CN102555323A - Base board combination with conducting film layer and manufacture method thereof - Google Patents
Base board combination with conducting film layer and manufacture method thereof Download PDFInfo
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- CN102555323A CN102555323A CN2010106164469A CN201010616446A CN102555323A CN 102555323 A CN102555323 A CN 102555323A CN 2010106164469 A CN2010106164469 A CN 2010106164469A CN 201010616446 A CN201010616446 A CN 201010616446A CN 102555323 A CN102555323 A CN 102555323A
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Abstract
The invention relates to a base board combination with a conducting film layer and a manufacture method thereof. The base board combination comprises a macromolecule substrate, a surface treatment layer formed on the macromolecule substrate and the conducting film layer formed on the surface treatment layer. The surface treatment layer is formed by an auxiliary firing filling material and a macromolecule composite material, the conducting film layer is formed by firing metal electric conduction printing ink, the auxiliary firing filling material in the surface treatment layer has energy conduction characters and conducts energy to the metal electric conduction printing ink in an auxiliary mode, and the base board combination is favorable for firing of the metal electric conduction printing ink.
Description
[technical field]
The present invention relates to a kind of substrate in combination, particularly relate to a kind of substrate in combination and manufacturing approach thereof with conductive film layer.
[background technology]
The application majority of at present flexible (flexible) electronic technology is directly to print the conducting wire on flexible base, board, to reduce manufacturing cost, in order to reach the conducting wire of high-reliability, needs to increase the adhesive force between conducting wire and the flexible base, board.
The mode that increases adhesive force between conducting wire and the flexible base, board traditionally can be divided into the electrically conductive ink upgrading type to the adhesive force enhancing of electrically conductive ink, and the substrate upgrading type that is directed against the adhesive force enhancing of substrate.The mode of electrically conductive ink upgrading type is for example utilized mixing of porous matter conductor material and porous matter macromolecular material in the open US 2007/0048514 of United States Patent (USP), mentioning, increases the adhesive strength between conductor layer and the polymeric substrate.In addition, mention that in the open US 2004/0144958 of United States Patent (USP) the macromolecular material that in electrically conductive ink, adds low glass state inversion point (Tg) promotes additive as adhesion, to increase the adhesive force of printing ink to substrate.
The mode of substrate upgrading type for example uses the metal alkoxide layer to handle with the mode of cracking, microwave or hydrolysis at substrate surface in the open US 2009/0104474 of United States Patent (USP), mentioning, forms the oxide adhesion coating, to improve the adhesive force of substrate surface.In addition, in U.S. Pat 5190795, mention, utilize mode of heating to make it be attached to substrate surface again, increase the adhesive force between substrate and the metal by this in utilizing couplant (coupling agent) at substrate surface coating one deck inorganic oxide.
The mode of above-mentioned electrically conductive ink upgrading type mainly is in electrically conductive ink, to add macromolecular material; By conductive film layer behind the macromolecular material enhancement sintering (Sinter) and the adhesive force between the substrate, yet the macromolecular material in the printing ink can reduce the conductivity degree of conductive film layer; And the mode of substrate upgrading type mainly is to form at substrate surface for example to be the adhesion coating of oxide, increases the adhesive force of substrate surface, yet the adhesion coating of this substrate surface does not have other adjections except increasing adhesive force.
[summary of the invention]
The present invention provides a kind of substrate in combination with conductive film layer; Comprise: the polymer-based end; Be arranged at the suprabasil surface-treated layer of macromolecule, and be arranged at the conductive film layer on the surface-treated layer, wherein surface-treated layer is to be formed by assisted sintering packing material and high molecular composite; Conductive film layer is to be formed by metallic conduction printing ink sintering; Assisted sintering packing material in the surface-treated layer has the energy conduction characteristic, and its auxiliary transmission energy to metallic conduction printing ink helps the sintering of metallic conduction printing ink.
In addition, the present invention also provides a kind of manufacturing approach with substrate in combination of conductive film layer, comprising: the polymer-based end is provided; To contain assisted sintering packing material and high molecular mixture coats at polymer-based the end; With this assisted sintering packing material and high molecular mixture solidified, form surface-treated layer, metallic conduction printing ink is coated on the surface-treated layer; And apply first energy source; And auxiliary apply second energy source, and make metallic conduction printing ink sintering form conductive film layer, wherein the assisted sintering packing material of surface-treated layer has the energy conduction characteristic; Energy to the metallic conduction printing ink of its auxiliary transmission first energy source and second energy source helps the sintering of metallic conduction printing ink.
