TW202202511A - 用於薄膜沉積的第5族金屬化合物和使用該化合物形成含第5族金屬的薄膜的方法 - Google Patents
用於薄膜沉積的第5族金屬化合物和使用該化合物形成含第5族金屬的薄膜的方法 Download PDFInfo
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- 150000002736 metal compounds Chemical class 0.000 title claims abstract description 43
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 45
- 239000002184 metal Substances 0.000 title claims description 29
- 239000010409 thin film Substances 0.000 title claims description 24
- 238000000427 thin-film deposition Methods 0.000 title description 3
- 239000000126 substance Substances 0.000 claims abstract description 37
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 23
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 238000000231 atomic layer deposition Methods 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 12
- 238000005137 deposition process Methods 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- -1 tert-amyl group Chemical group 0.000 claims description 9
- 238000005229 chemical vapour deposition Methods 0.000 claims description 7
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 claims description 7
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 7
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 6
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 4
- 230000005587 bubbling Effects 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 4
- 125000003538 pentan-3-yl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])C([H])([H])[H] 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 claims description 2
- 239000001272 nitrous oxide Substances 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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 2
- 239000012159 carrier gas Substances 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000010955 niobium Substances 0.000 description 32
- 150000001875 compounds Chemical class 0.000 description 15
- 125000003253 isopropoxy group Chemical group [H]C([H])([H])C([H])(O*)C([H])([H])[H] 0.000 description 14
- 229910052758 niobium Inorganic materials 0.000 description 11
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 11
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 9
