CN111171379B - Preparation method of spherical Ag @ T-ZnOw powder, and preparation method and application of high-dielectric polymer composite film - Google Patents
Preparation method of spherical Ag @ T-ZnOw powder, and preparation method and application of high-dielectric polymer composite film Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000000843 powder Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003990 capacitor Substances 0.000 claims abstract description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 229920002379 silicone rubber Polymers 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 13
- 230000000694 effects Effects 0.000 abstract description 8
- 230000005641 tunneling Effects 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 230000010287 polarization Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001354 calcination Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
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- 239000000945 filler Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
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- 238000004377 microelectronic Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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Abstract
A preparation method of spherical Ag @ T-ZnOw powder, a method for preparing a high dielectric polymer composite film and application thereof relate to a preparation method of spherical composite powder and application thereof. The invention aims to solve the technical problem that the dielectric property requirements of modern micro-capacitors and sensors are difficult to meet due to the fact that spherical nano-silver serving as a reinforcing phase cannot generate a quantum tunneling effect. The method comprises the steps of preparing spherical Ag by using silver nitrate, polyvinylpyrrolidone and ethylene glycol as raw materials, adding tetrapod-shaped zinc oxide, reacting, washing, centrifuging and drying to obtain the spherical Ag @ T-ZnOw powder. And preparing the dielectric polymer composite film by adopting film laying and tabletting. The spherical Ag @ T-ZnOw powder can generate quantum tunneling effect, has excellent electrical property, can be used for preparing devices such as sensors, micro-capacitors and the like after being added into a polymer matrix, and has wide application prospect.
Description
Technical Field
The invention relates to a preparation method and application of spherical composite powder; in particular to a preparation method of spherical Ag @ T-ZnOw powder and a method for preparing a high dielectric polymer composite film and application thereof; the spherical Ag @ T-ZnOw powder is used for manufacturing micro-capacitors, sensor devices and the like.
Background
With the rapid development of electronic information technology and nanotechnology, embedded capacitors have been widely used in various microelectronic systems. Among them, the increasing miniaturization and weight reduction of electronic components have put higher demands on the integration, safety, and lifetime of devices. The development trend of preparing composite materials with high dielectric constant and low electrical loss by using polymers as substrates becomes a modern dielectric material.
Dielectric materials store energy in the form of static electricity and have very important applications in the information, electronics and power industries. The application of the traditional inorganic piezoelectric ceramic material is limited due to the defects of complex preparation process, brittleness, large dielectric loss, poor compatibility with the current circuit integrated processing technology and the like.
The spherical nano silver has large specific surface area, low density and good conductivity, can greatly improve the dielectric property of the material, but because the spherical nano silver has low yield and single appearance, the spherical nano silver adopted as a reinforcing phase can not generate tip touch and can not form a conductive network, so that the quantum tunneling effect can not be generated; the requirements of modern micro-capacitors and sensors on dielectric properties are difficult to meet.
Disclosure of Invention
The invention aims to solve the technical problem that the dielectric property requirements of modern micro-capacitors and sensors are difficult to meet due to the fact that spherical nano-silver serving as a reinforcing phase cannot generate a quantum tunneling effect; and provides a preparation method of the spherical Ag @ T-ZnOw powder, a method for preparing a high dielectric polymer composite film and application.
In order to solve the technical problem, the preparation method of the spherical Ag @ T-ZnOw powder is carried out according to the following steps:
step one, mixing silver nitrate and polyvinylpyrrolidone, then adding ethylene glycol, heating to 140-170 ℃ while stirring, preserving heat for 30min-2h, and naturally cooling to 60-80 ℃;
step two, adding the tetrapod-like zinc oxide, keeping the temperature and stirring for 2-4 h at 60-80 ℃, and cooling to room temperature;
and step three, washing by using an ethanol solution with the volume concentration of 95%, centrifuging for at least 3 times, and drying to obtain Ag @ T-ZnOw powder.
