CN1382548A - Process for preparing Nb and/or Ta powder - Google Patents
Process for preparing Nb and/or Ta powder Download PDFInfo
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- CN1382548A CN1382548A CN 02108392 CN02108392A CN1382548A CN 1382548 A CN1382548 A CN 1382548A CN 02108392 CN02108392 CN 02108392 CN 02108392 A CN02108392 A CN 02108392A CN 1382548 A CN1382548 A CN 1382548A
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Abstract
A process for preparing Nb and/or Ta powder features that under the action of reducer chosen from alkali metal plus at least one of the halides of Mg, Ca, Sr, Ba, Li and Ce, the alkali-metal fluonidobium and/or tantalate is reduced at 300-1050 deg.C to obtain said products. Its advantages are high recovery rate for reduction, and large specific surface area, high porosity and low oxygen content of product.
Description
Technical field
The present invention relates to the production method of niobium and/or tantalum powder.
Background technology
The niobium that is called as valve metal has similar character with tantalum, can be used for making the anode of electrolytic condenser, promptly imbed compression moulding in niobium powder or the tantalum powder with niobium silk or tantalum wire, sinter porous sintered body into, then in electrolyte solution, carry out anodic oxidation, form dielectric oxide film in porous sintered surface, on oxide film, form Manganse Dioxide or electroconductibility organic polymer solid electrolyte more in turn, form carbon-coating, silver layer negative electrode as electrical condenser, pick out anode terminal and cathode terminal, carry out resin-encapsulate then, obtain niobium/tantalum solid electrolytic capacitor.
As the niobium powder or the tantalum powder of electrolytic condenser sintered compact, the niobium powder that requirement is reunited or the foreign matter content of tantalum powder are low, and specific surface area is big, and porosity is big.
In the existing technology, the tantalum powder of producing with basic metal reduction tantalum potassium fluoride is general adopted method.The tantalum powder that this method is produced is the coacervate granulometric composition that is made of many primary particals, and this tantalum powder particles internal porosity is big, is particularly suitable for making electrolytic condenser.This method has multiple improved form, is exemplified below:
United States Patent (USP) 4,149,876th is made thinner with alkali metal halide, stirs reduction K at 760 ℃～1000 ℃
2TaF
7And control annotates sodium speed, forces cooling reactor and obtains the tantalum powder.
United States Patent (USP) 4,684,399 also is to adopt alkali metal halide to make thinner, under 600 ℃～950 ℃ stirring condition, with K
2TaF
7Gradation joins and annotates sodium reduction in the reactor.
World patent WO 91/18,121st, a kind of method of the sodium reduction tantalum potassium fluoride that has improved is in the sodium reduction process, adds a spot of promoting agent before heating up in reactor, obtains high-specific surface area, the tantalum powder of low impurity content.
United States Patent (USP) 5,442,978 also is the method for the sodium reduction tantalum potassium fluoride that improved of another kind, (NaCl) makes thinner with sodium-chlor, add the speed of solid metal sodium with control, and, temperature of reaction is controlled at 950 ℃～1100 ℃ scope by cooling off, obtain high specific volume, the tantalum powder of low leakage current.
The above-mentioned method of utilizing basic metal reduction tantalum potassium fluoride in order to obtain thin metal-powder, all adopts alkali metal halide (as NaCl, KCl, KF etc.) as thinner.
In theory, use the same method, can reduce potassium niobate fluoride (K with basic metal
2NbF
7) produce the niobium powder, yet, owing to when producing potassium niobate fluoride, often be difficult to obtain purified potassium niobate fluoride, but obtain containing the potassium fluooxycolumbate (K of niobium oxides
2NbOF
5) and the mixture of potassium niobate fluoride.Also have, as everyone knows, basic metal can not the reduction-oxidation tantalum, niobium oxides, therefore, the tantalum potassium fluoride that contains the potassium niobate fluoride of niobium oxides and/or contain tantalum oxide with basic metal reduction can not obtain purified niobium powder and/or tantalum powder, and will cause the loss of noble metal tantalum, niobium.
In addition, adopt the reaction vessel and the agitator of nickel-bass alloy material, during with basic metal reduction potassium niobate fluoride, can cause pollution to the niobium powder, so, up to now, also not in the industrial precedent of utilizing basic metal reduction potassium niobate fluoride to produce the success of capacitor grade niobium powder.
