GB679172A - Improvements in or relating to the production of metal or metal oxide powders and products therefrom - Google Patents
Improvements in or relating to the production of metal or metal oxide powders and products therefromInfo
- Publication number
- GB679172A GB679172A GB1118348A GB1118348A GB679172A GB 679172 A GB679172 A GB 679172A GB 1118348 A GB1118348 A GB 1118348A GB 1118348 A GB1118348 A GB 1118348A GB 679172 A GB679172 A GB 679172A
- Authority
- GB
- United Kingdom
- Prior art keywords
- oxalates
- sulphate
- solution
- sulphates
- metal
- 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.)
- Expired
Links
- 229910052751 metal Inorganic materials 0.000 title abstract 16
- 239000002184 metal Substances 0.000 title abstract 16
- 239000000843 powder Substances 0.000 title abstract 6
- 238000004519 manufacturing process Methods 0.000 title abstract 5
- 229910044991 metal oxide Inorganic materials 0.000 title abstract 5
- 150000004706 metal oxides Chemical class 0.000 title abstract 5
- 150000003891 oxalate salts Chemical class 0.000 abstract 17
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 12
- 239000000243 solution Substances 0.000 abstract 11
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract 9
- 229910021653 sulphate ion Inorganic materials 0.000 abstract 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 abstract 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 7
- 239000007864 aqueous solution Substances 0.000 abstract 7
- 239000008103 glucose Substances 0.000 abstract 7
- 150000002739 metals Chemical class 0.000 abstract 7
- 150000003467 sulfuric acid derivatives Chemical class 0.000 abstract 7
- 235000011149 sulphuric acid Nutrition 0.000 abstract 7
- 239000001117 sulphuric acid Substances 0.000 abstract 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 6
- 235000003891 ferrous sulphate Nutrition 0.000 abstract 6
- 239000002244 precipitate Substances 0.000 abstract 6
- 239000003638 chemical reducing agent Substances 0.000 abstract 5
- 238000000354 decomposition reaction Methods 0.000 abstract 5
- 235000006408 oxalic acid Nutrition 0.000 abstract 5
- 238000001556 precipitation Methods 0.000 abstract 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 abstract 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 abstract 4
- 230000015572 biosynthetic process Effects 0.000 abstract 4
- 229910052759 nickel Inorganic materials 0.000 abstract 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 3
- 230000001747 exhibiting effect Effects 0.000 abstract 3
- 239000001257 hydrogen Substances 0.000 abstract 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 abstract 3
- 238000000034 method Methods 0.000 abstract 3
- 238000003825 pressing Methods 0.000 abstract 3
- 238000005245 sintering Methods 0.000 abstract 3
- 229910000531 Co alloy Inorganic materials 0.000 abstract 2
- 229910001313 Cobalt-iron alloy Inorganic materials 0.000 abstract 2
- 229910000640 Fe alloy Inorganic materials 0.000 abstract 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract 2
- 229910000990 Ni alloy Inorganic materials 0.000 abstract 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 2
- 239000002253 acid Substances 0.000 abstract 2
- 239000010941 cobalt Substances 0.000 abstract 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 abstract 2
- MPMSMUBQXQALQI-UHFFFAOYSA-N cobalt phthalocyanine Chemical compound [Co+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 MPMSMUBQXQALQI-UHFFFAOYSA-N 0.000 abstract 2
- 239000011790 ferrous sulphate Substances 0.000 abstract 2
- 239000011521 glass Substances 0.000 abstract 2
- 229910052742 iron Inorganic materials 0.000 abstract 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract 2
- 229910001004 magnetic alloy Inorganic materials 0.000 abstract 2
- 239000000203 mixture Substances 0.000 abstract 2
- 229910052750 molybdenum Inorganic materials 0.000 abstract 2
- 239000011733 molybdenum Substances 0.000 abstract 2
- ICYJJTNLBFMCOZ-UHFFFAOYSA-J molybdenum(4+);disulfate Chemical compound [Mo+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ICYJJTNLBFMCOZ-UHFFFAOYSA-J 0.000 abstract 2
- 229910000480 nickel oxide Inorganic materials 0.000 abstract 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 abstract 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 abstract 2
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 abstract 2
- 239000007787 solid Substances 0.000 abstract 2
- 238000001179 sorption measurement Methods 0.000 abstract 2
- 229910052596 spinel Inorganic materials 0.000 abstract 2
- 239000011029 spinel Substances 0.000 abstract 2
- 229910052566 spinel group Inorganic materials 0.000 abstract 2
- -1 sulphate ions Chemical class 0.000 abstract 2
- 229910052725 zinc Inorganic materials 0.000 abstract 2
