CN1264758C - Cobalt oxide ultra-fine powder and its preparation method - Google Patents
Cobalt oxide ultra-fine powder and its preparation method Download PDFInfo
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- CN1264758C CN1264758C CN 200310121805 CN200310121805A CN1264758C CN 1264758 C CN1264758 C CN 1264758C CN 200310121805 CN200310121805 CN 200310121805 CN 200310121805 A CN200310121805 A CN 200310121805A CN 1264758 C CN1264758 C CN 1264758C
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229910000428 cobalt oxide Inorganic materials 0.000 title claims abstract description 17
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 title claims description 18
- 238000000034 method Methods 0.000 claims abstract description 33
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 25
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 22
- 239000010941 cobalt Substances 0.000 claims abstract description 22
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 22
- LBFUKZWYPLNNJC-UHFFFAOYSA-N cobalt(ii,iii) oxide Chemical compound [Co]=O.O=[Co]O[Co]=O LBFUKZWYPLNNJC-UHFFFAOYSA-N 0.000 claims abstract description 18
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 14
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 14
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 28
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 claims description 12
- 229910000001 cobalt(II) carbonate Inorganic materials 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 150000001868 cobalt Chemical class 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000006213 oxygenation reaction Methods 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 1
- 238000001556 precipitation Methods 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 6
- 230000001419 dependent effect Effects 0.000 abstract description 5
- 239000011521 glass Substances 0.000 abstract description 5
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- 238000004062 sedimentation Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000002019 doping agent Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 description 4
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 235000006408 oxalic acid Nutrition 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 241000370738 Chlorion Species 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 2
- JJEJDZONIFQNHG-UHFFFAOYSA-N [C+4].N Chemical compound [C+4].N JJEJDZONIFQNHG-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- MULYSYXKGICWJF-UHFFFAOYSA-L cobalt(2+);oxalate Chemical compound [Co+2].[O-]C(=O)C([O-])=O MULYSYXKGICWJF-UHFFFAOYSA-L 0.000 description 2
- KDPJLLVSZLZTAN-UHFFFAOYSA-K cobalt(3+);carbonate;hydroxide Chemical compound [OH-].[Co+3].[O-]C([O-])=O KDPJLLVSZLZTAN-UHFFFAOYSA-K 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- NSRBDSZKIKAZHT-UHFFFAOYSA-N tellurium zinc Chemical compound [Zn].[Te] NSRBDSZKIKAZHT-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000004931 aggregating effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910021446 cobalt carbonate Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention belongs to the preparation field for cobalt oxide for electronic industry, particularly to cobalt oxide powder mixed with materials for making electronic elements of lightning arresters, thermistors, voltage dependent resistors, display tube glass shells, etc., and a preparation method thereof. The method of the present invention is characterized in that a cobalt nitrate solution which is obtained from the metallic cobalt of a nitric acid dissolution is adopted, the cobalt nitrate solution is filled into ammonium bicarbonate at a certain controlled speed, the ammonium bicarbonate is quickly dissolved by the self-generation heat of reaction, and a dissolving speed is high. The residual acid content of a target solution is very low, and a dissolving process is stable and controllable. Submicron level cobalt oxide powder is prepared by the working procedures of precipitation, filtration, washing, roasting, etc. The diameters d50 of the particles of the submicron level cobalt oxide powder are 0.1 to 1 mu m, and the particles are uniformly distributed. The process of the method is simple, a product prepared by the method is a good quality doping material of electronic elements, and the performance of the electronic elements is obviously enhanced.
Description
Technical field
The invention belongs to preparation used in electronic industry cobalt oxide field, particularly be doped in cobalt oxide powder of materials of electronic components such as making thunder arrester, thermistor, voltage dependent resistor, picture tube glass bulb and preparation method thereof.
Background technology
Cobalt oxide except its chemical ingredients is had high requirements, also has some particular requirements to physicalies such as its particulate crystalline structure, pattern, aggregating state, particle diameter, size-grade distribution, specific surface areas as the electric function ceramic dopant material.
In China's Chemicals, the preparation method of cobalt oxide powder generally is that carbonate, nitrate or the oxyhydroxide with cobalt is raw material, obtains through calcining.Also having plenty of with the cobalt chloride is raw material, adds ammonium oxalate and generates cobalt oxalate precipitation, calcining and getting in air again.By the product that aforesaid method obtains, the content of basic metal, alkaline-earth metal and chlorion is higher, coarse size, and it is also inhomogeneous to distribute, and does not therefore meet the requirement of electronic component adulterated powder material.