Summary of the invention
In order to address the above problem, the invention discloses the production method of a kind of niobium and/or tantalum powder.
The inventive method is alkali metal fluosilicate niobium and/or the tantalate that contains oxide compound with the halogenide reduction of basic metal and at least a Mg of being selected from, Ca, Sr, Ba, Li, Ce, fluorochemical and the oxide compound and produce the method for metal niobium and/or tantalum powder wherein of reduction simultaneously.
The purpose of this invention is to provide the niobium of the reunion that a kind of impurity content is low, specific surface area is big, porosity is big and/or the preparation method of tantalum metal powder, this method is to have in the presence of the thinner of alkali metal halide, alkali metal fluosilicate niobium and/or tantalate that reduction contains oxide compound carry out, and wherein reduction reaction is that halogenide and described alkali metal fluosilicate niobium and/or the tantalate that contains oxide compound of basic metal and at least a Mg of being selected from, Ca, Sr, Ba, Li, Ce are reacted.
The alkali metal fluosilicate niobium that contains oxide compound and/or the tantalate that can use in the present invention can be the tantalum potassium fluoride (K that contains niobium oxides and/or tantalum oxide
2TaF
7), fluorotantalic acid sodium (Na
2TaF
7), potassium niobate fluoride (K
2NbF
7) and fluorine sodium columbate (Na
2NbF
7), as potassium fluooxycolumbate (K
2NbOF
5); The morphological structure of optional oxide compound and alkali metal fluosilicate niobium and/or tantalate and both ratios.
Present invention resides in and use at least a alkali metal halide to make thinner in the reduction reaction, described alkali metal halide is sodium-chlor, Repone K, Potassium monofluoride and Sodium Fluoride for example.
Make reductive agent with basic metal in the inventive method, the preferred sodium of basic metal, potassium, lithium, more preferably sodium or potassium.Alkali-metal consumption be generally reduction contain the alkali metal fluosilicate niobium of oxide compound and/or tantalate institute must stoichiometric 1.0～1.3 times.
And the halogenide of described at least a Mg, Ca, Sr, Ba, Li, Ce in reduction reaction both as the indirect reduction agent as thinner, its consumption is generally reduction and contains in the alkali metal fluosilicate niobium of oxide compound and/or the tantalate required stoichiometric 0.5～8 times of oxide compound.The metal halide of Mg, Ca, Sr, Ba, Li, Ce, the more preferably halogenide of Mg, Ca is as calcium chloride, magnesium chloride.
According to the present invention, reducing agents places the reaction vessel of the sealing of band stirring arm to carry out; The reactor parts that contacts with material is refractory alloy or coats refractory alloy.
In order to prevent local superheating, obtain even-grained tantalum powder or niobium powder, can adopt existing various stirring means, the thermal energy dissipation that reaction is emitted is opened, and makes the melt temperature in the reactor even.
According to a kind of concrete scheme of the present invention, described method comprises the halogenide of at least a Mg of being selected from, Ca, Sr, Ba, Li, Ce and described alkali metal fluosilicate niobium and/or the tantalate that contains oxide compound, and optional at least a described alkali metal halide is packed in the reactor of sealing, reactor heating is so that form melting salt therein, be metered into liquid alkali metal then, the temperature of control reaction vessel makes the alkali metal fluosilicate niobium and/or the tantalate that contain oxide compound be reduced to metal niobium and/or tantalum powder.
Reduction reaction is generally carried out at 300～1050 ℃ in the inventive method, preferably carries out under 600～1000 ℃.For reduction reaction is fully carried out, reactant preferably kept 10～300 minutes down at 600～1000 ℃.
In the methods of the invention, reduction reaction is to carry out in inert atmosphere such as argon gas and/or nitrogen.After having reacted, reduzate is cooled to room temperature, with the reaction product of condensation according to the usual method fragmentation, with deionized water and inorganic acid solution washing, remove unnecessary basic metal, alkaline-earth metal, alkali metal halide, Mg, Ca, Sr, Ba, Li, Ce metal halide and oxide compound are separated the niobium and/or the tantalum metal powder of reuniting, and are washed till neutrality with deionized water at last.The above-mentioned niobium that obtains and/or tantalum metal powder are obtained reducing former powder according to the usual method oven dry.
