CN115197657A - High-power LED high-thermal-conductivity and electric-conductivity silver adhesive and preparation method thereof - Google Patents
High-power LED high-thermal-conductivity and electric-conductivity silver adhesive and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0806—Silver
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- C08K2201/004—Additives being defined by their length
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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- C08K2201/005—Additives being defined by their particle size in general
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Abstract
The invention relates to the technical field of conductive paste, in particular to high-power LED high-thermal-conductivity and electric-conductivity silver adhesive and a preparation method thereof, wherein the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components: 55 to 75 parts of micron silver powder, 5 to 10 parts of silver nanowire, 1 to 6 parts of low-melting-point alloy, 9 to 18 parts of epoxy resin, 1 to 7 parts of latent curing agent, 0.5 to 2 parts of toughening agent, 0.1 to 0.6 part of coupling agent, 0.1 to 0.5 part of curing accelerator and 0.1 to 1 part of soldering flux. The invention solves the problem of high packaging thermal resistance of the LED conductive adhesive in the prior art. The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is short in curing time, strong in electric conductivity, good in heat conductivity, large in shearing strength and strong in binding power, and can reduce the consumption of the micron silver powder while keeping low volume resistivity, so that the cost is reduced.
Description
Technical Field
The invention relates to the technical field of conductive paste, in particular to high-power LED high-thermal-conductivity and electric-conductivity silver adhesive and a preparation method thereof.
Background
As a special optoelectronic semiconductor device, LED has a series of advantages of small volume, all solid state, long service life, environmental protection, power saving, etc., and thus has been widely applied to various indoor and outdoor display screen automobiles, backlight sources, etc., and has become one of the main development directions of a new generation of energy-saving and environment-friendly illumination light source.
The LED conductive adhesive is used as a key material for bonding the LED chip and the substrate, has the functions of electric conduction, heat conduction and bonding, and therefore becomes one of the hot spots of the current domestic and foreign researches.
The choice of LED packaging method, materials, structure and process is mainly determined by the chip structure, optoelectronic/mechanical properties, specific application and cost, etc. Through development for more than 40 years, LED packaging successively goes through development stages such as a bracket type (Lamp LED), a surface mount type (SMD LED), a Power type LED (Power LED) and the like. With the increase of chip power, especially the development of solid-state lighting technology, new and higher requirements are put on the optical, thermal, electrical and mechanical structures of LED packages. In order to effectively reduce the package thermal resistance and improve the light extraction efficiency, a brand new technical idea must be adopted to design the LED package.
Disclosure of Invention
In view of the above disadvantages of the prior art, the present invention aims to provide a high thermal and electrical conductivity silver paste for a high power LED, which is used for solving the problem of high package thermal resistance of the LED electrical conductivity paste in the prior art, and also provides a preparation method of the high thermal and electrical conductivity silver paste for the high power LED. The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is short in curing time, strong in electric conductivity, good in heat conductivity, large in shearing strength and strong in binding power, and can reduce the consumption of micron silver powder while keeping low volume resistivity, so that the cost is reduced.
In order to attain the above and other related objects,
the invention provides a high-power LED high-thermal conductivity and electric conductivity silver adhesive, which comprises the following components in parts by weight: 55 to 75 parts of micron silver powder, 5 to 10 parts of silver nanowire, 1 to 6 parts of low-melting-point alloy, 9 to 18 parts of epoxy resin, 1 to 7 parts of latent curing agent, 0.5 to 2 parts of toughening agent, 0.1 to 0.6 part of coupling agent, 0.1 to 0.5 part of curing accelerator and 0.1 to 1 part of soldering flux.
The latent curing agent, the soldering flux, the coupling agent, the toughening agent and the curing accelerator are used as auxiliary agents.
The nano silver wire refers to a silver nano wire, which is dark gray or light gray, and can be stored in a solvent such as deionized water, ethanol, isopropanol and the like to form a suspension. The diameter of the nano silver wire ranges from tens of nanometers to hundreds of nanometers, and the length of the nano silver wire can reach dozens of micrometers according to different preparation conditions. The nano silver wire has excellent conductivity of silver due to the nano-scale rulerThe ITO transparent electrode has the advantages of good size effect, excellent light transmittance and bending resistance, so that the ITO transparent electrode is considered as a material most possibly replacing the traditional ITO transparent electrode, and the flexible and bendable LED display, the touch screen and the like are possible to realize. Even under the condition of low silver content, the conductive adhesive added with the nano silver wire has better conductive performance. Adding the nano silver wire into the conductive adhesive which takes the micron silver powder as the main filler, and sintering the nano silver among the micron silver powder (also sheet silver powder) after high-temperature curing and cooling, thereby reducing the contact resistance among the micron silver powder and obtaining the conductive adhesive with the volume resistivity of 5 multiplied by 10 -6 Omega cm (the volume resistivity refers to the volume resistivity of the high-power LED high-heat-conductivity and electric-conductivity silver adhesive in the scheme).
