CN106981342B - Adhesiveness high copper conductive film, preparation method and application - Google Patents
Adhesiveness high copper conductive film, preparation method and application Download PDFInfo
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- CN106981342B CN106981342B CN201610027828.5A CN201610027828A CN106981342B CN 106981342 B CN106981342 B CN 106981342B CN 201610027828 A CN201610027828 A CN 201610027828A CN 106981342 B CN106981342 B CN 106981342B
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- copper
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- film
- conductive film
- xenon lamp
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Laminated Bodies (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
Abstract
The invention discloses a kind of methods for preparing the high copper conductive film of adhesiveness comprising: partial size is greater than 50nm and copper particle of the surface oxide layer thickness less than 2nm is dispersed in substrate surface, forms copper film；Xenon lamp sintering is carried out to the copper film in air atmosphere, forms copper conductive film, wherein the temperature that the xenon lamp power used should be such that the substrate surface bears during the sintering process is lower than the glass transition temperature on the substrate surface layer.The invention also discloses a kind of copper conductive film that adhesiveness is high and its applications.The preparation method of the highly conductive copper film of adhesiveness provided by the invention is easy to operate, low-down xenon lamp power can be used, low energy consumption, and need to additionally add tackifier and can realize the preparation of the highly conductive copper film of adhesiveness on lower glass transition temperatures substrate, is suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of conductive copper films, especially a kind of copper conductive film that adhesiveness is high, preparation method and answer
With belonging to printed electronics field.
Background technique
In recent years, flexible electronic can directly apply to three-dimensional free surface working environment, promote biologic medical, leisure joy
People from fields-machine information such as happy is merged and is interacted, and meets the use demand of portability, comfort etc., to will greatly expand
The application range of Current electronic product, therefore the extensive concern by industry.(such as PET, PEN, PI on flexible substrates
Deng) printing prepare silver-based conducting wire technique (including ink preparation, printing technology, baking sintering process etc.) it is highly developed,
But the cost of material of silver-based conducting wire is very high, and silver-colored transfer ability is very good, causes its commercialization cost very high, and
Certain fields cannot apply.At this stage, copper-based electronic technology has low in cost, and transfer ability is poor, and conductivity is very high,
It is the main substitute technology of silver-based electronic technology.
However, causing its application to be extremely limited because copper has characteristic easy to oxidize.In recent years, with xenon
The development of lamp sintering technology solves the problems, such as that copper is sintered in air.But for the substrate in lower glass transition temperatures
The device of upper (such as PET, PEN) setting copper wire, still has very big defect by the way of xenon lamp sintering, this is because
Xenon lamp discharges larger numbers of luminous energy in moment (several milliseconds or a few tens of milliseconds), and copper transient absorption generates very high temperature,
Substrate can seriously be destroyed.In existing report mainly the copper oxide using copper oxide and surface with very thick (> 2nm),
The copper nano-particle of small particle needs relatively high xenon lamp energy (> 8J/cm2) could be by copper oxide and copper nano-particle surface
Copper oxide be reduced into conductive copper, so the copper conductor of xenon lamp sintering at this stage is mainly very high in glass transition temperature
PI (polyimides) on prepare, and the price of PI is very expensive, to significantly limit copper in commercialized application.
Postscript, in order to increase the adhesion strength of copper conductive film and polymeric substrates, most common way is will be in conductive ink
The resin or additive that can increase adhesion strength is added, however this will lead to the increase of copper conduction film resistivity again, while
It will lead to the promotion of cost.
Summary of the invention
The main purpose of the present invention is to provide a kind of method, adhesiveness for preparing the high copper conductive film of adhesiveness is high
Copper conductive film and its application, to overcome deficiency in the prior art.