According to the former powder of the metal-powder of niobium after the reduction provided by the invention and/or tantalum, be a kind of by the molecular porous agglomerating particles of bioblast.
In order to be used to make capacitor anode, the above-mentioned niobium of former powder and/or the metal-powder of tantalum of being referred to as also can mix, refining treatment such as deoxidation, heat groupization, and further the group changes into bigger particle.
According to the present invention, refining treatment such as heat groupization, deoxidation can adopt prior art to carry out.
According to the niobium of the inventive method preparation and/or the metal-powder of tantalum is a kind of by the molecular porous agglomerating particles of bioblast, and the BET specific surface area of the former powder of tantalum powder is preferably 0.5～20m
2/ g, the BET specific surface area of the former powder of niobium powder is preferably 0.8～30m
2/ g.
According to the metal-powder of the inventive method production niobium and/or tantalum, niobium, tantalum metal recovery rate are not less than 80%, and preferred embodiment is not less than 90%.
The oxygen level of niobium metal groupization powder provided by the present invention is different because its specific surface area is different, preferably in 3000～25000ppm scope.
The oxygen level of tantalum metal groupization powder provided by the present invention is different because its specific surface area is different, preferably in 2000～15000ppm scope.
Fe, Ni, the Cr content of impurities of niobium metal groupization powder provided by the present invention are lower than 150ppm, preferably are lower than 100ppm.
Fe, Ni, the Cr content of impurities of tantalum metal groupization powder provided by the present invention are lower than 100ppm, preferably are lower than 50ppm.
The porosity of the metal groupization powder of niobium provided by the present invention and/or tantalum is 80%～95%.
Description of drawings
Accompanying drawing 1 is the microcosmic stereoscan photograph of the reduction niobium powder (former powder) that provided according to the embodiment of the invention 1.
Accompanying drawing 2 is microcosmic stereoscan photographs of group's niobium powder particles of being provided according to the embodiment of the invention 1.
Accompanying drawing 3 is the graph of pore diameter distribution according to the reduction niobium powder (former powder) of the embodiment of the invention 1.
Accompanying drawing 4 is that to be pressed into density be 3.0g/cm to the group's niobium powder according to the embodiment of the invention 1
3, the graph of pore diameter distribution of the niobium sintered body that 1250 ℃ of sintering obtained in 20 minutes.
Embodiment
In order to further specify the present invention, below in conjunction with drawings and Examples the preferred embodiment of the present invention is described, can find out purpose of the present invention, feature and advantage significantly.But these are described just in order to further specify the features and advantages of the present invention, rather than limitation of the present invention.
The loose density of disclosed powder (SBD) is tested according to the method for CNS GB5060-85 regulation and is obtained in this specification sheets.The median size of disclosed powder (FSSS) is tested according to the method for CNS GB 3249-82 regulation and is obtained in this specification sheets.The ASAP2021 type specific surface determinator that the BET specific surface area of disclosed powder is to use Micro Meritics company to produce in this specification sheets is measured with the BET method.
The pore size distribution of the sintered compact that the niobium powder is made among the present invention is to analyze with the Autopore III pore size distribution instrument that U.S. Micro Meritics company goes out.The Micro-Structure Analysis of niobium powder of the present invention is carried out with NEC JSM-5600LV rough vacuum scanning electronic microscope.
The niobium and/or the tantalum metal powder that are provided by method of the present invention are the porous metal powders of a change, are suitable for being used for making electrolytic condenser.
In order to test the niobium that method of the present invention produces and/or the electric property of tantalum metal powder, make the electric property that capacitor anode is checked powder according to following method.
For the niobium powder, with every 100mg niobium powder, being pressed into density is 2.5～3.0g/cm
3, diameter is the briquet of 3.0mm, in vacuum oven, 1200 ℃ of sintering 20 minutes, again with agglomerate at 80 ℃, in 0.1% the phosphoric acid solution, apply the voltage of 30V, form the niobium anode, the anodic specific capacitance is higher than 60000 μ FV/g, its leakage current is less than 5nA/ μ FV.