- 239000011701 zinc Substances 0.000 abstract 2
- 239000011787 zinc oxide Substances 0.000 abstract 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 238000011068 loading method Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000012255 powdered metal Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
-
- 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
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Insoluble metal oxalates used for making finely divided metals or metal oxides by decomposition of the oxalates (see Groups II and III) are prepared by a precipitation method comprising the addition of oxalic acid to an aqueous solution of the corresponding sulphates, which solution contains at least one sulphate which is a lower valency sulphate of a metal exhibiting variable valency, said precipitation taking place at a temperature between 40 DEG and 90 DEG C. in the presence of an organic reducing agent not substantially more readily oxidized in the solution than formaldehyde, e.g. formaldehyde or a sugar such as glucose, and also in the presence of an amount of sulphuric acid sufficient to bring the pH of the solution to a value not exceeding 3. The reducing agent prevents formation of the higher valency sulphates, the acid prevents formation of basic sulphates and the temperature prevents adsorption of sulphate ions by the precipitate. Reference is made to the production of alloys of iron, nickel and cobalt such as those capable of being sealed through the glass of vacuum tubes and to magnetic bodies formed of mixed oxides of two or more metals such as the magnetic spinels. In examples: (1) in producing a 50 : 50 cobalt-iron alloy, mixed oxalates are precipitated by oxalic acid from an aqueous solution of cobaltous and ferrous sulphates containing sulphuric acid and glucose at 70 DEG C., the precipitate is washed, dried and powdered; (2) in producing a magnetic spinel formed of zinc oxide, nickel oxide and ferric oxide in the solar ratios of 35, 15 and 50 per cent respectively, the mixed oxalates are precipitated from an aqueous solution of zinc, nickel and ferrous sulphates containing sulphuric acid and glucose at 70 DEG C., the precipitate is washed, dried and sieved; (3) in producing a magnetic alloy containing nickel, molybdenum and iron in the proportions 78.5, 4 and 17.5 per cent, the mixed oxalates are precipitated as in (1) from a solution of nickel sulphate, ferrous sulphate and molybdenum sulphate.ALSO:A process for making finely divided metal oxides by the decomposition of insoluble oxalates of the metals includes the precipitation of metal oxalates by the addition of oxalic acid to an aqueous solution of the corresponding sulphates which solution contains at least one sulphate which is a lower valency sulphate of a metal exhibiting variable valency in which said presipitation takes place at a temperature between 40 DEG and 90 DEG C in the presence of an organic reducing agent not substantially more readily oxidized in the solution than formaldehyde, e.g. formaldehyde or a sugar such as glucose, and also in the presence of an amount of sulphuric acid sufficient to bring the pH of the solution to a value not exceeding 3. The reducing agent prevents formation of the higher valency sulphates, the acid prevents formation of basic sulphates and the temperature prevents adsorption of sulphate ions by the precipitate. The precipitated oxalates are heated to between 400 DEG and 800 DEG C in the presence of air or oxygen to form the metal oxides. The resulting metal oxide powders are made into solid bodies by pressing and sintering and to obtain a high density, it is preferred to use a mixture of powders formed by decomposition of the oxalates at different respective temperatures. Reference is made to the production of magnetic bodies formed of mixed oxides of two or more metals such as the magnetic spinels. In one example, a magnetic spinel formed of zinc oxide, nickel oxide and ferric oxide in the molar ratios of 35, 15 and 50 per cent respectively is prepared by co-precipitating the mixed oxalates by addition of oxalic acid to an aqueous solution of zinc, nickel and ferrous sulphates containing sulphuric acid and glucose at 70 DEG C, the precipitate is washed, dried and sieved and then decomposed in air in two batches at 750 DEG and 600 DEG C to form mixed oxides which are used to form an inductance core (see Group XXXV).ALSO:A process for making finely divided metals by the decomposition of insoluble oxalates of the metals includes the precipitation of metal oxalates by the addition of oxalic acid to an aqueous solution of the corresponding sulphates which solution contains at least one sulphate which is a lower valency sulphate of a metal exhibiting variable valency