DEP0049166DA - Process for the separation of niobium and tantalum. - Google Patents
Process for the separation of niobium and tantalum.Info
- Publication number
- DEP0049166DA DEP0049166DA DEP0049166DA DE P0049166D A DEP0049166D A DE P0049166DA DE P0049166D A DEP0049166D A DE P0049166DA
- Authority
- DE
- Germany
- Prior art keywords
- tantalum
- niobium
- gaseous
- nitride
- formation
- 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.)
- Expired
Links
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims description 14
- 229910052715 tantalum Inorganic materials 0.000 title claims description 13
- 239000010955 niobium Substances 0.000 title claims description 9
- 229910052758 niobium Inorganic materials 0.000 title claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 title claims description 6
- 238000000034 method Methods 0.000 title claims description 5
- 238000000926 separation method Methods 0.000 title description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 150000004767 nitrides Chemical class 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 2
- 238000009833 condensation Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 2
- WFKSADNZWSKCRZ-UHFFFAOYSA-N Diethatyl-ethyl Chemical compound CCOC(=O)CN(C(=O)CCl)C1=C(CC)C=CC=C1CC WFKSADNZWSKCRZ-UHFFFAOYSA-N 0.000 claims 1
- JUVIOZPCNVVQFO-HBGVWJBISA-N rotenone Chemical compound O([C@H](CC1=C2O3)C(C)=C)C1=CC=C2C(=O)[C@@H]1[C@H]3COC2=C1C=C(OC)C(OC)=C2 JUVIOZPCNVVQFO-HBGVWJBISA-N 0.000 claims 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 240000003834 Triticum spelta Species 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
Description
Pfm., den 15.7.Pfm., July 15
Sociltl Glalrai® Mitallnrglqu· d· liob©k«it Soel£ tiSociltl Glalrai® Mitallnrglqu · d · liob © k «i t Soel £ ti
Verfahren sur Trennung von Mob and Tantal«Procedure for the separation of mob and tantalum "
Di® Krfladung besieht sich auf die Behandlung von M®tall«ö der.5·Gruppe des jx*riodiechon Syst®®® und ingboeonder* auf die Trennung 3®s Miobs von Tantal, die bekanntlich a©hr schwierig 1st« Die Erfindung g«stßtfe®t @in® rasch« Trennung ύ®Β rUobs von Tantal und auch von anderen Metallen der S^rupi5® dee periodi®eh@n Systems durch ©is einfaohca ?®rfahr@ne Di® Krfladung refers to the treatment of M®tall «ö der.5 · Group of the jx * riodiechon Syst®®® and ingboeonder * to the separation of 3®s Miobs from tantalum, which is known to be extremely difficult« The invention g «stasstfe®t @ in® quickly« separation ύ®Β rUobs from tantalum and also from other metals of the S ^ rupi 5 ® dee periodi®eh @ n system by © is einfaohca? ®rfahr @ n e
Srfindtißgßgesass wird derart ¥®rf®hr®ne dass ein Stoffgemis©ne das Klob tind Tantal la F@r® von Pettto^don »nt» haltg d@F Fiaiiirkung ©in®@ ffltri^d® bild®ad@n läitt®ls9 se^e gasförmigem 4^ioniake unt@rworf@Q wird unter Bedingungen^ bei denen ffiob-Ptntox^d in Niob-Hitrid umgewandelt «ilrd und das gebildet© !fiob-Nitrid ä®r Wirkung tines hmlog@nier<®n<l®n MittelsSrfindtißgßgesass is such ¥ ®rf®hr®n e that a Stoffgemis © n e the Klob tind tantalum la F @ r® of Pettto ^ don "nt" haltg d @ F Fiaiiirkung © in® @ ^ ffltri d® bild®ad @ In läitt®ls 9 s e ^ e gaseous 4 ^ ioniak e unt @ rworf @ Q is converted into niobium nitride under conditions in which ffiobium ptntox ^ d is converted into niobium nitride and the! fiob nitride is formed for its effect hmlog @ nier <®n <l®n means
wird ι ύ&Μ ία ein flüchtiges Ni©b=-Hadog@nld über» wirdg das dann durch ttegtillatloa und Kondensationif ι ύ & Μ ία a volatile Ni © b = -Hadog @ nld over »it is then through ttegtillatloa and condensation
wa dem Tantal->P®nt@ijd ftwonnen wirde als Haloge-wa the tantalum-> P®nt @ ijd ftwonnen e as halogen-
kdnn@n Ohl&r9 Bros @dnr Jod oder mersetslioh® d@r
Die
folg@n4@fökdnn @ n Ohl & r 9 Bros @dnr iodine or mersetslioh® d @ r
the
follow @ n4 @ fö
2 WB «· 5 OX9 m 2'llbGl.·»-2 WB «· 5 OX 9 m 2'llbGl. ·» -
£->Stra)iienprüfiiag@a hsb@n g®m@igt8 dass di® Umwandlung von Niob Iq Nitride gogon 6@© beginnt 9 während di® Reaktion mit Tantal @rst b@i @twa 8©©° anfängt,, Infolgedessen wird die Umwandlung des Kiobs ia Nitrid bei dem vorstehend erläuterten Verfahren »wischen 6o©° aod βοοθ @ TOrsugs^sis® la der Haönb&rseaaft ψοά etwa 7®@° durchgeführt.£ -> Stra) iienprüfiiag @ a hsb @ ng®m @ igt 8 that the conversion of niobium Iq Nitride gogon 6 @ © starts 9 while the reaction with tantalum @rst b @ i @ about 8 starts. As a result, the conversion of the Kiobs ia nitride is carried out in the process explained above »wischen 6o © ° aod βοο θ @ TOrsugs ^ sis® la der Haönb & rseaaft ψοά about 7® @ °.
