CN108607987A - Reduce the method and its equipment of anode tantalum core oxygen content - Google Patents
Reduce the method and its equipment of anode tantalum core oxygen content Download PDFInfo
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- CN108607987A CN108607987A CN201810461400.0A CN201810461400A CN108607987A CN 108607987 A CN108607987 A CN 108607987A CN 201810461400 A CN201810461400 A CN 201810461400A CN 108607987 A CN108607987 A CN 108607987A
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- tantalum core
- inert gas
- oxygen content
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- 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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The present invention provides a kind of methods and its equipment reducing anode tantalum core oxygen content, are related to electronic component manufacturing technology field.The method for reducing anode tantalum core oxygen content, includes the following steps：(a) by the inert gas plasma with alkalinous metal steam, the inert gas plasma containing alkalinous metal is formed；(b) tantalum core is placed in the inert gas plasma containing alkalinous metal；(c) alkalinous metal vapour source is isolated, is passed through inert gas, tantalum core is made to be placed in inert gas plasma.The method of the present invention accelerates the reaction speed of oxygen atom and alkaline metal ions, reduces the time of deoxidation process；Required environment temperature and pressure are relatively low, improve controllability and the safety of production process；It is effectively reduced the oxygen concentration of tantalum core inner, improves the performances such as the pressure resistance of final tantalum capacitance.
Description
Technical field
The present invention relates to electronic component manufacturing technology fields, more particularly, to a kind of side reducing anode tantalum core oxygen content
Method and its equipment.
Background technology
The anode of tantalum capacitance is typically by Ta powder used in capacitor by compression moulding, is prepared after high temperature sintering.Manufacture is former
Mixed oxygen atom can make the performance of tantalum capacitance larger shadow in impurity oxygen atom and production process tantalum powder in material in tantalum powder
It rings.When oxygen impurity concentration inside anode tantalum core is higher, the proof voltage energy of final tantalum capacitance can be influenced, or makes tantalum capacitance
Leakage current and angle of loss are bigger than normal.
Solve the problems, such as that this most direct scheme is that suppress capacitance using high-purity, the tantalum powder of low oxygen content Ta powder used,
And pay attention to keeping condition of high vacuum degree in high-sintering process, so that volatilizable oxide is volatilized as possible.But the former passes through tantalum powder
Scheme can greatly improve the purchase cost and difficulty of raw material, the latter is by the scheme of sintering process then by technical conditions and burning
The limitation of junction temperature.
It is reacted at high temperature with the oxygen in tantalum core to reduce oxygen content in tantalum core using alkalinous metal steam in the prior art
Method.This method is in actual use by a variety of limitations.First, reaction temperature must control the high temperature in tantalum core
Sintering temperature hereinafter, otherwise excessively high reaction temperature can make tantalum capacitance be modified, so that its capacitance is changed.Secondly, it directly heats
The method efficiency of reaction is relatively low, and reaction speed is not fast enough.For this reason, it may be necessary to the processing time of tantalum core, it usually needs processing 10 is small
When more than.The method that another kind accelerates processing is the temperature and pressure by improving reaction chamber, but causes the manufacture of equipment difficult
It spends higher, while controlling in technique also highly difficult.Therefore, technological deficiency below exists in the prior art：(1) it directly heats
Reaction, efficiency is low, and reaction speed is slow；(2) requirement of high temperature, high pressure to equipment is relatively high, and controllability and safety are low.
In consideration of it, special propose the present invention.
Invention content
The first object of the present invention is to provide a kind of method reducing anode tantalum core oxygen content, to alleviate in the prior art
The existing reaction efficiency that directly heats is low, and reaction speed is slow, and chamber interior reaction temperature is high, pressure is big, and controllability and safety are low
Etc. technical problems.
