CN106496940A - A kind of piezoelectric polymer composite and preparation method thereof - Google Patents
A kind of piezoelectric polymer composite and preparation method thereof Download PDFInfo
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- CN106496940A CN106496940A CN201610960359.2A CN201610960359A CN106496940A CN 106496940 A CN106496940 A CN 106496940A CN 201610960359 A CN201610960359 A CN 201610960359A CN 106496940 A CN106496940 A CN 106496940A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention provides a kind of piezoelectric polymer composite and preparation method thereof.Preparation method is as follows：（1）Nano barium phthalate, 3 aminopropyl trimethoxysilanes, γ aminopropyl trimethoxysilanes and ethyl acetate are mixed reaction, is cleaned after filtration, be put in baking oven and dry；（2）Mix with Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, sodium hydroxide after cooling, be placed in agate mortar and grind, deionized water is added through being cleaned by ultrasonic 35 times；（3）It is put in calorstat and dries；（4）Acetone stirring is added after taking-up, adds glycolylurea epoxide resin and Kynoar to continue stirring at 80 90 DEG C of temperature to acetone volatilization completely；（5）The stirring of polydimethylsiloxane, Tissuemat E and stearic acid is added, extrusion molding in double screw extruder is inserted and is obtained final product.The piezoelectric polymer Tensile Properties of Composites of the present invention is good, and dielectric constant is high, and dielectric loss is little, and piezoelectric property is good.
Description
Technical field
The present invention relates to field of electronic materials, and in particular to a kind of piezoelectric polymer composite and preparation method thereof.
Background technology
Perovskite material with lead titanates and Barium metatitanate. as representative, due to having prominent piezoelectric property, wide at present
General it is applied to all types of underwater sounds, ultrasound, electroacoustic transducer and based on the agitator of piezoelectricity equivalent circuit, wave filter and sensor etc.
Field.But although these inorganic piezoelectric materials, with good piezoelectric property, hardness is high, and fragility is big, it is impossible to meet more
Extensive use demand.Thus, piezoelectric polymer composite arises at the historic moment, and it is typically by macromolecule matrix and inorganic piezoelectric
Body powder is composited, possess high-molecular organic material pliability, good mechanical performance and workability the advantages of and nothing
The excellent piezoelectric property of machine piezoelectric.And the continuous development with economic science and technology, all trades and professions are for piezoelectric performance
Also more and more higher is required, therefore, constantly improves the performance of piezoelectric, expanding its range of application becomes the task of top priority.
Content of the invention
Technical problem to be solved：It is an object of the invention to provide a kind of piezoelectric polymer composite, tensile property is good,
Dielectric constant is high, and dielectric loss is little, and piezoelectric property is good.
Technical scheme：A kind of piezoelectric polymer composite, is prepared from weight portion by following component：Hydantoin epoxy tree
Fat 30-45 parts, Kynoar 5-15 parts, polydimethylsiloxane 3-6 parts, nano barium phthalate 30-50 parts, Lanthanum (III) nitrate 5-8 parts,
Neodymium nitrate 3-6 parts, 3- aminopropyl trimethoxysilane 6-8 parts, γ-aminopropyltrimethoxysilane 6-8 parts, lauryl alcohol polyoxy
Vinyl Ether 10-18 parts, Tissuemat E 1-3 parts, stearic acid 1-2 parts, sodium hydroxide 1-3 parts, ethyl acetate 60-90 part, acetone 40-
70 parts.
It is further preferred that a kind of described piezoelectric polymer composite, is prepared from weight portion by following component：
Glycolylurea epoxide resin 35-40 parts, Kynoar 7-12 parts, polydimethylsiloxane 4-5 parts, nano barium phthalate 35-45 parts, nitre
Sour lanthanum 6-7 parts, neodymium nitrate 4-5 parts, 3- aminopropyl trimethoxysilane 6.5-7.5 parts, γ-aminopropyltrimethoxysilane
6.5-7.5 parts, polyoxyethylene lauryl ether 12-16 parts, Tissuemat E 1.5-2.5 parts, stearic acid 1.3-1.8 parts, sodium hydroxide
1.5-2.5 parts, ethyl acetate 70-80 part, acetone 50-60 parts.
