CN109810576A - A kind of ultraviolet light solidification electrically conductive ink and preparation method thereof - Google Patents
A kind of ultraviolet light solidification electrically conductive ink and preparation method thereof Download PDFInfo
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- CN109810576A CN109810576A CN201711160715.3A CN201711160715A CN109810576A CN 109810576 A CN109810576 A CN 109810576A CN 201711160715 A CN201711160715 A CN 201711160715A CN 109810576 A CN109810576 A CN 109810576A
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Abstract
The present invention relates to a kind of ultraviolet light solidification electrically conductive inks and preparation method thereof, electrically conductive ink includes following components and parts by weight content: 11.1-18.2 parts of polyurethane acrylate prepolymer, 12-15 parts of 1,6- hexylene glycol double methacrylate, 0.2-0.4 parts of photoinitiator and 65-70 parts of silver powder；When preparation, after 1,6- hexylene glycol double methacrylate is heated to 45-55 DEG C, photoinitiator is added, is then cooled to 25-35 DEG C, and successively adds silver powder, polyurethane acrylate prepolymer, mixture is obtained, is successively stirred mixture grinding distribution, filtering, homogeneous to get electrically conductive ink is arrived.Compared with prior art, the present invention has the extensive adaptability to different printed substrates, can satisfy the environmental requirement of European Union ROSH and WEEE, has a extensive future.
Description
Technical field
The invention belongs to electrically conductive ink technical field, it is related to a kind of ultraviolet light solidification electrically conductive ink and preparation method thereof.
Background technique
Electrically conductive ink is widely used in the fields such as printed circuit, semiconductor packages, solar battery.Currently, conductive oil
The curing mode of ink is mainly heat cure, and this curing process has the drawbacks such as energy consumption is high, curing time is long, and is solidifying
Cheng Zhong can be polluted the environment, it is difficult to meet the increasingly stringent environmental protection condition requirement of electronic technology because of the volatilization of a large amount of solvent.
The advantage that UV-curing technology has economic, energy conservation, curing rate fast and environmental-friendly, be widely used in chemical industry, machinery,
The fields such as electronics and communication.Curing rate can not only be accelerated using the electrically conductive ink of UV-curing technology, promote production effect
Rate, and have on printed with fine degree and be obviously improved (technique that is heating and curing can be such that printed pattern spreads).Current Domestic pair
It is more more and more intense in the requirement of high-fineness printing technology, such as touch screen conducting wire, RFID antenna conducting wire, automobile remove
Mist line etc., but electrically conductive ink manufacturer domestic at present can not produce satisfactory ultraviolet light solidification electrically conductive ink, nothing
Method meets the needs of market solidifies electrically conductive ink for ultraviolet light.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of solidifications of ultraviolet light to lead
Electric ink and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of ultraviolet light solidification electrically conductive ink, which is characterized in that the electrically conductive ink includes following components and parts by weight content:
11.1-18.2 parts of polyurethane acrylate prepolymer, 12-15 parts of 1,6-HD double methacrylate, 0.2-0.4 parts of photoinitiator
And 65-70 parts of silver powder.
Using silver powder as conductive phase, the electric conductivity of electrically conductive ink can be enhanced；Using polyurethane acrylate prepolymer
As Binder Phase, it is aided with photoinitiator, can makes silver paste that there is the characteristic of photocuring, and enhance to the extensive of different printed substrates
Adaptability；Using solventless formulation, the environmental requirement of European Union ROSH and WEEE can satisfy.
Further, the polyurethane acrylate prepolymer includes following components and parts by weight content: toluene two is different
5-8 parts of cyanate, 5-8 parts of polyethylene glycol, 1-2 parts of hydroxyethyl methacrylate and 0.1-0.2 parts of dibutyl tin dilaurate.
