CN1425077A - 用氢化的吸气剂合金纯化有机金属化合物或杂原子有机化合物的方法 - Google Patents
用氢化的吸气剂合金纯化有机金属化合物或杂原子有机化合物的方法 Download PDFInfo
- Publication number
- CN1425077A CN1425077A CN01808292A CN01808292A CN1425077A CN 1425077 A CN1425077 A CN 1425077A CN 01808292 A CN01808292 A CN 01808292A CN 01808292 A CN01808292 A CN 01808292A CN 1425077 A CN1425077 A CN 1425077A
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- China
- Prior art keywords
- tetramethyl
- heptane
- ketonize
- compound
- iron
- 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.)
- Granted
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 53
- 239000000956 alloy Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 35
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- 238000000746 purification Methods 0.000 title claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 42
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000007789 gas Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 claims abstract description 21
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 125000002524 organometallic group Chemical group 0.000 claims abstract description 17
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- 239000012159 carrier gas Substances 0.000 claims abstract description 10
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 10
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 10
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 8
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- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 4
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- RVIXKDRPFPUUOO-UHFFFAOYSA-N dimethylselenide Chemical compound C[Se]C RVIXKDRPFPUUOO-UHFFFAOYSA-N 0.000 claims description 4
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- 239000011777 magnesium Substances 0.000 claims description 4
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- 239000000126 substance Substances 0.000 claims description 4
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- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
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- 229910052723 transition metal Inorganic materials 0.000 claims description 3
