CN105174933A - Preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability - Google Patents
Preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability Download PDFInfo
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Abstract
The invention discloses a preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability. The method comprises the following steps: adding ferrous chloride, manganese chloride, zinc chloride and nickel chloride into hydrochloric acid, after completion of dissolving, adding yttrium oxide and strontium oxide, and carrying out stirring until completion of dissolving so as to obtain a material A; dropwise adding a sodium hydroxide solution into the material A until a pH value is 9 to 11, carrying out standing and aging for 10 to 15 h, then adding triethanolamine and polyvinyl alcohol under stirring, then carrying out standing and hydrothermal reaction, and carrying out natural cooling, washing, filtering and drying so as to obtain a material B; and mixing zirconium oxide, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, tin oxide, indium oxide, borax, calcium carbonate, strontium carbonate and absolute ethanol, then carrying out ball milling, adding the material B and an adhesive and then carrying out uniform mixing, and carrying out pressing molding, microwave sintering and cooling so as to obtain the soft magnetic ferrite with high saturation, high magnetic induction intensity and high magnetic permeability.
Description
Technical field
The present invention relates to soft magnetic ferrite technical field, particularly relate to the ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic.
Background technology
Soft magnetic ferrite refers to that those are easily magnetized, a kind of magneticsubstance of easily demagnetization again under outside magnetic field effect, often by ferric oxide and other one or more metal oxides, through sintering the composite oxides obtained.Soft magnetic materials application in the industry starts from late nineteenth century, and the rise along with electric power electrician and telecom technology occurs, its range of application is extremely extensive.Soft magnetic materials is not only applied to field of household appliances, informatization, automotive field and other supporting fields, and more importantly soft magnetic materials brings demand endlessly as the main raw material(s) of Electronic Components Manufacturing for it.
At present, the industrial process of soft magnetic ferrite is adopt powder metallurgical technique substantially.Preparing nano level ultracrystallite by hydrothermal method is one of investigation of materials field the most active just grown up the nearly more than ten years, and it has important effect to raising Ferrite Material performance.About Ferrite Material preparation and property studies always the concern of extremely chemist and Materials science worker.Along with continuing to bring out of new synthetic method, carrying out structure of modification to improve its performance to conventional iron ferrite is an important research direction.
Along with the expansion in the development and apply field of electron trade, also more and more higher to the requirement of magneticsubstance, and classificating requirement refinement and the specialization more to material behavior, but soft magnetic ferrite of the prior art often permeability and saturation induction density not ideal enough, wish that the powder index that product is corresponding can reach: saturation induction density > 480mT when 25 DEG C, and initial magnetic permeability is more than 3800, but current used material cannot ensure to produce in batches the product meeting this and require, now need a kind of newly there is high saturated magnetic induction high permeability soft magnetic Ferrite Material.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes the ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic, method is simple, and can save energy reduction of discharging, gained soft magnetic ferrite has high saturated magnetic induction and outstanding initial magnetic permeability.
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1, iron protochloride, Manganous chloride tetrahydrate, zinc chloride, nickelous chloride added dissolve completely in hydrochloric acid after, then add yttrium oxide, strontium oxide, be stirred to after dissolving completely and obtain material A;
S2, in material A, drip sodium hydroxide solution to pH value be 9-11, and still aging 10-15h, then adds trolamine and polyvinyl alcohol stirs, and carries out hydro-thermal reaction, naturally cooling after leaving standstill, washing, and suction filtration is dried and obtained material B;
S3, by zirconium white, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder and dehydrated alcohol mix after, ball milling, add material B again and tamanori mixes, compression moulding, carry out microwave sintering again, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Preferably, in S1, the mol ratio of iron protochloride, Manganous chloride tetrahydrate, zinc chloride, nickelous chloride is 53-56:20-24:18-22:5-8.
Preferably, in S1, the mol ratio of yttrium oxide, strontium oxide and iron protochloride is 3.6-5.2:1.8-2.5:53-56.
Preferably, in S2, drip in the process of sodium hydroxide solution and do not stop to stir.
Preferably, in S2, the weight ratio of trolamine, polyvinyl alcohol and material A is 5-8:4-10:100.
