CN1035852A - Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction - Google Patents
Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction Download PDFInfo
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- CN1035852A CN1035852A CN 88105687 CN88105687A CN1035852A CN 1035852 A CN1035852 A CN 1035852A CN 88105687 CN88105687 CN 88105687 CN 88105687 A CN88105687 A CN 88105687A CN 1035852 A CN1035852 A CN 1035852A
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Abstract
Carbon reduction method is produced capacitor level high pressure, high specific volume (63 volts, 2800 microfarad volt/grams) tantalum powder, belongs to extracting field of metallurgy.The technology that the invention is characterized in employing is earlier to Ta
2O
5Two sections carbon reductions, hydraulic classification, part doping, allotment and dehydrogenation thermal treatment are carried out in high temperature sintering refining again, hydrogenation powder process then.Technological process is simple, and facility investment is few, metal yield height (93～95%), and production cost is low, remarkable in economical benefits, and good by the tantalum powder physical and chemical performance and the electrical property of output of the present invention, steady quality is used to make the yield rate height of electrical condenser.
Description
The present invention relates to the tantalum pentoxide is raw material, produces the extraction metallurgical process of capacitor level high-voltage high specific capacitance (63 volts, 2800 microfarad volt/grams) tantalum powder with the vacuum carbon reduction method.
The tantalum powder is the critical material that electronic industry is produced tantalum electrolytic capacitor.The capacitor level complete series tantalum powder of each country's production generally adopts two kinds of methods of tantalum potassium fluoride sodium Metal 99.5 reducing process and " electron beam melting-hydrogenation " technology to realize at present.Before a kind of method tantalum powder characteristics of producing be the bulking value height, but operating voltage is low, major part is 25 volts following solid electrolyte capacitators uses, small part is used for 40 volts of electrical condensers, and reductive agent-sodium cost an arm and a leg the Production Flow Chart complexity.Want to produce withstand voltage 63 volts of above Ta powder used in capacitor, also need sodium reduction tantalum powder is prepared once more through " electron beam melting-hydrogenation " technology.United States Patent (USP) 3635693, English Patent 1219748, Japan specially permit clear and 52-142615, United States Patent (USP) 4441927 have been introduced 63 volts of " electron beam melting-hydrogenation " prepared or 63 volts of above Ta powder used in capacitor respectively.This class " electron beam melting-hydrogenation " tantalum powder (also claiming so-called " bombardment tantalum powder ") operating voltage height, but metal recovery rate only is 76～86%, and required equipment costliness, complexity, the once investment of production is big.
The objective of the invention is to intend working out a kind of single carbon reduction processing method that can produce 63 volts of capacitor levels, 2800 microfarad volt/gram tantalum powder, make technical process shorter, facility investment is few, and production cost is low, the metal recovery rate height.
Principle technical process of the present invention mainly comprises eight steps as shown in drawings:
1. reduction furnace charge preparation
With GB3626-83 first grade tantalum pentoxide is raw material, and graphite is reductive agent.The granularity that requires tantalum pentoxide is less than 0.175mm, and its loose density is 0.35～0.80 gram per centimeter
3; Fixed carbon in the Graphite Powder 99 of selecting for use 〉=96.5%, moisture content≤0.18%, fugitive constituent≤3.31%, ash≤0.05%, Graphite Powder 99 size composition are that 0.037～0.062mm accounts for 85%, 0.062～0.074mm accounts for 15%, loose density 0.35～0.45 gram per centimeter
3For the product that makes production is not subjected to the influence of carbon, when batching, adopt the principle of polyoxy de-carbon, the tantalum pentoxide of allocating into will surpass stoichiometry 3～5%.In addition, material flies upward and strengthens mixed effect in order to prevent to prepare burden, and must add 1% analytical pure alcohol.Above-mentioned material mixed in blender 36～50 hours, get upper, middle and lower-ranking material sample and analyze carbon, at content difference less than 2～3% o'clock, promptly with 200～500 kilograms per centimeter
2Pressure material is pressed into density is 2.7～3.3 gram per centimeters
3Reduction base bar.
