CN106299199A - A kind of preparation method of lithium battery diaphragm - Google Patents
A kind of preparation method of lithium battery diaphragm Download PDFInfo
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- CN106299199A CN106299199A CN201610700408.9A CN201610700408A CN106299199A CN 106299199 A CN106299199 A CN 106299199A CN 201610700408 A CN201610700408 A CN 201610700408A CN 106299199 A CN106299199 A CN 106299199A
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- Prior art keywords
- preparation
- lithium battery
- battery diaphragm
- directing agent
- structure directing
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides the preparation method of a kind of lithium battery diaphragm, including: precursor compound, structure directing agent and hydrochloric acid are added in the first mixed solution, stirring, after alcoholysis reaction, obtain colloidal sol；Described colloidal sol is applied to porous film surface, cleans, after hot-air seasoning, obtain lithium battery diaphragm.The present invention is with perforated membrane as basement membrane, with tetraethyl orthosilicate, methyl silicate, Silicon chloride., titanium tetrachloride and tetrabutyl titanate as presoma, with block copolymer as structure directing agent, between porous fenestra, it is coated with resistant to elevated temperatures inorganic compound, is effectively improved the thermostability of barrier film.Second, coat barrier film between hole and the wellability of electrolyte is significantly improved, imbibition water retainability is greatly improved, the 3rd, utilizes the thickness of lithium battery diaphragm prepared by the method for coating between hole and weight to increase less, is conducive to improving the energy density per unit volume of battery.Test result indicate that, lithium battery diaphragm prepared by the present invention has good heat resistance and the wellability to electrolyte, and thickness is less.
Description
Technical field
The present invention relates to technical field of lithium ion, particularly relate to the preparation method of a kind of lithium battery diaphragm.
Background technology
Along with the development of information technology, the demand of portable power source is the most quickly increased by we, meanwhile, with conventional batteries phase
Ratio, the direction of demand also there occurs transformation: energy is high, volume is little, lightweight, security performance is high, has had become as portable power source
The new direction of development.Lithium ion battery owing to its energy density is high, have extended cycle life, the property of safety nuisance free, quick impulse electricity
Can, become the first-selection of numerous mancarried electronic aid and electric automobile.Lithium ion battery includes electrode, electrolyte, battery diaphragm
Deng, the barrier film between two of which electrode serves critically important effect, and it not only to play separation the two poles of the earth, makes battery be unlikely to
The effect of internal short-circuit, also to play the effect through ion, and certain porosity ensure that battery diaphragm has well
On the premise of transmitance, moreover it is possible to ensure good mechanical performance.
At present, the lithium battery diaphragm of commercialization is based on polyolefin (PP, PE) single thin film or plural layers.Polyolefin
Material has higher intensity and preferable chemical stability, and as a kind of thermoplastic, porous polyolefin is being higher than
Having the self-closing function of shrinkage porosity under conditions of vitrification point, impedance substantially rises, and is limited by the electric current of battery
System, can prevent due to overheated and phenomenons such as the blast that causes to a certain extent, be a kind of relatively reliable lithium battery diaphragm material
Material.But, the fusing point of polyolefin-based separator is typically below 180 DEG C, and under high temperature, deformation is serious.When battery temperature outside or
Raising under internal factor effect, barrier film can deform contraction, it is likely that causes battery short circuit, causes the generation of accident.Especially
The electrokinetic cell of high power discharge, during use, internal temperature of battery is higher, and it is the most thermally safe that this just requires that barrier film has
Property.
In order to solve the problems referred to above, Chinese patent CN1969407A, CN102306726A and United States Patent (USP) US2013/
0183570A1 proposition PVDF-HFP is as adhesive and Al2O3、BaTiO3It is made into slurry Deng inorganic filler and is coated in polyolefin
On barrier film, improve the thermostability of barrier film to a certain extent and absorb the ability keeping electrolyte.Chinese patent
CN101689624A discloses a kind of with polyalkene diaphragm as supporting layer, at one layer of imide resin Han heat resistant poly of applied atop
Composite diaphragm with metal hydroxides.Chinese patent CN103000848A discloses a kind of property of water-bearing adhesive, inorganic particle
With the composite diaphragm of the coat of other aqueous promoters, improve the thermostability of polyalkene diaphragm.Although above several ways is certain
Improve in degree barrier film heat resistance and with the wellability of electrolyte, but considerably increase weight and the thickness of barrier film, from
And reduce the energy density per unit volume of battery.