«.ach d®r physikaliseh® Zustand de® ία ¥®mrb@ifc@ad@a Oxydg®slashes besitit eine gewisse B#d®tifeungö Mit Vorteil «erden präcipitiert® Osjd® angewendete Di® R©dtikti©M|i©dißgiiag©B ©in ."»eaig variieren je nach d®r Katar dtr O^d® tmd d@a turen, bei weleh.@a ei© ¥orh®r ©srö®t©t worden«.According to the physical state of the® ία ¥ ®mrb @ ifc @ ad @ a Oxydg®slashes has a certain B # d®tifeung ö It is advantageous to« earth precipitiert® Osjd® applied Di® R © dtikti © M | i © dißgiiag © B © in. "» eaig vary depending on d®r Qatar dtr O ^ d® tmd d @ a tures, at which. @ a ei © ¥ orh®r © srö®t © t
B@i 7@®Θ dlsso©ii©rt das A©m@ai®k in »Ίο ßefoaden «tirdt, kaaa aaeh ©ine Mi@chnag ¥»& Stickstoff .und wasserstoff fir di® Uawaadiimg d©r Q^jd® Is Hitrid® v©re@nd@t la dies©» Fall® liegt jedoefi di© Temp@i?attiF mkx für ditB @ i 7 @ ® Θ dlsso © ii © rt the A © m @ ai®k in »Ίο ßefoaden« tirdt, kaaa aaeh © ine Mi @ chnag ¥ »& nitrogen. And hydrogen fir di® Uawaadiimg d © r Q ^ jd® Is Hitrid® v © re @ nd @ t la dies © »Fall® is jedoefi di © Temp @ i? attiF mkx for dit
in HitoiS® hötero Bei anwendung ®in®r Mischung fön Wasserstoffgai und Stiekstoff ®ntsp?eah@ad der Forsisl des afflffloaiak» liegt di® Umwaadltmgstempcirattir %eB0 bei etwa 9oo°ein HitoiS® higher o When using a ®in®r mixture for hydrogen gas and carbon dioxide ®ntsp? eah @ ad der Forsisl des afflffloaiak », the Umwaadltmgstempcirattir % e B 0 is about 900 ° e
Xn msmctmn Fällen g®h@is. gerlog* Mang©η τοα Tantal in das kondensiert© NioboMorid \ib®w* Dies beruht auf fei©s©ag w®leh® oadhst@h@nd korn besehri@b@a ^©rd#a @©ll@ae Xn msmctmn cases g®h @ is. gerlog * Mang © η τοα tantalum condensed into the © NioboMorid \ ib®w * This is based on fei © s © a g w®leh® oadhst @ h @ nd korn besehri @ b @ a ^ © rd # a @ © ll @ a e
Da Tantal ©in© äöii®?® kifimit&t stö Stickstoff alt st als Niob kann ein Austaoaoh T@fi Stickstoff aa@h d@r Formel 2 HM ♦ ?@2°5 ° 2 Ts^ * ^2°5 stGfctf ijadG^o Das g®bild®t@ Tastalnitriä witd alsdmnn ehlori®rt and das gebildete Tantal» ©älorid (TmCIc) g®at al® ?©ruar@iiiig(ing in das produkt über e Di®©© R©akti@a Te rl auf t inS®ss@a langsaae da si® mir tei Kontakt ued Diffusion stattfinde« Um ©in® möglichst vollständig® fr^HQüog ι® β^Ι®Ι#®§ ®epf!©felt ©s oi©h9 das Tr®fintings¥@rfakKn bei TOEfe-äl-fealsoasslg ni@dr£g®r Temperatur in kartei1 Zeit, tmd mit @in®r pul^®rförmi@«i Misehong a9 Since tantalum © in © äöii®? ® kifimit & t stö nitrogen old st than niobium, an Austaoaoh T @ fi nitrogen aa @ hd @ r Formula 2 HM ♦? @ 2 ° 5 ° 2 Ts ^ * ^ 2 ° 5 st Gfctf ijadG ^ o The g®bild®t @ Tastalnitriä witd alsdmnn ehlori®rt and the tantalum formed »© älorid (TmCIc) g®at al®? © ruar @ iiiig (ing in the product via e Di® © © R © akti @ a Te rl auf t inS®ss @ a langsaa e da si® with partial contact and diffusion take place «Um © in® as completely as possible® for ^ HQüog ι® β ^ Ι®Ι # ® § ®epf! © felt © s oi © h 9 das Tr®fintings ¥ @ rfakKn at TOEfe-äl-fealsoasslg ni @ dr £ g®r temperature in kartei 1 time, tmd with @ in®r pul ^ ®rörmi @ «i Misehong a 9
Ela® ander® ilmaebi für di® ¥©raar©iaif|uitg©ffi des kann auf dsr Bildimg ¥«m Miob®*j®U.oi?id is Sinn®Ela® anders® ilmaebi for di® ¥ © raar © iaif | uitg © ffi des can on the picture img ¥ «m Miob® * j®U.oi? Id is Sinn®