The method provided by the invention for reducing anode tantalum core oxygen content, includes the following steps：
(a) temperature more than the fusing point of alkalinous metal, boiling point hereinafter, pressure be 700-45000Pa under conditions of, will carry
The inert gas plasma of alkalinous metal steam forms the inert gas plasma containing alkalinous metal；
(b) tantalum core is placed in the inert gas plasma containing alkalinous metal, keeps the oxygen of tantalum in-core and alkalinous metal anti-
Alkaline metal oxide should be generated；
(c) alkalinous metal vapour source is isolated, is passed through inert gas, so that tantalum core is placed in inert gas plasma, make life
At alkaline metal oxide be discharged with inert gas；
Optional, carry out step (d)：Cooling system completes cooling.
Further, the alkalinous metal is selected from least one of magnesium, aluminium, calcium, preferably magnesium.
Further, the temperature is 650-1000 DEG C, preferably 700-950 DEG C, further preferably 750-900 DEG C；
The pressure is 2000-35000Pa, preferably 10000-20000Pa.
Further, the inert gas with alkalinous metal steam is by inert gas flow path alkalinous metal vapour source
It obtains, the preferably described alkalinous metal vapour source is waved by heating alkalinous metal to fusing point liquid formed above by liquid
Hair obtains.
Further, the temperature of the inert gas be 650-1200 DEG C, preferably 750-1050 DEG C, further preferably
800-1000℃。
Further, the inert gas is argon gas.
Further, in the step (b), time for tantalum core being placed in the inert gas plasma containing alkalinous metal
For 5-1000min, preferably 50-800min, further preferably 200-600min.
Further, in the step (c), make tantalum core be placed in the time in inert gas plasma be 1-100min,
Preferably 10-80min, further preferably 40-60min.
Further, the plasma is magnetized plasma；Preferably capacitively coupled plasma, inductively etc.
Gas ions or magnetic field-enhanced CCP radio frequency plasmas.
The second object of the present invention is to provide a kind of equipment reducing anode tantalum core oxygen content, and the equipment investment is few, fortune
Row expense is low, reliable and stable, convenient operation and management, and treated, and anode tantalum core oxygen content is substantially reduced, and improves the resistance to of tantalum capacitance
Voltage performance.
The equipment provided by the invention for reducing anode tantalum core oxygen content, including utilidor, the utilidor unicom are protected
One end of warm container, the utilidor is equipped with import, and the bottom of the cool-bag is equipped with outlet, is set in the utilidor
There are container and liftable cover board, the cover board to be located at the top of container, the container is equipped with induction heater, the heat preservation
Top electrode and lower electrode are equipped in container, the top electrode connects high frequency electric source with lower electrode.
The invention has the advantages that：
It is Ta powder used that the present invention using conventional use of tantalum powder suppresses capacitance as raw material, is alkalinous metal in reaction temperature
Fusing point more than, boiling point hereinafter, pressure be 700-45000Pa under conditions of, alkalinous metal is plasma-activated, after activation
Alkaline metal ions are reacted with the oxygen of tantalum core inner generates alkaline metal oxide, is finally discharged with inert gas, completes this hair
The bright deoxidation technique to anode tantalum core.The method of the present invention suppresses capacitor stage tantalum using conventional use of tantalum powder as raw material
Powder, need not using high-purity, the tantalum powder of low oxygen content, capacitance is Ta powder used suppressing, be greatly saved the purchases of raw material at
This, reduces buying difficulty；The present invention method using plasma activated basic metal activated after alkalinous metal from
Son accelerates the reaction speed of oxygen atom and alkaline metal ions, reduces the time of deoxidation process；Required for the present invention
Environment temperature be the fusing point of alkalinous metal or more, boiling point hereinafter, pressure is 700-45000Pa, reaction temperature is controlled in alkalinity
It is more than the fusing point of metal, boiling point hereinafter, alkalinous metal steam can be kept to evaporate, but will not boil, while plasma
Body discharges heat, can prevent alkalinous metal devaporation on the inner wall of equipment, improve the controllability and peace of production process
Quan Xing；The method of the present invention can be effectively reduced the oxygen concentration of tantalum core inner, improve the performances such as the pressure resistance of final tantalum capacitance.