The low-melting-point alloy has a lower melting point, and is melted and infiltrated around the micron silver powder in the curing process of the conductive adhesive; after the conductive adhesive is solidified and completely cooled, the conductive adhesive and the low-melting-point alloy form a diversified metallurgical bonding in the conductive adhesive, so that the volume resistivity of the conductive adhesive is reduced.
The epoxy resin with low viscosity is adopted, so that better dispersion of the conductive filler (micron silver powder) can be promoted, and the addition amount of the conductive filler (micron silver powder) in the conductive silver adhesive can be increased.
The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is short in curing time, strong in electric conductivity, good in heat conductivity, large in shearing strength and strong in binding power, and can reduce the consumption of the micron silver powder while keeping low volume resistivity, so that the cost is reduced.
In an embodiment of the invention, the high-power LED high thermal and electrical conductivity silver paste comprises the following components in parts by weight: 65 parts of micron silver powder, 10 parts of silver nanowires, 6 parts of low-melting-point alloy, 14 parts of epoxy resin, 2 parts of latent curing agent, 2 parts of toughening agent, 0.2 part of coupling agent, 0.2 part of curing accelerator and 0.6 part of soldering flux.
In one embodiment of the invention, the micron silver powder is flake silver powder with an average particle size of 3-6 μm; the silver nano-wire is 2-5 μm long and 20-80 nm in diameter; the epoxy resin is selected from at least one of bisphenol A type epoxy resin E-44, bisphenol F type epoxy resin and alicyclic epoxy resin; the low-melting point alloy is Sn-Bi alloy (such as SnBi35Ag1, snBi58, snBi57Ag1 and the like); the latent curing agent is the Yingchuang epoxy curing agent 2753; the toughening agent is RICON MA maleic anhydride polybutadiene copolymer; the coupling agent is organic silicon coupling agent Silquest A-174; the curing accelerator is Acksu curing agent M50; the soldering flux is alpha lead-free soldering flux.
The flux is alpha lead-free flux with excellent hole filling capacity, and the alpha lead-free flux has hole filling coverage of more than 96% for 10mil (1mil = 0.00254cm). The alpha lead-free soldering flux has excellent lead-free soldering performance on various surface final processing circuit boards, has uniform residue distribution and no viscosity, can be used in high-density and common lead-free wave soldering processes, and is also suitable for lead-free and lead-containing processes.
The coupling agent is a mixed coupling aid prepared from a Silquest A-174 silane coupling agent (the mixed coupling aid contains a film-forming agent, a lubricating agent and an antistatic agent). The coupling agent can enhance the mechanical strength of the composite material (in the scheme, the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is also the composite material). The coupling agent improves the dry-wet mechanical strength of the polyester composite material (in the scheme, the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is also a polyester composite material), and improves the wet electrical property of the composite material.
The curing agent adopts a wound-winning epoxy polyamide curing agent, has good normal-temperature curing performance and can resist the temperature below 300 ℃.
The second aspect of the invention provides a preparation method of high-power LED high-thermal-conductivity and electric-conductivity silver adhesive, which comprises the following steps:
s1, weighing epoxy resin and a latent curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the latent curing agent into a stirring container, and stirring until the epoxy resin and the latent curing agent are in a transparent liquid state to obtain a carrier;
s2, weighing micron silver powder, silver nanowires, low-melting-point alloy, a toughening agent, a coupling agent, a curing accelerator and soldering flux according to corresponding proportions, sequentially adding the micron silver powder, the silver nanowires, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the high-thermal-conductivity and electric-conductivity silver colloid for the high-power LED.
The solvent can be selected from ethyl acetate, isoamyl acetate, methyl isobutyl ketone, etc.
