CN202063985U - Tantalum surface passivation device with refrigerating device - Google Patents
Tantalum surface passivation device with refrigerating device Download PDFInfo
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- CN202063985U CN202063985U CN2011201151301U CN201120115130U CN202063985U CN 202063985 U CN202063985 U CN 202063985U CN 2011201151301 U CN2011201151301 U CN 2011201151301U CN 201120115130 U CN201120115130 U CN 201120115130U CN 202063985 U CN202063985 U CN 202063985U
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- tantalum
- surface passivation
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000002161 passivation Methods 0.000 title claims abstract description 42
- 229910052715 tantalum Inorganic materials 0.000 title abstract description 23
- 239000007789 gas Substances 0.000 claims abstract description 100
- 238000006243 chemical reaction Methods 0.000 claims abstract description 69
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 33
- 239000001301 oxygen Substances 0.000 claims abstract description 33
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 33
- 238000005057 refrigeration Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000007669 thermal treatment Methods 0.000 claims description 13
- 239000003507 refrigerant Substances 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 17
- 238000000034 method Methods 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract 5
- 230000003139 buffering effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 18
- 230000003647 oxidation Effects 0.000 description 14
- 229910052786 argon Inorganic materials 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000498 cooling water Substances 0.000 description 6
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 229910001936 tantalum oxide Inorganic materials 0.000 description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000001146 hypoxic effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- APLLYCDGAWQGRK-UHFFFAOYSA-H potassium;hexafluorotantalum(1-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[Ta+5] APLLYCDGAWQGRK-UHFFFAOYSA-H 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003481 tantalum Chemical class 0.000 description 1
- -1 tantalum metals Chemical class 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- ZIRLXLUNCURZTP-UHFFFAOYSA-I tantalum(5+);pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Ta+5] ZIRLXLUNCURZTP-UHFFFAOYSA-I 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The utility model relates to a tantalum surface passivation device with a refrigerating device, comprising a thermal treating furnace, and a gas cycling and cooling system in a reactor, wherein the gas cycling and cooling system mainly comprises a gas cooling pipeline, a gas buffering chamber, a refrigerating chamber and a gas cycling pump; the gas cycling pump sends gas into the refrigerating chamber to be refrigerated, and sends the refrigerated gas into the lower part of a reaction chamber; and gas with higher temperature in the reaction chamber is exhausted from the upper part of the reaction chamber, is cooled through a gas cooling pipeline, then is sent to the refrigerating chamber to be refrigerated and is sent to the lower part of the reaction chamber again, so that the cycling process can be achieved. By utilizing the tantalum surface passivation device, the tantalum surface passivation is carried out, the effects of safety and reliability can be realized, the production efficiency is high, and the intense oxidization of tantalum can not occur; and the obtained tantalum is low in oxygen content, the tantalum anode manufacture by adopting the method has low leakage current, and the electrical property is good.
Description
Technical field
The utility model relates to a kind of tantalum metal surface passivation device, relates to a kind of tantalum metal surface passivation device that comprises oxygen-containing gas refrigeration and circulation device specifically.