- 239000010408 film Substances 0.000 description 7
- 238000002411 thermogravimetry Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 125000004433 nitrogen atom Chemical group N* 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- 239000007983 Tris buffer Substances 0.000 description 4
- 229910052715 tantalum Inorganic materials 0.000 description 4
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 4
- 238000000113 differential scanning calorimetry Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000003990 capacitor Substances 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- JQOAQUXIUNVRQW-UHFFFAOYSA-N hexane Chemical compound CCCCCC.CCCCCC JQOAQUXIUNVRQW-UHFFFAOYSA-N 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 2
- KMYWSWPDQIMANY-UHFFFAOYSA-N 1-cyclopentylcyclopenta-1,3-diene Chemical compound C1CCCC1C1=CC=CC1 KMYWSWPDQIMANY-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007707 calorimetry Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- UZBQIPPOMKBLAS-UHFFFAOYSA-N diethylazanide Chemical compound CC[N-]CC UZBQIPPOMKBLAS-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 125000003548 sec-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
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Abstract
根據本公開的實施方案的第5族金屬化合物由以下＜化學式1＞和＜化學式2＞中的任一個表示：
在＜化學式1＞和＜化學式2＞中，
M是選自第5族金屬元素中的任意一種，
n是選自1至5的整數中的任意一個，
R1
是選自具有3至6個碳原子的直鏈烷基基團和具有3至6個碳原子的支鏈烷基基團中的任意一種，並且
R2
和R3
各自獨立地為選自氫、具有1至4個碳原子的直鏈烷基基團和具有1至4個碳原子的支鏈烷基基團中的任意一種。
Description
本公開涉及第5族金屬化合物和使用該化合物形成金屬薄膜的方法，更具體地，涉及用作前體的第5族金屬前體化合物和使用該化合物形成含第5族金屬的薄膜的方法。
隨著電子技術的發展，對用於各種電子設備中的電子元件的小型化和輕量化的需求正在迅速增加。為了形成精細的電子元件，已經提出了各種物理和化學氣相沉積方法，並且已經對通過這種沉積方法製造諸如金屬薄膜、金屬氧化物薄膜和金屬氮化物薄膜之類的各種電子元件進行了各種研究。
在半導體元件的製造中，通常使用金屬有機化學氣相沉積(MOCVD)或原子層沉積(ALD)製程形成含第5族金屬化合物的薄膜。
然而，與MOCVD製程相比，由於ALD製程進行自限反應，因此其具有優異的階梯覆蓋性，並且由於ALD製程是相對低溫的製程，因此其可以避免因熱擴散導致的元件特性劣化。
含第5族金屬化合物的薄膜中的氧化鋯(ZrO2
)薄膜已被用作電容器結構中絕緣層的高k材料。最近，已發現介於兩個ZrO2
介電層之間的氧化鈮(Nb2
O5
)薄膜可顯著降低漏電流並有助於穩定ZrO2
的立方晶系/四方晶系相。所產生的ZrO2
/Nb2
O5
/ZrO2
層壓板在動態隨機存取記憶體(DRAM)的當前金屬-絕緣體-金屬(MIM)電容器中提供更高的k值(檔[Alumina, J. Vac. Sci. Technol A 4 (6), 1986和Microelectronic Engineering 86 (2009) 1789-1795])。