Description of the drawings
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art are briefly described, it should be apparent that, in being described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, other drawings may also be obtained based on these drawings.
Fig. 1 is the result schematic diagram of the equipment provided by the invention for reducing anode tantalum core oxygen content；
Fig. 2 is the structural schematic diagram of sealing ring provided by the invention；
The structural schematic diagram of the positions Fig. 3 object carrying support provided by the invention.
Icon：1- metal material magnesium；2- containers；3- induction heaters；4- utilidors；5- cool-bags；6- imports；7-
Cover board；8- plasmas；9- high frequency electric sources；10- is exported；Electrode under 11-；12- top electrodes；13- tantalum cores；14- through-holes；15- drives
Lever；16- sealing rings；17- object carrying supports.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
The every other embodiment that personnel are obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that term "center", "upper", "lower", "left", "right", "vertical",
The orientation or positional relationship of the instructions such as "horizontal", "inner", "outside" be based on the orientation or positional relationship shown in the drawings, merely to
Convenient for the description present invention and simplify description, do not indicate or imply the indicated device or element must have a particular orientation,
With specific azimuth configuration and operation, therefore it is not considered as limiting the invention.In addition, term " first ", " second ",
" third " is used for description purposes only, and is not understood to indicate or imply relative importance.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
Can also be electrical connection to be mechanical connection；It can be directly connected, can also indirectly connected through an intermediary, Ke Yishi
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
According to an aspect of the present invention, the present invention provides a kind of methods reducing anode tantalum core oxygen content, including such as
Lower step：
(a) temperature more than the fusing point of alkalinous metal, boiling point hereinafter, pressure be 700-45000Pa under conditions of, will carry
The inert gas plasma of alkalinous metal steam forms the inert gas plasma containing alkalinous metal；
(b) tantalum core is placed in the inert gas plasma containing alkalinous metal, keeps the oxygen of tantalum in-core and alkalinous metal anti-
Alkaline metal oxide should be generated；
(c) alkalinous metal vapour source is isolated, is passed through inert gas, so that tantalum core is placed in inert gas plasma, make life
At alkaline metal oxide be discharged with inert gas.
It is Ta powder used that the present invention using conventional use of tantalum powder suppresses capacitance as raw material, is alkalinous metal in reaction temperature
Fusing point more than, boiling point hereinafter, pressure be 700-45000Pa under conditions of, alkalinous metal is plasma-activated, after activation
Alkaline metal ions are reacted with the oxygen of tantalum core inner generates alkaline metal oxide, is finally discharged with inert gas, completes this hair
The bright deoxidation technique to anode tantalum core.The method of the present invention suppresses capacitor stage tantalum using conventional use of tantalum powder as raw material
Powder, need not using high-purity, the tantalum powder of low oxygen content, capacitance is Ta powder used suppressing, be greatly saved the purchases of raw material at
This, reduces buying difficulty；The present invention method using plasma activated basic metal activated after alkalinous metal from
Son accelerates the reaction speed of oxygen atom and alkaline metal ions, reduces the time of deoxidation process；Required for the present invention
Environment temperature be the fusing point of alkalinous metal or more, boiling point hereinafter, pressure is 700-45000Pa, reaction temperature is controlled in alkalinity
It is more than the fusing point of metal, boiling point hereinafter, alkalinous metal steam can be kept to evaporate, but will not boil, while plasma
Body discharges heat, can prevent alkalinous metal devaporation on the inner wall of equipment, improve the controllability and peace of production process
Quan Xing；The method of the present invention can be effectively reduced the oxygen concentration of tantalum core inner, improve the performances such as the pressure resistance of final tantalum capacitance.