Background technology
Because the tantalum metal is a kind of and the very big metal of oxygen affinity, the formation tantalum pentoxide is closed in tantalum and oxidation.How the people finds will form the thick oxide film of the about 3～8nm of one deck (referring to Observations on the morphology of Sodium-reduced Tantalum Powders and modification to their physical properties. 41 in the tantalum metallic surface in to the research of sodium reduction tantalum powder microtexture
StTIC Symposium, San Francisco. Oct. 22
Nd～25
Th2000:255～271.).If there is one deck dense oxidation film on the surface of tantalum powder, can prevent the continuation oxidation of tantalum.Because the thermal expansivity of metal tantalum and tantalum oxide is different, this tantalum particle one that is covered by dense oxidation film be when being heated to about temperature more than 100 ℃, fine and close tantalum-oxide film cracking and destroyed; When the tantalum pruinescence is heated to more than 700 ℃, the partial oxygen of oxide film is dissolved in the tantalum matrix, partial oxygen loss, enrichment.So, when contacting with oxygen-containing medium in the back that is cooled, the tantalum powder after the heating in the vacuum oven begins oxidation from the surface again, absorb new oxygen, if do not carry out passivation, even the temperature of tantalum powder is cooled to then take out in vacuum oven below 0 ℃, discovery begins slowly heating, then heat up rapidly, it is more and more hotter to become, and blazes up from one suddenly, spreads very soon and catches fire, reach hot, also be difficult to put out even at this moment the tantalum powder is immersed in the water, the tantalum powder continues and the water reaction under the high temperature, generates tantalum oxide and tantalum hydroxide.Therefore, people have developed the passivating technique of tantalum powder controllable oxidization.The passivation of described tantalum powder is when contacting with oxygen-containing medium again after the oxide film of tantalum powder is destroyed, control the feed speed of oxygen artificially, thereby the oxidation rate and the temperature of control tantalum powder under controlled situation make tantalum powder surface form the passive oxidation film, avoid fierce oxidation.So (specific surface area is greater than 0.1 m for the higher tantalum powder of specific surface area
2/ g) after thermal treatment, to carry out Passivation Treatment.Tantalum metal surface passivation process is actually controlled oxidation reaction.
The described tantalum metal surface passivation of this specification sheets comprises the surface passivation of tantalum powder and the surface passivation of the porous insert that formed by tantalum powder compacting, sintering.
Comprise that the prior art of patent documentation US 6927967B2, US 6432161B1, US 6238456B1, CN 1919508A, CN101404213A, US 6992881B2, US 7485256B2 and CN 1899728A has disclosed the passivation of tantalum powder, but these prior aries be the oxygen-containing gas under the room temperature be passed into be equipped with through Overheating Treatment and be cooled to room temperature or the vacuum oven of higher temperature in and be stranded in the reaction chamber, the heat that the reaction of oxygen-containing gas and tantalum powder is produced also is stranded in wherein; Such Passivation Treatment time is long, and often causes the fierce oxidation of tantalum powder.Publication number is that the Chinese patent of CN101348891A discloses a kind of tantalum powder controlled passivation magnesium processing deoxidization method, wherein uses pure oxygen to carry out Passivation Treatment; The problem that this method exists is to be not suitable for the high specific surface area tantalum powder is heat-treated post-passivation.All be that oxygen-containing gas is charged in the reactor to the tantalum powder passivation after the thermal treatment in the prior art, transfixion, because the heat that passivation produces raises tantalum powder temperature, vicious cycle appears in the high temperature promote the oxidation, is difficult to controlled oxidation speed.There is passivation time long like this, the problem that productivity is low.
Because the problems referred to above that prior art exists, thereby so this area still wish to have a kind of device that fierce oxidation obtains hypoxic tantalum powder and porous tantalum powder sintering body of in tantalum metal surface passivation process, can avoiding occurring.
Summary of the invention
In view of above-mentioned problems of the prior art, the purpose of this utility model provides a kind of can avoid taking place fierce oxidation and tantalum metal surface passivation device efficiently.
A kind of tantalum metal surface passivation device with refrigeration plant, it comprises heat treatment furnace, described heat treatment furnace comprises: reaction chamber, form the band water-cooling jacket of described reaction chamber furnace shell, the pipeline of finding time, be arranged at the well heater in the described reaction chamber and place the thermal treatment crucible that holds the tantalum metal in the well heater, it is characterized in that this tantalum metal surface passivation device comprises that also one makes the gas cooling recycle system in the reactor, the described gas cooling recycle system mainly comprises: gas cooling pipeline, gas buffer chamber, refrigeration cabinet and gas recycle pump, wherein
-gas cooling pipeline, the inlet mouth of this gas cooling pipeline links to each other with the outlet of reaction chamber top, and its outlet links to each other with the refrigeration cabinet import, and the oxygen-containing gas that is cooled enters refrigeration cabinet and further cools off;
-gas buffer chamber, this gas buffer chamber are provided with inert gas entrance and oxygen-containing gas inlet, and are communicated with refrigeration cabinet, and it is cooled that gas enters refrigeration cabinet by surge chamber;
-refrigeration cabinet, be provided with the refrigerant pipe that links to each other with refrigerator in this refrigeration cabinet, and its outlet is connected with utilidor, gas enters the cooled back of refrigeration cabinet from coming out through cooling duct cooling back gas, through utilidor, send into the reaction chamber bottom from the gas inlet with recycle pump;
-gas recycle pump, this gas recycle pump is located on the utilidor, and is communicated to the gas that the reaction chamber gas inlet is cooled by pipeline and sends into the reaction chamber bottom from the reaction chamber gas inlet, will react the higher gas of room temp simultaneously and extract out from reaction chamber top;
The per minute of described recycle pump is taken out, deflation rate is heat treatment reaction chamber volumetrical 1/10～4/1;
Described gas cooling pipeline has at least 3 meters of the length that contact with refrigerant.
