CN206709595U - A kind of tantalum anode block malleation sintering equipment of batch (-type) - Google Patents
A kind of tantalum anode block malleation sintering equipment of batch (-type) Download PDFInfo
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- CN206709595U CN206709595U CN201720091582.8U CN201720091582U CN206709595U CN 206709595 U CN206709595 U CN 206709595U CN 201720091582 U CN201720091582 U CN 201720091582U CN 206709595 U CN206709595 U CN 206709595U
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- sintering
- tantalum
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Abstract
The utility model discloses a kind of tantalum anode block malleation sintering equipment of batch (-type), the device mainly includes sintering body of heater, vacuum system, temperature control system, argon gas protection system, electrical apparatus control system and cooling water recirculation system.When carrying out tantalum anode block high temperature positive sintering using the device, after first being vacuumized to body of heater, flowing high-purity argon gas is passed through again and keeps certain argon flow amount, tantalum anode block carries out high temperature positive sintering under the flowing argon atmosphere of certain pressure in stove, the properties of product gone out after sintering are stable, and this method effectively avoids anode block from being oxidized, and flow argon gas and greatly shorten anode block temperature fall time, energy consumption is saved, greatly improves production efficiency.
Description
Technical field
It the utility model is related to tantalum manufacture field, and in particular to a kind of malleation sintering equipment of tantalum anode block and sintering side
Method.
Background technology
Tantalum electric capacity full name is tantalum electrochemical capacitor, is succeeded in developing by AT＆T Labs of the U.S. within 1956, is widely used in automobile work
Industry, communication apparatus and military industry field.Tantalum electric capacity uses electrolyte as medium different from general electrolytic electric capacity, its medium be
One layer of very thin tantalum pentoxide film of metal tantalum Surface Creation, one end of this layer of oxide film dielectric and composition capacitor are combined into one
Individual entirety, it is impossible to individualism, form negative electrode；As wrapped tantalum metal derby and tantalum wire lead composition anode, referred to as tantalum
Anode block, tantalum anode block require that purity is high, and leakage current is small, and capacity is stable.
Tantalum powder manufacturer and tantalum capacitor manufacturing firm carry out tantalum anode block burning by the way of vacuum-sintering at present
Knot, this method is sintering furnace is reached the purpose of isolating oxygen by using vacuum equipment, and vacuum-sintering is to equipment and production environment
It is required that higher, its shortcoming is：(1) vacuum level requirements are high in sintering process in vertical vacuum furnace soon for tantalum anode, and technical difficulty is big,
Vacuum will at least reach 5.0X10 in vacuum drying oven-4Pa, it just can guarantee that tantalum anode block is not oxidized in sintering and insulating process
And the leakage rate of tantalum anode block and capacity reach certain requirement after sintering；(2) tantalum heating frame cooling down under vacuum conditions
Time is grown, low production efficiency, high energy consumption.
Utility model content
The technical problems to be solved in the utility model is：For current tantalum anode block in vacuum-sintering vacuum level requirements
Height, the problems such as tantalam heater temperature fall time is long, low production efficiency, there is provided a kind of tantalum anode block malleation sintering equipment of batch (-type),
Inert gas replacement can be completed under the relatively low requirement of vacuum, under malleation inert gas shielding, reach tantalum anode block sintering
It is required that while shorten the tantalum heating frame cooling down time, improve production efficiency, increase production capacity, save energy consumption.
To reach above-mentioned purpose, the utility model uses following technical scheme：
A kind of tantalum anode block malleation sintering equipment of batch (-type), the device mainly include one sintering body of heater, vacuum system,
Temperature control system, cooling water recirculation system, it is characterised in that also protect system containing argon gas.
Described sintering body of heater is vertical sintering furnace body.
Described argon gas protection system contains above argon inlet mouth and sintering body of heater below sintering body of heater
Argon gas exhaust outlet, described argon gas exhaust outlet are connected with negative-pressure damping device.
