CN109097650A - Wear-resisting PCD composite sheet and preparation method thereof - Google Patents

Wear-resisting PCD composite sheet and preparation method thereof Download PDF

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Publication number
CN109097650A
CN109097650A CN201811022030.7A CN201811022030A CN109097650A CN 109097650 A CN109097650 A CN 109097650A CN 201811022030 A CN201811022030 A CN 201811022030A CN 109097650 A CN109097650 A CN 109097650A
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salt
preparation
alcohol
composite sheet
aqueous solution
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刘永
陶峰
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Wuhu Ruide Machinery Technology Co Ltd
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Wuhu Ruide Machinery Technology Co Ltd
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Priority to CN201811022030.7A priority Critical patent/CN109097650A/en
Publication of CN109097650A publication Critical patent/CN109097650A/en
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C26/00Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
    • B22F1/0003
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F2005/001Cutting tools, earth boring or grinding tool other than table ware

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention discloses a kind of wear-resisting PCD composite sheets and preparation method thereof, the preparation method includes: 1) to disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, it is subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate mixing, then lye is added dropwise and stirs, is finally aged, is dry to obtain xerogel;2) xerogel is heat-treated to obtain heat-treated products;3) heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder are subjected to ball milling to obtain bonding agent;4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa‑10×1011Sintering is under Pa to be made the high rigidity PCD composite sheet.The PCD composite sheet has excellent wearability, while the preparation method has the advantages that process is simply and easy to operate.