- 150000003624 transition metals Chemical class 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- JFVGXQWOTDPEFY-UHFFFAOYSA-N 1,1,1,2-tetraethoxy-2,3,3,4-tetramethylheptane Chemical compound CC(C(C(C(OCC)(OCC)OCC)(OCC)C)(C)C)CCC JFVGXQWOTDPEFY-UHFFFAOYSA-N 0.000 claims description 2
- KIHWDDBAWFJUAA-UHFFFAOYSA-N 1,1,1,2-tetramethoxy-2,3,3,4-tetramethylheptane Chemical compound CC(C(C(C(OC)(OC)OC)(OC)C)(C)C)CCC KIHWDDBAWFJUAA-UHFFFAOYSA-N 0.000 claims description 2
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 claims description 2
- YTNSNFSZEOAYRF-UHFFFAOYSA-N CN(C)C.P Chemical compound CN(C)C.P YTNSNFSZEOAYRF-UHFFFAOYSA-N 0.000 claims description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 2
- 241000588731 Hafnia Species 0.000 claims description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 2
- 125000003368 amide group Chemical group 0.000 claims description 2
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- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- AZWXAPCAJCYGIA-UHFFFAOYSA-N bis(2-methylpropyl)alumane Chemical compound CC(C)C[AlH]CC(C)C AZWXAPCAJCYGIA-UHFFFAOYSA-N 0.000 claims description 2
- 229910000085 borane Inorganic materials 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 claims description 2
- UJYLYGDHTIVYRI-UHFFFAOYSA-N cadmium(2+);ethane Chemical compound [Cd+2].[CH2-]C.[CH2-]C UJYLYGDHTIVYRI-UHFFFAOYSA-N 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 229910052804 chromium Inorganic materials 0.000 claims description 2
- 239000011651 chromium Substances 0.000 claims description 2
- UZBQIPPOMKBLAS-UHFFFAOYSA-N diethylazanide Chemical compound CC[N-]CC UZBQIPPOMKBLAS-UHFFFAOYSA-N 0.000 claims description 2
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical group CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 claims description 2
- SIPUZPBQZHNSDW-UHFFFAOYSA-N diisobutylaluminium hydride Substances CC(C)C[Al]CC(C)C SIPUZPBQZHNSDW-UHFFFAOYSA-N 0.000 claims description 2
- YMUZFVVKDBZHGP-UHFFFAOYSA-N dimethyl telluride Chemical compound C[Te]C YMUZFVVKDBZHGP-UHFFFAOYSA-N 0.000 claims description 2
- GCPCLEKQVMKXJM-UHFFFAOYSA-N ethoxy(diethyl)alumane Chemical compound CCO[Al](CC)CC GCPCLEKQVMKXJM-UHFFFAOYSA-N 0.000 claims description 2