Negative-pressure damping device is made up of closed buffering empty bottle and the loosely capped vial equipped with liquid such as running water, and closed buffering is empty
Bottle volume >=running water loosely capped vial volume.When sintering furnace cools, due to the principle expanded with heat and contract with cold, negative pressure occurs in sintering furnace
Phenomenon, when argon flow amount is not enough to keep malleation in sintering furnace, it can cause occur negative pressure appearance in sintering furnace in very short time,
Now negative-pressure damping device is played a role, and the running water in loosely capped vial is sucked in closed buffering empty bottle, in closed buffering empty bottle
In argon gas suction sintering furnace, play a protective role.
Described cooling water recirculation system includes interior water cooling protection system and outer water cooling protection system；Described outer water cooling is protected
Protecting system is located at that sintering furnace is external, and described interior water cooling protection system is located in sintering furnace body.Cooling water recirculation system is used for protecting
Protect malleation sintering equipment.
It is sintering bell above described sintering body of heater, is vacuum drying oven interior room below sintering bell, vacuum drying oven interior room is fixed
In frame.
Specifically, sintering bell is fixed in vacuum drying oven interior room by clamping device, seals vacuum drying oven interior room.
Specifically, described sintering furnace interior room is from outside to inside containing interior water cooling protection system, inner casing tantalum heat screen, tantalum heating
Frame, and the hanging basket in tantalum heating frame.More specifically, described interior water cooling protection system is wrapped in inner casing tantalum heat screen,
The tantalum heating frame of suspension connection distribution system is protect in inner casing tantalum heat screen, is hung in tantalum heating frame and is placed with hanging basket.It is described
Hanging basket by under tantalum heat screen protection on hanging basket, placing tantalum anode block, hanging basket hung on tantalum heating frame by the horizontal bolt of hanging basket
Side is hung on tantalum heating frame by the horizontal bolt of hanging basket.
Flowmeter is provided with described frame, flowmeter connects argon gas exhaust outlet and negative-pressure damping device respectively.
Described vacuum system contains the vacuum-evacuate pipe below the vacuum drying oven interior room of sintering body of heater, described vacuum
Evacuation tube connects with vacuum drying oven interior room.On vacuum-evacuate pipe, vacuum gauge and the double pressure tables of air pressure are provided with.
In an embodiment of the present utility model, described argon inlet mouth is located above vacuum-evacuate pipe, with vacuum
Connected in furnace chamber.
In the preferred embodiment of utility model one, described argon gas exhaust outlet is located at below sintering furnace feed inlet and outlet flange
At 50mm, parallel to heater, to ensure that argon gas is enough to flood heater.
The malleation sintering equipment also contains distribution system and switch board, and switch board is used to control temperature control system and cooling to follow
Ring water system.
Described temperature control system contains thermocouple junction, thermocouple.
Described thermocouple junction is located above vacuum-evacuate pipe, and described thermocouple is located at vacuum drying oven interior room.
In the utility model preferred embodiment, the probe of described thermocouple is through annular tantalum heating frame side clearance
It is placed in and about at 1cm, to determine the sintering temperature of tantalum anode block, reflects the stove of sintering zone apart from annular tantalum heating frame inwall
Temperature, to adjust the temperature of sintering zone in time.Control for Kiln Temperature is directly connected to parameter specific volume size important in the production of tantalum electric capacity,
The height of sintering zone temperature can be ensured in the transition process that tantalum powder powder releases energy, and make to be formed in loose structure between particle
Contact surface increases, and the increase of briquetting intensity, keeps tantalum anode block capacitance.
Temperature control system adjusts the temperature of sintering furnace by thermocouple junction, thermocouple, tantalum heating frame, distribution system, switch board
Degree.
