CN102838958A - Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity - Google Patents
Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity Download PDFInfo
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- CN102838958A CN102838958A CN2012103457607A CN201210345760A CN102838958A CN 102838958 A CN102838958 A CN 102838958A CN 2012103457607 A CN2012103457607 A CN 2012103457607A CN 201210345760 A CN201210345760 A CN 201210345760A CN 102838958 A CN102838958 A CN 102838958A
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- carbon nanotube
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- elargol
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Abstract
The invention relates to a preparation method of a silver colloid for an LED (Light Emitting Diode) with high thermal conductivity. The method comprises the following steps of: ball-milling and activating carbon nano tubes; after carrying out ultrasonic dispersion in organic solution, mixing and stirring with the silver colloid to obtain mixed liquor of the carbon nano tubes and the silver colloid; putting the mixed liquor into a flat magnetic field with the magnetic field intensity being 10-25 Tesla, or a high frequency alternating electric field with the electric field intensity being 1-2.5*10<6>V/m and the frequency being 1-10MHz; and after directional aligning the carbon nano tubes, heating the mixed liquor, so that the organic solution is volatilized, and the viscosity is improved. The electric field and the magnetic field are simultaneously adopted to directionally align the carbon nano tubes in the mixed liquor, so that the heat-conducting property of the silver colloid can be well improved. Through selection of the intensity and the direction of the electric field and the magnetic field, the control on the orientation, the density and the distribution of the carbon nano tubes is realized; and silver colloid solution of the directionally aligned carbon nano tubes with different densities and distributions can be obtained, and is then used for packaging the LED.
Description
Technical field
The invention belongs to the processing technique field of high thermal conductivity LED, the method for particularly relate to a kind of controlling carbon nanotube orientation, arranging and distributing with elargol.
Background technology
LED has energy-conserving and environment-protective, long service life, and advantages such as advantages of small volume are widely used in image display, and traffic signal shows that automotive industry is used lamp, backlight, fields such as lighting source.And conductive silver glue indispensable a kind of colloid during to be LED encapsulation produce is a conduction to the requirement of conductive silver glue, and heat conductivility will be got well, and bonding force is eager to excel.Through years of development; Along with the LED industry develops towards brightness, high-power direction, to the optics of LED encapsulation with elargol, calorifics, electricity and physical construction etc. have proposed renewal; Higher requirement, the conductive silver glue that wherein has the good heat conductive characteristic is one of development priority.
Great power LED can produce a large amount of heats normal in luminous, and heat dispersion is influence its stability and the principal element in work-ing life, leads away like untimely heat with the great power LED generation to leave, and this great power LED will wear out rapidly and burn.
The main effect at thermally conductive material interface just provide a LED and heat sink between heat dissipation channel; Reduce the interface thermal contact resistance between two or more materials; Heat is led away from the high temperature sensitive part; Elargol has very strong cementability and good electroconductibility and resistance to elevated temperatures as the matrix material between chip and the substrate.Have in the prior art through add graphite with reduce metal(lic)powder granularity improve the heat conductivility of elargol, also can only arrive 25.8W/mK but heat conductivility is the highest, the working life of high power device is still had certain restriction.
Carbon nanotube is the seamless nanotube-shaped shell structure of being curled and being formed by the single or multiple lift graphite flake; It is reported that the thermal conductivity of carbon nanotube is more than 10 times of argent, carbon nanotube can be improved better the thermal conductivity of heat-conducting glue as the packing material of heat-conducting glue.
Domestic patent (application number 201010155479.8) discloses the isotropic heat-conducting glue of a kind of filling carbon nano-pipe, and its average thermal conductivity is 25.5W/mK, and this patented process only is that carbon nanotube is mixed in the heat-conducting glue simply.
Domestic patent (application number 200410009281.3) introduction is adopted the orientations and the distribution of high frequency alternating electric field controlling carbon nanotube; The drips of solution that this method requires to contain carbon nanotube is on the prefabricated substrate that electrode arranged; Requirement is carried out electrode design to substrate, is inappropriate for the use of large-scale production of LED encapsulation enterprise.
Domestic patent (application number 201010155343.7) introduction is statically placed in dull and stereotyped magnetic field with the carbon nanotube mixed solution, and the room temperature baking-curing finally cuts on chip and the mint-mark circuit afterwards, this method complicated operation, and difficulty of processing is big.
Summary of the invention
The invention provides a kind of method of improving the elargol thermal conductivity, through in elargol, adding carbon nanotube, and to the orientation of carbon nanotube, density and distribution are controlled, and can obtain different densities, the aligned nanotubes of distribution.
This method is simple to operate, can realize carbon nanotube on a large scale, the orientations on the various substrates, and fully automated.
