CN102555323B - 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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- CN102555323B CN102555323B CN201010616446.9A CN201010616446A CN102555323B CN 102555323 B CN102555323 B CN 102555323B CN 201010616446 A CN201010616446 A CN 201010616446A CN 102555323 B CN102555323 B CN 102555323B
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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 the manufacture method thereof with conductive film layer.
[background technology]
The application majority of current flexibility (flexible) electronic technology directly prints 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 flexible base board.
The mode increasing adhesive force between conducting wire and flexible base board traditionally can be divided into the electrically conductive ink upgrading type of the Adhesion enhancement for electrically conductive ink, and the substrate upgrading type of Adhesion enhancement for substrate.The mode of electrically conductive ink upgrading type such as utilizes mixing of Porous conductor material and Porous macromolecular material for mentioning in U.S. Patent Publication US 2007/0048514, increases the adhesive strength between conductor layer and polymeric substrate.In addition, in U.S. Patent Publication US 2004/0144958, mention that the macromolecular material adding low glass state inversion point (Tg) in electrically conductive ink promotes additive, to increase the adhesive force of ink to substrate as adhesion.
The mode of substrate upgrading type such as uses metal alkoxide layer to process in the mode of cracking, microwave or hydrolysis at substrate surface for mentioning in U.S. Patent Publication US 2009/0104474, forms oxide adhesion coating, to improve the adhesive force of substrate surface.In addition, mention in utilizing couplant (coupling agent) to be coated with one deck inorganic oxide at substrate surface in US Patent No. 5190795, recycling mode of heating makes it be attached to substrate surface, increases the adhesive force between substrate and metal by this.
The mode of above-mentioned electrically conductive ink upgrading type mainly adds macromolecular material in electrically conductive ink, promote the adhesive force between the conductive film layer after sintering (Sinter) and substrate by macromolecular material, but the macromolecular material in ink can reduce the conductivity degree of conductive film layer; And the mode of substrate upgrading type is such as mainly the adhesion coating of oxide in substrate surface formation, increase the adhesive force of substrate surface, but the adhesion coating of this substrate surface is except increasing adhesive force, there is no other adjections.
[summary of the invention]
The 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 the conductive film layer be arranged on surface-treated layer, wherein surface-treated layer formed by assisted sintering packing material and high molecular composite, conductive film layer is sintered by metallic conductive inks to form, assisted sintering packing material in surface-treated layer has energy conduction characteristics, its auxiliary transmission energy, to metallic conductive inks, contributes to the sintering of metallic conductive inks.
In addition, the present invention also provides a kind of manufacture method with the substrate in combination of conductive film layer, comprise: the polymer-based end is provided, to coat containing assisted sintering packing material and high molecular mixture at polymer-based the end, by this assisted sintering packing material and high molecular mixture solidified, form surface-treated layer, metallic conductive inks is coated on surface-treated layer, and apply the first energy source, and auxiliary applying second energy source, metallic conductive inks is sintered and forms conductive film layer, wherein the assisted sintering packing material of surface-treated layer has energy conduction characteristics, the energy of its auxiliary transmission first energy source and the second energy source is to metallic conductive inks, help the sintering of metallic conductive inks.
In order to above-mentioned purpose of the present invention, feature and advantage can more be become apparent, below in conjunction with accompanying drawing, be described in detail below:
[accompanying drawing explanation]
Fig. 1 shows the generalized section according to an embodiment of the present invention with the substrate in combination of conductive film layer.
Fig. 2 A to 2D figure shows the generalized section according to an embodiment of the present invention formation with each fabrication stage of the substrate in combination of conductive film layer.
[Main Reference Numerals explanation]
10 ~ polymer-based the end; 17 ~ metallic conductive inks;
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;
[detailed description of the invention]
Refer to Fig. 1, the generalized section of the substrate in combination 100 with conductive film layer of its display an embodiment of the present invention, this substrate in combination 100 comprises the polymer-based end 10, the polymer-based end 10 has surface-treated layer 16, and have conductive film layer 18 on surface-treated layer 16.
