CN1128733A - Production of hydrated tantalum and/or niobium oxide and resultant tantalates and niobates - Google Patents
Production of hydrated tantalum and/or niobium oxide and resultant tantalates and niobates Download PDFInfo
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- CN1128733A CN1128733A CN 95109143 CN95109143A CN1128733A CN 1128733 A CN1128733 A CN 1128733A CN 95109143 CN95109143 CN 95109143 CN 95109143 A CN95109143 A CN 95109143A CN 1128733 A CN1128733 A CN 1128733A
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- 229910001936 tantalum oxide Inorganic materials 0.000 title claims abstract description 20
- 229910000484 niobium oxide Inorganic materials 0.000 title claims abstract description 14
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 title claims abstract description 14
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000010955 niobium Substances 0.000 claims abstract description 19
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 16
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 3
- 230000002378 acidificating effect Effects 0.000 claims abstract description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 11
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 150000004706 metal oxides Chemical class 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 4
- 239000000463 material Substances 0.000 claims 2
- 229910000000 metal hydroxide Inorganic materials 0.000 claims 1
- 150000004692 metal hydroxides Chemical class 0.000 claims 1
- 230000001376 precipitating effect Effects 0.000 claims 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 22
- 239000000243 solution Substances 0.000 description 16
- 239000006185 dispersion Substances 0.000 description 13
- 238000001035 drying Methods 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 239000002253 acid Substances 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- XWSXTFIXZGRXSI-UHFFFAOYSA-K [OH-].[Zn+2].C([O-])([O-])=O.[Zn+2] Chemical compound [OH-].[Zn+2].C([O-])([O-])=O.[Zn+2] XWSXTFIXZGRXSI-UHFFFAOYSA-K 0.000 description 3
- PRKQVKDSMLBJBJ-UHFFFAOYSA-N ammonium carbonate Chemical class N.N.OC(O)=O PRKQVKDSMLBJBJ-UHFFFAOYSA-N 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- -1 fluorine tantalum hydroxide Chemical compound 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- SHLNMHIRQGRGOL-UHFFFAOYSA-N barium zinc Chemical compound [Zn].[Ba] SHLNMHIRQGRGOL-UHFFFAOYSA-N 0.000 description 1
- BJXXCWDIBHXWOH-UHFFFAOYSA-N barium(2+);oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Ba+2].[Ba+2].[Ba+2].[Ba+2].[Ba+2].[Ta+5].[Ta+5].[Ta+5].[Ta+5] BJXXCWDIBHXWOH-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- PSVBHJWAIYBPRO-UHFFFAOYSA-N lithium;niobium(5+);oxygen(2-) Chemical compound [Li+].[O-2].[O-2].[O-2].[Nb+5] PSVBHJWAIYBPRO-UHFFFAOYSA-N 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229960001708 magnesium carbonate Drugs 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 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
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- UKDIAJWKFXFVFG-UHFFFAOYSA-N potassium;oxido(dioxo)niobium Chemical compound [K+].[O-][Nb](=O)=O UKDIAJWKFXFVFG-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003482 tantalum compounds Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G35/00—Compounds of tantalum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
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- 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
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/11—Powder tap density
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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Abstract
Ammonia solution containing CO2 is input into acidic fluoride solution containing Ta or Nb to increase the pH of a reaction system to a value above 7 so as to prepare spherical tantalum oxide and/or niobium oxide, and/or hydrous tantalum oxide and/or hydrous niobium oxide. Metallic tantalite and/or metallic niobate are or is prepared with tantalum and/or niobium oxide or hydrous oxide.
Description
The present invention relates to production method and the thus obtained metal tantalum hydrochlorate and/or the niobate of spherical hydrated tantalum oxide and/or niobium oxides or tantalum oxide and/or niobium oxides.
Spherical tantalum oxide can pass through the organic tantalum compound of sol/gel method (Chem.Mater.1991,3, the 335-339 pages or leaves) hydrolysis and obtain.But,, also do not obtain the economic worth of any reality so far because this method is very expensive.So far there is not known precipitin reaction to produce spherical product by fluorochemical or muriate approach yet.
