CN1069564C - Technology for making tantalum powder - Google Patents
Technology for making tantalum powder Download PDFInfo
- Publication number
- CN1069564C CN1069564C CN98115687A CN98115687A CN1069564C CN 1069564 C CN1069564 C CN 1069564C CN 98115687 A CN98115687 A CN 98115687A CN 98115687 A CN98115687 A CN 98115687A CN 1069564 C CN1069564 C CN 1069564C
- Authority
- CN
- China
- Prior art keywords
- tantalum
- reduction
- diluent
- alkali halide
- reactor
- 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 - Fee Related
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000005516 engineering process Methods 0.000 title description 3
- 238000000034 method Methods 0.000 claims abstract description 37
- 238000006722 reduction reaction Methods 0.000 claims abstract description 36
- 150000003482 tantalum compounds Chemical class 0.000 claims abstract description 25
- 239000003085 diluting agent Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 150000004820 halides Chemical class 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 16
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000011734 sodium Substances 0.000 claims description 26
- 229910052708 sodium Inorganic materials 0.000 claims description 23
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 229910052700 potassium Inorganic materials 0.000 claims description 10
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 239000005864 Sulphur Substances 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 229910052796 boron Inorganic materials 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 235000011164 potassium chloride Nutrition 0.000 claims 1
- 239000001103 potassium chloride Substances 0.000 claims 1
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- 150000002739 metals Chemical class 0.000 abstract 2
- 235000015424 sodium Nutrition 0.000 description 21
- 239000000843 powder Substances 0.000 description 17
- 239000003990 capacitor Substances 0.000 description 16
- 239000012535 impurity Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 229910052715 tantalum Inorganic materials 0.000 description 7
- 230000000704 physical effect Effects 0.000 description 6
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 5
- 238000006073 displacement reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 238000005554 pickling Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 238000011026 diafiltration Methods 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910001338 liquidmetal Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- -1 alkali metal salts Chemical class 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention provides a method for manufacturing tantalum powder by restoring tantalum compounds by reducing metals, which is characterized in that after a portion of alkali halide as a diluting agent is heated and melted in a reaction vessel, the tantalum compounds are added to the reaction vessel and stirred; then, the reducing metals in liquid states are added to the reaction vessel to carry out a reduction reaction; at the same time with the reduction reaction, a portion of the alkali halide as the diluting agent or the mixtures of the alkali halide and the tantalum compounds are added to the reaction vessel.
Description
The present invention relates to make the method for the Ta powder used in capacitor of high-specific surface area, low impurity content with reducing metal reduction tantalum compound.
The main application of tantalum powder is to be used to manufacture tantalum capacitor.The index of weighing the tantalum capacitor quality mainly contains operating voltage, capacitance, leakage current.These parameters all are to be determined by the performance of tantalum powder and capacitor manufacture technology.Under certain operating voltage, capacitor volume is directly proportional with the specific area of capacitor anode, promptly under certain capacitor manufacture technology condition, the specific area of tantalum powder is big more, and the tantalum capacitor capacity of making is high more, that is to say, the specific area of tantalum powder is big more, and its specific volume is high more; The specific volume of tantalum powder is high more, and the capacitor volume of making certain specification is just more little, and used tantalum powder is also just few more.
The leakage current of capacitor is one of important parameter of weighing its quality, this parameter depends on the chemical purity of tantalum powder to a great extent, particularly the content of O, Fe, Ni, Cr, K and the Na in the tantalum powder is the important assurance of producing the high-quality tantalum capacitor so high-purity tantalum powder is provided.
The sodium reduction potassium floutaramite is an important method of producing the tantalum powder, particularly produces the main method of high specific capacitance tantalum powder.Since inventing with the sodium reduction potassium floutaramite, He Lier Martin produces the tantalum powder to today, existing about 40 years history, and in order to obtain the purity height, the tantalum powder that specific area is big, people have paid many effort, and this has been proposed many improving one's methods.