2. direct two sections carbon reductions
By the last prepared reduction base bar vacuum carbon reduction stove of packing into, electrically heated.Two sections systems are adopted in reduction.First section reduction be incubated when being warmed up to 1450～1550 ℃ of temperature to vacuum tightness be 3 * 10
-1Holder is warmed up to 1700～1800 ℃ again; Be incubated to vacuum tightness be 6 * 10
-2After the holder, having a power failure naturally cools to room temperature.Then a section of reduction material being come out of the stove is crushed to below the 0.147mm, and through 2 hours mixings, once more with 1000～3000 kilograms per centimeter
2Pressure be pressed into the base bar, keeping density is 10.0～12.8 gram per centimeters
3, second section reduction carried out in shove charge.Second section also originally was warmed up to 1800～1900 ℃, was incubated to vacuum 2 * 10
-3The holder, be raised to 1950～2000 ℃ again, be incubated to vacuum tightness be 5 * 10
-4Holder, having a power failure feeds 0.2 kilograms per centimeter when being cooled to 800 ℃
2Hydrogen and naturally cool to room temperature, control is gone back original product and is contained oxygen 1000～3000ppm, carbon containing 50～150ppm.
3. vacuum sintering refining
In order to strengthen the Combination of material, guarantee that composition is even, need to go back the broken once more mixing of original product, with 2500～4000 kilograms per centimeter
2Pressure be pressed into the base bar (weight is 1～1.3 kilogram/bar) of 14 * 14 * 400mm or 16 * 16 * 400mm.The base bar vacuum sintering stove of packing into is warmed up to 1750 ℃, be incubated to vacuum tightness be 1 * 10
-3The holder, be raised to 2050 ℃ again, be incubated to vacuum tightness be 5 * 10
-4Holder is warmed up to 2700 ℃ again again, is 5 * 10 in vacuum tightness
-5Insulation cooling after 3 hours under the condition of holder, the tantalum bar after the refining of control sintering contains oxygen 100～400ppm, carbon containing＜30ppm.
4. the vacuum sintering product is packed into and handle in the hydrogenation furnace.The tantalum bar is earlier 5 * 10
-5In 1000～1200 ℃ of insulations 2 hours, remove the gas of surface adsorption under the vacuum condition of holder,, then be cooled to 800～900 ℃, feed 1.5～2.0 kilograms per centimeter with activation tantalum bar surface
2Hydrogen.In order to guarantee that the tantalum bar has enough hydrogens, and make broken easily and powder particle be without prejudice, temperature-fall period both too soon can not be too slow, therefore cooling gradually under the situation that hydrogen is supplied with will guaranteed, and when 800 ℃, 600 ℃, 400 ℃ and 200 ℃, respectively be incubated 1 hour respectively, naturally cooling again, control hydrogenated tantal bar hydrogen content is 3000～4000ppm.Hydrogenated tantal strip adoption XZM100 type rapping machine rapping fragmentation, control rapping speed is 960 times/minute, 100～300 grams of at every turn feeding, each rapping time is 10～30 seconds, makes tantalum powder after the rapping all below 0.044mm.
5. tantalum powder pickling
The hydrogenated tantal powder is through 20% chlorohydric acid pickling 2～3 times, and 60～80 ℃ of temperature are washed till no Cl with ion exchanged water (resistivity 〉=2 megaohms)
-, and 60 ℃ of oven dry down.
6. tantalum powder classification
Tantalum powder after the rapping fragmentation carries out size classification with reverse-flow hydroclassifier, controls the flow of water in 100: 3～100: 6 with liquid-solid ratio.Graded product is divided into 14～15 μ, 10～11 μ, 7～8 μ, 5～6 μ, 4 ± 0.5 μ and six grades of 3 ± 0.5 μ by the control of Fei Shi (F.s.s.s) particle diameter, dries powder allotment fully down respectively at 60 ℃ and uses.
7. tantalum powder doping treatment and allotment
Specific volume and reduction powder sintering shrinkage when making electrical condenser in order to improve the tantalum powder will carry out the allotment of doping treatment and powder before dehydrogenation and thermal treatment.For 63 volts, 2800 microfarad volt/gram tantalum powder, need not whole the doping, as long as part is mixed phosphorus, boron.The concrete operations step of this operation is earlier 7～8 μ and 10～11 μ and three grades of 14～15 μ, 5～6 μ and three grades of 4 ± 0.5 and 3 ± 0.5 μ to be mixed respectively; Again 0.1M primary ammonium phosphate and 0.1M boric acid are added by in the tantalum powder behind 5～6 μ, 4 ± 0.5 μ, three grade mixings of 3 ± 0.5 μ with solution morphology, and, control the phosphorous 20～200ppm of this part tantalum powder, boracic 10～100ppm 60 ℃ of oven dry down; And then will mix the tantalum powder of phosphorus, boron and the tantalum powder allotment of not mixing again, controlling deployed tantalum powder Fei Shi particle diameter is 6～8 μ.Send to dehydrogenation and thermal treatment through doping treatment and deployed tantalum powder.
