CN104379792B - A kind of capacitor level tantalum-niobium alloy silk material powder and preparation method thereof - Google Patents
A kind of capacitor level tantalum-niobium alloy silk material powder and preparation method thereof Download PDFInfo
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- CN104379792B CN104379792B CN201380032441.3A CN201380032441A CN104379792B CN 104379792 B CN104379792 B CN 104379792B CN 201380032441 A CN201380032441 A CN 201380032441A CN 104379792 B CN104379792 B CN 104379792B
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- tantalum
- niobium
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/12—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of wires
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/008—Terminals
- H01G9/012—Terminals specially adapted for solid capacitors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
Abstract
Capacitor level tantalum-niobium alloy silk material powder and preparation method thereof, described powder is made up of tantalum powder and niobium powder, and wherein tantalum powder is 1:2 to 3:2 with the part by weight of niobium powder, and the purity of tantalum powder and niobium powder is all higher than 99.9 weight %；The granularity of tantalum powder is 80 mesh to 150 mesh, and the granularity of niobium powder is 150 mesh to 200 mesh, and the loose specific weight of powder is 3.0 4.3g/cm3；The preparation method of this powder includes dispensing, hand mix, first batch mixing, rerolling and No. three batch mixings, thus obtains capacitor level tantalum-niobium alloy silk material powder.This preparation method is reasonable in design, the most two different kinds of metal powder material full and uniform；Whole production process high degree of controlled, constant product quality thus the production of beneficially capacitor level tantalum-niobium alloy silk material.
Description
Technical field
The present invention relates to capacitor area, and be more particularly to a kind of capacitor level tantalum-niobium alloy silk
Material powder and preparation method thereof.
Background technology
Capacitor level tantalum-niobium alloy silk material is applied to capacitor, is commonly used to fabricate capacitor anode
Lead-in wire.Manufacture capacitor level tantalum-niobium alloy silk material raw materials used for tantalum powder with niobium powder.By a definite proportion
The tantalum powder of example and niobium powder through batch mixing, compressing, vacuum-sintering or melting, roll or forge,
The techniques such as intermediate annealing, drawing, finished products are finally manufactured into capacitor level tantalum-niobium alloy silk material.
Capacitor level tantalum-niobium alloy silk material powder is the former of manufacture container levels tantalum-niobium alloy silk material
Material, the uniformity of described powder directly affects the quality of final products.Traditional capacitor tantalum wire
It is single tantalum powder with powder, because not containing other metals so batch mixing uniformity easily realizes.
In capacitor level tantalum-niobium alloy silk material powder, the granularity of niobium powder is less, and unit volume is particles contained
The relative tantalum powder of number is more.Substantial amounts of little granule niobium powder flocks together, and during batch mixing
It is difficult to dispersion, therefore there is non-uniform phenomenon at microcosmic.Therefore, in order to prepare capacitor
Level tantalum-niobium alloy silk material, it is desirable to provide the tantalite niobite power end mixture of good mixing.
Summary of the invention
It is an object of the invention to provide a kind of capacitor level tantalum-niobium alloy silk material powder and
The method of this powder of steady production, utilizes the method can produce tantalum-niobium alloy silk on an industrial scale
Material powder, described tantalum-niobium alloy silk material powder has high uniformity.By for the first time
Adding proportion (such as, the tantalum powder and first of tantalum powder and niobium powder is to a certain degree determined during batch mixing
Part niobium powder weight ratio is about 2:1) can avoid too much causing because disposable niobium powder adds
Non-uniform phenomenon.And control batch mixing speed and ensure that niobium powder is sufficiently mixed with tantalum powder and keeps away further
Exempt from the powder dough phenomenon caused because of batch mixing excessive velocities.Described powder is particularly well-suited to system
Make capacitor level tantalum-niobium alloy silk.