United States Patent (USP) 4,149, proposed in No. 876 Liquid Sodium is added to the method for producing the tantalum powder in the molten salt bath of the potassium floutaramite of fusion and diluent, this method is by inject sodium fast under lower temperature, so that temperature of charge rises, adopt big diluent ratio, force cooling, under lower temperature, carry out reduction reaction, keep stationary temperature in the grain growth phase, produce particle diameter tantalum powder carefully and uniformly thus, yet there is the lower shortcoming of specific volume in the tantalum powder that this method is produced.
United States Patent (USP) 4,684 discloses the method that a kind of sodium reduction is produced the tantalum powder in No. 399.This method is by earlier diluent being placed reactor, after external heat makes it fusing, then with the compound of tantalum for example potassium floutaramite and sodium metal join several times in the reactor continuously or semi-continuously, stir reduction and make the tantalum powder.
United States Patent (USP) 5,442 discloses a kind of method of sodium reduction of the alkali metal fluosilicate tantalates that at high temperature carries out highly diluted agent ratio in No. 978.This method is to reduce by solid sodium piece is joined in the reactor.The shortcoming of this method is that solid metallic sodium piece joins in the reactor and can not be distributed in the fuse salt equably very soon, and will realize the equipment complexity that this method needs.
In above-mentioned various sodium reduction methods, all be that whole diluents is joined in the reactor in advance, then by external heat fusing, reach reaction temperature after, begin to inject sodium and carry out reduction reaction.Because material is long heat time heating time in reactor, and in heating process, the air that evaporates, moisture and acid gas and reactor, agitator effect generation metal oxide enter and melt in the salt, and then enter in the tantalum powder when sodium reduction, cause the impurity content height of tantalum powder.
In addition, the reaction of sodium reduction potassium floutaramite is a fierce exothermic reaction, and liberated heat should shed as early as possible, just can make material keep certain temperature, makes fine grain, the tantalum powder that specific area is big.And force the method for reactor vessel cooled outer wall can cause temperature of charge inhomogeneous, and low near the temperature of charge of reactor wall, reactor center temperature of charge height.
The object of the present invention is to provide a kind of improved method of making Ta powder used in capacitor with reducing metal reduction tantalum compound.
In order to reach above-mentioned purpose of the present invention, the inventor improves existing method with reducing metal reduction tantalum compound production tantalum powder.According to the present invention, at first will be in reactor after the heat fused as the part of the alkali halide of diluent, compound with tantalum joins in the reactor again, after reaching reduction temperature, when reduce the adding reducing metal, the mixture that adds a part of alkali halide or alkali halide and tantalum compound stirs, and can make the tantalum powder of high-specific surface area, low impurity content thus.
According to the present invention, the reducing metal can be selected from least a in sodium metal, potassium or its alloy; Tantalum compound can be selected from K
2TaF
7Or Na
2TaF
7Or at least a in their mixture; Diluent can be selected at least a in alkali metal salts such as NaCl, KCl, KF or their mixture.
Accompanying drawing 1 is for implementing the reaction unit schematic diagram of the inventive method.
In accompanying drawing 1,11 for annotating the sodium mouth, and 12 are the argon gas inlet, and 13 is two temperature tubes, and 14 is electrothermal furnace, and 15 is reactor, and 16 is reaction mass, and 17 is paddle, and 18 is charge door, and 19 is exhaust outlet.
According to the present invention, first a part of diluent is joined in the reactor 15, found time by exhaust outlet 19 after sealing, Ar gas is entered from entrance 12, discharge from exhaust outlet 19, then make it fusing with heating wire 14 heating, to stirring with agitator 17 more than 800 ℃, tantalum compound is joined in the reactor 15 by charge door 18, continue to add thermal agitation, during 800～1000 ℃ of the reduction temperatures of setting to be reached, adding the liquid reduction metal makes tantalum compound be reduced into the metal tantalum powder, the mixture that adds simultaneously alkali halide diluent or alkali halide and tantalum compound, the amount of the alkali halide that adds during reduction is 10%～40% of diluent total amount, the tantalum compound that adds during reduction is 0～50% of tantalum compound total amount. In the course of reaction, measure the temperature of material with 2 thermocouples 13. According to the present invention, add the liquid reduction metal and also can hocket with the mixture that adds alkali halide or alkali halide and tantalum compound.