Summary of the invention
Present invention solves the technical problem that the preparation method being to provide a kind of lithium battery diaphragm, the lithium battery diaphragm of preparation
Having good heat resistance and the wellability to electrolyte, thickness is less.
In view of this, the invention provides the preparation method of a kind of lithium battery diaphragm, comprise the following steps: by presoma
Compound, structure directing agent and hydrochloric acid add in the first mixed solution, stirring, obtain colloidal sol, described first mixing after alcoholysis reaction
Solution includes second alcohol and water, and described precursor compound is selected from tetraethyl orthosilicate, methyl silicate, Silicon chloride., titanium tetrachloride
With one or more in tetrabutyl titanate, described structure directing agent is block copolymer；Described colloidal sol is applied to perforated membrane
Surface, cleans, the lithium battery diaphragm after hot-air seasoning.
Preferably, described structure directing agent is F127 and/or P123.
Preferably, the weight average molecular weight of described F127 is 8000～15000g/mol.
Preferably, the weight average molecular weight of described P123 is 4000～8000g/mol.
Preferably, described precursor compound, structure directing agent, the ratio of second alcohol and water are 110-440ml:126-
378g:1150-1200ml:360-900ml.
Preferably, the temperature of alcoholysis reaction is 20～80 DEG C, and the time of alcoholysis reaction is 1～12 hour.
Preferably, described perforated membrane is polyethylene porous thin film, polypropylene porous membrane or polypropylene, polyethylene/poly-third
Alkene composite porous film.
Preferably, the thickness of described perforated membrane is 5～40 μm, and porosity is 30～80%, and average pore size is 0.01～10 μ
m。
Preferably, the speed of described coating is 0.2～15m/min, and hot blast temperature is 50～100 DEG C.
Preferably, also include the pretreatment of perforated membrane: mixed with linear low density polyethylene by ultra-high molecular weight polyethylene,
Being placed in solvent, heated and stirred is dissolved, and obtains the second mixed solution；Described second mixed solution is coated in the table of perforated membrane
Face.
The present invention provides the preparation method of a kind of lithium battery diaphragm, including: by precursor compound, structure directing agent and salt
Acid adds in the first mixed solution, and stirring obtains colloidal sol after alcoholysis reaction；Described colloidal sol is applied to porous film surface, cleans,
Lithium battery diaphragm after hot-air seasoning.Compared with prior art, the present invention is with perforated membrane as basement membrane, with tetraethyl orthosilicate, positive silicon
Acid methyl ester, Silicon chloride., titanium tetrachloride and tetrabutyl titanate are presoma, with block copolymer as structure directing agent, in porous
It is coated with resistant to elevated temperatures inorganic compound between fenestra, is effectively improved the thermostability of barrier film.Second, coat barrier film between hole to electrolyte
Wellability significantly improve, imbibition water retainability is greatly improved, the 3rd, utilizes the lithium battery that between hole prepared by the method for coating
The thickness of barrier film and weight increase less, are conducive to improving the energy density per unit volume of battery.Test result indicate that, prepared by the present invention
Lithium battery diaphragm has good heat resistance and the wellability to electrolyte, and thickness is less.
Accompanying drawing explanation
Fig. 1 is the coating barrier film SEM figure of the embodiment of the present invention 1 preparation；
Fig. 2 is the electrolyte conservation rate curve of the barrier film of the embodiment of the present invention 1 and comparative example 1 preparation.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but
Should be appreciated that these describe simply as to further illustrate the features and advantages of the present invention rather than to the claims in the present invention
Limit.
The embodiment of the invention discloses the preparation method of a kind of lithium battery diaphragm, comprise the following steps: by presoma chemical combination
Thing, structure directing agent and hydrochloric acid add in the first mixed solution, stirring, obtain colloidal sol after alcoholysis reaction, and described first mixing is molten
Liquid includes second alcohol and water, described precursor compound selected from tetraethyl orthosilicate, methyl silicate, Silicon chloride., titanium tetrachloride and
One or more in tetrabutyl titanate, described structure directing agent is block copolymer；Described colloidal sol is applied to perforated membrane table
Face, cleans, the lithium battery diaphragm after hot-air seasoning.
The present invention is with perforated membrane as basement membrane, with tetraethyl orthosilicate, methyl silicate, Silicon chloride., titanium tetrachloride and metatitanic acid
N-butyl is presoma, with block copolymer as structure directing agent, is coated with resistant to elevated temperatures inorganic compound, shape between porous fenestra
Become by the coat composed coating barrier film of the high temperature resistant inorganic between basement membrane and hole, improve the heat resistance of barrier film and to electrolyte
Wellability；Weight and the thickness of coating metacneme increase less, are conducive to improving the volume energy density of battery.
