CN105427919B - Self-antibacterial nano conductive silver paste and preparation method and application thereof - Google Patents
Self-antibacterial nano conductive silver paste and preparation method and application thereof Download PDFInfo
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- CN105427919B CN105427919B CN201510821907.9A CN201510821907A CN105427919B CN 105427919 B CN105427919 B CN 105427919B CN 201510821907 A CN201510821907 A CN 201510821907A CN 105427919 B CN105427919 B CN 105427919B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The present invention discloses self-antibacterial nano conductive silver paste and a preparation method and application thereof. The self-antibacterial nano conductive silver paste consists of the following components in percentage by mass: 9-20% acrylic ester, 7-14% of cyclohexanone, 40-75% of nano silver powder, 2.9-8% polyurethane resin, 1-6% epoxy resin, 0.1-1% of caprolactam, and 5-11% of curing agent. According to the present invention, nano silver powder in different forms is prepared through a microwave reaction, is used in conductive silver paste to obtain self-antibacterial nano conductive silver paste with different conductive properties, and the self-antibacterial nano conductive silver paste is controllable in conductive property. The self-antibacterial nano conductive silver paste prepared by the method disclosed by the present invention has good adhesion and antibacterial performance; and moreover, the self-antibacterial nano conductive silver paste disclosed by the present invention is based on content of the high-content nano silver powder, is not added with assistants such as a dispersant, an anti-settling agent and the like, and has high stability.
Description
Technical field
The invention belongs to conductive silver paste technical field, and in particular to one kind is from antimicrobial nano conductive silver paste and preparation method thereof
And application.
Background technology
Conductive silver paste has very excellent normal temperature electric conductivity, hardness, tack and bending resistance, in new touch-screen
Photoelectric material application aspect, is the key function material for preparing various electronic devices and components.Nano Silver is for preparing high-performance conductive
Silver paste has good purposes.The form of conductive silver paste Nano Silver has important work for the electric conductivity of conductive silver paste
With its preparation technology has great importance for industrialized production and quality control.
Nano Silver has excellent anti-microbial property.Because Nano Silver surface charge is high, good stability has no drug resistance, and is one
Excellent broad-spectrum antibacterial agent is planted, is particularly suited for the suppression to drug-fast bacteria.The investigation of one research shows：It is dirty with regard to room microenvironment
For dye, the total number of bacteria in city and rural area is respectively 72.10cfu/cm2And 138.94cfu/cm2, the dirt of living environment microorganism
Dye is serious.Because microorganism present in life is inevitable, therefore, that what is researched and developed efficiently and have no toxic side effect is anti-
Bacterium material has become the important topic of researcher.Conductive nano silver paste is with good electric conductivity and good antibiotic property
Can, contribute to the subjective antisepsis of institute's application product, it is an important branch of novel high-performance antimicrobial composite material.
The content of the invention
To solve the shortcoming and defect part of prior art, the primary and foremost purpose of the present invention is to provide one kind from antimicrobial nano
Conductive silver paste.
Further object is that providing the above-mentioned preparation method from antimicrobial nano conductive silver paste.
It is yet a further object of the present invention to provide the above-mentioned application from antimicrobial nano conductive silver paste.
The object of the invention is achieved through the following technical solutions：
, from antimicrobial nano conductive silver paste, it is by acrylate, cyclohexanone, Nano Silver powder, polyurethane resin, epoxy for one kind
Resin, caprolactam and curing agent composition, is counted, each component quality from the gross mass of antimicrobial nano conductive silver paste with this as 100%
Percentage composition is as follows：
The Nano Silver powder is prepared by ethylene glycol, polyvinylpyrrolidone, silver nitrate and sodium chloride for raw material, with
The gross mass of Nano Silver powder preparing raw material is 100% meter, and each component weight/mass percentage composition is as follows：
The polyurethane resin is polyurethane acrylic resin prepolymer.
The epoxy resin is epoxy acrylic resin prepolymer.