Tantalum anode block malleation sintering equipment of the present utility model, is first evacuated to gas to vacuum drying oven interior room using vacuum system
Pressure≤5.0 × 10-2Pa, stop vacuumizing, then be passed through high-purity argon gas, the double pressure tables of observation air pressure, reach malleation to vacuum drying oven interior room,
Operational control cabinet while holding high-purity argon gas circulation, is burnt by tantalum heating frame to compressing tantalum anode block
Knot.Specifically, the tantalum anode block malleation sintering step is：
(1) first the tantalum anode block that the tantalum powder pressed compact of capacitor stage shapes is inserted in tantalum sintering furnace, tantalum powder specific volume is 17000 μ
The μ FV/g of FV/g~70000；
(2) sintering body of heater is carried out being evacuated to vacuum≤5.0 × 10-2Pa using vavuum pump；
(3) circulate high-purity argon gas to body of heater, maintains furnace pressure in+0.01Mpa~+0.03Mpa；
(4) under the conditions of cooling water circulation, tantalum anode block is subjected to high temperature sintering at a temperature of 1100 DEG C~1600 DEG C
5min~30min；
(5) less than 35 degrees Celsius are cooled in the case where flowing argon gas after terminating to come out of the stove.
The purity of argon gas is 99.999%.
The beneficial effect that malleation sintering equipment of the present utility model obtains：
1) production cycle is shortened：First in tantalum anode block sintering art, for anode block of tantalum capacitor vacuum-sintering process
In easily be oxidized and sintering temperature fall time it is long the problem of, research and develop a kind of batch (-type) tantalum anode block malleation sintering equipment and should
With, the device is easy to operate, and the properties of product sintered out are reliable and stable, and sinter temperature fall time be vacuum-sintering half even more
It is few, the production cycle is greatly shortened, improves production and conventional efficient.
2) good electric property：The tantalum that the tantalum anode block that argon gas positive pressure sintering equipment sinters out sinters out with vaccum sintering device
For anode block in capacitance, leakage current and breakdown voltage without significant difference, disclosure satisfy that can tantalum capacitor anode core performance requirements.
3) after malleation sintering, tantalum anode block purity is high.
Brief description of the drawings
The schematic diagram of tantalum anode block malleation sintering equipment in Fig. 1 the utility model embodiments 1
Schema explanation
1. sinter bell, 2. outer water coolings protection systems, 3. distribution systems, water cooling protects system, 5. vacuum gauges, 6. in 4.
Thermocouple junction, 7. argon inlet mouths, 8. vacuum-evacuate pipes, tantalum heat screen, the horizontal bolt of 10. hanging baskets, the exhaust of 11. argon gas on 9. hanging baskets
Mouth, 12. inner casing tantalum heat screens, 13. tantalum heating frames, 14. thermocouples, 15. tantalum anode blocks, 16. hanging baskets, 17. switch boards, 18. folders
The double pressure tables of tight device, 19. air pressure, 20. flowmeters, 21. negative-pressure damping devices, 22. vacuum drying oven interior rooms, 23. frames
Embodiment
The technical solution of the utility model is further illustrated below by way of specific embodiment, specific embodiment does not represent pair
The limitation of scope of protection of the utility model.Some nonessential modifications and tune that other people are made according to the utility model theory
It is whole to still fall within the scope of protection of the utility model.
A kind of tantalum anode block malleation sintering equipment of 1 batch (-type) of embodiment
Tantalum anode block malleation sintering equipment as shown in Figure 1, described sintering equipment contain vertical sintering furnace body.
The top of vertical sintering furnace body is sintering bell 1, and the sintering lower chamber of bell 1 is vacuum drying oven interior room 22, sintering furnace
Lid 1 is fixed in vacuum drying oven interior room 22 by clamping device 18.Vacuum drying oven interior room 22 is arranged in frame 23, and frame is built with stream
Gauge 20, flowmeter 20 connect argon gas exhaust outlet 11 and negative-pressure damping device 21 respectively.Vacuum drying oven interior room 22 is from outside to inside successively
Protect system 4, inner casing tantalum heat screen 12, tantalum heating frame 13 and hanging basket 16, hanging basket 16 heat-insulated by tantalum on hanging basket for interior water cooling
Shield 9 protection downs and put tantalum anode block 15, hanging basket 16 hangs on the top of tantalum heating frame 13, thermocouple junction 6 by the horizontal bolt 10 of hanging basket
Thermocouple 14 is drawn through interior water cooling protection system 4, inner casing tantalum heat screen 12, is fixed in tantalum heating frame 13.
