AU2015216114B2 - Nickel powder production method - Google Patents
Nickel powder production method Download PDFInfo
- Publication number
- AU2015216114B2 AU2015216114B2 AU2015216114A AU2015216114A AU2015216114B2 AU 2015216114 B2 AU2015216114 B2 AU 2015216114B2 AU 2015216114 A AU2015216114 A AU 2015216114A AU 2015216114 A AU2015216114 A AU 2015216114A AU 2015216114 B2 AU2015216114 B2 AU 2015216114B2
- Authority
- AU
- Australia
- Prior art keywords
- nickel
- insoluble solid
- nickel powder
- solution
- mixed slurry
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 209
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 73
- 239000007787 solid Substances 0.000 claims abstract description 61
- 239000011268 mixed slurry Substances 0.000 claims abstract description 37
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000001556 precipitation Methods 0.000 claims abstract description 20
- 239000002244 precipitate Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 150000002500 ions Chemical class 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 24
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 10
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 16
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 abstract description 10
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 abstract description 9
- 239000000243 solution Substances 0.000 description 68
- 238000000034 method Methods 0.000 description 19
- 239000000843 powder Substances 0.000 description 19
- 239000002270 dispersing agent Substances 0.000 description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 239000011159 matrix material Substances 0.000 description 10
- 239000002002 slurry Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 229920005552 sodium lignosulfonate Polymers 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 238000002386 leaching Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229920001732 Lignosulfonate Polymers 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 239000013462 industrial intermediate Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- -1 nickel sulfate amine Chemical class 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F9/26—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions using gaseous reductors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/15—Nickel or cobalt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2014027902 | 2014-02-17 | ||
| JP2014-027902 | 2014-02-17 | ||
| JP2014-155511 | 2014-07-30 | ||
| JP2014155511A JP6099601B2 (ja) | 2014-02-17 | 2014-07-30 | ニッケル粉の製造方法 |
| PCT/JP2015/054281 WO2015122535A1 (ja) | 2014-02-17 | 2015-02-17 | ニッケル粉の製造方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| AU2015216114A1 AU2015216114A1 (en) | 2016-09-01 |
| AU2015216114B2 true AU2015216114B2 (en) | 2017-04-13 |
Family
ID=53800271
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2015216114A Ceased AU2015216114B2 (en) | 2014-02-17 | 2015-02-17 | Nickel powder production method |
| AU2015216113A Ceased AU2015216113B2 (en) | 2014-02-17 | 2015-02-17 | Nickel powder production method |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AU2015216113A Ceased AU2015216113B2 (en) | 2014-02-17 | 2015-02-17 | Nickel powder production method |
Country Status (8)
| Country | Link |
|---|---|
| US (2) | US10092955B2 (https=) |
| EP (2) | EP3144084B1 (https=) |
| JP (1) | JP6099601B2 (https=) |
| CN (2) | CN106029268B (https=) |
| AU (2) | AU2015216114B2 (https=) |
| CA (2) | CA2939513C (https=) |
| PH (2) | PH12016501628B1 (https=) |
| WO (2) | WO2015122535A1 (https=) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5936783B2 (ja) * | 2014-02-21 | 2016-06-22 | 国立大学法人高知大学 | ニッケル粉の製造方法 |
| JP6350830B2 (ja) * | 2015-10-26 | 2018-07-04 | 住友金属鉱山株式会社 | コバルト粉の種結晶の製造方法 |
| JP6202348B2 (ja) * | 2015-10-26 | 2017-09-27 | 住友金属鉱山株式会社 | 高密度ニッケル粉の製造方法 |
| JP6726396B2 (ja) * | 2016-02-22 | 2020-07-22 | 住友金属鉱山株式会社 | ニッケル粉の製造方法 |
| JP6641632B2 (ja) * | 2016-03-04 | 2020-02-05 | 住友金属鉱山株式会社 | ニッケル粉の製造方法 |
| JP6245314B2 (ja) | 2016-05-30 | 2017-12-13 | 住友金属鉱山株式会社 | ニッケル粉の製造方法 |
| JP2018141203A (ja) * | 2017-02-28 | 2018-09-13 | 住友金属鉱山株式会社 | 種晶用ニッケル粉末の製造方法 |
| JP6624464B2 (ja) * | 2017-12-21 | 2019-12-25 | 住友金属鉱山株式会社 | ニッケル粉の製造方法 |
| CN121467686B (zh) * | 2026-01-09 | 2026-04-14 | 西安稀有金属材料研究院有限公司 | 一种高分散超细球形镍粉的制备方法 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2734821A (en) * | 1956-02-14 | Table ix |