Being learnt by Japanese patent application 1/115820 can be by adding NH
3(NH
4)
2CO
3Mixture produce the oxyhydroxide of low fluorine content, as long as it join acidic solution in the alkaline reagents solution and keep alkaline range.The Ta that has learnt
2O
5Various crystalline forms (except the sphere) obtain by this method.These products demonstrate as unsuitable sintering and shrinkage character, therefore seldom are suitable for as raw material such as electronic ceramics component.
So main purpose of the present invention provides the production method of a kind of spherical tantalum oxide and/or niobium oxides, it does not have the described shortcoming of prior art.
Be surprisingly found out that at present when sal volatile being joined in the acidic fluoride solutions that contains tantalum and/or contain niobium and can obtain sphere, low fluorine tantalum hydroxide or Ta greater than 7 the time up to the pH of this solution value
2O
5And sphere, low fluorine niobium hydroxide or Nb
2O
5This method is a purpose of the present invention.Preferably, the unsaturated carbonate ammonium solution makes reaction be transformed into alkaline range in the thorough clearly acid metal fluoride aqueous solution thus to carry out according to precipitin reaction of the present invention from acidity by being joined.Obtain easy filtering hydrous oxide thus, they are easy to flushing, and main particle is a spheric.After being transformed into oxide compound through calcining oxyhydroxide, globosity remains unchanged.When oxyhydroxide being used for produce the derivative product with the reaction of other metal oxide or metal carbonate, globosity even still remain unchanged.Form blended oxide compound or metal tantalum hydrochlorate and/or niobate in such a way, its globosity remains unchanged.
By the CO that will discharge between the reaction period
2Be input to NH
3In the water so as it be used for next sedimentary NH
3Reaction can economic especially enforcement method of the present invention.
Tantalum oxide that obtains by method of the present invention and/or niobium oxides or hydrous oxide and tantalate and the niobate produced by their present good precipitation and filtering feature, low fluorine content, narrow particle size dispersion and have BET value＜1m
2The little powder surface of/g.
The following examples are intended to set forth the present invention, rather than by any way to its restriction.These embodiment comprise the Photomicrograph of the Fig. 1-5 that relates to various multiples as described below.Every figure has a microcosmic fiducial mark.
Embodiment 1
The unsaturated carbonate ammonium solution joined include solution (the about 120g Ta that fluoridizes tantalum
2O
5/ be 8.5 in l) until pH.With the CO that discharges between the reaction period
2Be input to 25%NH
3In the solution, be reacted into volatile salt.Sedimentary hydrous oxide is filtered and uses by known method the NH of dilution in suction filter
3The flushing of solution or water, dry and 850 ℃ of calcinings 2 hours.In the SEM Photomicrograph, the spherical main particulate diameter that exsiccant hydrated tantalum oxide and incinerating oxide compound show is about 1 μ m (Fig. 1; Following 10000 times of 20KV).
| According to SEM sphere (%) | ????????＞90 |
| Tap density (Tap density) (g/cm 3) | ????????2.2 |
| Tap density (g/ inch 3) | ????????15.8 |
| BET(m 2/g) * | ????????0.7 |
| Particle size dispersion (μ m) d90% d50% d10% | ????????2.7 ????????1.9 ????????1.3 |
| F in the oxide hydroxide (ppm) | ????????300 |
| F in the calcined oxide thing (ppm) | ????????＜5 |
*) pressing nitrogen one point method (DIN 66 131) determines
Embodiment 2
With 25%NH
3Solution joins and comprises solution (the about 120g Nb that fluoridizes niobium
2O
5/ be 6 to add the 25%NH be rich in 5% (volume) then in l) up to pH
3The unsaturated carbonate ammonium solution of solution is 9 up to pH.By the NH of known method with dilution
3Solution and water wash the hydration oxide precipitation in suction filter, dry and 850 ℃ of calcinings 2 hours.In the SEM Photomicrograph, both are about 0.1 μ m by spherical main particulate diameter.