The curing agent is amine curing agent.
A kind of preparation method from antimicrobial nano conductive silver paste, comprises the steps：
(1) by mass percentage, in microwave reaction kettle, 8-20% ethylene glycol, 22-50% polyvinylpyrrolidines are added
Ketone, 30-53% silver nitrates and 0-10% sodium chloride, stir 10-20 minutes under zero energy, then stir under 80-300 watt of power
2-20 minutes；After being cooled to normal temperature, centrifugation, solid ethanol and water washing, vacuum drying obtains Nano Silver powder, standby
With；
(2) by mass percentage, in another reactor, 9-20% acrylate and 7-14% cyclohexanone are added,
Stir 5-10 minutes under 50-100 rev/min of rotating speed；Nano Silver powder obtained in 40-75% steps (1) is subsequently adding,
Stir 20-40 minutes under 200-500 rev/min of rotating speed；Add 2.9-8% polyurethane resins, 1-6% epoxy resin and
0.1-1% caprolactams, stir 1-2 hours under 100-300 rev/min of rotating speed；5-11% curing agent is eventually adding,
Stir 10-20 minutes under 100-300 rev/min of rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
It is above-mentioned to can be applicable to prepare various electronic devices and components from antimicrobial nano conductive silver paste.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) present invention prepares the Nano Silver powder of different shape by microwave reaction, and for conductive silver paste in, obtain not
With electric conductivity from antimicrobial nano conductive silver paste, its electric conductivity has controllability；
(2) present invention has good adhesion property from antimicrobial nano conductive silver paste；
(3) present invention is excellent from antimicrobial nano conductive silver paste anti-microbial property；
(4) present invention from antimicrobial nano conductive silver paste be based on high-load Nano Silver content of powder, do not add dispersant and
The auxiliary agents such as anti-settling agent, stability is high.
Description of the drawings
Three kinds of linear nano silver powder, rod-like nano silver powder and the spherical Nano Silver powder that Fig. 1 is prepared for embodiment is not
With the scanning electron microscope (SEM) photograph at form nano-silver powder end.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.The percentage of each material quantity is mass percent in the embodiment of the present invention and comparative example.
Embodiment 1
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 20% acrylate (Changxing EM235) and 14% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；40% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
Add 8% polyurethane resin (Changxing 615-100), 6% epoxy resin (Sartomer CN121) and 1% caprolactam, 200 turns/
Stir 1.5 hours under the rotating speed of minute；11% curing agent (ADEKA EH-4360S) is eventually adding, in 200 revs/min of rotating speed
Lower stirring 15 minutes, obtains of the present invention from antimicrobial nano conductive silver paste.
Embodiment 2
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 17% acrylate (Changxing EM235) and 14% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；48% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
6% polyurethane resin (Changxing 615-100), 4.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 1.5 hours under 200 revs/min of rotating speed；10% curing agent (ADEKA EH-4360S) is eventually adding, at 200 revs/min
Rotating speed under stir 15 minutes, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 3
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 16% acrylate (Changxing EM235) and 13% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；55% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 1.5 hours under 200 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 200 revs/min
Rotating speed under stir 15 minutes, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 4
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 12% acrylate (Changxing EM235) and 9% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；65% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 2.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 1.5 hours under 200 revs/min of rotating speed；7% curing agent (ADEKA EH-4360S) is eventually adding, at 200 revs/min
Rotating speed under stir 15 minutes, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 5
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 9% acrylate (Changxing EM235) and 7% cyclohexanone are added, at 80 revs/min
Rotating speed under stir 8 minutes；75% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then plus
Enter 2.9% polyurethane resin (Changxing 615-100), 1% epoxy resin (Sartomer CN121) and 0.1% caprolactam, 200
Rev/min rotating speed under stir 1.5 hours；5% curing agent (ADEKA EH-4360S) is eventually adding, in 200 revs/min turn
The lower stirring of speed 15 minutes, obtains of the present invention from antimicrobial nano conductive silver paste.
