CN101088665B - Nanometer silver-silver slurry and its preparation process - Google Patents
Nanometer silver-silver slurry and its preparation process Download PDFInfo
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- CN101088665B CN101088665B CN2006100854464A CN200610085446A CN101088665B CN 101088665 B CN101088665 B CN 101088665B CN 2006100854464 A CN2006100854464 A CN 2006100854464A CN 200610085446 A CN200610085446 A CN 200610085446A CN 101088665 B CN101088665 B CN 101088665B
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Abstract
The present invention relates to one kind of nanometer silver-silver oxide slurry and is preparation process. The 20-500 nm silver-silver oxide slurry is prepared through mixing nanometer metal oxide in 0-10 % into silver-base slurry, and further nanometer fining. The nanometer silver-silver oxide slurry has effectively raised pulse resistance and improved fusing performance.
Description
Technical field
The present invention relates to a kind of electrocondution slurry, specifically relate to a kind of preparation method who is used to produce nanometer silver-silver slurry and this slurry of fuse fuse.
Background technology
Adopting silver-based paste thick film screen printing technology to make fuse is one of important production technology of electronic devices and components industry.Particle is the above particle size of micron in traditional silver-based paste.The fuse class components and parts that use traditional silver-based paste to produce by the thick film screen printing technology, more weak aspect anti-pulse ability, under rated current, can not fuse accurately and reliably.All the time, improve the anti-pulse ability of fusible link and under rated current accurately and reliably the ability of fusing be the focus of research of technique in the industry; The main direction of R﹠D work before this is the shape of fusible link for a change, perhaps improves radiating condition etc.; But these methods are improved DeGrain.
Nanometer technology is high speed development in the world, and in recent years, it is used and has been penetrated into all trades and professions.The technology of preparing of Nano Silver, nano phase ag_2 o and various nano-metal-oxides is very ripe.Do not changing under the member condition, the adjusting by preparation technology parameter obtains having different-grain diameter, the nano material of distributional pattern and surface topography, can realize the very big improvement of the every physics of material, chemical property.The doping of nano material is because its specific surface is big, and the scattering and permeating ability is strong in doping system, and the doping composition can be given full play to effectiveness, thereby " nano material is trace doped " this strong nano modification technological means is provided.Chinese patent 03113552.8 discloses a kind of low content nano-silver conductive slurry, but this slurry be not with solve anti-pulse and accurately fusing problem, therefore, having the anti-pulse and the slurry that further can fuse accurately and reliably under rated current remains to be developed.
Summary of the invention
The purpose of this invention is to provide a kind of nanometer silver-silver slurry that is used to produce the fuse fuse, this slurry can improve anti-pulse ability effectively, and improves fusing performance.
The said nanometer silver-silver slurry that is used to produce the fuse fuse of the present invention, make by the following method: the 0-10% that in silver-based paste, mixes (weight) nano-metal-oxide, then, utilize conventional nanometer thinning method, make the nanometer silver-silver slurry of 20-500nm.
Ratio in this specification is weight ratio except that special instruction is arranged.
Silver-based paste described in the present invention is meant that with silver-silver oxide, solvent adhesive be the electrocondution slurry of main component.Can adopt market existing, as mine, Sumitomo company thick film conductor paste C-4425, C-4420, C4101S, S-8200B, and the like product of Du Pont, clear honor, Tanaka's noble metal company; Also can prepare by existing method with silver-silver oxide and solvent adhesive.
Based on conduction and the operating chacteristics research to nanometer silver-silver: promptly the particle diameter of nanometer silver-silver, distribution and surface topography are to the influence of its conduction with fusing performance, present technique can be passed through the different micro-structurals of preparation, or the nanometer silver-silver of the micro-nano-metal-oxide that mixes, obtain the slurry of different operating chacteristicses and anti-pulse ability.In the present invention, when the ratio of dopen Nano metal oxide was 0%, the slurry that makes just can improve anti-pulse ability, and improve fusing performance.