- JMMJWXHSCXIWRF-UHFFFAOYSA-N ethyl(dimethyl)indigane Chemical compound CC[In](C)C JMMJWXHSCXIWRF-UHFFFAOYSA-N 0.000 claims description 2
- ALCDAWARCQFJBA-UHFFFAOYSA-N ethylselanylethane Chemical compound CC[Se]CC ALCDAWARCQFJBA-UHFFFAOYSA-N 0.000 claims description 2
- ILXWFJOFKUNZJA-UHFFFAOYSA-N ethyltellanylethane Chemical group CC[Te]CC ILXWFJOFKUNZJA-UHFFFAOYSA-N 0.000 claims description 2
- 150000002222 fluorine compounds Chemical class 0.000 claims description 2
- 229910052733 gallium Inorganic materials 0.000 claims description 2
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- 150000003949 imides Chemical class 0.000 claims description 2
- 229910052753 mercury Inorganic materials 0.000 claims description 2
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims description 2
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- ZGNPLWZYVAFUNZ-UHFFFAOYSA-N tert-butylphosphane Chemical compound CC(C)(C)P ZGNPLWZYVAFUNZ-UHFFFAOYSA-N 0.000 claims description 2
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- UORVGPXVDQYIDP-UHFFFAOYSA-N trihydridoboron Substances B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 claims description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 claims description 2
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- 239000002904 solvent Substances 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
一种纯化有机金属化合物或杂原子有机化合物，除去氧、水以及由水和氧与欲纯化的有机金属或杂原子化合物的反应中产生的化合物的方法，包括将液态、纯粹的或载气中蒸气形式的待纯化的有机金属或杂原子化合物与氢化的吸气剂合金，以及任选的一种或多种气体吸收材料接触的操作，所述气体吸收材料选自多孔载体上的钯和载于沸石上的铁和锰的混合物。
Description
本发明涉及一种用氢化的吸气剂合金纯化有机金属化合物或杂原子有机化合物的方法。
有机金属化合物的特征在于在一个金属原子(在金属中还包括砷、硒或碲)和一个碳原子之间存在键，所述碳原子构成，例如脂族或芳族，饱和或不饱和的烃基的有机基团的一部分；引申开来，有机金属化合物的定义就是含有通过碳之外的原子，与有机基团，例如醇基(-OR)或酯基(-O-CO-R)，键F合的金属原子的化合物。
杂原子有机化合物(以下也简单定义为杂原子的)是那些除碳和氢之外，还含有，例如氧、氮、卤素、硫、磷、硅和硼的原子的有机化合物。
这些化合物中的许多已经长期用于传统的化学应用。在该领域中，一般不需要纯度非常高的试剂，并且它们的纯化是通过，例如蒸馏(任选在减压下，以降低沸点并因此减少化合物热分解的危险)或从溶剂中重结晶的技术进行的。
但是，最近这些化合物已经被用于高技术应用，特别是半导体工业。在这些应用中，有机金属化合物和杂原子化合物被作为试剂，用于从气态进行化学沉积的工艺(已知本领域定义为“化学蒸汽淀积”并简称为CVD)中。在这些技术中，一种或多种有机金属或杂原子化合物的气流(或含有已知浓度的上述化合物的载气流)被传输到操作室；并且在操作室中，化合物被随后分解或反应，并因此就地形成了含金属原子或杂原子的原料(一般以薄层形式)。有机金属或杂原子化合物可以已经是气态，但其也可以是液体形式。在上述第二种情况下，通过蒸发化合物(此时气流仅由感兴趣的化合物组成)或通过向容器中的液体鼓入气体(此时气流含有载气中的化合物蒸气)得到化合物的气流。