Embodiment 6
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 15% acrylate (Changxing EM235) and 12% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；57% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 1.5 hours under 200 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 200 revs/min
Rotating speed under stir 15 minutes, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 7
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 13% acrylate (Changxing EM235) and 11% cyclohexanone are added, at 80 revs/min
Stir 8 minutes under the rotating speed of clock；60% Nano Silver powder is added, is stirred 30 minutes under 350 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 1.5 hours under 200 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 200 revs/min
Rotating speed under stir 15 minutes, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 8
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% chlorine are added
Change sodium, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, 16% acrylate (Changxing EM235) and 13% cyclohexanone are added, at 50 revs/min
Stir 10 minutes under the rotating speed of clock；55% Nano Silver powder is added, is stirred 20 minutes under 500 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 2 hours under 100 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 100 revs/min
Stir 20 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 9
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% chlorine are added
Change sodium, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, 15% acrylate (Changxing EM235) and 12% cyclohexanone are added, at 50 revs/min
Stir 10 minutes under the rotating speed of clock；57% Nano Silver powder is added, is stirred 20 minutes under 500 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 2 hours under 100 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 100 revs/min
Stir 20 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 10
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% chlorine are added
Change sodium, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, 13% acrylate (Changxing EM235) and 11% cyclohexanone are added, at 50 revs/min
Stir 10 minutes under the rotating speed of clock；60% Nano Silver powder is added, is stirred 20 minutes under 500 revs/min of rotating speed；Then
4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam are added,
Stir 2 hours under 100 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 100 revs/min
Stir 20 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 11
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% chlorine are added
Change sodium, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, add 16% acrylate (Changxing EM235) and 13% cyclohexanone, 100 turns/
Stir 5 minutes under the rotating speed of minute；55% Nano Silver powder is added, is stirred 40 minutes under 200 revs/min of rotating speed；So
After add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam,
Stir 1 hour under 300 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 300 revs/min
Stir 10 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 12
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% chlorine are added
Change sodium, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, add 15% acrylate (Changxing EM235) and 12% cyclohexanone, 100 turns/
Stir 5 minutes under the rotating speed of minute；57% Nano Silver powder is added, is stirred 40 minutes under 200 revs/min of rotating speed；So
After add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam,
Stir 1 hour under 300 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 300 revs/min
Stir 10 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 13
The present embodiment is prepared by step and prepares from antimicrobial nano conductive silver paste：
(1) in microwave reaction kettle, 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% chlorine are added
Change sodium, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power；After being cooled to normal temperature, centrifugation, solid
Washed with ethanol and deionized water, be vacuum dried, obtain Nano Silver powder, it is standby；
(2) in another reactor, add 13% acrylate (Changxing EM235) and 11% cyclohexanone, 100 turns/
Stir 5 minutes under the rotating speed of minute；60% Nano Silver powder is added, is stirred 40 minutes under 200 revs/min of rotating speed；So
After add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam,
Stir 1 hour under 300 revs/min of rotating speed；8% curing agent (ADEKA EH-4360S) is eventually adding, at 300 revs/min
Stir 10 minutes under rotating speed, obtain of the present invention from antimicrobial nano conductive silver paste.
Comparative example 1
The conductive nano silver paste of this comparative example is prepared via a method which to obtain：Except caprolactam addition is 0, remaining
All raw materials and preparation method are same as Example 1, and step is as follows：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 20 mass parts acrylate (Changxing EM235) and 14 mass parts cyclohexanone are added,
Stir 8 minutes under 80 revs/min of rotating speed；40 mass parts Nano Silver powder are added, is stirred under 350 revs/min of rotating speed
Mix 30 minutes；It is subsequently adding 8 mass parts polyurethane resins (Changxing 615-100) and 6 mass parts epoxy resin (Sartomers
CN121), stir 1.5 hours under 200 revs/min of rotating speed；It is eventually adding 11 mass parts curing agent (ADEKA EH-
4360S), stir 15 minutes under 200 revs/min of rotating speed, obtain a kind of conductive nano silver paste.
