CN204430275U - Oxygen device falls in a kind of novel tantalum powder magnesium-reduced - Google Patents
Oxygen device falls in a kind of novel tantalum powder magnesium-reduced Download PDFInfo
- Publication number
- CN204430275U CN204430275U CN201420777210.7U CN201420777210U CN204430275U CN 204430275 U CN204430275 U CN 204430275U CN 201420777210 U CN201420777210 U CN 201420777210U CN 204430275 U CN204430275 U CN 204430275U
- Authority
- CN
- China
- Prior art keywords
- reaction vessel
- tantalum powder
- thermocouples
- reduced
- magnesium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The utility model relates to the magnesium-reduced of a kind of novel tantalum powder and falls oxygen device.Comprise reaction vessel body (10) and reaction vessel lid (11), be characterized in: on described reaction vessel lid (11), have through hole, also comprise a thermocouples tube (14), one end of this thermocouples tube (14) is passed and is stretched into reaction vessel body (10) bottom from this through hole, is inserted with at least 3 armouring thermocouples (20) in this thermocouples tube (14).Device of the present utility model changes thermometric mode, improves the accuracy of thermometric, reduces the difficulty of shove charge, adds reactor dischargeable capacity, can expand the magnesium-reduced of tantalum powder and fall oxygen list stove batch, reduces production cost.The temperature-measuring heat couple structure of the utility model device is simple, and on original device basic, transformation can be implemented a little, carries out the magnesium-reduced of tantalum powder fall oxygen according to the utility model device, and thermometric is more accurate, and shove charge is convenient, expands batch, reduces production cost.
Description
Technical field
The utility model relates to the magnesium-reduced of a kind of novel tantalum powder and falls oxygen device.
Background technology
Tantalum metal is a kind of rare precious metal, and its important use makes electrolytic capacitor.Tantalum powder as capacitor requires very high purity.That production Ta powder used in capacitor adopts usually is potassium floutaramite (K
2taF
7) sodium reduction method obtains former powder, then carrying out vacuum heat, just reaching the requirement for making electrolytic capacitor.But having very large affinity due to tantalum metal pair oxygen, the tantalum powder obtained through above-mentioned operation is often containing very high oxygen, and this is very disadvantageous for making electrolytic capacitor, and condenser leakage current can be caused high, and proof voltage is poor, so must carry out falling oxygen process.
The oxygen process of falling of tantalum powder generally adopts magnesium-reduced to carry out falling oxygen process, and its reaction unit used generally all adopts device as shown in Figure 1.And separately have some devices to be on the basis of accompanying drawing 1, in the middle of heat screen, add a magnesium collecting device.These devices have a common feature, cover exactly be provided with 3 ~ 4 thermocouples tubes at reaction vessel, and are that the fixing reaction vessel that is welded on covers.Like this, in order to slot milling, to ensure that 3 ~ 4 thermocouples tubes can load in reaction vessel smoothly, the size reducing dress tantalum powder crucible and bin of just having a mind to, if add in some reaction unit the argon inlet pipe stretched at the bottom of bullet, just more reduce the size of dress tantalum powder crucible and bin, thus the batch of single heat is reduced, add production cost.Simultaneously in the process of carrying out shove charge, especially after bullet lid employs many stoves, thermocouples tube very easily occurs bending and deformation in shove charge or put procedure, thus the bin rubbed in reaction bullet, bullet lid is caused not confine, gas leakage waits shove charge difficulty, even can play on wall and the problem such as cause thermometric inaccurate because thermocouples tube abuts against.
Utility model content
The purpose of this utility model is to provide the magnesium-reduced of a kind of novel tantalum powder and falls oxygen device, can improve the accuracy of thermometric, reduces the difficulty of shove charge simultaneously and adds reactor dischargeable capacity.
Oxygen device falls in a kind of novel tantalum powder magnesium-reduced, comprise reaction vessel body and reaction vessel lid, its special feature is: cover at described reaction vessel and have through hole, also comprise a thermocouples tube, one end of this thermocouples tube is passed and stretches into reaction vessel body bottom portion from this through hole, is inserted with at least 3 armouring thermocouples in this thermocouples tube.
Wherein armouring thermocouple has 3, and its respective thermometric end is distributed on the position, three, upper, middle and lower of reaction vessel body successively.
Wherein thermocouples tube adopts internal diameter to be the stainless steel tube of 10-30mm, this stainless steel tube wall thickness 3-10mm and lower end closed.
