CN103265924A - Silvered carbon nano-tube and epoxy resin conductive adhesive - Google Patents
Silvered carbon nano-tube and epoxy resin conductive adhesive Download PDFInfo
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- CN103265924A CN103265924A CN2013101818287A CN201310181828A CN103265924A CN 103265924 A CN103265924 A CN 103265924A CN 2013101818287 A CN2013101818287 A CN 2013101818287A CN 201310181828 A CN201310181828 A CN 201310181828A CN 103265924 A CN103265924 A CN 103265924A
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Abstract
The invention discloses a silvered carbon nano-tube and epoxy resin conductive adhesive. The surface of the carbon nano-tube is chemically silvered to prepare silvered carbon nano-tube, and then, the silvered carbon nano-tube is introduced to an epoxy resin collectivity to prepare the silvered carbon nano-tube and epoxy resin conductive adhesive. The epoxy resin conductive adhesive with stable performance, good dispersibility and favorable conductivity can be obtained, and the preparation process is simple and easy to operate.
Description
Technical field
The present invention relates to the sizing agent field, particularly a kind of is the epoxide resin conductive adhesive of filler with silver-plated carbon nanotube.
Background technology
Conductive resin (electrically conductive adhesive) is a kind of extraordinary sizing agent with conducting function.In the electronic industry in future, can be used as the substitute of tin lead welding connection technology, and the benefit that has a tin burning bar of lead not have.At first, conductive resin is than the environmental protection more of a tin burning bar of lead.Eutectic tin-lead solder is the interconnection material of using at present the most widely, but plumbous well-known for the harm of human body and environment, promulgates that corresponding laws and regulations reduce this harm so various countries are numerous and confused.From the 80's ends of 20th century so far, developed country has promulgated that one after another law limits and forbid the use of slicker solder welding rod.Secondly, the technological temperature of conductive resin is low.The welding temperature that a tin burning bar of lead needs is 200 ℃, and temperature is higher than 230 ℃ in the plumbous connection of the tin technology, and the thermal stresses of giving birth to can damage device and substrate.And conductive resin only needs 80～150 ℃ just can solidify, and has so just made things convenient for those assemblings for the components and parts of high temp. sensitive, also can select the substrate of those non-refractories to assemble, and greatly reduces production cost.The 3rd, distance between centers of tracks reduces.Since the 90's of 20th century, the I/O density requirements that constantly uprises on the unicircuit connects material and has very high linear resolution.Wiping solder can only satisfy the connection in the following pitch of 0. 65 mm, has not caught up with the needs of unicircuit development.
The main dependence on import of the conductive resin of our domestic usefulness now, in three most widely used fields of conductive resin: quartz-crystal resonator, in LED and the IC field, external conductive resin has occupied the most market share.In the quartz-crystal resonator field, Shanghai synthetic resins institute part has replaced the product of Japanese Three-Bond company, but still based on the product of Japanese import; LED aspect, homemade conductive resin do not have to form the scale of oneself, and the titanium gram company in Shenzhen has some to use in low power LED product, but middle high power products does not just have the figure of homemade conductive resin fully; And in the highest IC encapsulation field of scientific and technological content, just almost completely not having homemade goods to occur, this mainly is external blockade on new techniques to us, even adhesion is produced raw material all from external import.
The electronic industry of China is being introduced and independent research SMT production line now in a large number, so conductive resin has wide application prospect in China.And the conductive resin of China is started late, so the high-performance conducting resin that uses mainly depends on import now.Therefore, develop novel high-performance conducting resin, and understand solidification value and set time, particle content, bonding pressure to the influence of conductive adhesive performance, become the task of top priority of China's Electronic Packaging industry.
Conductive resin generally is made up of matrix resin and conductive filler material two parts, and wherein conductive filler material becomes the main focus of every performance study of conductive resin.Argent is specific conductivity and the highest material of thermal conductivity in the common metal, stable in properties, oxidation slowly and its oxide compound also have electroconductibility, add moderate cost, so silver is one of the most widely used conductive resin filler.The conductive filler material of present commercially available silver conductive adhesive is based on micro-silver powder, and the subject matter of existence is that large usage quantity, the specific conductivity of silver is low, and having restricted silver is the high-end applications of conductive resin.
Summary of the invention
The objective of the invention is to overcome the defective that prior art exists, a kind of stable performance, good dispersion property, the good epoxide resin conductive adhesive of conductivity are provided.
In order to realize above goal of the invention, the present invention by the following technical solutions: a kind of silver-plated carbon nano tube epoxy resin conductive resin comprises the component of following mass fraction: 100 parts of Resins, epoxy; 20～30 parts of silver-plated carbon nanotubes; 10～20 parts in softening agent; 5～10 parts in solidifying agent; 1～5 part of promotor.
Described Resins, epoxy is a kind of in bisphenol A-type, Bisphenol F type or the ethylene oxidic ester epoxy resin.
Described softening agent is dibutyl phthalate.
Described solidifying agent is the ICAM-8409 latent curing agent.
Described promotor is DBU resting form promotor.
Carbon nanotube is since 1991 are at first found by Electronic Speculum expert professor Iijima of Japanese NEC, and between the short more than ten years, the carbonaceous pipe of this nano-scale has just caused the extensive interest of scientific circles such as global physics, chemistry and material.Since the special construction of carbon nanotube and excellent mechanics, electricity and optical property with and potential industrial value, make it become the research focus of ambits such as chemistry, physics and material gradually, the people is arranged even it is described as " the black diamond of 21 century ".Because carbon nanotube has good electroconductibility, have bigger length-to-diameter ratio again simultaneously, thereby be well suited for doing conductive filler material, with respect to other metallic particles and graphite granule, just can form with seldom amount and to conduct electricity network chain, and its density is more much smaller than metallic particles, difficult effect coagulation because of gravity.The present invention utilizes these characteristics of carbon nanotube that it is joined in the coating as conducting medium just, to increase the conductivity of electrically conducting coating.The silver of conductivity excellence is plated in the surface of carbon nanotube, can strengthens its conductivity.
Major advantage of the present invention and beneficial effect are: carbon nano tube surface is carried out chemical silvering, make silver-plated carbon nanotube, to introduce the silver-plated carbon nano tube epoxy resin conductive resin of preparation in the Resins, epoxy collective then, availability is stable, good dispersion property, the good epoxide resin conductive adhesive of conductivity, and preparation technology is simple, easy handling.
Embodiment
The present invention is further illustrated below by embodiment.
Embodiment one:
With carbon nanotube oxide treatment 2h in the vitriol oil/concentrated nitric acid of equal-volume ratio, filtration and distilled water repetitive scrubbing are to neutral, put into chemical plating liquid afterwards, 25 ℃ slowly add glucose, reaction 30min, to neutrality, 105 ℃ of vacuum-drying 2h get silver-plated carbon nanotube through suction filtration, distilled water repetitive scrubbing;
100 parts of ethylene oxidic ester epoxy resins, 10 parts of dibutyl phthalates, 6 parts of solidifying agent ICAM-8409 and 1 part of vulkacit D BU are mixed, shear agitation is even, slowly add 25 parts of silver-plated carbon nanotubes, continue to stir, namely make silver-plated carbon nano tube epoxy resin conductive resin.
Embodiment two:
With carbon nanotube oxide treatment 2h in the vitriol oil/concentrated nitric acid of equal-volume ratio, filtration and distilled water repetitive scrubbing are to neutral, put into chemical plating liquid afterwards, 25 ℃ slowly add glucose, reaction 30min, to neutrality, 105 ℃ of vacuum-drying 2h get silver-plated carbon nanotube through suction filtration, distilled water repetitive scrubbing;
100 parts of bisphenol A type epoxy resins, 20 parts of dibutyl phthalates, 8 parts of solidifying agent ICAM-8409 and 2 parts of vulkacit D BU are mixed, shear agitation is even, slowly add 20 parts of silver-plated carbon nanotubes, continue to stir, namely make silver-plated carbon nano tube epoxy resin conductive resin.
Embodiment three:
With carbon nanotube oxide treatment 2h in the vitriol oil/concentrated nitric acid of equal-volume ratio, filtration and distilled water repetitive scrubbing are to neutral, put into chemical plating liquid afterwards, 25 ℃ slowly add glucose, reaction 30min, to neutrality, 105 ℃ of vacuum-drying 2h get silver-plated carbon nanotube through suction filtration, distilled water repetitive scrubbing;
100 parts of bisphenol f type epoxy resins, 12 parts of dibutyl phthalates, 5 parts of solidifying agent ICAM-8409 and 3 parts of vulkacit D BU are mixed, shear agitation is even, slowly add 22 parts of silver-plated carbon nanotubes, continue to stir, namely make silver-plated carbon nano tube epoxy resin conductive resin.
Embodiment four:
With carbon nanotube oxide treatment 2h in the vitriol oil/concentrated nitric acid of equal-volume ratio, filtration and distilled water repetitive scrubbing are to neutral, put into chemical plating liquid afterwards, 25 ℃ slowly add glucose, reaction 30min, to neutrality, 105 ℃ of vacuum-drying 2h get silver-plated carbon nanotube through suction filtration, distilled water repetitive scrubbing;
100 parts of ethylene oxidic ester epoxy resins, 18 parts of dibutyl phthalates, 7 parts of solidifying agent ICAM-8409 and 4 parts of vulkacit D BU are mixed, shear agitation is even, slowly add 28 parts of silver-plated carbon nanotubes, continue to stir, namely make silver-plated carbon nano tube epoxy resin conductive resin.
Embodiment five:
With carbon nanotube oxide treatment 2h in the vitriol oil/concentrated nitric acid of equal-volume ratio, filtration and distilled water repetitive scrubbing are to neutral, put into chemical plating liquid afterwards, 25 ℃ slowly add glucose, reaction 30min, to neutrality, 105 ℃ of vacuum-drying 2h get silver-plated carbon nanotube through suction filtration, distilled water repetitive scrubbing;
100 parts of bisphenol f type epoxy resins, 15 parts of dibutyl phthalates, 10 parts of solidifying agent ICAM-8409 and 5 parts of vulkacit D BU are mixed, shear agitation is even, slowly add 30 parts of silver-plated carbon nanotubes, continue to stir, namely make silver-plated carbon nano tube epoxy resin conductive resin.
Performance test:
(1) volume specific resistance and specific conductivity: conductive resin evenly is coated in (glue thickness is 0.1～0.2 mm) between the copper sheet that diameter is 2cm, solidify the back and accurately measure bondline thickness (bondline thickness=total thickness-copper sheet thickness * 2) with screw micrometer, measure the room temperature resistivity of conductive resin again with the standard type digital multimeter; Calculate volume specific resistance and the specific conductivity of conductive resin at last according to following formula.ρv?=（R·S）/L?σ=1/ρv
In the formula: ρ v, R are volume specific resistance (Ω cm), resistance (Ω); S, L are glue-line area (cm
2), thickness (cm); σ is specific conductivity (S/cm).
(2) shearing resistance: according to GB 7124-2008 standards (metal/metal), adopt electronic universal mechanical test instrument to measure (rate of extension is 5 mm/min, and the aluminium alloy print is in advance through sand papering, rare HCl and acetone clean).
(3) thermostability: adopt thermogravimetric analysis (TGA) method to characterize (high-purity N
2Atmosphere, temperature rise rate are 8 K/min).