The polymer-based end 10 can be the flexible substrates be made up of thermal plastic high polymer, thermosetting polymer or aforesaid composite, such as, be PETG (polyethylene terephthalate; Be called for short 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
14more than Ω/ (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 (Tg) at the polymer-based end 10 can be more than 80 DEG C, preferably between 80 DEG C to 160 DEG C, more preferably between 100 DEG C to 150 DEG C.
Surface-treated layer 16 mainly formed by assisted sintering packing material 12 composite with macromolecule 14, and one of effect of surface-treated layer 16 is increase adhesive force at conductive film layer 18 and the polymer-based end 10 by macromolecule 14 wherein; Another effect of surface-treated layer 16 is then the curing action by assisted sintering packing material 12 reinforced metal electrically conductive ink wherein, forms conductive film layer 18.The insulating surfaces resistance of surface-treated layer 16 is 10
6Ω/more than sq, and the adhesive force between surface-treated layer 16 and the polymer-based end 10 and conductive film layer 18 is more than 4B.
In embodiments of the present invention, the part by weight of the assisted sintering packing material 12 in surface-treated layer 16, for being less than 5wt%, being preferably between 0.01wt% to 5wt%, being more preferably between 0.05wt% to 3wt%.Assisted sintering packing material 12 can be nanotube, nanosphere, material with carbon element, clay or aforesaid combination, and wherein nanotube is such as CNT, metal nano-tube or non pinetallic nano pipe; Nanosphere is such as Nano carbon balls, metal nano ball or non pinetallic nano ball; Material with carbon element is such as graphite or graphite oxide; Clay is such as the clay compound of IA race oxide on chemical periodic table, IIA race oxide and IVA race oxide composition.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 non pinetallic nano pipe and non pinetallic nano ball can be titanium oxide, manganese oxide, zinc oxide, silver oxide, iron oxide, tin oxide, nickel oxide, indium oxide or other metal oxides.
Macromolecule 14 in surface-treated layer 16 can be thermal plastic high polymer, thermosetting polymer or aforementioned composite, and its glass transition temperature is between 75 DEG C to 200 DEG C.Thermal plastic high polymer is such as polyethylene (polyethylene), polypropylene (polypropylene), polyformaldehyde (polyoxymethylene), Merlon (polycarbonate), polyvinyl chloride (polyvinylchloride), polyvinyl alcohol (polyvinyl alcohol), polymethyl methacrylate (polymethyl methacrylate), polystyrene (polystyrene), polyimides (polyimide), PEN (polyethylene naphthalate) or polyethylene glycol succinate (poly (ethylene succidate)), thermosetting polymer is such as epoxy resin (epoxy resin), acrylic resin (acrylic resin), unsaturated polyester (UP) (unsaturated polyester), phenolic resins (phenolic resin) or silicon polymer (silicon polymers).In addition, in surface-treated layer 16, except assisted sintering packing material 12 and macromolecule 14, other the inorganic or organic additives helping processing procedure processing or surface-treated layer characteristic can also be added with.
Conductive film layer 18 be by metallic conductive inks sinter form, in embodiments of the present invention, metallic conductive inks mainly consist of metallo-organic compound and solvent.In metallic conductive inks, metal-organic part by weight is below 60wt%, is preferably between 25wt% to 50wt%.Metallo-organic compound is the predecessor forming conductive film layer, and its chemical constitution is (RCOO)
ym
(y), wherein R is the C of straight or branched
nh
2n+1, n is the integer of 5 ~ 20; M is metal, and its kind comprises and is selected from least one material in copper, silver, gold, aluminium, titanium, nickel, tin, iron, platinum, palladium or other alternative materials; Y is the valence mumber of metal.Metallo-organic compound can via thermal cracking (Metallo-Organic Decomposition; MOD) react, reduction forms nano metal particles, relends the low temperature melting characteristic helping nano metal particles, forms the simple metal conductive film layer 18 of high conductivity, therefore can form the metallic diaphragm of high connductivity under low process temperatures.Utilize the conductive film layer 18 that metal-organic reduction mode is formed, its process temperatures depends on metal-organic reduction temperature.
