CN102262915A - Environment-friendly silver conductive paste based on surface mount of high-power light-emitting diode (LED) chip and preparation method for paste - Google Patents
Environment-friendly silver conductive paste based on surface mount of high-power light-emitting diode (LED) chip and preparation method for paste Download PDFInfo
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- CN102262915A CN102262915A CN2011102012194A CN201110201219A CN102262915A CN 102262915 A CN102262915 A CN 102262915A CN 2011102012194 A CN2011102012194 A CN 2011102012194A CN 201110201219 A CN201110201219 A CN 201110201219A CN 102262915 A CN102262915 A CN 102262915A
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Abstract
The invention relates to the field of manufacturing of high-power light-emitting diode (LED) chip surface mount photoelectric devices, in particular to an environment-friendly silver conductive paste based on surface mount of a high-power LED chip and a preparation method for the environment-friendly silver conductive paste. The environment-friendly silver conductive paste based on surface mount of the high-power LED chip is prepared from the following raw materials: 65 to 80 mass percent of ultrafine silver powder, 2 to 7 mass percent of nano copper powder, 5 to 12 mass percent of organic resin, 5 to 8 mass percent of solvent and 2 to 11 mass percent of additive. The paste prepared by the method has the advantages of high electrical conductivity, strong adhesive force, high stability, low possibility of being oxidized and the like, and has excellent wettability and compatibility with the high-power LED chip and a chip substrate.
Description
Technical field
The present invention relates to photoelectric component manufacturing fields such as high-power LED chip mounts, especially relate to a kind of mounting and use environment-friendly silver conductor paste and preparation method thereof based on high-power LED chip.
Background technology
Development along with microelectronics industry, especially in the photoelectricity industry, people require more and more higher to photoelectric cell, produce and adopt procedures, standardization to carry out more to reduce cost, just mounting of led chip mounted by original welding, fluid welding technical development production line till now, the appearance of great power LED, demand has the conductor paste of new requirement and mounting of high-power LED chip to be complementary especially, and the research of carrying out new conductor paste is also just imperative.
In general, the main component of electric slurry includes function mutually as metal, noble metal powder etc., inorganic binder such as glass powder, oxide powder etc., organic binder bond, other solvent and additive.Usually, function in the electric slurry plays electric action mutually, have good electric conductivity, is generally served as by metal dust or noble metal powder, metal dust commonly used has copper powder, aluminium powder, zinc powder, nickel powder etc., and precious metal powder commonly used has bronze, silver powder, platinum powder, palladium powder etc.Inorganic binder plays fixedly that electric slurry is generally served as by oxide powder and glass powder to base material, but this composition is lower at the proportion of electric slurry, have in addition do not have; Organic binder bond mainly plays a part to make slurry to have certain shape, be easy to print or apply, mainly contain macromolecule resin, the micromolecule resin waits and serves as, along with this part effect in electric slurry of chemical industry development of technology is more and more outstanding, the composition that changes organic binder bond just can change drying, the sintering character of electric slurry.
In existing electric slurry field, silver-colored serial conductor paste has the conductance height, and stable performance with characteristics such as the substrate bond strength are big, is widely used in the production of electronic devices and components such as integrated circuit, chip attachment, thin film switch.In general, the silver conductive paste that is used for optoelectronic areas is conductive silver glue again, mainly containing glue matrix, conductive filler, curing agent, curing accelerator, flexibilizer and other auxiliary agent forms, wherein as the glue matrix, epoxy resin, phenolic resins, polyurethane, acrylate etc. are arranged.Because the bonding property of epoxy resin is good, easy to use, therefore in conducting resinl, use the most generally.The kind of used silver powder, ratio, granularity and shape have a significant impact the performance of conducting resinl in the silver powder filled conductive glue.According to manufacture method, it is multiple that silver powder can be divided into electrolytic silver powder, electronation silver powder, ball milling silver powder and injection silver powder etc., and what use morely at present is electrolytic silver powder and electronation silver powder.The consumption of silver powder is generally about 40-80%.Consumption as silver powder is very few, and then glue-joint strength can be guaranteed, but electric conductivity descends; The consumption of silver powder is too much, and then electric conductivity increases, but glue-joint strength obviously descends, and cost is also corresponding to be increased.But, mounted the many conductor pastes made from chloride element in field at led chip in the past, enforcement along with various environmental regulations, the chlorine element becomes the material that national governments and environmental protection organization ban use of, electric slurry faces suchlike problem too to be needed to solve, the problem of environmental protection does not solve, and has just limited the development of conductor paste in product for civilian use market.