Further, the slurry of the nano-metal-oxide that mixed can correspondingly improve anti-pulse ability better, improves fusing performance.Nano-metal-oxide described in the present invention, recommending but being not limited to is in nano oxidized potassium, sodium oxide molybdena, bismuth oxide, tin oxide, zinc oxide, nickel oxide and the manganese oxide one or more; The preferred 10-100nm of particle diameter of wherein nano oxidized potassium, sodium oxide molybdena and bismuth oxide, 50nm preferably, dopen Nano potassium oxide, sodium oxide molybdena or bismuth oxide can further improve the performance accurately and reliably of fusing; The preferred 10-100nm of the particle diameter of nano tin dioxide, zinc oxide, manganese oxide and nickel oxide wherein, 40nm preferably, dopen Nano tin oxide, zinc oxide or nickel oxide then can anti-better pulse performances.The preferred 1%-10% of nano-metal-oxide doping ratio, preferably 5-7% among the present invention.
Existing conventional nanometer thinning method all can be used for the present invention, specifically can be but is not limited to the method for giving: wet ball grinding method, Ultrasonic Pulverization method, microwave method.The preferred wet ball grinding method of the present invention.Specifically be, in high speed ball mill, ground 0.5-50 hour, make slurry of the present invention.More particularly, the high speed ball mill service intermittent is preferably worked and was stopped in 15 minutes 10 minutes to avoid temperature too high, and rotating speed 500-1200 rpm, preferred 800 rpms.Reacting under the hot conditions when preventing the high speed ball milling causes slurry rotten, vacuumizes and charge into protective gas before the ball grinder work, preferred argon gas.Can also add dispersion stabilizer as required, as polyesters, the polyester salt, polyurethanes prevents to reunite as BYK104S etc., and preferred dispersion stabilizer needs to select according to concrete raw material; Add surfactant such as NP9, NP10, the surface topography of modulation nano particles such as OP15 also promotes the nano particle self assembly colloid environment under, preferred activating agent also needs according to specifically raw material selection.The consumption of dispersion stabilizer and activating agent and kind are that those skilled in the art know or energy is determined according to existing existing art.
The process ball milling can obtain the nanometer silver-silver slurry of particle diameter 20-500nm, under the immovable situation of other conditions, reduces with particle, and it is big that the resistive fuse rate becomes, and anti-pulse ability strengthens.Nanometer silver-silver particle monodispersity is big more in the slurry, surface topography is consistent more, silver in the slurry-silver oxide nano particle self assembly situation is perfect more, it is evenly fine and close to constitute three-dimensional conductive network in the epoxy resin colloid system, under the immovable situation of other conditions, it is more little that the self assembly situation is improved the resistive fuse rate more, and anti-pulse ability also is enhanced.
Another object of the present invention provides the preparation method of described nanometer silver-silver slurry.
The preparation method of described nanometer silver-silver slurry is: doping 0-10% nano-metal-oxide in silver-based paste, then, utilize conventional nanometer thinning method, and make the nanometer silver-silver slurry of 20-500nm.
In above-mentioned preparation process, nano-metal-oxide can mix after the nanometer refinement at silver-based paste again and mix, and can make the said nanometer silver-silver slurry of the present invention equally.
Use nm of gold, nanometer platinum to replace nanometer silver-silver also can realize the anti-pulse of slurry and operating chacteristics accurately and reliably, but cost is higher.
The present invention is a raw material with existing silver-based paste, and the nanometer silver-silver slurry of preparation can improve anti-pulse ability effectively, and improves fusing performance.The slurry of the present invention of nano-metal-oxide has particularly mixed, because above-mentioned nano-metal-oxide as trace doped material, particle diameter is 10m-100nm, size is less than the average grain diameter of its doped system, the activity that its skin effect and quantum effect increase can effectively influence the energy conversion process of original system under high temperature, the pulse current condition, thus the performance that further improves anti-pulse and fuse accurately and reliably.
Description of drawings
Fig. 1 is the nanometer silver-silver slurry TEM photo after ultrasonic dispersion in alcohol solvent.The transmission electron microscope model is JEM-200CX, accelerating potential 200KV.
The specific embodiment
The present invention is further described below in conjunction with drawings and Examples.