In an embodiment of the present invention, the process for preparing the micron silver powder includes: respectively adding a surface active agent PVP (polyvinylpyrrolidone) into a silver nitrate solution and a ferrous sulfate solution, respectively dispersing half of PVP in the silver nitrate solution and the ferrous sulfate solution, directly pouring the ferrous sulfate solution into the silver nitrate solution after uniform dispersion, reacting for 10min at room temperature, filtering, washing and drying to obtain 3-6 mu m micrometer silver powder; wherein the molar ratio of the ferrous sulfate to the silver nitrate is 1.6:1, the amount of the surfactant PVP (mass ratio with respect to the silver nitrate) was 20wt%. The diameter of the silver powder sheet is reduced by the micron silver powder through the surface active agent PVP, and the bridging conduction rate between the silver powder and the silver powder is enhanced, so that the volume resistivity of the high-heat-conduction and electric-conduction silver adhesive of the high-power LED is reduced.
The particle size of the micron silver powder is 3-6 mu m, the silver nanowire is 2-5 mu m long and 20-80 nm in diameter, and the prepared conductive silver colloid has smaller fineness and can be adapted to smaller electronic elements; in addition, the silver paste and the substrate are favorably bonded into a whole, for example, the curing agent influences the quick curing time of the silver paste, the solder resist influences the reliability of the contact point of the high-heat-conductivity and electric-conduction silver paste of the high-power LED and the chip, and the temperature resistance of the chip in the hot-pressing process.
As mentioned above, the high-thermal conductivity and electric conductivity silver colloid for the high-power LED and the preparation method thereof have the following beneficial effects:
1. adding the nano silver wire into the conductive adhesive which takes the micron silver powder as the main filler, solidifying and cooling at high temperature, and sintering the nano silver among the micron silver powder (also sheet silver powder), thereby reducing the contact resistance among the micron silver powder and obtaining the conductive adhesive with the volume resistivity of 5 multiplied by 10 -6 The volume resistivity of the omega-cm high-power LED high-heat-conductivity and electric-conductivity silver adhesive.
2. The low-melting-point alloy has a lower melting point, and is melted and infiltrated around the micron silver powder in the curing process of the conductive adhesive; after the conductive adhesive is solidified and completely cooled, the conductive adhesive and the low-melting-point alloy form a diversified metallurgical bonding in the conductive adhesive, so that the volume resistivity of the conductive adhesive is reduced.
3. The epoxy resin with low viscosity is adopted, so that the conductive filler (micron silver powder) can be better dispersed, and the addition amount of the conductive filler (micron silver powder) in the conductive silver adhesive can be increased. The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is short in curing time, strong in electric conductivity, good in heat conductivity, large in shearing strength and strong in binding power, and can reduce the consumption of micron silver powder while keeping low volume resistivity, so that the cost is reduced.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Example 1
The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components in parts by weight: 65 parts of micron silver powder, 10 parts of silver nanowires, 6 parts of low-melting-point alloy, 14 parts of epoxy resin, 2 parts of latent curing agent, 2 parts of toughening agent, 0.2 part of coupling agent, 0.2 part of curing accelerator and 0.6 part of soldering flux;
wherein the micron silver powder is flake silver powder with the average particle size of 3-6 μm; the silver nano-wire is 2-5 μm long and 20-80 nm in diameter; the epoxy resin is bisphenol F type resin; the low-melting-point alloy is Sn-Bi alloy (SnBi 35Ag 1); the latent curing agent is the Yingchuang epoxy curing agent 2753; the toughening agent is RICON MA maleic anhydride polybutadiene copolymer; the coupling agent is organic silicon coupling agent Silquest A-174; the curing accelerator is Acksu curing agent M50; alpha lead-free soldering flux is selected as the soldering flux.
The preparation method of the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following steps:
s1, weighing epoxy resin and a latent curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the latent curing agent into a stirring container, and stirring until the epoxy resin and the latent curing agent are in a transparent liquid state to obtain a carrier;
s2, weighing micron silver powder, silver nanowires, low-melting-point alloy, a toughening agent, a coupling agent, a curing accelerator and soldering flux according to corresponding proportions, sequentially adding the micron silver powder, the silver nanowires, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the high-thermal-conductivity and electric-conductivity silver colloid for the high-power LED.
The high-heat-conductivity and electric-conductivity silver adhesive for the high-power LED realizes advanced curing through low-melting-point alloy, and has the following advantages:
(1) the curing time is shortened; the electrical property is expressed in advance under the same condition, the shorter the curing time of the matching process is, the better the electrical property is, and on the contrary, the longer the curing time is, the worse the electrical property is;
(2) the yield of enterprises is improved, and the energy consumption of the process is reduced.