Family Cites Families (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2805139A (en) * | 1956-10-19 | 1957-09-03 | American Cyanamid Co | Gaseous precipitation of metals from solution |
| US3399050A (en) | 1964-04-13 | 1968-08-27 | Sherritt Gordon Mines Ltd | Production of nickel powder |
| US3767762A (en) | 1972-01-04 | 1973-10-23 | Sherritt Gordon Mines Ltd | Recovery and separation of nickel and cobalt from reduced laterite nickel ore |
| US4545814A (en) * | 1984-05-23 | 1985-10-08 | Amax Inc. | Production of cobalt and nickel powder |
| US4758266A (en) * | 1986-08-11 | 1988-07-19 | Amax Inc. | Production of high surface area nickel powder |
| JPS6379904A (ja) * | 1986-09-25 | 1988-04-09 | Sumitomo Metal Mining Co Ltd | 金粉の製造方法 |
| US5584908A (en) * | 1994-11-14 | 1996-12-17 | Sherritt Inc. | Micron-sized nickel metal powder and a process for the preparation thereof |
| JPH10219363A (ja) * | 1997-02-07 | 1998-08-18 | Nanao Kogyo Kk | 溶液中の金属の回収方法および装置 |
| FI106635B (fi) * | 1999-11-09 | 2001-03-15 | Outokumpu Oy | Menetelmä nikkelin pelkistämiseksi vesiliuoksesta |
| CA2359347A1 (en) | 2001-10-18 | 2003-04-18 | Cesur Celik | Laminated ceramic capacitor internal electrode material |
| AUPR917701A0 (en) | 2001-11-29 | 2001-12-20 | QNI Technology Limited | Integrated ammoniacal solvent extraction and hydrogen reduction of nickel |
| KR101014158B1 (ko) | 2002-08-28 | 2011-02-14 | 도호 티타늄 가부시키가이샤 | 금속 니켈 분말 및 그 제조 방법 |
| CN1292866C (zh) * | 2005-01-10 | 2007-01-03 | 北京工业大学 | 一种纳米镍粉的制备方法 |
| WO2007004664A1 (ja) * | 2005-07-06 | 2007-01-11 | Kobelco Eco-Solutions Co., Ltd. | 金属の回収方法とその装置 |
| JP4811881B2 (ja) | 2009-03-18 | 2011-11-09 | 東京エレクトロン株式会社 | 基板熱処理装置 |
| JP5407495B2 (ja) | 2009-04-02 | 2014-02-05 | 住友電気工業株式会社 | 金属粉末および金属粉末製造方法、導電性ペースト、並びに積層セラミックコンデンサ |
| JP2011214143A (ja) * | 2010-03-17 | 2011-10-27 | Nippon Steel Chem Co Ltd | ニッケルナノ粒子の製造方法 |
| WO2011115213A1 (ja) | 2010-03-17 | 2011-09-22 | 新日鐵化学株式会社 | ニッケルナノ粒子の製造方法 |
| CN103391824B (zh) * | 2011-02-25 | 2015-11-25 | 株式会社村田制作所 | 镍粉末的制造方法 |
-
2014
- 2014-07-30 JP JP2014155511A patent/JP6099601B2/ja active Active
-
2015
- 2015-02-17 WO PCT/JP2015/054281 patent/WO2015122535A1/ja not_active Ceased
- 2015-02-17 CA CA2939513A patent/CA2939513C/en not_active Expired - Fee Related
- 2015-02-17 CA CA2939493A patent/CA2939493C/en not_active Expired - Fee Related
- 2015-02-17 WO PCT/JP2015/054280 patent/WO2015122534A1/ja not_active Ceased
- 2015-02-17 CN CN201580008758.2A patent/CN106029268B/zh not_active Expired - Fee Related
- 2015-02-17 US US15/117,855 patent/US10092955B2/en not_active Expired - Fee Related
- 2015-02-17 EP EP15748828.9A patent/EP3144084B1/en active Active
- 2015-02-17 EP EP15748557.4A patent/EP3108986B1/en active Active
- 2015-02-17 AU AU2015216114A patent/AU2015216114B2/en not_active Ceased
- 2015-02-17 CN CN201580008922.XA patent/CN106029269B/zh not_active Expired - Fee Related
- 2015-02-17 AU AU2015216113A patent/AU2015216113B2/en not_active Ceased
- 2015-02-17 US US15/117,823 patent/US10220446B2/en not_active Expired - Fee Related
-
2016
- 2016-08-16 PH PH12016501628A patent/PH12016501628B1/en unknown
- 2016-08-17 PH PH12016501637A patent/PH12016501637B1/en unknown
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2734821A (en) * | 1956-02-14 | Table ix |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106029269B (zh) | 2017-12-12 |
| EP3144084B1 (en) | 2019-06-05 |
| EP3108986A4 (en) | 2018-01-10 |
| PH12016501637B1 (en) | 2018-06-06 |
| EP3144084A4 (en) | 2018-01-03 |
| JP2015166488A (ja) | 2015-09-24 |
| PH12016501628A1 (en) | 2017-02-06 |
| PH12016501637A1 (en) | 2017-02-06 |
| EP3108986B1 (en) | 2019-05-22 |
| EP3108986A1 (en) | 2016-12-28 |
| US20160354844A1 (en) | 2016-12-08 |
| CN106029268A (zh) | 2016-10-12 |
| US20160368059A1 (en) | 2016-12-22 |
| CN106029269A (zh) | 2016-10-12 |
| CA2939513A1 (en) | 2015-08-20 |
| EP3144084A1 (en) | 2017-03-22 |
| US10092955B2 (en) | 2018-10-09 |
| JP6099601B2 (ja) | 2017-03-22 |
| PH12016501628B1 (en) | 2017-02-06 |
| AU2015216113A1 (en) | 2016-09-01 |
| AU2015216113B2 (en) | 2017-03-09 |
| AU2015216114A1 (en) | 2016-09-01 |
| WO2015122535A1 (ja) | 2015-08-20 |
| CA2939493A1 (en) | 2015-08-20 |
| US10220446B2 (en) | 2019-03-05 |
| CN106029268B (zh) | 2017-12-12 |
| CA2939493C (en) | 2018-02-27 |
| CA2939513C (en) | 2017-04-04 |
| WO2015122534A1 (ja) | 2015-08-20 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FGA | Letters patent sealed or granted (standard patent) | ||
| MK14 | Patent ceased section 143(a) (annual fees not paid) or expired |