For let above-mentioned purpose of the present invention, characteristic, and advantage can be more obviously understandable, below in conjunction with accompanying drawing, elaborate as follows:
[description of drawings]
Fig. 1 shows the generalized section that has the substrate in combination of conductive film layer according to an embodiment of the present invention.
Fig. 2 A to 2D figure shows the generalized section that forms each fabrication stage of the substrate in combination with conductive film layer according to an embodiment of the present invention.
[main description of reference numerals]
10~polymer-based the end; 17~metallic conduction printing ink;
12~assisted sintering packing material; 18~conductive film layer;
13~curing process; 20~the second energy sources;
14~macromolecule; 30~the first energy sources;
15~solvent; 100~substrate in combination.
16~surface-treated layer;
[specific embodiment]
See also Fig. 1; It shows the generalized section of the substrate in combination with conductive film layer 100 of an embodiment of the present invention; This substrate in combination 100 comprises the polymer-based end 10, on the polymer-based end 10, has surface-treated layer 16, and on surface-treated layer 16, has conductive film layer 18.
The polymer-based end 10 can be the flexible substrates of being processed by thermal plastic high polymer, thermosetting polymer or aforesaid composite, for example is PETG (polyethylene terephthalate; Abbreviation PET), polyacrylic (polyacrylic; Be called for short U-Polymer) or Merlon (polycarbonate; Be called for short PC) etc. material.The insulating surfaces resistance at the polymer-based end 10 can be 10
14Ω/ is (more than the Ω/sq), preferably between 10
14Ω/sq to 10
16Between Ω/sq, more preferably between 10
15Ω/sq to 10
16Between Ω/sq.The glass transition temperature at the polymer-based end 10 (Tg) can be more than 80 ℃, preferably between 80 ℃ to 160 ℃, more preferably between 100 ℃ to 150 ℃.
Surface-treated layer 16 mainly is to be formed by assisted sintering packing material 12 composite with macromolecule 14, and one of effect of surface-treated layer 16 is macromolecule 14 increase conductive film layer 18 and the adhesive force at the polymer-based end 10 by wherein; Another effect of surface-treated layer 16 then is the curing action by wherein assisted sintering packing material 12 reinforced metal electrically conductive inks, forms conductive film layer 18.The insulating surfaces resistance of surface-treated layer 16 is 10
6More than Ω/sq, and the adhesive force between surface-treated layer 16 and the polymer-based end 10 and the conductive film layer 18 is more than the 4B.
In embodiments of the present invention, the part by weight of the assisted sintering packing material 12 in the surface-treated layer 16 is less than 5wt%, is preferably between the 0.01wt% to 5wt%, more preferably between the 0.05wt% to 3wt%.Assisted sintering packing material 12 can be nanotube, nanosphere, material with carbon element, clay or aforesaid combination, and wherein nanotube for example is CNT, metal nano-tube or nonmetal nanotube; Nanosphere for example is Nano carbon balls, metal nano ball or nonmetal nanosphere; Material with carbon element for example is graphite or graphite oxide; Clay for example is the clay compound that IA family oxide on the chemical periodic table, IIA family oxide and IVA family oxide are formed.Above-mentioned CNT can be SWCN or multi-walled carbon nano-tubes; The composition of metal nano-tube and metal nano ball can be selected from titanium, manganese, zinc, copper, silver, gold, tin, iron, nickel, cobalt, indium and aluminium or other alternative materials; The composition of nonmetal nanotube and nonmetal nanosphere can be titanium oxide, manganese oxide, zinc oxide, silver oxide, iron oxide, tin oxide, nickel oxide, indium oxide or other metal oxides.
Assisted sintering packing material 12 in the surface-treated layer 16 has the characteristic of conduct energy; By the transfer function of assisted sintering packing material 12 for heat, light or energy waves homenergic; Can transfer its energy in the metallic conduction printing ink effectively; Make the metal-organic also proper energy rank in the printing ink change, reduce its reduction temperature.In addition; Assisted sintering packing material 12 also can transfer its energy to the nano metal particles that the metallo-organic compound reduction forms; Make its local temperature be increased to fusing point; Effectively reduce the sintering temperature of metallic conduction printing ink, and then under lower ambient temperature and in short hardening time (curing time), form simple metal conductive film layer 18, therefore be applicable to the polymer-based end 10 of hanging down softening temperature.