in which said precipitation takes place at a temperature between 40 DEG and 90 DEG C in the presence of an organic reducing agent not substantially more readily oxidized in the solution than formaldehyde, e.g. formaldehyde or a sugar such as glucose, and also in the presence of an amount of sulphuric acid sufficient to bring the pH of the solution to a value not exceeding 3. The precipitated oxalates are heated to between 400 DEG and 800 DEG C in the presence of an atmosphere of hydrogen preferably containing between 1 2 and 10 per cent of water vapour to form the metals. The resulting metal powders are made into solid bodies by pressing and sintering and to obtain a high density, it is preferred to use a mixture of powders formed by decomposition of the oxalates at different respective temperatures. Reference is made to the production of alloys of iron, nickel and cobalt such as those capable of being sealed through the glass of vacuum tubes. In examples (1) a 50 : 50 cobalt-iron alloy is prepared by co-precipitation of the mixed oxalates from an aqueous solution of cobaltous and ferrous sulphates containing sulphuric acid and glucose at 70 DEG C, the precipitate is washed, dried, powdered and reduced in hydrogen in two batches at 525 DEG C and 675 DEG C, and the resulting powdered metals are mixed in the proportions of 16 per cent of the first batch and 84 of the second batch and then pressed to desired shape and sintered to form thin discs, e.g. telephone diaphragms; (2) a magnetic alloy containing nickel, molybdenum and iron in the proportions 78.5, 4 and 17.5 per cent is prepared by co-precipitating the mixed oxalates as in (1) from a solution of nickel sulphate, ferrous sulphate and molybdenum sulphate, reducing the mixed powdered oxalates in hydrogen in two batches at 700 DEG C and 575 DEG C, mixing the resulting metal powders in the proportions 84 : 16 per cent and then pressing and sintering to desired shape. The Provisional Specification refers to the production of cores of loading coils or other inductances, pole pieces of telephone receiver magnets and telephone or telegraph relay magnets.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB1118348A GB679172A (en) | 1948-04-23 | 1948-04-23 | Improvements in or relating to the production of metal or metal oxide powders and products therefrom |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB1118348A GB679172A (en) | 1948-04-23 | 1948-04-23 | Improvements in or relating to the production of metal or metal oxide powders and products therefrom |
Publications (1)
Publication Number | Publication Date |
---|---|
GB679172A true GB679172A (en) | 1952-09-17 |
Family
ID=9981541
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB1118348A Expired GB679172A (en) | 1948-04-23 | 1948-04-23 | Improvements in or relating to the production of metal or metal oxide powders and products therefrom |
Country Status (1)
Country | Link |
---|---|
GB (1) | GB679172A (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2320182A1 (en) * | 1972-04-21 | 1973-10-31 | Anvar | PROCESS FOR THE PREPARATION OF SOLID SOLUTIONS FROM OXIDES OF IRON AND DIVALENT METALS |
DE2540758A1 (en) * | 1974-09-13 | 1976-03-25 | Anvar | Process for the preparation of solid solutions from iron oxides and divalent metals |
CN106623962A (en) * | 2016-12-31 | 2017-05-10 | 湖南省华京粉体材料有限公司 | Method for preparing nanometer tungsten powder by organizing sodium tungstate |
CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
US11607734B2 (en) | 2018-05-30 | 2023-03-21 | Hela Novel Metals Llc | Methods for the production of fine metal powders from metal compounds |
-
1948
- 1948-04-23 GB GB1118348A patent/GB679172A/en not_active Expired
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2320182A1 (en) * | 1972-04-21 | 1973-10-31 | Anvar | PROCESS FOR THE PREPARATION OF SOLID SOLUTIONS FROM OXIDES OF IRON AND DIVALENT METALS |
DE2540758A1 (en) * | 1974-09-13 | 1976-03-25 | Anvar | Process for the preparation of solid solutions from iron oxides and divalent metals |
CN106623962A (en) * | 2016-12-31 | 2017-05-10 | 湖南省华京粉体材料有限公司 | Method for preparing nanometer tungsten powder by organizing sodium tungstate |
CN106735282A (en) * | 2016-12-31 | 2017-05-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
CN106623962B (en) * | 2016-12-31 | 2018-07-31 | 湖南省华京粉体材料有限公司 | A kind of sodium tungstate organises the method for preparing nano-tungsten powder |
CN106735282B (en) * | 2016-12-31 | 2018-07-31 | 湖南省华京粉体材料有限公司 | A kind of sodium molybdate organises the method for preparing nano Mo powder |
US11607734B2 (en) | 2018-05-30 | 2023-03-21 | Hela Novel Metals Llc | Methods for the production of fine metal powders from metal compounds |
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