For the tantalum powder, with every 150mg tantalum powder, being pressed into density is 4.5g/cm
3, diameter is the briquet of 3.0mm, in vacuum oven, 1300 ℃ of sintering 20 minutes, again with agglomerate at 60 ℃, in 0.1% the phosphoric acid solution, apply the voltage of 50V, form tantalum anode, the anodic specific capacitance is higher than 20000 μ FV/g, its leakage current is less than 5nA/ μ FV.
Embodiment 1
15 kilograms of potassium fluooxycolumbates (are contained 1.02 kilograms of Nb
2O
5) niobium raw material, with 25 kilograms of NaCl, 15 kilograms KCl, 12 kilograms of CaCl
2The inside that is incorporated with the airtight band stirring arm of rare gas element import and export serves as a contrast in the reaction vessel of refractory alloy material, under argon gas atmosphere, be heated to 700 ℃, inject liquid metal sodium 6500 grams, make it that reduction reaction take place, heat up then, to 800 ℃ of insulations 1 hour, behind the cool to room temperature reaction mass is peeled off out, through drying after washing, the pickling, obtain niobium powder 4107 grams, the BET specific surface area of former powder is 6.56m
2/ g, the oxygen level of the former powder of niobium powder is 9800ppm.Accompanying drawing 1 is the microtexture stereoscan photograph of this niobium powder, and as can be seen, the niobium powder particles is by the molecular porous of many bioblasts, coacervate that specific surface area is big.Use Autopore III pore size distribution instrument to analyze the porosity and the pore size distribution of above-mentioned reduction niobium powder (former powder), porosity is 93.70%, and pore size distribution is seen accompanying drawing 3, and as can be seen from the figure, pore size distribution has a peak value, and the peak value in aperture is about 2.2 μ m.The yield that reverts back of niobium powder sees Table 1.
The above-mentioned former powder of niobium powder that obtains is according to subsequent disposal such as existing technology doping, deoxidation, thermal treatments, the niobium powder that the group of obtaining has changed.Niobium powder ball particulate scan electromicroscopic photograph is seen accompanying drawing 2, between this group niobium powder primary partical bigger open pores is arranged.
The porosity of analyzing above-mentioned group niobium powder is 89.41%, and pore size distribution has two peak values, and a peak value is about 2.2 μ m, also has a lot of macropores, and the peak value of macropore diameter is about 10.2 μ m.
The main impurity atom content of niobium powder such as table 2, physicals are as shown in table 3.
Use above-mentioned group niobium powder to be pressed into density and be 3.0g/cm
3Briquet, the niobium sintered body that obtained in 20 minutes at 1200 ℃ of sintering, using Autopore III pore size distribution instrument to analyze its porosity is 66.24%, pore size distribution is more concentrated, the peak value in aperture is about 1 μ m.
Use above-mentioned group niobium powder to be pressed into density and be 3.0g/cm
3Briquet, the niobium sintered body that obtained in 20 minutes at 1250 ℃ of sintering, using Autopore III pore size distribution instrument to analyze its porosity is 58.99%, pore size distribution is more concentrated, the peak value in aperture is about 0.9 μ m, sees accompanying drawing 4.
Use above-mentioned group niobium powder to be pressed into density and be 3.0g/cm
3Briquet, the niobium sintered body in that 1200 ℃ of sintering obtained in 20 minutes at 80 ℃, in 0.1% the phosphoric acid solution, applies the voltage of 30V with this sintered compact, forms the niobium anode, electric property such as tables 4 such as anodic specific capacitance and leakage current.
Comparative example 1
Different with embodiment 1 is that the thinner that is added is 25 kilograms of NaCl, 20 kilograms of KCl, and the niobium raw material that is added, conversion unit and reduction process are all identical with embodiment 1.Obtain niobium powder 3710 grams, the BET specific surface area of former powder is 2.66m
2/ g, the oxygen level of the former powder of niobium powder is 26000ppm, the yield that reverts back of niobium powder sees Table 1.
The above-mentioned former powder of niobium powder that obtains according to mix with embodiment 1 identical method, deoxidation and heat group handle the niobium powder that the group of obtaining has changed.
The main impurity atom content of niobium powder such as table 2, physicals are as shown in table 3.
The electric property such as the table 4 of niobium powder.