d#r Ροέ®®1 5 RbGLe * fa^o^—=> IbOCl g φ 5 TmCIc beruhen· Di®s@ R©akti@a ksM& während ά®τ Gttl®ri@fti£ig @tattfiBd#a@ 9Mm dasd # r Ροέ®®1 5 RbGLe * fa ^ o ^ - => IbOCl g φ 5 TmCIc based Di®s @ R © akti @ a ksM & while ά®τ Gttl®ri @ fti £ ig @ tattfiBd # a @ 9mm that
gemisches durchdringt. Hierbei können nicht unbeträchtliche Verluste an Tantal entstehen % wenn örtliche Uebrrhitaung®n stattfinden« lim. Ueberhitzungen und die dadurch bedingten teile zu vermeiden* empfiehlt es oichs dom Chlor ein ine üaSg g.B,stickstoff@ ziiaumiachen« IUe Gase der ünlorieruagsoperation^ weiche Stickstoff enthalten^ können zu diesem ?@rw@n<iung finden, nuf all® Falle empfiehlt es BiCh1 alt dünnen Schichten au arbeiten und di« Chlorierung bei den niedrigsten Temperaturen durchsuführeaf welche f ;r e Ine genügend rasche Durchfihraag dee Vorgang» In Betracht kommen.mixture penetrates. Not inconsiderable losses of tantalum can occur here % if local overruns take place « lim. Overheating and the consequent parts to avoid * it is recommended Oich s dom of chlorine ine üaSg gB, nitrogen @ ziiaumiachen "IUE gases of ünlorieruagsoperation ^ ^ soft contain nitrogen can this? @ Rw @ n <iung find nuf all® case recommends it work au Bich one old thin layers and di «chlorination at the lowest temperatures durchsuführea f that f; re Ine sufficiently rapid Durchfihraag dee process" come to be considered.
In eixiom typischen Fall wurden Geraisohe von Wiob— oxyd und Taataloxyd bei Temperataren von et*a 9oo° mit gasförmige® ammoniak behandelt. Die Oxyde enthalten H7t*$- Nb0O1- und 49t9^ Ta2Oc* H&ch 2/2 stunden war der Wass®rstoff durch stickstoff ersetzt und die Temperatur auf etwa ^oo° erniedrigt« Die Chlorierung mit reines Chlor dauerte eine halbe •;'tundee In a typical case, Geraisohe von Wioboxyd and Taataloxyd were treated with gaseous ammonia at temperatures of about 900 °. The oxides contain H7 t * $ - Nb 0 O 1 - and 49t9 ^ Ta 2 Oc * H & ch 2/2 hours the hydrogen was replaced by nitrogen and the temperature lowered to about 60 °. The chlorination with pure chlorine lasted one hour half • ; 'tunde e
'v'ach erfolgter Chlorierung''enthielt d©r Rückstand 1896$ Nb3O, und ?B9&X ^2"V ^^^ß®84^^ *tur&®a etwa 83»5^ abgetrennt»After the chlorination, the residue contained 18 9 6 $ Nb 3 O, and ? B 9 & X ^ 2 "V ^^^ ß® 84 ^^ * tur & ®a about 83» 5 ^ separated »
Durchführung der Jm van dl u/ig in Nitride beiCarrying out the Jm van dl u / ig in nitrides at
7oo° w'ihrend 13 /2 Pt linden- enthielt der GhlorierqngsrückatandThe ghlorierqngsrückatand contained 7oo ° while 13/2 pt
t Nb^O1- und '88»o?< Tao0ce :!iefb@l «urd@n 83?' d@s Nlobe abgetrennt. Immerhin gingen 4fS* d®s Tantals in das kondensierte "iioböhlorid übere t Nb ^ O 1 - and '88 »o <Ta o ce 0: IEFB @ l" urd @ n 83 '? d @ s Nlobe separated. After all, 4 f S * d®s tantalum went into the condensed "iioböhlorid over e
Beim arbeiten ait ®in#r Mischung von Jhlor und Stickstoff wird eiae erheblich besser® Separation des NiobsWhen working with a mixture of chlorine and nitrogen, the separation of the niobium is considerably better
Claims (1)
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