Preferably, described structure directing agent is preferably F127 and/or P123.The weight average molecular weight of described F127 is excellent
Elect 8000～15000g/mol as, more preferably 11500g/mol.The weight average molecular weight of described P123 is 4000～8000g/
Mol, more preferably 5800g/mol.Described F127 and P123 is the both sexes triblock polymer that ethoxy-propoxy is formed,
But block composition difference.The molecular formula of P123 is EO20PO70EO20, the molecular formula of F127 is EO106PO70EO106, wherein EO table
Show that ethyoxyl, PO represent propoxyl group.As both sexes triblock polymer, F127 and P123 adds a certain amount of the most permissible in water
Form micelle.Owing to the hydrophilic of EO block is better than PO block, so formation micelle is with PO as kernel in water, EO is shell.
Precursor compound, structure directing agent and hydrochloric acid are added and carry out alcoholysis reaction in the first mixed solution by the present invention,
Obtain colloidal sol.Described precursor compound, structure directing agent, the ratio of second alcohol and water are preferably 110-440ml:126-378g:
1150-1200ml:360-900ml, more preferably 220-440ml:126-300g:1150-1200ml:360-900ml.Alcoholysis is anti-
The temperature answered is preferably 20～80 DEG C, more preferably 60 DEG C；The time of alcoholysis reaction is preferably 1～12 hour, and more preferably 2 is little
Time.Wherein, alcoholysis reaction too high or too low for temperature, all cause alcoholysis reaction not to be smoothed out.
After obtaining colloidal sol, described colloidal sol is applied to porous film surface.Described perforated membrane be preferably polyethylene porous thin film,
Polypropylene porous membrane or polypropylene, polyethylene/polypropylene composite materials porous membrane.The thickness of described perforated membrane is preferably 5～40 μ
M, more preferably 5～25 μm；Porosity is preferably 30～80%, more preferably 40～80%；Average pore size be preferably 0.01～
10 μm, more preferably 0.01～1 μm.The porosity of the perforated membrane that the present invention uses and the size in aperture, make to a certain extent
About coating effect, wherein, if porosity and aperture are the least, between hole coating be easy to plug-hole, it is difficult to reach the effect wanted.
During colloidal sol is applied to porous film surface, the speed of coating also has large effect for the present invention, is coated with
The speed of cloth is crossed affects production efficiency slowly, and the excessive velocities of coating does not often reach and well coats effect.The present invention uses
The speed of coating is preferably 0.2～15m/min, more preferably 0.5～5m/min；Hot blast temperature is preferably 50～100 DEG C, more excellent
Elect 50～80 DEG C as.
Preferably, the present invention further preferably includes the pretreatment of perforated membrane: by ultra-high molecular weight polyethylene with linear
Low Density Polyethylene mixes, and is placed in solvent, and heated and stirred is dissolved, and obtains the second mixed solution；By described second mixed solution
It is coated in the surface of perforated membrane.The present invention use described solvent be preferably decahydronaphthalene, kerosene, benzene, toluene, chloroform, ether, three
One or more in vinyl chloride, paraffin or liquid paraffin.Described ultra-high molecular weight polyethylene, linear low density polyethylene and molten
The mass ratio of agent is preferably 1～10:1～10:80～100, more preferably 1～4:5～10:90～100.Superelevation is divided by the present invention
Sub-weight northylen and linear low density polyethylene are fully dissolved, thus and have better caking property between perforated membrane.
The weight average molecular weight of described ultra-high molecular weight polyethylene is preferably 1 × 106～7 × 106, more preferably 3 × 106～4
×106；The molecular weight distribution of ultra-high molecular weight polyethylene is preferably 3～30, more preferably 10～20；Linear low density polyethylene
Weight average molecular weight be preferably 1 × 104～8 × 104, more preferably 2 × 104～5 × 104；The molecule of linear low density polyethylene
Amount distribution is preferably 1.5～5, more preferably 2～3.
The present invention utilizes ultra-high molecular weight polyethylene and linear low density polyethylene perforated membrane to be carried out pretreatment, on the one hand
Improve the porosity of barrier film, strengthen permeability, on the other hand, the most resistant to elevated temperatures inorganic compound is in the painting on its surface
Cloth, improves the thermostability of barrier film.