用于这些应用中的主要的有机金属气体是四叔丁氧化铪、三甲基铝、三乙基铝、三叔丁基铝、氢化二异丁基铝、氯化二甲基铝、乙氧基化二乙基铝、氢化二甲基铝、三甲基锑、三乙基锑、三异丙基锑、三-二甲基氨基锑、苯基胂、三甲基砷、三-二甲基氨基砷、叔丁基胂、双-四甲基庚烷二酮化(bis-tetramethylheptanedionate)钡、三-四甲基庚烷二酮化铋、二甲基镉、二乙基镉、五羰基铁、双-环戊二烯基铁、三-乙酰丙酮化铁、三-四甲基庚烷二酮化铁、三甲基镓、三乙基镓、三异丙基镓、三异丁基镓、三甲基铟、三乙基铟、二甲基乙基铟、三-四甲基庚烷二酮化钇、三-四甲基庚烷二酮化镧、双-甲基环戊二烯基镁、双-环戊二烯基镁、双-四甲基庚烷二酮化镁、二甲基汞、乙酰丙酮化二甲基金、双-四甲基庚烷二酮化铅、乙酰丙酮化双-六氟化铜、双-四甲基庚烷二酮化铜、二甲基硒、二乙基硒、三-四甲基庚烷二酮化钪、四甲基锡、四乙基锡、双-四甲基庚烷二酮化锶、四甲基四乙氧基庚烷二酮化钽、四甲基四甲氧基庚烷二酮化钽、四甲基四异丙氧基庚烷二酮化钽、三-二乙基叔丁基酰氨基酰亚胺钽、二乙基碲、二异丙基碲、二甲基碲、双-四甲基-双-异丙氧基庚烷二酮化钛、四二甲基酰胺钛、四二乙基酰胺钛、二甲基锌、二乙基锌、双-四甲基庚烷二酮化锌、四-四甲基庚烷二酮化锆、四甲基-三-异丙氧基庚烷二酮化锆和双-乙酰丙酮化锌。
用于这些应用的主要的杂原子化合物是三甲基硼烷、不对称的二甲基肼(即其中两个甲基键连在相同的氮原子上)、叔丁胺、苯基肼、三甲基磷、叔丁基膦和叔丁基硫醇。
这些方法的一些典型的应用例子是例如GaAs或InP的III-V型，或者例如ZnSe的II-VI型半导体的制备；用于传统硅基半导体装置的p掺杂(例如与硼)或n掺杂(例如与磷)的用途；用于铁电存储元件的具有高介电常数的材料(例如，诸如PbZrxTi1-xO3的化合物)的制备；或者用于半导体装置中绝缘电接点的具有低介电常数的材料(例如SiO2)的制备。
为了上述应用，需要试剂必须具有10-1-10-2ppm数量级水平的非常高的纯度，而传统的化学技术不能达到杂质含量低于约10ppm的水平。而且，甚至在制备纯度非常高的有机金属或杂原子化合物的情况下，因为从容器壁释放的气体，存储成为了污染的来源，使得无论如何需要在即将应用之前使用净化器(因此称为“使用瞬时(point-of-use)净化器”)。
专利US5470555描述了通过使用由铜或镍金属形成的催化剂，或通过用氢气还原活化，沉积在例如氧化铝、二氧化硅或硅酸盐的相关氧化物，从有机金属化合物中脱除作为杂质存在的氧气。根据该专利，通过这一方法，从有机金属化合物流中脱除氧气最低可达到10-2ppm的值。
但是，氧气不是必须从有机金属化合物或杂原子化合物中除去的仅有的杂质。其它有害于CVD操作的杂质是例如水，以及特别是由同一有机金属化合物或杂原子化合物的蚀变(alteration)产生的物质，所述蚀变通常是伴随着与水或氧的不希望的反应的。例如，在普通的有机金属化合物MRn的情况下，其中M表示金属，R是有机基团，且n是金属M的化合价，会由MRn-x(-OR)x物质产生污染，其中x是在1和n之间变化的整数。这些氧化的物质有害于CVD操作，因为它们将氧原子引入到即将形成的物质中，因此明显地改变了其电特性。
本发明的目的在于提供了一种纯化有机金属化合物或杂原子有机化合物，除去氧、水以及由水和氧与欲纯化的有机金属或杂原子化合物的反应中产生的化合物的方法。
本发明的这一目的可以通过以下方法实现：其中将待纯化的有机金属或杂原子化合物与氢化的吸气剂合金接触。纯化可以在液态或气态的有机金属或杂原子化合物上进行。
除吸气剂合金之外，还可以使用其它的杂质吸附材料，例如多孔载体上的钯和载于沸石上的铁和锰的混合物。
吸气剂合金在用于微电子工业的惰性气体、氮气或氢气的纯化中的用途是已知的。此外，从专利EP-B-470936中可知氢化的吸气剂合金在简单氢化物，例如SiH4、PH3和AsH3的纯化中的用途。
但是，已经发现，氢化的吸气剂合金还能够从有机金属或杂原子化合物(液体，或以纯粹的或载气中的蒸气形式)中除去水和氧，并且将含MRn-x(-OR)x型氧的物质转化为最初的化合物或MRn-xHx型的化合物，所述化合物因其不含氧而无害于CVD操作。
以下将参照附图描述本发明，其中：
-图1显示了本发明方法的第一实施方案中可能使用的纯化器的剖视图；
-图2显示了本发明方法的第二实施方案中可能使用的纯化器的剖视图。
在其一个实施方案中，本发明方法的要素在于将氢化的吸气剂合金与液态的待纯化的化合物接触。所述接触可以通过将吸气剂合金引入液体化合物的容器而简单进行，液体化合物通过加热或与载气一起从该容器中蒸发。
但是，在优选实施方案中，纯化是通过将氢化的吸气剂合金与有机金属或杂原子化合物的纯粹的或载气中的蒸气接触而进行的。接下来，特别参考气态下的纯化描述本发明，因为所述条件是工业中最常用的。
适用于本发明的吸气剂合金是基于钛和/或锆与一种或多种选自过渡金属和铝的元素的合金，以及一种或多种这些合金与钛和/或锆的混合物。特别用于本发明的是：
-申请人的专利US5180568中描述的合金ZrM2，其中M是选自Cr、Mn、Fe、Co或Ni的一种或多种过渡金属；
-由申请人制造和销售的名称为St909的金属间化合物Zr1Mn1Fe1；
-申请人的专利US4312669中描述的合金Zr-V-Fe，其绘制为组合物三元图表的组合物重量百分比，包括在具有以下的点的顶角的三角形中：a)Zr75％-V20％-Fe5％；b)Zr45％-V20％-Fe35％；c)Zr45％-V50％-Fe5％以及特别是申请人生产和销售的名称为St707的合金，其组分的重量百分比是Zr70％-V24.6％-Fe5.4％；