Further, the polyurethane acrylate prepolymer preparation process the following steps are included:
1) toluene di-isocyanate(TDI) is added into reaction kettle, and is warming up to 35-45 DEG C, later with 1.2-1.8h by poly- second
Glycol is added dropwise in reaction kettle, the reaction was continued 2-3h after being added dropwise to complete；
2) reaction kettle is warming up to 65-75 DEG C, it later will be dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate
It is added into reaction kettle, arrives the polyurethane acrylate prepolymer after reaction 2.5-3.5h.
Further, the photoinitiator includes following components and parts by weight content: 2- isopropyl thioxanthone 0.1-
0.2 part and 0.1-0.2 parts of phosphine oxide of phenyl bis- (2,4,6- trimethylbenzoyls).
Further, the silver powder is super fine silver powder.
The partial size of the super fine silver powder is 5-6 μm as a preferred technical solution,.
A kind of ultraviolet light solidifies the preparation method of electrically conductive ink, this method are as follows: heats 1,6- hexylene glycol double methacrylate
To after 45-55 DEG C, photoinitiator is added, is then cooled to 25-35 DEG C, and it is poly- successively to add silver powder, polyurethane acrylate prepolymer
Object obtains mixture, successively stirs mixture grinding distribution, filtering, homogeneous to get the electrically conductive ink is arrived.
The weighing of each component cooperates record group as weighing tool using plum Teller-support benefit BBA211 type electronic scale
Part, operator can add the raw material of corresponding code name according to Display panel value, and precision controlling is in a ten thousandth.
Further, the grinding distribution process the following steps are included:
1) mixture is stirred, silver powder is made to be uniformly dispersed；
2) mixture is once ground on three-roll grinder, is stirred later；
3) secondary grinding is carried out to mixture on three-roll grinder, be stirred later；
4) mixture is ground on three-roll grinder three times, is stirred later.
In step 1), first the material barrel equipped with mixture is moved on high speed dispersion machine platform, is then turned on high speed point
Machine switch is dissipated, stirring-head is down to away from variable frequency switch at the 2cm of bucket bottom, is opened to 60Hz, continuously stirs 3min after timing is set, most
Observation silver paste is integrally in silver gray slurry and without silver powder particles afterwards, then is uniformly dispersed.
Further, in a process of lapping, the gap between the fast roller and central roll of three-roll grinder is 0.25-
0.30mm；In the secondary process of lapping, the gap between the fast roller and central roll of three-roll grinder is 0.20-0.25mm；Institute
In the process of lapping three times stated, the gap between the fast roller and central roll of three-roll grinder is 0.15-0.20mm.
By carrying out gradient type grinding to mixture, by easy stages it is gradually reduced the fineness of mixture.In regulating roller
The uniformity coefficient of discharging is also observed during gap, carry out process detection after grinding three times.
Further, after grinding three times, fineness≤10 μm of mixture.Subsequent step is carried out when detecting fineness≤10 μm
Suddenly.
Further, described to be filtered into vacuum filter.Vacuum filtration step is the silk-screen of the used mesh number of analog subscriber
Halftone carries out vacuum filter, and main function is to separate the large granular impurity generated in process of lapping.Vacuum filtration process
Connection stainless steel cavity is pumped using powerful vacuum, stainless steel material barrel is placed in stainless steel cavity, is finally existed as needed
The stainless (steel) wire of installation 250-400 mesh above stainless steel cavity.In use, vacuum pump switch is first opened, then in stainless (steel) wire
On constantly topple over the conductive silver paste that grinding distribution finishes, blend rubber scraper plate constantly paves silver paste, makes its rapid filtration to built-in
In stainless steel material barrel.The low-temperature conductive silver paste in material barrel is semi-finished product to be checked at this time, and inspector is according to examination criteria pair
It is detected, and detected value carries out subsequent step after reaching standard.By using homemade vacuum filter, can effectively simulate
The silk-screen printing effect of client filters out electrically conductive ink impurity produced during the preparation process.
