JP2014039045A - 誘電体フィルムを形成する方法、新規前駆体および半導体製造におけるそれらの使用 - Google Patents
誘電体フィルムを形成する方法、新規前駆体および半導体製造におけるそれらの使用 Download PDFInfo
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- JP2014039045A JP2014039045A JP2013186819A JP2013186819A JP2014039045A JP 2014039045 A JP2014039045 A JP 2014039045A JP 2013186819 A JP2013186819 A JP 2013186819A JP 2013186819 A JP2013186819 A JP 2013186819A JP 2014039045 A JP2014039045 A JP 2014039045A
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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Abstract
【解決手段】基板を反応チャンバーの中に提供する工程a)と、-Zr(MeCp)(NMe 2 ) 3 、Zr(EtCp)(NMe 2 ) 3 、ZrCp(NMe 2 ) 3 、Zr(MeCp)(NEtMe) 3 、Zr(EtCp)(NEtMe) 3 、ZrCp(NEtMe) 3 、Zr(MeCp)(NEt 2 ) 3 、Zr(EtCp)(NEt 2 ) 3 、ZrCp(NEt 2 ) 3 、Zr(iPr 2 Cp)(NMe 2 ) 3 、およびZr(tBu 2 Cp)(NMe 2 ) 3 から選択される Zr金属含有前駆体を気化させる工程b)と、-前記第1の気相金属源と前記任意の第2の気相金属源とにより、前記基板上に式(I)の化合物を含有する金属含有誘電体フィルムの堆積する。
【選択図】なし
Description
- それらは室温で液体であるか、または50℃未満の融点を持つ
- それらは熱的に安定であり、粒子を発生することなく適切な分配(気相または直接液体注入)を可能にする
- それらは熱的に安定であり、広い自己制限ALDウインドウを可能にし、4)1つの共反応物質または共反応物質の組合せ(H2、NH3、O2、H2O、O3、SiH4、Si2H6、Si3H8、TriDMAS、BDMAS、BDEAS、TDEAS、TDMAS、TEMAS、(SiH3)3N、(SiH3)2O、TMA またはアルミニウム含有前駆体、 TBTDET、TAT-DMAE、PET、TBTDEN、PEN、Ln(tmhd)3のようなランタノイド含有前駆体からなる群より選択される)を用いることによって、三元または四元材料を含む種々のIV族金属含有フィルムの堆積を可能にする
という利点を持つことが見出された。
0≦a<1、
0<b≦3、好ましくは1.5≦b≦2.5、
0≦c≦1
であり、
M1はハフニウム(Hf)、ジルコニウム(Zr)およびチタニウム(Ti)から選択される金属を示し、
M2はマグネシウム(Mg)、カルシウム(Ca)、亜鉛(Zn)、ホウ素(B)、アルミニウム(A)、インジウム(In)、ケイ素(Si)、ゲルマニウム(Ge)、スズ(Sn)、ハフニウム(Hf)、チタニウム(Ti)、バナジウム(V)、ニオブ(Nb)、タンタル(Ta)およびランタノイド原子、より具体的にはスカンジウム(Sc)、イットリウム(Y)およびランタン(La)および希土類金属原子から選択される金属を示す)の化合物を含有する少なくとも1つの金属含有誘電体フィルムを堆積する方法に関し、
- 反応チャンバーに基板を提供する工程a)と、
- 少なくとも1つの式(II):(R1 yOp)x (R2 tCp)z M1 R’4-x-z (ここで、
M1は先に定義されたものであり、
0≦x≦3、好ましくはx=0または1であり、
0≦z≦3、好ましくはz=1または2であり、
1≦(x+z)≦4であり、
0≦y≦7好ましくはy=2、0≦t≦5、好ましくはt=1であり、
(R1 yOp)は、置換されていないか、または1つ以上のR1基によって置換されているかのいずれかのペンタジエニル(Op)配位子を示し、yは前記ペンタジエニル配位子上のR1置換基の数を示し、
(R2 tCp)は、置換されていないか、または1つ以上のR2基によって置換されているかのいずれかのシクロペンタジエニル(Cp)配位子を示し、tは前記シクロペンタジエニル配位子上のR1置換基の数を示し、