Description

Wear-resisting PCD composite sheet and preparation method thereof
Technical field
The present invention relates to PCD cutters, and in particular, to a kind of wear-resisting PCD composite sheet and its preparation side.
Background technique
Diamond is applied to machining as a kind of ultrahard cutting tool material and has centuries history.Cutter development course, From late nineteenth century to the twentieth century phase, cutter material is using high-speed steel as main representative;Nineteen twenty-seven, Germany developed hard first Alloy cutter material is simultaneously widely applied;Nineteen fifties, the U.S. of Sweden are respectively synthesized out diamond, cutting It is to represent period that cutter, which is stepped into from this with superhard material,.Nineteen seventies, people are synthesized using high-pressure synthesis technology Polycrystalline diamond (PCD) solves the problems, such as natural diamond rare numbers, expensive, expands diamond cutter application range Open up the multiple fields such as Aeronautics and Astronautics, automobile, electronics, stone material.
Diamond cutter has the characteristics such as hardness is high, compression strength is high, thermal conductivity and wearability are good, can high-speed cutting acquisition Very high manufacturing accuracy processing efficiency.The above-mentioned characteristic of diamond cutter is determined by diamond crystal state.Diamond crystal, carbon atom Four valence electrons press tetrahedral structure bonding, and each carbon atom and four adjacent atoms form covalent bond, and then form diamond Structure, the structure binding force directionality is very strong, so that diamond be made to have extreme hardness.Since polycrystalline diamond PCD structure takes To different fine-particle diamond sintered body, although joined bonding agent, hardness and wearability are still below single-crystal diamond.
Summary of the invention
The object of the present invention is to provide a kind of wear-resisting PCD composite sheet and preparation method thereof, which has excellent Wearability, while the preparation method has the advantages that process is simply and easy to operate.
To achieve the goals above, the present invention provides a kind of preparation methods of wear-resisting PCD composite sheet, comprising:
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel;
2) xerogel is heat-treated to obtain heat-treated products;
3) heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder are subjected to ball milling to obtain bonding agent;
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011Sintering is under Pa to be made the height Hardness PCD composite sheet.
The present invention also provides a kind of wear-resisting PCD composite sheet, which is prepared by above-mentioned preparation method And it obtains.
In above-mentioned technical proposal, the present invention pass through first sol-gel method be made xerogel, then by heat treatment so that Xerogel resolves into the complex being made of many oxide, finally by heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder It is combined to form bonding agent, finally bonding agent, diamond dust is calcined, PCD composite sheet is made;The bonding agent enables to PCD composite sheet obtained has excellent wearability, while the preparation method has the advantages that process is simply and easy to operate.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of preparation methods of wear-resisting PCD composite sheet, comprising:
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel;
2) xerogel is heat-treated to obtain heat-treated products;
3) heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder are subjected to ball milling to obtain bonding agent;
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011Sintering is under Pa to be made the height Hardness PCD composite sheet.
In step 1) of the invention, the dosage of each material can select in a wide range, but in order to further mention The wearability of PCD composite sheet made from height, it is preferable that in step 1), nano silica, sodium salt, aluminium salt, boric acid, zirconates, Yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.4-0.6:0.7-0.9:0.2-0.4:0.05-0.15:0.08-0.12: 0.1-0.3:0.25-0.35.
In step 1) of the invention, hydrochloric acid, the aqueous solution of alcohol, lye dosage can select in a wide range, but The wearability in order to further increase PCD composite sheet obtained, it is preferable that in step 1), nano silica, hydrochloric acid, The aqueous solution of alcohol, lye amount ratio be 1mmol:2-3mL:5-10mL:4-6mL, and in the aqueous solution of alcohol alcohol volume fraction It is 4-5 for 30-40%, the pH of hydrochloric acid, the pH of lye is 11-13.
In step 1) of the invention, the type of each material can select in a wide range, but in order to further mention The wearability of PCD composite sheet made from height, it is preferable that in step 1), the alcohol of the aqueous solution of alcohol is selected from ethyl alcohol, methanol, propyl alcohol At least one of with isopropanol;Lye is selected from least one of potassium hydroxide aqueous solution, sodium hydrate aqueous solution;Sodium salt choosing From at least one of sodium chloride, sodium sulphate, sodium nitrate;Aluminium salt is selected from least one of aluminum nitrate, aluminium chloride, aluminum acetate; Zirconates is selected from least one of zirconium nitrate, citric acid zirconates;Yttrium salt is selected from yttrium nitrate, three (radical) yttrium salts, fluoroform At least one of alkyl sulfonic acid yttrium;Nickel salt is selected from least one of nickel nitrate, nickel sulfate, nickel chloride.
In step 1) of the invention, the condition of ageing can select in a wide range, but in order to further increase The wearability of PCD composite sheet obtained, it is preferable that in step 1), ageing meets the following conditions: Aging Temperature is 25-35 DEG C, Digestion time is 18-24h.
In step 1) of the invention, dry condition can select in a wide range, but in order to further increase The wearability of PCD composite sheet obtained, in step 1), drying meets the following conditions: drying temperature is 100-110 DEG C, dry Time is 2-4h.
In step 1) of the invention, the mixed time can select in a wide range, but in order to further increase The wearability of PCD composite sheet obtained, it is preferable that in step 1), the mixed time is 15-20min.