According to the present invention, the speed that adds the reducing metal is that 1～25kg/ divides, being preferably 1～15kg/ divides, more preferably 2～10kg/ divides, in reduction, the speed that adds the mixture of diluent or diluent and tantalum compound is that 1～30kg/ divides, and is preferably 1～20kg/ and divides, and more preferably 2～15kg/ divides.
After method reduction reaction of the present invention, can be incubated a period of time again, so that tantalum compound reduces fully, then cool to room temperature, reaction mass peeled off out from reactor and carry out fragmentation, then carry out conventional washing, pickling, diafiltration, oven dry, screening and obtain the tantalum powder, this tantalum powder is called former powder. The former powder that reduction obtains also will carry out the processing of heat groupization.
In order to improve the specific volume of tantalum powder, before sodium reduction or in the sodium reduction process or in the subsequent processes of former powder, can mix, doped chemical can be selected from the simple substance of one or more elements in phosphorus, boron, sulphur, oxygen, nitrogen, the silicon etc. or their compound.
According to the present invention, the compound of tantalum is just to join in the reactor after part diluent fusing, a part of diluent is to add when reaction is carried out, thereby has alleviated material the burn into of reactor has been improved tantalum powder purity.
According to the present invention, add the heat that solid-state diluent absorption reaction emits reaction is carried out fast.Temperature of charge uniformity in the reactor even react, also can obtain the tantalum powder of high specific volume, and tantalum powder degree is even under higher temperature.
Following example is used for the present invention is described in further detail, but the present invention is not constituted any restriction.
Embodiment 1
90 kilograms of KCl and 60 kilograms of KF are packed in the reactor 15, and sealing is found time, and with the displacement of Ar gas, is heated to 860 ℃ in Ar atmosphere then, starts agitator 17 and stirs, with 200 kilograms of K
2TaF
7Be added to the reactor 15 from charge door 19, after treating that temperature is raised to 860 ℃, the speed of sodium metal with 1.0～5.0 thousand Grams Per Minutes is joined the reactor from annotating sodium mouth 11, simultaneously 60 kilograms KCl is added to the reactor from charge door 19 with 1.5～6.0 kilograms/component velocity, make material evenly and react by agitator 17, the speed that adds sodium by control is controlled reaction temperature with the speed that adds diluent KCl, make reaction temperature be controlled at 860～970 ℃, (two electric thermo-couple temperatures differ 2 ℃ at most), reaction back insulation 2 hours, cool to room temperature then, reaction mass is peeled off out, through fragmentation, with deionized water eccysis lixiviating metal from reactor, alkali halide and soluble-salt, pickling then, remove metal impurities, diafiltration then, oven dry is sieved, obtain former powder, physical property and chemical impurity content are listed in table 1, in the table 2.Former powder through processing of routine groupization and deoxidation treatment, obtains Ta powder used in capacitor again, this tantalum powder is carried out the wet type electric property detect, and being pressed into diameter with 0.2 a gram/tantalum powder is 3.0 millimeters cylinder piece, and the density of briquet is 5.5 gram per centimeters
3, then 1450 ℃ of sintering 20 minutes, at 0.1%H
3PO
4Carry out anodic oxidation in the liquid under 80 ℃, 50V voltage kept 2 hours down, and anode block is at 10% H
3PO
4Survey capacity and loss in the solution are surveyed DC leakage current after 2 minutes applying the 35V DC voltage, and the results are shown in Table 3.
