CN101880847B - Heat treatment method of tantalum crucible - Google Patents
Heat treatment method of tantalum crucible Download PDFInfo
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- CN101880847B CN101880847B CN2010102041510A CN201010204151A CN101880847B CN 101880847 B CN101880847 B CN 101880847B CN 2010102041510 A CN2010102041510 A CN 2010102041510A CN 201010204151 A CN201010204151 A CN 201010204151A CN 101880847 B CN101880847 B CN 101880847B
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- Prior art keywords
- tantalum
- tantalum crucible
- crucible
- heat treatment
- thermal treatment
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000010438 heat treatment Methods 0.000 title claims abstract description 19
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 10
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 4
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 4
- 238000007669 thermal treatment Methods 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000009413 insulation Methods 0.000 description 6
- 229910052728 basic metal Inorganic materials 0.000 description 5
- 150000003818 basic metals Chemical class 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen 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
- 238000007789 sealing Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005382 thermal cycling Methods 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a heat treatment method of a tantalum crucible. In the method, the tantalum crucible is put in the atmosphere with alkali earth metals and alkali metals for carrying out heat treatment at high temperature. The service life of the tantalum crucible which is subject to heat treatment according to the method of the invention is prolonged.
Description
Technical field
The present invention relates to a kind of heat treating method of tantalum crucible, particularly a kind ofly be used for the heat treated tantalum crucible of tantalum powder carries out high-temperature heat treatment in alkaline-earth metal and alkali-metal atmosphere method.
Background technology
Tantalum powder producing method commonly used is to obtain former powder with the sodium reduction tantalum potassium fluoride, and the former powder that reduction obtains generally also will carry out vacuum heat treatment under 800 ℃～1500 ℃ high temperature, former powder is purified, and improve its physicals.Not contaminated in order to guarantee the tantalum powder, the thermal treatment of tantalum powder normally uses tantalum matter crucible (tantalum crucible) to hold the tantalum powder.Tantalum crucible in heat treatment process, repeated multiple times be subjected to heating under vacuum-and atmosphere contact cooling-heating under vacuum-and the cycling hot of atmosphere contact cooling impact.Like this through repeatedly thermal cycling, and gases such as adsorption of oxygen, nitrogen, carbon monoxide and carbonic acid gas, make thickization of crystal grain of tantalum crucible, interstitial element is enriched to crystal boundary, makes tantalum crucible produce embrittlement.Like this, the work-ing life of tantalum crucible is short, causes tantalum powder production cost height.
Summary of the invention
In order to address the above problem, the invention provides a kind of heat treating method of tantalum crucible, reduce and eliminate this embrittlement phenomenon of tantalum crucible, prolong the work-ing life of tantalum crucible.
For achieving the above object, the present invention by the following technical solutions: a kind of heat treating method of tantalum crucible has placed tantalum crucible in alkaline-earth metal and the alkali-metal atmosphere and to have carried out high-temperature heat treatment.
Further, described thermal treatment is carried out under 700 ℃～1050 ℃ temperature.
Further, described high-temperature heat treatment kept 5 hours at least.
Further, described high-temperature heat treatment kept 5～20 hours at least.
Further, described high-temperature heat treatment is carried out in the atmosphere of argon gas.
Further, described basic metal adds at least 50 grams, and described alkaline-earth metal adds at least 100 grams.
The invention has the beneficial effects as follows: according to the tantalum crucible after the inventive method thermal treatment, prolong its work-ing life.
Embodiment
Reach technique means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, below in conjunction with preferred embodiment, embodiment, feature and the effect of the heat treating method of the tantalum crucible that foundation the present invention is proposed are described in detail as follows.
According to the inventive method, thermal treatment tantalum powder was used repeatedly tantalum crucible, after for example using 40 times, tantalum crucible is placed the thermally resistant container of a hermetic seal, add alkaline-earth metal, basic metal, add-on does not have strict restriction, mainly be to determine according to the amount of pending tantalum crucible and the size of processing vessel, common industrial production is handled the tantalum crucible more than 10, general alkaline-earth metal and at least 50 basic metal that add at least 100 grams, wherein alkaline-earth metal can be selected metal magnesium powder, calcium grain for use; Basic metal can be selected potassium metal, sodium for use.Alkaline-earth metal and basic metal can be concentrated placement, also can disperse to place, and preferably dispersedly alkaline-earth metal are placed in each tantalum crucible.With being evacuated down to about 200Pa after the container sealing, charge into argon gas, pressure position 0.1MPa～0.13MPa in the container is warmed up to 700 ℃～1200 ℃, and insulation is more than 3 hours.The temperature height, soaking time is long, the flexibility of tantalum crucible is recovered favourable, yet temperature is too high, and the time is oversize, the equipment cost height; Preferred temperature is to be incubated under 800 ℃～1100 ℃, preferably is incubated 6～20 hours.Pressure in the reaction vessel is had no particular limits, and preferably in whole heat treatment process, a 0.1MPa～0.13MPa keep-ups pressure.After the thermal treatment, water is rinsed tantalum crucible well, uses after the oven dry again.
The heat treated tantalum crucible of The above results can carry out high-temperature heat treatment according to identical or different condition again after reusing several times, carry out repeatedly circularly so repeatedly.