In addition; In metallic conduction printing ink except metallo-organic compound and solvent; Can also add metal-powder; It can be time micron and the nano metal powder of spherical or sheet, and the size of metal-powder is less than 500nm, and the composition of metal-powder is selected from copper, silver, gold, aluminium, titanium, nickel, tin, iron, platinum and palladium.Solvent in the metallic conduction printing ink can be polarity or non-polar solven, for example is xylenes (xylene), toluene (tolene), terpineol (terpenol) or aforesaid combination.In addition, in metallic conduction printing ink, can also be added with other inorganic or organic processing aids that help processing procedure processing or conductive film layer characteristic.
In addition; Metallic conduction printing ink also can directly use metallic and solvent combinations to form; Assisted sintering packing material 12 in the surface-treated layer 16 can transfer its energy to metallic; Make its local temperature be increased to fusing point, effectively reduce the sintering temperature of metallic conduction printing ink, help metallic conduction printing ink sintering to form conductive film layer 18.
See also Fig. 2 A to 2D, it shows a foundation embodiment of the present invention, forms the generalized section of each fabrication stage of the substrate in combination 100 with conductive film layer.Consult Fig. 2 A, the polymer-based end 10 at first is provided, then with the wet coat mode, processing procedure such as rotary coating or serigraphy for example, the mixture 11 that assisted sintering packing material 12, macromolecule 14 and solvent 15 are formed is coated at polymer-based the end 10.Then, utilizing curing process 13, for example is modes such as UV light or heating, and said mixture 11 is solidified, and removes solvent 15 wherein, forms surface-treated layer 16, shown in Fig. 2 B.
Consult Fig. 2 C, utilize the wet coat mode, for example processing procedure such as rotary coating or serigraphy is coated on metallic conduction printing ink 17 on the surface-treated layer 16.Then, the polymer-based end 10, surface-treated layer 16 and metallic conduction printing ink 17 are applied first energy source 30, and auxiliaryly apply second energy source 20, make metallic conduction printing ink 17 sintering, form conductive film layer 18, shown in Fig. 2 D.In one embodiment, the resistivity of conductive film layer 18 is less than 10x10
-3Ω cm.
Because the assisted sintering packing material 12 that contains in the surface-treated layer 16 has the energy conduction characteristic; But therefore in energy to the metallic conduction printing ink 17 of auxiliary transmission first energy source and second energy source; Help the sintering of metallic conduction printing ink to carry out; Therefore can under lower ambient temperature and in the short sintering time, form conductive film layer 18, make the polymer-based end 10 of hanging down softening temperature can not produce deformation.
Below enumerate each embodiment and comparative example the manufacturing approach of substrate in combination 100 of the present invention, material and characteristic thereof be described:
[embodiment 1-4]
To contain many walls of 1wt% type CNT (bright prosperous science and technology; The mixture of the 55wt% acrylic resin CN104Q CNT) and 45wt% MEK (methyl ethyl ketone is called for short MEK) is coated thickness 150 μ m; Glass transition temperature is 80 ℃, and insulating surfaces resistance is 1.82x10
13On the PETG of Ω/sq (PET) base material, behind the use UV photocuring, form surface-treated layer, its insulating surfaces resistance is greater than 10
14Ω/sq.
Then, with 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, form mixed uniformly silver metal electrically conductive ink, through rotary coating process; Coat on the surface-treated layer, adopt 150 ℃ ambient temperature, be aided with the far red light irradiation; Carry out the sintering of metallic conduction printing ink, form the conductive film layer of embodiment 1-4.
Utilize hundred lattice (Cross-Cut Method) tests (ASTM D3330), four-point probe method test and hardness test (ASTM D3363) to measure the conductive film layer of embodiment 1-4, resulting adhesive force, sheet resistance (Sheet Resistance) value and film hardness such as table 1 are listed.