On the premise of ensuring rapid curing, the reliability between the conductive adhesive and the chip of the high-power LED high-thermal-conductivity conductive silver adhesive ensures the soldering resistance of the conductive adhesive by adding the soldering flux (selecting lead-free soldering flux) so as to improve the thrust of the high-power LED high-thermal-conductivity conductive silver adhesive.
Comparative example 1
The LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components in parts by weight: 80 parts of micron silver powder, 6 parts of low-melting-point alloy, 14 parts of epoxy resin, 2 parts of latent curing agent, 2 parts of toughening agent, 0.2 part of coupling agent, 0.2 part of curing accelerator and 0.6 part of soldering flux;
wherein the micron silver powder is flake silver powder with the average grain diameter of 3-6 μm; the epoxy resin is bisphenol F type resin; the low-melting-point alloy is Sn-Bi alloy (SnBi 35Ag 1); the latent curing agent is the Yingchuang epoxy curing agent 2753; the toughening agent is RICON MA maleic anhydride polybutadiene copolymer; the coupling agent is organic silicon coupling agent Silquest A-174; the curing accelerator is Acksu curing agent M50; alpha lead-free soldering flux is selected as the soldering flux.
The preparation method of the LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following steps:
s1, weighing epoxy resin and a latent curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the latent curing agent into a stirring container, and stirring the epoxy resin and the latent curing agent until the epoxy resin and the latent curing agent are in a transparent liquid state to obtain a carrier;
s2, weighing the micron silver powder, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux according to corresponding proportions, sequentially adding the micron silver powder, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the LED high-thermal-conductivity and electric-conductivity silver adhesive.
Comparative example 1 differs from example 1 in that: comparative example 1 only 80 parts of the silver powder of micron was added, whereas example 1 is a mixture of "65 parts of silver powder of micron +10 parts of silver nanowires +5 parts of low melting point alloy". The conductivity of the conductive silver paste in example 1 is higher than that in comparative example 1, and the impedance of example 1 is reduced by 30% compared with that of comparative example 1. Therefore, the silver nanowires can reduce the impedance. Compared with the comparative example 1, the conductive silver paste added with the silver nanowires not only improves the conductivity, but also reduces the silver content (the addition amount of the silver content is less than 5 parts). In addition, the effect of reducing the silver content can be achieved by mixing a small amount of low-melting-point alloy to solidify the conductive silver paste in advance (the addition amount of the silver content is less than 5 parts).
Example 2
The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components in parts by weight: 75 parts of micron silver powder, 10 parts of silver nanowires, 6 parts of low-melting-point alloy, 18 parts of epoxy resin, 5 parts of latent curing agent, 2 parts of toughening agent, 0.6 part of coupling agent, 0.5 part of curing accelerator and 1 part of soldering flux;
wherein the micron silver powder is flake silver powder with the average grain diameter of 3-6 μm; the silver nano-wire is 2-5 μm long and 20-80 nm in diameter; the epoxy resin is bisphenol A type epoxy resin E-44; the low-melting-point alloy is Sn-Bi alloy (SnBi 35Ag 1); the latent curing agent is Yingchuang epoxy curing agent 2753; the toughening agent is RICON MA maleic anhydride polybutadiene copolymer; the coupling agent is organic silicon coupling agent Silquest A-174; the curing accelerator is Acksu curing agent M50; the soldering flux is alpha lead-free soldering flux.
The preparation method of the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following steps:
s1, weighing epoxy resin and a latent curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the latent curing agent into a stirring container, and stirring the epoxy resin and the latent curing agent until the epoxy resin and the latent curing agent are in a transparent liquid state to obtain a carrier;
s2, weighing micron silver powder, silver nanowires, low-melting-point alloy, a toughening agent, a coupling agent, a curing accelerator and soldering flux according to corresponding proportions, sequentially adding the micron silver powder, the silver nanowires, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the high-thermal-conductivity and electric-conductivity silver colloid of the high-power LED.
Example 3
The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components in parts by weight: 55 parts of micron silver powder, 7 parts of silver nanowires, 6 parts of low-melting-point alloy, 10 parts of epoxy resin, 3 parts of latent curing agent, 1 part of toughening agent, 0.3 part of coupling agent, 0.2 part of curing accelerator and 0.5 part of soldering flux;
wherein the micron silver powder is flake silver powder with the average particle size of 3-6 μm; the silver nano-wire is 2-5 μm long and 20-80 nm in diameter; the epoxy resin is bisphenol A type epoxy resin E-44; the low-melting-point alloy is Sn-Bi alloy (SnBi 35Ag 1); the latent curing agent is the Yingchuang epoxy curing agent 2753; the toughening agent is RICON MA maleic anhydride polybutadiene copolymer; the coupling agent is organic silicon coupling agent Silquest A-174; the curing accelerator is Acksu curing agent M50; the soldering flux is alpha lead-free soldering flux.