Assisted sintering packing material 12 in surface-treated layer 16 has the characteristic of conduction energy, by the transmission effect of assisted sintering packing material 12 for heat, light or energy wave homenergic, can effectively transfer its energy in metallic conductive inks, metal-organic also proper energy rank in ink are changed, reduces its reduction temperature.In addition, assisted sintering packing material 12 also can transfer its energy to the nano metal particles of metallo-organic compound reduction, its local temperature is made to be increased to fusing point, the sintering temperature of effective reduction metallic conductive inks, and then simple metal conductive film layer 18 is formed under lower ambient temperature with in shorter hardening time (curing time), be therefore applicable to the polymer-based end 10 of low softening temperature.
In addition, in metallic conductive inks except metallo-organic compound and solvent, metal-powder can also be added, it can be spherical or the secondary micron of sheet and nano metal powder, 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 metallic conductive inks can be polarity or non-polar solven, such as, be dimethylbenzene (xylene), toluene (tolene), terpineol (terpenol) or aforesaid combination.In addition, other the inorganic or organic processing aid helping processing procedure processing or conductive film layer characteristic can also be added with in metallic conductive inks.
In addition, metallic conductive inks also can directly use metallic and solvent to combine, assisted sintering packing material 12 in surface-treated layer 16 can transfer its energy to metallic, its local temperature is made to be increased to fusing point, the sintering temperature of effective reduction metallic conductive inks, contributes to metallic conductive inks sintering and forms conductive film layer 18.
Refer to Fig. 2 A to 2D, its display, according to one embodiment of the present invention, forms the generalized section with each fabrication stage of the substrate in combination 100 of conductive film layer.Consult Fig. 2 A, first the polymer-based end 10 is provided, then coating method, the such as processing procedure such as rotary coating or serigraphy in a wet process, 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, utilize curing process 13, such as, be the mode such as UV light or heating, solidified by said mixture 11, removing solvent 15 wherein, forms surface-treated layer 16, as shown in Figure 2 B.
Consult Fig. 2 C, utilize wet coating mode, such as the processing procedure such as rotary coating or serigraphy, is coated on metallic conductive inks 17 on surface-treated layer 16.Then, the first energy source 30 is applied to the polymer-based end 10, surface-treated layer 16 and metallic conductive inks 17, and auxiliary applying second energy source 20, metallic conductive inks 17 is sintered, forms conductive film layer 18, as shown in Figure 2 D.In one embodiment, the resistivity of conductive film layer 18 is less than 10x10
-3Ω cm.
First energy source 30 and the second energy source 20 can be the forms such as heat, light, energy wave or laser, it is applied in the combination of the polymer-based end 10, surface-treated layer 16 and metallic conductive inks 17 by all directions, be not limited to the direction shown in Fig. 2 C, wherein thermal energy source can comprise: heat by conduction, advection heat or radiant heat homenergic source; Light energy source can comprise: ultraviolet light, near infrared light, mid-infrared light or far red light energy source; Energy wave comprises the microwave etc. of wavelength 300MHz ~ 300GHz; Laser energy sources comprises: gas laser, solid-state laser or liquid laser homenergic source, and wherein gas laser comprises: PRK, argon laser, carbon dioxide laser or hydrogen fluorine laser etc.; Solid-state laser can comprise: diode laser, and the wavelength of diode laser comprises 266nm, 355nm, 532nm or 1064nm etc.First energy source is different from the form of the second energy source, in one embodiment, the energy of the first energy source for providing by baking system, its temperature range between 90 DEG C to 150 DEG C, preferably between 100 DEG C to 130 DEG C, can be more preferably about 120 DEG C; Second energy source then irradiates for far red light, its auxiliary sintering carrying out metallic conductive inks 17.
Because the assisted sintering packing material 12 contained in surface-treated layer 16 has energy conduction characteristics, therefore can the energy of auxiliary transmission first energy source and the second energy source in metallic conductive inks 17, the sintering contributing to metallic conductive inks carries out, therefore can form conductive film layer 18 under lower ambient temperature with in shorter sintering time, make the polymer-based end 10 of low softening temperature to produce deformation.
Below enumerate each embodiment and comparative example and the manufacture method of substrate in combination 100 of the present invention, material and characteristic thereof be described:
[embodiment 1-4]
Will containing 1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) 55wt% acrylic resin and 45wt% MEK (methyl ethyl ketone, be called for short MEK) mixture, coat thickness 150 μm, glass transition temperature is 80 DEG C, and insulating surfaces resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after using UV photocuring, form surface-treated layer, its insulating surfaces resistance is greater than 10
14Ω/sq.