Further limiting, in the first step, 0.25g to 0.4g of silver nitrate and 0.8g to 1.2mg of polyvinylpyrrolidone are mixed, and then 90mL to 120mL of ethylene glycol is added; and adding 1.5g-2g of tetrapod-like zinc oxide in the second step.
Further limiting, the centrifugation speed in the third step is 2000rpm-3000 rpm; the drying temperature is 80-90 ℃.
The method for preparing the high dielectric polymer composite film by the spherical Ag @ T-ZnOw powder prepared by the method is completed by the following steps:
step 1, dissolving spherical Ag @ T-ZnOw powder in N, N dimethylformamide for ultrasonic oscillation, then adding a polymer matrix, and ultrasonically dissolving at a certain temperature to obtain sol;
step 2, filtering impurities and exhausting bubbles from the sol obtained in the step one, and drying after film paving;
and step 3, tabletting to obtain the spherical Ag @ T-ZnOw polymer composite film.
Ultrasonic oscillation is carried out for at least 1h in the step 1; ultrasonic dissolving reaction is carried out for 2 to 4 hours at the temperature of between 70 and 90 ℃.
In the step 1, the polymer is polyvinylidene fluoride, polyurethane, silicon rubber or polyacrylate.
In the step 1, 0.25mg-1g of spherical Ag @ T-ZnOw powder is dissolved in 50 mL-60 mL of N, N-dimethylformamide for ultrasonic oscillation, and then 5g-6g of polymer is added.
Spreading the film by adopting a film spreading machine in the step 2; the thickness of the film is 0.2 mm-0.6 mm.
And 3, tabletting by using a flat vulcanizing machine.
And 3, tabletting at the temperature of 170-180 ℃ and under the pressure of 10-20 MPa for 10-20 min.
The high dielectric polymer composite film prepared by the method is used for manufacturing a micro-capacitor or a sensor.
The method of the invention compounds the spherical nano silver and the four-needle zinc oxide, can generate quantum tunneling effect, has excellent electrical property, can prepare devices such as sensors, micro-capacitors and the like after being added into a polymer matrix, and has wide application prospect.
The powder is favorable for forming a network in the deformation process, the tetrapod-shaped zinc oxide whiskers are the only nano zinc oxide with a three-dimensional regular space structure, the crystal structure is complete, the tip effect can be generated, a conductive network is formed, the spherical nano silver is used for coating the tetrapod-shaped zinc oxide, the number of current carriers can be increased, the distance between the tetrapod-shaped zinc oxide and the quantum tunneling effect can be favorably generated, the dielectric property of the composite material can be better improved after the spherical nano silver and the tetrapod-shaped zinc oxide are combined and added into a polymer matrix, and the tetrapod-shaped zinc oxide whiskers are used for manufacturing a micro-capacitor or a sensor.
The high-dielectric spherical Ag @ T-ZnOw polymer composite film prepared by the invention is applied to the preparation of embedded micro-capacitors and sensor devices, can effectively increase the compatibility of the film and a main board polymer, effectively improve the capacitance, storage capacity and conductivity of the film, and provide a new technology for the development of micro embedded capacitors and sensor devices.
According to the high-dielectric spherical Ag @ T-ZnOw polymer composite film prepared by the invention, spherical nano silver particles are used for coating the tetrapod-shaped zinc oxide as a filler, so that electronic polarization can be generated, further a quantum tunneling effect is generated, and the dielectric property of the material is greatly improved.
The thickness of the spherical Ag @ T-ZnOw polymer composite film with high dielectric constant prepared by the invention is 0.2 mm-0.6 mm. The composite material has small thickness, light weight, strong dielectric property and good compatibility with a main board polymer, and fully exerts the application capability of devices such as an embedded micro-capacitor, a sensor and the like.
The high-dielectric spherical Ag @ T-ZnOw polymer composite film prepared by the invention has the advantages of simple preparation method, non-toxic and harmless raw materials, environmental friendliness, easy obtainment of the raw materials, no need of high-temperature and high-pressure calcination treatment in the preparation process, low cost, high safety coefficient and suitability for industrial production.