Wherein cover at reaction vessel and also have 2 through holes, in these 2 through holes, be inserted with argon gas respectively enter pipe and gas outlet pipe.
The through hole side wherein covered at reaction vessel is provided with a lower flange, and at thermocouples tube outer also fixed cover, a upper flange plate is housed, between this lower flange and upper flange plate, be provided with seal, thus coordinate by flange and thermocouples tube is detachably arranged on reaction vessel covers.
The lower flange side wherein covered at reaction vessel is provided with cooling jacket, thus can coolant seal part.
Through probationary certificate, device of the present utility model changes thermometric mode, improves the accuracy of thermometric, reduces the difficulty of shove charge, adds reactor dischargeable capacity, can expand the magnesium-reduced of tantalum powder and fall oxygen list stove batch, reduces production cost.Other beneficial effect is as follows: the temperature-measuring heat couple structure of the utility model device is simple, on original device basic, transformation can be implemented a little, in general, carry out the magnesium-reduced of tantalum powder according to the utility model device and fall oxygen, thermometric is more accurate, shove charge is convenient, expands batch, reduces production cost.
Accompanying drawing explanation
Accompanying drawing 1 is the structural representation for the treatment of apparatus in the utility model background technology;
Accompanying drawing 2 is structural representation of the present utility model;
Accompanying drawing 3 is the structural representation of thermocouples tube 14 part in the utility model.
Detailed description of the invention
As shown in Figure 2,3, the utility model is that oxygen device falls in the magnesium-reduced of a kind of novel tantalum powder, comprise reaction vessel body 10 and reaction vessel lid 11, described reaction vessel lid 11 has through hole, also comprise a thermocouples tube 14, one end of this thermocouples tube 14 is passed and is stretched into bottom reaction vessel body 10 from this through hole, is inserted with at least 3 armouring thermocouples 20 (i.e. thermocouple also can be armored temperature measuring thermocouple) in this thermocouples tube 14.On reaction vessel lid 11, also have 2 through holes in addition, in these 2 through holes, be inserted with argon gas respectively enter pipe 12 and gas outlet pipe 13.
Wherein armouring thermocouple 20 has 3, and its respective thermometric end is distributed on the position, three, upper, middle and lower of reaction vessel body 10 successively.In addition particular/special requirement be there is no to thermocouples tube 14 material, thermocouples tube material of the prior art can be used, the material of yet optional energy resistance to high temperature oxidation and corrosion; The internal-and external diameter of thermocouples tube is not particularly limited, and preferred internal diameter is the stainless steel tube of 10-30mm, wall thickness 3-10mm, lower end closed.
Through hole wherein on reaction vessel lid 11 is other is provided with a lower flange, and at thermocouples tube 14 outer also fixed cover, a upper flange plate is housed, this lower flange and between be provided with seal, thus by flange coordinate thermocouples tube 14 is detachably arranged on reaction vessel lid 11.Lower flange in addition on reaction vessel lid 11 is other is provided with cooling jacket, thus can coolant seal part.
The utility model comprises reaction vessel body 10, uses seal and reaction vessel to carry out the reaction vessel lid 11 sealed, and crucible and the bin 15 of tantalum powder are housed.Reaction vessel lid 11 is provided with some through holes, be respectively equipped with argon gas in through hole and enter pipe 12, gas outlet pipe 13, thermocouples tube 14, the length of thermocouples tube 14 has no particular limits, but in order to the accuracy of reaction vessel upper, middle and lower thermometric, is stretched into by thermocouples tube 14 bottom reaction bullet as far as possible.In order to not affect upper, middle and lower segment thermometric, even four sections of thermometrics, the utility model uses the armouring thermocouple 20 of three or four sealings of different length according to the position of different point for measuring temperature, and their height according to different point for measuring temperature are fixed together, then be inserted in thermocouples tube 14, achieve the object of multi-point temperature measurement so equally.
In order to the accuracy of shove charge and thermometric more can be convenient to, the utility model is connected adopting between thermocouples tube 14 with reaction vessel lid 11 to live, like this when shove charge first by reaction vessel lid 11 to covering well, then will be inserted with in the thermocouples tube 14 intercalation reaction container cover 11 of the several armouring thermocouples 20 fixed, confine sealing; When coming out of the stove, first thermocouples tube 14 is taken out, then uncap again and come out of the stove, such thermocouples tube 14 would not become curved, thus also can not rub bullet wall, thus thermometric is more accurate, go out shove charge also convenient, simultaneously owing to being the independent thermocouples tube 14 of employing 1, and adopt the rear thermocouples tube 14 of connection of living should not become curved, be thus just that the space that thermocouples tube 14 is reserved reduces further in the size designing dress tantalum powder crucible and bin 15, namely increase the size filling tantalum powder crucible and bin 15 as much as possible, improve the batch of single heat, reduce production cost.
