CN101367756A - 用于制造相变存储器材料的碲(Te)前驱体 - Google Patents
用于制造相变存储器材料的碲(Te)前驱体 Download PDFInfo
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- CN101367756A CN101367756A CNA2008101258763A CN200810125876A CN101367756A CN 101367756 A CN101367756 A CN 101367756A CN A2008101258763 A CNA2008101258763 A CN A2008101258763A CN 200810125876 A CN200810125876 A CN 200810125876A CN 101367756 A CN101367756 A CN 101367756A
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 32
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000002243 precursor Substances 0.000 title abstract 3
- 239000000463 material Substances 0.000 title description 6
- 238000000034 method Methods 0.000 claims abstract description 54
- 239000012782 phase change material Substances 0.000 claims abstract description 18
- 150000004770 chalcogenides Chemical class 0.000 claims abstract description 13
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 10
- 230000008021 deposition Effects 0.000 claims description 39
- 229910052739 hydrogen Inorganic materials 0.000 claims description 33
- 239000001257 hydrogen Substances 0.000 claims description 33
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000203 mixture Substances 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 17
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims description 13
- 229910052805 deuterium Inorganic materials 0.000 claims description 13
- -1 amino antimony alkane Chemical class 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 229910052732 germanium Inorganic materials 0.000 claims description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- GMEFXBFKMIZRMO-UHFFFAOYSA-N aminogermanium Chemical compound [Ge]N GMEFXBFKMIZRMO-UHFFFAOYSA-N 0.000 claims description 8
- 125000004663 dialkyl amino group Chemical group 0.000 claims description 8
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 8
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 claims description 8
- NNCGPRGCYAWTAF-UHFFFAOYSA-N tellurium hexafluoride Chemical compound F[Te](F)(F)(F)(F)F NNCGPRGCYAWTAF-UHFFFAOYSA-N 0.000 claims description 8
- 125000003342 alkenyl group Chemical group 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- YENXDKGOGVLOPS-UHFFFAOYSA-N butane-1-tellurol Chemical group CCCC[TeH] YENXDKGOGVLOPS-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 238000000151 deposition Methods 0.000 description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 9
- 238000005229 chemical vapour deposition Methods 0.000 description 9
- 239000013078 crystal Substances 0.000 description 5