Further, the homogeneous whipping process carries out in homogenizer.The effect of homogeneous stirring is mainly to conduction
Ink carries out deaeration and prevents silver powder from settling, and the conductive silver paste after homogeneous can be very fine and smooth uniform.In use, vacuum degree is set as
0.08-0.12Mpa, then the conductive silver paste that tinning is finished are put into stirring 3min in homogenizer.Low temperature after homogeneous stirring
Conductive silver paste can directly outbound it is filling.It by using homogeneous blender, can effectively make electrically conductive ink deaeration, and make each group
Divide and be further sufficiently mixed, reaches more preferably fineness.
Compared with prior art, the invention has the characteristics that:
1) it is designed by the formula to ink coating, different raw material is screened, are compounded, prepare novel purple
Outer light curable conductive ink, wherein the selection of silver powder is equal to the electric conductivity of electrically conductive ink coating, bending resistance and adhesive force
It is promoted；Using polyurethane acrylate prepolymer as Binder Phase, it is aided with photoinitiator, can makes silver paste that there is photocuring
Characteristic, and enhance to the extensive adaptability of different printed substrates；Select solventless formulation special to the environmental protection of conductive silver paste coating
The performances such as property, curing rate, printed with fine degree have promotion castering action；
2) preparation process for solidifying electrically conductive ink to ultraviolet light is designed and optimizes, and obtains the stable conductive oil of performance
Ink, and make the electrically conductive ink that there is apparent defoaming effect, and advanced optimized ink fineness.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.The present embodiment is based on the technical solution of the present invention
Implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention be not limited to it is following
Embodiment.
Embodiment 1-5:
Ultraviolet light solidify electrically conductive ink each component and content it is as shown in table 1.Urethane acrylate as Binder Phase
The preparation process of prepolymer are as follows: will first react, then added dissolved with tin dilaurate after toluene di-isocyanate(TDI) and polyethylene glycol heating
The hydroxyethyl methacrylate of dibutyl tin simultaneously heats reaction and is made；The macromolecule resin used is the double acrylic acid of 1,6-HD
Ester；The photoinitiator used is 2- isopropyl thioxanthone and bis- (2,4,6- trimethylbenzoyl) phosphine oxides of phenyl；It uses
Silver powder be super fine silver powder, average grain diameter is at 5-6 μm.
1 ultraviolet light of table solidifies the component and content of electrically conductive ink
Toluene di-isocyanate(TDI) is added in reaction kettle according to formula rate, and is gradually heated to 40 DEG C, then by poly- second
Glycol is added reaction kettle in a manner of being added dropwise, time for adding 1.5h, the reaction was continued after being added dropwise to complete 2.5h.Then, it will react
Kettle is warming up to 70 DEG C, will dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate be added reaction kettle, react 3h after while hot
Discharging, obtains polyurethane acrylate prepolymer, is kept in dark place.The step of ingredient, has used Mei Tele-support benefit BBA211 type
Electronic scale cooperates record component as weighing tool, and operator can add the former material of corresponding code name according to Display panel value
Material, precision controlling is in a ten thousandth.The sequence of batch weighing is: 1,6-HD double methacrylate is warming up to 50 DEG C → addition
Photoinitiator → be cooled to 30 DEG C → addition super fine silver powder → addition polyurethane acrylate prepolymer.
Material barrel is moved on high speed dispersion machine platform after weighing, high speed disperser switch is then turned on, will stir
It mixes head to be down to away from variable frequency switch at the 2cm of bucket bottom, is opened to 60Hz, continuously stirs 3min after timing is set.Then material barrel is moved
To three-roll grinder platform, the rolling of three-roll grinder needs three circulations, every to have rolled a silver paste and require to carry out again
A time high speed dispersion step.Then the continuous gap controlled in three-roll grinder between fast roller and central roll by easy stages, first
All over the roller gap of grinding low-temperature conductive silver paste in 0.3mm, second time roller gap is controlled in 0.25mm, third all over roller gap
0.2mm.It is up to 10 μm of fineness material barrels below and moves to vacuum filter platform, it is stainless that 300 purposes are installed above filter
Steel mesh is simultaneously complete by ink filter.Complete semi-finished product, which will be filtered, transfers to detection department to detect, and carries out after reaching company standard
Matter stirring, is set as 0.12Mpa for vacuum degree, then the silver paste that tinning is finished is put into stirring 3min in homogenizer.Ultraviolet light
The performance of curing conductive ink is as shown in table 2.