Then, by 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, form mixed uniformly silver metal electrically conductive ink, pass through rotary coating process, coat on surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light to irradiate, carry out the sintering of metallic conductive inks, form the conductive film layer of embodiment 1-4.
Utilize the test of hundred lattice (Cross-Cut Method) test (ASTM D3330), four-point probe method and hardness test (ASTM D3363) to measure the conductive film layer of embodiment 1-4, the adhesive force obtained, sheet resistance (Sheet Resistance) value and film hardness are as listed in table 1.
[comparative example 1-4]
The mixture of 55wt% acrylic resin and 45wt% MEK (MEK) is coated thickness 150 μm, and glass transition temperature is 80 DEG C, and insulating surfaces resistance is 1.82x10
13in the PET base material of Ω/sq, form surface-treated layer after using UV solidification, its insulating surfaces resistance is greater than 9.55X10
10Ω/sq.
By 39.8wt% organic acid silver (C
7h
15cOOAg) be dissolved in 59.7wt% dimethylbenzene, form mixed uniformly silver metal electrically conductive ink, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt hot processing procedure, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 1-4.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 1-4, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 1.
The composition of the conductive film layer of table 1 embodiment 1-4 and comparative example 1-4 and characteristic
As shown in table 1 test result, compared to the surface-treated layer not adding many wall-shaped CNT, there are 10 minutes auxiliary Infrared irradiations and in surface-treated layer, add the conductive film layer that many wall-shaped CNTs obtains and can obtain best surface resistance (surface resistance).In addition, compared to the condition without auxiliary energy, coating metal electrically conductive ink on the surface-treated layer adding many wall-shaped CNT, and under there is the condition of auxiliary energy, more stable conductive film layer hardness and adhesive force can be obtained.
[embodiment 5-8]
The mixture of the polyacrylic containing 1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) and 1-METHYLPYRROLIDONE solvent is coated thickness 150 μm, and glass transition temperature is 160 DEG C, and insulaion resistance is greater than 10
14on polyacrylic (U-Polymer) base material of Ω/sq, form surface-treated layer after using UV photocuring, its insulaion resistance is 9.95X10
10Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 5-8.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 5-8, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 2.
[comparative example 5-8]
The mixture of polyacrylic (U-Polymer) and 1-METHYLPYRROLIDONE solvent is coated thickness 150 μm, and glass transition temperature is 160 DEG C, and insulaion resistance is greater than 10
14on polyacrylic (U-Polymer) base material of Ω/sq, form surface-treated layer after using UV photocuring, its insulaion resistance is greater than 10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 5-8.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 5-8, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 2.
The composition of the conductive film layer of table 2 embodiment 5-8 and comparative example 5-8 and characteristic
X: non-resistance value, represents that resistance value is too high
As shown in table 2 test result, compared to the condition without auxiliary energy, coating metal electrically conductive ink on the polyacrylic surface-treated layer adding many wall-shaped CNT, have under the auxiliary energy treatment conditions of 10 minutes, the conductive film layer obtained has higher hardness 2B and adhesive force 5B.
[embodiment 9-12]
By the mixture of the 5wt% polyvinyl alcohol containing 1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) and alcohol solvent, coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.07X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 9-12.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 9-12, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 3.
[comparative example 9-12]
5wt% polyvinyl alcohol (PVA) and the mixture of alcohol solvent are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface treatment rete, its insulaion resistance is 1.02X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 9-12.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 9-12, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 3.
The composition of the conductive film layer of table 3 embodiment 9-12 and comparative example 9-12 and characteristic
As shown in table 3 test result, compared to the condition without auxiliary energy, coating metal electrically conductive ink on the polyvinyl alcohol surface-treated layer adding many wall-shaped CNT, under 10 minutes treatment conditions with auxiliary energy, adhesive force (4B) can be obtained high and stable, and the conductive film layer that surface patch resistance (0.35 Ω/sq) is lower.
[embodiment 13-16]
By the mixture of the 5wt% polyvinyl alcohol (PVA) containing 1wt% clay additive (Clay) with alcohol solvent, coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface treatment rete, its insulaion resistance is 5.34X10
12Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 13-16.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 13-16, the adhesive force obtained, sheet resistance values and film hardness are listed by table 4.