For realization aforementioned invention purpose, the technical solution adopted by the present invention includes:
The embodiment of the invention provides a kind of methods for preparing the high copper conductive film of adhesiveness comprising:
The copper particle that partial size is 50~300nm and surface oxide layer thickness is 0~2nm is dispersed in substrate surface, is formed
Copper film；
Xenon lamp sintering is carried out to the copper film in air atmosphere, copper conductive film is formed, wherein the xenon lamp power used
The temperature that the substrate surface should be made to bear during the sintering process is higher than the glass transition temperature on the substrate surface layer.
In some more preferred embodiments, the preparation method includes:
It disperses the copper particle in solvent and forms dispersion liquid；
Using the dispersion liquid as ink, the copper film is formed in the substrate surface by mode of printing.
The embodiment of the invention also provides the high copper conductive films of the adhesiveness prepared by preceding method.
The embodiment of the invention also provides a kind of devices comprising: substrate；And using preceding method in the substrate
Surface prepares the copper conductive film to be formed.
Further, low Tg flexible substrates can be selected in aforementioned substrates.
Compared with prior art, the invention has the advantages that
(1) method of the high copper conductive film of preparation adhesiveness provided only needs low-down xenon lamp energy, energy conservation and environmental protection,
Sintering velocity is fast, is suitable for large-scale industrial production；
(2) method of the high copper conductive film of the preparation adhesiveness provided can be in the polymer of lower glass transition temperatures
It is realized on substrate, is commercially produced product, it is cheap and easy to get, it does not need to carry out special surface treatment；
(3) in the method for the high copper conductive film of preparation adhesiveness provided, not needing additionally to be added tackifier can be
High adhesion strength is generated between copper conductive film and substrate, especially copper conductive film can partially be embedded at institute during heat-agglomerating
It states in substrate；
(4) conductivity of copper conductive film prepared by the present invention is high, high with substrate adhesion strength, is suitable for preparing various flexibilities
Printed electronic device.
Detailed description of the invention
Fig. 1 is in a typical embodiments of the invention with the schematic diagram of low energy xenon lamp sintering copper film.
Specific embodiment
As previously mentioned, inventor is studied for a long period of time and largely practiced in view of the deficiencies in the prior art, this hair is proposed
Bright technical solution will give more specific detail as follows.
The one aspect of the embodiment of the present invention provides a kind of method for preparing the high copper conductive film of adhesiveness, packet
It includes:
The copper particle that partial size is 50~300nm and surface oxide layer thickness is 0~2nm is dispersed in substrate surface, is formed
Copper film；
Xenon lamp sintering is carried out to the copper film in air atmosphere, copper conductive film is formed, wherein the xenon lamp power used
The temperature that the substrate surface should be made to bear during the sintering process is higher than the glass transition temperature on the substrate surface layer.
Wherein, the principle of the preparation method sees Fig. 1.
In some embodiments, the preparation method may include: that printing prepares the copper very thin by surface oxide layer
The copper film of particle composition, is sintered using low-power xenon lamp on the substrate of substrate, especially lower glass transition temperatures, is glued
The attached preferable copper conductive film of power.
In some more preferred embodiments, the preparation method includes:
It disperses the copper particle in solvent and forms dispersion liquid；
Using the dispersion liquid as ink, the copper film is formed in the substrate surface by mode of printing.
Further, the mode of printing includes silk-screen printing, aerosol printing, intaglio printing, appointing in ink jet printing
It anticipates one kind, but not limited to this.
More preferred, the dispersion liquid is free of any tackifier, the especially described dispersion liquid can by the copper particle and
Solvent composition.
Further, the solvent includes water and/or organic solvent, such as ethyl alcohol, ethylene glycol, diethylene glycol, three second two
Alcohol, ethylene glycol monomethyl ether etc., but not limited to this.
In some embodiments, the thickness of the copper particle surface oxide layer is greater than 0.
It is more preferred, the copper film with a thickness of 0.4~1.6 micron.
It is more preferred, 0.5~5J/cm of the xenon lamp power2。
Further, copper conductive film lower part is embedded in the substrate.