The preparation method of the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following steps:
s1, weighing epoxy resin and a latent curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the latent curing agent into a stirring container, and stirring the epoxy resin and the latent curing agent until the epoxy resin and the latent curing agent are in a transparent liquid state to obtain a carrier;
s2, weighing micrometer silver powder, silver nanowires, low-melting-point alloy, a toughening agent, a coupling agent, a curing accelerator and soldering flux according to a corresponding proportion, sequentially adding the micrometer silver powder, the silver nanowires, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the high-thermal-conductivity and electric-conductivity silver colloid of the high-power LED.
Comparative example 2
The LED conductive silver adhesive comprises the following components in parts by mass: 68-80% of 65 parts of micron silver sheet, 3 parts of nano silver wire, 14 parts of epoxy resin, 2 parts of curing agent, 2 parts of diluent, 1-4% of functional additive, 0.4% of defoaming agent, 0.2% of flatting agent and 0.5% of dispersing agent;
wherein the micron silver powder is flake silver powder with the average particle size of 3-6 μm; the silver nano-wire is 2-5 μm long and 20-80 nm in diameter; the epoxy resin is bisphenol F type resin; the curing agent is dicyandiamide; the diluent is selected from trimethylolethane triglycidyl ether; TEGO410 is selected as the leveling agent; the dispersant is TEGO Dispers 755w.
The preparation method of the LED conductive silver adhesive comprises the following steps:
s1, weighing epoxy resin and a curing agent according to a corresponding ratio, sequentially adding the epoxy resin and the curing agent into a stirring container, and stirring until the mixture is in a transparent liquid state to obtain a carrier;
s2, weighing micron silver powder, silver nanowires, a curing agent, a moisture absorbent, a functional assistant, a defoaming agent, a leveling agent and a dispersing agent according to corresponding proportions, sequentially adding the micron silver powder, the silver nanowires, the curing agent, the moisture absorbent, the functional assistant, the defoaming agent, the leveling agent and the dispersing agent into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, and then adding a solvent into the slurry under the stirring condition to adjust the viscosity of the slurry to be 5000-7000 CPS, so as to obtain the high-thermal-conductivity and electric-conductivity silver colloid of the high-power LED.
The conductive silver paste prepared in the above examples 1 to 3 and comparative example 2 has the following performance test data, as shown in table 1:
table 1
| Item | Example 1 | Example 2 | Example 3 | Comparative example 2 |
| Curing temperature/. Degree.C | 150 | 150 | 150 | 150 |
| Curing time/min | 30～40 | 30～40 | 30～40 | 60～90 |
| Volume resistivity/Ω · cm | 5×10 -6 | 5×10 -6 | 5×10 -6 | 6×10 -6 |
| ACA chip thrust/N | 12 | 13 | 13 | 7 |
| viscosity/CPS | 13000 | 13500 | 13400 | 15000 |
| Thermal conductivity/(W/m.K) | >19 | >20 | >20 | >14 |
| Shear strength/MPa | >10 | >12 | >11 | >14 |
As can be seen from Table 1, the high thermal conductivity and electric conductivity silver paste for the high power LED in the embodiments 1-3 can have a low silver content of about 55% and a high silver content of about 75%. The silver nanowires are added into the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive, so that the electrical property, the thermal conductivity, the bonding strength and the contact resistance of the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive are better than those of the prior art, the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive does not need too many additives, and the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is fine and smooth in product, free of bubbles and smooth in surface.
In conclusion, the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive disclosed by the invention is short in curing time, strong in electric conductivity, good in heat conductivity, large in shear strength and strong in binding power, and the consumption of the micron silver powder can be reduced while the low volume resistivity is kept, so that the cost is reduced. Therefore, the invention effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
1. The high-power LED high-thermal-conductivity and electric-conductivity silver adhesive is characterized by comprising the following components in parts by weight: 55 to 75 parts of micron silver powder, 5 to 10 parts of silver nanowire, 1 to 6 parts of low-melting-point alloy, 9 to 18 parts of epoxy resin, 1 to 7 parts of latent curing agent, 0.5 to 2 parts of toughening agent, 0.1 to 0.6 part of coupling agent, 0.1 to 0.5 part of curing accelerator and 0.1 to 1 part of soldering flux.