Drawings
FIG. 1 is a scanning electron microscope image of high dielectric spherical Ag @ T-ZnOw powder, FIG. 1 a-FIG. 1 b-FIG. 1 c-FIG. 1 d- (the four images are different multiples, a is 10000 times, b is 10000 times, c is 40000 times, d is 5000 times);
FIG. 2 is a graph of the dielectric constant of a spherical Ag @ T-ZnOw polymer composite film obtained by the method of example 1;
FIG. 3 is a graph of the dielectric loss of a spherical Ag @ T-ZnOw polymer composite film made by the method of example 1.
Detailed Description
Example 1: the preparation method of the spherical Ag @ T-ZnOw powder in the embodiment is carried out according to the following steps:
step one, mixing 0.25g of silver nitrate and 1.0g of polyvinylpyrrolidone, then adding 100mL of ethylene glycol, heating to 150 ℃ while stirring, preserving heat for 2h, and naturally cooling to 70 ℃;
step two, then adding 2g of tetrapod-like zinc oxide, keeping the temperature at 70 ℃, stirring at 1500rmp rate for 2h, and cooling to room temperature;
and step three, washing by using an ethanol solution with the volume concentration of 95%, centrifuging at the speed of 2000rpm for 3 times, and drying at the temperature of 80 ℃ to obtain Ag @ T-ZnOw powder, wherein as shown in figures 1a-1d, the surface of the tetrapod-shaped zinc oxide is coated with spherical nano-silver particles, and the shape is good.
The method for preparing the high dielectric polymer composite film by the spherical Ag @ T-ZnOw powder prepared by the method is completed by the following steps:
step 1, dissolving 1.0g of spherical Ag @ T-ZnOw powder in 50mLN, N-dimethylformamide, ultrasonically oscillating for 1h, then adding 5g of polyurethane, and ultrasonically dissolving and reacting for 2h at 70 ℃ to obtain sol;
step 2, filtering impurities and exhausting bubbles from the sol obtained in the step one, paving a film with the thickness of 0.4mm by using a film paving machine, and then drying at 80 ℃;
and 3, tabletting at the temperature of 180 ℃ and under the pressure of 20MPa by using a flat vulcanizing machine, and obtaining the spherical Ag @ T-ZnOw polymer composite film after 10 min.
The dielectric properties of the spherical Ag @ T-ZnOw polymer composite film prepared by the method of the embodiment are shown in figures 2 and 3
As can be seen from fig. 2, at power frequency, adding tetrapod-like zinc oxide to polyurethane improves the dielectric constant of the material, and after adding spherical silver to coat tetrapod-like zinc oxide, a conductive network is formed by using the three-dimensional structure of tetrapod-like zinc oxide, and the spherical silver preferably increases the number of carriers, so that molecular polarization occurs, and the dielectric constant of the composite material is increased.
As can be seen from fig. 3, the dielectric loss of the composite film shows a tendency of decreasing first and then increasing with increasing frequency, and at low frequency, the dielectric loss of the composite film mainly comes from the interface polarization loss and decreases with increasing frequency. As the frequency continues to increase, the polyurethane molecular polarization relaxes and polarization loss occurs, which increases with increasing frequency and replaces interfacial polarization as the primary factor of dielectric loss. After the spherical silver is coated on the tetrapod-like zinc oxide, the spacing distance between the tetrapod-like zinc oxide is gradually reduced, and a conductive path is generated in the polyurethane matrix, so that the electric leakage phenomenon is generated, and the loss is increased. The dielectric loss of the composite film is always leakage loss which is the main loss, and the leakage loss is inversely related to the frequency, so that the dielectric loss is weakened along with the increase of the frequency. The high dielectric polymer composite film prepared by the method of the embodiment is used for manufacturing a micro capacitor or a sensor.
