KR101616559B1 - Method of manufacturing tantalum powder - Google Patents
Method of manufacturing tantalum powder Download PDFInfo
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- KR101616559B1 KR101616559B1 KR1020160008655A KR20160008655A KR101616559B1 KR 101616559 B1 KR101616559 B1 KR 101616559B1 KR 1020160008655 A KR1020160008655 A KR 1020160008655A KR 20160008655 A KR20160008655 A KR 20160008655A KR 101616559 B1 KR101616559 B1 KR 101616559B1
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- C01G35/00—Compounds of tantalum
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- C—CHEMISTRY; METALLURGY
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- C01P2006/00—Physical properties of inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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Abstract
Description
The present invention relates to a method for producing a tantalum powder.
Conventionally, in the production of tantalum powder, fine tantalum (Ta) powder having a BET specific surface area (specific surface area) exceeding 5 m < 2 > / g is obtained by reducing with alkali metal such as sodium, There has been a problem in that it is adversely affecting the capacity and electric characteristics of the electrolyte receptor when it is used as an advanced material for an electrolyte capacitor.
As the tantalum powder becomes finer, the specific surface area becomes larger and the specific capacity becomes larger accordingly.
However, since the reaction of the alkali metal reducing agent to obtain fine powder is an exothermic reaction, if it is desired to obtain a fine powder having a particle diameter of 0.1 to 1.0 μm, ultrafine fine particles of 0.05 μm or less are generated due to thermal inhomogeneity during the reduction process, Sintering) uniformity is unstable.
Since the tantalum oxide is in contact with the alkali metal directly, the reaction time is very short and a large amount of heat is generated. The particle size of the tantalum powder is controlled by the reduction temperature and the reaction temperature can not be completely controlled. Therefore, Can not be obtained stably.
The most common method for producing conventional tantalum powders is a sodium fluoro-reduction method.
In this process, particle size and specific surface area can be controlled by addition of inert salt such as KCl, NaCl and NaF, and the amount of inert salt can be increased to finer tantalum powder. However, when the inert salt concentration is increased, do.
In this reduction process, the production of tantalum powder with finer initial particle size requires increased ratio of reducing agent and stirring speed, which makes the control of the reaction process more difficult and increases the production cost.
Accordingly, it is urgent for manufacturers of tantalum capacitors to produce uniform particle size, low oxygen content, and higher specific capacity tantalum powder.
To provide a method for manufacturing a high-quality tantalum metal powder suitable for capacitor production and maximizing specific capacity.
In one embodiment of the present invention, tantalum oxide is reduced with one of yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), and neodymium (Nd) A first reducing step of adjusting the oxygen content in the tantalum oxide to 5.0 wt% or more and 15.0 wt% or less based on 100 wt% of the total oxide; A first washing step of pickling or washing with water the tantalum oxide obtained in the first reducing step to remove the reducing agent remaining on the surface of the tantalum oxide powder; A second reduction step of the first magnesium (Mg), tantalum oxide obtained by the reduction step, and a magnesium (Mg) -M 1 was reduced by one kind of the alloy, or two or more of these reducing agent, to yield a tantalum powder; And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step, Is adjusted to a content of not less than 0.30 times and not more than 0.40 times with respect to the stoichiometric amount of the reducing agent required to remove all the oxygen contained in the tantalum oxide, and the reducing agent in the second reducing step Wherein the amount of the tantalum powder is controlled to be 0.5 times or more and 1.5 times or less with respect to the stoichiometric amount of the reducing agent required to remove all remaining oxygen in the tantalum oxide obtained in the first reduction step.
The M 1 may include Ca, Zn, Y, La, Ce, or Nd.
Wherein the reducing agent is a mixture of yttrium (Y) and lanthanum (La), and the content ratio of lanthanum (La) to the content of yttrium (Y) in the mixture is 0.5 or more and 1.5 or less . More specifically, it may be one.