In one preferred embodiment, step (d) is carried out：Cooling system completes cooling.Deoxidation operation to tantalum core
It after completion, needs to lower the temperature of system, convenient for maintenance system and takes out tantalum core.
In one preferred embodiment, the alkalinous metal is selected from least one of magnesium, aluminium, calcium.
In a preferred embodiment, the alkalinous metal is magnesium, and temperature is 650-1000 DEG C, preferably 700-
950 DEG C, further preferably 750-900 DEG C；Pressure is 2000-35000Pa, under conditions of preferably 10000-20000Pa, energy
It is enough to guarantee that magnesium vapor is kept to evaporate, but will not boil, improve controllability and the safety of production process, pressure
It is too high or too low all be not easy to form plasma.
Optionally, temperature is 650 DEG C, 700 DEG C, 750 DEG C, 850 DEG C, 900 DEG C, 950 DEG C or 1000 DEG C.
Optionally, pressure 700Pa, 2000Pa, 4500Pa, 10000Pa, 15000Pa, 20000Pa, 35000Pa or
45000Pa。
In one preferred embodiment, the inert gas with alkalinous metal steam is by inert gas flow path
Alkalinous metal vapour source obtains, and the preferably described alkalinous metal vapour source is by heating alkalinous metal to fusing point liquid formed above
Body, and by evaporating to obtain.
In one preferred embodiment, the temperature of the inert gas is 650-1200 DEG C, preferably 750-1050
DEG C, further preferably 800-1000 DEG C.Inert gas is preheated to 650-1200 DEG C, reaction can be given to provide required temperature
Condition can prevent alkalinous metal devaporation on the inner wall of equipment.
Optionally, temperature is 650 DEG C, 750 DEG C, 800 DEG C, 900 DEG C, 1000 DEG C, 1050 DEG C, 1100 DEG C or 1200 DEG C.
In one preferred embodiment, the inert gas is argon gas.In inert gas, nitrogen is strictly not
It is inert gas, under activation, is easy to react to form nitrogen oxides with oxygen；Helium and neon price are somewhat expensive, in order to drop
Low cost does not use generally；Argon gas, it is cheap, it activates the lower property of lower effect and stablizes.
In one preferred embodiment, in the step (b), tantalum core is placed in the inert gas etc. containing alkalinous metal
Time in gas ions is 5-1000min, and preferably 50-800min, further preferably 200-600min make the oxygen of tantalum in-core
It is reacted with alkalinous metal and generates alkaline metal oxide.Anode tantalum core is suppressed with powder, if compacting is dense, is formed
Capacitance capacity it is smaller, effect it is more difficult, need the time acted on long；If the comparison of compacting is loose, the electricity of formation
The capacity of appearance is bigger, and effect is easier, and needs the time acted on shorter.
Optionally, the time is 5min, 50min, 200min, 400min, 500min, 600min, 800min, 900min
Or 1000min.
In one preferred embodiment, in the step (c), make tantalum core be placed in inert gas plasma when
Between be 1-100min, preferably 10-80min, further preferably 40-60min make the alkaline metal oxide of generation with inertia
Gas is discharged.
Optionally, the time is 1min, 10min, 40min, 50min, 60min, 80min or 100min.
In one preferred embodiment, the plasma is magnetized plasma；Preferably capacitive coupling etc. from
Daughter, inductively coupled plasma or magnetic field-enhanced CCP radio frequency plasmas.Magnetized plasma is different from high-temperature plasma
Body forms plasma under lower temperature, high frequency oscillation electromagnetic action, anode material will not be made to be denaturalized.
According to the second aspect of the invention, the present invention provides a kind of equipment reducing anode tantalum core oxygen content, including
One end of utilidor, the utilidor unicom cool-bag, the utilidor is equipped with import, the bottom of the cool-bag
Portion is equipped with outlet, is equipped with container and liftable cover board in the utilidor, the cover board is located at the top of container, the appearance
Device is equipped with induction heater, is equipped with top electrode and lower electrode in the cool-bag, the top electrode connects height with lower electrode
Frequency power.
