enters particle controller, and metal mixed steam is cooled by the inert gas entering particle controller simultaneously, disperse in the middle of gas, collision, forms the drop of nanometer or submicron order, and being cooled subsequently is frozen into alloyed powder;
(4) alloyed powder of step (3) gained is by being collected after gas-solid separator under gas carries, and obtains sub-micron solder alloy powder end, and solder alloy powder is collected in solder powder collector; Gas is through the use or emptying of supercooling Posterior circle;
The device systems that above-mentioned preparation process relates to, its internal system pressure is 0.05 ~ 0.2MPa.
As preferably, the soldering alloy raw metal described in step (1) is granular, little bulk, segment shape etc., and composition is identical or close with the target soldering alloy meal component that will produce.
Simple metal described in above-mentioned steps of the present invention (1) is namely at preparation Sn-Ag-Cu solder powder (Sn:94.9 ~ 99.8%, Ag:0.1 ~ 4.2%, Cu:0.1 ~ 0.9%; And the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns) time, when feeding intake, in crucible, drop into the fine copper of soldering alloy gold raw material weight 0.5 ~ 2.0%; When preparation Sn-Bi-Ag solder powder (Sn:25.8 ~ 74.9%, Bi:25 ~ 70%, Ag:0.1 ~ 4.2%, and the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns), add the soldering alloy gold fine silver of raw material weight 0.1 ~ 2.0% and the pure tin of 5 ~ 30%.
As preferably, the working gas of the plasma transferred arc described in step (2) is one or more mist of argon gas, nitrogen, hydrogen, ammonia, helium, is preferably: the mist of nitrogen or nitrogen and hydrogen.
The device systems that the whole process of preparation method of the present invention relates to, the pressure of this internal system (from step (1) just control) be preferably 0.08 ~ 0.15MPa.
High-temperature metal evaporimeter of the present invention is the high-temperature metal evaporimeter in patent 201110119245.2, and this evaporation structure is as follows: comprise the crucible for holding metal derby and the metal liquid after melting, plasma transferred arc torch, plasma transferred arc, graphite, power supply and wire; The air inlet pipe that supplied gas enters is provided with in described plasma transferred arc torch; The plasma transferred arc lower end that described plasma transferred arc torch produces connects with the metal bath surface in crucible; Described graphite is located at the bottom of crucible; Described plasma transferred arc torch, plasma transferred arc, crucible, graphite, form electric loop between power supply and wire, the top of described plasma transferred arc is provided with the feed pipe added for raw metal.
Production process of the present invention can also be specifically described as: the simple metal of the higher contained in the soldering alloy metal (commercially available prod) of corresponding formula components and this alloy is put into high-temperature metal evaporimeter, the air-tightness of inspection machine is qualified rear (air tight),-85KPa or lower is vacuumized to system, then, be filled with high pure nitrogen again to rinse system, make intrasystem atmosphere be inertia, plasma transferred arc is as heating source, heating soldering alloy and simple metal raw material are to molten state, open charger, reinforced in crucible with given pace, under plasma transferred arc continuous action, metal mixed steam is evaporated, be transported in particle controller by gas transmission pipeline, in particle controller, metal mixed steam is cooled by inert gas, formed by dozens or even hundreds of former molecular atomic thin atom family, the disperse in the middle of gas of small atom family, collision, grow up into the drop of nanometer or submicron order, be cooled subsequently and be frozen into alloyed powder, because alloyed powder is collided by thousands of small atom families to grow up, so the composition of the soldering alloy powder of gained is uniform, gas-solid mixing gas is after gas-solid separator, alloyed powder is collected, gas be cooled Posterior circle use.