Comparative example 2
The conductive nano silver paste of this comparative example is prepared via a method which to obtain：Except caprolactam addition is 0, remaining
All raw materials and preparation method are same as Example 6, and step is as follows：
(1) in microwave reaction kettle, 15% ethylene glycol, 22% polyvinylpyrrolidone, 53% silver nitrate and 10% are added
Sodium chloride, stirs 20 minutes under zero energy, then stirs 20 minutes under 80 watts of power；After being cooled to normal temperature, centrifugation, Gu
Body is washed with ethanol and deionized water, vacuum drying, obtains Nano Silver powder, standby；
(2) in another reactor, 15 mass parts acrylate (Changxing EM235) and 12 mass parts cyclohexanone are added,
Stir 8 minutes under 80 revs/min of rotating speed；57 mass parts Nano Silver powder are added, is stirred under 350 revs/min of rotating speed
Mix 30 minutes；It is subsequently adding 4 mass parts polyurethane resins (Changxing 615-100) and 3.5 mass parts epoxy resin (Sartomers
CN121), stir 1.5 hours under 200 revs/min of rotating speed；8 mass parts curing agent (ADEKA EH-4360S) are eventually adding,
Stir 15 minutes under 200 revs/min of rotating speed, obtain a kind of conductive nano silver paste.
Comparative example 3
The conductive nano silver paste of this comparative example is prepared by step and prepares：
(1) Nano Silver powder prepare it is same as Example 4, i.e., in microwave reaction kettle, add 15% ethylene glycol, 22%
Polyvinylpyrrolidone, 53% silver nitrate and 10% sodium chloride, stir 20 minutes under zero energy, then stir under 80 watts of power
20 minutes；After being cooled to normal temperature, centrifugation, solid is washed with ethanol and deionized water, vacuum drying, obtains nano-silver powder
End, it is standby；
(2) in another reactor, 8% acrylate (Changxing EM221), 9% cyclohexanone, 60% nano-silver powder are added
End, 6% polyurethane resin (Changxing 6145) and 10% epoxy resin (Changxing 621-100), stir under 400 revs/min of rotating speed
Mix 5 hours；7% curing agent (ADEKA EH-4360S) is eventually adding, is stirred 1 hour under 400 revs/min of rotating speed, obtained
The conductive nano silver paste of contrast.
Comparative example 4
The conductive nano silver paste of this comparative example is prepared by step and prepares：
In a kettle., add 8% acrylate (Changxing EM221), 9% cyclohexanone, 60% commercially available Nano Silver powder,
6% polyurethane resin (Changxing 6145) and 10% epoxy resin (Changxing 621-100), under 400 revs/min of rotating speed 5 are stirred
Hour；7% curing agent (ADEKA EH-4360S) is eventually adding, is stirred 1 hour under 400 revs/min of rotating speed, contrasted
Conductive nano silver paste.
Embodiment 1 to embodiment 7 obtains linear nano silver powder, and embodiment 8 to embodiment 10 obtains rod-like nano silver powder
End, embodiment 11 to embodiment 13 obtains spherical Nano Silver powder, and the scanning electron microscope (SEM) photograph of three kinds of different shape Nano Silver powder is such as
Shown in Fig. 1.
Embodiment 1 to embodiment 13 obtain from antimicrobial nano conductive silver paste, at 110 DEG C solidify 3 minutes, testing conductive
Performance, adhesion property and anti-microbial property；And by it is uncured place 3 months at room temperature from antimicrobial nano conductive silver paste after,
Solidify 3 minutes at 110 DEG C, testing conductive performance, adhesion property and anti-microbial property again, items the results are shown in Table 1 and table 2.Contrast
The conductive nano silver paste that example 1 to comparative example 4 is obtained, adopts same method of testing, items to the results are shown in Table 3 with embodiment.