Embodiment 2
150 kilograms of KCl are packed in the reactor 15, and sealing is found time, and with the displacement of Ar gas, is heated to 860 ℃ in Ar atmosphere then, stirs and with 200 kilograms of K
2TaF
7Be added in the reactor, after treating that temperature is raised to 860 ℃, the speed of sodium metal with 1.0～5.0 thousand Grams Per Minutes is joined the reactor from advancing sodium mouth 12, simultaneously 60 kilograms NaCl is added in the reactor with the speed of 1.5～6.0 thousand Grams Per Minutes, make material evenly and react by stirring, the control reaction temperature is at 860～965 ℃, obtain former powder by embodiment 1 method, the physical property of former powder and chemical impurity content are listed in table 1, in the table 2, and carry out subsequent treatment by embodiment 1 method, obtain Ta powder used in capacitor and carry out the detection of wet type electrical property by embodiment 1, testing result is listed in the table 3.
Embodiment 3
With 120 kilograms of NaCl sealing in the reactor 10 of packing into, the back of finding time is heated to 860 ℃, then with 150 kilograms of K with the displacement of Ar gas under Ar atmosphere
2TaF
7Join in the reactor and stir, treat that temperature is raised to after 860 ℃, liquid metal sodium is joined in the reactor with 1.0～5.0 kilograms/component velocity, 40 kilograms of K
2TaF
7Divide with the speed of 2.0～8.0 thousand Grams Per Minutes with the mixed salt of 50 kilograms of NaCl and alternately to join in the reactor with sodium metal 6 times, reduction temperature is controlled between 860～970 ℃, obtain former powder by embodiment 1 method, its physical property and chemical impurity content are listed in table 1, the table 2, and carry out subsequent treatment by embodiment 1 method, obtain Ta powder used in capacitor and carry out the wet type detection by embodiment 1, the results are shown in Table 3.
Comparative example 1
Press United States Patent (USP) 4,684,399 methods are packed 150 kilograms of KCl and 60 kilograms of KF in the reactor into, are heated to 730 ℃ and make material melting, then with 200 kilograms of K
2TaF
7Divide 10 times, each 10 kilograms join in the reactor, add K at every turn
2TaF
7After, inject about 3.24 kilograms of liquid metal sodiums, reaction temperature is controlled at 750～800 ℃, be warmed up to 860 ℃ after having reacted, cool to room temperature then obtains former powder according to come out of the stove material stripping and washing pickling of embodiment 1, the physical property of former powder and chemical impurity content are listed in table 1, the table 2, and carry out subsequent treatment by embodiment 1 method, and the tantalum powder that obtains carries out electrical detection by embodiment 1, and the results are shown in Table 3.
Comparative example 2
Press United States Patent (USP) 4,149, disclosed method in 876 is with 200 kilograms of K
2TaF
7Pack in the reactor with 150 kilograms of KCl and 60Kg KF, the back of finding time is with the displacement of Ar gas, under Ar atmosphere, be raised to 900 ℃ after the heat fused, annotate sodium and make the generation reduction reaction, react and then obtain former powder, record its physical property and chemical impurity content is listed in table 1, table 2 by embodiment 1 method; And carry out subsequent treatment by embodiment 1, and obtain Ta powder used in capacitor and carry out wet type by embodiment 1 and detect, the results are shown in Table 3.