From above scheme it can be seen that the present invention is with perforated membrane as basement membrane, with tetraethyl orthosilicate, methyl silicate, tetrachloro
SiClx, titanium tetrachloride and tetrabutyl titanate are presoma, with block copolymer as structure directing agent, are coated with resistance between porous fenestra
The inorganic compound of high temperature, is effectively improved the thermostability of barrier film.Second, coat barrier film between hole obvious to the wellability of electrolyte
Improving, imbibition water retainability is greatly improved, the 3rd, utilize lithium battery diaphragm prepared by the method for coating between hole thickness and
Weight increases less, is conducive to improving the energy density per unit volume of battery.
In order to be further appreciated by the present invention, the technical scheme provided the present invention below in conjunction with embodiment is carried out specifically
Bright, protection scope of the present invention is not limited by the following examples.
The raw material that the embodiment of the present invention uses is commercial.
Embodiment 1
126gF127 is dissolved in the mixed solution of 60 DEG C that 1150ml ethanol and 360ml water are formed, waits F127 complete
Dissolving, add 110ml tetraethyl orthosilicate, be 2～3 by adding hydrochloric acid conditioning solution pH value, in hydrochloric acid, HCl concentration is 0.5M,
Continuing stirring 2h makes reaction obtain colloidal sol completely.
Above-mentioned colloidal sol is coated on PE film by the way of dip-coating, the porosity 60% of PE film, average pore size 80nm, thick
Spending 20 μ, coating speed is 1m/min, cleans with ethanol and water mixed solvent and goes skim-coat gel, 80 DEG C of hot air dryings to be coated with
Cover barrier film.
The coating barrier film preparing the embodiment of the present invention carries out sem analysis, as it is shown in figure 1, be the high property of embodiment 1 preparation
Barrier film SEM figure can be coated between hole.
Embodiment 2
250gF127 is dissolved in the mixed solution of 60 DEG C that 1200ml ethanol and 900ml water are formed, waits F127 complete
Dissolve, add 220ml tetraethyl orthosilicate in the solution, be 2～3 by adding hydrochloric acid conditioning solution pH value, HCl concentration in hydrochloric acid
For 1M, it is further continued for stirring 2h and makes reaction obtain colloidal sol completely.
Above-mentioned colloidal sol is coated on PE basement membrane by the way of dip-coating, the porosity 60% of PE film, average pore size 80nm,
Thickness 20 μ, coating speed is 1m/min, cleans with ethanol and water mixed solvent and goes skim-coat gel, 80 DEG C of hot air dryings to obtain
Coating barrier film.
Embodiment 3
300gF127 is dissolved in the mixed solution of 60 DEG C that 1200ml ethanol and 660ml water are formed, waits F127 complete
Dissolving, 220ml tetraethyl orthosilicate, be 2～3 by adding hydrochloric acid conditioning solution pH value, in hydrochloric acid, HCl concentration is 0.5M, followed by
Continuous stirring 2h makes reaction obtain colloidal sol completely.
Above-mentioned colloidal sol is coated on PP film by the way of dip-coating, the porosity 50% of PP film, average pore size 50nm, thick
Spending 16 μ, coating speed is 1m/min, cleans with ethanol and water mixed solvent and goes skim-coat gel, 80 DEG C of hot air dryings to be coated with
Cover barrier film.
Embodiment 4
378g F127 is dissolved in the mixed solution of 60 DEG C that 1150ml ethanol and 900ml water are formed, waits F127 complete
Dissolve, add 440ml tetraethyl orthosilicate in the solution, be 2～3 by adding hydrochloric acid conditioning solution pH value, HCl concentration in hydrochloric acid
For 1M, it is further continued for stirring 2h and makes reaction obtain colloidal sol completely.
Above-mentioned colloidal sol is coated on PP basement membrane by the way of dip-coating, the porosity 50% of PP film, average pore size 50nm,
Thickness 16 μ, coating speed is 1m/min, cleans with ethanol and water mixed solvent and goes skim-coat gel, 80 DEG C of hot air dryings to obtain
Coating barrier film.
Embodiment 5
It is 3.8 × 10 by 2.1kg weight average molecular weight6, molecular weight distribution be the ultra-high molecular weight polyethylene of 5.2,0.5kg weight
Average molecular weight is 4 × 104, molecular weight distribution be 2.1 linear low density polyethylene mix with 37.6kg decahydronaphthalene, add stirring
In tank, under the stir speed (S.S.) of 60r/min, it is warming up to 130 DEG C, heated and stirred 2h, obtain mixed solution, by described mixed solution
Being coated to the two sides of PP film, the running speed of coating machine is 2.5m/min, and the thickness of coat is 1 μm, the PP after being coated
Film；
300gF127 is dissolved in the mixed solution of 60 DEG C that 1200ml ethanol and 660ml water are formed, waits F127 complete
Dissolving, 220ml tetraethyl orthosilicate, be 2～3 by adding hydrochloric acid conditioning solution pH value, in hydrochloric acid, HCl concentration is 0.5M, followed by
Continuous stirring 2h makes reaction obtain colloidal sol completely.