Preferably, in S2, the temperature of hydro-thermal reaction is 180-200 DEG C, and the time of hydro-thermal reaction is 12-14h.
Preferably, in S3, the weight ratio of zirconium white, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder and dehydrated alcohol is 2-5:7-10:2.8-4.6:3-6:0.2-0.6:3-8:1-2:0.5-0.8:2-4:0.2-0.4: 10-12:8-10:0.3-0.6:20-25.
Preferably, in S3, the weight ratio of zirconium white, material B and tamanori is 0.02-0.05:100:1-1.8.
Preferably, in S3, tamanori is polyvinyl acetal, polycarbonate or polyimide.
Preferably, in S3, Ball-milling Time is 18-24h.
Preferably, in S3, the pressure of compression moulding is 5-8MPa, and the time of compression moulding is 10-16s, and in compression moulding process, temperature is 160-180 DEG C.
Preferably, in S3, the power of microwave sintering is 1.2-2kW, and the time of microwave sintering is 120-140min, and the frequency of microwave treatment is 1500-2200MHz.
The present invention adopts yttrium oxide, strontium oxide is dissolved in hydrochloric acid and forms salts solution and make in material A containing ferrous ion, mn ion, zine ion, nickel ion, ruthenium ion and strontium ion, and by limiting each cationic mol ratio, gained soft magnetic ferrite uniform crystal particles of the present invention can be made, and permeability is high, impedance is high, powder is made to have suitable activity, obtain good microtexture, and obtain higher sintered density, thus obtain high saturation induction density, drip alkaline solution of sodium hydroxide, form precipitation of hydroxide thing, then leaving standstill makes throw out evenly increase, add trolamine and polyvinyl alcohol again as template, then hydro-thermal reaction is carried out, owing to containing nitrogen-atoms and Sauerstoffatom in trolamine and polyvinyl alcohol, be easy to atoms metal generation coordination, trolamine has stronger structure-directing effect simultaneously, and polyvinyl alcohol molecule is larger, larger space can be occupied, make inorganic molecule carry out crystallization around trolamine and polyvinyl alcohol, obtain micropore ferrite, pass through zirconium white again, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder adds in dehydrated alcohol and carries out ball milling, not only reduce the particle diameter of each oxide powder, each oxide powder can also be improved active, be easy to follow-up sintering, add material B again and tamanori is pressed, limit the temperature of compression moulding, time and pressure, after making compacting, base substrate is easy to shaping, be convenient to sintering, and microwave sintering penetrates ferrite inside by electromagnetic field radiation, there is dielectric loss and heat up in ferrite entirety, each several part has a narrow range of temperature, and microwave sintering is that ferrite Fast Sintering is fine and close, obtain densification, uniform tissue, material microstructure improves, performance is more excellent, and microwave sintering energy consumption is low, efficiency is high, more energy-conservation than conventional sintering 80%, wherein titanium oxide, zirconium white coordinate with micropore ferrite, ferritic mass transfer and sintering can be promoted, accelerate grain growing, improve the initial permeability of product, also effectively can reduce core loss, and vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide and micropore ferrite with the use of, further reduction core loss of the present invention, the simultaneously raw material such as borax, calcium carbonate, Strontium carbonate powder, change microtexture of the present invention, reduce grain-size, improve resistivity.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes.
Embodiment
As shown in Figure 1, Fig. 1 is the schematic flow sheet of the ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes.