R1およびR2は同一または異なり、かつ、塩素基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN-アルキルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖であり1ないし4個の個の炭素原子を持つN,N-ジアルキルアミノ基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルコキシ基、アルキルシリルアミド基、アミジナート基およびカルボニル基からなる群より独立に選択され、
R’は、水素、フッ素、塩素、臭素またはヨウ素原子、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つ直鎖または分岐鎖であるN-アルキルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN,N-ジアルキルアミノ基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルコキシ基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキルシリルアミノ基、互いに同一または異なる各々のアルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つジアルキルシリルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つトリアルキルシリルアミノ基、アミジナート基およびカルボニルからなる群より独立に選択される配位子を示し、前記式(II)が2つ以上のR’基を含む場合は、各々のR’が互いに同一または異なり得ると理解される)のM1金属含有前駆体を気化させ、前記第1の気相金属源を形成する工程(b)と、
- 任意で、少なくとも1つのM2金属含有前駆体 (M2は先に定義されたものである)を気化させ、任意の第2の気相金属源を形成する工程b')と、
- 前記第1の気相金属源と前記任意の第2の気相金属源とを反応チャンバーに導入し、それらと前記基板との接触を生じさせ、前記基板上に先に定義された式(I)の化合物を含有する金属含有誘電性フィルムの堆積を生じさせる工程c)と
を含む(ただし、形成される少なくとも1つの金属含有誘電体フィルムが、a=0、b=2、かつc=0であるところの先に定義された式(I)に相当する式(I'):M1 1 O2の化合物を含む場合、および工程b)で用いられるM1金属含有前駆体が、x=0かつz=2であるところの先に定義された式(II)に相当する式(II'):(R2 tCp)2 M1 R’2の化合物を含む場合は、前記式(II')における2つの(R2 tCp)配位子の少なくとも1つにおいてt>0である)。
ジシロキサン、トリシリルアミン、ジシラン、トリシラン、式(III1):SiHx(OR3)4-x(ここで0≦x≦3であり、R3は1ないし6個の炭素原子を持つ直鎖または分岐鎖炭化水素を示す)のアルコキシシラン、
式(III2):Si(OH)x(OR4)4-x (ここで、1≦x≦3であり、R4は1ないし6個の炭素原子を持つ直鎖または分岐鎖炭化水素基を示す)、好ましくはSi(OH)(OR4)3、より好ましくはSi(OH)(OtBu)3のシラノール誘導体、
式(III3):SiHx(NR5R6)4-x (ここで0≦x≦3であり、R5およびR6は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、好ましくはSiH(NMe2)3 (TriDMAS)、SiH2(NHtBu)2 (BTBAS)、SiH2(NEt2)2 (BDEAS)のアミノシラン誘導体およびそれらの混合物
のようなケイ素誘導体またはそれらのゲルマニウム同族体と、
トリメチルアルミニウム [Al(CH3)3]、水素化ジメチルアルミニウム [AlH(CH3)2]、式(IV1):AlR8 x(OR7)3-x (ここで0≦x≦3であり、R7は1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示し、R8はR7と同一または異なり、水素原子を示す)、
または好ましくは、独立に1ないし6個の炭素原子を示す同一または異なるR9とR10とを有するAlR9R10(OR7)、最も好ましくはAlMe2(OiPr)のアルコキシアラン、
式(IV2):AlR11 x(NR12R13)3-xのアミドアラン(ここで0≦x≦3であり、R12およびR13は同一または異なり、水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示し、R11はR7と同一または異なり、水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなアルミニウム誘導体と、