-申请人生产和销售的名称为St737的金属间化合物Zr1V1Fe1；
-申请人的专利US5961750中描述的合金Zr-Co-A，其绘制为组合物三元图表的组合物的重量百分比包括在具有以下的点的顶角的多角形中：a)Zr81％-Co9％-A10％b)Zr68％-Co22％-A10％c)Zr74％-Co24％-A2％d)Zr88％-Co10％-A2％
其中A是选自钇、镧、稀土元素或这些元素的混合物的任意元素；以及特别是由申请人生产和销售的名称为St787的合金，其组分的重量百分比是Zr80.8％-Co14.2％-A5％；
-Ti-Ni合金；
-专利US4457891中描述的Ti-V-Mn。
用氢气加载上述合金通常采用已经位于最后容器(纯化器的腔体)中的合金进行的。该操作在室温和约400℃的温度下进行。高于400℃的温度是不可取的，因为加载到合金上的氢气的最大量将随着温度的升高而下降。可以使用最高约10bar的氢气压力进行操作，优选高于大气压。高于10bar的压力是不可取的，因为需要使用特殊的装置和安全系统，与较低的压力相比不会带来特殊的优点，而压力低于大气压则需要在纯化器的下游使用真空系统，以形成氢化所需的气流。实际上，氢化可以以各种方式进行。例如，可以在合金上传输氢气和其它气体的混合物(例如氢气和氩气的50％混合物)流，并监测出口气体的组分，当检测到后者的氢气压力高于预定值时，停止反应。或者，可实验性地确定用于各合金的确定的步骤。例如，在上述的合金St707的情况下，传输氩气流，以除去体系中存在的空气；数分钟后，在氩气流中于350℃开始预热。且氢气的流量与氩气的流量相等，因此形成了两种气体的50％混合物，保持该条件3小时；中断氩气流，同时将温度降低至150℃并保持该条件1.5小时；随后中断氢气流，同时将氩气流再打开0.5小时，无需加热；最后，关闭位于纯化器上游和下游的两个阀门，隔离纯化器。
用于纯化有机金属或杂原子化合物的温度范围约室温至约100℃，低于室温的温度下，限制了氧的除去，而在高于约100℃的温度下，可能会产生待纯化化合物的分解反应。
在优选约1-10bar的绝对压力下，待纯化的气流可以在约0.1-20slpm(在标准条件下测量的升气体/每分钟)范围内变化。
该气流可以仅由待纯化化合物的蒸气形成，也可以由所述蒸气在载气流中形成。载气可以是对氢化的吸气剂合金(或其它可能使用的气体吸收材料)和沉积操作(其中使用了有机金属或杂原子化合物)都没有影响的任何气体。常用的是氩气、氮气甚至氢气。
图1是可能用于本发明方法的第一实施方案的纯化器的剖视图。纯化器10由通常是柱状的腔体11组成；在腔体11的两端，提供了配管12，用作气体进入纯化器的入口，以及配管13，用作气体出口。吸气剂合金14位于腔体11内部。气体的入口12和出口13优选提供VCR型的标准连接件，所述标准连接件是本领域已知(图中未示出)的与纯化器的上游和下游气体管线的连接件。纯化器的腔体可以由各种金属材料制造，用于此目的的优选材料是钢AISI316。优选将与气体接触的纯化器腔体的内表面电抛光，直至得到低于约0.5μm的表面粗糙度。为了防止纯化器下游的出口气流携带的痕量吸气剂合金粉末，可以在纯化器腔体的出口13处放置保留颗粒的装置，例如网状物或多孔的隔片，其“空隙”或孔的尺寸适于留住颗粒而不会导致气流的过量压力降低；这些开口的尺寸通常是约10-0.003μm。在纯化器中，吸气剂合金14以粉末形式存在，但优选如图所示，以压缩粉末得到的片状形式使用。
除氢化的吸气剂合金之外，待纯化的气体流还与至少一种其它材料接触，所述其它材料选自多孔载体上的钯和载于沸石的铁和锰的混合物，或以上二者。
载于多孔载体的钯形成的材料优选含0.3-4重量％的金属。多孔载体可以是本领域常用的任何材料，例如分子筛、沸石、陶瓷、多孔玻璃等。许多生产用于化学工业的催化剂的公司出售载于多孔载体的含钯催化剂，例如Süd Chemie、Degussa和Engelhard公司。使用该材料的最佳温度是约-20℃至100℃，优选介于约室温至50℃。
由载于沸石的铁和锰的混合物形成的材料优选具有7∶1至1∶1的铁和锰的重量比，更优选该比值为约2∶1。该材料可以根据申请人的专利US5716588中描述的形式制备。使用该材料的最佳温度是-20℃至100℃，优选室温至50℃。
其它的材料(或其它的材料等)可以沿气流的方向，有差别地位于氢化的吸气剂合金的上游或下游。当使用上述其它的两种材料时，也可以它们中的一种位于氢化的吸气剂合金的上游，而另一种位于下游。
其它的材料(或其它的材料等)优选放置于分离的腔体中，所述分离的腔体通过配管和接头与含有氢化的吸气剂合金的纯化器的腔体11相连，例如上述的VCR型。该第二腔体的制造材料和表面加工水平优选与所述腔体11相同。
优选将其它材料(或其它的材料等)安置于提供了氢化的吸气剂合金的同一纯化器腔体中。此时，不同的材料可以混合，但它们在纯化器腔体中优选是分离的。