[comparative example 1-4]
The mixture of 55wt% acrylic resin and 45wt% MEK (MEK) is coated thickness 150 μ m, and glass transition temperature is 80 ℃, and insulating surfaces resistance is 1.82x10
13On the PET base material of Ω/sq, use UV to solidify the back and form surface-treated layer, its insulating surfaces resistance is greater than 9.55X10
10Ω/sq.
With 39.8wt% organic acid silver (C
7H
15COOAg) be dissolved in the 59.7wt% xylenes; Form mixed uniformly silver metal electrically conductive ink,, coat on the above-mentioned surface-treated layer through rotary coating process; Adopt hot processing procedure; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 1-4.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 1-4, resulting adhesive force, sheet resistance value and film hardness such as table 1 are listed.
The composition of the conductive film layer of table 1 embodiment 1-4 and comparative example 1-4 and characteristic
Shown in table 1 test result; Than the surface-treated layer that does not add many walls type CNT, have auxiliary infrared light irradiation in 10 minutes and the resulting conductive film layer of surface-treated layer interior interpolation many walls type CNT and can obtain best surface resistance (surface resistance).In addition, than the condition of no auxiliary energy, coating metal electrically conductive ink on the surface-treated layer that adds many walls type CNT, and have under the condition of auxiliary energy, can obtain more stable conductive film layer hardness and adhesive force.
[embodiment 5-8]
To contain the polyacrylic of many walls of 1wt% type CNT (bright prosperous science and technology, CN104Q CNT) and the mixture of N-crassitude ketone solvent and coat thickness 150 μ m, glass transition temperature is 160 ℃, and insulaion resistance is greater than 10
14On the polyacrylic of Ω/sq (U-Polymer) base material, form surface-treated layer behind the use UV photocuring, its insulaion resistance is 9.95X10
10Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 5-8.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 5-8, resulting adhesive force, sheet resistance value and film hardness such as table 2 are listed.
[comparative example 5-8]
The mixture of polyacrylic (U-Polymer) and N-crassitude ketone solvent is coated thickness 150 μ m, and glass transition temperature is 160 ℃, and insulaion resistance is greater than 10
14On the polyacrylic of Ω/sq (U-Polymer) base material, form surface-treated layer behind the use UV photocuring, its insulaion resistance is greater than 10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 5-8.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 5-8, resulting adhesive force, sheet resistance value and film hardness such as table 2 are listed.
The composition of the conductive film layer of table 2 embodiment 5-8 and comparative example 5-8 and characteristic
X: the non-resistance value, the expression resistance value is too high
Shown in table 2 test result; Condition than no auxiliary energy; Coating metal electrically conductive ink on the polyacrylic surface-treated layer that adds many walls type CNT has under 10 minutes the treatment conditions of auxiliary energy, and resulting conductive film layer has higher hardness 2B and adhesive force 5B.
[embodiment 9-12]
To contain the 5wt% polyvinyl alcohol of many walls of 1wt% type CNT (bright prosperous science and technology, CN104Q CNT) and the mixture of alcohol solvent, and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.07X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 9-12.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 9-12, resulting adhesive force, sheet resistance value and film hardness such as table 3 are listed.
[comparative example 9-12]
The 5wt% polyvinyl alcohol (PVA) and the mixture of alcohol solvent are coated thickness 150 μ m, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form the surface treatment rete, its insulaion resistance is 1.02X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 9-12.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 9-12, resulting adhesive force, sheet resistance value and film hardness such as table 3 are listed.
The composition of the conductive film layer of table 3 embodiment 9-12 and comparative example 9-12 and characteristic
Shown in table 3 test result; Condition than no auxiliary energy; Coating metal electrically conductive ink on the polyvinyl alcohol surface-treated layer that adds many walls type CNT; Under 10 minutes treatment conditions with auxiliary energy, it is high and stable to obtain adhesive force (4B), and the surface patch resistance (conductive film layer that 0.35 Ω/sq) is lower.
[embodiment 13-16]
To contain the 5wt% polyvinyl alcohol (PVA) of 1wt% clay additive (Clay) and the mixture of alcohol solvent, and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form the surface treatment rete, its insulaion resistance is 5.34X10
12Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 13-16.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 13-16, resulting adhesive force, sheet resistance value and film hardness such as table 4 are listed.
The composition and the characteristic of the conductive film layer of table 4 embodiment 13-16
Shown in table 4 test result; Condition than no auxiliary energy; Adding coating metal electrically conductive ink on the surface-treated layer of clay, have 5 minutes of auxiliary energy and 10 minutes treatment conditions under, can obtain the lower and stable conductive film layer of surface patch resistance value.