The equipment provided by the invention for reducing anode tantalum core oxygen content, the course of work are：Metal material magnesium is placed on appearance
In device, magnesium material is molten by liquid by the induction heater of container surroundings.In the case where environment is low pressure, generates magnesium and steam
Gas.The high-purity argon gas being preheating to more than magnesium melting temperature is passed through from import, and when above flow path container, magnesium steam is brought by argon gas
In utilidor, and enter eventually into cool-bag.
In the center of cool-bag, by discharging between the top electrode and lower electrode of high frequency electric source, by the argon with magnesium steam
Gas is ionized into plasma.Tantalum core to be treated is placed on heating region.When tantalum core is by one section of corona treatment
Between after, the opening of container is closed by upper cover plate.After cover board is closed, plasma will no longer carry magnesium steam, in tantalum core
Magnesium and oxide will be diffused in argon plasma and be taken away by outlet.After pure argon venting process continues for some time,
Stop input argon gas, and close the high frequency electric source of plasma source, system gradually cools down, and completes cooling.
The equipment of the present invention, the equipment investment is few, and operating cost is low, reliable and stable, convenient operation and management.
It should be noted that being vertically equipped with drive rod on the cover board, the utilidor is equipped with through-hole, the driving
Bar passes through through-hole, and can be moved up and down in through-hole.Cover board moves down, and the opening of container is closed, plasma will not
Magnesium vapor is carried again；Cover board moves up, and the opening of container is opened, and magnesium vapor evaporates, and plasma can carry magnesium steaming
Gas.The setting of through-hole, is easy for installation and removal, and shaking is generated when can also cover board be avoided to move up and down.
It should be noted that the drive rod is driven by driving unit, the driving unit is manual actuation, hydraulic cylinder drive
Dynamic, pneumatic cylinder driving or motor driving.
It should also be noted that, being sealed by sealing structure between the through-hole and drive rod.The purpose of sealing is
In order to avoid the magnesium vapor in utilidor is reacted with extraneous oxygen.Preferably, the sealing structure is a sealing ring, described
Sealing ring is located in through-hole, and the drive rod is contacted with sealing ring.The structure of sealing ring is simple, and installation and removal are convenient, sealing
Effect is good.
It should also be noted that, can also be sealed by blowing argon gas, i.e. the contact position Argon in through-hole and drive rod
Gas passes through argon gas and extraneous oxygen-barrier.It should also be noted that, the lower electrode is equipped with object carrying support holder.Loading
For holder for placing tantalum core, tantalum core carries out deoxidation processing on object carrying support holder, and tantalum core and lower electrode is avoided to be in direct contact pair
Lower electrode damages.Object carrying support can be in direct contact with lower electrode, or be set on lower electrode by other support constructions.
It should also be noted that, the material of the object carrying support is heat-resisting material.The material of object carrying support can be but
It is not limited to the metals such as molybdenum, tungsten, tantalum.In order to contribute to the clearer understanding present invention, below in conjunction with embodiment and comparative example
Technical scheme of the present invention is described further.
Embodiment one
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 750 DEG C in temperature, under conditions of pressure is 10000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
800 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 2000Pa, by band
There is the argon plasma of magnesium steam, forms the argon plasma of the steam containing magnesium, plasma is capacitively coupled plasma；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 400min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 50min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
As shown in Figs. 1-3, the present embodiment additionally provides a kind of equipment reducing anode tantalum core oxygen content, including utilidor
4, one end of 4 unicom cool-bag 5 of insulating tube, utilidor 4 is equipped with import 6, and the bottom of cool-bag 5 is equipped with outlet 10,
Container 2 and liftable cover board 7 are equipped in utilidor 4, cover board 7 is located at the top of container 2, and being vertically equipped with one on cover board 7 drives
Lever 15, drive rod 15 passes through through-hole 14, and can be moved up and down in through-hole 14, by close between through-hole 14 and drive rod 15
Seal 16 is sealed, and sealing ring 16 is located in through-hole 14, and drive rod 15 is contacted with sealing ring 16, and container 2 is equipped with induction and adds
Hot device 3, cool-bag 5 is interior to be equipped with top electrode 12 and lower electrode 11, and lower electrode 11 is equipped with an object carrying support 17, object carrying support 17
Material be tantalum, top electrode 12 and lower electrode 11 connect high frequency electric source 9.