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/cm 3) | ?????1.0 |
| Tap density (g/ inch 3) | ?????6.9 |
| BET(m 2/g) | ?????3 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????3.8 ?????1.7 ?????1 |
| F in the oxide hydroxide (ppm) | ?????550 |
Embodiment 3
With 25%NH
3Solution joins and comprises solution (the about 120g Nb that fluoridizes niobium
2O
5/ be 6 to add saturated sal volatile then in l) up to pH9 up to pH.The hydrous oxide that 2 days post crystallizations are gone out is by known method NH with dilution in suction filter
3The flushing of solution and water, dry and 850 ℃ of calcinings 2 hours.
In the SEM Photomicrograph, the spherical main particulate diameter that exsiccant hydrous oxide and incinerating oxide compound show is about 1 μ m (Fig. 2; Following 5000 times of 20KV).
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/cm 3) | ?????1.1 |
| Tap density (g/ inch 3) | ?????10.3 |
| BET(m 2/g) | ?????1.1 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????8.4 ?????5 ?????3 |
| F in the oxide hydroxide (ppm) | ?????730 |
Embodiment 4
With 25.54g Li
2CO
3(18.7%Li content) joins in the moistening hydrated tantalum oxide of 300g strainer (41.5%Ta content), then homogenizing 1 hour in mixing tank.Then with the paste mixture drying and 1000 ℃ of calcinings 2 hours.
Obtain the pure phase lithium tantalate that spherical main particle diameter is about 1 μ m.
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/cm 3) | ?????1.6 |
| Tap density (g/ inch 3) | ?????12 |
| BET(m 2/g) | ?????0.81 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????9.8 ?????5 ?????2.8 |
Embodiment 5
The hydrated tantalum oxide that the 2000g strainer is moistening (41.5%Ta content), 255.2g zinc hydroxide zinc carbonate double salt (59.8%Zn content) and 1381.4g barium carbonate are used 1500ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 2 hours at 1000 ℃.
The spherical main particle diameter of the pure phase barium tantalate zinc that obtains is about 1 μ m (Fig. 3; Following 10000 times of 20KV).
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/cm 3) | ?????2 |
| Tap density (g/ inch 3) | ?????16.5 |
| BET(m 2/g) | ?????0.33 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????9.5 ?????5.4 ?????2.6 |
Embodiment 6
With 3000g water contain tantalum oxide (74.19%Ta content) and 705.4g zinc hydroxide zinc carbonate double salt (57%Zn content) in the Thyssen-Henschel mixing tank with 3500ml water homogenizing 30 minutes.After the drying, paste mixture was calcined 2 hours down at 1000 ℃.
The spherical main particulate diameter of the pure phase tantalic acid zinc that obtains is about 1 μ m.
| According to SEM shape (%) | ??????＞90 |
| Tap density (g/cm 3) | ??????1.8 |
| Tap density (g/ inch 3) | ??????14.0 |
| BET(m 2/g) | ??????0.36 |
| Particle size dispersion (μ m) d90% d50% d10% | ??????11.0 ??????6.2 ??????3.5 |
Embodiment 7
3000g hydrated tantalum oxide (74.19%Ta content) and 850.1g salt of wormwood (56.58%K content) are used 2500ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 2 hours down at 1000 ℃.
The spherical main particle diameter of the pure phase potassium tantalate that obtains is about 1 μ m.
| According to SEM sphere (%) | ??????＞90 |
| Tap density (g/cm 3) | ??????1.9 |
| Tap density (g/ inch 3) | ??????15.9 |
| BET(m 2/g) | ??????0.31 |
| Particle size dispersion (μ m) d90% d50% d10% | ??????11.0 ??????6.8 ??????3.8 |
Embodiment 8
Aqua oxidation niobium (25%Nb content) that the 5000g strainer is moistening and 497.1g Quilonum Retard (18.8%Li content) are used 1000ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 6 hours down at 850 ℃.