The beneficial effects of the utility model are as follows: utilize tantalum metal surface passivation device of the present utility model to carry out the tantalum metal surface passivation, safe and reliable, the fierce oxidation of tantalum metal can not take place in the production efficiency height; The tantalum metal oxygen level that obtains is low, and low by the tantalum metal anode leakage current that so makes, good electrical property.
Description of drawings
Fig. 1 is the tantalum metal surface passivation device synoptic diagram that has the oxygen-containing gas cooling-cycle device of the present utility model; Wherein:
01. refrigeration cabinet 01-1. flowing water mouth 02. refrigeration cabinet gas inlet
03. refrigerator 04. refrigerant pipe 05. refrigeration cabinet pneumatic outlet
06. insulating pipe 07. reaction chamber pneumatic outlet 08. gas cooling pipeline
08-1. entrance of cooling water 08-2. cooling water outlet 09. gas recycle pump
10. the furnace shell 11-1. cooling water inlet of reaction chamber 11. band water-cooling jackets,
11-2. cooling water outlet 12. pressure warning units gas buffer chambers 20.
30. heat protection screens 21. inert gas entrance 22. oxygen-containing gass enter the mouth
40.The reaction chamber gas inlet
The pipeline 41. find time
50. well heater
60. reaction chamber ingress thermopair
61. reaction chamber bottom thermopair 62. reaction chamber middle heat galvanic couples 63. reaction chamber upper thermocouple 70. tantalum metals
80. crucible
100A. circulating cooling system
Fig. 1 shows tantalum metal surface passivation device after the thermal treatment that the utility model has gas cooling pipeline and refrigeration cabinet, this device mainly comprises: the furnace shell 11 of the band water-cooling jacket of reaction chamber 10, the heat protection screen 30 that is arranged at 10 li of reaction chambers, the well heater 50 that is arranged on described heat protection screen 30 the insides, the described reaction chamber 10 of composition, wherein 11-1 is a cooling water inlet pipe, and 11-2 is a cooling water outlet pipe; The vacuum manometer 12 that communicates with described reaction chamber 10; Tantalum metal surface passivation device also comprises gas cooling pipeline 08, refrigeration cabinet 01, gas buffer chamber 20 and gas recycle pump 09 after the described thermal treatment; Wherein the rate of air sucked in required of gas recycle pump per minute is 1/3 of a reaction chamber volume; Wherein, rare gas element 21 enters surge chamber 20 from entering the mouth, and oxygen-containing gas 22 enters surge chamber 20 from entering the mouth; Enter refrigerant pipe 04 heat exchange that the gas of refrigeration cabinet 01 links to each other with refrigerator 03 and cooled, cooled gas comes out from the outlet 05 of refrigeration cabinet, send the bottom of reaction chamber 10 to from the gas inlet 40 of reaction chamber by the connecting tube 06 of insulation with gas recycle pump 09 gas that temperature is lower, oxygen in the oxygen-containing gas and tantalum metal reaction, form oxide film in the tantalum metallic surface, and the gas temperature in tantalum metal and the reaction chamber is raise, the higher gas of temperature is extracted out from the relief outlet 07 on reaction chamber top in the reaction chamber, cool off through gas cooling pipeline 08, wherein water coolant enters from water inlet pipe 08-1, discharge from water shoot 08-2, cooling duct and refrigerant contact length are 6 meters; It is cooled with the main coolant pipe 04 generation heat exchange that links to each other with refrigerator 03 that the oxygen-containing gas of process cooling duct then enters refrigeration cabinet 01 from refrigeration cabinet inlet 02, cooled oxygen-containing gas comes out from the outlet 05 of refrigeration cabinet, by gas recycle pump 09 oxygen-containing gas is sent into the bottom of reaction chamber by the pipeline 06 that thermal insulation layer is arranged from reaction