On the one hand, the invention provides a kind of capacitor level tantalum-niobium alloy silk material powder, described
Powder is made up of tantalum powder and niobium powder, and wherein tantalum powder is 1:2 to 3:2 with the part by weight of niobium powder,
The purity of described tantalum powder and niobium powder is all higher than 99.9 weight %, and the granularity of described tantalum powder is-80 mesh
To-150 mesh, and the granularity of described niobium powder is-150 mesh to-200 mesh, and described powder
Loose specific weight is 3.0-4.3g/cm3。
On the other hand, the invention provides and prepare the side of capacitor level tantalum-niobium alloy silk material powder
Method, the method comprising the steps of:
(1) dispensing: weighing niobium powder and tantalum powder by proportioning, the purity of described tantalum powder and niobium powder is equal
More than 99.9 weight %, the granularity of described tantalum powder is-80 mesh to-150 mesh, the grain of described niobium powder
Degree is-150 mesh to-200 mesh, and wherein tantalum powder is 1:2 to 3:2 with the part by weight of niobium powder；
(2) hand mix: described niobium powder is divided into Part I and Part II, and by institute
The whole tantalum powder and the Part I niobium powder that weigh are placed in rustless steel container, then enter by shovel
Row hand operated mixing mixes；
(3) first batch mixing: then the powder after hand mix is put into batch mixer and goes forward side by side
Step mixing, first mixes 0.4-0.6 hour by the speed of 10-15 rev/min,
(4) rerolling: mix 0.9-1.1 hour by the speed of 20-25 rev/min again, with
And
No. (5) three batch mixings: remaining Part II niobium powder is put into batch mixer, go forward side by side one
The speed of step 25-30 rev/min mixes 0.9-1.1 hour thus obtains capacitor level tantalum niobium and close
Spun gold material powder.
In the step (2) of the inventive method, the weight of described Part I niobium powder is described
The 45%-55% of tantalum grain weight amount, and preferably 50%.
The technical characterstic of the inventive method is:
The ratio adding niobium powder and tantalum powder the most for the first time controls: first interpolation niobium powder and the weight of tantalum powder
Ratio should control at about 1:2, continues in residue niobium powder adds to after rerolling batch mixer again
Batch mixing.
(2) batch mixing: manual batch mixing control 3-6 minute, first batch mixing speed be 10-15 turn/
Minute and mixing time be 0.4-0.6 hour, rerolling speed is 20-25 rev/min and mixed
The material time is 0.9-1.1 hour, and the speed of No. three batch mixings is 25-30 rev/min and mixing time
For 0.9-1.1 hour.
Detailed description of the invention
In the present invention, " mesh " is used to represent that the granularity of niobium powder or tantalum powder is (according to the U.S.
ASTM standard).Just as used in this application with known in those skilled in the art,
When representing the granularity of powder with mesh number, the "-" number before mesh number represents " passing through " described mesh
The screen cloth of number.Such as "-150 mesh " represents the granule screen cloth by 150 mesh of powder.
Below by specific embodiment, the present invention is illustrated.But should be clearly
It is to the invention is not restricted to these specific embodiments.
Embodiment 1
Weigh-160 mesh niobium powder 4kg and-100 mesh tantalum powder 6kg by proportioning, then will be weighed
Total weight tantalum powder and 3kg niobium powder be placed in rustless steel container.First the evenest by shovel
Speed stirring 3 minutes, then puts into V-shaped batch mixer by the powder after hand mix, first uses
The speed of 10 revs/min mixes 0.5 hour, then mixes 1 hour by the speed of 20 revs/min,
Then shut down and residue niobium powder is put into batch mixer and to mix 1 by the speed of 25 revs/min little
Time.Gained powder is capacitor level tantalum-niobium alloy silk material powder, and gained powder pine ratio is
4.21g/cm3。
Embodiment 2
Weigh-160 mesh niobium powder 10kg and-100 mesh tantalum powder 10kg in proportion, then will be weighed
Total weight tantalum powder and 5kg niobium powder be placed in rustless steel container.First the evenest by shovel
Speed stirring 3 minutes, then puts into V-shaped batch mixer by the powder after hand mix, first uses
The speed of 12 revs/min mixes 0.5 hour, then mixes 1 hour by the speed of 22 revs/min,
Then shut down and residue niobium powder is put into batch mixer and to mix 1 by the speed of 27 revs/min little
Time.Gained powder is capacitor level tantalum-niobium alloy silk material powder, and gained powder pine ratio is
4.11g/cm3。
Embodiment 3
Weigh-150 mesh niobium powder 12kg and-90 mesh tantalum powder 8kg by proportioning, then will be weighed
Total weight tantalum powder and 4kg niobium powder be placed in rustless steel container.First the evenest by shovel
Speed stirring 3 minutes, then puts into V-shaped batch mixer by the powder after hand mix, first uses
The speed of 12 revs/min mixes 0.5 hour, then mixes 1 hour by the speed of 22 revs/min,
Then shut down and residue niobium powder is put into batch mixer and to mix 1 by the speed of 27 revs/min little
Time.Gained powder is capacitor level tantalum-niobium alloy silk material powder, and gained powder pine ratio is
4.01g/cm3。
Embodiment 4