Sintering equipment reaches protection sintering bell 1, vacuum drying oven interior room 22, distribution system 3 by cooling water recirculation system
Effect.Cooling water recirculation system includes outer water cooling protection system 2 and interior water cooling protection system 4.
Sintering equipment also contains vacuum system.Vacuum system contains the vacuum-evacuate pipe 8 below sintering body of heater, described
Vacuum-evacuate pipe 8 be connected with vacuum drying oven interior room 22.On vacuum-evacuate pipe 8, be provided with vacuum gauge 5, thermocouple junction 6,
Argon inlet mouth 7 and the double pressure tables 19 of air pressure.
Sintering equipment also contains argon inlet mouth 7 and argon gas exhaust outlet 11 containing argon gas protection system, argon gas protection system.
Argon inlet mouth 7 and argon gas exhaust outlet 11 connect with vacuum drying oven interior room 22.
Argon gas exhaust outlet is connected with negative-pressure damping device 21.Negative-pressure damping device 21 is by closed buffering empty bottle and equipped with originally
The loosely capped vial composition of aqueous, closed buffering empty bottle volume >=running water loosely capped vial volume.
Described sintering equipment also contains temperature control system, and described temperature control system contains thermocouple junction 6 and thermocouple 14.
Thermocouple junction 6 is located on vacuum-evacuate pipe, and the probe of thermocouple 14 is placed in rang ring through annular tantalum heating frame side clearance
The inwall of shape tantalum heating frame 13 is about at 1cm.Temperature control system passes through thermocouple junction 6, thermocouple 14, tantalum heating frame 13, distribution system 3
Completed with switch board 17.
Embodiment 2 uses the sintering method of the tantalum anode block malleation sintering equipment of batch (-type)
Tantalum powder pressed compact that specific volume is 17000 μ FV/g is protected into system 2 and interior water cooling into after tantalum anode block, opening outer water cooling
Protection system 4, sintering bell 1 is opened, extracts the horizontal bolt 10 of hanging basket, hanging basket 16 is proposed, evenly distributed be put into of tantalum anode block 15 is hung
In basket 16, hanging basket 16 is hung in tantalum heating frame 13 in the case where ensureing to insulate, covers heat screen 9 on hanging basket, insertion is hung
The horizontal bolt 10 of basket, covers sintering furnace bell 1, loads onto clamping device 18 and fixes bell 1 and vacuum drying oven interior room 22, closes argon inlet
Mouth 7 and argon gas exhaust outlet 11, open vacuum valve and connect vavuum pump with vacuum-evacuate pipe 8, pass through electrical control cubicles 17 and open vacuum
Pump evacuates to vacuum drying oven interior room 22, under the measure of vacuum gauge 5, when air pressure≤4.0 × 10 of vacuum drying oven interior room 22-2Pa
When, close vacuum valve and stop evacuating vacuum interior room 22, open the valve of argon inlet mouth 7, be passed through high-purity argon gas, observe gas
The double pressure tables 19 of pressure, when pointer is 0 on the double pressure tables 19 of air pressure, the valve of argon inlet mouth 7 is closed, opens vacuum valve by vavuum pump
Connected with vacuum tube 8, open vavuum pump by electrical control cubicles 17 is evacuated displacement again to vacuum drying oven interior room 22, continuously replaces three
After secondary, the valve of argon inlet mouth 7 is kept, the valve of argon gas exhaust outlet 11 is opened, vacuum drying oven is controlled by adjusting flowmeter 20
Air pressure in interior room 22 is that pressure-fired is+0.02Mpa, passes through switch board 17, the height at 1500 DEG C to tantalum anode block of distribution system 3
Temperature sintering 10mins, comes out of the stove after terminating after carrying out being cooled to 35 degree under flowing argon gas.