The second reduction stage; in, the reducing agent is magnesium (Mg), and magnesium-yttrium alloy, and a mixture of (Mg 2 Y), magnesium for the content of magnesium (Mg) and the mixture-yttrium alloy (Mg 2 Y) May be 0.5 or more, and 1.5 or less. More specifically, it may be one.
The first reducing step is a step of reducing the tantalum oxide with one of yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), and neodymium (Nd) , And adjusting the oxygen content in the tantalum oxide to not less than 5.6 wt% and not more than 11.23 wt% with respect to 100 wt% of the total oxide.
The first reduction step may be performed at a temperature of 500 ° C or higher and 1100 ° C or lower.
The first reduction step may be performed for a time of 4 hours or more, and a time of 9 hours or less.
The second reduction step may be performed at a temperature of 250 ° C or more, and 1000 ° C or less.
The second reducing step may be performed for 2.5 hours or more and 7 hours or less.
The tantalum powder finally produced by the above-mentioned method has a particle size of not less than 0.3 μm and not more than 1.8 μm, a BET specific surface area of not less than 5.0 m 2 / g and not more than 9.0 m 2 / g, ) May be at least 144000 u FV / g.
The first reduction step may be performed in a mixed atmosphere of argon (Ar) and hydrogen (H 2 ).
The second reduction step may be performed in a mixed atmosphere of argon (Ar) and hydrogen (H 2 ).
Wherein the acid used in the pickling is selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid, sulfuric acid, nitric acid, sulfuric acid, Sulfuric acid, or a combination thereof.
And a first washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by acid washing or water washing of the tantalum oxide obtained in the first reducing step, wherein the water washing is deionized water, DIW). ≪ / RTI >
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing of the tantalum powder obtained in the second reducing step, wherein the acid used for the acid washing is hydrochloric acid, nitric acid, sulfuric acid , Or a combination thereof.
And a second washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by pickling or washing with water the tantalum oxide obtained in the second reducing step, wherein the water washing is deionized water, DIW). ≪ / RTI >
A first washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing of the tantalum powder obtained in the first reducing step; and performing the acid washing and the water washing alternately .
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step is performed by alternately performing the pickling and the water washing .
Removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step; Thereafter, drying the washed tantalum powder may be further included.
Drying the washed tantalum powder may be performed at a temperature of 80 ° C or higher and 160 ° C or lower.
An embodiment of the present invention provides a method for manufacturing a high-grade tantalum metal powder suitable for capacitor fabrication and maximizing specific capacity.
Hereinafter, embodiments of the present invention will be described in detail. However, it should be understood that the present invention is not limited thereto, and the present invention is only defined by the scope of the following claims.
In one embodiment of the present invention, tantalum oxide is reduced with one of yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), and neodymium (Nd) A first reducing step of adjusting the oxygen content in the tantalum oxide to 5.0 wt% or more and 15.0 wt% or less based on 100 wt% of the total oxide; A first washing step of pickling or washing with water the tantalum oxide obtained in the first reducing step to remove the reducing agent remaining on the surface of the tantalum oxide powder; A second reduction step of the first magnesium (Mg), tantalum oxide obtained by the reduction step, and a magnesium (Mg) -M 1 was reduced by one kind of the alloy, or two or more of these reducing agent, to yield a tantalum powder; And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step, Is adjusted to a content of not less than 0.30 times and not more than 0.40 times with respect to the stoichiometric amount of the reducing agent required to remove all the oxygen contained in the tantalum oxide, and the reducing agent in the second reducing step Wherein the amount of the tantalum powder is controlled to be 0.5 times or more and 1.5 times or less with respect to the stoichiometric amount of the reducing agent required to remove all remaining oxygen in the tantalum oxide obtained in the first reduction step.
The M 1 may include Ca, Zn, Y, La, Ce, or Nd.