Weigh-150 mesh niobium powder 30kg and-90 mesh tantalum powder 24kg by proportioning, then will be weighed
Total weight tantalum powder and 12kg niobium powder be placed in rustless steel container.First the evenest by shovel
Speed stirring 3 minutes, then puts into V-shaped batch mixer by the powder after hand mix, first uses
The speed of 15 revs/min mixes 0.5 hour, then mixes 1 hour by the speed of 25 revs/min,
Then shut down and residue niobium powder is put into batch mixer and to mix 1 by the speed of 30 revs/min little
Time.Gained powder is capacitor level tantalum-niobium alloy silk material powder, and gained powder pine ratio is
4.07g/cm3。
Comparative example
Weigh-160 mesh niobium powder 4kg and-100 mesh tantalum powder 6kg, then whole by weighed
Weight tantalum powder and niobium powder are placed in batch mixer, use the speed of 25 revs/min to mix 2.5 little
Time.Gained powder pine is than for 4.16g/cm3。
Above example 1-4 uses manufacture method involved in the present invention, and comparative example is normal
Rule method.The tantalum-niobium alloy silk material powder manufacture method that the present invention relates to can obtain have fabulous
The powder of uniformity；Tantalum-niobium alloy silk material is manufactured by this powder by following process process, permissible
The advantage fully demonstrating the tantalum-niobium alloy silk material powder of the present invention further.At tantalum-niobium alloy
In the silk material course of processing, the tantalum-niobium alloy silk material drawing course of processing would generally occur fracture of wire existing
As.It has been generally acknowledged that the occurrence frequency of this fracture of wire phenomenon is closely related with the uniformity of powder.Tool
Body ground, powder is the most uniform, then the fracture of wire frequency in the silk material drawing course of processing is the lowest；For changing
It, powder is the most uneven, then the fracture of wire frequency in the silk material drawing course of processing is the highest.Use reality
Execute example 1-4 and comparative example gained powder carries out alloy wire processing, all in the course of processing
Process conditions and equipment all keep consistent, and add up fracture of wire frequency in the course of processing (with
The fracture of wire number of times often processing the generation of ten thousand metres silk material represents).The wire-drawing equipment used is
LZ180 type linear drawing machine, institute's drawing silk material a diameter of 0.18mm concrete outcome such as table 1 below
Shown in.
Table 1
| Sequence number | Tantalum-niobium alloy silk material drawing process every ten thousand metres fracture of wire number of times |
| Embodiment 1 | 0.23 time |
| Embodiment 2 | 0.32 time |
| Embodiment 3 | 0.25 time |
| Embodiment 4 | 0.29 time |
| Comparative example | 1.4 it is secondary |
As it can be seen from table 1 in tantalum-niobium alloy silk material drawing process, embodiment 1-4 gained
The fracture of wire frequency of powder is substantially less than comparative example；This demonstrate the tantalum-niobium alloy powder of the present invention
Uniformity is significantly better than comparative example.Additionally, due to relatively low fracture of wire frequency is remarkably improved production
Efficiency, therefore the tantalum-niobium alloy powder of the present invention is highly suitable for manufacturing capacitor level tantalum-niobium alloy
Silk material, and the technique effect of excellence can be realized.
Claims (3)
1. a capacitor level tantalum-niobium alloy silk material powder, described powder is by tantalum powder and niobium powder group
Becoming, wherein the part by weight of tantalum powder and niobium powder is 1:2 to 3:2, described tantalum powder and niobium powder pure
Degree is all higher than 99.9 weight %, and the granularity of described tantalum powder is-80 mesh to-150 mesh, and described niobium
The granularity of powder is-150 mesh to-200 mesh, and the loose specific weight of described powder is
3.0-4.3g/cm3。
2. prepare the side of capacitor level tantalum-niobium alloy silk material powder as claimed in claim 1
Method, the method comprises the following steps:
(1) dispensing: weighing niobium powder and tantalum powder by proportioning, the purity of described tantalum powder and niobium powder is equal
More than 99.9 weight %, the granularity of described tantalum powder is-80 mesh to-150 mesh, described niobium powder
Granularity is-150 mesh to-200 mesh, and the part by weight of wherein tantalum powder and niobium powder be 1:2 extremely
3:2；
(2) hand mix: described niobium powder is divided into Part I and Part II, and by institute
The whole tantalum powder and the Part I niobium powder that weigh are placed in rustless steel container, then enter by shovel
Row hand operated mixing mixes；
(3) first batch mixing: the powder after hand mix is put into batch mixer, uses 10-15
Rev/min speed mix 0.4-0.6 hour；
(4) rerolling: mix 0.9-1.1 hour by the speed of 20-25 rev/min again；
No. (5) three batch mixings: remaining Part II niobium powder is put into batch mixer, go forward side by side one
Step mixes 0.9-1.1 hour by the speed of 25-30 rev/min, thus obtains capacitor level tantalum niobium
Alloy wire powder,
In step (2), the weight of described Part I niobium powder is described tantalum grain weight amount
45%-55%.