chamber gas inlet 40, constitute the gas circuit circulation.This device of the utility model, also can be used for to the cooling that circulates of tantalum powder after the thermal treatment, promptly oxygen-containing gas inlet mouth 22 valve closess, feed rare gas element from 21, pure inert gas carries out heat exchange and cooled through refrigeration cabinet 01 and heat-eliminating medium pipe 04, and recycle pump 09 is sent cooled pure inert gas into the reaction chamber bottom from reaction chamber gas inlet 40, rare gas element temperature is higher from reaction chamber top 07 is extracted out, constitutes the gas circulation cooling.After heat-treating, 01-1 opens with valve at every turn, with hot blast heat exchanger and pipeline is cleaned up, and then valve 01-1 is closed.
Embodiment 1
With specific surface area is 1.79m
2/ g, loose density is 0.50g/cm
3, porosity is that 97.0% oxygen level is the former powder of the sodium reduction tantalum potassium fluoride preparation of 6200ppm, mixes the phosphorus by tantalum grain weight amount 120ppm, carries out the nodularization granulation, obtaining loose density is 1.01 g/cm
3Spheroidal particle with porosity of 93.9%.Pouring above-mentioned nodularization granulation tantalum powder into the tantalum crucible porosity is 96.8% of former powder porosity, pour granulation tantalum powder into tantalum crucible 80 li, crucible is packed in as shown in Figure 1 the tantalum powder thermal treatment passivation device, make the thickness of tantalum powder in tantalum crucible be about 45mm, in a plurality of tantalum crucibles of same horizontal plane, leaving the space of about 1cm between the tantalum crucible, in the vacuum heat treatment furnace of packing into like this, is 1.33 * 10 at pressure
-1Be heated to 1200 ℃ of insulations 30 minutes in the vacuum below the Pa, stop heating then, after cooling to 120 ℃, feed argon gas from 21, argon gas enters into that heat exchange takes place for refrigerant pipe 04 that 01 li of heat exchanger chamber links to each other with refrigerator and cooled, cooled argon gas comes out by pipeline 06 from exporting 05, sends into heat treatment reaction chamber reaction chamber bottom from the gas inlet 40 of heat treatment reaction chamber; The higher argon gas of temperature in the reaction chamber comes out from reaction chamber outlet 07, is 20 ℃ water-cooled pipeline 08 by having temperature, with recycle pump 09 argon gas is circulated, and it is cooled to enter into refrigeration cabinet 01; The round-robin argon gas makes crucible and the cooling of tantalum powder in the heat treatment reaction chamber, makes the reaction room temp be reduced to about 20 ℃, makes the tantalum powder carry out passivation.Passivating process is: earlier refrigeration cycle portion gas inlet 40 is closed, the reaction indoor gas is found time from pump-line 41, vacuum tightness is opened valve 40 then, and valve 22 is slowly opened to about 0.092MPa, allow air admission, the pilot-gas flow, and start recycle pump 09 and refrigerator immediately, air enters the bottom of reaction chamber 10 from reaction chamber gas inlet 40 through refrigeration cabinet 01, pipeline 06, mix with remaining argon gas in the reaction chamber, reaction chamber ingress temperature is-10 ℃; The higher mixed gas of temperature is extracted out from reaction chamber pneumatic outlet 07 in the reaction chamber, through the gas cooling pipeline 08 that the outside has water coolant to circulate, gets back to the vacuum reaction chamber bottom again; About 10 minutes the pressure in the vacuum reaction chamber is charged to about 0.098～0.10 MPa greatly, stops air inlet, allow gas circulation 15 minutes; So carry out totally 8 times, last stop circulation after the 8th time oxygen-containing gas being charged into reaction chamber, allow oxygen-containing gas in reaction chamber, be detained 50 minutes.For the first time to finding time according to following table 1 for the 8th time and filling air.