2 ultraviolet light of table solidifies the performance test results of electrically conductive ink
Embodiment 6:
A kind of ultraviolet light solidification electrically conductive ink, which includes following components and parts by weight content: polyurethane propylene
11.1 parts of acid esters prepolymer, 15 parts of 1,6-HD double methacrylate, 0.2 part of photoinitiator and 70 parts of silver powder.
Wherein, polyurethane acrylate prepolymer includes following components and parts by weight content: 5 parts of toluene di-isocyanate(TDI),
8 parts of polyethylene glycol, 1 part of hydroxyethyl methacrylate and 0.2 part of dibutyl tin dilaurate.Polyurethane acrylate prepolymer
Preparation process the following steps are included:
1) toluene di-isocyanate(TDI) is added into reaction kettle, and is warming up to 35 DEG C, later dripped polyethylene glycol with 1.8h
It adds in reaction kettle, the reaction was continued 2h after being added dropwise to complete；
2) reaction kettle is warming up to 75 DEG C, will be added later dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate
Into reaction kettle, polyurethane acrylate prepolymer is arrived after reaction 2.5h.
Photoinitiator includes following components and parts by weight content: 0.2 part of 2- isopropyl thioxanthone and the bis- (2,4,6- of phenyl
Trimethylbenzoyl) 0.1 part of phosphine oxide；Silver powder is super fine silver powder.
Ultraviolet light solidify electrically conductive ink the preparation method comprises the following steps: by 1, after 6- hexylene glycol double methacrylate is heated to 55 DEG C, add
Enter photoinitiator, be then cooled to 25 DEG C, and successively add silver powder, polyurethane acrylate prepolymer, obtains mixture, successively
Homogeneous stirring is carried out by mixture grinding distribution, filtering, and in homogenizer to get electrically conductive ink is arrived.
Wherein, grinding distribution process the following steps are included:
1) mixture is stirred, silver powder is made to be uniformly dispersed；
2) mixture is once ground on three-roll grinder, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.30mm, is stirred later；
3) secondary grinding is carried out to mixture on three-roll grinder, controlled between the fast roller of three-roll grinder and central roll
Gap is 0.25mm, is stirred later；
4) mixture is ground on three-roll grinder three times, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.20mm, is stirred later, after grinding three times, fineness≤10 μm of mixture.
Embodiment 7:
A kind of ultraviolet light solidification electrically conductive ink, which includes following components and parts by weight content: polyurethane propylene
18.2 parts of acid esters prepolymer, 12 parts of 1,6-HD double methacrylate, 0.4 part of photoinitiator and 65 parts of silver powder.
Wherein, polyurethane acrylate prepolymer includes following components and parts by weight content: 8 parts of toluene di-isocyanate(TDI),
5 parts of polyethylene glycol, 2 parts of hydroxyethyl methacrylate and 0.1 part of dibutyl tin dilaurate.Polyurethane acrylate prepolymer
Preparation process the following steps are included:
1) toluene di-isocyanate(TDI) is added into reaction kettle, and is warming up to 45 DEG C, later dripped polyethylene glycol with 1.2h
It adds in reaction kettle, the reaction was continued 3h after being added dropwise to complete；
2) reaction kettle is warming up to 65 DEG C, will be added later dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate
Into reaction kettle, polyurethane acrylate prepolymer is arrived after reaction 3.5h.