The preparation method of above-mentioned piezoelectric polymer composite is comprised the following steps：
（1）Nano barium phthalate, 3- aminopropyl trimethoxysilanes, γ-aminopropyltrimethoxysilane and ethyl acetate are mixed
Close, stirring reaction 5-6 hour at temperature 60-65 DEG C, clean after filtration, be put in baking oven and dry at temperature 90-100 DEG C；
（2）Mix with Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, sodium hydroxide after cooling, be placed in agate mortar, grind
Mill 6-10 hours, add deionized water through being cleaned by ultrasonic 3-5 time；
（3）It is put in calorstat and dries at temperature 80-85 DEG C；
（4）Acetone stirring 10-20 minutes are added after taking-up, add glycolylurea epoxide resin and Kynoar in temperature 80-90 DEG C
Lower continuation stirring is complete to acetone volatilization；
（5）Polydimethylsiloxane, Tissuemat E and stearic acid stirring 10-30 minutes are added, is inserted in double screw extruder and is squeezed
Go out molding to obtain final product, each area's temperature is 175-190 DEG C, and screw speed is 50-70r/min.
Further, the preparation method of described a kind of piezoelectric polymer composite, described step（1）During middle stirring
Between be 5.5 hours, drying temperature be 95 DEG C.
Further, the preparation method of described a kind of piezoelectric polymer composite, described step（2）During middle grinding
Between 7-9 hours.
Further, the preparation method of described a kind of piezoelectric polymer composite, described step（4）During middle stirring
Between be 15 minutes, whipping temp be 85 DEG C.
Further, the preparation method of described a kind of piezoelectric polymer composite, described step（5）During middle stirring
Between be 15-25 minutes, each area's temperature be 180-185 DEG C, screw speed is 55-65r/min.
Beneficial effect：The tensile strength of the piezoelectric polymer composite of the present invention is high, and highest can be 85.5MPa, have
There is a good tensile property, dielectric constant also may be up at 664,25 DEG C fissipation factor between 0.66-0.73, dielectric loss
Little, piezoelectric property is good.
Specific embodiment
Embodiment 1
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：30 parts of glycolylurea epoxide resin, poly- inclined fluorine
5 parts of ethylene, 3 parts of polydimethylsiloxane, 30 parts of nano barium phthalate, 5 parts of Lanthanum (III) nitrate, 3 parts of neodymium nitrate, 3- aminopropyl trimethoxies
6 parts of silane, 6 parts of γ-aminopropyltrimethoxysilane, 10 parts of polyoxyethylene lauryl ether, 1 part of Tissuemat E, 1 part of stearic acid,
1 part of sodium hydroxide, 60 parts of ethyl acetate, 40 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
The mixing of alkane, γ-aminopropyltrimethoxysilane and ethyl acetate, stirring reaction 5 hours under temperature 60 C are cleaned after filtration,
It is put in baking oven and dries at 90 DEG C of temperature；（2）With Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, sodium hydroxide after cooling
Mixing, is placed in agate mortar, grinds 6 hours, adds deionized water through being cleaned by ultrasonic 3 times；（3）It is put in calorstat in temperature
Dry at 80 DEG C；（4）Add acetone to stir after taking-up 10 minutes, glycolylurea epoxide resin and Kynoar is added in 80 DEG C of temperature
Lower continuation stirring is complete to acetone volatilization；（5）Add polydimethylsiloxane, Tissuemat E and stearic acid to stir 10 minutes, put
Enter extrusion molding in double screw extruder to obtain final product, each area's temperature is 175 DEG C, and screw speed is 50r/min.