About 4 hours of whole passivating process, temperature change between 18 ℃～26 ℃, through charging into air trapping temperature-stable to 22 ℃ after 15 minutes for the 8th time.After coming out of the stove the tantalum powder is taken out, do not have fierce oxidative phenomena.Tantalum powder after the above-mentioned thermal treatment sieves through 80 mesh sieve, obtains S-1h tantalum powder, analyzes the oxygen level of tantalum powder, and the results are shown in Table 2.
Comparative example 1
With the tantalum powder identical with embodiment 1, pack in the vacuum oven, heat-treat under identical temperature with embodiment 1, after stopping heating, in vacuum, cool to 200 ℃, logical argon gas is stranded in reaction chamber and cools off, temperature drops to 32 ℃, begin to carry out passivation, passivating process is that argon gas in the reaction chamber is evacuated to about 200Pa, for the first time divide 8 stages that 31 ℃ of air are charged into heat treatment reaction chamber, make the reaction chamber internal pressure from 200Pa to 0.1MPa:(200Pa～0.005MPa)/120 minute, (0.005 MPa～0.01 MPa)/60 minutes, (0.01 MPa～0.02 MPa)/60 minutes, (0.02 MPa～0.03 MPa)/60 minutes, (0.03 MPa～0.045 MPa)/30 minutes, (0.045 MPa～0.06 MPa)/30 minutes, (0.06 MPa～0.08MPa)/30 minute, (0.08 MPa～0.1 MPa)/amounted to 7 hours in 30 minutes.Wherein temperature rises 6 times suddenly in gas replenishment process, and top temperature rises to 50 ℃ when finding that temperature rises suddenly, stops inflation immediately, and equitemperature is reduced to about 32 ℃ and inflates in reaction chamber.For the second time divide 8 stages that 31 ℃ of air are charged into heat treatment furnace, make furnace pressure from 200 handkerchiefs to 0.1MPa:(200Pa～0.005MPa)/60 minute, (0.005 MPa～0.01 MPa)/60 minutes, (0.01 MPa～0.02 MPa)/60 minutes, (0.02 MPa～0.03 MPa)/60 minutes, (0.03 MPa～0.045 MPa)/30 minutes, (0.045 MPa～0.06 MPa)/30 minutes, (0.06 MPa～0.08MPa)/30 minute, (0.08 MPa～0.1 MPa)/amounted to 6 hours in 30 minutes.1 temperature wherein takes place rise to 50 ℃ suddenly.For the third time and for the third time same procedure is carried out the passivation inflation with 31 ℃ of air, amounts to 6 hours.31 ℃ of air of the 4th usefulness divide 4 stages from 200 handkerchiefs be charged to 0.1MPa:(200Pa～0.01MPa)/30 minute, (0.01 MPa～0.03 MPa)/30 minutes, (0.03 MPa～0.06 MPa)/30 minutes, (0.06 MPa～0.10MPa)/30 minute, amount to 2 hours.Amount to passivation 21 hours 4 times.After the passivation tantalum powder is taken out, heating is serious.Tantalum powder after the above-mentioned thermal treatment sieves through 80 mesh sieve, obtains E-1h tantalum powder, analyzes the oxygen level of tantalum powder, and the results are shown in Table 2.
Save a lot of times according to embodiment 1 of the present utility model than the tantalum powder passivating method of prior art comparative example, and tantalum powder oxygen level after thermal treatment of embodiment 1 is lower, just can make tantalum powder oxygen level reach requirement through a deoxidation thermal treatment, and the tantalum powder oxygen level of comparative example thermal treatment post-passivation is higher, to be used as electrical condenser, must be through twice above magnesium reduction deoxidation treatment.