Ta(OMe)5、Ta(OEt)5、Ta(NMe2)5、Ta(NEt2)5、Ta(NEt2)5、式(V1):Ta(OR14)4[O-C(R15)(R16)-CH2-OR17] (ここでR14、R15、R16およびR17は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、好ましくはTa(OEt)4(OCMe2CH2-OMe) (TAT-DMAE)のタンタル誘導体、
式(V2):Ta(OR18)4[O-C(R19)(R20)-CH2-N(R21)(R22)]のタンタル誘導体(ここでR18、R19、R20、R21およびR22は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、
式(V3):Ta(=NR24)(NR25R26)3のタンタル誘導体(ここでR24、R25およびR26は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなタンタル誘導体と、
Nb(OMe)5、Nb(OEt)5、Nb(NMe2)5、Nb(NEt2)4、Nb(NEt2)5、式(VI1):Nb(OR27)4(O-C(R28)(R29)-CH2-OR30) (ここで、R27、R28、R29および R30は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、好ましくはNb(OEt)4(OCMe2CH2-OMe) (NBT-DMAE)のニオブ誘導体、
式(VI2):Nb(OR31)4[O-C(R32)(R33)-CH2-N(R34)(R35)]のニオブ誘導体(ここでR31、R32、R33、R34およびR35は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、
式(VI3):Nb(=NR36)(NR37R38)3のニオブ誘導体(ここでR36、R37およびR38は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなニオブ誘導体と、
スカンジウム誘導体、イットリウム誘導体、セリウム誘導体、プラセオジム誘導体、ガドリニウム誘導体、ジスプロジウム誘導体、エルビウム誘導体、ランタン誘導体、少なくとも1つのβジケトナート配位子または1ないし6個の炭素原子を持つ1つまたは複数の直鎖または分岐鎖アルキル基で任意に置換された少なくとも1つのシクロペンタジエニル配位子を有する誘導体
のようなランタノイド誘導体と、
少なくとも1つのβジケトナート配位子または1ないし6個の炭素原子を持つ1つまたは複数の直鎖または分岐鎖アルキル基で任意に置換された少なくとも1つのシクロペンタジエニル配位子を有するストロンチウム(Sr)、バリウム(Ba)、マグネシウム(Mg)、カルシウム(Ca)または亜鉛(Zn)誘導体
のような2価金属誘導体と、
タングステン(W)、モリブデン(Mo)、ハフニウム(Hf)またはジルコニウム(Zr)誘導体、例えばアルコキシ誘導体、アミノ誘導体またはこれらの化学種を含有する付加体
のような他の金属誘導体(前記誘導体は先に定義された式(II)の化合物ではないと理解される)と
からなる群より選択される。
- 少なくとも1つの式(II)のM1金属含有前駆体と、必要ならば少なくとも1つのM2金属含有前駆体とが、工程c)に先立って少なくとも1つの反応物質と混合される工程d)
を含む。
- 少なくとも1つの式(II)のM1金属含有前駆体と、必要ならば少なくとも1つのM2金属含有前駆体とが、反応チャンバー中で少なくとも1つの反応物質と混合される工程d'')
を含む。
式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3およびそれらの混合物からなる群より選択される。
式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3およびそれらの混合物からなる群より選択される。
ここで式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3からなる群より選択され、M2金属含有前駆体は、好ましくは先に定義されたケイ素誘導体またはそれらのゲルマニウム同族体、タンタル誘導体、ランタノイド誘導体およびマグネシウム誘導体からなる群より選択される。
ここで式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3からなる群より選択され、M2金属含有前駆体は、好ましくは先に定義されたケイ素誘導体またはそれらのゲルマニウム等価物、タンタル誘導体、ランタノイド誘導体およびマグネシウム同族体から選択され、少なくとも1つの酸素含有前駆体と少なくとも1つの窒素含有前駆体とが反応器に導入される。
式(II1)の化合物を生成するために、工程1で調製された式(VII1)の化合物とNH(R39)(R40)との反応からなる工程2と
を含むプロセスに関する。
堆積されるフィルムは、a=0、b=2かつc=0である式(I)の化合物を含有する。
a) 式(II)の化合物は、Zr(MeCp)2Me2、Zr(EtCp)2Me2、Hf(MeCp)2Me2およびHf(MeCp)2Me2から選択され、
液体での分子の配送は、通常、不活性ガス(N2、He、Arなど)を液体中にバブリングし、不活性ガスと液体ガスとの混合物を反応器に提供することによって実行される。
堆積されるフィルムは、a=0であり、かつbおよびcはゼロではない式(I)の化合物を含有する。
堆積されるフィルムは、a≠0、b≠0かつc=0である式(I)の化合物を含有する。
a) ケイ素(またはゲルマニウム)源、例えばSi(OH)(OtBu)3、SiH(NMe2)3 (TriDMAS)、SiH2(NHtBu)2 (BTBAS)およびSiH2(NEt2)2 (BDEAS)、
b) アルミニウム源、例えばAlMe2(OiPr)、または、
c) タンタル(またはニオブ)源、例えばTa(OMe)5、Ta(OEt)5およびTa(OEt)(OCMe2CH2-OMe) (TATDMAE)
であるべきである。
堆積されるフィルムは、a≠0、b≠0かつc≠0である式(I)の化合物を含有する。
Zr(EtCp)(NMe2)3は3段階で調製される。
熱重量測定装置を水蒸気および酸素含有量を1 ppmv未満に維持したアルゴングローブボックス中に保持した。熱重量分析は、35 mgのサンプルをアルミニウム坩堝中に配置することによって実行された。サンプルは、10℃ / minの温度傾斜で35℃から400℃まで加熱された。質量減少は、坩堝温度の関数としてモニターされた。残渣のレベルは、260℃の全気化温度において2.6%であった。得られたグラフは図1である。
Zr(EtCp)(NMe2)3は容器の中に保持される。容器は90℃に加熱され、N2が50 sccmの流量でキャリアガスとして使用される。容器の圧力は50 Torrに制御される。O3が酸素源として使用される。基板は350℃に加熱される。最初の工程の間、Zr(EtCp)(NMe2)3が反応チャンバーに2秒間導入される。その後5秒のN2パージが第2の工程として実行される。次に第3の工程としてO3のパルスが反応チャンバーに2秒間導入され、その後第4の工程として2秒間のN2パージが導入される。ZrO2フィルムを得るために、4つの工程全てが100回繰り返される。自己制限原子層堆積が得られる。
Zr(EtCp)(NMe2)3は容器の中に保持される。容器は90℃に加熱され、N2が50 sccmの流量でキャリアガスとして使用される。容器の圧力は50 Torrに制御される。 Zr(EtCp)(NMe2)3がO2/N2ガス混合物と反応チャンバーの中で混合される。基板は500℃に加熱される。反応チャンバー内の圧力は10 Torrに設定される。酸化ジルコニウムのフィルムが得られる。同様の実験はHf類縁体について実行され得る。
Zr(EtCp)(NMe2)3およびZr(NEtMe)4の熱重量分析は同じ条件で実行される。熱重量分析装置は、1 ppmv未満の水蒸気および酸素含有量のアルゴングローブボックス中に保持された。熱重量分析は、35 mgのサンプルをアルミニウム坩堝中に配置することによって実行された。次にサンプルは、10℃/ minの温度傾斜で35℃から400℃まで加熱された。質量減少は、坩堝温度の関数としてモニターされた。クローズドカップ構造において、気化を遅らせるために金属-有機化合物を含む坩堝の上に穴開きパン(0.8 mm)が配置された。これは高温での熱安定性を示す。結果は、Zr(EtCp)(NMe2)3はZr(NEtMe)4よりもはるかに熱的に安定であり、気相前駆体としての使用についてより魅力的であることを示す。結果は図2に示される。
Hf(EtCp)2Cl2は、1モルのHfCl4をEtCpNaと反応させることで容易に得られる。