8. dehydrogenation of tantalum powder and thermal treatment
Dehydrogenation of tantalum powder and combined with heat treatment all adopt this equipment of vacuum tungsten coil furnace together.Negative pressure mode is adopted in dehydrogenation, and 1000 ℃ of controlled temperature to vacuum tightness is 1～5 * 10
-5Holder.For the lattice eliminated in powder surface mechanical stress and the shattering process twisted, and make fine particle form larger particles, improve powder flowbility and compactibility, use, need after dehydrogenation finishes substantially, carry out two sections condensation heats and handle to adapt to electrical condenser factory automatic production line.First section is to be warmed up to 1300～1400 ℃ immediately, is incubated 1 hour, and control vacuum tightness is less than 5 * 10
-5Holder.After first section thermal treatment tantalum powder caking come out of the stove, manually smash to pieces to 0.147mm, carry out second section condensation heat again and handle; At 1400～1500 ℃, vacuum tightness less than 5 * 10
-5Be incubated 1～2 hour under the condition of holder, having a power failure then naturally cools to room temperature.The tantalum powder product of gained is 63 volts of the finished product-capacitor levels, 2800 microfarad volt/gram tantalum powder again through being crushed to below the 0.246mm.
The present invention has following advantage compared with the prior art: (1). and technological process is simple, metal recovery rate height (yield of tantalum reaches 93～95%), non-environmental-pollution; (2). product purity height, pulverized structure by present method output are reasonable, have good physicals and electrical property, and the volt-ampere characteristic that is used to make electrical condenser is good, yield rate is high; (3). production cost is low, facility investment is few, compares with " electron beam melting-hydride process ", reduce facility investment more than 50%, total remarkable in economical benefits.
Example 1: take by weighing 32 kilograms of GB3626-83 first grade tantalum pentoxides, it is sieved, control size is below the 0.175mm, and detecting its loose density is 0.48 gram per centimeter
3The reductive agent that uses is Graphite Powder 99, contain fixed carbon 96.5%, moisture content 0.18%, fugitive constituent 3.31%, ash 0.05%, it is sieved, get the part mixing of 0.062～0.074mm15% and 0.037～0.062mm85%, recording its loose density is 0.43 gram per centimeter
3The Charge Mixture Control tantalum pentoxide surpasses stoichiometry 3.8%, and adds the analytical pure alcohol of charging weight 1%, mixes 42 hours in the rocking type blender in the lump.The furnace charge of mixing is through 300 kilograms per centimeter
2Pressure compacting slivering, density is 2.9 gram per centimeters
3Reduce in the vacuum carbon reduction stove, stove power is 50KW.A section of reduction system is 1450 ℃ and is incubated to vacuum tightness 3 * 10
-1Holder is warming up to 1750 ℃ of insulation to 6 * 10 again
-2Holder, having a power failure feeds 0.2 kilograms per centimeter when being cooled to 800 ℃
2Hydrogen, naturally cool to room temperature, last 22 hours.A section of reduction material come out of the stove to be crushed to below the 0.147mm, and (density is 10.8 gram per centimeters to mix after 2 hours once more press strip
3), and second section reduction carried out in shove charge.The reduction system is to be warming up to 1850 ℃ in 120 minutes, and insulation is to 2 * 10
-3Holder is warming up to 1950 ℃ again, and insulation is to 5 * 10
-4Holder, the cooling that has a power failure feeds 0.2 kilograms per centimeter in the time of 800 ℃
2Hydrogen, naturally cool to room temperature.The reduction furnace charge mixed 2 hours once more through being crushed to below the 0.147mm, was pressed into the base bar of 14 * 14 * 400mm, and the base rod density is 11.5 gram per centimeters
3Be warming up to 1700 ℃ in 30 minutes during the refining of base bar sintering, insulation is to 1 * 10
-3Holder; Be warming up to 2000 ℃ then, insulation is to 5 * 10
-4Holder; Be warming up to 2700 ℃ again, and 5 * 10
-5The holder vacuum degree condition under the insulation 3 hours, with all sintering tantalum bars in hydrogenation furnace through 5 * 10