A kind of high thermal conductivity LED comprises the steps: with the preparation method of elargol
(1) carbon nanotube is carried out ball milling with its length of cutting,
(2) carbon nanotube is put in the strong acid oxidation and carries out activation treatment,
(3) carbon nanotube is joined carry out ultra-sonic dispersion in the organic solvent, the suspension-s that will contain carbon nanotube then mixes, stirs with elargol, obtains the mixed solution of carbon nanotube and elargol,
(4) mixed solution being placed magneticstrength is the dull and stereotyped magnetic field of 10-25 tesla, or strength of electric field is 1-2.5 * 10
6V/m, frequency are in the high frequency alternating electric field of 1-10MHz,
(5) etc. after the carbon nano-tube oriented arrangement, mixed solution is heated, make the organic solution volatilization, improve its viscosity.
Described carbon nanotube is selected single wall or multi-walled carbon nano-tubes for use.
Described elargol is a conductive silver glue, and conductive bodies adopts Powdered nanometer to micron-sized silver-colored particle, and tackiness agent is an epoxy resin.
The length of said carbon nanotube is 20-30um.
The percentage composition that said carbon nanotube adds is respectively 0.1%-1%.
Said strong acid is dense HCl, dense HNO
3Or dense H
2SO
4
Said organic solvent is an ethanol, acetone, normal hexane, Virahol, chloroform, N or 1,2-ethylene dichloride.
The present invention joins carbon nanotube in the middle of the elargol, on the basis that does not influence other performance, improves its heat conductivility.The present invention makes suspension with carbon nanotube with organic solvent and mixes with elargol, makes both mix more fully, adopts electric field or magnetic field that the carbon nanotube in the mixed solution is aligned simultaneously, to improve the heat conductivility of elargol better.
Through selection to electric field or magneticstrength and direction, realize orientation to carbon nanotube, density and distribution are controlled, and can obtain different densities, the fulmargin of the orientational alignment carbon nano-tube of distribution, and then be used for the encapsulation of LED.
Embodiment
The present invention can further describe through following embodiment.
Elargol is commercially available LED conductive silver glue.
The present invention provides a kind of LED and the steps include: with the preparation technology of elargol
1, carbon nanotube is put into ball mill and carry out ball milling, purpose is that the length of carbon nanotube is carried out cutting and chosen, and the length of choosing is 20-30um.
2, carbon nanotube is soaked in concentrated nitric acid to carry out activation treatment, the treatment time is 10 hours.
3, carbon nanotube is joined carry out ultra-sonic dispersion in the alcohol solvent, the suspension-s that will contain carbon nanotube then mixes with elargol, stirs, and obtains the mixed solution of carbon nanotube and elargol.
4, mixed solution being placed magneticstrength is the dull and stereotyped magnetic field of 10-25 tesla, left standstill 10-15 minute,
5, under magnetic field, continue afterwards mixed solution is heated, make the alcohol solvent volatilization, improve its viscosity.
Following table 1 is respectively and adopts elargol and elargol+carbon nanotube mixture as thermally-conductive interface, is packaged into the thermo-resistance measurement data of led light source.Because the thermal conductivity of heat-conducting glue test more complicated in the practical situation, so we, come the thermal conductivity of reflection interface heat-conducting glue indirectly through the thermal resistance value of test led light source.Can find out that through table 1 when in elargol, inserting carbon nanotube, and after it was aligned, the thermal resistance value of LED device had decline to a certain degree, dropped to 7.05 ° of C/W from 8.6.
We are through the thermal resistance of test LED device now, have obtained in processing procedure to carry out for the work in-process capacity of heat transmission method of real-time testing.
The thermo-resistance measurement data of table 1.LED light source
Claims (7)
1. a high thermal conductivity LED comprises the steps: with the preparation method of elargol
(1) carbon nanotube is carried out ball milling with cutting length,
(2) carbon nanotube is put in the strong acid oxidation and carries out activation treatment,
(2) carbon nanotube is joined carry out ultra-sonic dispersion in the organic solvent, the suspension-s that will contain carbon nanotube then mixes, stirs with elargol, obtains the mixed solution of carbon nanotube and elargol,
(3) mixed solution being placed magneticstrength is the dull and stereotyped magnetic field of 10-25 tesla, or strength of electric field is that 1-2.5 * 106V/m, frequency are in the high frequency alternating electric field of 1-10MHz,
(4) etc. after the carbon nano-tube oriented arrangement, mixed solution is heated, make the organic solution volatilization, improve its viscosity.
2. preparation method according to claim 1, the length of said carbon nanotube are 20-30um.
3. preparation method according to claim 1, the percentage composition that said carbon nanotube adds is respectively 0.1%-1%.