選擇適合於沉積製程的前體化合物以沉積含鈮(Nb)的薄膜是非常重要的。已知能夠形成含第5族金屬的薄膜的代表性有機金屬前體化合物包括五(二甲基醯氨基)鉭(PDMAT)、(叔丁基醯亞胺)三(二乙基醯氨基)鉭(TBTDET)、(叔丁基醯亞胺)三(二乙基醯氨基)鈮(TBTDEN)等。然而，由於PDMAT是固體，因此難以通過持續昇華PDMAT來供給，通過將液體容納在圓柱形容器中而使液體蒸發，或蒸發以恆定流速注入的液體的直接液體注入(DLI)裝置等已廣泛應用於半導體元件製造製程中。另外，由於PDMAT、TBTDET、TBTDEN等都具有較差的熱穩定性，在高溫下使用它們是不利的。因此，難以在原子層沉積(ALD)製程中使用這些化合物來於300℃在不平坦表面上形成具有均勻厚度的氧化膜。
因此，適用於原子層沉積 (ALD)製程的前體化合物應該在低溫下具有高蒸氣壓，應該足夠熱穩定，並且應該是具有低黏度的液體化合物，以便它可以容易轉移到反應室而不被分解。
[相關先前技術文獻]
[專利文獻]
(專利文獻1)韓國早期公開專利公開號2020-0008048 (2020.01.22.)
本公開的目的是通過解決常規使用的金屬前體化合物的缺點，提供一種在室溫下為液體、具有高揮發性且熱穩定的第5族金屬化合物，以及用於包括該第5族金屬化合物的用於薄膜沉積的前體組合物。此外，本公開的目的是提供一種使用包括第5族金屬化合物的用於薄膜沉積的前體組合物來沉積高品質薄膜的薄膜形成方法。
根據以下詳細描述，本公開的其他目的將變得更加明顯。
根據本公開的實施方案的第5族金屬化合物可以由以下化學式1和2中的任一個表示：
＜化學式1＞ ＜化學式2＞
在＜化學式1＞和＜化學式2＞中，M為選自第5族金屬元素[釩(V)、鈮(Nb)和鉭(Ta)]中的任意一種，n為選自1至5的整數，並且R1
為選自具有3至6個碳原子數的直鏈烷基基團和具有3至6個碳原子數的支鏈烷基基團中的任意一種。例如，R1
可以是選自正丙基基團、異丙基基團、正丁基基團、叔丁基基團、異丁基基團、仲丁基基團、正戊基基團、叔戊基基團、異戊基基團、仲戊基基團、新戊基基團和3-戊基基團中的任意一種。R2
和R3
各自獨立地為選自氫、具有1至4個碳原子的直鏈烷基基團和具有1至4個碳原子的支鏈烷基基團中的任意一種。例如，R2
和R3
可以各自獨立地為選自氫、甲基基團、乙基基團、正丙基基團、異丙基基團、正丁基基團、仲丁基基團、異丁基基團和叔丁基基團中的任意一種，並且R2
和R3
可以具有彼此相同的結構。
根據本公開實施方案的形成含第5族金屬的薄膜的方法包括通過金屬有機化學氣相沉積(MOCVD)製程或原子層沉積(ALD)製程，使用由化學式1和化學式2中的任一個表示的第5族金屬化合物作為前體在襯底上沉積薄膜。
當將根據本公開的實施方案的第 5 族金屬化合物與作為代表性鈮前體的(叔丁基醯亞胺)三(二乙氨基)鈮(V)(TBTDEN)進行比較時，第5族金屬化合物可以通過具有環戊二烯(CP)結構的優勢為金屬提供更多的電子。由於穩定的結構，增加了化合物的熱穩定性，通過作為現有均配配體的金屬-胺結構中的雜配配體結構(金屬-醇鹽、金屬-胺、金屬-烷基)有效減少沉積製程中的殘留物的量，並且由於將該化合物作為具有高揮發性的液體應用到該製程中是有利的，因此有可能在原子層沉積(ALD)製程中穩定地沉積單個原子層，並且ALD製程的視窗範圍可以擴展。
由於本公開的上述效果，當使用含第5族金屬化合物的組合物在襯底上沉積薄膜時，可以改進沉積在襯底上的薄膜的品質。
在下文中，將參照圖1和2更詳細地描述本公開的優選實施方案。本公開的實施方案可以以各種形式修改，並且本公開的範圍不應被解釋為限於以下描述的實施方案。提供本實施方案是為了向本公開所屬領域的普通技術人員更詳細地解釋本公開。因此，附圖中所示的每個元件的形狀可能被誇大以著重進行更清楚的解釋。
在本公開的整個說明書中，術語“烷基”或“烷基基團”包括具有1至12個碳原子、1至10個碳原子、1至8個碳原子、1至5個碳原子、1至3個碳原子、3至8個碳原子或3至5個碳原子的直鏈或支鏈烷基基團。例如，儘管烷基基團可選自甲基基團、乙基基團、正丙基基團(n
Pr)、異丙基基團(i
Pr)、正丁基基團(n
Bu)、叔丁基基團(t
Bu)、異丁基基團(i
Bu)、仲丁基基團(s
Bu)、正戊基基團、叔戊基基團、異戊基基團、仲戊基基團、新戊基基團、3-戊基基團、己基基團、異己基基團、庚基基團、4,4-二甲基戊基基團、辛基基團、2,2,4-三甲基戊基基團、壬基基團、癸基基團、十一烷基基團、十二烷基基團及其異構體，但其不限於此。
根據本公開的實施方案的第5族金屬化合物可以由以下化學式1和化學式2中的任一個表示：
＜化學式1＞ ＜化學式2＞
在＜化學式1＞和＜化學式2＞中，M為選自第5族金屬元素中的任意一種，n為選自1至5的整數，R1
為選自具有3至6個碳原子數的直鏈烷基基團和具有3至6個碳原子數的支鏈烷基基團中的任意一種，並且R2
和R3
各自獨立地為選自氫、具有1至4個碳原子的直鏈烷基基團和具有1至4個碳原子的支鏈烷基基團中的任意一種。
更具體地，M可以是選自釩(V)、鈮(Nb)和鉭(Ta)中的任意一種。此外，R1