With reference to Fig. 1, the ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1, iron protochloride, Manganous chloride tetrahydrate, zinc chloride, nickelous chloride added dissolve completely in hydrochloric acid after, then add yttrium oxide, strontium oxide, be stirred to after dissolving completely and obtain material A;
S2, in material A, drip sodium hydroxide solution to pH value be 9-11, and still aging 10-15h, then adds trolamine and polyvinyl alcohol stirs, and carries out hydro-thermal reaction, naturally cooling after leaving standstill, washing, and suction filtration is dried and obtained material B;
S3, by zirconium white, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder and dehydrated alcohol mix after, ball milling, add material B again and tamanori mixes, compression moulding, carry out microwave sintering again, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1,53 parts of iron protochlorides, 24 parts of Manganous chloride tetrahydrates, 18 parts of zinc chloride, 8 parts of nickelous chlorides added dissolve completely in hydrochloric acid by molar part after, then add 3.6 parts of yttrium oxide, 2.5 parts of strontium oxides, be stirred to after dissolving completely and obtain material A;
S2, in 100 parts of material A, to drip sodium hydroxide solution to pH value be by weight 9, drip in the process of sodium hydroxide solution and do not stop to stir, still aging 15h, then adds 5 parts of trolamines and 10 parts of polyvinyl alcohol stir, and carries out hydro-thermal reaction after leaving standstill, the temperature of hydro-thermal reaction is 180 DEG C, the time of hydro-thermal reaction is 14h, naturally cooling, washing, suction filtration, dries and obtains material B;
S3, by weight by 2 parts of zirconium whites, 10 parts of titanium oxide, 2.8 parts of vanadium oxides, 6 parts of magnesium oxide, 0.2 part of platinum oxide, 8 parts of molybdenum oxides, 1 part of barium oxide, 0.8 part of cerium oxide, 2 parts of stannic oxide, 0.4 part of Indium sesquioxide, 10 parts of boraxs, 10 parts of calcium carbonate, after 0.3 part of Strontium carbonate powder and 25 parts of dehydrated alcohols mix, ball milling 18h, add 10000 serving material B and 100 part polyvinyl acetals again to mix, compression moulding, the pressure of compression moulding is 8MPa, the time of compression moulding is 10s, in compression moulding process, temperature is 180 DEG C, carry out microwave sintering again, the power of microwave sintering is 1.2kW, the time of microwave sintering is 140min, the frequency of microwave treatment is 1500MHz, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Embodiment 2
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1,56 parts of iron protochlorides, 20 parts of Manganous chloride tetrahydrates, 22 parts of zinc chloride, 5 parts of nickelous chlorides added dissolve completely in hydrochloric acid by molar part after, then add 5.2 parts of yttrium oxide, 1.8 parts of strontium oxides, be stirred to after dissolving completely and obtain material A;
S2, in 100 parts of material A, to drip sodium hydroxide solution to pH value be by weight 11, drip in the process of sodium hydroxide solution and do not stop to stir, still aging 10h, then adds 8 parts of trolamines and 4 parts of polyvinyl alcohol stir, and carries out hydro-thermal reaction after leaving standstill, the temperature of hydro-thermal reaction is 200 DEG C, the time of hydro-thermal reaction is 12h, naturally cooling, washing, suction filtration, dries and obtains material B;
S3, by weight by 5 parts of zirconium whites, 7 parts of titanium oxide, 4.6 parts of vanadium oxides, 3 parts of magnesium oxide, 0.6 part of platinum oxide, 3 parts of molybdenum oxides, 2 parts of barium oxide, 0.5 part of cerium oxide, 4 parts of stannic oxide, 0.2 part of Indium sesquioxide, 12 parts of boraxs, 8 parts of calcium carbonate, after 0.6 part of Strontium carbonate powder and 20 parts of dehydrated alcohols mix, ball milling 24h, add 10000 serving material B and 180 part polyimide again to mix, compression moulding, the pressure of compression moulding is 5MPa, the time of compression moulding is 16s, in compression moulding process, temperature is 160 DEG C, carry out microwave sintering again, the power of microwave sintering is 2kW, the time of microwave sintering is 120min, the frequency of microwave treatment is 2200MHz, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Embodiment 3
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1,55 parts of iron protochlorides, 21 parts of Manganous chloride tetrahydrates, 21 parts of zinc chloride, 6 parts of nickelous chlorides added dissolve completely in hydrochloric acid by molar part after, then add 5 parts of yttrium oxide, 2 parts of strontium oxides, be stirred to after dissolving completely and obtain material A;