In addition, recently the great power LED of Xing Qiing requires higher to the silver conductive paste that mounts high-power LED chip and use, factors such as cracking, bonding are not firm appearred easily in the conductor paste of using in the led chip field of mounting when being used to mount high-power LED chip in the past, thereby had influenced the final effect of great power LED.
In view of the deficiency that above existing silver conductive paste exists, develop and a kind ofly mount based on high-power LED chip that also can substitute existing conductor paste just becomes the task of top priority with the environment-friendly silver conductor paste.
Summary of the invention
One of purpose of the present invention provides a kind of mounting based on high-power LED chip and uses the environment-friendly silver conductor paste, this slurry conducts electricity very well, strong adhesion, good stability, be difficult for oxidation, with high-power LED chip, chip substrate excellent wetting capacity and compatibility is arranged.In addition, this mounting with the environment-friendly silver conductor paste based on high-power LED chip do not contained harmful elements such as chlorine element, meets social development to environmental protection requirement.
For achieving the above object, the technical solution used in the present invention is: a kind of mounting based on high-power LED chip used the environment-friendly silver conductor paste, is that 65～80% super fine silver powder, mass percent are that 2～7% copper nanoparticles, mass percent 5～12% organic resins, mass percent are that the feedstock production of 5～8% solvents and mass percent 2～11% additives forms by mass percent.
Preferably, described super fine silver powder is that particle diameter is the super fine silver powder of 0.1～5 μ m; Described copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm.
Preferably, described organic resin is the combination of a kind of in polyurethane resin, polyacrylic resin, the epoxy resin or two kinds or three kinds.
Preferably, described solvent is the combination of a kind of in butyrolactone, ethylene glycol bisthioglycolate ethyl ester, the isopropyl alcohol or two kinds or three kinds.
Preferably, described additive is curing agent, defoamer, surfactant, and its percentage by weight is 0.2～5: 0.5～3: 0.01～7, and wherein curing agent is one or more in diacetayl amide, triethanolamine, the propylene glycol monomethyl ether acetamide; Defoamer is dodecyl sodium sulfate, 2-ethyl-4-methylimidazole, 4, one or more in the 4-MDA; Surfactant is one or more in dipropylene glycol methyl ether acetate, lactic acid esters of mono, the glycerol phosphate.
For achieving the above object, the technical solution used in the present invention is: a kind ofly mount preparation method with the environment-friendly silver conductor paste based on high-power LED chip, it is characterized in that: described preparation method carries out according to following steps:
1) 65～80% weighing particle diameters are the super fine silver powder of 0.1～5 μ m at first by mass percentage, 2～7% weighing particle diameters are the copper nanoparticle of 0.5～10nm by mass percentage, and are stand-by behind the mixing;
2) weighing mass percent is that 5～12% organic resin, mass percent are 5～8% solvent, fully stirs in homogenizer, and it is stand-by to be cooled to room temperature behind the mixing;
3) super fine silver powder that step 1) is obtained and the mixture of copper nanoparticle join step 2) organic resin and the mixture of solvent in, the adding mass percent is 2～11% additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
From above preparation method as can be seen, the above-mentioned conductor paste and the major advantage of preparation process thereof are the following aspects:
1, above-mentioned conductor paste is that large-scale production is easily accepted by people now because super fine silver powder is a kind of metal dust of technology comparative maturity mainly based on super fine silver powder and copper nanoparticle on the one hand; Copper nanoparticle is recently than more excellent nano material on the other hand, has optimized the partial properties of super fine silver powder after the adding, and the conductor paste electric conductivity of making is good, relatively meets high-power LED chip and mounts requirement for high conductivity.
2, analyze in conjunction with the physical and chemical performance of in the past conductor paste and to it, added the not resin of harmful substance such as chloride element, the wetability of slurry, surface smoothing, intermiscibility, good with the bond strength of high-power LED chip, chip substrate can substitute existing conductor paste fully and be used for the suitability for industrialized production manufacturing field that high-power LED chip mounts.
3, the solvent among the present invention has different boiling points and evaporation rate with additive, they fit together according to a certain percentage, make silver conductive paste mount volatilization one by one in the process at high-power LED chip, should not form defectives such as pore, crack, it is firm that conductor paste is connected with high-power LED chip, chip substrate, improves bonding strength.
Generally speaking, conductor paste electric conductivity, contact performance, the switching performance of preparation are good according to the method described above; The present invention can adapt with high-power LED chip, chip substrate by adjusting the content of various inorganic constituentss and organic principle, reaches the effect that makes properties of product better, has guaranteed the steady quality of product.
