CN105427919A - 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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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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, be specifically related to a kind of from antimicrobial nano conductive silver paste and its preparation method and application.
Background technology
Conductive silver paste has very excellent normal temperature conductivity, hardness, tack and bending resistance folding endurance, in novel touch-screen photoelectric material application aspect, is the key function material preparing various electronic devices and components.Nano Silver has good purposes for preparing high-performance conductive silver slurry.The form of conductive silver paste Nano Silver has important effect for the electric conductivity of conductive silver paste, and its preparation technology has great importance for suitability 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 a kind of excellent broad-spectrum antibacterial agent, is particularly useful for the suppression to drug-fast bacteria.The investigation of a research shows: with regard to room microenvironment is polluted, the total number of bacteria of city and country is 72.10cfu/cm respectively
2and 138.94cfu/cm
2, living environment microbial contamination is serious.Because the microbe existed in life is inevitable, therefore, the efficient and anti-biotic material had no side effect of research and development has become the important topic of researcher.Conductive nano silver slurry is with good electric conductivity and good anti-microbial property, and contributing to the subjective antisepsis of institute's application product, is an important branch of novel high-performance antimicrobial composite material.
Summary of the invention
For solving the shortcoming and defect part of prior art, primary and foremost purpose of the present invention is to provide a kind of from antimicrobial nano conductive silver paste.
Another object of the present invention is to provide the above-mentioned preparation method from antimicrobial nano conductive silver paste.
Another object of the present invention is to provide the above-mentioned application from antimicrobial nano conductive silver paste.
The object of the invention is achieved through the following technical solutions:
A kind of from antimicrobial nano conductive silver paste, it is made up of acrylate, cyclohexanone, Nano Silver powder, polyurethane resin, epoxy resin, caprolactam and curing agent, in this gross mass from antimicrobial nano conductive silver paste for 100%, each constituent mass percentage composition is as follows:
Described Nano Silver powder is that raw material prepares by ethylene glycol, polyvinylpyrrolidone, silver nitrate and sodium chloride, and in the gross mass of Nano Silver powder raw materials for 100%, each constituent mass percentage composition is as follows:
Described polyurethane resin is polyurethane acrylic resin prepolymer.
Described epoxy resin is epoxy acrylic resin prepolymer.
Described curing agent is amine curing agent.
From a preparation method for antimicrobial nano conductive silver paste, comprise the steps:
(1) by mass percentage, in microwave reaction kettle, add 8-20% ethylene glycol, 22-50% polyvinylpyrrolidone, 0-53% silver nitrate and 0-10% sodium chloride, under zero energy, stir 10-20 minute, then stir 2-20 minute under 80-300 watt of power; After being cooled to normal temperature, centrifugation, solid ethanol and water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) by mass percentage, in another reactor, add 9-20% acrylate and 7-14% cyclohexanone, under the rotating speed of 50-100 rev/min, stir 5-10 minute; Then add the Nano Silver powder that 40-75% step (1) is obtained, under the rotating speed of 200-500 rev/min, stir 20-40 minute; Add 2.9-8% polyurethane resin, 1-6% epoxy resin and 0.1-1% caprolactam again, under the rotating speed of 100-300 rev/min, stir 1-2 hour; Finally add 5-11% curing agent, under the rotating speed of 100-300 rev/min, stir 10-20 minute, obtain of the present invention from antimicrobial nano conductive silver paste.
Above-mentionedly can be applicable to prepare various electronic devices and components from antimicrobial nano conductive silver paste.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the present invention prepares the Nano Silver powder of different shape by microwave reaction, and in conductive silver paste, obtain different electric conductivity from antimicrobial nano conductive silver paste, its electric conductivity has controllability;
(2) the present invention has good adhesion property from antimicrobial nano conductive silver paste;
(3) the present invention is excellent from antimicrobial nano conductive silver paste anti-microbial property;
(4) the present invention is from antimicrobial nano conductive silver paste based on high-load Nano Silver content of powder, and do not add the auxiliary agent such as dispersant and anti-settling agent, stability is high.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of linear nano silver powder, rod-like nano silver powder and spherical Nano Silver powder three kinds of different shape Nano Silver powder prepared by embodiment.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.In the embodiment of the present invention and comparative example, the percentage of each material quantity is mass percent.