- 229910000618 GeSbTe Inorganic materials 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000003860 storage Methods 0.000 description 4
- 150000003498 tellurium compounds Chemical class 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000005240 physical vapour deposition Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910000078 germane Inorganic materials 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 238000001802 infusion Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- MSZZQUKSERFTTQ-UHFFFAOYSA-N N[Sb] Chemical class N[Sb] MSZZQUKSERFTTQ-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical group [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- LFQSCWFLJHTTHZ-WFVSFCRTSA-N deuteriooxyethane Chemical compound [2H]OCC LFQSCWFLJHTTHZ-WFVSFCRTSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- WMMYFRXVXJPWDI-UHFFFAOYSA-N dimethylaminoantimony Chemical compound CN(C)[Sb] WMMYFRXVXJPWDI-UHFFFAOYSA-N 0.000 description 1
- YNYBCPCYMAHDCS-UHFFFAOYSA-N dimethylaminogermanium Chemical compound CN(C)[Ge] YNYBCPCYMAHDCS-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000000155 isotopic effect Effects 0.000 description 1
- UBJFKNSINUCEAL-UHFFFAOYSA-N lithium;2-methylpropane Chemical compound [Li+].C[C-](C)C UBJFKNSINUCEAL-UHFFFAOYSA-N 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- OKKJLVBELUTLKV-VMNATFBRSA-N methanol-d1 Chemical compound [2H]OC OKKJLVBELUTLKV-VMNATFBRSA-N 0.000 description 1
- POPACFLNWGUDSR-UHFFFAOYSA-N methoxy(trimethyl)silane Chemical compound CO[Si](C)(C)C POPACFLNWGUDSR-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C07F11/00—Compounds containing elements of Groups 6 or 16 of the Periodic Table
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/002—Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
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- C07B59/00—Introduction of isotopes of elements into organic compounds ; Labelled organic compounds per se
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
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- C23C16/305—Sulfides, selenides, or tellurides
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Abstract
说明书中公开了用于制造相变存储器材料的碲(Te)前驱体，特别是含碲(Te)前驱体、含Te硫属元素化物相变材料。说明书中还公开了使用ALD、CVD或循环CVD法制造含Te硫属元素化物相变材料的方法，其中至少一种公开的含碲(Te)前驱体引入该方法。
Description
与相关申请的相互参考
[0001]按照35 U.S.C.§119(e)，本申请要求于2007年4月24日提交的在先提交的美国专利申请序列号60/913,798的优先权。
技术领域
本发明涉及用于制造相变存储器材料的碲(Te)前驱体。
背景技术
[0002]相变材料按照温度以晶体状态或无定形状态存在。相比无定形状态，晶体状态下的相变材料具有更低的电阻和更加有序的原子排布。基于操作温度，可以将相变材料可逆地由晶体状态向无定形状态转化。这种特性，即可逆的相变和不同状态下的不同电阻，被应用于新提出的电子器件，新型的非易失性存储器器件，相变随机存取存储器(PRAM)器件。PRAM的电阻可基于其含有的相变材料的状态(例如，晶体、无定形等)而变化。