Because the boiling point of each metallic element of component alloy is different, the speed of evaporation is also different, when several metallic element is together by heating evaporation, low-boiling elements vaporization speed is fast, the evaporation rate that boiling point is high is slow, in order to the component requirements that the composition of the mixed vapour be evaporated can be made to meet soldering alloy powder in final products, except adding as except the soldering alloy metal of raw-material commercially available formula rate using certain speed, in crucible, also suitably need add the simple metal of a certain amount of higher element, such as when producing Sn-Ag-Cu solder powder, when needing to feed intake, drop into the fine copper of the weighing scale 0.5 ~ 2.0% of soldering alloy in crucible in crucible, when producing Sn-Bi-Ag solder powder, add with the fine silver of weighing scale 0.1 ~ 2.0% of soldering alloy in crucible and the pure tin of 5 ~ 30%, to ensure final evaporation, the alloyed powder composition cooled down meets final products requirement.In the incipient following period of time of production, the composition of the metal liquid in crucible constantly changes, high boiling metal element content is more and more higher, lower boiling metal element content reduces, by adjustment feeding quantity, after the evaporation of certain hour, feeding quantity and evaporation capacity reach balance, the amount of each element namely entering crucible and be evaporated from crucible reaches balance, alloying component in crucible is stabilized to some values, system reaches balance, and the composition of alloyed powder is also stabilized to predetermined value, and production can be produced down continually and steadily.
Advantage of the present invention and beneficial effect:
1. sub-micron solder alloy powder of the present invention, its average grain diameter is 1.0 ~ 3.0 microns, pattern can be full spherical, the mobility of powder is fine, and therefore, particle diameter is narrow respectively, be applied to Electronic Packaging field, fine circuitry can be formed and effectively fill tiny pin hole, therefore, the requirement that electronic product becomes more meticulous can be met.
2. the particle diameter of solder powder can regulate between 1.0 ~ 5.0 microns, narrow particle size distribution.
3. sub-micron solder alloy powder of the present invention, adopt physical vapor legal system standby, preparation technology is simple, start sintering temperature low, sintering velocity is fast, is easy to operation, and all metal alloy powder effectively can be formed the sub-micron solder alloy powder that average grain diameter is 1.0 ~ 3.0 microns.
Accompanying drawing illustrates:
Fig. 1 sub-micron solder alloy powder preparation technology of the present invention flow chart.
Sn-3.5Ag-0.9Cu scanning electron microscope (SEM) photograph prepared by Fig. 2 embodiment 1.
Sn-57Bi-1.0Ag scanning electron microscope (SEM) photograph prepared by Fig. 3 embodiment 2.
Detailed description of the invention
Elaborate to embodiments of the invention below, but the present invention is not limited to following examples, any amendment in scope, all thinks and falls within the scope of protection of the present invention.
Embodiment 1:
Commercially available Sn-3.5Ag-0.9Cu B alloy wire is thrust into segment, this alloy section is put into crucible as raw material, weight is 15Kg, is added in crucible by the fine copper of 0.25Kg in addition.Nitrogen is as plasma transferred arc working gas, and pressure is 0.5MPa.The voltage of plasma transferred arc is 140V, with plasma transferred arc as heating source, alloy solder stick is heated to molten state rapidly, and open charger and in crucible, add alloy segment with the speed of 5.0Kg/h, system pressure is 110KPa.Through the composition adjustment of 2 hours, in crucible, the turnover of material reached balance.Metal vapors takes in particle controller by the nitrogen as refrigerating gas, metal vapors is gathered cold less than 200 DEG C, becomes solid state powder.Alloyed powder is collected after gas-solid separator.Gas be cooled Posterior circle use.
The solder powder alloying component produced is silver content: 3.5%, and copper content is: 0.9%.Oxygen content is: the general tin of 0.08%(calculates with surplus, and that is, be exactly tin except copper silver, an important quality index of solder powder is oxygen content in addition, so also write oxygen content here).If the too high oxygen level in solder powder, by causing the wettability of solder(ing) paste to decline, affect welding effect.Fusing point is: 217 DEG C.
Domain size distribution is for shown in table 1:
Table 1
Pattern: as shown in Figure 2.