图2是含有多于一种材料(以两种材料的情况为例)的可能的纯化器的剖视图。该图特别显示了根据优选方式制造的纯化器，其中不同的材料分别放置于纯化器腔体中。纯化器20由腔体21、气体入口22和气体出口23组成；在腔体21的内部，氢化的吸气剂合金24放置于入口22一侧，而在出口23一侧放置了材料25，所述材料25选自载于多孔载体的钯或载于沸石的铁和锰的混合物；优选在两种材料之间放置易于透过气体的机械部件26，例如金属网，以帮助保持二者的分离并保持材料最初的几何分布。
在两种不同的材料在同一时间存在于同一腔体的情况下(图2举例的情况)，纯化器应保持在与所有已有材料的操作温度一致的温度下，并因此优选介于室温至约50℃之间。
最后，还可以加入各种列举的材料，以及化学吸水剂，例如氧化钙和氧化硼，后者可以根据申请人的专利EP-A-960647的教导制备。
以下通过实施例进一步阐述本发明。该实施例并不限制发明的保护范围，并用于阐述可能的技术方案，用于教导本领域技术人员如何将本发明付诸实践，其可以视作本发明的最佳实施方式。
实施例1
制造图1所示的纯化器。纯化器的腔体由钢AISI316制造，内部容积为约50cm3。将72g片状的St707引入纯化器，其根据上述步骤氢化。随后，通过VCR连接件将纯化器的上游与含40ppm体积(ppmv)的水和100ppmv的氧的氮气瓶连接，下游与APIMS型质谱仪连接(常压电离质谱)，Sensar公司的TOF2000型，其对于水和氧均具有10-4ppmv的敏感阈值。实验在氮气而不是在有机金属化合物的蒸气流中进行，这是因为所用的分析仪(APIMS)在这些化合物的蒸气中敏感度降低，因此对有机金属化合物的实验不能得到明显的结果。在5bar下，将待纯化气体以0.1slpm的流量通过保持在室温下的纯化器。在实验开始时，纯化器气体出口的水和氧的量低于分析仪敏感阈值，这表明了氢化的吸气剂合金对于除去这些物质的官能度。继续实验，直至分析仪检测到纯化器出口气体中污染物含量为10-3ppmv；该出口气体污染物的值被用作纯化器损耗的指示。从实验数据可以看出，纯化器对于氧具有6l/l(在标准条件下测量的每升吸气剂合金的气体的升数)以及对水具有4l/l的生产能力。
Claims (23)
1、一种纯化有机金属化合物或杂原子有机化合物，除去氧、水以及由水和氧与欲纯化的有机金属或杂原子化合物的反应中产生的化合物的方法，包括将待纯化的有机金属或杂原子化合物与氢化的吸气剂合金接触的操作。
2、权利要求1的方法，其中氢化的吸气剂合金与纯粹的或与载气中蒸气形式的有机金属或杂原子化合物接触。
3、权利要求1的方法，其中吸气剂合金是基于钛和/或锆与一种或多种选自过渡金属和铝的元素的合金，以及一种或多种这些合金与钛和/或锆的混合物，并且用氢气加载是在室温至400℃和低于10bar的氢气压力下进行的。
4、权利要求3的方法，其中吸气剂合金的加载是在高于大气压的氢气压力下进行的。
5、权利要求3方法，其中氢化的吸气剂合金具有通式ZrM2，其中M是选自Cr、Mn、Fe、Co或Ni的一种或多种金属。
6、权利要求3方法，其中氢化的吸气剂合金是含有锆、钒和铁的合金，其绘制为组合物三元图表的组合物重量百分比，包括在具有以下的点的顶角的三角形中：
a)Zr75％-V20％-Fe5％；
b)Zr45％-V20％-Fe35％；
c)Zr45％-V50％-Fe5％。
7、权利要求3方法，其中氢化的吸气剂合金是含有锆、钴和选自钇、镧和稀土元素的一种或多种元素，其绘制为组合物三元图表的组合物的重量百分比包括在具有以下的点的顶角的多角形中：
a)Zr81％-Co9％-A10％
b)Zr68％-Co22％-A10％
c)Zr74％-Co24％-A2％
d)Zr88％-Co10％-A2％
其中A是选自钇、镧、稀土元素或这些元素混合物的任何元素。
8、权利要求3的方法，其中氢化的吸气剂合金是含有钛或镍的合金。
9、权利要求3的方法，其中氢化的吸气剂合金是含有钛、钒和锰的合金。
10、权利要求2的方法，其中所述操作在室温至约100℃的温度下进行。
11、权利要求2的方法，其中在约1-10bars的绝对压力下，所述操作以约0.1-20slpm待纯化气体流量进行。
12、权利要求1的方法，其中有机金属化合物选自四叔丁氧化铪、三甲基铝、三乙基铝、三叔丁基铝、氢化二异丁基铝、氯化二甲基铝、乙氧基化二乙基铝、氢化二甲基铝、三甲基锑、三乙基锑、三异丙基锑、三-二甲基氨基锑、苯基胂、三甲基砷、三-二甲基氨基砷、叔丁基胂、双-四甲基庚烷二酮化钡、三-四甲基庚烷二酮化铋、二甲基镉、二乙基镉、五羰基铁、双-环戊二烯基铁、三-乙酰丙酮化铁、三-四甲基庚烷二酮化铁、三甲基镓、三乙基镓、三异丙基镓、三异丁基镓、三甲基铟、三乙基铟、二甲基乙基铟、三-四甲基庚烷二酮化钇、三-四甲基庚烷二酮化镧、双-甲基环戊二烯基镁、双-环戊二烯基镁、双-四甲基庚烷二酮化镁、二甲基汞、乙酰丙酮化二甲基金、双-四甲基庚烷二酮化铅、乙酰丙酮化双-六氟化铜、双-四甲基庚烷二酮化铜、二甲基硒、二乙基硒、三-四甲基庚烷二酮化钪、四甲基锡、四乙基锡、双-四甲基庚烷二酮化锶、四甲基四乙氧基庚烷二酮化钽、四甲基四甲氧基庚烷二酮化钽、四甲基四异丙氧基庚烷二酮化钽、三-二乙基叔丁基酰氨基酰亚胺钽、二乙基碲、二异丙基碲、二甲基碲、双-四甲基-双-异丙氧基庚烷二酮化钛、四二甲基酰胺钛、四二乙基酰胺钛、二甲基锌、二乙基锌、双-四甲基庚烷二酮化锌、四-四甲基庚烷二酮化锆、四甲基-三-异丙氧基庚烷二酮化锆和双-乙酰丙酮化锌。