Liquid-phase precipitation method is precipitation agent to be joined precipitation is heat-treated after (perhaps adding conversely) in the metal salt solution.Chinese patent CN 1094903C discloses employing carboxylated compound precipitation cobalt salt and has obtained cobalt oxide (II), is mainly used in the electrode materials in the electrochemical secondary cell.Japanese Patent JP2208227A discloses a kind of method for preparing the low density cobalt oxide, this method is that the reaction of raw material and oxalic acid or ammonium oxalate generates cobalt carbonate hydroxide with the cobalt chloride solution, or be that raw material and heavy carbonic alkali reaction generate cobalt carbonate hydroxide with the cobalt nitrate solution, adding oxalic acid generation cobalt oxalate then, filtration, washing, drying make cobalt oxide powder after roasting oxalic acid bores; This method is produced electronic component adulterated powder material and is had Cl
-The ion-cleaning difficulty also is difficult for removing in follow-up calcining process.
More domestic applications for a patent for invention also relate to the preparation of relevant cobalt oxide, as:
Lei Huixu etc., the production method of used in electronic industry cobalt oxide, nickel oxide powder, patent publication No. CN1114639A, open day 1996.1.10 adopts ammonium oxalate to make precipitation agent;
Sun Sixiu etc., the preparation method of nano-cobaltosic oxide powder, patent publication No. CN1344682A, open day 2002.4.17 adopts the bicarbonate of ammonia suspension liquid to make precipitation agent, and the carbon ammonium bores to add in the solution to nitric acid and obtains cobaltous carbonate; Reaction back clear liquid pH=6.5～7.0;
Hu Tianbing etc., the manufacture method of nanometer cobalt oxide, patent publication No. CN1276345A, an open day 2000.12.13 adopts bicarbonate solution to make precipitation agent, also is that the carbon ammonium adds in cobalt nitrate solution and obtains cobaltous carbonate; And adopted tensio-active agent;
The cobalt oxide that these domestic inventions are made or for rod-shpaed particle and granularity thick excessively (ammonium oxalate is made precipitation agent), perhaps too thin, the bad reunion of the excessive formation of specific surface (nano powder) of powder, be difficult to evenly sneak into the electronic ceramics presoma, in the industrial applications process, all have certain problem.
Summary of the invention
One of purpose of the present invention is to overcome the deficiency of prior art, provides a kind of cobalt oxide powder grain graininess moderate, and after sneaking into the electronic ceramics presoma, the used in electronic industry cobalt oxide ultrafine powder that electronic component performance is improved.
A further object of the present invention provides a kind of simple preparation method of used in electronic industry cobalt oxide ultrafine powder.
The high-purity cobalt oxide ultrafine powder of used in electronic industry of the present invention outward appearance is a black powder, and thing is α-Co mutually
3O
4, cobalt contents is 70～73%, d
50=0.1～1 μ m, loose density 0.2-0.5g/cm
3
The preparation method of used in electronic industry cobalt oxide ultrafine powder of the present invention may further comprise the steps:
(1). the cobalt salt solution preparation:
Nitric acid added in the highly purified cobalt metal make cobalt nitrate solution, the cobalt contents in the solution is controlled at 100～300g/L, and free acid is controlled at below the 10g/L;
(2). the ammonium bicarbonate soln preparation:
With the bicarbonate of ammonia deionized water dissolving, be mixed with the solution that concentration is 10～25wt%;
(3). liquid phase is synthetic:
At normal temperatures, the ammonium bicarbonate soln of step (2) preparation is joined in the reactor that has agitator and thermometer, control stirring velocity 50～200rpm, by spinner-type flowmeter control feed rate, the cobalt nitrate solution of step (1) was joined in the ammonium bicarbonate soln in 3 minutes～5 hours, the ammonium weight of cobalt that control adds compares in 2.8～4.0 scope, 40～80 ℃ of synthesis temperatures;
(4). filtration washing:
The carbonic acid that step (3) reaction is generated bores dope filtration, and with hot deionized water wash for several times;
(5). roasting is decomposed:
Directly that step (4) washing is good cobaltous carbonate is put into stoving oven, and 300～500 ℃ of roastings 3～20 hours, roasting process need not logical oxygen and fragmentation, just can obtain the submicron order cobalt oxide powder of black, d
50=0.1～1 μ m.
The submicron order cobalt oxide powder that the inventive method is prepared, thing are α-Co mutually
3O
4, cobalt contents is 70～73%, the purity height, and foreign matter content is few, and the specific surface area height meets the requirement of electronic-grade powder body material.And, by control precipitation synthetic processing parameter, can prepare the cobalt oxide powder of different-grain diameter, satisfy the demand of variant production.