Wherein the reducing agent is a mixture of yttrium (Y) and lanthanum (La), and the content ratio of lanthanum (La) to the content of yttrium (Y) in the mixture is 0.5 or more and 1.5 or less . More specifically, the content ratio of lanthanum (La) to the content of yttrium (Y) in the mixture may be 1. By mixing the mixture of yttrium and lanthanum as the reducing agent within the above range, the residual oxygen amount of the tantalum oxide after the first reducing step can be efficiently controlled.
Specifically, the first reducing step may be a step in which the tantalum oxide is formed of one of yttrium (Y), lanthanum (La), cerium (Ce), praseodymium (Pr), and neodymium (Nd) To adjust the oxygen content in the tantalum oxide to not less than 5.6 wt% and not more than 11.23 wt% based on 100 wt% of the total oxide. This can be achieved by adjusting the amount of the reducing agent in the first reducing step to a content of 0.30 times or more and 0.40 times or less with respect to the stoichiometric amount of the reducing agent necessary for removing all the oxygen contained in the tantalum oxide have. More specifically 0.35 times or more, and 0.40 times or less.
If the oxygen content in the tantalum oxide powder produced in the first reduction step is less than 5.6 wt%, an excessive amount of reducing agent is used in the first reduction step, and a high temperature is generated in the reaction, Tantalum powder can not be produced. If the oxygen content in the tantalum oxide powder produced in the first reduction step is more than 11.23 wt%, it is necessary to use an excessive amount of reducing agent in the second reducing step, so that the oxide particles are coarse with high temperature generated during the second reducing step .
In order to obtain the finally obtained tantalum powder with a uniform particle size, a low impurity content, a large specific surface area and a high non-capacity property, it is most important to use an appropriate amount of the reducing agent accurately at each reducing step.
In one embodiment of the present invention, the amount of the reducing agent in the first reducing step is adjusted to a content of 0.30 times or more and 0.40 times or less with respect to the stoichiometric amount of the reducing agent required to remove all the oxygen contained in the tantalum oxide The amount of oxygen in the tantalum oxide obtained after the first reducing step is adjusted to an appropriate level (about 10% or so), so that a proper amount of the reducing agent can be introduced in the second reducing step, Tantalum powder having a large specific surface area and a high non-capacity property can be produced.
The reducing agent in the second reducing step is adjusted to a content of 0.5 times or more and 1.5 times or less with respect to a stoichiometric amount of a reducing agent necessary for removing all the residual oxygen in the tantalum oxide obtained in the first reducing step Lt; / RTI > More specifically, 0.9 times or more, and 1.1 times or less.
The second reduction stage; in, the reducing agent is magnesium (Mg), and magnesium-yttrium alloy, and a mixture of (Mg 2 Y), magnesium for the content of magnesium (Mg) and the mixture-yttrium alloy (Mg 2 Y) May be 0.5 or more, and 1.5 or less. More specifically, the content ratio of the magnesium-yttrium alloy (Mg 2 Y) to the content of magnesium (Mg) in the mixture may be 1. By combining the above-mentioned mixture of magnesium (Mg) and magnesium-yttrium alloy (Mg 2 Y) as a reducing agent within the above range, it is possible to effectively reduce the residual oxygen of the tantalum powder obtained after the second reducing step and to maximize the specific surface area and cost Tantalum powder can be produced.
The first reduction step may be performed at a temperature of 500 ° C or higher and 1100 ° C or lower.
If the reaction temperature is higher than 1100 ° C, the rate of the reduction reaction becomes too fast in the environment immediately before the melting or melting of the reducing agent, so the tantalum oxide may be sintered and the powder may become rough. More preferably, the reducing temperature of the first reducing step is preferably not higher than 1000 캜. If the reaction temperature is lower than 500 ° C, a complete reduction reaction may not occur.
The first reduction step may be performed for a time of 4 hours or more, and a time of 9 hours or less. If the reaction time exceeds 9 hours, the particles of the reaction product may become rough. If the reaction time is less than 4 hours, the reaction may not be sufficiently completed.