Embodiment 2
The niobium raw material that will contain 29 kilograms of the potassium fluooxycolumbates of 1.03 kilograms of niobium oxides is with 25 kilograms of NaCl, 2 kilograms of CaCl
2, 40 kilograms of KCl inject 11750 gram liquid metal sodiums according to embodiment 1 same method at 800 ℃, other production processes are all identical with embodiment 1.Obtain niobium powder 8350 grams, the BET specific surface area of former powder is 6.41m
2/ g, the oxygen level of the former powder of niobium powder is 11000ppm.The yield that reverts back of niobium powder sees Table 1.
The above-mentioned former powder of niobium powder that obtains is according to a niobium powder that mixes with embodiment 1 identical method, deoxidation and heat groupization processing have obtained changing.
The main impurity atom content of niobium powder such as table 2, physicals are as shown in table 3.The porosity of groupization niobium powder is 88.99%.
Use above-mentioned group niobium powder to make the niobium anode according to the method for embodiment 1, electric property such as tables 4 such as anodic specific capacitance and leakage current.
Embodiment 3
To contain the tantalum raw material of 2.10 kilograms of tantalum oxide, 30 kilograms of tantalum potassium fluorides and 65 kilograms of NaCl, 20 kilograms of KCl, 8.0 kilograms of MgCl
2The inside that is incorporated with the airtight band stirring arm of rare gas element import and export serves as a contrast in the reaction vessel of refractory alloy material.Under argon gas atmosphere, be heated to 800 ℃, inject liquid metal sodium 10500 grams, make it that reduction reaction take place, heat up then, to 850 ℃ of insulations 1 hour, behind the cool to room temperature reaction mass is peeled off out, through drying after washing, the pickling, obtain tantalum powder 14094 grams, the BET specific surface area of former powder is 3.86m
2/ g, its oxygen level is 7800ppm.The yield that reverts back of tantalum powder sees Table 1.
The tantalum powder that the above-mentioned former powder of tantalum powder that obtains has obtained changing according to existing method doping, deoxidation and the processing of heat groupization.
The main impurity atom content of tantalum powder such as table 2, physicals are as shown in table 3.The porosity of pelletized tantalum powder is 89.09%.
Use above-mentioned pelletized tantalum powder according to every 150mg tantalum powder, being pressed into density is 4.5g/cm
3, diameter is the briquet of 3.0mm, in vacuum oven, 1300 ℃ of sintering 20 minutes, again with agglomerate at 60 ℃, in 0.1% the phosphoric acid solution, apply the voltage of 50V, form tantalum anode, electric property such as tables 4 such as anodic specific capacitance and leakage current.
Embodiment 4
To contain the tantalum raw material of 20 kilograms of tantalum oxide, 18 kilograms of tantalum potassium fluorides and 65 kilograms of NaCl, 20 kilograms of KCl, 38 kilograms of CaCl
2The same with embodiment 3, under argon gas atmosphere, be heated to 860 ℃, inject liquid metal sodium 16500 grams, make it that reduction reaction take place, heat up then, to 880 ℃ of insulations 1 hour, behind the cool to room temperature reaction mass is peeled off out, through drying after washing, the pickling, obtain tantalum powder 22733 grams, the BET specific surface area of former powder is 7.86m
2/ g, its oxygen level is 14800ppm.The yield that reverts back of tantalum powder sees Table 1.
The tantalum powder that the above-mentioned former powder of tantalum powder that obtains has obtained changing according to existing method doping, deoxidation and the processing of heat groupization.
The main impurity atom content of tantalum powder such as table 2, physicals are as shown in table 3.The porosity of pelletized tantalum powder is 86.05%.