Embodiment
Embodiment 1:
A kind of mounting based on high-power LED chip used the environment-friendly silver conductor paste, and its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 65%, copper nanoparticle 5%, organic resin 12%, solvent 8% and additive 10%;
Super fine silver powder wherein is that particle diameter is the super fine silver powder of 0.1～5 μ m; Copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm; Organic resin is a polyurethane resin, and solvent is the ethylene glycol bisthioglycolate ethyl ester.Above-mentioned additive is curing agent, defoamer, surfactant, and it is 5: 0.5: 2 by weight percentage.Wherein curing agent is for being triethanolamine, and defoamer is a dodecyl sodium sulfate, and surfactant is a dipropylene glycol methyl ether acetate.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) the weighing particle diameter is that super fine silver powder and the particle diameter of 0.1～5 μ m is the copper nanoparticle of 0.5～10nm at first by mass percentage, and is stand-by behind the mixing;
2) by aforementioned mass percent weighing organic resin and solvent, in homogenizer, fully stir, it is stand-by to be cooled to room temperature behind the mixing;
3) mixture of aforesaid super fine silver powder and copper nanoparticle is joined in the mixture of organic resin and solvent, add additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
Embodiment 2:
A kind of mounting based on high-power LED chip used the environment-friendly silver conductor paste, and its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 70%, copper nanoparticle 7%, organic resin 10%, solvent 5% and additive 8%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1～5 μ m.Copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm, and organic resin is a polyacrylic resin, and solvent is an isopropyl alcohol.Above-mentioned additive is curing agent, defoamer, surfactant, and it is 0.2: 3: 5 by weight percentage.Wherein curing agent is for being diacetayl amide, and defoamer is a 2-ethyl-4-methylimidazole, and surfactant is a lactic acid esters of mono.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) the weighing particle diameter is that super fine silver powder and the particle diameter of 0.1～5 μ m is the copper nanoparticle of 0.5～10nm at first by mass percentage, and is stand-by behind the mixing;
2) by aforementioned mass percent weighing organic resin and solvent, in homogenizer, fully stir, it is stand-by to be cooled to room temperature behind the mixing;
3) mixture of aforesaid super fine silver powder and copper nanoparticle is joined in the mixture of organic resin and solvent, add additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
Embodiment 3:
A kind of mounting based on high-power LED chip used the environment-friendly silver conductor paste, and its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 76%, copper nanoparticle 2%, organic resin 5%, solvent 6% and additive 11%;
Wherein super fine silver powder is that particle diameter is the super fine silver powder of 0.1～5 μ m.Copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm, and organic resin is an epoxy resin, and solvent is a butyrolactone.Above-mentioned additive is curing agent, defoamer, surfactant, and it is 2: 3: 0.01 by weight percentage.Wherein curing agent is for being the propylene glycol monomethyl ether acetamide, and defoamer is 4,4-MDA, surfactant glycerol phosphate.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) the weighing particle diameter is that super fine silver powder and the particle diameter of 0.1～5 μ m is the copper nanoparticle of 0.5～10nm at first by mass percentage, and is stand-by behind the mixing;
2) by aforementioned mass percent weighing organic resin and solvent, in homogenizer, fully stir, it is stand-by to be cooled to room temperature behind the mixing;
3) mixture of aforesaid super fine silver powder and copper nanoparticle is joined in the mixture of organic resin and solvent, add additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
Embodiment 4:
A kind of mounting based on high-power LED chip used the environment-friendly silver conductor paste, and its concrete preparation is to finish according to following processing step:
At first prepare following raw material according to mass percent:
Super fine silver powder 80%, copper nanoparticle 3%, organic resin 10%, solvent 5% and additive 2%;
Super fine silver powder is that particle diameter is the super fine silver powder of 0.1～5 μ m.Copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm, and organic resin is the mixture of polyacrylic resin and epoxy resin (press mass ratio mixes at 3: 1), and solvent is the ethylene glycol bisthioglycolate ethyl ester.Above-mentioned additive is curing agent, defoamer, surfactant, and it is 2: 3: 7 by weight percentage.Wherein curing agent is the mixture for diacetayl amide and propylene glycol monomethyl ether acetamide (press mass ratio mixes at 2: 1), and defoamer is a 2-ethyl-4-methylimidazole, and surfactant is a dipropylene glycol methyl ether acetate.