The spherical main particle diameter of the pure phase Lithium niobium trioxide that obtains is about 1 μ m.
| According to SEM sphere (%) | ??????＞90 |
| Tap density (g/ inch 3) | ??????5.4 |
| BET(m 2/g) | ??????1.5 |
| Particle size dispersion (μ m) d90% d50% d10% | ??????4.2 ??????2.5 ??????1.7 |
Embodiment 9
Aqua oxidation niobium (25%Nb content) that the 5000g strainer is moistening and 929.7%g salt of wormwood (56.58%K content) are used 1000ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 6 hours down at 850 ℃.
The spherical main particle diameter of the pure phase potassium niobate that obtains is about 1 μ m.
| According to SEM sphere (%) | ??????＞90 |
| Tap density (g/ inch 3) | ??????7.0 |
| BET(m 2/g) | ??????＜2 |
| Particle size dispersion (μ m) d90% d50% d10% | ??????3.5 ??????2.0 ??????1.2 |
Embodiment 10
Aqua oxidation niobium (25%Nb content) that the 5000g strainer is moistening and 290g magnesium hydroxide magnesiumcarbonate double salt (57.5%Mg content) are used 2500ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 6 hours down at 850 ℃.
The spherical main particle diameter of the pure phase niobic acid magnesium that obtains is about 1 μ m (Fig. 4; Following 5000 times of 20KV).
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/ inch 3) | ?????6.4 |
| BET(m 2/g) | ?????5.8 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????2.0 ?????1.0 ?????0.5 |
Embodiment 11
Aqua oxidation niobium (25%Nb content) that the 2000g strainer is moistening and 743.5g nickelous carbonate cream (21.5%No content) are used 500ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 6 hours down at 850 ℃.
The spherical main particle diameter of the pure phase niobic acid nickel that obtains is about 1 μ m (Fig. 5; Following 5000 times of 20KV).
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/ inch 3) | ?????6.7 |
| BET(m 2/g) | ?????3.9 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????2.5 ?????1.3 ?????0.6 |
Embodiment 12
The aqua oxidation niobium (25%Nb content) that the 3000g strainer is moistening, 513.29 zinc hydroxide zinc carbonate double salt (54%Zn content) and 2389.6g barium carbonate (69.59%Ba content) are used 3000ml water homogenizing 30 minutes in the Thyssen-Henschel mixing tank.After the drying, paste mixture was calcined 6 hours at 850 ℃.
The spherical main particle diameter of the pure phase niobic acid barium zinc that obtains is about 1 μ m.
| According to SEM sphere (%) | ?????＞90 |
| Tap density (g/ inch 3) | ?????9.1 |
| BET(m 2/g) | ?????＜2 |
| Particle size dispersion (μ m) d90% d50% d10% | ?????4.0 ?????2.2 ?????1.4 |
Claims (7)
1. the production method of spherical hydrated tantalum oxide and/or niobium oxides or tantalum oxide and/or niobium oxides is characterized in that and will contain CO
2Ammonia solution join in the acidic fluoride solutions that contains tantalum and/or niobium up to the pH of this solution value greater than 7.
2. method as claimed in claim 1 is characterized in that the CO that will discharge between the reaction period
2Be input to NH
3In the water and and NH
3Reaction adopts such water to be used for precipitating next time.
3. by spherical hydrated tantalum oxide and/or niobium oxides or the tantalum oxide and/or the niobium oxides of the method for claim 1 or 2 preparation.
4. the production method of spherical metal tantalate and/or niobate, it is characterized in that the hydrated tantalum oxide and/or the niobium oxides of claim 3 are mixed with the material of corresponding stoichiometric number, this material is selected from by metal oxide, the group that metal hydroxides and metal carbonate are formed, wherein metal is selected from the group of being made up of tantalum and niobium, and with the mixture calcining that obtains.
5. by the spherical metal tantalate product of claim 4 method preparation.
6. by the spherical metal niobate product of claim 4 method preparation.