According to the electric conductivity experimental result from antimicrobial nano conductive silver paste of embodiment 1 to embodiment 5, with Nano Silver
The increase of powder addition, resistivity has the trend gradually increased after first swift and violent reduction.Conductive silver paste belongs to the poly- of filling property
Compound, the performance of such polymer is mainly determined by the performance of filler, therefore for conductive silver paste, its conductive ability depends on
In the quantity and performance of silver powder.With the increase of Nano Silver powder addition, resistivity has the trend of swift and violent reduction, and works as silver powder
Content more than 55-65% when, resistivity gradually increases again, and this reaches 55- mainly due to when the content of Nano Silver powder
When 65%, conductive silver paste is internally formed optimal conductive network.In addition, knowable to Tables 1 and 2, wire silver nano-grain has
It is substantially better than raising of other particles to electric conductivity.This is mainly likely due to linear Argent grain and more easily forms crosslinking
Conductive network, so as to promote the formation of conductive path, therefore under identical mass content, the Nano Silver of wire has more excellent
Different electric conductivity.
According to the adhesion property experimental result from antimicrobial nano conductive silver paste of embodiment 1 to embodiment 13, adhesion property
1 grade or 1-2 levels are, adhesion property is good.The experimental result of table 3 shows that the adhesion property of comparative example 1 and comparative example 2 is 4
Level, compared with embodiment 1 to embodiment 13, the adhesion property of comparative example is poor, this is because, acyl in oneself is added in embodiment
Amine, effectively lifts the adhesion property of conductive nano silver paste.
According to anti-microbial property experimental result, embodiment 1 to embodiment 13 obtain from antimicrobial nano conductive silver paste to big
The antibiotic rate of enterobacteria and to the antibiotic rate of staphylococcus aureus more than 99%, anti-microbial property is good.
Stability according in table 1 i.e. survey and 3 months after survey experimental result understand, embodiment 1 to embodiment 13 from resist
Bacterium conductive nano silver paste is respectively provided with preferable stability in terms of outward appearance, electric conductivity, adhesion property and anti-microbial property.Usual feelings
Under condition, in the case of high-load Nano Silver content of powder, not only the adhesive force of conductive silver paste is difficult to be guaranteed, and nanometer
Silver is easy to organic resin to be occurred being separated, and causes conductive silver paste unstable, the experiment of comparative example 3 and comparative example 4 such as in table 3
As a result it is shown.Conductive silver paste shown in the embodiment of the present invention 1 to embodiment 13 has concurrently while with good electric conductivity
There is good tack and good stability.
Performance of the table 1 from antimicrobial nano conductive silver paste
Performance of the table 2 from antimicrobial nano conductive silver paste
The performance of the comparative example conductive nano silver paste of table 3
Outward appearance, resistivity described in above-mentioned table 1-3, adhesion property, antibiotic rate method of testing are as follows：
(1) ESEM：After the gold-plated process of sample surfaces, the microcosmic of sample is observed on field emission scanning electron microscope
Structure.
(2) outward appearance：Range estimation.
(3) resistivity：Tested using resistivity tester.
(4) adhesion property：The cross cut test of GB/T 9286-1998 paint and varnish paint films.
(5) antibiotic rate：GB/T 21866-2008 antibiotic paints (paint film) antibiotic property determination method and antibacterial effect.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention not by above-described embodiment
Limit, other any Spirit Essences without departing from the present invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. one kind is from antimicrobial nano conductive silver paste, it is characterised in that it is described from antimicrobial nano conductive silver paste by acrylate, hexamethylene
Ketone, Nano Silver powder, polyurethane resin, epoxy resin, caprolactam and curing agent composition, with this from antimicrobial nano conductive silver paste
Gross mass be 100% meter, each component weight/mass percentage composition is as follows：
2. it is according to claim 1 from antimicrobial nano conductive silver paste, it is characterised in that the Nano Silver powder is by second two
Alcohol, polyvinylpyrrolidone, silver nitrate and sodium chloride are prepared for raw material, and the gross mass with Nano Silver powder preparing raw material is
100% meter, each component weight/mass percentage composition is as follows：
3. it is according to claim 1 from antimicrobial nano conductive silver paste, it is characterised in that the polyurethane resin is polyurethane
Acrylic resin prepolymer.