13、权利要求1的方法，其中杂原子有机化合物选自三甲基硼烷、不对称的二甲基肼、叔丁胺、苯基肼、三甲基磷、叔丁基膦和叔丁基硫醇。
14、权利要求1的方法，进一步包括将待纯化有机金属化合物或有机杂原子化合物与至少一种第二材料接触的操作，所述第二材料选自载于多孔载体的钯和载于沸石上的铁和锰的混合物。
15、权利要求14的方法，其中有机金属或杂原子化合物是纯蒸气或载气中蒸气的形式。
16、权利要求14的方法，其中第二材料是钯含量是0.3-4重量％的载于多孔载体的钯基催化剂。
17、权利要求15的方法，其中待纯化化合物与负载的钯的接触在约-20至100℃的温度下进行。
18、权利要求17的方法，其中所述接触在室温至50℃的温度下进行。
19、权利要求14方法，其中第二材料是载于沸石的铁和锰的混合物，其中铁和锰的重量比是7∶1至1∶1。
20、权利要求19的方法，其中所述重量比是约2∶1。
21、权利要求15的方法，其中待纯化的化合物与负载的铁和锰的混合物之间的接触在-20℃至100℃的温度下进行。
22、权利要求21的方法，其中所述接触在室温至50℃的温度下进行。
23、权利要求1的方法，其中还包括将待纯化有机金属或杂原子有机化合物与化学吸水剂进行接触的操作。
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| KR101294660B1 (ko) | 2011-04-26 | 2013-08-08 | 한국화학연구원 | 안티몬 아미노 알콕사이드 화합물 및 이의 제조방법 |
| CN103910753B (zh) * | 2013-01-06 | 2018-04-17 | 江苏爱姆欧光电材料有限公司 | 一种高纯烷基锌化合物的纯化方法 |
| CN108752179A (zh) * | 2018-07-16 | 2018-11-06 | 扬州工业职业技术学院 | 一种二甲基乙酰丙酮金的制备方法及其应用 |
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| IT1110271B (it) | 1979-02-05 | 1985-12-23 | Getters Spa | Lega ternaria getterante non evaporabile e metodo di suo impiego per l'assorbimento di acqua,vapore d'acqua,di altri gas |
| DE3210381C1 (de) | 1982-03-20 | 1983-05-19 | Daimler-Benz Ag, 7000 Stuttgart | Legierung zum Speichern von Wasserstoff |
| US4983194A (en) * | 1990-02-02 | 1991-01-08 | Air Products And Chemicals, Inc. | Production of high purity argon |
| IT1248676B (it) * | 1990-06-01 | 1995-01-26 | Getters Spa | Recupero di trizio e deuterio dai loro ossidi e composti intermetallici utili a questo scopo |
| IT1246358B (it) | 1990-07-12 | 1994-11-17 | Getters Spa | Processo per eliminare impurita' da un gas idruro |
| DE69202014T2 (de) | 1991-07-17 | 1995-08-31 | Japan Pionics | Verfahren zur Reinigung von gasförmigen organometallischen Verbindungen. |
| US5260585A (en) * | 1992-06-12 | 1993-11-09 | Novapure Corporation | Endpoint and/or back diffusion gas impurity detector, and method of using the same |
| US5385689A (en) * | 1993-06-29 | 1995-01-31 | Novapure Corporation | Process and composition for purifying semiconductor process gases to remove Lewis acid and oxidant impurities therefrom |
| IT1277458B1 (it) | 1995-08-07 | 1997-11-10 | Getters Spa | Processo per la rimozione di ossigeno da ammoniaca a temperatura ambiente |
| IT1290451B1 (it) | 1997-04-03 | 1998-12-03 | Getters Spa | Leghe getter non evaporabili |