The physical property of table 1 tantalum powder
The chemical impurity content (10-6) of table 2 tantalum powder
| Sequence number | Average grain diameter μ m | Apparent density g/cm 3 | Specific area (BET) M 2/g |
| Embodiment 1 | 0.70 | 0.82 | 1.15 |
| Embodiment 2 | 0.75 | 0.79 | 1.10 |
| Embodiment 3 | 0.68 | 0.78 | 1.13 |
| Comparative example 1 | 0.86 | 0.76 | 0.98 |
| Comparative example 2 | 1.02 | 1.01 | 0.89 |
| O | Fe | Ni | Cr | Mg | K | Na | |
| Embodiment 1 | 2030 | 10 | 5 | ＜5 | ＜5 | 6 | 3 |
| Embodiment 2 | 1980 | 18 | 5 | 5 | 5 | 6 | 4 |
| Embodiment 3 | 2050 | 20 | 6 | 5 | ＜5 | 6 | 3 |
| Comparative example 1 | 2200 | 15 | 5 | ＜5 | ＜5 | 15 | 8 |
| Comparative example 2 | 2000 | 30 | 10 | 8 | ＜5 | 13 | 5 |
Annotate: wherein O, Mg, K, Na content are the data through the tantalum powder of subsequent treatment.
The electric property of table 3 tantalum powder
From the result of table 1, table 2 and table 3 as can be seen, the tantalum powder produced than prior art of the tantalum powder of producing by the present invention has lower chemical impurity content and electric property preferably.
| Agglomerate shrinkage factor (%) | Specific volume | DC leakage current | ||
| Radially | Volume | (μF.V/g) | (μA/μF.V) | |
| Embodiment 1 | 5.1 | 11.5 | 35210 | 2.8×10 -4 |
| Embodiment 2 | 5.3 | 12.3 | 34980 | 2.0×10 -4 |
| Embodiment 3 | 5.3 | 12.0 | 35610 | 2.7×10 -4 |
| Comparative example 1 | 5.8 | 13.5 | 33060 | 3.6×10 -4 |
| Comparative example 2 | 4.9 | 10.8 | 29500 | 2.9×10 -4 |
Claims (10)
1. method of making tantalum powder with reducing metal reduction tantalum compound, it is characterized in that will as the part of alkali halide of reduction diluent in reactor after heat fused, in reactor, add tantalum compound and stir, when adding liquid reduction metal carries out reduction reaction, add the mixture of a part of diluent alkali halide or alkali halide and tantalum compound then.
2. the method for claim 1, it is characterized in that when reduction reaction is carried out a part of diluent alkali halide that adds or the mixture of diluent alkali halide and tantalum compound, add in mode continuously, intermittently or alternately.
3. method as claimed in claim 1 or 2 is characterized in that said tantalum compound is selected from potassium floutaramite (K
2TaF
7) or fluorotantalic acid sodium (Na
2TaF
7) or both mixture at least a.
4. method as claimed in claim 1 or 2 is characterized in that said reducing metal is selected from least a in sodium, potassium or their alloy.
5. method as claimed in claim 1 or 2 is characterized in that said diluent is selected from least a in sodium chloride (NaCl), potassium chloride (KCl), potassium fluoride (KF) or their mixture.
6. method as claimed in claim 1 or 2 is characterized in that said reduction reaction remains in 800～1000 ℃ of scopes.
7. the method for claim 1 is characterized in that saidly when adding liquid reduction metallic reducing tantalum compound, and the amount of a part of diluent alkali halide of adding is 10%～40% for the diluent total amount.
8. the method for claim 1 is characterized in that saidly when adding liquid reduction metallic reducing tantalum compound, and the amount of the tantalum compound of adding is 0～50% of a tantalum compound total amount.
9. method as claimed in claim 1 or 2 is characterized in that before reduction reaction or/and add in reactant in the reaction and be selected from least a as adulterant in phosphorus, boron, nitrogen, oxygen, sulphur, the silicon.
10. method as claimed in claim 9, it is at least a to it is characterized in that said adulterant is selected from the simple substance of phosphorus, boron, nitrogen, oxygen, sulphur, silicon or their compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115687A CN1069564C (en) | 1998-07-07 | 1998-07-07 | Technology for making tantalum powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98115687A CN1069564C (en) | 1998-07-07 | 1998-07-07 | Technology for making tantalum powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1240688A CN1240688A (en) | 2000-01-12 |
| CN1069564C true CN1069564C (en) | 2001-08-15 |
Family
ID=5224678
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98115687A Expired - Fee Related CN1069564C (en) | 1998-07-07 | 1998-07-07 | Technology for making tantalum powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1069564C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124060B (en) * | 2004-12-09 | 2011-08-03 | H.C.斯塔克股份公司 | Preparation of valve metal powder |
| WO2025260224A1 (en) | 2024-06-18 | 2025-12-26 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder by reduction of potassium fluorotantalate with sodium, and produced tantalum powder |
| WO2025260240A1 (en) | 2024-06-18 | 2025-12-26 | 宁夏东方钽业股份有限公司 | Potassium fluotantalate powder, method for reducing same with sodium to produce tantalum powder, tantalum powder obtained thereby, and use thereof |
Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1169643C (en) * | 2001-09-29 | 2004-10-06 | 宁夏东方钽业股份有限公司 | Preparation method of high specific surface area tantalum powder and/or niobium powder |
| DE60329388D1 (en) * | 2002-06-13 | 2009-11-05 | Found Promotion Ind Science | METHOD FOR PRODUCING METAL POWDER AND MANUFACTURED RAW MATERIAL PRODUCT FOR METAL |
| DE102004049040B4 (en) * | 2004-10-08 | 2008-11-27 | H.C. Starck Gmbh | Process for the preparation of solid electrolytic capacitors |
| 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 |
| CN102382993B (en) * | 2011-10-09 | 2013-08-28 | 广东致远新材料有限公司 | Preparation method of target-grade ultrahigh-purity tantalum metal |
| 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 |
| WO2015096048A1 (en) | 2013-12-25 | 2015-07-02 | 宁夏东方钽业股份有限公司 | Capacitor grade high specific volume tantalum powder improving electrical performance and preparation method therefor |
| CN104406408B (en) * | 2014-09-26 | 2016-09-07 | 江苏华东锂电技术研究院有限公司 | Powder sintering device |
| CN104801725B (en) * | 2015-05-18 | 2018-01-23 | 江门富祥电子材料有限公司 | A kind of reaction unit of sodium reduction potassium floutaramite and manufacture the method for tantalum powder with it |
| CN105855561B (en) * | 2016-04-29 | 2022-01-25 | 九江有色金属冶炼有限公司 | Preparation method of superfine/nano tantalum-tungsten composite powder and superfine/nano tantalum-tungsten composite powder prepared by same |
| CN110315088B (en) * | 2019-08-16 | 2022-01-04 | 广东广晟稀有金属光电新材料有限公司 | Preparation method of coralline high-purity tantalum powder |
| CN111910097B (en) * | 2020-06-22 | 2021-07-16 | 江门富祥电子材料有限公司 | Preparation method of silicon-doped tantalum wire |
| 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 |
| CN115420075B (en) * | 2022-08-31 | 2023-11-28 | 中国石油大学(北京) | A small test device for sludge drying, pyrolysis and condensation recovery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4483819A (en) * | 1981-07-31 | 1984-11-20 | Hermann C. Starck Berlin | Production of highly capacitive agglomerated valve metal powder and valve metal electrodes for the production of electrolytic capacitors |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| WO1997040199A1 (en) * | 1996-04-25 | 1997-10-30 | Cabot Corporation | Method of making tantalum metal powder with controlled size distribution and products made therefrom |
-
1998
- 1998-07-07 CN CN98115687A patent/CN1069564C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4483819A (en) * | 1981-07-31 | 1984-11-20 | Hermann C. Starck Berlin | Production of highly capacitive agglomerated valve metal powder and valve metal electrodes for the production of electrolytic capacitors |
| US5442978A (en) * | 1994-05-19 | 1995-08-22 | H. C. Starck, Inc. | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions |
| WO1997040199A1 (en) * | 1996-04-25 | 1997-10-30 | Cabot Corporation | Method of making tantalum metal powder with controlled size distribution and products made therefrom |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101124060B (en) * | 2004-12-09 | 2011-08-03 | H.C.斯塔克股份公司 | Preparation of valve metal powder |
| WO2025260224A1 (en) | 2024-06-18 | 2025-12-26 | 宁夏东方钽业股份有限公司 | Method for producing tantalum powder by reduction of potassium fluorotantalate with sodium, and produced tantalum powder |
| WO2025260240A1 (en) | 2024-06-18 | 2025-12-26 | 宁夏东方钽业股份有限公司 | Potassium fluotantalate powder, method for reducing same with sodium to produce tantalum powder, tantalum powder obtained thereby, and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1240688A (en) | 2000-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1069564C (en) | Technology for making tantalum powder | |
| US5442978A (en) | Tantalum production via a reduction of K2TAF7, with diluent salt, with reducing agent provided in a fast series of slug additions | |
| JP4756825B2 (en) | Method for producing high specific surface area tantalum and / or niobium powders | |
| JP4215911B2 (en) | Niobium powder agglomerates | |
| US5234491A (en) | Method of producing high surface area, low metal impurity | |
| EP3414035B1 (en) | Method of deoxygenating titanium or titanium alloy having oxygen dissolved therein in a solid solution | |
| JPS5835564B2 (en) | Method for producing metal powders of the group consisting of tantalum and niobium powders | |
| KR100449820B1 (en) | The continuous metal powder fabric apparatus with a screw | |
| RU2089350C1 (en) | Method of production of tantalum powder | |
| RU2431546C2 (en) | Method of reduction | |
| WO2004042095A1 (en) | A process for the production of niobium and/or tantalum powder with large surface area | |
| JPS5873708A (en) | Manufacturing method of tantalum powder | |
| Tang et al. | Preparation of titanium by electrochemical reduction of titanium dioxide powder in molten SrCl2–KCl | |
| CN108546964B (en) | Preparation device and preparation method of metallic titanium | |
| RU2284248C1 (en) | Valve metal powder production method | |
| JP2688452B2 (en) | Method for producing tantalum powder with high surface area and low metal impurities | |
| JP6077274B2 (en) | Nitrogen-containing tantalum powder and method for producing the same | |
| JP2926280B2 (en) | Rare earth-iron alloy production method | |
| RU2401874C2 (en) | Procedure by volkov for production of chemically active metals and device for implementation of this procedure | |
| Yoon et al. | The preparation of tantalum powder using a MR-EMR combination process | |
| CN118946421B (en) | Method for producing tantalum powder by reducing potassium fluorotantalate with sodium and the tantalum powder obtained | |
| RU2409450C1 (en) | Method of producing barrier metal powder | |
| JPS63118089A (en) | Manufacturing method of titanium and titanium alloys | |
| JPS5824495B2 (en) | Manufacturing method of heat-resistant conductive aluminum alloy | |
| EP4249644A1 (en) | Reduction method and system for high-melting-point metal oxide, using fluoride-based electrolytes |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Owner name: DONGFANG TANTALUM INDUSTRY CO. LTD., NINGXIA Free format text: FORMER OWNER: NINGXIA NON-FERROUS METAL SMELTERY;NINGXIA NON-FERROUS METALS SMELTERY Effective date: 20100804 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 753000 MAILBOX 105, SHIZUISHAN CITY, NINGXIAHUI AUTONOMOUS REGION TO: 753000 NO.119, YEJIN ROAD, DAWUKOU DISTRICT, SHIZUISHAN CITY, NINGXIA |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20100804 Address after: 753000 No. 119 metallurgical Road, Dawukou District, Ningxia, Shizuishan Patentee after: Dongfang Tantalum Industry Co., Ltd., Ningxia Address before: 753000 the Ningxia Hui Autonomous Region Shizuishan City P.O. Box 105 Patentee before: Ningxia Non-ferrous Metals Smeltery |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20010815 Termination date: 20150707 |
|
| EXPY | Termination of patent right or utility model |