The characteristics of the inventive method are the cobalt nitrate solutions that adopts the nitric acid dissolve cobalt metal to obtain, and control certain speed and add in bicarbonate of ammonia, utilize the hot accelerate dissolution of self-formed from reaction, and dissolution rate is short, and the residual acid content of target solution is extremely low, the dissolution process stable and controllable; Produce the submicron order cobalt oxide powder, its d through operations such as precipitation, filtration, washing, roastings
50=0.1～1 μ m, even particle distribution.This method not only technology is simple, and prepared product is the high-quality dopant material of electronic component, and the performance of electronic component is improved obviously.
The present invention compared with prior art has following advantage:
1. preparation flow novelty; Method is simple, is easy to industrial application and promotes;
2. dissolved cobalt sheet mode uniqueness adds nitric acid in the cobalt sheet that is dipped in water, does not have residual acid, and the dissolution process stable and controllable;
3. need not fragmentation, can be easy to make not conglomeration, favorable dispersity, d
50The submicron cobalt oxide of=0.1～1 μ m;
4. the precipitation building-up process is by controlling reinforced flow velocity Xiao Suangu to be added in ammonium bicarbonate soln, the content that can control cobalt in the tail washings is in very low scope (general 10～20ppm), control precipitation cobaltous carbonate reunion attitude pattern, cobalt utilization ratio higher (can reach 99.8%) with this;
5. change by the liquid phase synthesis condition, can prepare different-shape, d
50The cobalt carbonate particle of=0.1～1 μ m granularity;
6. it is simple than villaumite method washing process to adopt nitrate process to prepare cobalt oxide powder, has also avoided influencing the chlorion of electronic component electrical property;
7. adopt synthetic submicron order cobalt oxide powder of the present invention, the purity height, foreign matter content is few, and the specific surface area height meets the requirement of electronic-grade powder body material, and purposes is wide, and remarkable economic efficiency and social benefit are arranged.
Description of drawings
Fig. 1. the process flow diagram of the inventive method.
Embodiment
Embodiment 1:
Highly purified electrolytic metal cobalt joined in the chemical pure salpeter solution dissolve, the cobalt contents in the solution is 195 grams per liters, free acid 1.0 grams per liters, and foreign matter content is less than 100ppm; With hot deionized water dissolving food grade bicarbonate of ammonia, temperature is 30 ℃, and strength of solution is 185 grams per liters; Ammonium bicarbonate soln is stirred and heated to 50 ℃, under the stirring of 105rpm, the flow velocity of cobalt nitrate solution with 2L/ minute is joined in the reactor that fills bicarbonate of ammonia; Ammonium weight of cobalt ratio is 2.8; Reinforced finishing continues to stir 65 minutes; With the cobaltous carbonate sedimentation and filtration and with twice of 80 ℃ of deionized water wash; The cobaltous carbonate that washing is good was put into stoving oven, 400 ℃ of roastings 5 hours; Obtain the submicron cobalt oxide powder after sieving, be applicable to the dopant material of electronic components such as thunder arrester, thermistor, voltage dependent resistor, picture tube glass bulb.Performance index such as table 1.
Table 1
| Name of product | Outward appearance | Sedimentation D 50 | Co％ | Ni％ | Si％ | Ca％ | Na％ |
| The electronic-grade cobalt oxide | Black powder | 0.6μm | 71.5 | 0.004 | ＜0.005 | ＜0.005 | 0.01 |
| Loose density | The thing phase | Fe％ | Al％ | Mg％ | K％ | Cu％ | SO 4 2-％ |
| 0.304g/cm 3 | α-Co 3O 4 | 0.002 | 0.005 | 0.003 | ＜0.001 | 0.001 | 0.011 |
Embodiment 2:
Highly purified electrolytic metal cobalt joined in the chemical pure salpeter solution dissolve, the cobalt contents in the solution is 175 grams per liters, free acid 1.0 grams per liters, and foreign matter content is less than 100ppm; With hot deionized water dissolving food grade bicarbonate of ammonia, temperature is 30 ℃, and strength of solution is 185 grams per liters; Ammonium bicarbonate soln is stirred and heated to 40 ℃, under the stirring of 105rpm, the flow velocity of cobalt nitrate solution with 2L/ minute is joined in the reactor that fills bicarbonate of ammonia; Ammonium weight of cobalt ratio is 3.8; Reinforced finishing continues to stir 50 minutes; The cobaltous carbonate sedimentation and filtration is also used twice of deionized water wash; The cobaltous carbonate that washing is good was put into stoving oven, 400 ℃ of roastings 5 hours; Obtain the submicron cobalt oxide powder after sieving, be applicable to the dopant material of electronic components such as thunder arrester, thermistor, voltage dependent resistor, picture tube glass bulb.Performance index such as table 2.