Clear and definite restriction is not had for connected mode, can adopt lives connects, namely a ring flange is welded with according to 20 ~ 50mm place above described thermocouples tube 14, then on thermocouples tube 14 through hole of reaction vessel lid 11 correspondence, be welded with a ring flange according to bullet lid 50 ~ 80mm place, in order to prevent seal between two ring flanges by scalding, below the ring flange of bullet lid, be provided with cooling jacket.
Device of the present utility model also can be used in the middle reduction equi-index plate solid-solid reaction of niobium monoxide powder of Chinese patent " preparation method of low valence niobium oxide or niobium powder " (patent No. ZL200710145183.6) or the method for hydrogen reduction.
As shown in Figure 1, cover the thermocouples tube of fixing welding 3 ~ 4 differing heights at reaction vessel in prior art, only a thermocouple is installed in each thermocouples tube, like this in the process of carrying out shove charge, especially after reaction vessel lid employs many stoves, thermocouples tube very easily occurs bending and deformation in shove charge or put procedure, thus the bin rubbed in reaction bullet, bullet lid is caused not confine, gas leakage waits shove charge difficulty, even can play on wall and the problem such as cause thermometric inaccurate because thermocouples tube abuts against, make the batch of single heat reduce simultaneously, add production cost.
Be that oxygen modifying device falls in tantalum powder of the present utility model magnesium-reduced as shown in Figure 3, it mainly comprises reaction vessel body 10, has no particular limits the size of reaction vessel body 10, and generally its internal diameter is 40 ~ 150cm; Reaction vessel lid 11, reaction vessel lid 11 is provided with some through holes, be respectively equipped with in through hole that argon gas enters pipe 12, gas outlet pipe 13, marginal position on reaction vessel lid 11 are provided with thermocouples tube 14, the length of thermocouples tube 14 has no particular limits, as preferably, thermocouples tube 14 reaches the bottom of reaction vessel as far as possible, thermocouples tube 14 be provided with seal (adopting flange seal to be connected) between through hole; 3 the armouring thermocouples 20 fixed, in order to the temperature at bin 15 upper, middle and lower three positions in assaying reaction container.
Using method of the present utility model is:
When carrying out the magnesium-reduced of tantalum powder and falling oxygen, the hyperoxia tantalum powder 17 being mixed with magnesium powder is loaded tantalum crucible 16 li, tantalum crucible 16 is placed on bin 15, then the bin 15 that tantalum powder crucible is housed is loaded the bottom of the reaction vessel body 10 of drum type brake, then reaction vessel lid 11 to be covered on reaction vessel body 10 and to tighting a bolt well, again by thermocouples tube 14 by the respective through hole intercalation reaction vessel 10 of reaction vessel lid 11, and sealing tight a bolt.
To install and the reaction vessel body 10 of finding time to have replaced as shaft furnace 18 li, its pallet 19 is sitting on shaft furnace 18.Then fix three or four armouring thermocouples 20 are inserted in thermocouples tube 14, and correspondence is received on temperature-controlling system, then heat to 700 ~ 1000 DEG C of insulations 2 to 5 hours, cool to room temperature after finding time 1-5 hour, come out of the stove after passivation, after pickling vacuum drying, be reduced the tantalum powder of oxygen.
Claims (6)
1. oxygen device falls in novel tantalum powder magnesium-reduced, comprise reaction vessel body (10) and reaction vessel lid (11), it is characterized in that: on described reaction vessel lid (11), have through hole, also comprise a thermocouples tube (14), one end of this thermocouples tube (14) is passed and is stretched into reaction vessel body (10) bottom from this through hole, is inserted with at least 3 armouring thermocouples (20) in this thermocouples tube (14).
2. oxygen device falls in a kind of novel tantalum powder as claimed in claim 1 magnesium-reduced, it is characterized in that: wherein armouring thermocouple (20) has 3, and its respective thermometric end is distributed on the position, three, upper, middle and lower of reaction vessel body (10) successively.