Embodiment 1
Used 40 times 20 of tantalum crucibles to pack in the heatproof stainless steel vessel in thermal treatment tantalum powder, and about 60 gram sodium Metal 99.5s are packed in the container, 200 gram metal magnesium chips are sprinkling upon in each crucible dispersedly, are evacuated down to 150Pa, charge into argon gas, making the pressure in the reaction vessel is 0.12MPa, be warmed up to 950 ℃, insulation is 8 hours under the pressure of about 0.12MPa, then cool to room temperature, tantalum crucible is taken out, continue on for the thermal treatment of tantalum powder after the water flushing oven dry.After reusing 40 times, still tantalum crucible is carried out the flexible thermal treatment that recovers for the second time, use again 40 times, carry out the flexible thermal treatment that recovers according to above-mentioned condition for the third time according to the tantalum crucible after the inventive method thermal treatment according to above-mentioned condition.
Tantalum crucible after the thermal treatment for the third time (using altogether 120 times) is knocked with hammer, and tantalum crucible is distortion just, but does not break.
Embodiment 2
Used 40 times 26 of tantalum crucibles to pack in the heatproof stainless steel vessel in thermal treatment tantalum powder, and about 100 gram sodium Metal 99.5s are packed in the container, 250 gram metal magnesium chips are sprinkling upon in each crucible dispersedly, are evacuated down to 150Pa, charge into argon gas, making the pressure in the reaction vessel is 0.12MPa, be warmed up to 800 ℃, insulation is 18 hours under the pressure of about 0.12MPa, then cool to room temperature, tantalum crucible is taken out, continue on for the thermal treatment of tantalum powder after the water flushing oven dry.After reusing 40 times, according to the heat-treat condition shove charge first time, just for the second time be warmed up to 900 ℃, insulation is 10 hours under the pressure of about 0.12MPa.Tantalum crucible after the thermal treatment second time is used again 40 times, according to the heat-treat condition shove charge first time, just be warmed up to 1000 ℃ in the thermal treatment for the third time, insulation is 10 hours under the pressure of about 0.12MPa.
Tantalum crucible after the thermal treatment for the third time (using altogether 120 times) is knocked with hammer, and tantalum crucible is distortion just, but does not break.
Embodiment 3
Used 40 times 15 of tantalum crucibles to pack in the heatproof stainless steel vessel in thermal treatment tantalum powder, and about 100 gram sodium Metal 99.5s are packed in the container, 250 gram metal magnesium chips are sprinkling upon in each crucible dispersedly, are evacuated down to 150Pa, charge into argon gas, making the pressure in the reaction vessel is 0.12MPa, be warmed up to 1000 ℃, insulation is 12 hours under the pressure of about 0.12MPa, then cool to room temperature, tantalum crucible is taken out, continue on for the thermal treatment of tantalum powder after the water flushing oven dry.After reusing 40 times, according to the first time heat-treat condition heat-treat.Tantalum crucible after the thermal treatment second time is used again 40 times, according to the first time heat-treat condition heat-treat.
Tantalum crucible after the thermal treatment for the third time (using altogether 120 times) is knocked with hammer, and tantalum crucible is distortion just, but does not break.
Comparative example
Get 20 tantalum crucibles, be used for the thermal treatment of tantalum powder, use 50 times continuously after, begin to have 3 rhegma to occur, continue to use, use 57 times after, have rhegma 12 times.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, though the present invention discloses as above with preferred embodiment, yet be not in order to limit the present invention, any those skilled in the art, in not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be not break away from the technical solution of the present invention content, according to technical spirit of the present invention to any simple modification that above embodiment did, equivalent variations and modification all still belong in the scope of technical solution of the present invention.
Claims (3)
1. the heat treating method of a tantalum crucible is characterized in that, tantalum crucible has been placed in alkaline-earth metal and the alkali-metal atmosphere carried out high-temperature heat treatment, and described thermal treatment is carried out under 700 ℃～1050 ℃ temperature, and described high-temperature heat treatment kept 5 hours at least.
2. the heat treating method of tantalum crucible as claimed in claim 1 is characterized in that, described high-temperature heat treatment kept 5～20 hours at least.
3. the heat treating method of tantalum crucible as claimed in claim 1 is characterized in that, described high-temperature heat treatment is carried out in the atmosphere of argon gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102041510A CN101880847B (en) | 2010-06-18 | 2010-06-18 | Heat treatment method of tantalum crucible |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102041510A CN101880847B (en) | 2010-06-18 | 2010-06-18 | Heat treatment method of tantalum crucible |
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| Publication Number | Publication Date |
|---|---|
| CN101880847A CN101880847A (en) | 2010-11-10 |
| CN101880847B true CN101880847B (en) | 2011-12-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102041510A Active CN101880847B (en) | 2010-06-18 | 2010-06-18 | Heat treatment method of tantalum crucible |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102965525B (en) * | 2012-12-05 | 2013-11-27 | 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 |
| CN113122830A (en) * | 2021-04-25 | 2021-07-16 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Tungsten sheet or tungsten crucible surface tantalum coating layer and preparation method thereof |
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| JPH0897096A (en) * | 1994-09-28 | 1996-04-12 | Sutaruku Buitetsuku Kk | Tantalum powder and electrolytic capacitor employing it |
| CN1073480C (en) * | 1998-05-08 | 2001-10-24 | 宁夏有色金属冶炼厂 | Method for producing titanium powder aggregates |
| IL156802A0 (en) * | 2001-01-11 | 2004-02-08 | Cabot Corp | Tantalum and niobium billets and methods of producing same |
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