The composition of the conductive film layer of table 4 embodiment 13-16 and characteristic
As shown in table 4 test result, compared to the condition without auxiliary energy, coating metal electrically conductive ink on the surface-treated layer adding clay, under 5 minutes with auxiliary energy and 10 minutes treatment conditions, can obtain the conductive film layer that surface patch resistance value is lower and stable.
[embodiment 17-20]
5wt% polyvinyl alcohol (PVA) containing 1wt% Nano carbon balls (bright prosperous science and technology, CN107C Nano carbon balls) and the mixture of alcohol solvent are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.49X10
132Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 17-20.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 17-20, the adhesive force obtained, sheet resistance values and film hardness are as listed in table 5.
The composition of the conductive film layer of table 5 embodiment 17-20 and characteristic
As shown in table 5 test result, compared to without auxiliary energy and the process conditions of shorter hardening time (5min), coating metal electrically conductive ink on the surface-treated layer adding Nano carbon balls, under 5 minutes treatment conditions with auxiliary energy, comparatively high adhesion force (4B) and the conductive film layer of lower surface patch resistance (4.8 Ω/sq) can be obtained.
[embodiment 21-24]
5wt% polyvinyl alcohol (PVA) containing 1wt% CNT (bright prosperous science and technology, CN104Q CNT) and the mixture of alcohol solvent are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.07X10
132Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, add the 10wt% that mixed proportion is above-mentioned silver metallic ink again, particle size is the spherical silver powder of 400nm, obtains final electrically conductive ink, passes through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 21-24.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 21-24, the adhesive force obtained, sheet resistance values and film hardness are listed by table 6.
The composition of the conductive film layer of table 6 embodiment 21-24 and characteristic
As shown in table 6 test result, compared to the process conditions without auxiliary energy, coating metal electrically conductive ink on the surface-treated layer adding Nano carbon balls, under 10 minutes treatment conditions with auxiliary energy, adhesive force (5B) can be obtained close, and the conductive film layer that surface patch resistance (0.19 Ω/sq) is lower.
[embodiment 25-28]
The mixture of the 55wt% acrylic resin containing 0.1wt% graphite oxide (graphite oxide) and 45wt% MEK (MEK) is coated thickness 150 μm, and glass transition temperature is 80 DEG C, and insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, use UV photocuring, form surface-treated layer, its insulaion resistance is greater than 10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 25-28.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 25-28, the adhesive force obtained, sheet resistance values and film hardness are listed by table 7.
The composition of the conductive film layer of table 7 embodiment 25-28 and characteristic
As shown in table 7 test result, compared to the curing process condition without auxiliary energy, coating metal electrically conductive ink on the acrylic resin surface-treated layer adding graphite oxide, under 10 minutes conditions of cure with auxiliary energy, can obtain adhesive force increases (1B) and the conductive film layer of hardness close (5B).
[embodiment 29-32]
The mixture of the polyacrylic (U-Polymer) containing 0.1wt% graphite oxide (graphite oxide) and 1-METHYLPYRROLIDONE solvent is coated thickness 150 μm, and glass transition temperature is 160 DEG C, and insulaion resistance is greater than 10
14on polyacrylic (U-Polymer) base material of Ω/sq, use UV photocuring, form surface-treated layer, its insulaion resistance is 9.95X10
10Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 29-32.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 29-32, the adhesive force obtained, sheet resistance values and film hardness are listed by table 8.
The composition of the conductive film layer of table 8 embodiment 29-32 and characteristic
As shown in table 8 test result, coating metal electrically conductive ink on the polyacrylic surface-treated layer adding graphite oxide, under the process conditions with auxiliary energy, all can obtain sheet resistance characteristic good, and the conductive film layer that film hardness (6B) is suitable.
[embodiment 33-36]
Will containing 0.1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) 55wt% acrylic resin and the mixture of 45wt% MEK (MEK) coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.02X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 33-36.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 33-36, the adhesive force obtained, sheet resistance values and film hardness are listed by table 9.