S2, in 100 parts of material A, to drip sodium hydroxide solution to pH value be by weight 10, drip in the process of sodium hydroxide solution and do not stop to stir, still aging 14h, then adds 6 parts of trolamines and 8 parts of polyvinyl alcohol stir, and carries out hydro-thermal reaction after leaving standstill, the temperature of hydro-thermal reaction is 185 DEG C, the time of hydro-thermal reaction is 13.5h, naturally cooling, washing, suction filtration, dries and obtains material B;
S3, by weight by 3 parts of zirconium whites, 9 parts of titanium oxide, 3 parts of vanadium oxides, 5 parts of magnesium oxide, 0.3 part of platinum oxide, 6 parts of molybdenum oxides, 1.3 parts of barium oxide, 0.7 part of cerium oxide, 2.5 parts of stannic oxide, 0.34 part of Indium sesquioxide, 10.8 part borax, 9.6 parts of calcium carbonate, after 0.4 part of Strontium carbonate powder and 24 parts of dehydrated alcohols mix, ball milling 20h, add 10000 serving material B and 120 part polycarbonate again to mix, compression moulding, the pressure of compression moulding is 7MPa, the time of compression moulding is 12s, in compression moulding process, temperature is 175 DEG C, carry out microwave sintering again, the power of microwave sintering is 1.4kW, the time of microwave sintering is 135min, the frequency of microwave treatment is 1700MHz, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Embodiment 4
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1,54 parts of iron protochlorides, 23 parts of Manganous chloride tetrahydrates, 19 parts of zinc chloride, 7 parts of nickelous chlorides added dissolve completely in hydrochloric acid by molar part after, then add 4 parts of yttrium oxide, 2.4 parts of strontium oxides, be stirred to after dissolving completely and obtain material A;
S2, in 100 parts of material A, to drip sodium hydroxide solution to pH value be by weight 10, drip in the process of sodium hydroxide solution and do not stop to stir, still aging 11h, then adds 7 parts of trolamines and 5 parts of polyvinyl alcohol stir, and carries out hydro-thermal reaction after leaving standstill, the temperature of hydro-thermal reaction is 195 DEG C, the time of hydro-thermal reaction is 12.5h, naturally cooling, washing, suction filtration, dries and obtains material B;
S3, by weight by 4 parts of zirconium whites, 8 parts of titanium oxide, 4 parts of vanadium oxides, 4 parts of magnesium oxide, 0.5 part of platinum oxide, 4 parts of molybdenum oxides, 1.6 parts of barium oxide, 0.6 part of cerium oxide, 3.4 parts of stannic oxide, 0.23 part of Indium sesquioxide, 11.2 part borax, 8.8 parts of calcium carbonate, after 0.5 part of Strontium carbonate powder and 21 parts of dehydrated alcohols mix, ball milling 22h, add 10000 serving material B and 160 part polyvinyl acetals again to mix, compression moulding, the pressure of compression moulding is 6MPa, the time of compression moulding is 14s, in compression moulding process, temperature is 165 DEG C, carry out microwave sintering again, the power of microwave sintering is 1.8kW, the time of microwave sintering is 125min, the frequency of microwave treatment is 2000MHz, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Embodiment 5
The ferritic preparation method of a kind of high saturated magnetic induction high permeability soft magnetic that the present invention proposes, comprises the steps:
S1,54.5 parts of iron protochlorides, 22 parts of Manganous chloride tetrahydrates, 20 parts of zinc chloride, 6.7 parts of nickelous chlorides added dissolve completely in hydrochloric acid by molar part after, then add 4.5 parts of yttrium oxide, 2.2 parts of strontium oxides, be stirred to after dissolving completely and obtain material A;
S2, in 100 parts of material A, to drip sodium hydroxide solution to pH value be by weight 10, drip in the process of sodium hydroxide solution and do not stop to stir, still aging 12h, then adds 6.7 parts of trolamines and 7 parts of polyvinyl alcohol stir, and carries out hydro-thermal reaction after leaving standstill, the temperature of hydro-thermal reaction is 190 DEG C, the time of hydro-thermal reaction is 13h, naturally cooling, washing, suction filtration, dries and obtains material B;