Embodiment 2
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：35 parts of glycolylurea epoxide resin, poly- inclined fluorine
7 parts of ethylene, 4 parts of polydimethylsiloxane, 35 parts of nano barium phthalate, 6 parts of Lanthanum (III) nitrate, 4 parts of neodymium nitrate, 3- aminopropyl trimethoxies
6.5 parts of silane, 6.5 parts of γ-aminopropyltrimethoxysilane, 12 parts of polyoxyethylene lauryl ether, 1.5 parts of Tissuemat E, Hard Fat
1.3 parts of acid, 1.5 parts of sodium hydroxide, 70 parts of ethyl acetate, 50 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
The mixing of alkane, γ-aminopropyltrimethoxysilane and ethyl acetate, stirring reaction 5.5 hours at 62 DEG C of temperature are clear after filtration
Wash, be put in baking oven and dry at 95 DEG C of temperature；（2）With Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, hydrogen-oxygen after cooling
Change sodium mixing, be placed in agate mortar, grind 7 hours, deionized water is added through being cleaned by ultrasonic 3 times；（3）It is put in calorstat
Dry at 80 DEG C of temperature；（4）Add acetone to stir after taking-up 15 minutes, glycolylurea epoxide resin and Kynoar is added in temperature
Continue stirring at 85 DEG C complete to acetone volatilization；（5）Polydimethylsiloxane, Tissuemat E and stearic acid is added to stir 15 points
Clock, inserts extrusion molding in double screw extruder and obtains final product, and each area's temperature is 180 DEG C, and screw speed is 55r/min.
Embodiment 3
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：37.5 parts of glycolylurea epoxide resin, poly- partially
10 parts of fluorothene, 4.5 parts of polydimethylsiloxane, 40 parts of nano barium phthalate, 6.5 parts of Lanthanum (III) nitrate, 4.5 parts of neodymium nitrate, 3- ammonia third
7 parts of base trimethoxy silane, 7 parts of γ-aminopropyltrimethoxysilane, 14 parts of polyoxyethylene lauryl ether, 2 parts of Tissuemat E,
1.5 parts of stearic acid, 2 parts of sodium hydroxide, 75 parts of ethyl acetate, 55 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
The mixing of alkane, γ-aminopropyltrimethoxysilane and ethyl acetate, stirring reaction 5.5 hours at 62 DEG C of temperature are clear after filtration
Wash, be put in baking oven and dry at 95 DEG C of temperature；（2）With Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, hydrogen-oxygen after cooling
Change sodium mixing, be placed in agate mortar, grind 6-10 hours, deionized water is added through being cleaned by ultrasonic 4 times；（3）It is put into calorstat
In dry at 82 DEG C of temperature；（4）Add acetone to stir after taking-up 15 minutes, add glycolylurea epoxide resin and Kynoar to exist
Continue stirring at 85 DEG C of temperature complete to acetone volatilization；（5）Add polydimethylsiloxane, Tissuemat E and stearic acid stirring 20
Minute, to insert extrusion molding in double screw extruder and obtain final product, each area's temperature is 183 DEG C, and screw speed is 60r/min.
Embodiment 4
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：40 parts of glycolylurea epoxide resin, poly- inclined fluorine
12 parts of ethylene, 5 parts of polydimethylsiloxane, 45 parts of nano barium phthalate, 7 parts of Lanthanum (III) nitrate, 5 parts of neodymium nitrate, 3- aminopropyl trimethoxies
7.5 parts of base silane, 7.5 parts of γ-aminopropyltrimethoxysilane, 16 parts of polyoxyethylene lauryl ether, 2.5 parts of Tissuemat E, hard
1.8 parts of fat acid, 2.5 parts of sodium hydroxide, 80 parts of ethyl acetate, 60 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
The mixing of alkane, γ-aminopropyltrimethoxysilane and ethyl acetate, stirring reaction 5.5 hours at 64 DEG C of temperature are clear after filtration
Wash, be put in baking oven and dry at 95 DEG C of temperature；（2）With Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, hydrogen-oxygen after cooling
Change sodium mixing, be placed in agate mortar, grind 9 hours, deionized water is added through being cleaned by ultrasonic 4 times；（3）It is put in calorstat
Dry at 85 DEG C of temperature；（4）Add acetone to stir after taking-up 15 minutes, glycolylurea epoxide resin and Kynoar is added in temperature
Continue stirring at 85 DEG C complete to acetone volatilization；（5）Polydimethylsiloxane, Tissuemat E and stearic acid is added to stir 25 points
Clock, inserts extrusion molding in double screw extruder and obtains final product, and each area's temperature is 185 DEG C, and screw speed is 65r/min.