-5Held in the palm 1200 ℃ of vacuum heat treatment 2 hours, and be cooled to 850 ℃ thereupon, feed purified hydrogen, keep the interior hydrogen pressure of stove in 1.5～2.0 kilograms per centimeter
2, that reduces furnace temperature and companion gradually respectively is incubated 1 hour at 800 ℃, 600 ℃, 400 ℃ and 200 ℃.Go in the rapping crusher the hydrogenated tantal of coming out of the stove is packaged, each charge amount is 250 grams, rapping 18 seconds, and all sieve, control size is below the 0.044mm, dries behind 20% salt acid elution again.Gained tantalum powder control liquid-solid ratio is through reverse-flow hydroclassifier to be divided into six grades at 100: 5, carries out doping treatment and allotment by preceding method, and a part of tantalum powder of controlled doping contains 50ppm phosphorus, 25ppm boron.Tantalum powder after the allotment is packed into and is carried out dehydrogenation and thermal treatment in the vacuum tungsten coil furnace.Batch is 6 kilograms, under vacuum condition in 1000 ℃ hydrogen removed after, improve temperature to 1350 ℃, be incubated 1 hour, vacuum tightness is 5 * 10
-5Holder.After tantalum powder caking is come out of the stove, be crushed to once more below the 0.147mm, shove charge again, at 1450 ℃, vacuum tightness less than 5 * 10
-5Insulation is 1.5 hours under the condition of holder.Come out of the stove after cooling, product is crushed to below the 0.246mm, obtain 12 kilograms 63 volts, 2800 microfarad volt/gram tantalum powder (obtaining 12.96 kilograms 63 volts, 2300 microfarad volt/gram tantalum powder simultaneously).The Chemical Composition of this tantalum powder is (ppm): O
21200, H
220, N
230, Nb30, C40, Fe20, Si20, W15, Mo10, Mn10, Al10, Ti10, Ni10, Cr10, it is qualified to send system CA and GCA type product to carry out the routine test examination by Chinese SJ1059-79 standard, and product qualified rate reaches 80.3～92.8%.
Example 2: take by weighing 40 kilograms of GB3626-83 first grade tantalum pentoxides, chemical purity and physicals are with example 1.Graphite Powder 99 is also with example 1.The control tantalum pentoxide surpasses stoichiometry 4% during batching.Subordinate phase reduction system is to be warming up to 1870 ℃ in 120 minutes, and insulation is to 2 * 10
-3Holder is warming up to 1980 ℃ again, and insulation is to 5 * 10
-4Holder.All the other conditions are with example 1.Common property goes out 15 kilograms of 63V2800 μ FV/g tantalum powder (obtaining 16.20 kilograms 63 volts, 2300 microfarad volt/gram tantalum powder simultaneously).
The chemical constitution of this tantalum powder (ppm) is: O
21250, C25, Fe22, surplus with example 1 send system CA and GCA type product qualified by the examination that makes an exception of Chinese SJ1059-79 standard, and product qualified rate reaches 82～88%.
Claims (9)
1, the method for a kind of production capacitor level high-voltage high specific capacitance (63 volts, 2800 microfarad volt/grams) tantalum powder, be to adopt " sodium reduction--electron beam melting ", the invention is characterized in and earlier tantalum pentoxide is carried out direct two sections carbon reductions, vacuum high-temperature sintering refining again, hydrogenation powder process are carried out powder hydraulic classification then, are mixed and allocate and negative dehydrogenation thermal treatment.
2, method according to claim 1 is characterized in that tantalum pentoxide adopting direct two sections carbon reduction modes to produce ta powder after batching, first section be incubated when also originally being warmed up to 1450～1550 ℃ to vacuum tightness be 3 * 10
-1The holder, be incubated when being warming up to 1700～1800 ℃ again to vacuum tightness be 6 * 10
-2Holder is crushed to reducing material below the 0.147mm after being cooled to room temperature, and press strip behind 2 hours mixings carries out second section reduction then, heat up earlier be incubated 1800～1900 ℃ the time to vacuum tightness be 2 * 10
-3The holder, be incubated when being warmed up to 1950～2000 ℃ again to vacuum tightness be 5 * 10
-4Holder, having a power failure feeds 0.2 kilograms per centimeter when being cooled to 800 ℃
2Hydrogen and naturally cool to room temperature, to go back the original product oxygen level be 1000～3000ppm in control, carbon containing 50～150ppm.
