CN202954080U - Magnesium reduction and deoxygenation device of tantalum powder - Google Patents

Magnesium reduction and deoxygenation device of tantalum powder Download PDF

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Publication number
CN202954080U
CN202954080U CN 201220665129 CN201220665129U CN202954080U CN 202954080 U CN202954080 U CN 202954080U CN 201220665129 CN201220665129 CN 201220665129 CN 201220665129 U CN201220665129 U CN 201220665129U CN 202954080 U CN202954080 U CN 202954080U
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magnesium
tantalum powder
reaction vessel
collecting device
crucible
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朱德忠
郑浩宇
杨进
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F & X Electro-Materials Ltd
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F & X Electro-Materials Ltd
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Abstract

The utility model discloses a magnesium reduction and deoxygenation device of tantalum powder. The magnesium reduction and deoxygenation device comprises an electric heating well type furnace and a cylindrical reaction container arranged in the well type furnace, wherein the reaction container mainly comprises an inert gas inlet pipe, a gas exhaust pipe, a thermocouple pipe and a crucible containing the tantalum powder, wherein a heater is arranged outside the reaction container of the crucible part, the crucible is arranged at the lower part of the reaction container, a magnesium collector is arranged above the tantalum powder crucible, a lower heat insulation screen is arranged between the magnesium collector and the tantalum powder crucible, an upper heat insulation screen is arranged above the magnesium collector, a cooling device is arranged outside the reaction container of the upper heat insulation screen part, and the inert gas inlet pipe extends into the bottom of the reaction container. By using the device disclosed by the utility model to perform magnesium reduction and deoxygenation on the tantalum powder, the loss of the tantalum powder is low, the oxygen content in the tantalum powder is low, recovered metal magnesium can be reutilized, and the environmental pollution is reduced.

Description

The oxygen device falls in the magnesium reduction of tantalum powder
Technical field
The utility model relates to the utility model and relates to the magnesium reduction of a kind of tantalum powder and fall the oxygen device.
Background technology
The tantalum metal is a kind of rare precious metal, and its important use is to make electrolytic condenser.The tantalum powder of using as electrical condenser requires very high purity.Producing Ta powder used in capacitor is normally having under thinner salt (as NaCl, KCl and KF etc.) existence with sodium Metal 99.5 (Na) reduction tantalum potassium fluoride (K 2TaF 7) product that comprises tantalum powder, basic metal and polybasic salt that obtains, its washing is reclaimed and obtained the tantalum powder, then carry out the pickling washing, the tantalum powder after washing will carry out vacuum heat treatment, just can reach for making the requirement of electrolytic condenser.Yet, because tantalum metal pair oxygen has very large avidity, the tantalum powder made through above-mentioned operation often contains too high oxygen, this is very disadvantageous for making electrolytic condenser, can cause condenser leakage current high, proof voltage is poor, so must be fallen oxygen, processes.In addition, the oxygen that also will be fallen had at the electrical condenser base become with the tantalum powder sintering is processed.The oxygen processing falls in the general employing of the oxygen processing magnesium reduction of falling of tantalum powder.
With the tantalum oxide (Ta in magnesium reduction tantalum powder 2O 5+ 5Mg → 5MgO+2Ta) variation of Gibbs free energy is as shown in table 1:
Table 1
Figure BDA00002529791200011
From the table data can find out, it is very suitable that the tantalum powder falls oxygen with magnesium reduction.
Based on the required amount meter tantalum powder oxygen-content reduction to 0 in theory, preferably use 1.1 times to the 3 times reductive agent magnesium that stoichiometry is excessive.After falling oxygen, magnesium used and the magnesium oxide formed during falling oxygen are removed with mineral acid, preferably use one or more in hydrochloric acid, sulfuric acid, nitric acid, hydrogen peroxide.
U.S. Pat 4483819A, US4537641A have proposed the method that oxygen falls in the tantalum material, soon there being reductive agent to heat-treat at 600 ℃ ~ 1200 ℃ under as existence such as Ca, Mg, Al, the fast oxygen level of tantalum powder and tantalum sintering are reduced tantalum powder and tantalum sintering.
In order to effectively reduce the oxygen level of tantalum powder, usually to add based on tantalum powder oxygen level meter, add the magnesium powder of 1.5 times ~ 3 times of stoichiometries, like this, after insulation reaction is complete, in the tantalum powder, also can remain considerable magnesium.In the tantalum powder, remaining magnesium is very unfavorable to the tantalum powder, because magnesium and oxygen have very large avidity, when the tantalum powder is come out of the stove, magnesium will even cause that the tantalum powder catches fire with oxygen kickback heat release, and when the tantalum powder containing a large amount of magnesium is put in Acidwash solution, also can emit large calorimetric due to magnesium and dilute acid soln intense reaction, sometimes also can cause and catch fire, this is also unfavorable to environment; And tantalum powder and magnesium form Ta-Mg-O containing water complex, cause the loss of tantalum powder when pickling, washing, and finally cause that the Mg of tantalum powder, O content are high.Therefore, people take to be incubated under positive pressure 1 ~ 3 hour 800 ℃ ~ 1000 ℃ elder generations the tantalum powder being carried out when oxygen falls in magnesium reduction, then at 800 ℃ ~ 1000 ℃, are found time.Yet, because the fusing point of magnesium is 651 ℃, boiling point is 1107 ℃, higher in the vapour pressure of 800 ℃ ~ 1000 ℃ of magnesium, the vapour pressure of magnesium at some temperature is in Table 2.Magnesium unnecessary in the tantalum powder is except having small part by tantalum powder surface adsorption, all the other major parts are present in crucible bottom with liquid form, so, as at 927 ℃, if the pressure while finding time in reaction vessel is lower than the 134.9mm mercury column, can make liquid magnesium boiling unnecessary in the tantalum powder crucible and cause that the tantalum powder is ejected in reaction vessel, on thermoscreen, even be pumped to vacuum pipe, blocking pipe, this part the tantalum powder that can collect is also polluted, and produces serious financial loss.
Table 2 magnesium vapor is pressed the relation with temperature
Temperature/℃ 427 527 627 651 727 827 927 1027 1107
Pressure/mm mercury column 0.0071 0.148 1.66 2.63 8.71 39.8 134.9 407.4 760
The utility model content
The utility model is for the deficiencies in the prior art, provide a kind of tantalum powder loss less, tantalum powder that tantalum powder oxygen level is low falls oxygen technique and the oxygen device falls in the tantalum powder.
For achieving the above object, the utility model by the following technical solutions:
A kind of device that falls oxygen for the magnesium reduction of tantalum powder, comprise the electrically heated pit furnace and as for the drum type brake reaction vessel in this pit furnace, described reaction vessel mainly includes rare gas element and enters pipe, gas outlet pipe, thermocouples tube and the crucible that the tantalum powder is housed, the reaction vessel peripheral hardware having heaters at this crucible position, described crucible is placed in the reaction vessel bottom, be provided with magnesium collecting device above the tantalum powder crucible, be provided with lower thermoscreen between magnesium collecting device and tantalum powder crucible, the top of magnesium collecting device has upper heat insulation, reaction vessel outside at upper thermoscreen position is provided with refrigerating unit, described rare gas element enters pipe and extend into reaction container bottom.
The oxygen device falls in tantalum powder of the present utility model magnesium reduction, wherein, shape for magnesium collecting device has no particular limits, for perpendicular pot type reaction vessel, preferably magnesium collecting device is one and comprises chassis and sidewall upper shed disk, more preferably a plurality ofly comprises that chassis and sidewall upper shed disk stack up and down, these magnesium collecting device disks are in different positions, when the circulation rare gas element, the temperature difference of each magnesium collecting device, can collect the magnesium vapor evaporated up from the reaction vessel bottom effectively.
The oxygen device falls in the magnesium reduction of described tantalum powder, and in order effectively to collect the steam magnesium risen from reaction container bottom, preferably the diameter of magnesium collecting device disk is less than approximately 10 ~ 20cm of reaction vessel internal diameter, and its upper edge is 2 ~ 5cm to the degree of depth of bottom.The material of manufacturing magnesium collecting device is had no particular limits, and the angle of using from economy is considered, stainless steel plate that can be thick with 2 ~ 4mm or the manufacture of nickel plate.
The oxygen device falls in tantalum powder of the present utility model magnesium reduction, and wherein magnesium collecting device below has thermoscreen plectane under a slice at least, preferably has 2 ~ 3 layers, and interfloor distance is 4 ~ 10cm, and the superiors' plectane and orlop magnesium collecting device spacing are 4 ~ 10cm.
The oxygen device falls in tantalum powder of the present utility model magnesium reduction, wherein, there is thermoscreen on multilayer the magnesium collecting device top, wherein at least near magnesium collecting device, a slice thermoscreen being arranged is inverted circular cone panel, it is 4 ~ 10cm through hole that there is diameter centre, the upper bore of inverted conical face is less than reaction vessel internal diameter 1 ~ 4cm, and the angle of cone surface is 170 ° ~ 120 °, reaches the 4 ~ 10cm that is spaced apart of cone plate and magnesium collecting device between thermoscreen.
The oxygen device falls in tantalum powder of the present utility model magnesium reduction, wherein, has a temperature measuring equipment at least between the magnesium collecting device outside and reaction vessel inwall, for measuring the temperature at magnesium collecting device position.
Like this, because the diameter of lower thermoscreen and magnesium collecting device is less, temperature is higher, and the diameter of upper thermoscreen is larger, temperature is lower, at high temperature, when rare gas element being passed into to reaction container bottom being circulated, rare gas element flows from bottom to up, unnecessary magnesium volatilization in the tantalum powder in the tantalum powder crucible under high temperature, magnesium steam rises along with the air-flow risen, when the top of magnesium steam rising to magnesium collecting device, run into the upper thermoscreen of the inverted conical face that the larger temperature of diameter is lower, upper at thermoscreen, lower two sides is condensed into liquid magnesium or solid-state magnesium, liquid magnesium is past dirty along the thermoscreen of inverted cone surface, or flow in magnesium collecting device by centre hole.
The beneficial effects of the utility model are: device of the present utility model is simple, and on original device basic, transformation gets final product a little, easily implements; Use device of the present utility model to carry out the magnesium reduction of tantalum powder and fall oxygen, the loss of tantalum powder is few, and tantalum powder oxygen level is low, and the MAGNESIUM METAL of recovery can recycle, and reduces the pollution to environment.
The accompanying drawing explanation
Fig. 1 is that oxygen device schematic diagram falls in tantalum powder of the present utility model magnesium reduction.
Fig. 2 is E-E cross section upward view in Fig. 1
Fig. 3 is that oxygen device schematic diagram falls in the magnesium reduction of prior art tantalum powder.
Fig. 4 is that oxygen device schematic diagram falls in another tantalum powder magnesium reduction of the utility model
Fig. 5 the utility model falls oxygen in the magnesium reduction of tantalum powder and is passed to the outside, magnesium collecting device middle part of outage mensuration and the temperature variation between the reaction vessel inwall from rare gas element.
Embodiment
Fig. 1 is that the oxygen device falls in the tantalum powder magnesium reduction that the utility model is used, comprise pit furnace 14 and as for the drum type brake reactor 10 in pit furnace 14, the bottom heater 141 that in burner hearth, bottom is comprised of the resistance heating wire, the cylinder side wall made progress from bottom is by the sidewall well heater 142 be comprised of 6 sections resistance heating wires, the top of sidewall well heater heater strip 142 topmost higher than on last layer tantalum powder crucible 16 in reaction vessel 10 along about 8cm, guarantee that by automatic control there is uniform preset temperature at tantalum powder crucible 16 positions.
Reaction vessel 10 mainly comprises: top is the reaction vessel lid 11 of sealed reaction vessel, on reaction vessel lid 11, be provided with find time, vapor pipe 20(valve, threeway be not shown), have the rare gas element from be deep into reaction container bottom near the reaction vessel perisporium to enter pipe 19, an end that enters pipe connection inert gas source at rare gas element is connected with gas meter 191; The gas that is filled with air (or nitrogen) enters pipe 21; The vacuum manometer 22 of assaying reaction container inner pressure; Be deep at least 4 thermocouples tubes 23 of different depths in reaction vessel near the reaction vessel perisporium from the same circumference of reaction vessel lid, measure respectively the temperature at bottom, middle part, upper position and magnesium collecting device 24 positions of tantalum powder crucible with 4 thermocouples tube 23A, 23B, 23C and 23D, as depicted in figs. 1 and 2; With 4 union levers (only illustrating 2 in Fig. 1) 184, the first thermoscreen 181 (5) magnesium collecting device 24 and the second thermoscreen 182 are connected on reaction vessel lid 11, wherein, the liquid magnesium that magnesium vapor runs into the first thermoscreen 181 condensations flow into 24 li of magnesium collecting devices, the first thermoscreen 181 of the circle flat board that in Fig. 1, the thermoscreen on magnesium collecting device 24 tops is identical by 5 plate shapes forms, and each interfloor distance is about 6cm.Thermoscreen on magnesium collecting device 24 also can all be comprised of inverted cone surface, as Fig. 4.
Magnesium collecting device 24 at least comprise a disk towards upper shed with hold from the liquid magnesium of thermoscreen drippage, 2 opening up disks by the about 3cm of the degree of depth in Fig. 1 form, magnesium collecting device disk periphery and reaction vessel inwall spacing are about 6cm, wherein, the bottom of magnesium collecting device disk bottom is about 12cm from the upper edge of the superiors' tantalum powder crucible.Have second thermoscreen 182 at least below magnesium collecting device, make the larger temperature head of the interior formation of distance shorter between tantalum crucible and magnesium collecting device, in Fig. 1, two stacked circular plate types the second thermoscreen 182 is arranged, its diameter and magnesium collecting device diameter phase.Between the second thermoscreen and the spacing between the second thermoscreen and magnesium collecting device disk be about 4 ~ 6cm.
Outer reaction vessel 10 upper periphery of the first thermoscreen have cooling water jecket 13, and it comprises water inlet pipe 131 and rising pipe 132.Cover lower position from tantalum powder crucible position to reaction vessel in reaction vessel 10 inside like this, form one by high temperature the thermograde to low temperature, in the tantalum crucible position, be temperature of reaction (as 920 ℃), in the position of magnesium collecting device, temperature is about 600 ℃ ~ 800 ℃.Because the reaction vessel at the first thermoscreen position is with cooling water jecket outward, and diameter is larger, like this, the upper thermoscreen be cooled becomes the baffle plate of cohesion magnesium vapor, at high temperature, when rare gas element being passed into to reaction container bottom being circulated, rare gas element flows from bottom to up, unnecessary magnesium volatilization in the tantalum powder in the tantalum powder crucible under high temperature, magnesium steam rises along with the air-flow risen, and when the top of magnesium steam rising to magnesium collecting device 24, runs into the first thermoscreen and is cooled, the magnesium devaporation be cooled becomes liquid magnesium or solid-state magnesium, and liquid magnesium is in magnesium collecting device.Wherein, the first thermoscreen, magnesium collecting device and the second thermoscreen can be to be fixedly attached to reaction vessel to cover, and the magnesium for easy cleaning is collected, also can be made into dismountable parts, as on union lever 184, sleeve pipe arranged, at the bottom of the second thermoscreen screw-driving.
When carrying out the magnesium reduction of tantalum powder and fall oxygen, pack into 16 li of tantalum crucibles of the high tantalum powder 17 of the oxygen that is mixed with the magnesium powder, tantalum crucible 16 is placed on bin 15, then the bin 15 that the tantalum powder crucible is housed is put into to the bottom of the drum type brake reaction vessel 10 that internal diameter is 80cm, drum type brake reaction vessel 10 is placed in to 14 li of pit furnaces, and its pallet 12 is sitting on pit furnace.
The utility model also provides a kind of said apparatus that utilizes to carry out the technique that oxygen falls in the magnesium reduction of tantalum powder, and the step of this technique comprises:
The high tantalum powder of oxygen is mixed with the magnesium powder of the 1wt% ~ 3wt% of tantalum powder, in the tantalum crucible in the reaction vessel of packing into, the reaction vessel that the tantalum powder is housed is hung in pit furnace;
Be filled with rare gas element after reaction vessel is found time, in inert atmosphere, pressure is that lower tantalum powder of 0.1 ~ 0.2MPa is heated to 800 ~ 1000 ℃ of maintenances 30 minutes ~ 2 hours, and in this step, in magnesium and tantalum powder, oxygen reacts, and removes the oxygen in the tantalum powder;
Then, in tantalum powder temperature, it is 800 ~ 1000 ℃, under about 0.1MPa pressure, with rare gas element circulation 30 minutes ~ 3 hours, the circulation speed of rare gas element is 10 liter/mins ~ 300 liter/mins, the flow velocity of rare gas element is mainly determined by the reaction vessel size, reaction vessel is large, the rare gas element flow velocity can be more greatly, in the meantime, the magnesium continuation reacts with the oxygen in the tantalum powder, and, due to a lasting upstream being arranged, at tantalum powder crucible position, temperature is high, in crucible, magnesium in the tantalum powder has higher magnesium vapor and presses, magnesium steam is along with upstream, arrival closes on the upper thermoscreen position of magnesium collecting device, the temperature here is about 650 ℃ ~ 800 ℃ scopes, upper and lower surface at upper thermoscreen, magnesium steam condenses into rapidly liquid magnesium or solid particles, liquid magnesium just flows in magnesium collecting device, wherein, time to the rare gas element circulation does not have strict restriction, can according to the tantalum powder of packing in the temperature of tantalum powder height and reaction vessel the number, excessive number and rare gas element circulation speed decides to add the magnesium stoichiometry, general temperature is higher, magnesium vapor is pressed higher, the rare gas element circulation time can be shorter, inert gas flow is large, row's magnesium time is short, if in reaction vessel, the total amount of excessive magnesium is many, the time of circulation will suitably lengthen so, general circulation 0.5 hour to 3 hours, after the rare gas element that goes into circulation, in the situation that it is temperature-resistant to control tantalum powder crucible position, the magnesium vapor stream risen takes heat to top, can make magnesium collecting device position temperature raise, after most of magnesium evaporation in the tantalum powder, the temperature at magnesium collecting device position can return to again the temperature approached while starting to carry out the rare gas element circulation, at this time, the liquid magnesium of the cohesion in the tantalum powder is evaporated completely basically,
Through the rare gas element circulation, after definite unnecessary liquid magnesium basically is discharged from and collects magnesium collecting device, gas exhaust duct is connect to vacuum pump is found time to reduce pressure, at this time not there will be the magnesium spray, the tantalum powder is taken out of to the phenomenon of crucible, finding time is to keep 30 minutes ~ 2 hours at 800 ~ 1000 ℃, and pressure reaches below about 300Pa, is enough to like this make the magnesium that is adsorbed on tantalum powder surface also can be pumped;
Then the tantalum powder in reaction vessel is cooling, discharging after passivation, collected the magnesium in magnesium collecting device, and reaction vessel is cleaned, dries together with magnesium collecting device, and next time is stand-by, and the tantalum powder is carried out to pickling, the oven dry of washing final vacuum, the tantalum powder of the oxygen that has been reduced.
Fig. 3 is that the oxygen device falls in the tantalum powder magnesium reduction that prior art is used, and it is different that with the utility model tantalum powder, the oxygen device falls in magnesium reduction: only have dull and stereotyped thermoscreen above the tantalum powder crucible, there is no magnesium collecting device; Rare gas element enter pipe only be deep into reaction vessel lid below, be not deep into reaction container bottom.
The oxygen that falls of prior art tantalum powder is to carry out in device as shown in Figure 3, after mixing with a certain amount of magnesium powder, tantalum powder that will be high containing oxygen forms containing pack into 16 li of tantalum crucibles of magnesium tantalum powder 17, after adding a cover 11 sealings, find time, then be filled with argon gas, be heated to 800 ℃ ~ 1000 ℃ 14 li of pit furnaces by resistance heating wire 14-1 and 14-2, be incubated 2 ~ 6 hours in the atmosphere of rare gas element and/or under vacuum, then cool to room temperature, carrying out after passivation comes out of the stove carries out the pickling washing, dries and obtains falling oxygen tantalum powder.Between soak, magnesium volatilization in the tantalum powder, the magnesium steam rising, run into the thermoscreen that temperature is lower, only has a small amount of magnesium steam to condense upon on thermoscreen with solid-state magnesium or the reaction vessel inwall, a large amount of magnesium steam condense upon on thermoscreen with liquid magnesium, drippage goes down again, continues volatilization, like this, iterative cycles, hinder the magnesium volatilization in the tantalum powder.
Embodiment
The tantalum powder that is 6800ppm by the 100kg oxygen level, add 2000 gram magnesium powder, (based in theory oxygen in the tantalum powder all being removed, having reacted rear residue magnesium 980 grams need to be with magnesium 1020 gram-in fact can not all remove), the magnesium powder is mixed with the tantalum powder, be respectively charged into 16 li of 11 tantalum crucibles, 10 li of the reaction vessels that the crucible 16 that the tantalum powder 17 of sneaking into the magnesium powder is housed is packed into as described in Figure 1, reaction vessel 10 is hung in to 14 li of pit furnaces, open cooling water pipeline 13, from water inlet pipe 131 water inlets, from water shoot 132, discharge, be evacuated to about 200Pa from vapor pipe 20, stop finding time rear argon gas from pipeline 19 is filled into reaction vessel 10, make 10 li pressure of reaction vessel remain on 0.11MPa ~ 0.14MPa, heating up makes A, B and C place temperature to 920 ℃, is incubated 1 hour, then open argon gas circulation valve, with under meter 191, make the argon gas flow velocity remain on 40 ~ 60 liter/mins, and open vent valve 20, the about 0.1MPa of reaction vessel internal pressure, make A, B and C place temperature keep approximately 920 ℃, the circulation argon gas, while going into circulation argon gas, the temperature at the magnesium collecting device position of tantalum powder crucible top rises rapidly, the heat that the magnesium vapor zone is described passes to magnesium collecting device with upper part, magnesium steam is condensed into liquid magnesium or solid-state magnesium at upper thermoscreen, liquid magnesium flows in magnesium collecting device, and emit heat, after continuing for some time like this, the temperature slow decreasing, to the temperature dropped to while approach starting, keep for some time to circulating argon gas 2 hours, then close argon gas, vent valve 20 is connect to vacuum pump, find time, the reaction vessel internal pressure is lower than 300Pa, and making A, B and C place temperature is 920 ℃, and at this moment the temperature at the D position of magnesium collecting device has a little rising, then be reduced to again the temperature approached while starting to find time, find time altogether 1 hour.
Fig. 5 shown from the circulation rare gas element to find time complete during, D temperature variation between magnesium collecting device periphery and reaction vessel inwall.
After finding time, stop heating, be filled with argon gas, make the reaction vessel internal pressure remain on 0.11 ~ 0.14MPa, A, B and C place are cooled to and approach room temperature, enter pipe 21 from gas and slowly be filled with air and carry out passivation, then the tantalum powder is taken out from reaction vessel, do not find that there is tantalum powder ejection phenomenon.Magnesium in magnesium collecting device is collected, the tantalum powder is carried out to pickling, there is no the intense reaction phenomenon simultaneously, the tantalum powder washs through peroxy-nitric acid-aqueous hydrogen peroxide solution, then washes neutrality with deionized water, then vacuum drying, obtain tantalum powder 99.7kg, the oxygen level of tantalum powder is 3300ppm, and Mg content is lower than 3ppm.Collect magnesium 512 grams.
Comparative example 1
With the tantalum powder 100kg identical with embodiment, add equally 2000 gram magnesium powder, use reaction vessel as shown in Figure 3, after shove charge, reaction vessel is hung in to 10 li of pit furnaces, be filled with argon gas after finding time, at 0.11MPa ~ 0.14MPa, be warmed up to 920 ℃, be incubated 4 hours, cooling has a power failure, cooling after and embodiment 1 carry out equally passivation, then the tantalum powder is taken out from reaction vessel, the tantalum powder is when carrying out pickling, due to more residue magnesium being arranged in the tantalum powder, starting has intense reaction, and " plain soup " phenomenon arranged, washing obtains tantalum powder 99.1kg after drying, the oxygen level of tantalum powder is 3800ppm, Mg content is 6ppm.
Comparative example 2
With the tantalum powder 100kg identical with embodiment, add equally 2000 gram magnesium powder, use reaction vessel as shown in Figure 3, after shove charge, reaction vessel is hung in to 10 li of pit furnaces, be filled with argon gas after finding time, at 0.11MPa ~ 0.14MPa, be warmed up to 920 ℃, be incubated 2 hours, then from vapor pipe 20, found time, 920, find time 2 hours, cooling has a power failure, cooling after and embodiment 1 carry out equally passivation, then the tantalum powder is taken out from reaction vessel, find in reaction vessel, on thermoscreen, evacuation tube has the tantalum powder, collect the tantalum powder 1.1kg of pollution, tantalum powder in the tantalum powder crucible is carried out to pickling, washing obtains tantalum powder 96.4kg after drying, the oxygen level of tantalum powder is 3420ppm, Mg content is 3ppm.
Can fully understand superiority of the present utility model from above embodiment and comparative example, the utility model also is applicable to the oxygen that falls that falls oxygen processing and sintered anode of niobium powder to be processed.
The above, it is only preferred embodiment of the present utility model, not the utility model is done to any pro forma restriction, any those skilled in the art, within not breaking away from the technical solutions of the utility model scope, make many changes or be modified to the equivalent example of equivalent variations when the technology contents that can utilize above-mentioned announcement, all still belong in the technical scheme scope that the utility model is new.

Claims (5)

1. the oxygen device falls in the magnesium reduction of tantalum powder, comprise the electrically heated pit furnace and as for the drum type brake reaction vessel in this pit furnace, described reaction vessel mainly includes rare gas element and enters pipe, gas outlet pipe, thermocouples tube and the crucible that the tantalum powder is housed, the reaction vessel peripheral hardware having heaters at this crucible position, it is characterized in that: described crucible is placed in the reaction vessel bottom, be provided with magnesium collecting device above the tantalum powder crucible, be provided with lower thermoscreen between magnesium collecting device and tantalum powder crucible, there is upper thermoscreen the top of magnesium collecting device, reaction vessel outside at upper thermoscreen position is provided with refrigerating unit, described rare gas element enters pipe and extend into reaction container bottom.
2. the oxygen device falls in tantalum powder according to claim 1 magnesium reduction, it is characterized in that, described magnesium collecting device is to be comprised the container of the upper shed of chassis and sidewall by least one.
3. the oxygen device falls in tantalum powder according to claim 1 magnesium reduction, it is characterized in that, described magnesium collecting device is the disk of manufacturing with stainless steel plate, and the diameter of described magnesium collecting device is less than approximately 8 ~ 20cmcm of described reaction vessel internal diameter.
4. the oxygen device falls in tantalum powder according to claim 1 magnesium reduction, it is characterized in that, the lower thermoscreen of described magnesium collecting device below is comprised of one or more layers stainless steel plectane.
5. according to the described tantalum powder of claim 1-4 any one, the oxygen device falls in magnesium reduction, it is characterized in that having a temperature measuring equipment at least between the magnesium collecting device outside and reaction vessel inwall.
CN 201220665129 2012-12-05 2012-12-05 Magnesium reduction and deoxygenation device of tantalum powder Expired - Fee Related CN202954080U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965525A (en) * 2012-12-05 2013-03-13 江门富祥电子材料有限公司 Device and method for carrying out magnesium reduction and deoxidization on tantalum powder
CN108607987A (en) * 2018-05-15 2018-10-02 江苏振华新云电子有限公司 Reduce the method and its equipment of anode tantalum core oxygen content

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102965525A (en) * 2012-12-05 2013-03-13 江门富祥电子材料有限公司 Device and method for carrying out magnesium reduction and deoxidization on tantalum powder
CN108607987A (en) * 2018-05-15 2018-10-02 江苏振华新云电子有限公司 Reduce the method and its equipment of anode tantalum core oxygen content

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