Claims (9)
1. The method for preparing the high dielectric polymer composite film by the spherical Ag @ T-ZnOw powder is characterized by comprising the following steps of:
step 1, dissolving spherical Ag @ T-ZnOw powder in N, N dimethylformamide for ultrasonic oscillation, then adding a polymer, and ultrasonically dissolving at a certain temperature to obtain sol;
step 2, filtering impurities and exhausting bubbles from the sol obtained in the step one, and drying after film paving;
step 3, tabletting to obtain a spherical Ag @ T-ZnOw polymer composite film;
the preparation method of the spherical Ag @ T-ZnOw powder in the step 1 comprises the following steps:
step one, mixing silver nitrate and polyvinylpyrrolidone, then adding ethylene glycol, heating to 140-170 ℃ while stirring, preserving heat for 30min-2h, and naturally cooling to 60-80 ℃;
step two, adding the tetrapod-like zinc oxide, keeping the temperature and stirring for 2-4 h at 60-80 ℃, and cooling to room temperature;
and step three, washing by using an ethanol solution with the volume concentration of 95%, centrifuging for at least 3 times, and drying to obtain Ag @ T-ZnOw powder.
2. The method for preparing the high dielectric polymer composite film from the spherical Ag @ T-ZnOw powder as claimed in claim 1, wherein 0.25g to 0.4g of silver nitrate and 0.8g to 1.2g of polyvinylpyrrolidone are mixed, and then 90mL to 120mL of ethylene glycol is added.
3. The method for preparing the high dielectric polymer composite film from the spherical Ag @ T-ZnOw powder as claimed in claim 2, wherein 1.5g to 2g of tetrapod-like zinc oxide is added in the second step.
4. The method for preparing the high dielectric polymer composite film by the spherical Ag @ T-ZnOw powder according to claim 2 or 3, wherein the centrifugal speed in the third step is 2000rpm-3000 rpm; the drying temperature is 80-90 ℃.
5. The method for preparing the high dielectric polymer composite film from the spherical Ag @ T-ZnOw powder as claimed in claim 1, wherein the ultrasonic vibration is carried out for at least 1h in the step 1; performing ultrasonic dissolution reaction for 2-4 h at 70-90 ℃; the polymer is polyvinylidene fluoride, polyurethane, silicon rubber or polyacrylate; 0.25g-1g of spherical Ag @ T-ZnOw powder is dissolved in 50 mL-60 mLN, N dimethylformamide and ultrasonically vibrated, and then 5g-6g of polymer is added.
6. The method for preparing the high-dielectric polymer composite film by the spherical Ag @ T-ZnOw powder according to claim 1, wherein a film spreading machine is adopted to spread the film in the step 2; the thickness of the spread film is 0.2 mm-0.6 mm.
7. The method for preparing the high dielectric polymer composite film from the spherical Ag @ T-ZnOw powder as claimed in claim 1, wherein a press vulcanizer is used for tabletting in step 2.
8. The method for preparing the high-dielectric polymer composite film from the spherical Ag @ T-ZnOw powder as claimed in claim 1, wherein the high-dielectric polymer composite film is pressed at a temperature of 170-180 ℃ and a pressure of 10-20 MPa for 10-20 min.
9. The high dielectric polymer composite film prepared by the method of claim 1 is used for manufacturing a micro-capacitor or a sensor.
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| CN101550497A (en) * | 2009-04-20 | 2009-10-07 | 浙江理工大学 | Method of preparing zinc oxide composite coated with nano-silver particles by one step wet heating |
| CN103951976A (en) * | 2014-05-22 | 2014-07-30 | 哈尔滨理工大学 | Nano core-shell particle/polyimide (PI) composite film, and preparation method and application thereof |
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| CN103951976A (en) * | 2014-05-22 | 2014-07-30 | 哈尔滨理工大学 | Nano core-shell particle/polyimide (PI) composite film, and preparation method and application thereof |
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| "四针状氧化锌晶须的表面改性及其光催化性能研究";王婕;《中国优秀硕士学位论文全文数据库 信息科技辑》;20120415;第12-14、45-46页 * |
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