4. it is according to claim 1 from antimicrobial nano conductive silver paste, it is characterised in that the epoxy resin is propylene oxide
Acid resin prepolymer.
5. it is according to claim 1 from antimicrobial nano conductive silver paste, it is characterised in that the curing agent is amine-type cure
Agent.
6. a kind of preparation method from antimicrobial nano conductive silver paste, it is characterised in that comprise the steps：
(1) by mass percentage, in microwave reaction kettle, add 8-20% ethylene glycol, 22-50% polyvinylpyrrolidones,
30-53% silver nitrates and 0-10% sodium chloride, stir 10-20 minutes under zero energy, then stir 2- under 80-300 watt of power
20 minutes；After being cooled to normal temperature, centrifugation, solid ethanol and water washing, vacuum drying obtains Nano Silver powder, standby；
(2) by mass percentage, in another reactor, 9-20% acrylate and 7-14% cyclohexanone are added, in 50-
Stir 5-10 minutes under 100 revs/min of rotating speed；Nano Silver powder obtained in 40-75% steps (1) is subsequently adding, in 200-
Stir 20-40 minutes under 500 revs/min of rotating speed；Add 2.9-8% polyurethane resins, 1-6% epoxy resin and 0.1-
1% caprolactam, stirs 1-2 hours under 100-300 rev/min of rotating speed；5-11% curing agent is eventually adding, in 100-
Stir 10-20 minutes under 300 revs/min of rotating speed, obtain described from antimicrobial nano conductive silver paste.
7. the application from antimicrobial nano conductive silver paste in various electronic devices and components are prepared described in claim 1.
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| CN1903946A (en) * | 2005-07-28 | 2007-01-31 | 上海三瑞化学有限公司 | Preparation method of high dispersed nano-silver particle |
| CN101645318A (en) * | 2008-08-07 | 2010-02-10 | 上海昌银电子材料科技有限公司 | Conductive silver paste special for circuit of laptop keyboard and preparation method thereof |
| CN103059767A (en) * | 2013-01-15 | 2013-04-24 | 宁波晶鑫电子材料有限公司 | Conductive silver paste with high-temperature resistance and low sheet resistance and preparation method of conductive silver paste |
| CN103515025A (en) * | 2013-09-30 | 2014-01-15 | 无锡晶睿光电新材料有限公司 | Low-temperature curing type light sensing conduction slurry and method for manufacturing conduction circuit with conduction slurry |
| CN104227017A (en) * | 2014-09-28 | 2014-12-24 | 重庆文理学院 | Preparation method of silver nanoparticle with controllable particle size |
| CN104858437A (en) * | 2015-04-24 | 2015-08-26 | 昆明理工大学 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1903946A (en) * | 2005-07-28 | 2007-01-31 | 上海三瑞化学有限公司 | Preparation method of high dispersed nano-silver particle |
| CN101645318A (en) * | 2008-08-07 | 2010-02-10 | 上海昌银电子材料科技有限公司 | Conductive silver paste special for circuit of laptop keyboard and preparation method thereof |
| CN103059767A (en) * | 2013-01-15 | 2013-04-24 | 宁波晶鑫电子材料有限公司 | Conductive silver paste with high-temperature resistance and low sheet resistance and preparation method of conductive silver paste |
| CN103515025A (en) * | 2013-09-30 | 2014-01-15 | 无锡晶睿光电新材料有限公司 | Low-temperature curing type light sensing conduction slurry and method for manufacturing conduction circuit with conduction slurry |
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| CN104858437A (en) * | 2015-04-24 | 2015-08-26 | 昆明理工大学 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
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