In step 2) of the invention, the condition of heat treatment can select in a wide range, but in order to further mention The wearability of PCD composite sheet made from height, it is preferable that in step 2, heat treatment meets the following conditions: treatment temperature 510- 530 DEG C, the processing time is 6-10h.
In step 3) of the invention, the dosage of each material can select in a wide range, but in order to further mention The wearability of PCD composite sheet made from height, it is preferable that in step 3), heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder Weight ratio is 10:1-3:1.6-2:1.7-2.1:0.5-0.8.
In step 3) of the invention, the condition of ball milling can select in a wide range, but in order to further increase The wearability of PCD composite sheet obtained, it is preferable that in step 3), ball milling meets the following conditions: the mass ratio of abrading-ball and material For 20:0.8-1.2, revolving speed 1600-1800rpm, Ball-milling Time 40-60min.
In step 4) of the invention, the time of calcining can select in a wide range, but in order to further increase The wearability of PCD composite sheet obtained, it is preferable that in step 4), the time of calcining is 12-15h;
In step 4) of the invention, the granularity of diamond dust can select in a wide range, but in order to further mention The wearability of PCD composite sheet made from height, it is preferable that in step 4), the granularity of diamond dust is 2-4 μm.
The present invention also provides a kind of wear-resisting PCD composite sheet, which is prepared by above-mentioned preparation method And it obtains.
The present invention will be described in detail by way of examples below.
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (ethyl alcohol), is subsequently added into sodium salt (sodium chloride), aluminium Salt (aluminum nitrate), boric acid, zirconates (zirconium nitrate), yttrium salt (yttrium nitrate), nickel salt (nickel nitrate), butyl titanate mixing 18min, so Lye (potassium hydroxide aqueous solution) is added dropwise afterwards and stirs 18min, finally ageing (Aging Temperature is 30 DEG C, digestion time 20h), Dry (drying temperature is 105 DEG C, drying time 3h) is to obtain xerogel;Wherein, nano silica, sodium salt, aluminium salt, boron Acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.5:0.8:0.3:0.1:0.1:0.2:0.30;Nano-silica SiClx, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:2.5mL:8mL:5mL, and alcohol in the aqueous solution of the alcohol Volume fraction is 35%, and the pH of the hydrochloric acid is 4.5, and the pH of the lye is 12;
2) xerogel is heat-treated (treatment temperature is 520 DEG C, and the processing time is 8h) to obtain heat-treated products;
3) by heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder according to the weight ratio row ball milling (mill of 10:2:1.8:1.9:0.7 The mass ratio of ball and material is 20:1, revolving speed 1700rpm, Ball-milling Time 50min) to obtain bonding agent A1.
Embodiment 2
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (propyl alcohol), is subsequently added into sodium salt (sodium sulphate), aluminium salt (aluminium chloride), boric acid, zirconates (citric acid zirconates), yttrium salt (three (radical) yttrium salts), nickel salt (nickel sulfate), butyl titanate 15min is mixed, lye (sodium hydrate aqueous solution) is then added dropwise and stirs 15min, (Aging Temperature is 25 DEG C, old for finally ageing Changing the time is for 24 hours), dry (drying temperature is 100 DEG C, drying time 4h) to obtain xerogel;Wherein, nanometer titanium dioxide Silicon, sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.4:0.7:0.2:0.05:0.08: 0.1:0.25;Nano silica, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:2mL:5mL:4mL, and it is described The volume fraction of alcohol is 30% in the aqueous solution of alcohol, and the pH of the hydrochloric acid is 4, and the pH of the lye is 11;
2) xerogel is heat-treated (treatment temperature is 510 DEG C, and the processing time is 10h) to obtain heat-treated products;
3) by heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder according to the weight ratio row ball milling (mill of 10:1:1.6:1.7:0.5 The mass ratio of ball and material is 20:0.8, revolving speed 1600rpm, Ball-milling Time 60min) to obtain bonding agent A2.
Embodiment 3
1) it disperses nano silica, hydrochloric acid in the aqueous solution of alcohol (isopropanol), is subsequently added into sodium salt (sodium nitrate), aluminium salt (aluminum acetate), boric acid, zirconates (citric acid zirconates), yttrium salt (trifluoromethayl sulfonic acid yttrium), nickel salt (nickel chloride), butyl titanate are mixed 20min is closed, lye (sodium hydrate aqueous solution) is then added dropwise and stirs 20min, (Aging Temperature is 35 DEG C, ageing for finally ageing Time is 18h), dry (drying temperature is 110 DEG C, drying time 2h) to obtain xerogel;Wherein, nano silica, Sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.6:0.9:0.4:0.15:0.12: 0.3:0.35;Nano silica, hydrochloric acid, the aqueous solution of alcohol, lye amount ratio be 1mmol:3mL:10mL:6mL, and it is described The volume fraction of alcohol is 40% in the aqueous solution of alcohol, and the pH of the hydrochloric acid is 5, and the pH of the lye is 13;
2) xerogel is heat-treated (treatment temperature is 530 DEG C, and the processing time is 6h) to obtain heat-treated products;
3) by heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder according to the weight ratio row ball milling (abrading-ball of 10:3:2:2.1:0.8 Mass ratio with material is 20:1.2, revolving speed 1800rpm, Ball-milling Time 40min) to obtain bonding agent A3.
Application examples 1
By granularity be 2 μm of diamond dusts, above-mentioned bonding agent according to the weight ratio of 1:5 in 1700 DEG C, 7 × 1011It is sintered under Pa Then 13h detects the thermal coefficient of PCD composite sheet, the results are shown in Table 1 so that wear-resisting PCD composite sheet is made.
Table 1
Bonding agent A1 A2 A3
Thermal coefficient (W/mK) 786 779 769
Wherein, thermal coefficient is higher, is more avoided that the abrasion of PCD composite sheet, and then improve the wearability of PCD composite sheet.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (10)