Embodiment 1
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 20% acrylate (Changxing EM235) and 14% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 40% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 8% polyurethane resin (Changxing 615-100), 6% epoxy resin (Sartomer CN121) and 1% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 11% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 2
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 17% acrylate (Changxing EM235) and 14% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 48% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 6% polyurethane resin (Changxing 615-100), 4.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 10% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 3
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 16% acrylate (Changxing EM235) and 13% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 55% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 4
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 12% acrylate (Changxing EM235) and 9% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 65% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 2.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 7% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 5
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 9% acrylate (Changxing EM235) and 7% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 75% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 2.9% polyurethane resin (Changxing 615-100), 1% epoxy resin (Sartomer CN121) and 0.1% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 5% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 6
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 15% acrylate (Changxing EM235) and 12% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 57% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 7
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 13% acrylate (Changxing EM235) and 11% cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 60% Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 8
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% sodium chloride, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 16% acrylate (Changxing EM235) and 13% cyclohexanone, stir 10 minutes under the rotating speed of 50 revs/min; Add 55% Nano Silver powder again, stir 20 minutes under the rotating speed of 500 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 2 hours under the rotating speed of 100 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 20 minutes under the rotating speed of 100 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 9
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% sodium chloride, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 15% acrylate (Changxing EM235) and 12% cyclohexanone, stir 10 minutes under the rotating speed of 50 revs/min; Add 57% Nano Silver powder again, stir 20 minutes under the rotating speed of 500 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 2 hours under the rotating speed of 100 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 20 minutes under the rotating speed of 100 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 10
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 8% ethylene glycol, 43% polyvinylpyrrolidone, 42% silver nitrate and 7% sodium chloride, stir 15 minutes under zero energy, then stir 5 minutes under 250 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 13% acrylate (Changxing EM235) and 11% cyclohexanone, stir 10 minutes under the rotating speed of 50 revs/min; Add 60% Nano Silver powder again, stir 20 minutes under the rotating speed of 500 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 2 hours under the rotating speed of 100 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 20 minutes under the rotating speed of 100 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 11
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% sodium chloride, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 16% acrylate (Changxing EM235) and 13% cyclohexanone, stir 5 minutes under the rotating speed of 100 revs/min; Add 55% Nano Silver powder again, stir 40 minutes under the rotating speed of 200 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1 hour under the rotating speed of 300 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 10 minutes under the rotating speed of 300 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 12
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% sodium chloride, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 15% acrylate (Changxing EM235) and 12% cyclohexanone, stir 5 minutes under the rotating speed of 100 revs/min; Add 57% Nano Silver powder again, stir 40 minutes under the rotating speed of 200 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1 hour under the rotating speed of 300 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 10 minutes under the rotating speed of 300 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Embodiment 13
Being prepared by following preparation process from antimicrobial nano conductive silver paste of the present embodiment:
(1) in microwave reaction kettle, add 20% ethylene glycol, 50% polyvinylpyrrolidone, 30% silver nitrate and 0% sodium chloride, stir 10 minutes under zero energy, then stir 2 minutes under 300 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 13% acrylate (Changxing EM235) and 11% cyclohexanone, stir 5 minutes under the rotating speed of 100 revs/min; Add 60% Nano Silver powder again, stir 40 minutes under the rotating speed of 200 revs/min; Then add 4% polyurethane resin (Changxing 615-100), 3.5% epoxy resin (Sartomer CN121) and 0.5% caprolactam, stir 1 hour under the rotating speed of 300 revs/min; Finally add 8% curing agent (ADEKAEH-4360S), stir 10 minutes under the rotating speed of 300 revs/min, obtain of the present invention from antimicrobial nano conductive silver paste.
Comparative example 1
The conductive nano silver slurry of this comparative example prepares by the following method: except caprolactam addition is 0, all the other all raw materials are identical with embodiment 1 with preparation method, and step is as follows:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 20 mass parts acrylate (Changxing EM235) and 14 mass parts cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 40 mass parts Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 8 mass parts polyurethane resins (Changxing 615-100) and 6 mass parts epoxy resin (Sartomer CN121), stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 11 mass parts curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain a kind of conductive nano silver slurry.