3, method according to claim 1 is characterized in that reducing material once more behind fragmentation, mixing, the press strip, be incubated when in the vacuum sintering stove, being warmed up to 1750 ℃ to vacuum tightness be 1 * 10
-3Holder, insulation is to 5 * 10 when being warmed up to 2050 ℃ again
-4Holder when being warmed up to 2700 ℃ again then, is 5 * 10 in vacuum tightness
-5Insulation cooling again in 3 hours under the condition of holder, the tantalum bar after the control refining contains oxygen 100～400ppm, and carbon containing is less than 30ppm.
4, method according to claim 1 is characterized in that the metal tantalum bar after the refining is packed into when handling in the hydrogenation furnace, is 5 * 10
-5In 1000～1200 ℃ of insulations 2 hours, feed 1.5～2.0 kilograms per centimeter when being cooled to 800～900 ℃ again under the vacuum condition of holder
2Hydrogen, and cooling gradually under the situation that keeps hydrogen to supply with respectively is incubated 1 hour at 800 ℃, 600 ℃, 400 ℃ and 200 ℃ respectively, naturally cooling thereafter, control hydrogenated tantal bar hydrogen content is 3000～4000ppm.
5, method according to claim 1, it is characterized in that the crumbling method to the hydrogenated tantal bar is the rapping fragmentation, control rapping machine rapping speed is 960 times/minute, and each charge amount is 100～300 grams, each rapping 10～30 seconds, and make tantalum powder after the rapping all below 0.044mm.
6, method according to claim 1, it is characterized in that the tantalum powder after the rapping fragmentation is carried out classification with reverse-flow hydroclassifier, control the flow of water with liquid-solid ratio 100/3～100/6, graded product is divided into 14～15 μ, 10～11 μ, 7～8 μ, 5～6 μ, 4 ± 0.5 μ and six grades of 3 ± 0.5 μ by Fei Shi (F.s.s.s) granularity.
7, method according to claim 1, the allotment tantalum powder that it is characterized in that mixing divided for three steps carried out, the first step is respectively 7～8 μ and 10～11 μ and three grades of 14～15 μ, 5～6 μ and 4 ± 0.5 μ and three grade mixings of 3 ± 0.5 μ, second step only added 0.1M primary ammonium phosphate and 0.1M boric acid solution by in the tantalum powder behind 5～6 μ, 4 ± 0.5 μ, three grade mixings of 3 ± 0.5 μ, control the phosphorous 20～200ppm of this part tantalum powder, boracic 10～100ppm, the 3rd step, controlling its Fisher particle size was 6～8 μ with the doping tantalum powder and the tantalum powder allotment of not mixing.
8, method according to claim 1 is characterized in that dehydrogenation of tantalum powder and combined with heat treatment are carried out in an equipment, its process in two steps, 1000 ℃ of the first step dehydrogenation controlled temperature are to vacuum tightness 1～5 * 10
-5After the holder, be warmed up to 1300～1400 ℃ immediately, keep vacuum tightness less than 5 * 10
-5Holder, thermal treatment 1 hour, second step for the first time thermal treatment tantalum powder caking come out of the stove and manually smash to pieces to 0.147mm, again at 1450～1550 ℃, vacuum tightness less than 5 * 10
-5Thermal treatment is 1～2 hour under the holder condition, reduces to room temperature thereafter, takes out tantalum powder cake broke to 0.246mm.