[embodiment 17-20]
The 5wt% polyvinyl alcohol (PVA) that will contain 1wt% Nano carbon balls (bright prosperous science and technology, CN107C Nano carbon balls) is coated thickness 150 μ m with the mixture of alcohol solvent, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.49X10
132Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 17-20.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 17-20, resulting adhesive force, sheet resistance value and film hardness such as table 5 are listed.
The composition and the characteristic of the conductive film layer of table 5 embodiment 17-20
Shown in table 5 test result; Than no auxiliary energy and the process conditions of short hardening time (5min); Coating metal electrically conductive ink on the surface-treated layer that adds Nano carbon balls; Have under 5 minutes treatment conditions of auxiliary energy, can obtain than high adhesion force (4B) and the low surface patch resistance (conductive film layer of 4.8 Ω/sq).
[embodiment 21-24]
The 5wt% polyvinyl alcohol (PVA) that will contain 1wt% CNT (bright prosperous science and technology, CN104Q CNT) is coated thickness 150 μ m with the mixture of alcohol solvent, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.07X10
132Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed adds the 10wt% that mixed proportion is above-mentioned silver metal printing ink again; Particle size is the spherical silver powder of 400nm, obtains final electrically conductive ink, through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 21-24.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 21-24, resulting adhesive force, sheet resistance value and film hardness such as table 6 are listed.
The composition and the characteristic of the conductive film layer of table 6 embodiment 21-24
Shown in table 6 test result; Process conditions than no auxiliary energy; Coating metal electrically conductive ink on the surface-treated layer that adds Nano carbon balls; Have under 10 minutes treatment conditions of auxiliary energy, it is close to obtain adhesive force (5B), and the surface patch resistance (conductive film layer that 0.19 Ω/sq) is lower.
[embodiment 25-28]
To contain the 55wt% acrylic resin of 0.1wt% graphite oxide (graphite oxide) and the mixture of 45wt% MEK (MEK) and coat thickness 150 μ m, glass transition temperature is 80 ℃, and insulaion resistance is 1.82x10
13On the PETG of Ω/sq (PET) base material, use the UV photocuring, form surface-treated layer, its insulaion resistance is greater than 10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 25-28.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 25-28, resulting adhesive force, sheet resistance value and film hardness such as table 7 are listed.
The composition and the characteristic of the conductive film layer of table 7 embodiment 25-28
Shown in table 7 test result; Curing process condition than no auxiliary energy; Coating metal electrically conductive ink on the acrylic resin surface-treated layer that adds graphite oxide; Have under 10 minutes conditions of cure of auxiliary energy, can obtain the conductive film layer that adhesive force increases (1B) and hardness close (5B).
[embodiment 29-32]
To contain the polyacrylic (U-Polymer) of 0.1wt% graphite oxide (graphite oxide) and the mixture of N-crassitude ketone solvent and coat thickness 150 μ m, glass transition temperature is 160 ℃, and insulaion resistance is greater than 10
14On the polyacrylic of Ω/sq (U-Polymer) base material, use the UV photocuring, form surface-treated layer, its insulaion resistance is 9.95X10
10Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 29-32.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 29-32, resulting adhesive force, sheet resistance value and film hardness such as table 8 are listed.
The composition and the characteristic of the conductive film layer of table 8 embodiment 29-32
Shown in table 8 test result, coating metal electrically conductive ink on the polyacrylic surface-treated layer that adds graphite oxide has under the process conditions of auxiliary energy, and it is good all can to obtain the sheet resistance characteristic, and the suitable conductive film layer of film hardness (6B).
[embodiment 33-36]
To contain the 55wt% acrylic resin of many walls of 0.1wt% type CNT (bright prosperous science and technology, CN104Q CNT) and the mixture of 45wt% MEK (MEK) and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.02X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 33-36.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 33-36, resulting adhesive force, sheet resistance value and film hardness such as table 9 are listed.