In some more specific embodiments, the preparation method includes: that prepare surface oxide layer very thin
Copper particle；Prepare the copper ink of silk-screen printing；Using being screen printed onto the pattern for preparing copper in low Tg flexible substrates；
Sintering in air is carried out using the xenon lamp of low-down power and obtains the higher copper film of conductivity.
The embodiment of the invention also provides the high copper conductive films of the adhesiveness prepared by preceding method.
The embodiment of the invention also provides a kind of devices comprising: substrate；And using preceding method in the substrate
Surface prepares the copper conductive film to be formed.
Further, low Tg flexible substrates, the composition material packet of the flexible substrates can be selected in aforementioned substrates
Polyethylene terephthalate (PET) or polyethylene naphthalate (PEN) are included, but not limited to this.
Below with reference to several embodiments, further description of the technical solution of the present invention.
Embodiment 1
(1) choose surface oxide layer thickness be 0~0.5nm, the copper particle that partial size is 60~80nm；
(2) dispersion is added into ethylene glycol in above-mentioned copper particle and obtains printable copper ink, it is molten using silk-screen printing, gas
Glue spray printing or one kind of ink jet printing prepare copper film in the printing of pet sheet face；The thickness of copper film is greater than 0 and is less than or equal to
400nm；
(3) it is sintered to obtain conductive copper films using xenon lamp, xenon lamp power is 0.5~1J/cm2；Adhesion strength is adopted international standards
ASTM D3359 is tested, and is 5B grades.The conductivity of the conductive copper films is 20~50 μ Ω cm.
Embodiment 2
(1) choose surface oxide layer thickness be 0.5~1.0nm, the copper particle that partial size is 80~120nm；
(2) by above-mentioned copper particle be added into ethylene glycol monomethyl ether dispersion obtain printable copper ink, using silk-screen printing,
Aerosol spray printing or one kind of ink jet printing prepare copper film in PEN surface printing；Copper film with a thickness of 400~800nm；
(3) it is sintered to obtain conductive copper film using xenon lamp, xenon lamp power is 1~2J/cm2；Adhesion strength is adopted international standards
ASTM D3359 is tested, and is 5B grades.The conductivity of the conductive copper films is 50~100 μ Ω cm.
Embodiment 3
(1) choose surface oxide layer thickness be 1.0~1.5nm, the copper particle that partial size is 120~150nm；
(2) dispersion is added into triethylene glycol in above-mentioned copper particle and obtains printable copper ink, using silk-screen printing, gas
Colloidal sol spray printing or one kind of ink jet printing prepare copper film in the printing of pet sheet face；Copper film with a thickness of 800~1200nm；
(3) it is sintered to obtain conductive copper film using xenon lamp, xenon lamp power is 2~4J/cm2；Adhesion strength is adopted international standards
ASTM D3359 is tested, and is 5B grades.The conductivity of the conductive copper films is 100~150 μ Ω cm.
Embodiment 4
(1) choose surface oxide layer thickness be 1.5~2nm, the copper particle that partial size is 150~250nm；
(2) dispersion is added into glycerine in above-mentioned copper particle and obtains printable copper ink, it is molten using silk-screen printing, gas
Glue spray printing or one kind of ink jet printing prepare copper film in the printing of pet sheet face；Copper film with a thickness of 1200~1600nm；
(3) it is sintered to obtain conductive copper film using xenon lamp, xenon lamp power is 4~5J/cm2；Adhesion strength is adopted international standards
ASTM D3359 is tested, and is 5B grades.The conductivity of the conductive copper films is 100~150 μ Ω cm.
A kind of preparation method of the highly conductive copper film of adhesiveness provided by the invention is easy to operate, and low-down xenon lamp can be used
Power, low energy consumption, and need to additionally add tackifier and can realize adhesiveness combarloy on lower glass transition temperatures substrate
The preparation of film is suitable for industrialized production.