7. by the spherical metal tantalate/niobate product of claim 4 method preparation.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP4422761.2 | 1994-06-29 | ||
| DE19944422761 DE4422761C1 (en) | 1994-06-29 | 1994-06-29 | Process for the preparation of tantalum and / or niobium oxide hydrate and their use |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1128733A true CN1128733A (en) | 1996-08-14 |
Family
ID=6521817
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95109143 Pending CN1128733A (en) | 1994-06-29 | 1995-06-29 | Production of hydrated tantalum and/or niobium oxide and resultant tantalates and niobates |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JPH0812333A (en) |
| CN (1) | CN1128733A (en) |
| BR (1) | BR9502973A (en) |
| DE (1) | DE4422761C1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339308C (en) * | 2001-12-27 | 2007-09-26 | 三井金属鉱业株式会社 | Powder of tantalum oxide or niobium oxide, and method for production thereof |
| CN101234347B (en) * | 2008-02-29 | 2010-06-23 | 中国建筑材料科学研究总院 | Method for preparing niobate composition metal oxide nano particle |
| CN1849265B (en) * | 2003-09-12 | 2011-11-16 | H.C.施塔克股份有限公司 | Vaccum tube metal-oxide powder and method for producing said powder |
| CN105883919A (en) * | 2016-04-28 | 2016-08-24 | 宁夏东方钽业股份有限公司 | Preparation method of spherical tantalum oxide or spherical niobium oxide |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6338832B1 (en) * | 1995-10-12 | 2002-01-15 | Cabot Corporation | Process for producing niobium and tantalum compounds |
| DE10195586B4 (en) * | 2000-12-20 | 2008-08-21 | Murata Mfg. Co., Ltd., Nagaokakyo | Translucent ceramic material, process for its preparation and its use |
| JP4996016B2 (en) * | 2001-06-01 | 2012-08-08 | 三井金属鉱業株式会社 | Niobium oxide slurry, niobium oxide powder and production method thereof |
| DE102004052696A1 (en) * | 2004-10-29 | 2006-05-04 | Companhia Brasileira De Metalurgia E Mineracao | Porous niobium acid catalyst |
| JP4576532B2 (en) * | 2005-09-09 | 2010-11-10 | 独立行政法人産業技術総合研究所 | Method for producing potassium tantalate microcrystals |
| TW202342632A (en) * | 2022-04-21 | 2023-11-01 | 日商Ｄｉｃ股份有限公司 | Tantalic acid salt particles, method for producing tantalic acid salt particles, resin composition, and molded object |
| CN115093121B (en) * | 2022-07-27 | 2023-09-01 | 秦皇岛玻璃工业研究设计院有限公司 | Lithium aluminum silicon microcrystalline glass and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3428788C2 (en) * | 1983-08-11 | 1986-07-10 | Günter J. 8510 Fürth Bauer | Process for the continuous production of low-fluoride tantalum or niobium pentoxides |
-
1994
- 1994-06-29 DE DE19944422761 patent/DE4422761C1/en not_active Expired - Fee Related
-
1995
- 1995-06-28 BR BR9502973A patent/BR9502973A/en not_active Application Discontinuation
- 1995-06-28 JP JP18323095A patent/JPH0812333A/en active Pending
- 1995-06-29 CN CN 95109143 patent/CN1128733A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100339308C (en) * | 2001-12-27 | 2007-09-26 | 三井金属鉱业株式会社 | Powder of tantalum oxide or niobium oxide, and method for production thereof |
| CN1849265B (en) * | 2003-09-12 | 2011-11-16 | H.C.施塔克股份有限公司 | Vaccum tube metal-oxide powder and method for producing said powder |
| CN101234347B (en) * | 2008-02-29 | 2010-06-23 | 中国建筑材料科学研究总院 | Method for preparing niobate composition metal oxide nano particle |
| CN105883919A (en) * | 2016-04-28 | 2016-08-24 | 宁夏东方钽业股份有限公司 | Preparation method of spherical tantalum oxide or spherical niobium oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| BR9502973A (en) | 1996-03-12 |
| DE4422761C1 (en) | 1996-03-07 |
| JPH0812333A (en) | 1996-01-16 |
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