Embodiment 3 uses the sintering method of the tantalum anode block malleation sintering equipment of batch (-type)
By tantalum powder pressed compact that specific volume is 40000 μ FV/g into tantalum sintering furnace is inserted after tantalum anode block, remaining presses the step of case study on implementation 2,
By tantalum anode block at 1400 DEG C high temperature sintering 10mins, come out of the stove after terminating after carrying out being cooled to 35 degree under flowing argon gas.
Embodiment 4 uses the sintering method of the tantalum anode block malleation sintering equipment of batch (-type)
By tantalum powder pressed compact that specific volume is 70000 μ FV/g into tantalum sintering furnace is inserted after tantalum anode block, remaining presses case study on implementation 2
Step, by tantalum anode block at 1320 DEG C high temperature sintering 10mins, carry out in the case where flowing argon gas being cooled to 35 degree after terminating
After come out of the stove.
The vacuum-sintering of comparative example 1
By tantalum powder pressed compact that specific volume is 17000 μ FV/g into inserting tantalum sintering furnace after tantalum anode block,
Sintering body of heater is vacuumized using vavuum pump, when in stove vacuum up to 3.0 × 10-4After Pa,
By tantalum anode block at 1500 DEG C high temperature sintering 10mins, to coming out of the stove after 35 degree under natural cooling after terminating.
The vacuum-sintering of comparative example 2
By tantalum powder pressed compact that specific volume is 40000 μ FV/g into inserting tantalum sintering furnace after tantalum anode block,
Sintering body of heater is vacuumized using vavuum pump, when in stove vacuum up to 3.0 × 10-4After Pa,
By tantalum anode block at 1400 DEG C high temperature sintering 10mins, to coming out of the stove after 35 degree under natural cooling after terminating.
The vacuum-sintering of comparative example 3
By tantalum powder pressed compact that specific volume is 70000 μ FV/g into inserting tantalum sintering furnace after tantalum anode block,
Sintering body of heater is vacuumized using vavuum pump, when in stove vacuum up to 3.0 × 10-4After Pa,
By tantalum anode block at 1320 DEG C high temperature sintering 10mins, to coming out of the stove after 35 degree under natural cooling after terminating.
The performance measurement of the tantalum anode block of embodiment 5
To embodiment 2-4, the performance of the tantalum anode block after comparative example 1-3 sintering is measured：Include N, O, H analysis and electricity
Performance (capacitance, leakage current, breakdown voltage).
N is analyzed：With reference to the measure of nitrogen quantity in GB/T15076.13 tantalum niobium chemical analysis method tantalums
O is analyzed：With reference to the measure of oxygen amount in GB/T15076.14 tantalum niobium chemical analysis method tantalums
H is analyzed：With reference to the measure of hydrogen amount in GB/T15076.15 tantalum niobium chemical analysis method tantalums
Electrical property determines：With reference to the tantalum powder for capacitor electrical property detection methods of GB/T 3137
Analysis result is shown in Table -1 table 3
The embodiment 2 of table 1 and the sintered anode block performance comparison of comparative example 1
The embodiment 3 of table 2 and the sintered anode block performance comparison of comparative example 2
The embodiment 4 of table 3 and the sintered anode block performance comparison of comparative example 3
From table 1- tables 3, the tantalum anode block of malleation sintering is carried out using malleation sintering equipment of the present utility model,
(1) tantalum anode block content without significant difference, illustrates that this practicality is new after O, N, H content and vacuum-sintering in tantalum anode block
The argon gas stream malleation sintering protecting effect of type device is preferable.
(2) electrical property such as tantalum anode block leakage current, loss, capacity, breakdown voltage value and vacuum-sintering tantalum anode block are without bright
Significant difference is other, can meet tantalum capacitor anode core performance requirements.
(3) malleation sintering total time is only half even following, the utility model device pole that vacuum-sintering needs the time
Big reduces sintering time, saves energy consumption, improves efficiency.