The equipment provided in this embodiment for reducing anode tantalum core oxygen content, the course of work are：Metal material magnesium 1 is placed on
In container 2, magnesium material is molten by liquid by heater 3.Manual actuation cover board 7 moves up, and the opening of container 2 is opened,
In the case where environment is low pressure, magnesium vapor is generated.The high-purity argon gas being preheating to more than magnesium melting temperature is passed through from import 6, is flowed
When the top of diameter container 2, magnesium steam is brought by argon gas in utilidor 4, and is entered eventually into cool-bag 5.
In the center of cool-bag 5, by capacitive coupling discharging between the top electrode 12 and lower electrode 11 of high frequency electric source 9,
Argon gas with magnesium steam is ionized into plasma 8.Tantalum core 13 to be treated is placed on object carrying support 17, and positioned at etc. from
Daughter region.Tantalum core 13 by corona treatment for a period of time after, manual actuation cover board 7 moves down, by the opening of container 2
It closes, after cover board 7 is closed, plasma will no longer carry magnesium steam, and the magnesium and oxide in tantalum core 13 will diffuse to argon gas etc.
It is taken away in gas ions and by outlet 10.After pure argon venting process continues for some time, stop input argon gas, and close etc. from
The high frequency electric source 9 in daughter source, system gradually cools down, and completes cooling.
Embodiment two
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 900 DEG C in temperature, under conditions of pressure is 20000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
1000 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 14000Pa, will
Argon plasma with magnesium steam forms the argon plasma of the steam containing magnesium, and plasma is inductive couple plasma
Body；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 200min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 60min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Embodiment three
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 650 DEG C in temperature, under conditions of pressure is 2000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
650 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 360Pa, by band
There is the argon plasma of magnesium steam, form the argon plasma of the steam containing magnesium, plasma is magnetic field-enhanced CCP radio frequencies etc.
Gas ions；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 600min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 40min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Example IV
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 850 DEG C in temperature, under conditions of pressure is 15000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
900 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 7800Pa, by band
There is the argon plasma of magnesium steam, forms the argon plasma of the steam containing magnesium, plasma is capacitively coupled plasma；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 500min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 80min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Embodiment five
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 950 DEG C in temperature, under conditions of pressure is 35000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
1050 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 25000Pa, will
Argon plasma with magnesium steam forms the argon plasma of the steam containing magnesium, and plasma is inductive couple plasma
Body；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 800min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 10min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Embodiment six
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 700 DEG C in temperature, under conditions of pressure is 4500Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
750 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 900Pa, by band
There is the argon plasma of magnesium steam, form the argon plasma of the steam containing magnesium, plasma is magnetic field-enhanced CCP radio frequencies etc.
Gas ions；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 1000min, make the oxygen and magnesium ion of tantalum in-core
Reaction generates magnesia；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 1min, make generation
Alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Embodiment seven
A kind of method reducing anode tantalum core oxygen content is present embodiments provided, is included the following steps：
(a) it is 1000 DEG C in temperature, under conditions of pressure is 45000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
1200 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 40000Pa, will
Argon plasma with magnesium steam, forms the argon plasma of the steam containing magnesium, and plasma is capacitive coupling plasma
Body；
(b) tantalum core is placed in the argon plasma of the steam containing magnesium and keeps 50min, keep the oxygen of tantalum in-core and magnesium ion anti-
Magnesia should be generated；
(c) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon plasma and keep 100min, make life
At alkaline metal oxide be discharged with inert gas；
(d) stop input argon gas, and close the high frequency electric source of plasma source, cooling system completes the deoxidation work of tantalum core
Skill operates.