It is pointed out that the technical concepts and features of above-described embodiment only to illustrate the invention, it is ripe its object is to allow
The personage for knowing technique cans understand the content of the present invention and implement it accordingly, and protection model of the invention can not be limited with this
It encloses.Any equivalent change or modification in accordance with the spirit of the invention should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method for the copper conductive film that adhesiveness is high, characterized by comprising:
It disperses the copper particle that partial size is 50~300nm and surface oxide layer thickness is 0~2nm in solvent and forms dispersion liquid；
Using the dispersion liquid as ink, copper film is formed in substrate surface by mode of printing；
Xenon lamp sintering is carried out to the copper film in air atmosphere, wherein the xenon lamp power used should be such that the substrate surface is burning
The temperature born during knot is higher than the glass transition temperature on the substrate surface layer, to form copper conductive film, and makes the copper
Conductive film lower part is embedded in the substrate.
2. preparation method according to claim 1, it is characterised in that: the mode of printing includes silk-screen printing, aerosol
Printing, intaglio printing, any one in ink jet printing.
3. preparation method according to claim 1, it is characterised in that: the dispersion liquid is by the copper particle and solvent group
Include water and/or organic solvent at, the solvent, the organic solvent include ethyl alcohol, ethylene glycol, diethylene glycol, triethylene glycol,
Ethylene glycol monomethyl ether, n-butanol, diglycol, any one or two or more combinations in glycerine.
4. preparation method according to claim 1, it is characterised in that: the copper film with a thickness of 0.4~1.6 micron.
5. preparation method according to claim 1, it is characterised in that: 0.5~5 J/cm of xenon lamp power2。
6. preparation method according to claim 1, it is characterised in that: the substrate selects low Tg flexibility base
Bottom, the composition material of the flexible substrates include polyethylene terephthalate or polyethylene naphthalate.
7. by the high copper conductive film of adhesiveness prepared by any one of claim 1-6 the method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610027828.5A CN106981342B (en) | 2016-01-15 | 2016-01-15 | Adhesiveness high copper conductive film, preparation method and application |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610027828.5A CN106981342B (en) | 2016-01-15 | 2016-01-15 | Adhesiveness high copper conductive film, preparation method and application |
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| Publication Number | Publication Date |
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| CN106981342A CN106981342A (en) | 2017-07-25 |
| CN106981342B true CN106981342B (en) | 2019-03-08 |
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| CN111234286A (en) * | 2020-01-10 | 2020-06-05 | 深圳市百柔新材料技术有限公司 | Flexible conductive film and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1209698A1 (en) * | 2000-05-21 | 2002-05-29 | TDK Corporation | Transparent conductive multilayer body and method for producing the same |
| CN101801674A (en) * | 2007-05-18 | 2010-08-11 | 应用纳米技术控股股份有限公司 | metallic ink |
| CN103108492A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Manufacturing method and manufacturing device of flexible printed circuit |
| CN103108499A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Packaging method and packaging device of flexible electronic circuit |
| CN104750311A (en) * | 2015-03-16 | 2015-07-01 | 深圳市宇顺电子股份有限公司 | Manufacturing method of metal mesh conducting film, metal mesh conducting film and touch panel |
-
2016
- 2016-01-15 CN CN201610027828.5A patent/CN106981342B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1209698A1 (en) * | 2000-05-21 | 2002-05-29 | TDK Corporation | Transparent conductive multilayer body and method for producing the same |
| CN101801674A (en) * | 2007-05-18 | 2010-08-11 | 应用纳米技术控股股份有限公司 | metallic ink |
| CN103108492A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Manufacturing method and manufacturing device of flexible printed circuit |
| CN103108499A (en) * | 2013-01-17 | 2013-05-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Packaging method and packaging device of flexible electronic circuit |
| CN104750311A (en) * | 2015-03-16 | 2015-07-01 | 深圳市宇顺电子股份有限公司 | Manufacturing method of metal mesh conducting film, metal mesh conducting film and touch panel |
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| CN106981342A (en) | 2017-07-25 |
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