[comparative example 13-16]
The mixture of 55wt% acrylic resin and 45wt% MEK (MEK) is coated thickness 150 μ m, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form the surface treatment rete, its insulaion resistance is 1.02X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 13-16.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 13-16, resulting adhesive force, sheet resistance value and film hardness such as table 9 are listed
The composition of the conductive film layer of table 9 embodiment 33-36 and comparative example 13-16 and characteristic
X: the non-resistance value, the expression resistance value is too high
Shown in table 9 test result; Coating metal electrically conductive ink on the acrylic resin surface-treated layer that contains many walls of 0.1wt% type CNT; Have under the process conditions of auxiliary energy; Can under the curing of short time, obtain sheet resistance favorable conductive rete, and at 10 minutes the conductive film layer that can obtain adhesive force 3B hardening time.
[embodiment 37-40]
To contain the 55wt% acrylic resin of 0.1wt% graphite oxide and the mixture of 45wt% MEK (MEK), and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.42X10
14On the Merlon of Ω/sq (PC) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.02X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 37-40.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 37-40, resulting adhesive force, sheet resistance value and film hardness such as table 10 are listed.
The composition and the characteristic of the conductive film layer of table 10 embodiment 37-40
Shown in table 10 test result, containing coating metal electrically conductive ink on the acrylic resin surface-treated layer of 0.1wt% graphite oxide, have under the process conditions of auxiliary energy, can under the curing of short time, obtain sheet resistance favorable conductive rete.
[embodiment 41-44]
To contain many walls of 0.1wt% type CNT (bright prosperous science and technology; The CN104Q CNT) 55wt% Merlon (PC) is coated thickness 150 μ m with the mixture of 45wt% cyclopentanone (cyclopentanone); 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 7.78X10
12Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 41-44.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 41-44, resulting adhesive force, sheet resistance value and film hardness such as table 11 are listed.
[comparative example 17-20]
The 55wt% Merlon (PC) and the mixture of 45wt% cyclopentanone are coated thickness 150 μ m, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.14X10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 17-20.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 17-20, resulting adhesive force, sheet resistance value and film hardness such as table 11 are listed.
The composition of the conductive film layer of table 11 embodiment 41-44 and comparative example 17-20 and characteristic
Shown in table 11 test result; Containing coating metal electrically conductive ink on Merlon (PC) surface-treated layer of many walls of 0.1wt% type CNT; Have under the process conditions of auxiliary energy, obtaining the conductive film layer that attachment characteristic is good and hardness is high under can solidifying in the short time.
[embodiment 45-48]
The 55wt% Merlon (PC) that will contain the 0.1wt% graphite oxide is coated thickness 150 μ m with the mixture of 45wt% cyclopentanone, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 1.26X10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 45-48.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 45-48, resulting adhesive force, sheet resistance value and film hardness such as table 12 are listed.
The composition and the characteristic of the conductive film layer of table 12 embodiment 45-48
Shown in table 12 test result; Coating metal electrically conductive ink on the Merlon that contains the 0.1wt% graphite oxide (PC) surface-treated layer; Have under the process conditions of auxiliary energy, can obtain adhesive force and hardness (the favorable conductive rete of hardness performance 4B>5B>6B) 10 minutes hardening time.
[embodiment 49-52]
To contain the 55wt% Merlon of 0.1wt% clay and the mixture of 45wt% cyclopentanone, and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind 150 ℃ of baking-curings, form surface-treated layer, its insulaion resistance is 8.39X10
11Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 49-52.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 49-52, resulting adhesive force, sheet resistance value and film hardness such as table 13 are listed.
The composition and the characteristic of the conductive film layer of table 13 embodiment 49-52
Shown in table 13 test result, coating metal electrically conductive ink on the Merlon that contains the 0.1wt% clay (PC) surface-treated layer can obtain optimal hardness (the 2H) (conductive film layer of hardness performance H>B) under the curing with auxiliary energy.
[embodiment 53-56]
To contain the polyacrylic (U-Polymer) of many walls of 0.1wt% type CNT (bright prosperous science and technology, CN104Q CNT) and the mixture of N-crassitude ketone solvent and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind the use UV photocuring, form surface-treated layer, its insulaion resistance is 4.57X10
13Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 53-56.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 53-56, resulting adhesive force, sheet resistance value and film hardness such as table 14 are listed.
[comparative example 21-24]
The 55wt% polyacrylic (polyacrylic is called for short U-Polymer) and the mixture of N-crassitude ketone solvent are coated thickness 150 μ m, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, use UV light that polyacrylic is solidified, form surface-treated layer, its insulaion resistance is 1.42X10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of comparative example 21-24.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 21-24, resulting adhesive force, sheet resistance value and film hardness such as table 14 are listed.