Above-mentioned colloidal sol is coated with by the way of dip-coating on PP film after application, the porosity 50% of PP film, average hole
Footpath 50nm, thickness 16 μ, coating speed is 1m/min, cleans with ethanol and water mixed solvent and removes skim-coat gel, 80 DEG C of hot air dryings
Dry obtaining coats barrier film.
Comparative example 1
Above-mentioned uncoated PE basement membrane.It addition, as shown in Figure 1, the wellability of electrolyte is significantly improved by composite diaphragm, inhales
Liquid water retainability is greatly improved.And for the embodiment that other is similar, there is similar improvement effect.
Comparative example 2
Above-mentioned uncoated PP basement membrane.
The performance that embodiment 1～3 preparation coats barrier film respectively is measured, and result is as shown in table 1.
The results of property of barrier film prepared by table 1 embodiment of the present invention and comparative example
Fig. 2 is the electrolyte conservation rate curve of the barrier film of the embodiment of the present invention 1 and comparative example 1 preparation.As shown in Figure 2, multiple
Closing barrier film to significantly improve the wellability of electrolyte, imbibition water retainability is greatly improved.And for the reality that other is similar
Execute example, there is similar improvement effect.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (10)
1. the preparation method of a lithium battery diaphragm, it is characterised in that comprise the following steps:
Precursor compound, structure directing agent and hydrochloric acid are added in the first mixed solution, stirring, obtain molten after alcoholysis reaction
Glue, described first mixed solution includes second alcohol and water, described precursor compound selected from tetraethyl orthosilicate, methyl silicate, four
One or more in silicon chloride, titanium tetrachloride and tetrabutyl titanate, described structure directing agent is block copolymer；
Described colloidal sol is applied to porous film surface, cleans, after hot-air seasoning, obtain lithium battery diaphragm.
Preparation method the most according to claim 1, it is characterised in that described structure directing agent is F127 and/or P123.
Preparation method the most according to claim 2, it is characterised in that the weight average molecular weight of described F127 be 8000～
15000g/mol。
Preparation method the most according to claim 2, it is characterised in that the weight average molecular weight of described P123 be 4000～
8000g/mol。
Preparation method the most according to claim 1, it is characterised in that described precursor compound, structure directing agent, ethanol
It is 110-440ml:126-378g:1150-1200ml:360-900ml with the ratio of water.
Preparation method the most according to claim 1, it is characterised in that the temperature of alcoholysis reaction is 20～80 DEG C, and alcoholysis is anti-
The time answered is 1～12 hour.
7. according to the preparation method described in claim 1～6 any one, it is characterised in that described perforated membrane is that polyethylene is many
Hole thin film, polypropylene porous membrane or polypropylene, polyethylene/polypropylene composite materials porous membrane.
8. according to the preparation method described in claim 1～6 any one, it is characterised in that the thickness of described perforated membrane be 5～
40 μm, porosity is 30～80%, and average pore size is 0.01～10 μm.
9. according to the preparation method described in claim 1～6 any one, it is characterised in that the speed of described coating be 0.2～
15m/min, hot blast temperature is 50～100 DEG C.
10. according to the preparation method described in claim 1～6 any one, it is characterised in that also include the pre-place of perforated membrane
Reason:
Being mixed with linear low density polyethylene by ultra-high molecular weight polyethylene, be placed in solvent, heated and stirred is dissolved, and obtains second
Mixed solution；
Described second mixed solution is coated in the surface of perforated membrane.
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| CN108448034A (en) * | 2018-02-05 | 2018-08-24 | 合肥国轩高科动力能源有限公司 | A kind of Low ESR lithium battery diaphragm and preparation method thereof |
| CN110880574A (en) * | 2019-11-28 | 2020-03-13 | 衡阳市鑫晟新能源有限公司 | Lithium battery isolation film and preparation method thereof |
| CN111900313A (en) * | 2020-07-27 | 2020-11-06 | 珠海冠宇电池股份有限公司 | Diaphragm and application thereof |
| CN113385224A (en) * | 2020-03-11 | 2021-09-14 | 吴中区木渎拓科环保技术服务部 | Trace precious metal modified titanium-silicon nano porous material and application thereof |
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Application publication date: 20170104 |