This kind based semiconductor chip attachment is as follows with the preparation method of environment-friendly silver conductor paste:
1) the weighing particle diameter is that super fine silver powder and the particle diameter of 0.1～5 μ m is the copper nanoparticle of 0.5～10nm at first by mass percentage, and is stand-by behind the mixing;
2) by aforementioned mass percent weighing organic resin and solvent, in homogenizer, fully stir, it is stand-by to be cooled to room temperature behind the mixing;
3) mixture of aforesaid super fine silver powder and copper nanoparticle is joined in the mixture of organic resin and solvent, add additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
Claims (6)
1. one kind mounts based on high-power LED chip and to use the environment-friendly silver conductor paste, it is characterized in that: by mass percent is that 65～80% super fine silver powder, mass percent are that 2～7% copper nanoparticles, mass percent 5～12% organic resins, mass percent are that the feedstock production of 5～8% solvents and mass percent 2～11% additives forms.
2. as claimed in claim 1 mounting based on high-power LED chip used the environment-friendly silver conductor paste, it is characterized in that: described super fine silver powder is that particle diameter is the super fine silver powder of 0.1～5 μ m; Described copper nanoparticle is that particle diameter is the copper nanoparticle of 0.5～10nm.
3. as claimed in claim 1 mounting based on high-power LED chip used the environment-friendly silver conductor paste, it is characterized in that: described organic resin is the combination of a kind of in polyurethane resin, polyacrylic resin, the epoxy resin or two kinds or three kinds.
4. as claimed in claim 1 mounting based on high-power LED chip used the environment-friendly silver conductor paste, it is characterized in that: described solvent is the combination of a kind of, two kinds or three kinds in butyrolactone, ethylene glycol bisthioglycolate ethyl ester, the isopropyl alcohol.
5. as claimed in claim 1 mounting based on high-power LED chip used the environment-friendly silver conductor paste, it is characterized in that: described additive is curing agent, defoamer, surfactant, its percentage by weight is 0.2～5: 0.5～3: 0.01～7, and wherein curing agent is one or more in diacetayl amide, triethanolamine, the propylene glycol monomethyl ether acetamide; Defoamer is dodecyl sodium sulfate, 2-ethyl-4-methylimidazole, 4, one or more in the 4-MDA; Surfactant is one or more in dipropylene glycol methyl ether acetate, lactic acid esters of mono, the glycerol phosphate.
6. according to claim 1ly a kind ofly mount preparation method with the environment-friendly silver conductor paste based on high-power LED chip, it is characterized in that: described preparation method carries out according to following steps:
1) 65～80% weighing particle diameters are the super fine silver powder of 0.1～5 μ m at first by mass percentage, 2～7% weighing particle diameters are the copper nanoparticle of 0.5～10nm by mass percentage, and are stand-by behind the mixing;
2) weighing mass percent is that 5～12% organic resin, mass percent are 5～8% solvent, fully stirs in homogenizer, and it is stand-by to be cooled to room temperature behind the mixing;
3) super fine silver powder that step 1) is obtained and the mixture of copper nanoparticle join step 2) organic resin and the mixture of solvent in, the adding mass percent is 2～11% additive, the above-mentioned preliminary slurry that obtains is mixed and pulverizing with colloid mill, the rotating speed and the running time of control colloid mill, till fineness is less than 5 μ m, obtain the slurry finished product.
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| CN 201110201219 CN102262915B (en) | 2011-07-19 | 2011-07-19 | Environment-friendly silver conductive paste based on surface mount of high-power light-emitting diode (LED) chip and preparation method for paste |
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| CN 201110201219 CN102262915B (en) | 2011-07-19 | 2011-07-19 | Environment-friendly silver conductive paste based on surface mount of high-power light-emitting diode (LED) chip and preparation method for paste |
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| CN102262915B CN102262915B (en) | 2013-09-11 |
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| CN102568649A (en) * | 2011-12-29 | 2012-07-11 | 彩虹集团公司 | Method for preparing electrode paste for grid buried crystal silicon solar cells |
| CN102935518A (en) * | 2012-10-31 | 2013-02-20 | 哈尔滨工业大学深圳研究生院 | Nano silver paste for chip mounting and method for preparing nano silver paste |
| CN104575674A (en) * | 2014-12-23 | 2015-04-29 | 合肥中南光电有限公司 | Low-square-resistance electric conduction silver paste |
| CN105825913A (en) * | 2016-05-16 | 2016-08-03 | 南通天盛新能源股份有限公司 | Anti-aging back silver pulp used in crystalline silicon solar cell and preparation method for same |
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