Photoinitiator includes following components and parts by weight content: 0.1 part of 2- isopropyl thioxanthone and the bis- (2,4,6- of phenyl
Trimethylbenzoyl) 0.2 part of phosphine oxide；Silver powder is super fine silver powder.
Ultraviolet light solidify electrically conductive ink the preparation method comprises the following steps: by 1, after 6- hexylene glycol double methacrylate is heated to 45 DEG C, add
Enter photoinitiator, be then cooled to 35 DEG C, and successively add silver powder, polyurethane acrylate prepolymer, obtains mixture, successively
Homogeneous stirring is carried out by mixture grinding distribution, filtering, and in homogenizer to get electrically conductive ink is arrived.
Wherein, grinding distribution process the following steps are included:
1) mixture is stirred, silver powder is made to be uniformly dispersed；
2) mixture is once ground on three-roll grinder, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.25mm, is stirred later；
3) secondary grinding is carried out to mixture on three-roll grinder, controlled between the fast roller of three-roll grinder and central roll
Gap is 0.20mm, is stirred later；
4) mixture is ground on three-roll grinder three times, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.15mm, is stirred later, after grinding three times, fineness≤10 μm of mixture.
Embodiment 8:
A kind of ultraviolet light solidification electrically conductive ink, which includes following components and parts by weight content: polyurethane propylene
14.65 parts of acid esters prepolymer, 13 parts of 1,6-HD double methacrylate, 0.3 part of photoinitiator and 67 parts of silver powder.
Wherein, polyurethane acrylate prepolymer includes following components and parts by weight content: 6 parts of toluene di-isocyanate(TDI),
7 parts of polyethylene glycol, 1.5 parts of hydroxyethyl methacrylate and 0.15 part of dibutyl tin dilaurate.Polyurethane acrylate prepolymer is poly-
The preparation process of object the following steps are included:
1) toluene di-isocyanate(TDI) is added into reaction kettle, and is warming up to 40 DEG C, later dripped polyethylene glycol with 1.5h
It adds in reaction kettle, the reaction was continued 2.5h after being added dropwise to complete；
2) reaction kettle is warming up to 70 DEG C, will be added later dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate
Into reaction kettle, polyurethane acrylate prepolymer is arrived after reaction 3h.
Photoinitiator includes following components and parts by weight content: 0.15 part of 2- isopropyl thioxanthone and phenyl it is bis- (2,4,
6- trimethylbenzoyl) 0.15 part of phosphine oxide；Silver powder is super fine silver powder.
Ultraviolet light solidify electrically conductive ink the preparation method comprises the following steps: by 1, after 6- hexylene glycol double methacrylate is heated to 50 DEG C, add
Enter photoinitiator, be then cooled to 30 DEG C, and successively add silver powder, polyurethane acrylate prepolymer, obtains mixture, successively
Homogeneous stirring is carried out by mixture grinding distribution, filtering, and in homogenizer to get electrically conductive ink is arrived.
Wherein, grinding distribution process the following steps are included:
1) mixture is stirred, silver powder is made to be uniformly dispersed；
2) mixture is once ground on three-roll grinder, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.258mm, is stirred later；
3) secondary grinding is carried out to mixture on three-roll grinder, controlled between the fast roller of three-roll grinder and central roll
Gap is 0.23mm, is stirred later；
4) mixture is ground on three-roll grinder three times, is controlled between the fast roller of three-roll grinder and central roll
Gap is 0.18mm, is stirred later, after grinding three times, fineness≤10 μm of mixture.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of ultraviolet light solidifies electrically conductive ink, which is characterized in that the electrically conductive ink includes following components and parts by weight content: poly-
11.1-18.2 parts of urethane acrylate prepolymer, 12-15 parts of 1,6-HD double methacrylate, 0.2-0.4 parts of photoinitiator and
65-70 parts of silver powder.