The second reduction step may be performed at a temperature of 250 ° C or more, and 1000 ° C or less. If the reaction temperature exceeds 1000 ° C, the reaction rate becomes faster and the tantalum powder may be sintered and the powder may become rough. If the reaction temperature is lower than 250 ° C, the reaction may not be sufficiently completed.
2.5 hours or more, and 7 hours or less. If the reaction time exceeds 7 hours, the particles of the reaction product may become rough. If the reaction time is less than 2.5 hours, the reaction may not be sufficiently completed.
The finally produced tantalum powder may have a particle size of 0.3 μm or more and 1.8 μm or less and a BET specific surface area of 5.0 m 2 / g or more and 9.0 m 2 / g or less. The electrical ratio of the finally produced tantalum powder The Specific Capacity may be 144000 uFV / g or more. More specifically, not less than 144000 uFV / g, and not more than 300,000 uFV / g.
As described above, by controlling the content of the reducing agent in the first and second reducing processes and performing the reduction at a specific temperature and time range, tantalum powder having a dense, high specific surface, and no specific capacity can be produced .
The first reducing step; And the second reduction step may be performed in a mixed atmosphere of argon (Ar) and hydrogen (H 2 ).
Wherein the acid used in the pickling is selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid, sulfuric acid, nitric acid, sulfuric acid, Sulfuric acid, or a combination thereof.
And a first washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by acid washing or water washing of the tantalum oxide obtained in the first reducing step, wherein the water washing is deionized water, DIW). ≪ / RTI >
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing of the tantalum powder obtained in the second reducing step, wherein the acid used for the acid washing is hydrochloric acid, nitric acid, sulfuric acid , Or a combination thereof.
And a second washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by pickling or washing with water the tantalum oxide obtained in the second reducing step, wherein the water washing is deionized water, DIW). ≪ / RTI >
In the first washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing of the tantalum powder obtained in the first reducing step, acid washing or water washing is repeatedly carried out if necessary And alternately performing the pickling, and the water washing alternately.
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step and performing acid pickling or water washing repeatedly And alternately performing the pickling, and the water washing alternately.
The method of manufacturing a tantalum powder according to an embodiment of the present invention includes the steps of pickling or washing with water the tantalum powder obtained in the second reducing step to remove the reducing agent remaining on the surface of the tantalum powder; Thereafter, drying the washed tantalum powder may be further included.
Drying the washed tantalum powder may be performed in an oven at a temperature of 80 ° C or higher, and 160 ° C or lower.
Hereinafter, preferred embodiments and comparative examples of the present invention will be described. However, the following examples are only a preferred embodiment of the present invention, and the present invention is not limited to the following examples.
Example One
The first reduction step
500 g of 100 mesh tantalum oxide (Ta 2 O- 5 ) powder and 350 g of a mixed powder of 80 mesh yttrium and lanthanum (based on yttrium: lanthanum = 1: 1 by weight) were uniformly mixed and placed in a molybdenum crucible. The weight of the mixed powder of yttrium and lanthanum is 0.35 times the stoichiometric amount of the reducing agent required to remove the oxygen contained in the tantalum oxide.
Thereafter, the molybdenum crucible was placed in a closed reaction vessel, vacuumed, filled with argon, and heated to 600 DEG C in an argon atmosphere.
The hydrogen was then charged to the reaction vessel at a rate of 50% relative to the argon volume and maintained at a temperature of 600 [deg.] C or more and 900 [deg.] C or less for 8 hours.
Thereafter, cooling and passivation were completed, and the powder in the molybdenum crucible was taken out and the residual reducing agent was removed from 8% by weight of hydrochloric acid water, and the powder was filtered and washed with deionized water and dried.
The oxygen content of the obtained tantalum oxide was analyzed by an infrared oxygen analyzer, and the oxygen content was found to be 5.6%.