この例は酸化ハフニウムフィルムの構築に関する。シリコンウェーハは、周囲にヒーターを具備した堆積チャンバーの中にマウントされ、所望されるフィルムがシリコンウェーハの表面に形成される。チャンバーはポンプによって真空にされる。金属前駆体、この場合ジメチルハフノセン HfMe2(EtCp)2は、加熱された液体容器の中に保持される。窒素ガスがHf(EtCp)2Me2のためのキャリアガスとして使用される。液体容器中のHf(EtCp)2Me2は、液化材料を通して窒素によって輸送される。窒素はマスフローコントローラーによって気化器に輸送される。Hf(EtCp)2Me2の蒸気は窒素によって運ばれ、一緒にチャンバーの中に供給されるか、または前駆体を反応器の中に導入することができる弁が閉じられている場合はバイパスラインの方に回される。酸素/オゾンガス混合物(酸化剤)も、マスフローコントローラーによってチャンバーの中またはバイパスラインのいずれかに供給される。蓋然性の高いCVD反応を避けるために、一方の側の酸素/オゾンと、他方の側のHf(EtCp)2Me2とは決して一緒に導入されない。それらは通常、1つずつ導入され、各々の反応物質パルスは、N2のみがチャンバー中に導入されるパージ時間に従って分割される。
圧力=3 torr、温度350℃、Hf(EtCp)2Me2の流量=0.5 sccm、O2の流量=100 sccm、O3の流量=8 sccm、N2の流量=100 sccm。
Claims (18)
- 式(I):(M1 1-a M2 a) Ob Nc(ここで、
0≦a<1、
0<b≦3、好ましくは1.5≦b≦2.5、
0≦c≦1、
M1はハフニウム(Hf)、ジルコニウム(Zr)およびチタン(Ti)から選択される金属を示し、
M2は、マグネシウム(Mg)、カルシウム(Ca)、亜鉛(Zn)、ホウ素(B)、アルミニウム(A)、インジウム(In)、ケイ素(Si)、ゲルマニウム(Ge)、スズ(Sn)、ハフニウム(Hf)、ジルコニウム(Zr)、チタン(Ti)、バナジウム(V)、ニオブ(Nb)、タンタル(Ta)、ならびにランタノイド原子、より具体的にはスカンジウム(Sc)、イットリウム(Y)およびランタン(La)および希土類金属原子からなる群より選択される金属原子を示す)の化合物を含む少なくとも1つの金属含有誘電体フィルムを基板上に堆積する方法であって、
- 基板を反応チャンバーの中に提供する工程a)と、
- 少なくとも1つの式(II):(R1 yOp)x (R2 tCp)z M1 R’4-x-z (ここで、
M1は先に定義されたものであり、
0≦x≦3、好ましくはx=0または1であり、
0≦z≦3、好ましくはz=1または2であり、
1≦(x+z)≦4であり、
0≦y≦7、好ましくはy=2、0≦t≦5、好ましくはt=1であり、
(R1 yOp)は、置換されていないか、または1つ以上のR1基によって置換されているかのいずれかであるペンタジエニル(Op)配位子を示し、yは前記ペンタジエニル配位子上のR1置換基の数を示し、
(R2 tCp)は、置換されていないか、または1つ以上のR2基によって置換されているかのいずれかであるシクロペンタジエニル(Cp)配位子を示し、tは前記シクロペンタジエニル配位子上のR1置換基の数を示し、
R1とR2は同一または異なり、塩素基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN-アルキルアミノ基、互いに同一または異なる各々のアルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN,N-ジアルキルアミノ基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルコキシ基、アルキルシリルアミド基、アミジナート基またはカルボニル基からなる群より独立に選択され、
R’は、水素、塩素、臭素またはヨウ素原子、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN-アルキルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つN,N-ジアルキルアミノ基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルコキシ基、1ないし4個の炭素原子を持つ直鎖または分岐鎖アルコキシ基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つアルキルシリルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つジアルキルシリルアミノ基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つトリアルキルシリルアミノ基、アミジナート基またはカルボニルからなる群より独立に選択される配位子を示し、前記式(II)が2つ以上のR’基を含む場合は、各々のR’は互いに同一または異なり得ると理解される)のM1金属含有前駆体を気化させ、第1の気相金属源を形成する工程b)と、
- 任意で、少なくとも1つのM2金属含有前駆体 (M2は先に定義されたものである) を気化させ、任意の第2の気相金属源を形成する工程b')と、
- 前記第1の気相金属源と前記任意の第2の気相金属源とを前記反応チャンバーに導入し、それらと前記基板との接触を生じさせ、前記基板上に先に定義された式(I)の化合物を含有する金属含有誘電体フィルムの堆積を生じさせる工程c)と
を含む(ただし、形成される少なくとも1つの金属含有誘電体フィルムが、a=0、b=2、かつc=0であるところの先に定義された式(I)に相当する式(I'):M1 1 O2の化合物を含む場合、および工程b)で用いられるM1金属含有前駆体が、x=0かつz=2であるところの先に定義された式(II)に相当する式(II'):(R2 tCp)2 M1 R’2の化合物を含む場合は、前記式(II')における2つの(R2 tCp)配位子の少なくとも1つにおいてt>0である)方法。 - 前記気化工程b)と前記気化工程b')とが、両方の源の気化工程b'')に1つに統合される請求項1による方法。
- 前記M2金属含有前駆体が、
ジシロキサン、トリシリルアミン、ジシラン、トリシラン、式(III1):SiHx(OR3)4-xのアルコキシシラン(ここで、0≦x≦3であり、R3は1ないし6個の炭素原子を持つ直鎖または分岐鎖炭化水素を示す)、
式(III2):Si(OH)x(OR4)4-x (ここで、1≦x≦3であり、R4は1ないし6個の炭素原子を持つ直鎖または分岐鎖炭化水素基を示す)、好ましくはSi(OH)(OR4)3、より好ましくはSi(OH)(OtBu)3のシラノール誘導体、
式(III3):SiHx(NR5R6)4-x (ここで0≦x≦3であり、R5およびR6は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、好ましくはSiH(NMe2)3 (TriDMAS)、SiH2(NHtBu)2 (BTBAS)、SiH2(NEt2)2 (BDEAS)のアミノシラン誘導体およびそれらの混合物
のようなケイ素誘導体またはそれらのゲルマニウム同族体と、
トリメチルアルミニウム [Al(CH3)3]、水素化ジメチルアルミニウム [AlH(CH3)2]、式(IV1):AlR8 x(OR7)3-x (ここで0≦x≦3であり、R7は1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示し、R8はR7と同一または異なり、水素原子を示す)、または好ましくは、独立に1ないし6個の炭素原子を持つ同一または異なるR9とR10とを有するAlR9R10(OR7)、最も好ましくはAlMe2(OiPr) のアルコキシアラン、
式(IV2):AlR11 x(NR12R13)3-xのアミドアラン(ここで0≦x≦3であり、R12およびR13は同一または異なり、水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示し、R11はR7と同一または異なり、水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなアルミニウム誘導体と、
Ta(OMe)5、Ta(OEt)5、Ta(NMe2)5、Ta(NEt2)5、Ta(NEt2)5、式(V1):Ta(OR14)4[O-C(R15)(R16)-CH2-OR17] (ここで、R14、R15、R16およびR17は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、好ましくはTa(OEt)4(OCMe2CH2-OMe) (TAT-DMAE)のタンタル誘導体、
式(V2):Ta(OR18)4[O-C(R19)(R20)-CH2-N(R21)(R22)]のタンタル誘導体(ここでR18、R19、R20、R21およびR22は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、
式(V3):Ta(=NR24)(NR25R26)3のタンタル誘導体(ここでR24、R25およびR26は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなタンタル誘導体と、
Nb(OMe)5、Nb(OEt)5、Nb(NMe2)5、Nb(NEt2)4、Nb(NEt2)5、式(VI1):Nb(OR27)4(O-C(R28)(R29)-CH2-OR30) (ここで、R27、R28、R29および R30は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)のニオブ誘導体、好ましくはNb(OEt)4(OCMe2CH2-OMe) (NBT-DMAE)、
式(VI2):Nb(OR31)4[O-C(R32)(R33)-CH2-N(R34)(R35)]のニオブ誘導体(ここでR31、R32、R33、R34およびR35は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)、
式(VI3):Nb(=NR36)(NR37R38)3のニオブ誘導体(ここでR36、R37およびR38は同一または異なり、独立に水素原子または1ないし6個の炭素原子を持つ直鎖または分岐鎖アルキルを示す)
のようなニオブ誘導体と、
スカンジウム誘導体、イットリウム誘導体、セリウム誘導体、プラセオジム誘導体、ガドリニウム誘導体またはNd誘導体、少なくとも1つのβジケトナート配位子または1ないし6個の炭素原子を持つ1つまたは複数の直鎖または分岐鎖アルキル基で任意に置換された少なくとも1つのシクロペンタジエニル配位子を有する誘導体
のようなランタノイド誘導体と、
少なくとも1つのβジケトナート配位子または1ないし6個の炭素原子を持つ1つまたは複数の直鎖または分岐鎖アルキル基で任意に置換された少なくとも1つのシクロペンタジエニル配位子を有するストロンチウム(Sr)、バリウム(Ba)、マグネシウム(Mg)、カルシウム(Ca)または亜鉛(Zn)誘導体
のような2価金属誘導体と、
タングステン(W)、モリブデン(Mo)、ハフニウム(Hf)またはジルコニウム(Zr)誘導体、例えばアルコキシ誘導体、アミノ誘導体またはこれらの化学種を含有する付加体
のような他の金属誘導体(前記誘導体は先に定義された式(II)の化合物ではないと理解される)と
からなる群より選択される、請求項1または2による方法。 - 前記少なくとも1つの式(II)のM1金属含有前駆体と、必要ならば前記少なくとも1つのM2金属含有前駆体とが、工程c)に先立って少なくとも1つの反応物質と混合される工程d)をさらに含む、請求項1ないし3の1項による方法。
- 前記少なくとも1つの式(II)のM1金属含有前駆体と、必要ならば前記少なくとも1つのM2含有前駆体とが、前記反応チャンバー中で少なくとも1つの反応物質と混合される工程d')をさらに含む、請求項1ないし4の1項による方法。
- 前記工程(b)が、前記式(II)の少なくとも1つの金属含有前駆体を、次の第2の前駆体M1(NMe2)4、M1(NEt2)4、M1(NMeEt)4、M1(mmp)4、M1(OtBu)4、M1(OtBu)2(mmp)2およびそれらの混合物のうちの少なくとも1つと一緒に混合する工程(b1)と、前記混合物を気化させる工程(b2)とからなる、請求項1ないし5の1項による方法。
- 前記M1金属含有前駆体がx=0、z=1であり、かつR’は基N(R39)(R40) (ここでR39およびR40は同一または異なり、独立に水素原子、または1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つアルキルシリル基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つジアルキルシリル基、または各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つトリアルキルシリル基を示す)を示すところの前記式(II)に相当する式(II1):(R2 tCp)M1[N(R39)(R40)]3のものである、請求項1ないし6の1項による方法。
- a=0、b=0かつc=0であるところの前記式(I)に相当する前記式(I1):M1O2の化合物を含有する金属含有誘電体フィルムの堆積の方法であり、前記式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3およびそれらの混合物からなる群より選択される、請求項1ないし7の1項による方法
- a=0、1.5≦b≦2.5かつ0<c≦0.5であるところの前記式(I)に相当する前記式(I2):M1Ob Ncの化合物を含有する金属含有誘電体フィルムの堆積であり、前記式(II)の金属含有前駆体は、HfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3およびそれらの混合物からなる群より選択される、請求項1ないし7の1項による方法。
- 0≦a<1かつc=0であるところの前記式(I)に相当する前記式(I3):(M1 1-a M2 a) Obの化合物を含有する金属含有誘電体フィルムの堆積であり、前記式(II)の金属含有前駆体はHfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3からなる群より選択され、前記M2含有先駆体は好ましくは先に定義されたケイ素誘導体またはそれらのゲルマニウム同族体、前記タンタル誘導体、ランタノイド誘導体および前記マグネシウム誘導体から選択される、請求項1ないし7の1項による方法。
- 0≦a<1かつ0<c≦0.5であるところの前記式(I)に相当する前記式(I4):(M1 1-a M2 a) Ob Ncの化合物を含有する金属含有誘電体フィルムの堆積であり前記式(II)の金属含有前駆体はHfCp2Cl2、Hf(MeCp)2Me2、HfCp(MeCp)Cl2、Hf(MeCp)2Cl2、HfCp(MeCp)Me2、Hf(EtCp)(MeCp)Me2、Hf(EtCp)2Me2、Hf(MeCp)2(CO)2、ZrCp2Cl2、Zr(MeCp)2Me2、ZrCp(MeCp)Cl2、Zr(MeCp)2Cl2、ZrCp(MeCp)Me2、Zr(EtCp)(MeCp)Me2、Zr(EtCp)2Me2、Zr(MeCp)2(CO)2、Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3からなる群より選択され、前記M2含有前駆体は、好ましくは先に定義された前記ケイ素誘導体またはそれらのゲルマニウム同族体物、前記タンタル誘導体、ランタノイド誘導体および前記マグネシウム誘導体から選択され、少なくとも1つの酸素含有前駆体と少なくとも1つの窒素含有前駆体とが前記反応器に導入される、請求項1ないし7の1項による方法。
- 誘電体フィルム、より具体的には集積回路用のものを作るための、またはランダムアクセスメモリーのための金属-絶縁体-金属(MIM)構造物の作製における、請求項1で定義された前記式(II)の化合物の使用。
- x=0、z=1であり、かつR’がN(R39)(R40)基(ここでR39およびR40は同一または異なり、独立に水素原子、または1ないし4個の炭素原子を持つ直鎖または分岐鎖アルキル基、アルキル基が直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つアルキルシリル基、各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つジアルキルシリル基、または各アルキル基が互いに同一または異なり、直鎖または分岐鎖でありかつ1ないし4個の炭素原子を持つトリアルキルシリル基を示す)を示すところの請求項1で定義された前記式(II)に相当する式(II1):(R2 tCp)M1[N(R39)(R40)]3の化合物。
- R2、R39およびR40が同一または異なり、独立にメチル、エチル、プロピル、イソプロピル、ブチル、イソブチル、sec-ブチルおよびtert-ブチル基からなる群より選択されるラジカルを示す、請求項13で定義された前記式(II1)の化合物。
- Zr(MeCp)(NMe2)3、Zr(EtCp)(NMe2)3、ZrCp(NMe2)3、Zr(MeCp)(NEtMe)3、Zr(EtCp)(NEtMe)3、ZrCp(NEtMe)3、Zr(MeCp)(NEt2)3、Zr(EtCp)(NEt2)3、ZrCp(NEt2)3、Zr(iPr2Cp)(NMe2)3、Zr(tBu2Cp)(NMe2)3、Hf(MeCp)(NMe2)3、Hf(EtCp)(NMe2)3、HfCp(NMe2)3、Hf(MeCp)(NEtMe)3、Hf(EtCp)(NEtMe)3、HfCp(NEtMe)3、Hf(MeCp)(NEt2)3、Hf(EtCp)(NEt2)3、HfCp(NEt2)3、Hf(iPr2Cp)(NMe2)3、Hf(tBu2Cp)(NMe2)3である、請求項14で定義された前記式(II1)の化合物。
- Zr(EtCp)(NMe2)3、Zr(MeCp)(NMe2)3、ZrCp(NMe2)3、Hf(EtCp)(NMe2)3、Hf(MeCp)(NMe2)3およびHfCp(NMe2)3である、請求項15で定義された前記式(II1)の化合物。
- 請求項13ないし16の1項で定義された前記式(II1)の化合物を調製するためのプロセスであって、
M1Cl4と(R2 tCp)Naの反応による式(VII1):(R2 tCp)M1Cl3の化合物(ここでM1、R2およびtは前記式(II)について先に定義されたものである)の調製からなる工程1と、
前記式(II1)の化合物を生成するための、工程1で調製された前記式(VII1)の化合物とNH(R39)(R40)との反応からなる工程2と
を含むプロセス。 - Hf(EtCp)2Me2、Zr(MeCp)2Me2またはZr(EtCp)2Me2である、請求項1で定義された前記式(II)の化合物。
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