2. a kind of ultraviolet light according to claim 1 solidifies electrically conductive ink, which is characterized in that the polyurethane acroleic acid
Ester prepolymer includes following components and parts by weight content: 5-8 parts of toluene di-isocyanate(TDI), 5-8 parts of polyethylene glycol, methacrylic acid
1-2 parts of hydroxyl ethyl ester and 0.1-0.2 parts of dibutyl tin dilaurate.
3. a kind of ultraviolet light according to claim 2 solidifies electrically conductive ink, which is characterized in that the polyurethane acroleic acid
The preparation process of ester prepolymer the following steps are included:
1) toluene di-isocyanate(TDI) is added into reaction kettle, and is warming up to 35-45 DEG C, later with 1.2-1.8h by polyethylene glycol
It is added dropwise in reaction kettle, the reaction was continued 2-3h after being added dropwise to complete；
2) reaction kettle is warming up to 65-75 DEG C, will be added later dissolved with the hydroxyethyl methacrylate of dibutyl tin dilaurate
Into reaction kettle, the polyurethane acrylate prepolymer is arrived after reaction 2.5-3.5h.
4. a kind of ultraviolet light according to claim 1 solidifies electrically conductive ink, which is characterized in that the photoinitiator includes
Following components and parts by weight content: 0.1-0.2 parts of 2- isopropyl thioxanthone and phenyl are bis- (2,4,6- trimethylbenzoyl)
0.1-0.2 parts of phosphine oxide.
5. a kind of ultraviolet light according to claim 1 solidifies electrically conductive ink, which is characterized in that the silver powder is ultra-fine silver
Powder.
6. a kind of preparation method for solidifying electrically conductive ink such as ultraviolet light described in any one of claim 1 to 5, which is characterized in that
This method are as follows: after 1,6- hexylene glycol double methacrylate is heated to 45-55 DEG C, photoinitiator is added, is then cooled to 25-35
DEG C, and successively add silver powder, polyurethane acrylate prepolymer, obtain mixture, successively by mixture grinding distribution, filtering,
Homogeneous stirs to arrive the electrically conductive ink.
7. the preparation method that a kind of ultraviolet light according to claim 6 solidifies electrically conductive ink, which is characterized in that described grinds
Grind dispersion process the following steps are included:
1) mixture is stirred, silver powder is made to be uniformly dispersed；
2) mixture is once ground on three-roll grinder, is stirred later；
3) secondary grinding is carried out to mixture on three-roll grinder, be stirred later；
4) mixture is ground on three-roll grinder three times, is stirred later.
8. the preparation method that a kind of ultraviolet light according to claim 7 solidifies electrically conductive ink, which is characterized in that
In process of lapping, the gap between the fast roller and central roll of three-roll grinder is 0.25-0.30mm；
In the secondary process of lapping, the gap between the fast roller and central roll of three-roll grinder is 0.20-0.25mm；
In the process of lapping three times, the gap between the fast roller and central roll of three-roll grinder is 0.15-0.20mm.
9. the preparation method that a kind of ultraviolet light according to claim 7 solidifies electrically conductive ink, which is characterized in that ground three times
After mill, fineness≤10 μm of mixture.
10. the preparation method that a kind of ultraviolet light according to claim 6 solidifies electrically conductive ink, which is characterized in that described
Homogeneous whipping process carries out in homogenizer.
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| CN201711160715.3A CN109810576A (en) | 2017-11-20 | 2017-11-20 | A kind of ultraviolet light solidification electrically conductive ink and preparation method thereof |
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| CN201711160715.3A CN109810576A (en) | 2017-11-20 | 2017-11-20 | A kind of ultraviolet light solidification electrically conductive ink and preparation method thereof |
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| CN114316174A (en) * | 2021-12-29 | 2022-04-12 | 重庆交通大学 | High molecular weight linear urethane acrylate prepolymer, dielectric elastomer and preparation |
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| CN102898597A (en) * | 2011-07-28 | 2013-01-30 | 中国科学院化学研究所 | Composite ink vehicle for intaglio printing |
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Application publication date: 20190528 |
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