S3, by weight by 3.4 parts of zirconium whites, 8.5 parts of titanium oxide, 3.4 parts of vanadium oxides, 4.5 parts of magnesium oxide, 0.4 part of platinum oxide, 5 parts of molybdenum oxides, 1.4 parts of barium oxide, 0.65 part of cerium oxide, 3 parts of stannic oxide, 0.3 part of Indium sesquioxide, 11 parts of boraxs, 9 parts of calcium carbonate, after 0.45 part of Strontium carbonate powder and 22 parts of dehydrated alcohols mix, ball milling 21h, add 10000 serving material B and 140 part polycarbonate again to mix, compression moulding, the pressure of compression moulding is 6.5MPa, the time of compression moulding is 13s, in compression moulding process, temperature is 170 DEG C, carry out microwave sintering again, the power of microwave sintering is 1.6kW, the time of microwave sintering is 130min, the frequency of microwave treatment is 1800MHz, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
Carry out performance test to embodiment 5 gained high saturated magnetic induction high permeability soft magnetic ferrite, select ZP45 material as a control group, wherein saturation induction density detected temperatures is 25 DEG C; Its result is as follows:
Test item | Initial magnetic permeability | Saturation induction density, mT |
ZP3K | 3400±20% | 430 |
Embodiment 5 | 4000±20% | 490 |
As seen from the above table: saturation induction density of the present invention and initial magnetic permeability are better than prior art, realistic product requirement.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (10)
1. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic, is characterized in that, comprise the steps:
S1, iron protochloride, Manganous chloride tetrahydrate, zinc chloride, nickelous chloride added dissolve completely in hydrochloric acid after, then add yttrium oxide, strontium oxide, be stirred to after dissolving completely and obtain material A;
S2, in material A, drip sodium hydroxide solution to pH value be 9-11, and still aging 10-15h, then adds trolamine and polyvinyl alcohol stirs, and carries out hydro-thermal reaction, naturally cooling after leaving standstill, washing, and suction filtration is dried and obtained material B;
S3, by zirconium white, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder and dehydrated alcohol mix after, ball milling, add material B again and tamanori mixes, compression moulding, carry out microwave sintering again, cooling obtains high saturated magnetic induction high permeability soft magnetic ferrite.
2. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to claim 1, it is characterized in that, in S1, the mol ratio of iron protochloride, Manganous chloride tetrahydrate, zinc chloride, nickelous chloride is 53-56:20-24:18-22:5-8.
3. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to claim 1 or 2, is characterized in that, in S1, the mol ratio of yttrium oxide, strontium oxide and iron protochloride is 3.6-5.2:1.8-2.5:53-56.
4. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-3, is characterized in that, in S2, drips in the process of sodium hydroxide solution and does not stop to stir.
5. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-4, is characterized in that, in S2, the weight ratio of trolamine, polyvinyl alcohol and material A is 5-8:4-10:100.
6. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-5, is characterized in that, in S2, the temperature of hydro-thermal reaction is 180-200 DEG C, and the time of hydro-thermal reaction is 12-14h.
7. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-6, it is characterized in that, in S3, the weight ratio of zirconium white, titanium oxide, vanadium oxide, magnesium oxide, platinum oxide, molybdenum oxide, barium oxide, cerium oxide, stannic oxide, Indium sesquioxide, borax, calcium carbonate, Strontium carbonate powder and dehydrated alcohol is 2-5:7-10:2.8-4.6:3-6:0.2-0.6:3-8:1-2:0.5-0.8:2-4:0.2-0.4: 10-12:8-10:0.3-0.6:20-25.
8. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-7, is characterized in that, in S3, the weight ratio of zirconium white, material B and tamanori is 0.02-0.05:100:1-1.8; Preferably, in S3, tamanori is polyvinyl acetal, polycarbonate or polyimide; Preferably, in S3, Ball-milling Time is 18-24h.
9. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-8, it is characterized in that, in S3, the pressure of compression moulding is 5-8MPa, the time of compression moulding is 10-16s, and in compression moulding process, temperature is 160-180 DEG C.
10. the ferritic preparation method of high saturated magnetic induction high permeability soft magnetic according to any one of claim 1-9, it is characterized in that, in S3, the power of microwave sintering is 1.2-2kW, the time of microwave sintering is 120-140min, and the frequency of microwave treatment is 1500-2200MHz.
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CN115974165A (en) * | 2023-02-02 | 2023-04-18 | 中钢天源股份有限公司 | Method for preparing iron oxide red with high specific surface area by using ferrous sulfate as byproduct of titanium dioxide |
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Application publication date: 20151223 |