Use above-mentioned pelletized tantalum powder to make tantalum anode, electric property such as tables 4 such as anodic specific capacitance and leakage current according to the method for embodiment 3.Niobium, tantalum metal powder reverts back yield among table 1 embodiment
The impurity atom content of groupization powder among table 2 embodiment
The physicals of groupization powder among table 3 embodiment
The electric property of groupization niobium powder, tantalum powder among table 4 embodiment
| Example | The theoretical yield (gram) of niobium or tantalum | Niobium or tantalum actual recovered amount (gram) | Revert back yield (%) |
| Embodiment 1 | ????4984 | ????4107 | ????82.4 |
| Comparative example 1 | ????4984 | ????3710 | ????74.4 |
| Embodiment 2 | ????9609 | ????8350 | ????86.9 |
| Embodiment 3 | ????15643 | ????14094 | ????90.1 |
| Embodiment 4 | ????24684 | ????22733 | ????92.1 |
| Experimental example | ????O | ????C | ????Fe | ????Ni | ????Cr | ????Mg | ???Ca | ????Na |
| Embodiment 1 | ????4500 | ????50 | ????50 | ????＜50 | ????＜50 | ??＜20 | ???20 | ????20 |
| Comparative example 1 | ????12400 | ????55 | ????50 | ????＜50 | ????＜50 | ??＜20 | ???20 | ????120 |
| Embodiment 2 | ????4750 | ????50 | ????50 | ????＜50 | ????＜50 | ??＜20 | ???＜20 | ????20 |
| Embodiment 3 | ????4100 | ????40 | ????15 | ????12 | ????＜5 | ??＜5 | ???＜5 | ????5 |
| Embodiment 4 | ????8200 | ????45 | ????25 | ????10 | ????＜5 | ??5 | ???5 | ????5 |
| Lot number | ????FSSS ????μm | ????SBD ????G/CC | Mobile sec/50g | Size test result (%) | ||||
| ??-60/80 | ??-80/+200 | ??-200/+325 | ??-325/+400 | ????-400 | ||||
| Embodiment 1 | ????2.9 | ????0.81 | ????18.1 | ????2.1 | ????42.5 | ????18.2 | ????13.6 | ????23.6 |
| Comparative example 1 | ????2.4 | ????0.83 | ????32.3 | ????3.1 | ????32.5 | ????15.4 | ????16.9 | ????32.1 |
| Embodiment 2 | ????2.7 | ????0.78 | ????19.2 | ????2.0 | ????41.5 | ????18.0 | ????14.2 | ????24.3 |
| Embodiment 3 | ????3.0 | ????1.62 | ????9.0 | ????1.5 | ????45.6 | ????23.5 | ????12.9 | ????16.5 |
| Embodiment 4 | ????1.2 | ????1.75 | ????11.0 | ????3.5 | ????52.5 | ????22.8 | ????12.2 | ????9.0 |
| The tantalum powder | Leakage current nA/CV | ????CV ????μFV/g | ????tgδ ????％ | Pressing block density g/cc | Sinter density g/cc |
| Embodiment 1 | ????0.61 | ????98000 | ????24.5 | ????2.8 | ????3.0 |
| Comparative example 1 | ????1.80 | ????90000 | ????31.0 | ????2.8 | ????3.1 |
| Embodiment 2 | ????0.65 | ????89000 | ????25.1 | ????2.8 | ????3.0 |
| Embodiment 3 | ????0.28 | ????92100 | ????31.2 | ????4.5 | ????4.6 |
| Embodiment 4 | ????1.40 | ????130200 | ????65.2 | ????4.5 | ????4.5 |
From the result of above embodiment and comparative example as can be seen, revert back the yield height according to what the inventive method was produced niobium powder, tantalum powder, niobium powder, the tantalum powder specific surface area produced are big, and porosity is big, and oxygen level is lower, and this method is convenient to suitability for industrialized production; Make capacitor anode with niobium powder, tantalum powder that the inventive method makes, have the advantages that open-cell porosity is big, leakage current is low, specific volume is high.
Claims (7)
1. the production method of niobium and/or tantalum powder, this method is undertaken by reduction alkali metal fluosilicate niobium and/or tantalate, wherein reduction reaction temperature is 300-1050 ℃, and the reductive agent of employing is selected from basic metal and adds the halogenide of a kind of at least Mg of being selected from, Ca, Sr, Ba, Li, Ce and described alkali metal fluosilicate niobium and/or tantalate and react.
2. the production method of niobium according to claim 1 and/or tantalum powder is characterized in that also using in the reduction reaction at least a alkali metal halide to make thinner.
3. the production method of niobium according to claim 1 and 2 and/or tantalum powder, it is characterized in that halogenide and described alkali metal fluosilicate niobium and/or tantalate with at least a Mg of being selected from, Ca, Sr, Ba, Li, Ce, pack in the sealed reaction vessel, reacting by heating container then, in reaction vessel, form molten salt bath, be metered into basic metal then, control reaction temperature is so that alkali metal fluosilicate niobium and/or tantalate are reduced to metal niobium and/or tantalum.