Second Reduction Step
Thereafter, an 80 mesh magnesium powder and a yttrium-magnesium alloy (Mg 2 Y) mixed powder (magnesium powder: yttrium-magnesium alloy (Mg 2 Y) mixed powder = 1: 1 in a weight ratio) And stirred with the tantalum oxide powder obtained in the process.
Here, the amounts of the magnesium powder and the yttrium-magnesium alloy (Mg 2 Y) were equal to 0.9 times the stoichiometric amount of the reducing agent required to remove the residual oxygen of the tantalum oxide powder obtained in the first reduction step.
Thereafter, the homogeneously mixed mixture was placed in a molybdenum crucible, the crucible was placed in a closed reaction vessel, and then a vacuum state was established.
It was then charged with argon and heated to 600 < 0 > C under an argon atmosphere.
Thereafter, 50% hydrogen was injected into the reaction vessel at a ratio to the above argon volume, and maintained at 350 DEG C or more and 800 DEG C for 7 hours.
After cooling and passivation were completed, the tantalum powder in the molybdenum crucible was dissolved in 8% by weight of hydrochloric acid water to remove the residual reducing agent, and then the powder was filtered and washed with deionized water and dried to obtain high purity tantalum powder.
Example 2
The first reduction step
500 g of a powder of 150 mesh tantalum oxide (Ta 2 O 5 ) and 400 g of a mixed powder of 100 mesh yttrium and lanthanum (yttrium: lanthanum = 1: 1 on a weight basis) were uniformly mixed and placed in a molybdenum crucible. The weight of the mixed powder of yttrium and lanthanum is 0.4 times the stoichiometric amount of the reducing agent required to remove oxygen contained in the tantalum oxide.
Thereafter, the molybdenum crucible was placed in a sealed reaction vessel, and then vacuumed, filled with argon, and heated to 1000 캜 in an argon atmosphere.
The hydrogen was then charged to the reaction vessel at a rate of 50% relative to the volume of argon and maintained at a temperature above 700 [deg.] C and below 1100 [deg.] C for 9 hours.
After the cooling and passivation were completed, the powder in the molybdenum crucible was taken out and the residual reducing agent was removed from 10% by weight of hydrochloric acid, and the powder was filtered and washed with deionized water and dried.
The oxygen content of the obtained tantalum oxide was analyzed by an infrared oxygen analyzer, and the oxygen content was 11.23%.
Second Reduction Step
Thereafter, a 100 mesh magnesium powder and a yttrium-magnesium alloy (Mg 2 Y) mixed powder (magnesium powder: yttrium-magnesium alloy (Mg 2 Y) mixed powder = 1: 1 in a weight ratio) And stirred with the tantalum oxide powder obtained in the process.
Here, the amounts of the magnesium powder and the yttrium-magnesium alloy (Mg 2 Y) were set to be equal to 1.1 times the stoichiometric amount of the reducing agent required to remove all residual oxygen of the tantalum oxide powder obtained in the first reduction step.
Thereafter, the homogeneously mixed mixture was placed in a molybdenum crucible, the crucible was placed in a closed reaction vessel, and then a vacuum state was established.
It was then charged with argon and heated to 800 < 0 > C under an argon atmosphere.
Thereafter, 50% hydrogen was injected into the reaction vessel at a ratio to the above argon volume, and maintained at 600 캜 or higher and at 1000 캜 or lower for 5 hours.
Thereafter, cooling and passivation were completed, and the tantalum powder in the molybdenum crucible was dissolved in 5% by weight of hydrochloric acid water to remove the residual reducing agent, and then the powder was washed with deionized water and washed and dried to obtain high purity tantalum powder.