Employed in the present invention term unless other explanation is arranged, generally has the implication of those of ordinary skills' common sense.
Below in conjunction with specific embodiment, and comparable data is described the present invention in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit the scope of the invention by any way.
In following embodiment, various processes of Xiang Ximiaoshuing and method are not conventional methods as known in the art.The source of agents useful for same, trade name and be necessary to list its constituent person indicate when occurring first that all used thereafter identical reagent if no special instructions, and is all identical with the content of indicating first.
Embodiment 1
With mine, Sumitomo thick film conductor paste C-4420 is raw material, 1200 rpms of drum'ss speed of rotation, and the 15 minutes front yards 10 minutes of working vacuumize and charge into argon gas before the ball grinder work.Add macromolecule dispersing agent BYK104S, add surfactant OP15.Agate ball, ratio of grinding media to material 6: 1 was ground 5 hours, and this slurry average grain diameter 120nm makes fuse through the thick film screen printing technology.
Anti-pulse test
In experimental temperature: 23 degrees centigrade; Running current: 2A; Do anti-pulse test under the condition of pulse voltage: 15V, the result shown in table 1, table 2,2 times, 4 times under the pulse current of normal current, improve 10 times or more than former slurry its normal working hours.
Table 1. is 2 times of anti-pulse tests under the pulse current of normal current
| Normal current load resistance value (m Ω) | Electrical current (being equivalent to normal current %) | Former slurry C-4420 sample fusing time (ms) | Slurry sample fusing time of the present invention (ms) |
| 72 | 200％ | 1.8 | 62 |
| 73 | 200％ | 2.2 | 48 |
| 75 | 200％ | 2.4 | 72 |
| 76 | 200％ | 1.6 | 61 |
| 77 | 200％ | 2.1 | 44 |
| 78 | 200％ | 2.0 | 65 |
Table 2. is 4 times of anti-pulse tests under the pulse current of normal current
| Normal current load resistance value (m Ω) | Electrical current (being equivalent to normal current %) | Former slurry C-4420 sample fusing time (ms) | Slurry sample fusing time of the present invention (ms) |
| 72 | 400％ | 0.53 | 47 |
| 73 | 400％ | 0.40 | 32 |
| 75 | 400％ | 0.55 | 63 |
| 76 | 400％ | 0.38 | 38 |
| 77 | 400％ | 0.57 | 45 |
| 78 | 400％ | 0.42 | 60 |
The fusing performance test
(20A ,～ns) fusing situation, (adding 32V fusing voltage) under the blowout current condition.The former slurry C-4420 ratio that do not fuse: 15.0%～20.0%, the slurry of the present invention ratio that do not fuse: less than 10.0%.
Embodiment 2
Thick film conductor paste C-4425 is raw material with the mine, Sumitomo, the Na of the 5% average grain diameter 50nm that mixes
2O, 800 rpms of drum'ss speed of rotation are worked and were stopped 10 minutes in 15 minutes, vacuumize and charge into argon gas before the ball grinder work.Add macromolecule dispersing agent BYK104S, add surfactant NP10.Agate ball, ratio of grinding media to material 6: 1 was ground 2 hours, promptly obtained average grain diameter 280nm nanometer silver-silver slurry.
Test condition is with embodiment 1, slurry of the present invention as a result 2 times, 4 times under the pulse current of normal current, its impulsive condition improves 5 times than former slurry C-4425 following normal working hours; Rated current fuses fully.(fuse 15.0%～20.0% that former slurry C-4425 printing obtains can not accurately fuse in rated current);
Embodiment 3
With mine, Sumitomo thick film conductor paste C-4420 is raw material, 1200 rpms of drum'ss speed of rotation, and the 15 minutes front yards 10 minutes of working vacuumize and charge into argon gas before the ball grinder work.Add macromolecule dispersing agent BYK104S, add surfactant OP15.Agate ball, ratio of grinding media to material 6: 1 was ground 5 hours.This slurry average grain diameter 120nm makes fuse through the thick film screen printing technology.