Method the most according to claim 2, wherein in step (2), described first
The weight of part niobium powder is the 50% of described tantalum grain weight amount.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/CN2013/071875 WO2014131150A1 (en) | 2013-02-26 | 2013-02-26 | Powder material used for capacitor-level tantalum-niobium alloy wire material and preparing method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104379792A CN104379792A (en) | 2015-02-25 |
| CN104379792B true CN104379792B (en) | 2016-11-16 |
Family
ID=51427455
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201380032441.3A Active CN104379792B (en) | 2013-02-26 | 2013-02-26 | A kind of capacitor level tantalum-niobium alloy silk material powder and preparation method thereof |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP2016516124A (en) |
| CN (1) | CN104379792B (en) |
| IL (1) | IL236833A0 (en) |
| MX (1) | MX2015000570A (en) |
| WO (1) | WO2014131150A1 (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4017302A (en) * | 1976-02-04 | 1977-04-12 | Fansteel Inc. | Tantalum metal powder |
| CN1308566A (en) * | 1998-05-06 | 2001-08-15 | H·C·施塔克公司 | Metal powders produced by the reduction of the oxides with gaseous magnesium |
| CN1410209A (en) * | 2001-09-29 | 2003-04-16 | 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 |
| CN1607055A (en) * | 1998-05-06 | 2005-04-20 | H.C.施塔克公司 | Metal powders prepared by reduction of related oxides with gaseous magnesium |
| CN1919508A (en) * | 1998-05-06 | 2007-02-28 | H.C.施塔克公司 | Metal powders produced by the reduction of the oxides with gaseous magnesium |
| CN101184568A (en) * | 2005-05-31 | 2008-05-21 | 卡伯特超金属株式会社 | Metal powder and manufacturing methods thereof |
| CN101859649A (en) * | 2010-04-16 | 2010-10-13 | 株洲宏达电子有限公司 | Solid electrolyte tantalum-niobium composite capacitor and preparation method thereof |
-
2013
- 2013-02-26 JP JP2015558324A patent/JP2016516124A/en active Pending
- 2013-02-26 MX MX2015000570A patent/MX2015000570A/en unknown
- 2013-02-26 CN CN201380032441.3A patent/CN104379792B/en active Active
- 2013-02-26 WO PCT/CN2013/071875 patent/WO2014131150A1/en active Application Filing
-
2015
- 2015-01-21 IL IL236833A patent/IL236833A0/en unknown
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4017302A (en) * | 1976-02-04 | 1977-04-12 | Fansteel Inc. | Tantalum metal powder |
| CN1308566A (en) * | 1998-05-06 | 2001-08-15 | H·C·施塔克公司 | Metal powders produced by the reduction of the oxides with gaseous magnesium |
| CN1607055A (en) * | 1998-05-06 | 2005-04-20 | H.C.施塔克公司 | Metal powders prepared by reduction of related oxides with gaseous magnesium |
| CN1919508A (en) * | 1998-05-06 | 2007-02-28 | H.C.施塔克公司 | Metal powders produced by the reduction of the oxides with gaseous magnesium |
| CN1410209A (en) * | 2001-09-29 | 2003-04-16 | 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 |
| CN101184568A (en) * | 2005-05-31 | 2008-05-21 | 卡伯特超金属株式会社 | Metal powder and manufacturing methods thereof |
| CN101859649A (en) * | 2010-04-16 | 2010-10-13 | 株洲宏达电子有限公司 | Solid electrolyte tantalum-niobium composite capacitor and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| IL236833A0 (en) | 2015-03-31 |
| WO2014131150A1 (en) | 2014-09-04 |
| JP2016516124A (en) | 2016-06-02 |
| CN104379792A (en) | 2015-02-25 |
| MX2015000570A (en) | 2015-04-10 |
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