1. a kind of preparation method of wear-resisting PCD composite sheet characterized by comprising
1) disperse nano silica, hydrochloric acid in the aqueous solution of alcohol, be subsequently added into sodium salt, aluminium salt, boric acid, zirconates, yttrium salt, Then nickel salt, butyl titanate mixing are added dropwise lye and stir, be finally aged, be dry to obtain xerogel;
2) xerogel is heat-treated to obtain heat-treated products;
3) heat-treated products, zinc powder, molybdenum powder, titanium valve and aluminium powder are subjected to ball milling to obtain bonding agent;
4) by diamond dust, bonding agent in 1600-1800 DEG C, 2 × 1011Pa-10×1011It is sintered under Pa to be made described high hard Spend PCD composite sheet.
2. preparation method according to claim 1, wherein in step 1), the nano silica, sodium salt, aluminium salt, Boric acid, zirconates, yttrium salt, nickel salt, butyl titanate molar ratio be 1:0.4-0.6:0.7-0.9:0.2-0.4:0.05-0.15: 0.08-0.12:0.1-0.3:0.25-0.35.
3. preparation method according to claim 1, wherein in step 1), the nano silica, hydrochloric acid, alcohol Aqueous solution, lye amount ratio be 1mmol:2-3mL:5-10mL:4-6mL, and in the aqueous solution of the alcohol alcohol volume fraction It is 4-5 for 30-40%, the pH of the hydrochloric acid, the pH of the lye is 11-13;
Preferably, in step 1), the alcohol of the aqueous solution of the alcohol in ethyl alcohol, methanol, propyl alcohol and isopropanol at least one Person;The lye is selected from least one of potassium hydroxide aqueous solution, sodium hydrate aqueous solution;The sodium salt be selected from sodium chloride, At least one of sodium sulphate, sodium nitrate;The aluminium salt is selected from least one of aluminum nitrate, aluminium chloride, aluminum acetate;The zirconium Salt is selected from least one of zirconium nitrate, citric acid zirconates;The yttrium salt is selected from yttrium nitrate, three (radical) yttrium salts, trifluoro At least one of Loprazolam yttrium;The nickel salt is selected from least one of nickel nitrate, nickel sulfate, nickel chloride.
4. preparation method according to claim 1, wherein in step 1), the ageing meets the following conditions: ageing temperature Degree is 25-35 DEG C, digestion time 18-24h.
5. preparation method according to claim 1, wherein in step 1), the drying meets the following conditions: dry temperature Degree is 100-110 DEG C, drying time 2-4h.
6. preparation method according to claim 1, wherein in step 1), the mixed time is 15-20min.
7. preparation method according to claim 1, wherein in step 2, the heat treatment meets the following conditions: processing Temperature is 510-530 DEG C, and the processing time is 6-10h.
8. preparation method according to claim 1, wherein in step 3), the heat-treated products, zinc powder, molybdenum powder, titanium The weight ratio of powder and aluminium powder is 10:1-3:1.6-2:1.7-2.1:0.5-0.8.
9. preparation method according to claim 1, wherein in step 3), the ball milling meets the following conditions: abrading-ball with The mass ratio of material is 20:0.8-1.2, revolving speed 1600-1800rpm, Ball-milling Time 40-60min;
Preferably, in step 4), the time of the calcining is 12-15h;
It is highly preferred that the granularity of the diamond dust is 2-4 μm in step 4).
10. a kind of wear-resisting PCD composite sheet, which is characterized in that the wear-resisting PCD composite sheet passes through any one in claim 1-9 Preparation method described in is prepared.
CN201811022030.7A 2018-09-04 2018-09-04 Wear-resisting PCD composite sheet and preparation method thereof Withdrawn CN109097650A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115319647A (en) * 2022-08-09 2022-11-11 河南科技大学 Xerogel and preparation method thereof, organic-inorganic composite bonding agent, corundum abrasive tool and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103722174A (en) * 2013-12-30 2014-04-16 中原工学院 Self-sharpening polycrystalline diamond compact and preparation method thereof
WO2014143700A1 (en) * 2013-03-15 2014-09-18 Smith International, Inc. Carbonate pcd and methods of making the same
CN105108666A (en) * 2015-07-29 2015-12-02 苏州赛力精密工具有限公司 Ceramic diamond grinding wheel for machining PCD saw blades and preparation method thereof
CN106498253A (en) * 2016-09-21 2017-03-15 芜湖扬展新材料科技服务有限公司 A kind of polycrystalline diamond composite material with high stable wearability and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014143700A1 (en) * 2013-03-15 2014-09-18 Smith International, Inc. Carbonate pcd and methods of making the same
CN103722174A (en) * 2013-12-30 2014-04-16 中原工学院 Self-sharpening polycrystalline diamond compact and preparation method thereof
CN105108666A (en) * 2015-07-29 2015-12-02 苏州赛力精密工具有限公司 Ceramic diamond grinding wheel for machining PCD saw blades and preparation method thereof
CN106498253A (en) * 2016-09-21 2017-03-15 芜湖扬展新材料科技服务有限公司 A kind of polycrystalline diamond composite material with high stable wearability and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115319647A (en) * 2022-08-09 2022-11-11 河南科技大学 Xerogel and preparation method thereof, organic-inorganic composite bonding agent, corundum abrasive tool and preparation method thereof
CN115319647B (en) * 2022-08-09 2024-01-19 河南科技大学 Xerogel and preparation method thereof, organic-inorganic composite binding agent, corundum grinding tool and preparation method thereof

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Application publication date: 20181228