Claims (10)
1. a kind of tantalum anode block malleation sintering equipment, described device includes sintering body of heater, vacuum system, temperature control system, cooling
Water circulation system, it is characterised in that also protect system containing argon gas；
Described argon gas protection system contains argon inlet mouth and argon gas exhaust outlet on sintering body of heater；
Described cooling water recirculation system includes interior water cooling protection system and outer water cooling protection system；Described outer water cooling protection system
System is external positioned at sintering furnace, and interior water cooling protection system is located in sintering furnace body；
It is sintering bell above the sintering body of heater, is vacuum drying oven interior room below sintering bell, is frame below vacuum drying oven interior room；
Described sintering bell is fixed in vacuum drying oven interior room by clamping device；
The sintering furnace interior room is from outside to inside successively containing interior water cooling protection system, inner casing tantalum heat screen, tantalum heating frame and hanging basket；
Flowmeter is provided with described frame.
2. sintering equipment according to claim 1, it is characterised in that described argon gas protection system also buffers containing negative pressure
Device, described negative-pressure damping device connect with argon gas exhaust outlet.
3. sintering equipment according to claim 2, it is characterised in that it is empty that described negative-pressure damping device contains closed buffering
Bottle and the loosely capped vial being connected with closed surge flask；Further, closed buffering empty bottle volume >=running water loosely capped vial volume.
4. sintering equipment according to claim 1, it is characterised in that described vacuum system contains positioned at sintering body of heater
Vacuum-evacuate pipe below vacuum drying oven interior room, and the double pressure tables of vacuum gauge, air pressure on vacuum-evacuate pipe.
5. sintering equipment according to claim 4, it is characterised in that described argon inlet mouth is located at vacuum-evacuate pipe
On.
6. sintering equipment according to claim 1, it is characterised in that described argon gas exhaust outlet is positioned at sintering body of heater disengaging
Below material mouth flange at 50mm.
7. sintering equipment according to claim 4, it is characterised in that the temperature control system contains thermocouple junction, thermoelectricity
It is even.
8. sintering equipment according to claim 7, it is characterised in that described thermocouple junction is located on vacuum-evacuate pipe
Side.
9. sintering equipment according to claim 7, it is characterised in that the probe of described thermocouple is through tantalum heating frame side
Face, it is placed in apart from annular tantalum heating frame inwall about at 1cm.
10. sintering equipment according to claim 1, it is characterised in that also containing distribution system and switch board.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201720091582.8U CN206709595U (en) | 2017-01-22 | 2017-01-22 | A kind of tantalum anode block malleation sintering equipment of batch (-type) |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201720091582.8U CN206709595U (en) | 2017-01-22 | 2017-01-22 | A kind of tantalum anode block malleation sintering equipment of batch (-type) |
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| CN206709595U true CN206709595U (en) | 2017-12-05 |
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| CN201720091582.8U Withdrawn - After Issue CN206709595U (en) | 2017-01-22 | 2017-01-22 | A kind of tantalum anode block malleation sintering equipment of batch (-type) |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106643126A (en) * | 2017-01-22 | 2017-05-10 | 江门富祥电子材料有限公司 | Intermittent type positive pressing sintering device for tantalum anode block and sintering method |
| CN110734778A (en) * | 2019-11-12 | 2020-01-31 | 佛山科学技术学院 | organic matter microwave pyrolysis carbonization device |
-
2017
- 2017-01-22 CN CN201720091582.8U patent/CN206709595U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106643126A (en) * | 2017-01-22 | 2017-05-10 | 江门富祥电子材料有限公司 | Intermittent type positive pressing sintering device for tantalum anode block and sintering method |
| CN106643126B (en) * | 2017-01-22 | 2022-10-21 | 江门富祥电子材料有限公司 | Intermittent positive pressure sintering device and method for tantalum anode block |
| CN110734778A (en) * | 2019-11-12 | 2020-01-31 | 佛山科学技术学院 | organic matter microwave pyrolysis carbonization device |
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Granted publication date: 20171205 Effective date of abandoning: 20190403 |
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