2. The high thermal and electrical conductivity silver paste for the high power LED according to claim 1, wherein: the high-power LED high-thermal-conductivity and electric-conductivity silver adhesive comprises the following components in parts by weight: 65 parts of micron silver powder, 10 parts of silver nanowires, 6 parts of low-melting-point alloy, 14 parts of epoxy resin, 2 parts of latent curing agent, 2 parts of toughening agent, 0.2 part of coupling agent, 0.2 part of curing accelerator and 0.6 part of soldering flux.
3. The high thermal and electrical conductivity silver paste for the high power LED according to claim 1 or 2, wherein: the micron silver powder is flake silver powder, and the average particle size is 3-6 mu m; the silver nanowires have the length of 2-5 mu m and the diameter of 20-80 nm.
4. The high thermal and electrical conductivity silver paste for the high power LED according to claim 1 or 2, wherein: the epoxy resin is at least one of bisphenol A epoxy resin, bisphenol F epoxy resin and alicyclic epoxy resin.
5. The high thermal and electrical conductivity silver paste for the high power LED according to claim 1 or 2, wherein: the low melting point alloy is Sn-Bi alloy.
6. The high-power LED high-thermal-conductivity and electric-conductivity silver paste according to claim 5, characterized in that: the Sn-Bi alloy is at least one of SnBi35Ag1, snBi58 and SnBi57Ag 1.
7. The method for preparing high-power LED high-thermal-conductivity and electric-conductivity silver adhesive according to any one of claims 1 to 6, characterized by comprising the following steps:
s1, stirring epoxy resin and a latent curing agent to be in a transparent liquid state to obtain a carrier;
s2, sequentially adding the micron silver powder, the silver nanowires, the low-melting-point alloy, the toughening agent, the coupling agent, the curing accelerator and the soldering flux into the carrier prepared in the step S1, and continuously stirring and dispersing to obtain uniform slurry;
and S3, grinding the slurry prepared in the step S2, adding a solvent into the slurry under the stirring condition to adjust the viscosity to be 5000-7000 CPS, and obtaining the high-heat-conductivity and electric-conductivity silver colloid of the high-power LED.
8. The preparation method of the high-power LED high-thermal-conductivity and electric-conductivity silver paste according to claim 7, characterized in that: the preparation process of the micron silver powder comprises the following steps: and respectively adding polyvinylpyrrolidone into the silver nitrate solution and the ferrous sulfate solution, uniformly dispersing, directly pouring the ferrous sulfate solution into the silver nitrate solution, and reacting at room temperature to obtain the micron silver powder.
9. The preparation method of the high-power LED high-thermal-conductivity and electric-conductivity silver paste according to claim 8, characterized by comprising the following steps: the molar ratio of the ferrous sulfate to the silver nitrate is 1.6:1, the polyvinylpyrrolidone being used in an amount of 20% by weight with respect to the mass of silver nitrate.
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| CN102676102A (en) * | 2011-03-16 | 2012-09-19 | 上海富信新能源科技有限公司 | Silver nanowire doped conductive silver colloid and preparation method thereof |
| CN104449455A (en) * | 2014-12-29 | 2015-03-25 | 中科院广州化学有限公司 | Medium temperature curing high-performance conductive silver adhesive, preparation method thereof and application |
| WO2018006503A1 (en) * | 2016-07-07 | 2018-01-11 | 深圳先进技术研究院 | Silver salt-doped conductive silver adhesive, and preparation method and use thereof |
| CN109401664A (en) * | 2017-08-15 | 2019-03-01 | 电子科技大学中山学院 | High-thermal-conductivity and electric-conductivity silver adhesive and preparation method thereof |
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2021
- 2021-04-13 CN CN202110395438.4A patent/CN115197657A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102676102A (en) * | 2011-03-16 | 2012-09-19 | 上海富信新能源科技有限公司 | Silver nanowire doped conductive silver colloid and preparation method thereof |
| CN104449455A (en) * | 2014-12-29 | 2015-03-25 | 中科院广州化学有限公司 | Medium temperature curing high-performance conductive silver adhesive, preparation method thereof and application |
| WO2018006503A1 (en) * | 2016-07-07 | 2018-01-11 | 深圳先进技术研究院 | Silver salt-doped conductive silver adhesive, and preparation method and use thereof |
| CN109401664A (en) * | 2017-08-15 | 2019-03-01 | 电子科技大学中山学院 | High-thermal-conductivity and electric-conductivity silver adhesive and preparation method thereof |
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