3. oxygen device falls in a kind of novel tantalum powder as claimed in claim 1 magnesium-reduced, it is characterized in that: wherein thermocouples tube (14) adopts internal diameter to be the stainless steel tube of 10-30mm, this stainless steel tube wall thickness 3-10mm and lower end closed.
4. oxygen device falls in a kind of novel tantalum powder as claimed in claim 1 magnesium-reduced, it is characterized in that: wherein on reaction vessel lid (11), also have 2 through holes, in these 2 through holes, be inserted with argon gas respectively enter pipe (12) and gas outlet pipe (13).
5. oxygen device falls in tantalum powder as novel in the one in Claims 1-4 as described in any one magnesium-reduced, it is characterized in that: the through hole wherein on reaction vessel lid (11) is other is provided with a lower flange, and thermocouples tube (14) outward also fixed cover a upper flange plate is housed, between this lower flange and upper flange plate, be provided with seal, thus by flange cooperation, thermocouples tube (14) be detachably arranged on reaction vessel lid (11).
6. oxygen device falls in a kind of novel tantalum powder as claimed in claim 5 magnesium-reduced, it is characterized in that: the lower flange wherein on reaction vessel lid (11) is other is provided with cooling jacket, thus can coolant seal part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420777210.7U CN204430275U (en) | 2014-12-10 | 2014-12-10 | Oxygen device falls in a kind of novel tantalum powder magnesium-reduced |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201420777210.7U CN204430275U (en) | 2014-12-10 | 2014-12-10 | Oxygen device falls in a kind of novel tantalum powder magnesium-reduced |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN204430275U true CN204430275U (en) | 2015-07-01 |
Family
ID=53598195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201420777210.7U Active CN204430275U (en) | 2014-12-10 | 2014-12-10 | Oxygen device falls in a kind of novel tantalum powder magnesium-reduced |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN204430275U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052329A (en) * | 2017-05-18 | 2017-08-18 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
-
2014
- 2014-12-10 CN CN201420777210.7U patent/CN204430275U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052329A (en) * | 2017-05-18 | 2017-08-18 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
| CN107052329B (en) * | 2017-05-18 | 2019-08-23 | 江门富祥电子材料有限公司 | A kind of heat treatment method of tantalum powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109084834B (en) | Liquid level and temperature measuring device suitable for titanium sponge reduction reaction | |
| CN103728353B (en) | A kind of sealing high-temperature electrochemistry measurement mechanism | |
| CN204430275U (en) | Oxygen device falls in a kind of novel tantalum powder magnesium-reduced | |
| CN104316439A (en) | Device and method for determining rheological properties of high-temperature metallurgy molten slag | |
| CN105080427B (en) | A kind of HTHP water-cooled can weigh reactor | |
| CN103076820B (en) | A kind of experimental provision being applicable to realize solid phase oxygen control reaction | |
| CN106477618B (en) | A kind of fused salt solid solution and preparation method thereof and preparation facilities | |
| CN104388688B (en) | A kind of device and method of vacuum metal thermal reduction refining lithium | |
| CN202814851U (en) | Magnesium chloride stress corrosion test device for stainless steel test piece | |
| CN106338458A (en) | High-temperature melt surface tension measuring device and measuring method | |
| CN202599779U (en) | Iron ore reduction, pulverization and expansion metallurgy properties test device | |
| CN203807170U (en) | Device for preparing manganese nitride by performing microwave heating on MnO2 | |
| CN204281823U (en) | A kind of device of vacuum metal thermal reduction refining lithium | |
| CN204544169U (en) | Multipurpose microwave chemosynthesis instrument | |
| CN201653555U (en) | Infrared temperature measuring gun of AOD furnace | |
| CN206270209U (en) | A kind of blood cell analyzer and its reaction tank temperature control equipment | |
| CN212006746U (en) | Coal quality analyzer furnace and coal quality analyzer | |
| CN201841010U (en) | Small and medium-sized adiabatic reactor | |
| CN103984374A (en) | High temperature system for small punch test method | |
| CN204806896U (en) | Refractoriness survey device | |
| CN103018126A (en) | Liquid seal connecting device for thermogravimetric analyzer | |
| CN102878796B (en) | Well type high-temperature resistance furnace for heat treatment of PAN (polyacrylonitrile) based carbon felt | |
| CN204550683U (en) | The experimental installation of calcium metal prepared by a kind of internal heat type vacuum reducing calcium oxide | |
| CN207169642U (en) | High-temperature high-pressure reaction kettle | |
| CN201123144Y (en) | Miniature high-temperature combustion furnace |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |