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Hafnium compound, hafnium thin film-forming material and method for forming hafnium thin film

An amine compound and compound technology, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, metal material coating processes, etc., can solve the problem of difficult gasification, poor stability, and difficulty in supplying stable gases and other problems, to achieve the effect of stable supply and easy gasification

Active Publication Date: 2012-03-07
TRI CHEM LAB
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, gasification is difficult and stable gas supply is difficult
That is, it is difficult to stably supply raw materials, so it is impossible to stably form high-quality hafnium-based thin films
[0005] Tetrakis(dialkylamino)hafnium has low thermal stability
So it is difficult to supply a stable gas
That is, it is difficult to stably supply raw materials, so it is impossible to stably form high-quality hafnium-based thin films
[0006] The stability of tetra(alkoxy)hafnium is also poor
Therefore it is difficult to supply a stable gas
That is, it is difficult to stably supply raw materials, so it is impossible to stably form high-quality hafnium-based thin films

Method used

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  • Hafnium compound, hafnium thin film-forming material and method for forming hafnium thin film
  • Hafnium compound, hafnium thin film-forming material and method for forming hafnium thin film
  • Hafnium compound, hafnium thin film-forming material and method for forming hafnium thin film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] [The novel compound CpHf(NMe 2 ) 3 Synthesis]

[0055] Under a nitrogen atmosphere, 29 g of tetrakis(dimethylamino)hafnium and 5.3 g of cyclopentadiene were stirred in 70 mL of benzene for 1 hour. After heating the solution to reflux for 2 hours, benzene was distilled off under reduced pressure. The remaining yellow liquid was subjected to 0.1 torr vacuum distillation at 70-80° C. to obtain 25 g of yellow liquid.

[0056] The yellow liquid boiled at 75°C / 0.2 Torr.

[0057] In addition, the results and spectrum of NMR measurement showed the following resonance lines.

[0058] 1 H-NMR (C 6 D. 6 ): 3.0(s, 18H), 6.0(s, 5H)

[0059] What needs to be explained is that, figure 1 is the NMR spectrum of cyclopentadienyl tris(dimethylamino)hafnium.

[0060] And, judging from the above reaction form and NMR spectrum: the obtained yellow liquid is cyclopentadienyl tri(dimethylamino) hafnium [CpHf(NMe 2 ) 3 ].

[0061] Next, 150 g of CpHf(NMe 2 ) 3 It was charged int...

Embodiment 2

[0071] [Novel compound (MeCp)Hf(NMe 2 ) 3 Synthesis]

[0072] Under a nitrogen atmosphere, 10 g of tetrakis(dimethylamino)hafnium and 2 g of methylcyclopentadiene were stirred in 35 mL of benzene for 1 hour. After heating the solution to reflux for 2 hours, benzene was distilled off under reduced pressure. The remaining yellow liquid was subjected to 0.1 torr vacuum distillation at 70-80° C. to obtain 11 g of yellow liquid.

[0073] The yellow liquid has a boiling point of 72°C / 0.1 Torr.

[0074] In addition, the results and spectrum of NMR measurement showed the following resonance lines.

[0075] 1 H-NMR (C 6 D. 6 ): 2.1(s, 3H), 3.0(s, 18H), 5.8(m, 2H), 5.9(m, 2H)

[0076] What needs to be explained is that, image 3 is the NMR spectrum of methylcyclopentadienyl tris(dimethylamino)hafnium.

[0077] Moreover, judging from the above reaction form and NMR spectra: the obtained yellow liquid is methylcyclopentadienyl tris(dimethylamino)hafnium [(MeCp)Hf(NMe 2 ) 3 ]. ...

Embodiment 3

[0085] [Novel compound (EtCp)Hf(NMe 2 ) 3 Synthesis]

[0086] Under a nitrogen atmosphere, 25 g of tetrakis(dimethylamino)hafnium and 7 g of ethylcyclopentadiene were stirred in 60 mL of benzene for 1 hour. After heating the solution to reflux for 2 hours, benzene was distilled off under reduced pressure. The remaining yellow liquid was subjected to 0.1 torr vacuum distillation at 70-80° C. to obtain 19 g of yellow liquid.

[0087] The yellow liquid boiled at 78°C / 0.2 Torr.

[0088] In addition, the results and spectrum of NMR measurement showed the following resonance lines.

[0089] 1 H-NMR (C 6 D. 6 ): 1.1(t, 3H), 2.5(q, 2H), 3.0(s, 18H), 5.9(m, 2H), 6.0(m, 2H)

[0090] What needs to be explained is that, Figure 4 is the NMR spectrum of ethylcyclopentadienyl tris(dimethylamino)hafnium.

[0091] Moreover, judging from the above reaction form and NMR spectrum: the obtained yellow liquid is ethylcyclopentadienyl tri(dimethylamino) hafnium [(EtCp)Hf(NMe 2 ) 3 ].

...

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Abstract

The invention provides a hafnium compound which is in a liquid state at room temperature and has excellent stability. Also disclosed is a technique for stably forming a high-quality hafnium thin film for which a raw material can be stably supplied. Specifically disclosed is a hafnium thin film-forming material which is composed of a compound represented by the following general formula [I]: LHf(NR<1>R<2>)3[I] In the formula, L represents a cyclopentadienyl group or a substituted cyclopentadienyl group, and R<1> and R<2> respectively represent an alkyl group. R<1> and R<2> may be the same as or different from each other.

Description

technical field [0001] The present invention relates to a technique for forming a hafnium-based thin film. Background technique [0002] It has been proposed to use hafnium tetrahalide, tetra(dialkylamino) hafnium, tetra(alkoxy) hafnium or tetra(β-diketone) hafnium to form a hafnium-based film by chemical vapor growth or atomic layer controlled growth. [0003] However, it is necessary to vaporize the above compound when forming the hafnium-based thin film. Then, the above compound is heated for vaporization. [0004] However, hafnium tetrahalide and hafnium tetrakis(β-diketonate) are solids. Therefore, gasification is difficult and stable gas supply is difficult. That is, it is difficult to stably supply raw materials, and thus it is impossible to stably form a high-quality hafnium-based thin film. [0005] Tetrakis(dialkylamino)hafnium has low thermal stability. Therefore, it decomposes when heated and vaporized. Therefore, it is difficult to supply stable gas. That...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C16/18C07F7/00
CPCC23C16/18C07F17/00C07F7/00
Inventor 平木忠明三桥智太附圣椿谷晓人金炳洙刘升镐
Owner TRI CHEM LAB
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