[0003]可以将各种类型的相变材料用于存储器器件，最常用的相变材料是14族和15族元素的硫属元素化物的三元组合物，例如锗—锑—碲化合物，一般简写为GST。在加热和冷却的循环中，GST的固体相可以迅速地由晶体转变为无定形，或反之亦然。无定形GST具有相对较高的电阻，而晶体GST具有相对较低的电阻。
[0004]目前，在可擦写光盘的制造中采用物理气相沉积(PVD)法或溅射在塑料基底上涂覆相变材料薄层。然而，由于膜生长控制和涂膜性能，PVD法不适用于电子器件。为制造PRAM，采用化学气相沉积(CVD)或原子层沉积(ALD)技术在硅基底上沉积GST薄层。相变存储器的发展日益需要采用适于低温沉积的前驱体的ALD/CVD方法。
发明内容
[0005]本发明通过提供含碲化合物作为Te前驱体满足了采用低温ALD、CVD或循环CVD法沉积三元锗—锑—碲膜的需要。
[0006]本说明书公开了含Te的组合物。这种含Te组合物包括具有下列一般结构的氘化有机碲酚(organotellurol)：
R-Te-D
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基(organosilyl)和有机锗基(organogermyl)。
[0007]说明书中公开了含Te硫属元素化物相变材料。通过沉积选自
(a)有机碲酚(organotellurol)，其具有一般结构：
R-Te-R’
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基和有机锗基；R’选自氢和氘；
(b)具有以下一般结构的组合物：
R”2Te
其中R”选自氢和氘；和
(c)六氟化碲
的Te前驱体制备该含Te硫属元素化物相变材料。
[0008]说明书中还公开了在基底上沉积含Te硫属元素化物相变材料的方法。
该方法包括步骤：
沉积包括选自以下的含碲组合物的Te前驱体：
(a)有机碲酚，其具有一般结构：
R-Te-R’
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基和有机锗基；R’选自氢和氘；
(b)一般结构：
R”2Te
其中R”选自氢和氘；和
(c)六氟化碲，与氨反应；
沉积包括具有以下一般结构的氨基锗烷(germane)的Ge前驱体：
(R1R2N)4Ge
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基；和
沉积包括具有以下一般结构的氨基锑烷的Sb前驱体：
(R1R2N)3Sb
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基。
[0009]可以以任何顺序依次或同时实施该方法中的三个沉积步骤。或者，可以同时实施三个沉积步骤中的任何两个。在100—400℃通过ALD、CVD或循环CVD法实施该方法。
具体实施方式
[0010]本发明涉及作为Te前驱体的经选择的碲化合物，并使用经选择的碲化合物同氨基锗及氨基锑化合物一起通过ALD、CVD或循环CVD法在低温方法中生产三元锗—锑—碲膜。
[0011]在本发明的一个具体实施方式中，用于低温沉积方法的Te前驱体包括碲化氢(H2Te)。氨基金属化合物对水解具有反应活性。氢的硫属元素化物均比水酸性强。氨基锗烷和氨基锑烷与碲化氢在低温(<250℃)下反应形成金属碲化物。沉积四(二甲氨基)锗烷、(Me2N)4Ge和三(二甲氨基)锑、(Me2N)3Sb，随后经碲化氢处理，是ALD或CVD法制造用于相变存储器应用的GST膜的合适途径。碲化氢是沸点为—4℃的气态化合物。它在0℃以上不稳定，分解为元素碲和氢。为了克服这个问题，可以通过原位生成来生产碲化氢，并立即引入反应室中。
[0012]在本发明的另一个具体实施方式中，Te前驱体包括碲化氘(D2Te)。氘是氢的较重的同位素(其原子核含有额外的中子)。与相应的规则的碲化氢相比，碲化氘具有提高的热稳定性。
[0013]作为热稳定性更高的碲化合物，公开了有机碲酚和氘化有机碲酚作为更适于三元锗—锑—碲膜沉积的碲前驱体。
[0014]在本发明的另一个具体实施方式中，用于低温沉积工艺的Te前驱体包括有机碲酚。有机碲酚具有酸性的Te-H键，其对于氨基金属化合物中的Ge-N和Sb-N键具有高反应性。以挥发性的胺作为脱离化合物，在相对较低的温度下形成Te-Ge和Te-Sb键。该反应在下图中被说明：
[0015]含有机碲酚的Te前驱体具有一般结构式
R—Te—R’
其中R为含有1—10个碳的直链、支链或环状形式的烷基或烯基；或含C6-12的芳基，如苯基；或二烷氨基；或甲硅烷基；或有机锗基；R’为氢或氘。
[0016]烷基碲为优选的碲前驱体。它们是挥发性的液体，并可以通过蒸汽提取或直接液体注射法输送。叔丁基碲酚具有键能为26kcal/mol的弱Te-C键。叔丁基可以在相对较低的温度下断裂。这有助于降低所得GST膜中的碳含量。
[0017]与相应的规则的有机碲酚相比，氘化有机碲酚具有提高的热稳定性，导致较长的保存期和较宽的工艺范围。由于一级动力学同位素效应，Te-D键比Te-H键更稳定。因此，在储存和输送过程中氘化有机碲酚具有较小的分解趋向，而同时保持与锗和锑形成碲化物相似的化学反应活性。
[0018]包括氘化有机碲酚的例子为正丁基碲酚(butyltellurol)-D和叔丁基碲酚-D，其中“D”为氘。
[0019]在本发明的另一个具体实施方式中，Te前驱体包括四(二烷氨基)碲，其中，烷基独立地选自甲基、乙基、丙基、异丙基、丁基和叔丁基。
[0020]可以按希望的摩尔比将包括四(二甲氨基)碲的Te前驱体与四(二甲氨基)锗(Me2N)4Ge和三(二甲氨基)锑烷混合形成均匀溶液。通过直接液体注射法将这样的溶液引入沉积室中。将这些化学品沉积在热的基底表面。随后采用氢或氢等离子体的还原反应除去氨基并形成具有适宜元素比的GST层。这些步骤形成ALD或循环CVD法的循环。
[0021]在本发明的又一个具体实施方式中，Te前驱体包含六氟化碲。六氟化碲TeF6是沸点为-38℃的无色气体。与硫的类似体不同，六氟化碲不是化学惰性的。这可能归因于d轨道的较大的可利用性和可能的f轨道的可利用性，这一点硫或硒都不具备。