Claims (3)
1. tantalum metal surface passivation device with refrigeration plant, it comprises heat treatment furnace, described heat treatment furnace comprises: reaction chamber (10), the furnace shell (11) of forming the band water-cooling jacket of described reaction chamber (10), the pipeline of finding time (41), be arranged at the well heater (50) in the described reaction chamber and place the thermal treatment crucible (80) that holds tantalum metal (70) in the well heater (50), it is characterized in that this tantalum metal surface passivation device comprises that also one makes the gas cooling recycle system (100A) in the reactor, the described gas cooling recycle system (100A) mainly comprises:
-gas cooling pipeline (08), the inlet mouth of this gas cooling pipeline links to each other with reaction chamber top outlet (07), and its outlet links to each other with refrigeration cabinet import (02);
-gas buffer chamber (20), this gas buffer chamber (20) are provided with inert gas entrance (21) and oxygen-containing gas inlet (22), and are communicated with refrigeration cabinet (01);
-refrigeration cabinet (01), (01) is provided with the refrigerant pipe (04) that links to each other with refrigerator (03) in this refrigeration cabinet, and its outlet (05) is connected with utilidor (06);
-gas recycle pump (09), this gas recycle pump (09) is located on the utilidor (06), and is communicated to reaction chamber gas inlet (40) by pipeline.
2. the tantalum metal surface passivation device with refrigeration plant as claimed in claim 1 is characterized in that the per minute of described recycle pump (09) is taken out, deflation rate is a heat treatment reaction chamber volumetrical 1/10～4/1.
3. the tantalum metal surface passivation device with refrigeration plant as claimed in claim 1 is characterized in that described gas cooling pipeline has at least 3 meters of the length that contact with refrigerant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201151301U CN202063985U (en) | 2011-04-19 | 2011-04-19 | Tantalum surface passivation device with refrigerating device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011201151301U CN202063985U (en) | 2011-04-19 | 2011-04-19 | Tantalum surface passivation device with refrigerating device |
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| CN202063985U true CN202063985U (en) | 2011-12-07 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104524714A (en) * | 2014-12-30 | 2015-04-22 | 北京化工大学 | Gas phase passivation and desensitization method for easy self-ignition and self-heating material in production equipment |
| CN106123421A (en) * | 2016-08-26 | 2016-11-16 | 江西稀有稀土金属钨业集团有限公司 | Ultrafine tungsten powder cooling system |
| 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 |
| CN112276079A (en) * | 2020-06-22 | 2021-01-29 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
-
2011
- 2011-04-19 CN CN2011201151301U patent/CN202063985U/en not_active Expired - Lifetime
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104524714A (en) * | 2014-12-30 | 2015-04-22 | 北京化工大学 | Gas phase passivation and desensitization method for easy self-ignition and self-heating material in production equipment |
| CN104524714B (en) * | 2014-12-30 | 2017-08-15 | 北京化工大学 | Easy spontaneous combustion causes the blunt quick method that disappears from the gas phase of hot material in a kind of production equipment |
| CN106123421A (en) * | 2016-08-26 | 2016-11-16 | 江西稀有稀土金属钨业集团有限公司 | Ultrafine tungsten powder cooling system |
| 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 |
| CN112276079A (en) * | 2020-06-22 | 2021-01-29 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
| CN112276079B (en) * | 2020-06-22 | 2021-09-10 | 江门富祥电子材料有限公司 | Device and method for sintering tantalum briquette and removing binder |
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Owner name: DONGFANG TANTALUM INDUSTRY CO. LTD., NINGXIA Free format text: FORMER OWNER: PAN LUNTAO Effective date: 20150907 |
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Effective date of registration: 20150907 Address after: 753000 Dawukou Road, Shizuishan, the Ningxia Hui Autonomous Region metallurgical Road, No. 119 Patentee after: Dongfang Tantalum Industry Co., Ltd., Ningxia Address before: 753000 the Ningxia Hui Autonomous Region Shizuishan city Dawukou District Metallurgical Road No. 87-6 Patentee before: Pan Luntao |
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