9, the preparation of reduction furnace charge according to claim 2 is characterized in that used tantalum pentoxide is the GB3626-83 first grade, and granularity is less than 0.175mm, loose density 0.35～0.80 gram per centimeter
3, the fixed carbon of Graphite Powder 99 〉=96.5%, moisture content≤0.18%, fugitive constituent≤3.31%, ash≤0.05%, Graphite Powder 99 size composition be 0.037～0.062mm account for 85%, 0.062～0.074mm account for 15%, loose specific weight 0.35～0.45 gram per centimeter
3, add 1% analytical pure alcohol during batch mixing, mixed 36～50 hours, carbon content difference is less than 2～3% in the control upper, middle and lower-ranking material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105687 CN1018736B (en) | 1988-03-18 | 1988-03-18 | Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88105687 CN1018736B (en) | 1988-03-18 | 1988-03-18 | Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction |
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| Publication Number | Publication Date |
|---|---|
| CN1035852A true CN1035852A (en) | 1989-09-27 |
| CN1018736B CN1018736B (en) | 1992-10-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88105687 Expired CN1018736B (en) | 1988-03-18 | 1988-03-18 | Production of high-voltage high specific capacitance tantalum powder by means of carbon reduction |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102744415A (en) * | 2012-07-18 | 2012-10-24 | 江西景泰钽业有限公司 | Method for preparing metallurgical-grade powder by utilizing wastes of tantalum-niobium capacitor and carbonization-hydrogenation device |
| CN103447544A (en) * | 2013-09-24 | 2013-12-18 | 泰克科技(苏州)有限公司 | Preparation method of particle size distribution concentrated and controllable high-purity tantalum powder |
| CN103700504A (en) * | 2013-12-17 | 2014-04-02 | 中国振华（集团）新云电子元器件有限责任公司 | Sintering method for enhancing tantalum wire tension on anode block of tantalum capacitor |
| CN104087713A (en) * | 2014-06-26 | 2014-10-08 | 浙江锦诚耐火材料有限公司 | Processing technique of low-nitrogen low-hydrogen carburizing agent |
| CN104475747A (en) * | 2014-12-05 | 2015-04-01 | 宁夏东方钽业股份有限公司 | Method for sintering preparation of tantalum powder for high-purity tantalum ingots by carbon reduction process |
| CN105665731A (en) * | 2016-04-15 | 2016-06-15 | 陈尚军 | Method for preparing tantalum powder |
| CN108217596A (en) * | 2018-01-29 | 2018-06-29 | 吉林大学 | Niobium hydride and the method for tantalum hydride are prepared using non-hydrogen source solwution method |
| CN113560561A (en) * | 2021-06-16 | 2021-10-29 | 炎陵龙翔钽铌新材料有限责任公司 | Spherical tantalum powder, preparation method and application thereof |
-
1988
- 1988-03-18 CN CN 88105687 patent/CN1018736B/en not_active Expired
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102744415A (en) * | 2012-07-18 | 2012-10-24 | 江西景泰钽业有限公司 | Method for preparing metallurgical-grade powder by utilizing wastes of tantalum-niobium capacitor and carbonization-hydrogenation device |
| CN102744415B (en) * | 2012-07-18 | 2014-03-19 | 江西智诚新材料科技有限公司 | Method for preparing metallurgical-grade powder by utilizing wastes of tantalum-niobium capacitor and carbonization-hydrogenation device |
| CN103447544A (en) * | 2013-09-24 | 2013-12-18 | 泰克科技(苏州)有限公司 | Preparation method of particle size distribution concentrated and controllable high-purity tantalum powder |
| CN103447544B (en) * | 2013-09-24 | 2016-03-02 | 泰克科技(苏州)有限公司 | Size distribution concentrates controlled High-purity Tantalum powder, preparation method thereof |
| CN103700504A (en) * | 2013-12-17 | 2014-04-02 | 中国振华（集团）新云电子元器件有限责任公司 | Sintering method for enhancing tantalum wire tension on anode block of tantalum capacitor |
| CN103700504B (en) * | 2013-12-17 | 2016-07-20 | 中国振华（集团）新云电子元器件有限责任公司 | Improve the sintering method of anode block of tantalum capacitor tantalum wire pulling force |
| CN104087713A (en) * | 2014-06-26 | 2014-10-08 | 浙江锦诚耐火材料有限公司 | Processing technique of low-nitrogen low-hydrogen carburizing agent |
| CN104475747A (en) * | 2014-12-05 | 2015-04-01 | 宁夏东方钽业股份有限公司 | Method for sintering preparation of tantalum powder for high-purity tantalum ingots by carbon reduction process |
| CN105665731A (en) * | 2016-04-15 | 2016-06-15 | 陈尚军 | Method for preparing tantalum powder |
| CN108217596A (en) * | 2018-01-29 | 2018-06-29 | 吉林大学 | Niobium hydride and the method for tantalum hydride are prepared using non-hydrogen source solwution method |
| CN113560561A (en) * | 2021-06-16 | 2021-10-29 | 炎陵龙翔钽铌新材料有限责任公司 | Spherical tantalum powder, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1018736B (en) | 1992-10-21 |
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