Test condition is with embodiment 1, slurry of the present invention as a result 2 times, 4 times under the pulse current of normal current, its impulsive condition improves 5 times than former slurry C-4420 following normal working hours; Specified instantaneous large-current is not exclusively fusing 10% down, is better than former slurry C-4420.
Embodiment 4
Thick film conductor paste C-4425 is raw material with the mine, Sumitomo, and the bismuth oxide of the 7% average grain diameter 50nm that mixes is nanocrystalline, and 800 rpms of drum'ss speed of rotation are worked and stopped 10 minutes in 15 minutes, vacuumizes and charge into argon gas before the ball grinder charging back work.Add macromolecule dispersing agent BYK104S (0.5%), add surfactant NP10 (0.3%).Ball milling uses agate ball, and ratio of grinding media to material 6: 1 was ground 2 hours.Promptly obtain average grain diameter 280nm nanometer silver-silver slurry.
Test condition is with embodiment 1, slurry of the present invention as a result 2 times, 4 times under the pulse current of normal current, its impulsive condition improves 5 times than former slurry C-4425 following normal working hours.Specified instantaneous large-current is fusing 2% down not exclusively, significantly is better than former slurry (the C-4425 ratio that do not fuse: 15.0%～20.0%).
Embodiment 5
Thick film conductor paste C-4425 is raw material with the mine, Sumitomo, and the bismuth oxide of the 10% average grain diameter 10nm that mixes is nanocrystalline, and 500 rpms of drum'ss speed of rotation are worked and stopped 10 minutes in 10 minutes, vacuumizes and charge into argon gas before the ball grinder charging back work.Do not add dispersant, surfactant.Ball milling uses agate ball, and ratio of grinding media to material 6: 1 was ground 30 minutes.Obtain average grain diameter 500nm nanometer silver-silver slurry.
Test condition is with embodiment 1, slurry of the present invention as a result at 2 times, 4 times under the pulse current of normal current, its impulsive condition improves 5 times than former slurry C-4425 following normal working hours, and specified instantaneous large-current is not exclusively fusing 3% down, also improves a lot than former slurry.
Embodiment 6
Thick film conductor paste C-4425 is raw material with the mine, Sumitomo, and the bismuth oxide of the 1% average grain diameter 100nm that mixes is nanocrystalline, and 500 rpms of drum'ss speed of rotation are worked and stopped 10 minutes in 10 minutes, vacuumizes and charge into argon gas before the ball grinder charging back work.Do not add dispersant, surfactant.Ball milling uses agate ball, and ratio of grinding media to material 6: 1 was ground 30 minutes.Obtain average grain diameter 500nm nanometer silver-silver slurry.
Test condition is with embodiment 1, slurry of the present invention as a result 2 times, 4 times under the pulse current of normal current, its impulsive condition improves 5 times than former slurry C-4425 following normal working hours, specified instantaneous large-current is not exclusively fusing 5% down, is better than former slurry C-4425.
Embodiment 7
With mine, Sumitomo thick film conductor paste C-4420 is raw material, adds 40nm tin oxide (1%), zinc oxide (5%), and 1200 rpms of drum'ss speed of rotation, the 15 minutes front yards 10 minutes of working vacuumize and charge into argon gas before the ball grinder work.Add macromolecule dispersing agent BYK104S (0.5%), add surfactant OP15 (0.5%), NP9 (0.5%).Ball milling uses agate ball, and ratio of grinding media to material 6: 1 was ground 50 hours.This slurry average grain diameter 20nm, the electromicroscopic photograph of its sample such as Fig. 1.Make fuse through the thick film screen printing technology.
Test condition is with embodiment 1, slurry of the present invention as a result 2 times, 4 times under the pulse current of normal current, its impulsive condition improves more than 20 times than former slurry following normal working hours; Specified instantaneous large-current is not exclusively fusing 10% down.