[comparative example 13-16]
The mixture of 55wt% acrylic resin and 45wt% MEK (MEK) is coated thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface treatment rete, its insulaion resistance is 1.02X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 13-16.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 13-16, the adhesive force obtained, sheet resistance values and film hardness are listed by table 9
The composition of the conductive film layer of table 9 embodiment 33-36 and comparative example 13-16 and characteristic
X: non-resistance value, represents that resistance value is too high
As shown in table 9 test result, coating metal electrically conductive ink on the acrylic resin surface-treated layer containing 0.1wt% many wall-shaped CNT, under the process conditions with auxiliary energy, the good conductive film layer of sheet resistance can be obtained under the solidification of short time, and at the conductive film layer that can obtain adhesive force 3B hardening time of 10 minutes.
[embodiment 37-40]
By the mixture of the 55wt% acrylic resin containing 0.1wt% graphite oxide and 45wt% MEK (MEK), coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.42X10
14on Merlon (PC) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.02X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 37-40.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 37-40, the adhesive force obtained, sheet resistance values and film hardness are listed by table 10.
The composition of the conductive film layer of table 10 embodiment 37-40 and characteristic
As shown in table 10 test result, coating metal electrically conductive ink on the acrylic resin surface-treated layer containing 0.1wt% graphite oxide, under the process conditions with auxiliary energy, can obtain the good conductive film layer of sheet resistance under the solidification of short time.
[embodiment 41-44]
Will containing 0.1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) the mixture of 55wt% Merlon (PC) and 45wt% cyclopentanone (cyclopentanone) coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 7.78X10
12Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 41-44.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 41-44, the adhesive force obtained, sheet resistance values and film hardness are listed by table 11.
[comparative example 17-20]
55wt% Merlon (PC) and the mixture of 45wt% cyclopentanone are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.14X10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 17-20.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 17-20, the adhesive force obtained, sheet resistance values and film hardness are listed by table 11.
The composition of the conductive film layer of table 11 embodiment 41-44 and comparative example 17-20 and characteristic
As shown in table 11 test result, coating metal electrically conductive ink on Merlon (PC) surface-treated layer containing 0.1wt% many wall-shaped CNT, under the process conditions with auxiliary energy, the good and conductive film layer that hardness is high of attachment characteristic can be obtained under short time solidification.
[embodiment 45-48]
55wt% Merlon (PC) containing 0.1wt% graphite oxide and the mixture of 45wt% cyclopentanone are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 1.26X10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 45-48.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 45-48, the adhesive force obtained, sheet resistance values and film hardness are listed by table 12.
The composition of the conductive film layer of table 12 embodiment 45-48 and characteristic
As shown in table 12 test result, coating metal electrically conductive ink on Merlon (PC) surface-treated layer containing 0.1wt% graphite oxide, under the process conditions with auxiliary energy, adhesive force and the good conductive film layer of hardness (hardness shows 4B > 5B > 6B) can be obtained the hardening time of 10 minutes.
[embodiment 49-52]
By the mixture of the 55wt% Merlon containing 0.1wt% clay and 45wt% cyclopentanone, coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after 150 DEG C of baking-curings, form surface-treated layer, its insulaion resistance is 8.39X10
11Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 49-52.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 49-52, the adhesive force obtained, sheet resistance values and film hardness are listed by table 13.
The composition of the conductive film layer of table 13 embodiment 49-52 and characteristic
As shown in table 13 test result, coating metal electrically conductive ink on Merlon (PC) surface-treated layer containing 0.1wt% clay, can obtain the conductive film layer of optimal hardness (2H) (hardness performance H > B) under the solidification with auxiliary energy.
[embodiment 53-56]
Will containing 0.1wt% many wall-shaped CNT (bright prosperous science and technology, CN104Q CNT) polyacrylic (U-Polymer) and the mixture of 1-METHYLPYRROLIDONE solvent coat thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after using UV photocuring, form surface-treated layer, its insulaion resistance is 4.57X10
13Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 53-56.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 53-56, the adhesive force obtained, sheet resistance values and film hardness are listed by table 14.