4. preparation method according to claim 1, said strong acid is dense HCl, dense HNO
3Or dense H
2SO
4
5. preparation method according to claim 1, said organic solvent is an ethanol, acetone, normal hexane, Virahol, chloroform, N or 1, one or more mixing in the 2-ethylene dichloride.
6. according to the arbitrary described preparation method of claim 1-5, described carbon nanotube is selected single wall or multi-walled carbon nano-tubes for use.
7. according to the arbitrary described preparation method of claim 1-5, described elargol is a conductive silver glue, and conductive bodies adopts Powdered nanometer to micron-sized silver-colored particle, and tackiness agent is an epoxy resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103457607A CN102838958B (en) | 2012-09-17 | 2012-09-17 | Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity |
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|---|---|---|---|
| CN2012103457607A CN102838958B (en) | 2012-09-17 | 2012-09-17 | Preparation method of silver colloid for LED (Light Emitting Diode) with high thermal conductivity |
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| CN102838958A true CN102838958A (en) | 2012-12-26 |
| CN102838958B CN102838958B (en) | 2013-12-11 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084264A (en) * | 2016-06-17 | 2016-11-09 | 中国人民解放军装甲兵工程学院 | A kind of composite laminated plate preparation technology of carbon nano-tube oriented arrangement |
| CN106700957A (en) * | 2017-01-22 | 2017-05-24 | 上海大学 | Heat conduction material doped conductive adhesive and preparation method thereof and application |
| CN106928867A (en) * | 2017-03-28 | 2017-07-07 | 镓特半导体科技（上海）有限公司 | A kind of carbon nanotube conducting glue and its preparation method and application |
| CN108130053A (en) * | 2017-12-21 | 2018-06-08 | 惠州市富济电子材料有限公司 | A kind of heat conduction silver paste and preparation method thereof |
| CN108165192A (en) * | 2017-12-28 | 2018-06-15 | 张家港康得新光电材料有限公司 | Heat-conducting glue band and preparation method thereof |
| CN111640851A (en) * | 2020-05-29 | 2020-09-08 | 旭宇光电（深圳）股份有限公司 | Deep ultraviolet LED light source and packaging method thereof |
| CN114854176A (en) * | 2022-06-20 | 2022-08-05 | 苏州圣杰特种树脂有限公司 | High Tg temperature epoxy resin for aviation and production process thereof |
| CN115274639A (en) * | 2022-08-17 | 2022-11-01 | 珠海市宏科光电子有限公司 | Dimming and color mixing integrated COB light source and processing technology thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740228A (en) * | 2005-09-01 | 2006-03-01 | 沈阳建筑大学 | Composite material with directionally arranged reinforcer and its prepn process |
| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
-
2012
- 2012-09-17 CN CN2012103457607A patent/CN102838958B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1740228A (en) * | 2005-09-01 | 2006-03-01 | 沈阳建筑大学 | Composite material with directionally arranged reinforcer and its prepn process |
| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084264A (en) * | 2016-06-17 | 2016-11-09 | 中国人民解放军装甲兵工程学院 | A kind of composite laminated plate preparation technology of carbon nano-tube oriented arrangement |
| CN106084264B (en) * | 2016-06-17 | 2020-04-21 | 中国人民解放军装甲兵工程学院 | Preparation process of composite material laminated plate with directionally arranged carbon nano tubes |
| CN106700957A (en) * | 2017-01-22 | 2017-05-24 | 上海大学 | Heat conduction material doped conductive adhesive and preparation method thereof and application |
| CN106928867A (en) * | 2017-03-28 | 2017-07-07 | 镓特半导体科技（上海）有限公司 | A kind of carbon nanotube conducting glue and its preparation method and application |
| CN108130053A (en) * | 2017-12-21 | 2018-06-08 | 惠州市富济电子材料有限公司 | A kind of heat conduction silver paste and preparation method thereof |
| CN108165192A (en) * | 2017-12-28 | 2018-06-15 | 张家港康得新光电材料有限公司 | Heat-conducting glue band and preparation method thereof |
| CN111640851A (en) * | 2020-05-29 | 2020-09-08 | 旭宇光电（深圳）股份有限公司 | Deep ultraviolet LED light source and packaging method thereof |
| CN114854176A (en) * | 2022-06-20 | 2022-08-05 | 苏州圣杰特种树脂有限公司 | High Tg temperature epoxy resin for aviation and production process thereof |
| CN115274639A (en) * | 2022-08-17 | 2022-11-01 | 珠海市宏科光电子有限公司 | Dimming and color mixing integrated COB light source and processing technology thereof |
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| CN102838958B (en) | 2013-12-11 |
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Granted publication date: 20131211 Termination date: 20190917 |