Comparative example one
This comparative example provides a kind of method reducing anode tantalum core oxygen content, includes the following steps：
(a) it is 750 DEG C in temperature, under conditions of pressure is 10000Pa, heats magnesium material to obtain magnesium vapor, will be preheating to
800 DEG C of purity is more than the high-purity argon gas flow path magnesium vapour source of 5N, the wherein vapour pressure of magnesium steam generation about 2000Pa；
(c) tantalum core is placed in magnesium steam and keeps 400min；
(d) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon gas and keep 50min；
(d) stop input argon gas, cooling system completes the deoxidation technological operation of tantalum core.
Comparative example two
This comparative example provides a kind of method reducing anode tantalum core oxygen content, includes the following steps：
(a) in the case where temperature is 2000 DEG C, by the magnesium steam flow path tantalum core that pressure is 0.1Mpa；
(c) tantalum core is placed in magnesium steam and keeps 1000min；
(d) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon gas and keep 50min；
(d) stop input argon gas, cooling system completes the deoxidation technological operation of tantalum core.
Comparative example three
This comparative example provides a kind of method reducing anode tantalum core oxygen content, includes the following steps：
(a) in the case where temperature is 2000 DEG C, by the magnesium steam flow path tantalum core that pressure is 0.2Mpa；；
(c) tantalum core is placed in magnesium steam and keeps 400min；
(d) magnesium metal vapor source is isolated, is passed through argon gas, so that tantalum core is placed in argon gas and keep 50min；
(d) stop input argon gas, cooling system completes the deoxidation technological operation of tantalum core.
Comparative example four
It is handled without any technique.
The tantalum core that same batch produces is handled according to the method for each embodiment and comparative example respectively, with same after processing
Equipment and technique first complete completion under 1400 degree sintering, 2h is then completed under 0.02% phosphoric acid solution, 30V voltages
Chemical synthesis technology, finally carries out tantalum core electric performance test, and test result is as shown in table 1.
Tantalum core performance test result in each embodiment and comparative example is shown in Table 1.
1 tantalum core performance test result of table
As can be seen from the table, by the capacitance of present invention process treated tantalum core relative to comparative example four without any
Apparent variation does not occur for the capacitance for the tantalum core that technique is handled, but relative discharge stream has dropped, and breakdown voltage carries
Gao Liao, performance, which has, to be obviously improved.Wherein, by the capacitance of treated the tantalum core of the embodiment of the present invention one relative to comparative example four
The capacitance not apparent variation of generation without the tantalum core that any technique is handled, but relative discharge stream has dropped 40.6%,
Breakdown voltage improves 42.1%.Method in comparative example one does not carry out plasma processing to magnesium vapor, makes tantalum core and magnesium
Steam is directly reacted, and as a result shows that apparent variation does not occur for the capacitance of tantalum core, and relative discharge stream only declines 18.7%,
Breakdown voltage improves only 15.7%.Method in comparative example two does not carry out plasma processing to magnesium vapor, make tantalum core with
Magnesium vapor directly carries out high temperature, reacts for a long time, although relative discharge stream has dropped, breakdown voltage improves, and high temperature is anti-
The capacitance of tantalum core should be made to be obviously reduced.Method in comparative example three does not carry out plasma processing to magnesium vapor, makes tantalum core
High temperature, reaction under high pressure are directly carried out with magnesium vapor, although relative discharge stream has dropped, breakdown voltage improves, and high temperature is anti-
The capacitance of tantalum core should be made to be obviously reduced, and high temperature, height cause the manufacture difficulty of equipment higher, while being controlled in technique
It is highly difficult.