[comparative example 21-24]
55wt% polyacrylic (polyacrylic is called for short U-Polymer) and the mixture of 1-METHYLPYRROLIDONE solvent are coated thickness 150 μm, glass transition temperature 125 DEG C, and insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, use UV light to be solidified by polyacrylic, form surface-treated layer, its insulaion resistance is 1.42X10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of comparative example 21-24.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of comparative example 21-24, the adhesive force obtained, sheet resistance values and film hardness are listed by table 14.
The composition of the conductive film layer of table 14 embodiment 53-56 and comparative example 21-24 and characteristic
X: non-resistance value, represents that resistance value is too high
As shown in table 14 test result, coating metal electrically conductive ink on polyacrylic (U-Polymer) surface-treated layer containing 0.1wt% many wall-shaped CNT and PETG (PET) base material, under the solidifications in 10 minutes with auxiliary energy, the conductive film layer of best adhesion and hardness (hardness shows 3B > 6B) can be obtained.
[embodiment 57-60]
The mixture of the polyacrylic (U-Polymer) containing 0.1wt% graphite oxide (graphite oxide) and 1-METHYLPYRROLIDONE solvent is coated thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after using UV photocuring, form surface-treated layer, its insulaion resistance is 1.12X10
11Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 57-60.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 57-60, the adhesive force obtained, sheet resistance values and film hardness are listed by table 15.
The composition of the conductive film layer of table 15 embodiment 57-60 and characteristic
As shown in table 15 test result, coating metal electrically conductive ink on the polyacrylic surface-treated layer containing 0.1wt% graphite oxide and PETG (PET) base material, under the solidifications in 10 minutes with auxiliary energy, the conductive film layer that hardness (hardness performance 3B > 6B) is good can be obtained.
[embodiment 61-64]
Polyacrylic (U-Polymer) containing 0.1wt% clay is coated thickness 150 μm, glass transition temperature 125 DEG C, insulaion resistance is 1.82x10
13on PETG (PET) base material of Ω/sq, after using UV photocuring, form surface-treated layer, its insulaion resistance is 1.88X10
14Ω/sq.
By 50wt% organic acid silver (C
7h
15cOOAg) be dissolved in 50wt% dimethylbenzene, the silver metallic ink be uniformly mixed, pass through rotary coating process, coat on above-mentioned surface-treated layer, adopt the ambient temperature of 150 DEG C, be aided with far red light and irradiate the sintering carrying out metallic conductive inks, form the conductive film layer of embodiment 61-64.
Utilize hundred lattice test (ASTM D3330), four-point probe method test and hardness test (ASTMD3363) to measure the conductive film layer of embodiment 61-64, the adhesive force obtained, sheet resistance values and film hardness are listed by table 16.
The composition of the conductive film layer of table 16 embodiment 61-64 and characteristic
X: non-resistance value, represents that resistance value is too high
As shown in table 16 test result, coating metal electrically conductive ink on the polyacrylic surface-treated layer containing 0.1wt% clay and PETG (PET) base material, under 10 minute hardening time with auxiliary energy, the conductive film layer that conductive characteristic is good can be obtained.
In sum, substrate in combination of the present invention utilizes the surface-treated layer be arranged between the polymer-based end and conductive film layer, reach simultaneously and improve conductive film layer and the adhesive force at the polymer-based end, and utilize the conductive filling material in surface-treated layer to deliver power to metallic conductive inks, additional conductive rete sinters and is formed in low process temperatures with shorter hardening time, therefore, increase the mode of adhesive force compared to adding macromolecule traditionally in electrically conductive ink, the thickness of conductive film layer of the present invention can thinning reach good conductive characteristic.In addition, the surface-treated layer in substrate in combination of the present invention is suitable for use on flexible base board, meets the application of flexible electronic industry.
Although the present invention with preferred embodiment disclose as above, so itself and be not used to limit the present invention, any the technical staff in the technical field of the invention, without departing from the spirit and scope of the present invention, Ying Kezuo changes arbitrarily and retouches.Therefore, the scope that protection scope of the present invention should limit with appended claims is as the criterion.
Claims (15)
1. there is a substrate in combination for conductive film layer, comprising:
The polymer-based end;
Surface-treated layer, is 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 sintered by metallic conductive inks to form, and this assisted sintering packing material in this surface-treated layer has energy conduction characteristics, auxiliary transmission energy is to this metallic conductive inks, and this assisted sintering packing material is selected from the group of SWCN, multi-walled carbon nano-tubes, Nano carbon balls, graphite and graphite oxide composition.