可以是選自正丙基基團、異丙基基團、正丁基基團、叔丁基基團、異丁基基團、仲丁基基團、正戊基基團、叔戊基基團、異戊基基團、仲戊基基團、新戊基基團和3-戊基基團中的任意一種。此外，R2
和R3
可以各自獨立地為選自氫、甲基基團、乙基基團、正丙基基團、異丙基基團、正丁基基團、仲丁基基團、異丁基基團和叔丁基基團中的任意一種，並且R2
和R3
可以具有相同的結構。
更具體地，由化學式1表示的第5族金屬化合物可以是由以下化學式3表示的第5族金屬化合物：
＜化學式3＞
在化學式3中，M為選自第5族金屬元素中的任意一種，並且與化學式1中描述的相同。
此外，由化學式2表示的第5族金屬化合物可以是由以下化學式4表示的第5族金屬化合物：
＜化學式4＞
根據本公開的實施方案的第5族金屬化合物具有其中第5族金屬和環戊二烯直接連接的結構。根據本公開的實施方案的第5族金屬化合物具有優異的熱穩定性，因為第5族金屬化合物可以通過使電子能夠更容易地從環戊二烯提供給金屬而保持結構更穩定的狀態。因此，當使用根據本公開的實施方案的第5族金屬化合物來形成薄膜時，有可能減少沉積製程中生成的殘留物的量。此外，由於第5族金屬化合物易於應用於液體製程，因此其可用於原子層沉積(ALD)製程。
此外，在根據本發明的實施方案的第5族金屬化合物中，第5族金屬與一個氮原子形成雙鍵，並分別與兩個氧原子形成單鍵。第5族金屬，例如鈮(Nb)和氧原子(O)之間的鍵能大於鈮(Nb)和氮原子(N)之間的鍵能。因此，與其中通過允許第5族金屬與一個氮原子形成雙鍵並與兩個氮原子中的每一個形成單鍵而使第5族金屬和三個氮原子連接的化合物相比，根據本公開的實施方案的第5族金屬化合物具有更優異的熱穩定性。
在下文中，將通過以下實施例更詳細地描述根據本公開的第5族金屬化合物。然而，這僅是為了幫助理解本公開而提出，並且本公開不限於以下實施例。實施例 1 ： ((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2 的製備
在將20 g (0.0453 mol, 1當量)的雙(二乙基醯胺基)(叔丁基醯亞胺)(環戊基環戊二烯)鈮((η-C5
H5
)C5
H9
)(tBuN)Nb(NEt2
)2
和150 mL的己烷(正己烷)注入到火焰乾燥的500 mL Schlenk燒瓶中後，將注入的材料在室溫下攪拌。在於-20℃以下向燒瓶中滴加5.99 g (0.0997 mol, 2.2當量)的異丙醇(C3
H7
OH)後，將反應液在室溫下攪拌12小時。通過在減壓下從反應溶液中除去溶劑並在減壓下蒸餾除去了溶劑的反應溶液而獲得18.73 g(產率98%)的由((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
表示的淡黃色液體化合物。
實施例2：(η-C5
H5
)(tBuN)Nb(OiPr)2
的製備
在將11 g (0.029 mol, 1當量)的雙(二乙基醯胺)(叔丁基醯亞胺) (環戊二烯)鈮((η-C5
H5
)(tBuN)Nb(NEt2
)2
和150 mL的己烷(正己烷)注入到火焰乾燥的500 mL Schlenk燒瓶中後，將注入的材料在室溫下攪拌。在於-20℃以下向燒瓶中滴加3.8 g (0.063 mol, 2.2當量)的異丙醇(C3
H7
OH)後，將反應液在室溫下攪拌12小時。通過在減壓下從反應溶液中除去溶劑並在減壓下蒸餾除去了溶劑的反應溶液而獲得9 g(產率90%)的由((η-C5
H5
)(tBuN)Nb(OiPr)2
表示的淡黃色液體化合物。
實驗實施例：熱分析
為了找出根據比較例的(t-丁基醯亞胺)三(二乙氨基)鈮(V))(TBTDEN)、根據實施例1的((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
和根據實施例2的(η-C5
H5
)(tBuN)Nb(OiPr)2
在類似條件下的熱性能，進行了差示掃描量熱法(DSC)分析和熱重分析(TGA)。熱重裝置儲存在其中水分和氧氣含量保持在1 ppm以下的氮氣手套箱中。通過將15 mg的樣品放入坩堝中進行熱重分析。此後，以10℃/min的溫度梯度將樣品從35℃加熱到350℃。監測品質損失作為坩堝溫度的函數。根據DSC分析，比較例、實施例1和實施例2的分解溫度(Td)示於圖1中。另外，根據TGA的圖表結果示於圖2中。參考圖1和圖2，可以證實，根據實施例1製備的((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
和根據實施例2製備的(η-C5
H5
)(tBuN)Nb(OiPr)2
比根據對比例製備的TBTDEN更具熱穩定性。由此可以看出，根據實施例1的((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
和根據實施例2的(η-C5
H5
)(tBuN)Nb(OiPr)2
更有效地用作氣相前體。
在下文中，將描述根據本公開的實施方案的形成含第5族金屬的薄膜的方法。
根據本公開的實施方案的形成含第5族金屬的薄膜的方法使用根據本公開的實施方案的第5族金屬化合物作為前體通過沉積製程在襯底上沉積薄膜。