4. according to the production method of each described niobium and/or tantalum powder among the claim 1-3, it is characterized in that reduction reaction temperature is 600-1000 ℃.
5. according to the production method of each described niobium and/or tantalum powder among the claim 1-3, it is characterized in that, wherein basic metal is sodium, potassium or their alloy, and alkali-metal consumption contains required stoichiometric 1.0～1.3 times of the alkali metal fluosilicate niobium of oxide compound and/or tantalate for reduction.
6. according to the production method of each described niobium and/or tantalum powder among the claim 1-5, it is characterized in that alkali metal fluosilicate niobium and/or tantalate are selected from the tantalum potassium fluoride (K that contains niobium oxides and/or tantalum oxide
2TaF
7), fluorotantalic acid sodium (Na
2TaF
7), potassium niobate fluoride (K
2NbF
7) and fluorine sodium columbate (Na
2NbF
7) or their mixture.
7. according to the production method of each described niobium of claim 1-6 and/or tantalum powder, the halid consumption that it is characterized in that the wherein at least a Mg of being selected from, Ca, Sr, Ba, Li, Ce contains in the alkali metal fluosilicate niobium of oxide compound and/or the tantalate required stoichiometric 0.5～8 times of oxide compound for reduction.
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182602B (en) * | 2006-11-14 | 2010-04-14 | 宁夏东方钽业股份有限公司 | Tantalum and/or niobium powder for powder metallurgy and method of producing the same |
| CN102994780A (en) * | 2012-12-18 | 2013-03-27 | 宁夏东方钽业股份有限公司 | Method for purifying tantalum powder |
| CN103687685A (en) * | 2011-05-16 | 2014-03-26 | 波士顿电子材料有限公司 | Manufacturing and applications of metal powders and alloys |
| US9199307B2 (en) | 2009-03-05 | 2015-12-01 | Ningxia Orient Tantalum Industry Co., Ltd. | Method for preparing a tantalum powder |
| CN113500204A (en) * | 2021-07-08 | 2021-10-15 | 安徽理工大学 | Method for preparing fine niobium powder by thermal reduction of niobium chloride through calcium in calcium chloride molten salt |
| CN114192791A (en) * | 2021-12-15 | 2022-03-18 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder for capacitor by adopting alkaline earth metal to reduce tantalum oxide |
| CN115570127A (en) * | 2022-10-11 | 2023-01-06 | 江门富祥电子材料有限公司 | Tantalum powder with ultrahigh specific volume and preparation method thereof |
-
2002
- 2002-03-30 CN CN 02108392 patent/CN1278804C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182602B (en) * | 2006-11-14 | 2010-04-14 | 宁夏东方钽业股份有限公司 | Tantalum and/or niobium powder for powder metallurgy and method of producing the same |
| US9199307B2 (en) | 2009-03-05 | 2015-12-01 | Ningxia Orient Tantalum Industry Co., Ltd. | Method for preparing a tantalum powder |
| CN103687685A (en) * | 2011-05-16 | 2014-03-26 | 波士顿电子材料有限公司 | Manufacturing and applications of metal powders and alloys |
| CN102994780A (en) * | 2012-12-18 | 2013-03-27 | 宁夏东方钽业股份有限公司 | Method for purifying tantalum powder |
| CN102994780B (en) * | 2012-12-18 | 2014-05-28 | 宁夏东方钽业股份有限公司 | Method for purifying tantalum powder |
| CN113500204A (en) * | 2021-07-08 | 2021-10-15 | 安徽理工大学 | Method for preparing fine niobium powder by thermal reduction of niobium chloride through calcium in calcium chloride molten salt |
| CN114192791A (en) * | 2021-12-15 | 2022-03-18 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder for capacitor by adopting alkaline earth metal to reduce tantalum oxide |
| CN114192791B (en) * | 2021-12-15 | 2023-10-24 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder for capacitor by adopting alkaline earth metal to reduce tantalum oxide |
| CN115570127A (en) * | 2022-10-11 | 2023-01-06 | 江门富祥电子材料有限公司 | Tantalum powder with ultrahigh specific volume and preparation method thereof |
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|---|---|
| CN1278804C (en) | 2006-10-11 |
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