[0022]在本发明的另一个具体实施方式中，以任何已知的沉积方法，如ALD、CVD或循环CVD法，通过沉积选自任何前面公开的具体实施方式中的Te前驱体来合成含Te硫属元素化物相变材料。
[0023]在本发明的又一个具体实施方式中，制造含Te硫属元素化物相变材料的方法可以以任何已知的沉积方法，如ALD、CVD或循环CVD法，将前面公开的具体实施方式中的Te前驱体与Ge前驱体和Sb前驱体一起沉积。
[0024]Ge前驱体和Sb前驱体的例子是具有以下一般结构的氨基锗烷和氨基锑烷：
(R1R2N)4Ge和(R1R2N)3Sb
其中R1和R2独立地是含1至10个碳的，直链、支链或环状形式的烷基。
[0025]例如，作为碲前驱体，六氟化碲可以在沉积室中与氨反应以形成氨基碲，随后可以与氨基锗烷和氨基锑烷反应，接着是氢还原以在基底上形成GST膜。
TeF6+NH3---->[Te(NH2)n]+NH4F
[0026]在用于制造GST薄膜的方法中，可以依次沉积三种前驱体。将三种前驱体中的任何一种如Ge前驱体沉积在具有适于化学反应的温度的热的基底表面上。例如，在净化/清洗步骤之后，通过流入惰性气体将第二种前驱体如Sb前驱体沉积在具有Ge薄层的基底表面上。在另一次净化/清洁步骤之后，将最后一种前驱体如Te前驱体沉积在含有Ge和Sb薄层的基底表面上。三种前驱体中的任何一种都可以作为此方法中的第一种或第二种或第三种前驱体。为了本发明的目的，在基底上沉积不仅包括直接在基底本身上沉积，还包括在三种反应物中已经沉积在基底上的一种之上沉积另一种。
[0027]或者，沉积方法可以同时沉积三种前驱体中的任何两种，或同时沉积全部三种前驱体。
[0028]另外，可以重复沉积方法以制造多层膜。
[0029]可以在100—400℃实施膜沉积。
工作实施例
[0030]在用于低温沉积的Te前驱体的制备中，可以使用各种已知方法中的任一种。在已知的方法中，按照本发明实施例的具体实施方式的Te前驱体制备方法描述如下。
实施例I 合成正丁基碲酚-D
[0031]将6.4g(0.05mol)200目的碲粉、100ml二乙醚和20ml在己烷中的2.5M叔丁基锂加入到250ml的烧瓶中。在0℃下，将混合物搅拌8小时。所有碲的黑色粉末消失而形成泥色沉淀物。向该混合物中加入5.4g(0.05mol)三甲基氯硅烷。使混合物升至室温。搅拌2小时后，缓慢加入2.0g(0.06mol)氘化甲醇(MeOD)。搅拌1小时后，将混合物在惰性气氛下过滤。经蒸馏除去溶剂和副产物甲氧基三甲基硅烷。真空蒸馏得到正丁基碲酚-D。沸点为85℃/100mmHg。
实施例II 合成叔丁基碲酚-D
[0032]将12.8g(0.10mol)200目的碲粉、250ml二乙醚和50ml在二乙醚中的2.0M叔丁基氯化镁溶液加入到500ml的烧瓶中。室温下，将混合物搅拌24小时。所有碲的黑色粉末消失而形成亮灰色沉淀物。用干冰浴将混合物冷至-50℃。向该混合物中缓慢加入10.0g(0.21mol)氘化乙醇(EtOD)。使混合物升至室温。搅拌2小时后，将混合物在惰性气氛下过滤。蒸馏除去醚溶剂。真空蒸馏得到叔丁基碲酚-D。沸点为65℃/100mmHg。
[0032]包括工作实施例的上述本发明的具体实施方式是可以构成本发明的众多具体实施方式的示例。预期可以使用该方法的众多其它组合，且在该方法中使用的材料可以选自具体公开的那些材料之外的众多材料。
Claims (21)
1.含Te组合物，包括具有以下一般结构的氘化有机碲酚：
R-Te-D
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基和有机锗基。
2.权利要求1的含Te组合物，选自正丁基碲酚-D和叔丁基碲酚-D。
3.含Te硫属元素化物相变材料，通过选自以下的Te前驱体合成
(a)有机碲酚，其具有一般结构：
R-Te-R’
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基和有机锗基；R’选自氢和氘；
(b)具有以下一般结构的组合物：
R”2Te
其中R”选自氢和氘；和
(c)六氟化碲。
4.在基底上沉积含Te硫属元素化物相变材料的方法，包括以下步骤：
沉积包括具有以下一般结构的有机碲酚的Te前驱体：
R-Te-R’
其中R选自含1—10个碳的直链、支链或环状形式的烷基或烯基；含C6-12的芳基；二烷氨基；甲硅烷基和有机锗基；R’选自氢和氘；
沉积包括具有以下一般结构的氨基锗烷的Ge前驱体：
(R1R2N)4Ge
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基；和
沉积包括具有以下一般结构的氨基锑烷的Sb前驱体：
(R1R2N)3Sb
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基。
5.权利要求4的方法，其中该方法进一步包括在每个沉积步骤之后引入氢或氢等离子体的步骤。
6.权利要求4的方法，其中该方法进一步包括在三个沉积步骤之后引入氢或氢等离子体的步骤。
7.权利要求4的方法，其中依次或同时实施三个沉积步骤。
8.权利要求4的方法，其中同时实施三个沉积步骤中的任何两个。
9.权利要求4的方法，其中通过选自ALD、CVD和循环CVD法的方法实施沉积。
10.在基底上沉积含Te硫属元素化物相变材料的方法，包括以下步骤：
沉积包括具有以下一般结构的含Te组合物的Te前驱体：
R”2Te
其中R”选自氢和氘；
沉积包括具有以下一般结构的氨基锗烷的Ge前驱体：
(R1R2N)4Ge
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基；和
沉积包括具有以下一般结构的氨基锑烷的Sb前驱体：
R1R2N)3Sb
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基。
11.权利要求10的方法，其中该方法进一步包括在每个沉积步骤之后引入氢或氢等离子体的步骤。