Test result: the specific conductivity of conductive resin is 0.024～0.045 S/cm, the lead excellent performance; Maximum is held concurrently and intensity is 6.12MPa, and initial decomposition temperature is 730 ℃, and over-all properties is all stronger, has wide range of applications.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (5)
1. silver-plated carbon nano tube epoxy resin conductive resin is characterized in that comprising the component of following mass fraction: 100 parts of Resins, epoxy; 20～30 parts of silver-plated carbon nanotubes; 10～20 parts in softening agent; 5～10 parts in solidifying agent; 1～5 part of promotor.
2. silver-plated carbon nano tube epoxy resin conductive resin according to claim 1 is characterized in that: described Resins, epoxy is a kind of in bisphenol A-type, Bisphenol F type or the ethylene oxidic ester epoxy resin.
3. silver-plated carbon nano tube epoxy resin conductive resin according to claim 1, it is characterized in that: described softening agent is dibutyl phthalate.
4. silver-plated carbon nano tube epoxy resin conductive resin according to claim 1, it is characterized in that: described solidifying agent is the ICAM-8409 latent curing agent.
5. silver-plated carbon nano tube epoxy resin conductive resin according to claim 1, it is characterized in that: described promotor is DBU resting form promotor.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101818287A CN103265924A (en) | 2013-05-16 | 2013-05-16 | Silvered carbon nano-tube and epoxy resin conductive adhesive |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101818287A CN103265924A (en) | 2013-05-16 | 2013-05-16 | Silvered carbon nano-tube and epoxy resin conductive adhesive |
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| CN2013101818287A Pending CN103265924A (en) | 2013-05-16 | 2013-05-16 | Silvered carbon nano-tube and epoxy resin conductive adhesive |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881605A (en) * | 2014-04-18 | 2014-06-25 | 太仓泰邦电子科技有限公司 | Electrochromic lighting double sided tape |
| CN108018014A (en) * | 2018-01-12 | 2018-05-11 | 深圳名飞远科技有限公司 | A kind of preparation method of novel nano silver conductive adhesive |
| CN111205719A (en) * | 2020-03-03 | 2020-05-29 | 深圳市利红金科技有限公司 | Silver-copper conductive paint and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297975A (en) * | 1999-11-26 | 2001-06-06 | 三友（天津）高分子技术有限公司 | Quick-setting single-component surface adhesive |
| CN102191003A (en) * | 2011-07-20 | 2011-09-21 | 常州合润新材料科技有限公司 | Silver-plated carbon nanotube heat-conducting adhesive and preparation method thereof |
| CN102311713A (en) * | 2010-07-02 | 2012-01-11 | 重庆工商大学 | Nanometer conductive adhesive |
-
2013
- 2013-05-16 CN CN2013101818287A patent/CN103265924A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1297975A (en) * | 1999-11-26 | 2001-06-06 | 三友（天津）高分子技术有限公司 | Quick-setting single-component surface adhesive |
| CN102311713A (en) * | 2010-07-02 | 2012-01-11 | 重庆工商大学 | Nanometer conductive adhesive |
| CN102191003A (en) * | 2011-07-20 | 2011-09-21 | 常州合润新材料科技有限公司 | Silver-plated carbon nanotube heat-conducting adhesive and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 冯永成: "新型纳米导电胶的研究", 《中国有色金属学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881605A (en) * | 2014-04-18 | 2014-06-25 | 太仓泰邦电子科技有限公司 | Electrochromic lighting double sided tape |
| CN108018014A (en) * | 2018-01-12 | 2018-05-11 | 深圳名飞远科技有限公司 | A kind of preparation method of novel nano silver conductive adhesive |
| CN108018014B (en) * | 2018-01-12 | 2018-10-09 | 深圳名飞远科技有限公司 | A kind of preparation method of nano-silver conductive glue |
| CN111205719A (en) * | 2020-03-03 | 2020-05-29 | 深圳市利红金科技有限公司 | Silver-copper conductive paint and preparation method thereof |
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Application publication date: 20130828 |