Table 2
| Name of product | Outward appearance | Sedimentation D 50 | Co％ | Ni％ | Si％ | Ca％ | Na％ |
| The electronic-grade cobalt oxide | Black powder | 0.5μm | 71.36 | 0.0016 | ＜0.005 | ＜0.005 | 0.008 |
| Loose density | The thing phase | Fe％ | Al％ | Mg％ | K％ | Cu％ | SO 4 2-％ |
| 0.30g/cm 3 | α-Co 3O 4 | 0.012 | 0.005 | 0.005 | ＜0.001 | 0.005 | 0.01 |
Embodiment 3:
Highly purified electrolytic metal cobalt joined in the chemical pure salpeter solution dissolve, the cobalt contents in the solution is 150 grams per liters, free acid 1.0 grams per liters, and foreign matter content is less than 100ppm; With hot deionized water dissolving food grade bicarbonate of ammonia, temperature is 30 ℃, and strength of solution is 185 grams per liters; Ammonium bicarbonate soln is stirred and heated to 40 ℃, under the stirring of 105rpm, the flow velocity of cobalt nitrate solution with 2L/ minute is joined in the reactor that fills bicarbonate of ammonia; Ammonium weight of cobalt ratio is 3.8; Reinforced finishing continues to stir 30 minutes; Carbonic acid is bored sedimentation and filtration and uses twice of deionized water wash; The cobaltous carbonate that washing is good was put into stoving oven, 400 ℃ of roastings 5 hours; Obtain the submicron cobalt oxide powder after sieving, be applicable to the dopant material of electronic components such as thunder arrester, thermistor, voltage dependent resistor, picture tube glass bulb.Performance index such as table 3.
Table 3
| Name of product | Outward appearance | Sedimentation D 50 | Co％ | Ni％ | Si％ | Ca％ | Na％ |
| The electronic-grade cobalt oxide | Black powder | 0.4μm | 71.03 | 0.02 | ＜0.001 | 0.003 | 0.008 |
| Loose density | The thing phase | Fe％ | Al％ | Mg％ | K％ | Cu％ | SO 4 2-％ |
| 0.324g/cm 3 | α-Co 3O 4 | 0.0018 | 0.0014 | 0.0007 | ＜0.001 | 0.0009 | 0.0087 |
Claims (6)
1. the preparation method of a cobalt oxide ultrafine powder, it is characterized in that: described method may further comprise the steps:
(1). the cobalt salt solution preparation:
Nitric acid added make cobalt nitrate solution in the cobalt metal, the cobalt contents in the solution is controlled at 100～300g/L, and free acid is controlled at below the 10g/L;
(2). the ammonium bicarbonate soln preparation:
With the bicarbonate of ammonia water dissolution;
(3). liquid phase is synthetic:
The ammonium bicarbonate soln of step (2) preparation is joined in the reactor, stir, the cobalt nitrate solution of step (1) is joined in the ammonium bicarbonate soln, the ammonium weight of cobalt that control adds is than in 2.8～4.0 scope;
(4). filtration washing:
With the cobaltous carbonate dope filtration that step (3) reaction generates, washing;
(5). roasting is decomposed:
Directly the good cobaltous carbonate of step (4) washing is put into stoving oven, 300～500 ℃ of roastings, roasting process need not logical oxygen and fragmentation, gets the submicron order cobalt oxide powder.
2. the method for claim 1 is characterized in that: described cobalt oxide powder particulate d
50=0.1～1 μ m.
3. the method for claim 1, it is characterized in that: described step (3) stirring velocity is 50～200rpm.
4. the method for claim 1 is characterized in that: described step (3) cobalt nitrate solution joins that the used time is 3 minutes～5 hours in the ammonium bicarbonate soln.
5. the method for claim 1, it is characterized in that: the synthesis temperature when described step (3) cobalt nitrate solution joins in the ammonium bicarbonate soln is 40～80 ℃.
6. as claim 1,4 or 5 described methods, it is characterized in that: the concentration of described bicarbonate of ammonia is 10～25wt%.
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|---|---|---|---|
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| CN105731551B (en) * | 2014-12-09 | 2018-01-16 | 荆门市格林美新材料有限公司 | Adulterate cobalt carbonate, doped cobaltic-cobaltous oxide and preparation method thereof |
| CN111872370B (en) * | 2020-07-15 | 2022-04-26 | 深圳市惠拓电子材料有限公司 | Preparation method of NTC thermistor material with ultrafine particle size |
| CN113149084A (en) * | 2021-02-09 | 2021-07-23 | 荆门市格林美新材料有限公司 | Preparation method of superfine cobalt oxide |
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