12.权利要求10的方法，其中该方法进一步包括在三个沉积步骤之后引入氢或氢等离子体的步骤。
13.权利要求10的方法，其中依次或同时实施三个沉积步骤。
14.权利要求10的方法，其中同时实施三个沉积步骤中的任何两个。
15.权利要求10的方法，其中通过选自ALD、CVD和循环CVD法的方法实施沉积。
16.在基底上沉积含Te硫属元素化物相变材料的方法，包括以下步骤：
通过使六氟化碲与氨反应沉积包括氨基碲的Te前驱体：
沉积包括具有以下一般结构的氨基锗烷的Ge前驱体：
(R1R2N)4Ge
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基；和
沉积包括具有以下一般结构的氨基锑烷的Sb前驱体：
(R1R2N)3Sb
其中R1和R2为含有1—10个碳的直链、支链或环状形式的烷基。
17.权利要求16的方法，其中该方法进一步包括在每个沉积步骤之后引入氢或氢等离子体的步骤。
18.权利要求16的方法，其中该方法进一步包括在三个沉积步骤之后引入氢或氢等离子体的步骤。
19.权利要求16的方法，其中依次或同时实施三个沉积步骤。
20.权利要求16的方法，其中同时实施三个沉积步骤中的任何两个。
21.权利要求16的方法，其中通过选自ALD、CVD和循环CVD法的方法实施沉积。
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- 2008-04-23 JP JP2008112231A patent/JP5080345B2/ja not_active Expired - Fee Related
- 2008-04-23 EP EP08155034A patent/EP1995236B1/en not_active Not-in-force
- 2008-04-24 KR KR1020080038155A patent/KR100994346B1/ko not_active IP Right Cessation
- 2008-04-24 CN CN2008101258763A patent/CN101367756B/zh not_active Expired - Fee Related
- 2008-04-24 CN CN2012105682173A patent/CN103132050A/zh active Pending
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| CN102395528A (zh) * | 2009-04-15 | 2012-03-28 | 美光科技公司 | 形成碲烷氧化物的方法和形成混合的碲卤化物-烷氧化物的方法 |
| US8697486B2 (en) | 2009-04-15 | 2014-04-15 | Micro Technology, Inc. | Methods of forming phase change materials and methods of forming phase change memory circuitry |
| CN103882404A (zh) * | 2009-04-15 | 2014-06-25 | 美光科技公司 | 形成相变材料的方法和形成相变存储器电路的方法 |
| US8765519B2 (en) | 2009-04-15 | 2014-07-01 | Micron Technology, Inc. | Methods of forming phase change materials and methods of forming phase change memory circuitry |
| US9269900B2 (en) | 2009-04-15 | 2016-02-23 | Micron Technology, Inc. | Methods of depositing phase change materials and methods of forming memory |
| CN108288618A (zh) * | 2009-04-15 | 2018-07-17 | 美光科技公司 | 形成相变材料的方法和形成相变存储器电路的方法 |
| CN102163555A (zh) * | 2010-02-23 | 2011-08-24 | 气体产品与化学公司 | 制造多成分薄膜的方法 |
| CN104341355A (zh) * | 2014-10-22 | 2015-02-11 | 江南大学 | 用于相变存储材料的氨基嘧啶Ge(Ⅱ)前质体及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| JP5529836B2 (ja) | 2014-06-25 |
| US20130129603A1 (en) | 2013-05-23 |
| TW200844084A (en) | 2008-11-16 |
| EP1995236B1 (en) | 2012-12-26 |
| KR20080095800A (ko) | 2008-10-29 |
| JP5080345B2 (ja) | 2012-11-21 |
| US20090142881A1 (en) | 2009-06-04 |
| CN103132050A (zh) | 2013-06-05 |
| EP1995236A1 (en) | 2008-11-26 |
| US8377341B2 (en) | 2013-02-19 |
| JP2008291015A (ja) | 2008-12-04 |
| JP2012057254A (ja) | 2012-03-22 |
| KR100994346B1 (ko) | 2010-11-12 |
| CN101367756B (zh) | 2013-02-06 |
| TWI373463B (en) | 2012-10-01 |
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