Embodiment 2:
Sn-57Bi-1.0Ag B alloy wire is thrust into segment, this alloy section is put into crucible as raw material, weight is 20Kg.Add the fine silver of 0.3Kg and the pure tin of 4.4Kg simultaneously.Nitrogen is as plasma working gas, and pressure is 0.5MPa.Voltage is 150V, with plasma transferred arc as heating source, alloy solder stick is heated to molten state rapidly, opens charger and in crucible, add alloy segment with the speed of 6.0Kg/h, through the composition adjustment of 2.5 hours, the material of turnover crucible reached balance.Metal vapors takes in particle controller by the nitrogen as refrigerating gas, metal vapors is gathered cold less than 200 DEG C, becomes solid state powder.Alloyed powder is collected after gas-solid separator.Gas be cooled Posterior circle use.
The solder powder alloying component produced is silver content: 1.0%, and bi content is: 57.1%.Oxygen content is: 0.10%.Fusing point is: 217 DEG C.
Oxygen content is: 0.1%
Fusing point is: 140 DEG C.
Domain size distribution is for shown in table 2:
Table 2
Pattern as shown in Figure 3.
Claims (3)
1. a preparation method for sub-micron solder alloy powder, is characterized in that: preparation process comprises:
(1) the soldering alloy metal of formula rate and simple metal are put into the crucible of high-temperature metal evaporimeter, after the air-tightness of inspection machine is qualified, by the plasma transferred arc that produces between crucible and plasma torch as heating source, raw material are fused into metal liquid; Namely simple metal described in step (1) when preparing Sn-Ag-Cu solder powder, when feeding intake, drops into the fine copper of soldering alloy raw metal weight 0.5 ~ 2.0% in crucible; When preparing Sn-Bi-Ag solder powder, add the fine silver of soldering alloy raw metal weight 0.1 ~ 2.0% and the pure tin of 5 ~ 30%;
(2) start to continuous feed in crucible, feed rate is 5.5 ~ 20Kg/h, and the pressure of the working gas of plasma transferred arc is 0.3 ~ 0.8MPa, and the voltage of plasma transferred arc is 60 ~ 200V, under the effect of plasma transferred arc, metal liquid is heated to form metal mixed steam;
(3) the metal mixed steam be evaporated enters particle controller, and high-temperature metal mixed vapour is cooled by the inert gas entering particle controller simultaneously, disperse in the middle of gas, collision, forms drop, and being cooled subsequently is frozen into alloyed powder;
The alloyed powder of step (3) gained by being collected after gas-solid separator, obtains sub-micron solder alloy powder end under gas carries; Gas is through the use or emptying of supercooling Posterior circle;
The device systems that above-mentioned preparation process relates to, its internal system pressure is 0.05 ~ 0.2MPa;
Above-mentioned sub-micron solder alloy powder, this alloyed powder is made up of each metallic element of following percentage by weight: Sn:94.9 ~ 99.8%, Ag:0.1 ~ 4.2%, Cu:0.1 ~ 0.9%; And the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns;
Or
This alloyed powder is made up of each metallic element of following percentage by weight: Sn:25.8 ~ 74.9%, Bi:25 ~ 70%, Ag:0.1 ~ 4.2%, and the average grain diameter of alloyed powder is 1.0 ~ 3.0 microns;
Described sub-micron solder alloy powder is by the standby soldering alloy powder of physical vapor legal system, and the shape of particle of alloyed powder is spherical.
2. the preparation method of sub-micron solder alloy powder according to claim 1, is characterized in that: the plasma working gas described in step (1) is one or more mist of argon gas, nitrogen, hydrogen, ammonia, helium.
3. the preparation method of sub-micron solder alloy powder according to claim 1, is characterized in that: described system pressure is 0.08 ~ 0.15MPa.
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| CN114985750B (en) * | 2022-06-01 | 2024-02-13 | 深圳市百柔新材料技术有限公司 | Preparation method of tin-silver-copper alloy nano powder, tin-silver-copper nano alloy low-temperature slurry, preparation method and application thereof |
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