Embodiment 5
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：45 parts of glycolylurea epoxide resin, poly- inclined fluorine
15 parts of ethylene, 6 parts of polydimethylsiloxane, 50 parts of nano barium phthalate, 8 parts of Lanthanum (III) nitrate, 6 parts of neodymium nitrate, 3- aminopropyl trimethoxies
8 parts of base silane, 8 parts of γ-aminopropyltrimethoxysilane, 18 parts of polyoxyethylene lauryl ether, 3 parts of Tissuemat E, stearic acid 2
Part, 3 parts of sodium hydroxide, 90 parts of ethyl acetate, 70 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
Alkane, γ-aminopropyltrimethoxysilane and ethyl acetate mixing, stirring reaction 6 hours at 65 DEG C of temperature, cleans after filtration,
It is put in baking oven and dries at 100 DEG C of temperature；（2）With Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, hydroxide after cooling
Sodium mixes, and is placed in agate mortar, grinds 10 hours, adds deionized water through being cleaned by ultrasonic 5 times；（3）It is put in calorstat
Dry at 85 DEG C of temperature；（4）Add acetone to stir after taking-up 20 minutes, glycolylurea epoxide resin and Kynoar is added in temperature
Continue stirring at 90 DEG C complete to acetone volatilization；（5）Polydimethylsiloxane, Tissuemat E and stearic acid is added to stir 30 points
Clock, inserts extrusion molding in double screw extruder and obtains final product, and each area's temperature is 190 DEG C, and screw speed is 70r/min.
Comparative example 1
The present embodiment is not containing Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether and hydroxide with the difference of embodiment 1
Sodium.Specifically：
A kind of piezoelectric polymer composite, is prepared from weight portion by following component：30 parts of glycolylurea epoxide resin, poly- inclined fluorine
5 parts of ethylene, 3 parts of polydimethylsiloxane, 30 parts of nano barium phthalate, 5 parts of Lanthanum (III) nitrate, 3 parts of neodymium nitrate, 3- aminopropyl trimethoxies
6 parts of silane, 6 parts of γ-aminopropyltrimethoxysilane, 10 parts of polyoxyethylene lauryl ether, 1 part of Tissuemat E, 1 part of stearic acid,
1 part of sodium hydroxide, 60 parts of ethyl acetate, 40 parts of acetone.
The preparation method of above-mentioned piezoelectric polymer composite is：（1）By nano barium phthalate, 3- aminopropyl trimethoxy silicon
The mixing of alkane, γ-aminopropyltrimethoxysilane and ethyl acetate, stirring reaction 5 hours under temperature 60 C are cleaned after filtration,
It is put in baking oven and dries at 90 DEG C of temperature；（2）Add acetone to stir after taking-up 10 minutes, add glycolylurea epoxide resin and gather partially
Fluorothene continues stirring to acetone volatilization completely at 80 DEG C of temperature；（3）Add polydimethylsiloxane, Tissuemat E and Hard Fat
Acid stirring 10 minutes, inserts extrusion molding in double screw extruder and obtains final product, and each area's temperature is 175 DEG C, and screw speed is 50r/
min.
The tensile strength of the piezoelectric polymer composite of the present invention is high, and highest can be 85.5MPa, with stretching well
Performance, dielectric constant also may be up to 664,25 DEG C of fissipation factors between 0.66-0.73, and dielectric loss is little, and piezoelectric property is good.Right
After not containing Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether and sodium hydroxide in ratio 1, the dielectric constant of obtained material
Substantially reduce.