Example 3
The first reduction step
500 g of 100 mesh tantalum oxide (Ta 2 O- 5 ) powder and 350 g of a mixed powder of 80 mesh yttrium and lanthanum (based on yttrium: lanthanum = 1: 1 by weight) were uniformly mixed and placed in a molybdenum crucible. The weight of the mixed powder of yttrium and lanthanum is 0.35 times the stoichiometric amount of the reducing agent required to remove the oxygen contained in the tantalum oxide.
Thereafter, the molybdenum crucible was placed in a sealed reaction vessel, and then vacuumed, filled with argon, and heated to 1000 캜 in an argon atmosphere.
The hydrogen was then charged to the reaction vessel at a rate of 50% relative to the volume of argon and maintained at a temperature above 700 [deg.] C and below 1100 [deg.] C for 9 hours.
Thereafter, the cooling and passivation were completed, and the powder in the molybdenum crucible was taken out and the residual reducing agent was removed from 5% by weight of hydrochloric acid water, and the powder was then washed with deionized water and dried.
The oxygen content of the obtained tantalum oxide was analyzed by an infrared oxygen analyzer, and the oxygen content was found to be 7.25%.
Second Reduction Step
Thereafter, 800 mesh magnesium powder and a yttrium-magnesium alloy (Mg 2 Y) mixed powder (magnesium powder: yttrium-magnesium alloy (Mg 2 Y) mixed powder = 1: 1 in a weight ratio) And stirred with the tantalum oxide powder obtained in the process.
Here, the amounts of the magnesium powder and the yttrium-magnesium alloy (Mg 2 Y) were equal to 0.9 times the stoichiometric amount of the reducing agent required to remove the residual oxygen of the tantalum oxide powder obtained in the first reduction step.
Thereafter, the homogeneously mixed mixture was placed in a molybdenum crucible, the crucible was placed in a closed reaction vessel, and then a vacuum state was established.
It was then charged with argon and heated to 700 < 0 > C under an argon atmosphere.
Thereafter, 50% hydrogen was injected into the reaction vessel at a ratio to the above argon volume, and maintained at 600 캜 or higher and at 1000 캜 or lower for 7 hours.
After cooling and passivation were completed, the tantalum powder in the molybdenum crucible was dissolved in 10% by weight of hydrochloric acid water, and the remaining reducing agent was removed. The powder was then washed with deionized water and then washed and dried to obtain high purity tantalum powder.
Comparative Example One
The first reduction step
500 g of a 50 mesh tantalum oxide (Ta 2 O- 5 ) powder and 250 g of a mixed powder of yttrium and lanthanum (yttrium: lanthanum = 1: 1 on a weight basis) of 40 mesh were uniformly mixed and placed in a molybdenum crucible. The weight of the mixed powder of yttrium and lanthanum is 0.25 times the stoichiometric amount of the reducing agent required to remove oxygen contained in the tantalum oxide.
Thereafter, the molybdenum crucible was placed in a sealed reaction vessel, vacuumed, filled with argon, and heated to 500 DEG C in an argon atmosphere.
Hydrogen was then fed into the reaction vessel at a rate of 50% relative to the volume of argon and maintained at a temperature above 500 [deg.] C and below 1400 [deg.] C for 12 hours.
Thereafter, the cooling and passivation were completed, and the powder in the molybdenum crucible was taken out and the residual reducing agent was removed from 5% by weight of hydrochloric acid water, and the powder was then washed with deionized water and dried.
The oxygen content of the obtained tantalum oxide was analyzed by an infrared oxygen analyzer, and the oxygen content was 15.3%.
Second Reduction Step
Thereafter, 60 mesh magnesium powder and a yttrium-magnesium alloy (Mg 2 Y) mixed powder (magnesium powder: yttrium-magnesium alloy (Mg 2 Y) mixed powder = 1: 1 in a weight ratio) And stirred with the tantalum oxide powder obtained in the process.
Here, the amounts of the magnesium powder and the yttrium-magnesium alloy (Mg 2 Y) were equal to 0.4 times the stoichiometric amount of the reducing agent required to remove all residual oxygen of the tantalum oxide powder obtained in the first reduction step.