Comparative example 2
The conductive nano silver slurry of this comparative example prepares by the following method: except caprolactam addition is 0, all the other all raw materials are identical with embodiment 6 with preparation method, and step is as follows:
(1) 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 15 mass parts acrylate (Changxing EM235) and 12 mass parts cyclohexanone, stir 8 minutes under the rotating speed of 80 revs/min; Add 57 mass parts Nano Silver powder again, stir 30 minutes under the rotating speed of 350 revs/min; Then add 4 mass parts polyurethane resins (Changxing 615-100) and 3.5 mass parts epoxy resin (Sartomer CN121), stir 1.5 hours under the rotating speed of 200 revs/min; Finally add 8 mass parts curing agent (ADEKAEH-4360S), stir 15 minutes under the rotating speed of 200 revs/min, obtain a kind of conductive nano silver slurry.
Comparative example 3
The conductive nano silver slurry of this comparative example is prepared by following preparation process:
(1) preparation of Nano Silver powder is identical with embodiment 4, namely 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 20 minutes under 80 watts of power; After being cooled to normal temperature, centrifugation, solid ethanol and deionized water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) in another reactor, add 8% acrylate (Changxing EM221), 9% cyclohexanone, 60% Nano Silver powder, 6% polyurethane resin (Changxing 6145) and 10% epoxy resin (Changxing 621-100), stir 5 hours under the rotating speed of 400 revs/min; Finally add 7% curing agent (ADEKAEH-4360S), stir 1 hour under the rotating speed of 400 revs/min, obtain the conductive nano silver slurry contrasted.
Comparative example 4
The conductive nano silver slurry of this comparative example is prepared by following preparation process:
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), stir 5 hours under the rotating speed of 400 revs/min; Finally add 7% curing agent (ADEKAEH-4360S), stir 1 hour under the rotating speed of 400 revs/min, obtain the conductive nano silver slurry contrasted.
Embodiment 1 to embodiment 7 obtains linear nano silver powder, and embodiment 8 to embodiment 10 obtains rod-like nano silver powder, and 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 as shown in Figure 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 uncured after antimicrobial nano conductive silver paste at room temperature places 3 months, solidify 3 minutes at 110 DEG C, testing conductive performance, adhesion property and anti-microbial property again, everyly the results are shown in Table 1 and table 2.Conductive nano that comparative example 1 to comparative example 4 obtains silver slurry, adopts same method of testing with embodiment, everyly the results are shown in Table 3.
According to the electric conductivity experimental result from antimicrobial nano conductive silver paste of embodiment 1 to embodiment 5, along with the increase of Nano Silver powder addition, the trend that resistivity increases after having first swift and violent reduction gradually.Conductive silver paste belongs to the polymer of filling property, and the performance of this base polymer determines primarily of the performance of filler, and therefore with regard to conductive silver paste, the ability of its conduction depends on quantity and the performance of silver powder.Along with the increase of Nano Silver powder addition, resistivity has the swift and violent trend reduced, and when the content of silver powder is more than 55-65%, resistivity increases again gradually, this is mainly due to when the content of Nano Silver powder reaches 55-65%, and conductive silver paste inside forms best conductive network.In addition, from table 1 and table 2, wire silver nano-grain has and is obviously better than the raising of other particle to electric conductivity.This may be mainly because linear Argent grain is easy to form crosslinked conductive network more, thus promotes the formation of conductive path, and therefore under equal in quality content, the Nano Silver of wire has more excellent electric conductivity.
According to the adhesion property experimental result from antimicrobial nano conductive silver paste of embodiment 1 to embodiment 13, adhesion property is 1 grade or 1-2 level, and adhesion property is good.The experimental result display of table 3, the adhesion property of comparative example 1 and comparative example 2 is 4 grades, and compared with embodiment 1 to embodiment 13, the adhesion property of comparative example is poor, this is because, add caprolactam in an embodiment, effectively promote the adhesion property of conductive nano silver slurry.
According to anti-microbial property experimental result, embodiment 1 to embodiment 13 obtain from antimicrobial nano conductive silver paste to colibacillary antibiotic rate and to the antibiotic rate of staphylococcus aureus all more than 99%, anti-microbial property is good.