To sum up, method of the invention accelerates oxygen atom and alkalinous metal by plasma-activated alkaline metal ions
The reaction speed of ion reduces the time of deoxidation process；The method of the present invention is compared with previous conventional method, this hair
Bright required environment temperature and pressure are relatively low, improve controllability and the safety of production process；The method of the present invention can have
Effect ground reduces the oxygen concentration of tantalum core inner, improves the performances such as the pressure resistance of final tantalum capacitance.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of method reducing anode tantalum core oxygen content, which is characterized in that include the following steps：
(a) temperature more than the fusing point of alkalinous metal, boiling point hereinafter, pressure be 700-45000Pa under conditions of, will carry alkalinity
The inert gas plasma of metallic vapour forms the inert gas plasma containing alkalinous metal；
(b) tantalum core is placed in the inert gas plasma containing alkalinous metal, the oxygen of tantalum in-core is made to react life with alkalinous metal
At alkaline metal oxide；
(c) alkalinous metal vapour source is isolated, is passed through inert gas, so that tantalum core is placed in inert gas plasma, make generation
Alkaline metal oxide is discharged with inert gas；
Optional, carry out step (d)：Cooling system completes cooling.
2. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that the alkalinous metal is selected from
At least one of magnesium, aluminium, calcium, preferably magnesium.
3. the method according to claim 2 for reducing anode tantalum core oxygen content, which is characterized in that the temperature is 650-
1000 DEG C, preferably 700-950 DEG C, further preferably 750-900 DEG C；The pressure is 2000-35000Pa, preferably
10000-20000Pa。
4. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that described to carry alkalinous metal
The inert gas of steam is obtained by inert gas flow path alkalinous metal vapour source, and the preferably described alkalinous metal vapour source is logical
Heating alkalinous metal is crossed to fusing point liquid formed above, and by evaporating to obtain.
5. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that the temperature of the inert gas
Degree is 650-1200 DEG C, preferably 750-1050 DEG C, further preferably 800-1000 DEG C.
6. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that the inert gas is argon
Gas.
7. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that, will in the step (b)
Tantalum core is placed in the time in the inert gas plasma containing alkalinous metal for 5-1000min, preferably 50-800min, into one
Step is preferably 200-600min.
8. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that in the step (c), make
Tantalum core is placed in the time in inert gas plasma as 1-100min, preferably 10-80min, further preferably 40-
60min。
9. the method according to claim 1 for reducing anode tantalum core oxygen content, which is characterized in that the plasma is magnetic
Change plasma；Preferably capacitively coupled plasma, inductively coupled plasma or magnetic field-enhanced CCP radio frequency plasmas.
10. a kind of realizing that claim 1-9 any one of them reduces equipment used in the method for anode tantalum core oxygen content,
It is characterized in that, including utilidor, the utilidor unicom cool-bag, one end of the utilidor is equipped with import, institute
The bottom for stating cool-bag is equipped with outlet, and container and liftable cover board are equipped in the utilidor, and the cover board, which is located at, to be held
The top of device, the container are equipped with induction heater, top electrode and lower electrode, the top electrode are equipped in the cool-bag
High frequency electric source is connected with lower electrode.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110170651A (en) * | 2019-06-25 | 2019-08-27 | 江苏振华新云电子有限公司 | A kind of sintering method of sintering furnace and tantalum capacitor |
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| CN202954080U (en) * | 2012-12-05 | 2013-05-29 | 江门富祥电子材料有限公司 | Magnesium reduction and deoxygenation device of tantalum powder |
| CN203245360U (en) * | 2012-12-05 | 2013-10-23 | 江门富祥电子材料有限公司 | A device used for reducing tantalum powder by using magnesium to reduce oxygen content and provided with conic heat shields |
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| US6171363B1 (en) * | 1998-05-06 | 2001-01-09 | H. C. Starck, Inc. | Method for producing tantallum/niobium metal powders by the reduction of their oxides with gaseous magnesium |
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