The composition of the conductive film layer of table 14 embodiment 53-56 and comparative example 21-24 and characteristic
X: the non-resistance value, the expression resistance value is too high
Shown in table 14 test result; Coating metal electrically conductive ink on polyacrylic (U-Polymer) surface-treated layer that contains many walls of 0.1wt% type CNT and PETG (PET) base material; 10 minutes of auxiliary energy solidify down having, (hardness shows the conductive film layer of 3B>6B) can to obtain best adhesion and hardness.
[embodiment 57-60]
To contain the polyacrylic (U-Polymer) of 0.1wt% graphite oxide (graphite oxide) and the mixture of N-crassitude ketone solvent and coat thickness 150 μ m, 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind the use UV photocuring, form surface-treated layer, its insulaion resistance is 1.12X10
11Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 57-60.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 57-60, resulting adhesive force, sheet resistance value and film hardness such as table 15 are listed.
The composition and the characteristic of the conductive film layer of table 15 embodiment 57-60
Shown in table 15 test result; Coating metal electrically conductive ink on polyacrylic surface-treated layer that contains the 0.1wt% graphite oxide and PETG (PET) base material; 10 minutes of auxiliary energy solidify down having, (hardness shows the favorable conductive rete of 3B>6B) can to obtain hardness.
[embodiment 61-64]
The polyacrylic (U-Polymer) that will contain the 0.1wt% clay is coated thickness 150 μ m, and 125 ℃ of glass transition temperatures, insulaion resistance are 1.82x10
13On the PETG of Ω/sq (PET) base material, behind the use UV photocuring, form surface-treated layer, its insulaion resistance is 1.88X10
14Ω/sq.
With 50wt% organic acid silver (C
7H
15COOAg) be dissolved in the 50wt% xylenes, the silver metal printing ink that is uniformly mixed is through rotary coating process; Coat on the above-mentioned surface-treated layer; Adopt 150 ℃ ambient temperature, be aided with the sintering of far red light irradiation carrying out metallic conduction printing ink, form the conductive film layer of embodiment 61-64.
Utilize hundred lattice tests (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 61-64, resulting adhesive force, sheet resistance value and film hardness such as table 16 are listed.
The composition and the characteristic of the conductive film layer of table 16 embodiment 61-64
X: the non-resistance value, the expression resistance value is too high
Shown in table 16 test result; Coating metal electrically conductive ink on polyacrylic surface-treated layer that contains the 0.1wt% clay and PETG (PET) base material; Having under 10 minute hardening time of auxiliary energy, can obtain conductive characteristic favorable conductive rete.
In sum; Substrate in combination utilization of the present invention is arranged on the surface-treated layer between the polymer-based end and the conductive film layer; Reach simultaneously and improve conductive film layer and the adhesive force at the polymer-based end; And utilizing the conductive filling material in the surface-treated layer to deliver power to metallic conduction printing ink, additional conductive rete sintering in low process temperatures and shorter hardening time forms, therefore; Than in electrically conductive ink, adding the mode that macromolecule increases adhesive force traditionally, the thickness of conductive film layer of the present invention can thinning and is reached the favorable conductive characteristic.In addition, the surface-treated layer in the substrate in combination of the present invention is suitable for use on the flexible base, board, meets the application of flexible electronic industry.
Though the present invention discloses as above with preferred embodiment, so it is not that those skilled in the art under any the present invention are not breaking away from the spirit and scope of the present invention in order to qualification the present invention, and Ying Kezuo changes arbitrarily and retouches.Therefore, protection scope of the present invention should be as the criterion with the appended claims restricted portion.
Claims (15)
1. substrate in combination with conductive film layer comprises:
The polymer-based end;
Surface-treated layer was arranged on this polymer-based end; And
Conductive film layer is arranged on this surface-treated layer,
Wherein this surface-treated layer is assisted sintering packing material and high molecular composite; This conductive film layer is to be formed by metallic conduction printing ink sintering; And this assisted sintering packing material in this surface-treated layer has the energy conduction characteristic, and the auxiliary transmission energy is to this metallic conduction printing ink.