Stability according in table 1 namely survey and 3 months after survey experimental result, embodiment 1 to embodiment 13 in outward appearance, electric conductivity, adhesion property and anti-microbial property, all there is good stability from antimicrobial nano conductive silver paste.Under normal circumstances, when high-load Nano Silver content of powder, not only the adhesive force of conductive silver paste is difficult to be guaranteed, and Nano Silver and organic resin are easy to occur being separated, cause conductive silver paste unstable, as shown in the experimental result of comparative example in table 33 and comparative example 4.Conductive silver paste shown in the embodiment of the present invention 1 to embodiment 13 while there is good electric conductivity, with good tack and good stability.
Table 1 is from the performance of antimicrobial nano conductive silver paste
Table 2 is from the performance of antimicrobial nano conductive silver paste
The performance of table 3 comparative example conductive nano silver slurry
Outward appearance described in above-mentioned table 1-3, resistivity, adhesion property, antibiotic rate method of testing are as follows:
(1) ESEM: after the gold-plated process of sample surfaces, field emission scanning electron microscope is observed the microstructure of sample.
(2) outward appearance: range estimation.
(3) resistivity: use resistivity tester test.
(4) adhesion property: the cross cut test of GB/T9286-1998 paint and varnish paint film.
(5) antibiotic rate: GB/T21866-2008 antibiotic paint (paint film) antibiotic property determination method and antibacterial effect.
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (7)
1. one kind from antimicrobial nano conductive silver paste, it is characterized in that, describedly to be made up of acrylate, cyclohexanone, Nano Silver powder, polyurethane resin, epoxy resin, caprolactam and curing agent from antimicrobial nano conductive silver paste, in this gross mass from antimicrobial nano conductive silver paste for 100%, each constituent mass percentage composition is as follows:
2. according to claim 1 from antimicrobial nano conductive silver paste, it is characterized in that, described Nano Silver powder is that raw material prepares by ethylene glycol, polyvinylpyrrolidone, silver nitrate and sodium chloride, in the gross mass of Nano Silver powder raw materials for 100%, each constituent mass percentage composition is as follows:
3. according to claim 1ly it is characterized in that from antimicrobial nano conductive silver paste, described polyurethane resin is polyurethane acrylic resin prepolymer.
4. according to claim 1ly it is characterized in that from antimicrobial nano conductive silver paste, described epoxy resin is epoxy acrylic resin prepolymer.
5. according to claim 1ly it is characterized in that from antimicrobial nano conductive silver paste, described curing agent is amine curing agent.
6. from a preparation method for antimicrobial nano conductive silver paste, it is characterized in that, comprise the steps:
(1) by mass percentage, in microwave reaction kettle, add 8-20% ethylene glycol, 22-50% polyvinylpyrrolidone, 0-53% silver nitrate and 0-10% sodium chloride, under zero energy, stir 10-20 minute, then stir 2-20 minute under 80-300 watt of power; After being cooled to normal temperature, centrifugation, solid ethanol and water washing, vacuumize, obtains Nano Silver powder, for subsequent use;
(2) by mass percentage, in another reactor, add 9-20% acrylate and 7-14% cyclohexanone, under the rotating speed of 50-100 rev/min, stir 5-10 minute; Then add the Nano Silver powder that 40-75% step (1) is obtained, under the rotating speed of 200-500 rev/min, stir 20-40 minute; Add 2.9-8% polyurethane resin, 1-6% epoxy resin and 0.1-1% caprolactam again, under the rotating speed of 100-300 rev/min, stir 1-2 hour; Finally add 5-11% curing agent, under the rotating speed of 100-300 rev/min, stir 10-20 minute, obtain described from antimicrobial nano conductive silver paste.
7. according to claim 1 from the application of antimicrobial nano conductive silver paste in the various electronic devices and components of preparation.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107833653A (en) * | 2017-11-23 | 2018-03-23 | 安徽清龙泉印刷科技股份有限公司 | A kind of novel antibacterial conductive silver paste and its preparation technology |
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| 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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| CN107833653A (en) * | 2017-11-23 | 2018-03-23 | 安徽清龙泉印刷科技股份有限公司 | A kind of novel antibacterial conductive silver paste and its preparation technology |
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