The partial properties index of 1 piezoelectric polymer composite of table
| Name of product | Tensile strength（MPa） | Dielectric constant | 25 DEG C of fissipation factors |
| Embodiment 1 | 83.7 | 631 | 0.072 |
| Embodiment 2 | 84.3 | 647 | 0.068 |
| Embodiment 3 | 84.8 | 652 | 0.070 |
| Embodiment 4 | 85.5 | 664 | 0.073 |
| Embodiment 5 | 85.1 | 658 | 0.066 |
| Comparative example 1 | 83.4 | 603 | 0.076 |
Claims (7)
1. a kind of piezoelectric polymer composite, it is characterised in that：It is prepared from weight portion by following component：Hydantoin epoxy
Resin 30-45 parts, Kynoar 5-15 parts, polydimethylsiloxane 3-6 parts, nano barium phthalate 30-50 parts, Lanthanum (III) nitrate 5-8
Part, neodymium nitrate 3-6 parts, 3- aminopropyl trimethoxysilane 6-8 parts, γ-aminopropyltrimethoxysilane 6-8 parts, lauryl alcohol gather
Oxygen vinyl Ether 10-18 parts, Tissuemat E 1-3 parts, stearic acid 1-2 parts, sodium hydroxide 1-3 parts, ethyl acetate 60-90 part, acetone
40-70 parts.
2. a kind of piezoelectric polymer composite according to claim 1, it is characterised in that：By following component with weight
Part is prepared from：Glycolylurea epoxide resin 35-40 parts, Kynoar 7-12 parts, polydimethylsiloxane 4-5 parts, nano barium titanate
Barium 35-45 parts, Lanthanum (III) nitrate 6-7 parts, neodymium nitrate 4-5 parts, 3- aminopropyl trimethoxysilane 6.5-7.5 parts, γ-aminopropyl front three
TMOS 6.5-7.5 parts, polyoxyethylene lauryl ether 12-16 parts, Tissuemat E 1.5-2.5 parts, stearic acid 1.3-1.8 parts,
Sodium hydroxide 1.5-2.5 parts, ethyl acetate 70-80 part, acetone 50-60 parts.
3. the preparation method of a kind of piezoelectric polymer composite described in any one of claim 1 to 2, it is characterised in that：Bag
Include following steps：
（1）Nano barium phthalate, 3- aminopropyl trimethoxysilanes, γ-aminopropyltrimethoxysilane and ethyl acetate are mixed
Close, stirring reaction 5-6 hour at temperature 60-65 DEG C, clean after filtration, be put in baking oven and dry at temperature 90-100 DEG C；
（2）Mix with Lanthanum (III) nitrate, neodymium nitrate, polyoxyethylene lauryl ether, sodium hydroxide after cooling, be placed in agate mortar, grind
Mill 6-10 hours, add deionized water through being cleaned by ultrasonic 3-5 time；
（3）It is put in calorstat and dries at temperature 80-85 DEG C；
（4）Acetone stirring 10-20 minutes are added after taking-up, add glycolylurea epoxide resin and Kynoar in temperature 80-90 DEG C
Lower continuation stirring is complete to acetone volatilization；
（5）Polydimethylsiloxane, Tissuemat E and stearic acid stirring 10-30 minutes are added, is inserted in double screw extruder and is squeezed
Go out molding to obtain final product, each area's temperature is 175-190 DEG C, and screw speed is 50-70r/min.
4. the preparation method of a kind of piezoelectric polymer composite according to claim 3, it is characterised in that：The step
（1）Middle mixing time is 5.5 hours, and drying temperature is 95 DEG C.
5. the preparation method of a kind of piezoelectric polymer composite according to claim 3, it is characterised in that：The step
（2）Middle milling time 7-9 hour.
6. the preparation method of a kind of piezoelectric polymer composite according to claim 3, it is characterised in that：The step
（4）Middle mixing time is 15 minutes, and whipping temp is 85 DEG C.
7. the preparation method of a kind of piezoelectric polymer composite according to claim 3, it is characterised in that：The step
（5）Middle mixing time is 15-25 minutes, and each area's temperature is 180-185 DEG C, and screw speed is 55-65r/min.
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| CN114306652A (en) * | 2021-12-29 | 2022-04-12 | 华南理工大学 | Injectable piezoelectric hydrogel and preparation and application thereof |
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| CN114306652A (en) * | 2021-12-29 | 2022-04-12 | 华南理工大学 | Injectable piezoelectric hydrogel and preparation and application thereof |
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Application publication date: 20170315 |