Thereafter, the homogeneously mixed mixture was placed in a molybdenum crucible, the crucible was placed in a closed reaction vessel, and then a vacuum state was established.
It was then charged with argon and heated to 300 < 0 > C under an argon atmosphere.
Thereafter, 50% hydrogen was injected into the reaction vessel at a ratio to the argon volume, maintained at 250 캜 or higher, and at 600 캜 for 5 hours.
Thereafter, cooling and passivation were completed, and the tantalum powder in the molybdenum crucible was dissolved in 5% by weight of hydrochloric acid water to remove the residual reducing agent, and then the powder was washed with deionized water and washed and dried to obtain high purity tantalum powder.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims. As will be understood by those skilled in the art. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Experimental Example
The average particle diameter, specific surface area, specific bulk density, electrical specific capacity, and leakage current amount of tantalum powder finally obtained in Examples 1 to 3 and Comparative Example 1 were measured as follows.
- Average particle size: measured by Fsss method (Fisher sub sieve sizer).
- Specific surface area: measured with a BET meter.
- Specific volume density: measured by the SCOTT method.
- Electrical Specific Capacity and Leakage Amount: The tantalum powder obtained in Examples 1 to 3 and Comparative Example 1 was compacted to a density of 4.5 g / cm 3 and a diameter of 2.5 mm. The sintered sample was sintered in a vacuum furnace at 1200 ° C. for 30 minutes, and then an anode was formed by applying a voltage of 16-20 V in a 0.15% phosphoric acid solution at 75 ° C. to measure the capacity and the leakage current.
The measurement results are summarized in Table 1 below.
(umFass)
(g / cm 3)
(m 2 / g BET)
(uFV / g)
(nA / uFV)
As can be seen from Table 1, the tantalum powders produced by the manufacturing methods of Examples 1 to 3 are finer than those of Comparative Example 1, and accordingly, the volume density and the specific surface area are high and the electrical cost is high, Which is much better to be used for.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the present invention as defined by the following claims. As will be understood by those skilled in the art. It is therefore to be understood that the above-described embodiments are illustrative in all aspects and not restrictive.
Claims (23)
A first washing step of pickling or washing with water the tantalum oxide obtained in the first reducing step to remove the reducing agent remaining on the surface of the tantalum oxide powder;
A second reducing step of reducing the tantalum oxide subjected to the first washing step to a mixed powder having a weight ratio of magnesium (Mg) and magnesium-yttrium alloy (Mg 2 Y) of 1: 1 to obtain tantalum powder; And
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing the tantalum powder obtained in the second reducing step,
In the first reduction step, the mixed powder having a weight ratio of yttrium (Y) and lanthanum (La) of 1: 1 is mixed with the stoichiometric amount of the reducing agent required to remove all oxygen contained in the tantalum oxide , 0.30 times or more, and 0.40 times or less,
In the second reducing step, the mixed powder having a weight ratio of magnesium (Mg) and magnesium-yttrium alloy (Mg 2 Y) of 1: 1 removes residual oxygen in the tantalum oxide obtained in the first reducing step Wherein the amount of the reducing agent is adjusted to 0.5 times or more and 1.5 times or less with respect to the stoichiometric amount of the reducing agent required for the reaction.
A method for producing tantalum powder.
Wherein the first reducing step comprises:
Wherein the content of oxygen in the tantalum oxide is adjusted to not less than 5.6 wt% and not more than 11.23 wt% based on 100 wt% of the total oxide.
A method for producing tantalum powder.
Wherein the first reducing step comprises:
Gt; C, < / RTI > and < RTI ID = 0.0 &
A method for producing tantalum powder.
Wherein the first reducing step comprises:
More than 4 hours, and less than 9 hours.
A method for producing tantalum powder.
Wherein the second reducing step comprises:
≪ RTI ID = 0.0 > 250 C, < / RTI &
A method for producing tantalum powder.