2. have the substrate in combination of 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 DEG C to 160 DEG C.
3. there is the substrate in combination of conductive film layer as claimed in claim 2, wherein the material at this polymer-based end comprises polyesters macromolecule, polyacrylic acid family macromolecule, Merlon family macromolecule, epoxy resin family macromolecule or polyurethane class high molecular, and wherein this polyesters macromolecule comprises PETG.
4. have the substrate in combination of 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%.
5. have the substrate in combination of conductive film layer as claimed in claim 1, this macromolecule wherein in this surface-treated layer comprises thermal plastic high polymer, thermosetting polymer or aforesaid combination.
6. have the substrate in combination of conductive film layer as claimed in claim 1, this high molecular glass transition temperature wherein in this surface-treated layer is 75 DEG C to 200 DEG C.
7. have the substrate in combination of conductive film layer as claimed in claim 6, wherein this macromolecule is selected from polyacrylic, polyvinyl alcohol and Merlon.
8. there is the substrate in combination of conductive film layer as claimed in claim 1, wherein the composition of this metallic conductive inks 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 conductive inks is 25wt% to 60wt%.
9. have the substrate in combination of conductive film layer as claimed in claim 8, 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 the integer of 5 ~ 20; M is metal, and it is selected from copper, silver, gold, aluminium, titanium, nickel, tin, platinum and palladium; Y is the valence mumber of metal.
10. there is the substrate in combination of conductive film layer as claimed in claim 8, 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, this solvent is selected from dimethylbenzene, toluene and terpineol.
11. substrate in combination as claimed in claim 6 with conductive film layer, wherein this macromolecule is acrylic resin.
12. 1 kinds of manufacture methods with the substrate in combination of conductive film layer, comprising:
The polymer-based end, is provided;
To coat on this polymer-based end containing assisted sintering packing material and high molecular mixture;
By this conductive filling material and high molecular mixture solidified, form surface-treated layer;
Metallic conductive inks is coated on this surface-treated layer; And
Apply the first energy source, and auxiliary applying second energy source, this metallic conductive inks is sintered, form conductive film layer, this assisted sintering packing material wherein in this surface-treated layer has energy conduction characteristics, and the energy of this first energy source of auxiliary transmission and this second energy source is to this metallic conductive inks.
13. manufacture methods as claimed in claim 12 with the substrate in combination of conductive film layer, wherein this first energy source and this second energy source are selected from heat, light, energy wave and laser, and this first energy source is different from this second energy source, the temperature range being wherein selected from this first energy source of heat is 90 DEG C to 150 DEG C.
14. manufacture methods as claimed in claim 13 with the substrate in combination of conductive film layer, wherein this light with energy is selected from ultraviolet light, near infrared light, mid-infrared light and far red light, this energy wave comprises the microwave of wavelength 300MHz to 300GHz, and this laser is selected from gas laser, solid-state laser and liquid laser.
15. manufacture methods as claimed in claim 12 with the substrate in combination of conductive film layer, wherein this assisted sintering packing material and high molecular mixture, and this metallic conductive inks in a wet process coating process be coated with.
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| US9905327B2 (en) | 2015-11-20 | 2018-02-27 | Industrial Technology Research Institute | Metal conducting structure and wiring structure |
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| CN103187118B (en) * | 2013-02-06 | 2015-02-18 | 南昌欧菲光科技有限公司 | Conductive film, manufacturing method for conductive film and touch screen with conductive film |
| EP3337657B1 (en) | 2015-08-18 | 2020-05-06 | Hewlett-Packard Development Company, L.P. | Composite material |
| TWI608639B (en) | 2016-12-06 | 2017-12-11 | 財團法人工業技術研究院 | Flexible thermoelectric structure and method for manufacturing the same |
| CN108359308A (en) * | 2018-02-24 | 2018-08-03 | 东莞市银泰丰光学科技有限公司 | A method of heat dissipation ink and glass light guide plate printing heat dissipation ink |
| CN109246925B (en) | 2018-08-28 | 2020-03-31 | 庆鼎精密电子（淮安）有限公司 | Manufacturing method of soft and hard board |
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