Embodiment 8
With mine, Sumitomo conductor paste C-4420 is raw material, adds 40nm tin oxide (1%), zinc oxide (2%), and bismuth oxide (3%), 1200 rpms of drum'ss speed of rotation are worked and were stopped 10 minutes in 15 minutes, vacuumize and charge into argon gas before the ball grinder work.Add macromolecule dispersing agent BYK104S (0.5%), add surfactant OP15 (0.5%), NP9 (0.5%).Ball milling uses agate ball, and ratio of grinding media to material 6: 1 was ground 10 hours.Get the slurry of the present invention of average grain diameter 100nm, make fuse through the thick film screen printing technology.
Test condition is with embodiment 1, and slurry of the present invention as a result improves more than 10 times than former slurry at impulsive condition following normal working hours, and specified instantaneous large-current is not exclusively fusing 2% down.
Embodiment 9
With Du Pont's thick film conductor paste is raw material, adds 40nm tin oxide (1%), manganese oxide (2%), and bismuth oxide (3%), 1200 rpms of drum'ss speed of rotation are worked and were stopped 15 minutes in 15 minutes, vacuumize and charge into argon gas before the ball grinder work.Ball milling uses agate ball, and ratio of grinding media to material 3: 1 was ground 2 hours.This slurry average grain diameter 400nm makes fuse through the thick film screen printing technology.
Test condition is with embodiment 1, and slurry of the present invention as a result improves more than 5 times than Du Pont thick film conductor paste at impulsive condition following normal working hours, and specified instantaneous large-current is not exclusively fusing 10% down, is better than Du Pont's thick film conductor paste.
Embodiment 10
With Du Pont's thick film conductor paste is raw material, add 40nm tin oxide (1%) and zinc oxide (2%), 50nm bismuth oxide (1%), sodium oxide molybdena (1%), 1000 rpms of drum'ss speed of rotation, work and stopped 10 minutes in 15 minutes, directly add ball grinder and grind, ball milling uses agate ball, ratio of grinding media to material 4: 1 was ground 1 hour.This slurry average grain diameter 500nm makes fuse through the thick film screen printing technology.
Test condition is with embodiment 1, and slurry of the present invention as a result improves more than 5 times than Du Pont thick film conductor paste at impulsive condition following normal working hours, and specified instantaneous large-current is not exclusively fusing 10% down, is better than Du Pont's thick film conductor paste.
Claims (6)
1. Nano Silver-silver slurry that is used to produce the fuse fuse, it is characterized in that, it is 0-10% (weight) nano-metal-oxide that in the electrocondution slurry that with silver-silver oxide, solvent adhesive main component, mixes, then, utilize the nanometer thinning method, make Nano Silver-silver slurry of 20-500nm.
2. Nano Silver-silver slurry according to claim 1 is characterized in that: said nano-metal-oxide is one or more in nano oxidized potassium, sodium oxide molybdena, bismuth oxide, tin oxide, zinc oxide, nickel oxide and the manganese oxide.
3. Nano Silver-silver slurry according to claim 2 is characterized in that: said nano-metal-oxide mixes than being 1-10%.
4. Nano Silver-silver slurry according to claim 1 is characterized in that: the particle diameter of said nano-metal-oxide is 10-100nm.
5. the preparation method of the described Nano Silver-silver slurry of claim 1, it is characterized in that: doping 0-10% nano-metal-oxide in the electrocondution slurry that with silver-silver oxide, solvent adhesive is main component, then, utilize the nanometer thinning method, make Nano Silver-silver slurry of 20-500nm.
6. preparation method according to claim 5 is characterized in that: said nanometer thinning method is the wet ball grinding method.
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| KR20100109416A (en) * | 2009-03-31 | 2010-10-08 | 디아이씨 가부시끼가이샤 | Electroconductive paste composition and the method of producing the same |
| CN102157222B (en) * | 2011-04-13 | 2012-05-23 | 成都印钞有限公司 | Low-temperature conductive silver paste and preparation method thereof |
| CN103436197B (en) * | 2013-09-02 | 2015-11-11 | 南京萨特科技发展有限公司 | A kind of overtemperature and overcurrent protection element conductive resin and preparation method thereof |
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| CN1621388A (en) * | 2003-11-27 | 2005-06-01 | 北京赛奇特种陶瓷功能制品工程研究中心 | Special ceramic material with antibacterial and water activating functions and preparation method and application thereof |
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