Wherein the second reducing step comprises:
2.5 hours or more, and 7 hours or less.
A method for producing tantalum powder.
Wherein the finally produced tantalum powder has a particle diameter of 0.3um or more and 1.8um or less,
A method for producing tantalum powder.
Wherein the finally prepared tantalum powder has a BET specific surface area of 5.0 m 2 / g or more and 9.0 m 2 / g or less,
A method for producing tantalum powder.
The specific capacity of the finally produced tantalum powder is 144000 uFV / g or more.
A method for producing tantalum powder.
Wherein the first reducing step comprises:
Argon (Ar), and hydrogen (H 2 ).
A method for producing tantalum powder.
Wherein the second reducing step comprises:
Argon (Ar), and hydrogen (H 2 ).
A method for producing tantalum powder.
And a first washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by pickling or washing with water the tantalum oxide obtained in the first reducing step,
The acid used for the pickling is,
Hydrochloric acid, nitric acid, sulfuric acid, or a combination thereof.
A method for producing tantalum powder.
And a first washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by pickling or washing with water the tantalum oxide obtained in the first reducing step,
Wherein the water washing is performed using de-ionized water (DIW).
A method for producing tantalum powder.
And a second washing step of removing the reducing agent remaining on the surface of the tantalum powder by pickling or water washing the tantalum powder obtained in the second reducing step,
The acid used for the pickling is,
Hydrochloric acid, nitric acid, sulfuric acid, or a combination thereof.
A method for producing tantalum powder.
And a second washing step of removing the reducing agent remaining on the surface of the tantalum oxide powder by pickling or washing with water the tantalum oxide obtained in the second reducing step,
Wherein the water washing is performed using de-ionized water (DIW).
A method for producing tantalum powder.
A first washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing of the tantalum powder obtained in the first reducing step,
The acid pickling, and the water washing alternately.
A method for producing tantalum powder.
A second washing step of removing the reducing agent remaining on the surface of the tantalum powder by acid washing or water washing the tantalum powder obtained in the second reducing step,
The acid pickling, and the water washing alternately.
A method for producing tantalum powder.
Removing the reducing agent remaining on the surface of the tantalum powder by pickling or washing with water the tantalum powder obtained in the second reducing step; Since the,
And drying the washed tantalum powder.
A method for producing tantalum powder.
Drying the washed tantalum powder,
Lt; RTI ID = 0.0 > 80 C, < / RTI &
A method for producing tantalum powder.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100220881B1 (en) * | 1990-05-17 | 1999-09-15 | 마싸 앤 피네간 | Method of producing high surface area low metal impurity tantalum powder |
| KR20000010636A (en) * | 1996-04-25 | 2000-02-25 | 마르타 앤 피네간 | Method of making tantalum metal powder with controlled size distribution and products made therefrom |
| KR20080076597A (en) * | 2007-02-16 | 2008-08-20 | 충남대학교산학협력단 | Nano tantallum powder |
| KR20120065309A (en) * | 2009-06-25 | 2012-06-20 | 닝시아 오리엔트 탄탈럼 인더스트리 코포레이션 엘티디 | Process for preparing tantalum powder for capacitors |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100220881B1 (en) * | 1990-05-17 | 1999-09-15 | 마싸 앤 피네간 | Method of producing high surface area low metal impurity tantalum powder |
| KR20000010636A (en) * | 1996-04-25 | 2000-02-25 | 마르타 앤 피네간 | Method of making tantalum metal powder with controlled size distribution and products made therefrom |
| KR20080076597A (en) * | 2007-02-16 | 2008-08-20 | 충남대학교산학협력단 | Nano tantallum powder |
| KR20120065309A (en) * | 2009-06-25 | 2012-06-20 | 닝시아 오리엔트 탄탈럼 인더스트리 코포레이션 엘티디 | Process for preparing tantalum powder for capacitors |
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