| ITMI981138A1 (it) | 1998-05-21 | 1999-11-21 | Getters Spa | Processo per la rimozione di acqua da camere evacuate o da gas |
| US6521192B1 (en) * | 1999-08-06 | 2003-02-18 | Saes Pure Gas, Inc. | Rejuvenable ambient temperature purifier |
-
2001
- 2001-04-09 TW TW090108461A patent/TW550307B/zh not_active IP Right Cessation
- 2001-04-13 CN CN018082920A patent/CN1218065C/zh not_active Expired - Fee Related
- 2001-04-13 CN CN01808355A patent/CN1425078A/zh active Pending
- 2001-04-13 EP EP01925877A patent/EP1274879A1/en not_active Withdrawn
- 2001-04-13 KR KR1020027014012A patent/KR20030001435A/ko active IP Right Grant
- 2001-04-13 WO PCT/IT2001/000185 patent/WO2001079587A1/en not_active Application Discontinuation
- 2001-04-13 AU AU52549/01A patent/AU5254901A/en not_active Abandoned
- 2001-04-13 CA CA002404195A patent/CA2404195A1/en not_active Abandoned
- 2001-04-13 JP JP2001576967A patent/JP2003531151A/ja active Pending
- 2001-04-17 MY MYPI20011828A patent/MY127172A/en unknown
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2002
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101337192B (zh) * | 2007-07-04 | 2010-07-21 | 中国科学院大连化学物理研究所 | 一种中微孔金属有机化合物及其制备 |
| CN108069407A (zh) * | 2017-12-28 | 2018-05-25 | 江西石华精细化工科技协同创新有限公司 | 一种绝氧气体的脱水除氧方法 |
| CN108069407B (zh) * | 2017-12-28 | 2020-11-17 | 江西石华精细化工科技协同创新有限公司 | 一种绝氧气体的脱水除氧方法 |
| CN108059600A (zh) * | 2018-02-08 | 2018-05-22 | 浙江博瑞电子科技有限公司 | 一种四（二甲氨基）钛的精制方法 |
| CN108059600B (zh) * | 2018-02-08 | 2020-04-10 | 浙江博瑞电子科技有限公司 | 一种四（二甲氨基）钛的精制方法 |
| CN110483580A (zh) * | 2019-09-06 | 2019-11-22 | 广东先导先进材料股份有限公司 | 一种高纯度三烷基锑及其制备方法与应用 |
| CN110483580B (zh) * | 2019-09-06 | 2022-04-19 | 广东先导微电子科技有限公司 | 一种高纯度三烷基锑及其制备方法与应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1274879A1 (en) | 2003-01-15 |
| KR20030001435A (ko) | 2003-01-06 |
| WO2001079587A1 (en) | 2001-10-25 |
| CN1218065C (zh) | 2005-09-07 |
| CN1425078A (zh) | 2003-06-18 |
| US6797182B2 (en) | 2004-09-28 |
| TW550307B (en) | 2003-09-01 |
| MY127172A (en) | 2006-11-30 |
| AU5254901A (en) | 2001-10-30 |
| JP2003531151A (ja) | 2003-10-21 |
| US20030038082A1 (en) | 2003-02-27 |
| CA2404195A1 (en) | 2001-10-25 |
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