沉積製程可以包括原子層沉積(ALD)製程或化學氣相沉積(CVD)製程，例如金屬有機化學氣相沉積(MOCVD)製程。沉積製程可於50至700℃進行。
首先，將由化學式1和化學式2中的任一個表示的第5族金屬化合物轉移到襯底上。例如，雖然可以通過鼓泡法、氣相品質流量控制器法、直接氣體注入(DGI)法、直接液體注入(DLI)法、液體轉移法(其中液體溶解在有機溶劑中並轉移等)將第5族金屬化合物供應到襯底上，但是本公開不限於此。
更具體地，將第5族金屬化合物與載氣或稀釋氣體混合，該載氣或稀釋氣體包含選自氬氣(Ar)、氮氣(N2
)、氦氣(He)和氫氣(H2
)中的一種或多種，從而使第5族金屬化合物與載氣或稀釋氣體的混合物通過鼓泡法或DGI法轉移到襯底上。
同時，沉積製程可包括在形成含第5族金屬的薄膜時供應選自水蒸氣(H2
O)、氧氣(O2
)、臭氧(O3
)和過氧化氫(H2
O2
)的一種或多種反應氣體的步驟。此外，沉積製程可以包括在形成含第5族金屬的薄膜時，供應選自氨(NH3
)、肼(N2
H4
)、一氧化二氮(N2
O)和氮(N2
)的一種或多種反應氣體的步驟。由此，在襯底上形成的含金屬的薄膜可以是第5族金屬氧化物膜或第5族金屬氮化物膜。
在上文中，已經通過示例詳細描述了本公開，但是與其不同的其他類型的示例也是可能的。因此，下面闡述的請求項的技術精神和範圍不限於這些示例。
無
從結合附圖的以下詳細描述中，將更清楚地理解本公開的上述和其他方面、特徵和其他優點，其中：
圖1是示出了根據實施例1的((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
、根據實施例2的(η-C5
H5
)(tBuN)Nb(OiPr)2
和根據對比例的TBTDEN的熱量(差示掃描量熱法)分析結果的表；以及
圖2是示出了根據實施例1的((η-C5
H5
)C5
H9
)(tBuN)Nb(OiPr)2
、根據實施例2的(η-C5
H5
)(tBuN)Nb(OiPr)2
和根據比較例的TBTDEN的熱重分析(TGA)結果的圖。
Claims (12)
- 一種第5族金屬化合物，其由以下＜化學式1＞和＜化學式2＞中的任一個表示： ＜化學式1＞ ＜化學式2＞
在＜化學式1＞和＜化學式2＞中， M是選自第5族金屬元素中的任意一種， n是選自1至5的整數中的任意一個， R1 是選自具有3至6個碳原子的直鏈烷基基團和具有3至6個碳原子的支鏈烷基基團中的任意一種，並且 R2 和R3 各自獨立地為選自氫、具有1至4個碳原子的直鏈烷基基團和具有1至4個碳原子的支鏈烷基基團中的任意一種。
- 如請求項1所述的第5族金屬化合物，其中R1 是選自正丙基基團(n Pr)、異丙基基團(i Pr)、正丁基基團(n Bu)、叔丁基基團(t Bu)、異丁基基團(i Bu)、仲丁基基團(s Bu)、正戊基基團、叔戊基基團、異戊基基團、仲戊基基團、新戊基基團、3-戊基基團、己基基團和異己基基團中的任意一種。
- 如請求項1所述的第5族金屬化合物，其中R2 和R3 各自獨立地為選自氫、甲基基團、乙基基團、正丙基基團、異丙基基團、正丁基基團、仲丁基基團、異丁基基團和叔丁基基團中的任意一種。
- 如請求項1所述的第5族金屬化合物，其中所述第5族金屬化合物由以下化學式3表示： ＜化學式3＞其中M是選自所述第5族金屬元素中的任意一種。
- 如請求項1所述的第5族金屬化合物，其中所述第5族金屬化合物由以下化學式4表示： ＜化學式4＞。
- 一種用於沉積含第5族金屬的薄膜的前體組合物，所述前體組合物包含如請求項1至5中任一項所述的第5族金屬化合物。
- 一種形成含第5族金屬的薄膜的方法，所述方法包括使用如請求項1至5中任一項所述的第5族金屬化合物作為前體，通過金屬有機化學氣相沉積(MOCVD)製程或原子層沉積(ALD)製程在襯底上沉積薄膜。
- 如請求項7所述的方法，其中所述沉積製程在50至700℃的溫度範圍內進行。
- 如請求項7所述的方法，其中所述沉積製程包括通過選自鼓泡法、氣相品質流量控制器(MFC)法、直接氣體注入(DGI)法、直接液體注入(DLI)法和其中所述第5族金屬化合物溶解在有機溶劑中並移動的有機溶液供給法中的一種方法將所述第5族金屬化合物移動到所述襯底上。
- 如請求項9所述的方法，其中通過所述鼓泡法或所述DGI法將所述第5族金屬化合物與載氣一起移動到所述襯底上，並且所述載氣為包含選自氬氣(Ar)、氮氣(N2 )、氦氣(He)和氫氣(H2 )的一種或多種的混合物。
- 如請求項7所述的方法，其中所述沉積製程包括在形成所述含第5族金屬的薄膜時供應選自水蒸氣(H2 O)、氧氣(O2 )、臭氧(O3 )和過氧化氫(H2 O2 )的一種或多種反應氣體的步驟。
- 如請求項7所述的方法，其中所述沉積製程包括在形成所述含第5族金屬的薄膜時供應選自氨(NH3 )、肼(N2 H4 )、一氧化二氮(N2 O)和氮氣(N2 )的一種或多種反應氣體的步驟。
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