2. the substrate in combination with conductive film layer as claimed in claim 1, wherein the material at this polymer-based end comprises thermal plastic high polymer, thermosetting polymer or aforesaid combination, and the insulating surfaces resistance at this polymer-based end is 10
14Ω/sq to 10
16Ω/sq, the glass transition temperature at this polymer-based end is 80 ℃ to 160 ℃.
3. the substrate in combination with conductive film layer as claimed in claim 2; Wherein the material at this polymer-based end comprises polyesters macromolecule, polyacrylic acids macromolecule, Merlon family macromolecule, epoxy resin family macromolecule or polyurethane class high molecular, and wherein this polyesters macromolecule comprises PETG.
4. the substrate in combination with conductive film layer as claimed in claim 1; Wherein the part by weight of this assisted sintering packing material in this surface-treated layer is 0.01wt% to 5wt%, and this assisted sintering packing material is selected from nanotube, nanosphere, material with carbon element and clay.
5. the substrate in combination with conductive film layer as claimed in claim 4; Wherein this nanotube comprises SWCN, multi-walled carbon nano-tubes or aforesaid combination; This nanosphere comprises Nano carbon balls; This material with carbon element comprises graphite or graphite oxide, and this clay is selected from the clay compound that IA family oxide on the chemical periodic table, IIA family oxide and IVA family oxide are formed.
6. the substrate in combination with conductive film layer as claimed in claim 1, wherein this macromolecule in this surface-treated layer comprises thermal plastic high polymer, thermosetting polymer or aforesaid combination.
7. the substrate in combination with conductive film layer as claimed in claim 1, wherein this high molecular glass transition temperature in this surface-treated layer is 75 ℃ to 200 ℃.
8. the substrate in combination with conductive film layer as claimed in claim 7, wherein this macromolecule is selected from acrylic resin, polyacrylic, polyvinyl alcohol and Merlon.
9. the substrate in combination with conductive film layer as claimed in claim 1; Wherein the composition of this metallic conduction printing ink comprises the combination of metallo-organic compound and solvent; Or the combination of metallo-organic compound, metal-powder and solvent, and the part by weight of this metallo-organic compound in this metallic conduction printing ink is 25wt% to 60wt%.
10. the substrate in combination with conductive film layer as claimed in claim 9, wherein the chemical constitution of this organo-metallic compound is (RCOO)
yM
(y), and wherein R is the C of straight or branched
nH
2n+1, n is 5~20 integer; M is a metal, and it is selected from copper, silver, gold, aluminium, titanium, nickel, tin, platinum and palladium; Y is the valence mumber of metal.
11. the substrate in combination with conductive film layer as claimed in claim 9; Wherein the size of this metal-powder is less than 500nm; And this metal-powder is selected from copper, silver, gold, aluminium, titanium, nickel, tin, platinum and palladium, and this solvent is selected from xylenes, toluene and terpineol.
12. the manufacturing approach with substrate in combination of conductive film layer comprises:
The polymer-based end, be provided;
To contain assisted sintering packing material and high molecular mixture coated on this polymer-based end;
With this conductive filling material and high molecular mixture solidified, form surface-treated layer;
Metallic conduction printing ink is coated on this surface-treated layer; And
Apply first energy source; And auxiliary second energy source that applies; Make this metallic conduction printing ink sintering; Form conductive film layer, wherein this assisted sintering packing material in this surface-treated layer has the energy conduction characteristic, and the energy of this first energy source of auxiliary transmission and this second energy source is to this metallic conduction printing ink.
13. the manufacturing approach with substrate in combination of conductive film layer as claimed in claim 12; Wherein this first energy source and this second energy source are selected from heat, light, energy waves and laser; And this first energy source is different with this second energy source, and the temperature range of this first energy source is 90 ℃ to 150 ℃.
14. the manufacturing approach with substrate in combination of conductive film layer as claimed in claim 13; Wherein this light with energy is selected from ultraviolet light, near infrared light, mid-infrared light and far red light; This energy waves comprises the microwave of wavelength 300MHz to 300GHz, and this laser is selected from gaseous state laser, solid-state laser and liquid laser.
15. the manufacturing approach with substrate in combination of conductive film layer as claimed in claim 12, wherein this assisted sintering packing material and high molecular mixture, and this metallic conduction printing ink is coated with the wet coat processing procedure.
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