JP6598032B2 - 強誘電体セラミックス及びその製造方法 - Google Patents
強誘電体セラミックス及びその製造方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims description 31
- 238000004519 manufacturing process Methods 0.000 title claims description 20
- 239000000758 substrate Substances 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000002243 precursor Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 description 59
- 238000002441 X-ray diffraction Methods 0.000 description 47
- 230000000052 comparative effect Effects 0.000 description 17
- 239000013078 crystal Substances 0.000 description 17
- 238000004544 sputter deposition Methods 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010587 phase diagram Methods 0.000 description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000003980 solgel method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 229960002887 deanol Drugs 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000001552 radio frequency sputter deposition Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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Description
[1]Pb(Zr1−ATiA)O3膜と、
前記Pb(Zr1−ATiA)O3膜上に形成されたPb(Zr1−xTix)O3膜と、を具備し、
前記A及び前記xは下記式1〜式3を満たすことを特徴とする強誘電体セラミックス。
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3
なお、Pb(Zr1−xTix)O3膜は(001)に配向する。
前記Aが0であり、
前記Pb(Zr1−ATiA)O3がPbZrO3膜であることを特徴とする強誘電体セラミックス。
なお、Pb(Zr1−xTix)O3膜は(001)に配向する。
前記Pb(Zr1−ATiA)O3膜は酸化膜上に形成されていることを特徴とする強誘電体セラミックス。
なお、前記酸化膜は、ペロブスカイト構造の酸化物であることが好ましい。
前記酸化膜はSr(Ti,Ru)O3膜であることを特徴とする強誘電体セラミックス。
なお、前記Sr(Ti,Ru)O3膜は、Sr(Ti1−xRux)O3膜であることが好ましく、前記xは下記式4を満たす。
0.01≦x≦0.4 ・・・式4
前記Pb(Zr1−ATiA)O3膜は電極膜上に形成されていることを特徴とする強誘電体セラミックス。
前記電極膜は酸化物または金属からなることを特徴とする強誘電体セラミックス。
なお、前記酸化物はSr(Ti1−xRux)O3膜であってもよく、前記xは下記式4を満たす。
0.01≦x≦0.4 ・・・式4
前記電極膜はPt膜またはIr膜であることを特徴とする強誘電体セラミックス。
なお、Pt膜は(100)に配向する。
y 前記電極膜はZrO2膜上に形成されていることを特徴とする強誘電体セラミックス。
なお、ZrO2膜は(100)に配向する。
前記電極膜はSi基板上に形成されていることを特徴とする強誘電体セラミックス。
なお、Si基板は(100)に配向している。
前記A及び前記xは下記式1〜式3を満たすことを特徴とする強誘電体セラミックスの製造方法。
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3
なお、Pb(Zr1−xTix)O3膜は(001)に配向する。
前記Aが0であり、
前記Pb(Zr1−ATiA)O3膜がPbZrO3膜であることを特徴とする強誘電体セラミックスの製造方法。
なお、Pb(Zr1−xTix)O3膜は(001)に配向する。
[12]上記[10]または[11]において、
前記Pb(Zr1−ATiA)O3膜は、Pb(Zr1−ATiA)O3の前駆体溶液を基板上に塗布し、5atm以上(好ましくは7.5気圧以上)の酸素雰囲気で結晶化を行うことで形成されることを特徴とする強誘電体セラミックスの製造方法。
図1は、本発明の一態様に係る強誘電体セラミックスの製造方法を説明する模式的な断面図である。
0.01≦x≦0.4 ・・・式4
PZOは図23に示すように斜方晶である。このため、PZOは見かけ上格子定数が大きくなっている。それは、ペロブスカイトが縦に45°程度回転していて、あたかも回転した結晶を点線部分のように周囲を取り囲んで、大きな結晶のように取り扱っているためである。つまり、見かけ上、a,b,c軸の長さがとても長くなっているように取り扱うのが斜方晶の慣例である。実際のPZOは実線のような結晶で、通常のペロブスカイト結晶である。
0<x<1 ・・・式2'
PZT膜形成用ゾルゲル溶液としては、ブタノールを溶媒とする鉛が70%〜90%不足した量添加された、濃度10重量%濃度のE1溶液を用いた。
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3
上記式1を満たすこと、つまりTi比率を10%以下とすることで、初期核として用いるPb(Zr1−ATiA)O3膜が反強誘電性斜方晶相のPZT(つまりPb(Zr,Ti)O3の相図中、斜方晶領域(ortho領域)のPZT)となり、Pb(Zr1−ATiA)O3が全てのPb(Zr1−xTix)O3(PZT)のc軸長を伸ばす方向に働き、上記実施形態と同様の効果を得ることができる。
図2は、本発明の一態様に係る強誘電体セラミックスの製造方法を説明する模式的な断面図であり、図1と同一部分には同一符号を付す。
0.01≦x≦0.4(好ましくは0.05≦x≦0.2) ・・・式4
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3
上記式1を満たすことで第1の実施形態と同様の効果を得ることができる。
1.4mol/kg濃度の1.3PbZrO3形成用MOD溶液(豊島製作所製Lot.00050667-1),エタノール,2nブトキシエタノールを合わせて1000ml(それぞれ1:1:1の割合で混合)とし、その中に、ポリビニルピロリドン(日本触媒K-30)という白色粉末を20g添加し、撹拌溶解したものをPZO250nmの原料溶液とした、この溶液3mlを6inウェハ上に滴下し、3000rpmで10sec回転塗布した後、150℃ホットプレート上に30sec保持、次に250℃ホットプレート上に90sec保持した後、1atm-O2雰囲気中で600℃,3min焼結した。
図8に示すサンプルのSi基板11、ZrO2膜12及びPt膜13は、図3(A)に示す実施例1によるサンプルと同様の方法で作製された。
プロセス :RF−スパッタリング
ターゲット :Sr(Ti0.8Ru0.2)O3
RFパワー :400W/13.56MHz
プロセス圧力 :4Pa
ガス流量 Ar/O2(sccm):30/10
基板温度 :600℃
プロセス時間 :20sec
膜厚:50nm
アニール温度:600℃
導入ガス :酸素ガス
圧力 :9kg/cm2
昇温レート :100℃/sec
アニール時間:5分
(1)1.4mol/kg濃度の1.3PbZrO3形成用MOD溶液(豊島製作所製Lot.00050667-1),エタノール,2nブトキシエタノールを合わせて1000ml(それぞれ1:1:1の割合で混合)とし、その中に、ポリビニルピロリドン(日本触媒K-30)という白色粉末を10g添加し、撹拌溶解したものをPZO-50nmの原料溶液とした、この溶液3mlを6inウェハ上に滴下し、5000rpmで10sec回転塗布した後、150℃ホットプレート上に30sec保持、次に250℃ホットプレート上に90sec保持した後、1atm-O2雰囲気中で600℃,3min焼結し、厚さ50nmのPZO膜を形成した。
(2)1.4mol/kg濃度の1.3PbZrO3形成用MOD溶液(豊島製作所製Lot.00050667-1),エタノール,2nブトキシエタノールを合わせて1000ml(それぞれ1:1:1の割合で混合)とし、その中に、ポリビニルピロリドン(日本触媒K-30)という白色粉末を20g添加し、撹拌溶解したものをPZO-250nmの原料溶液とした、この溶液3mlを6inウェハ上に滴下し、3000rpmで10sec回転塗布した後、150℃ホットプレート上に30sec保持、次に250℃ホットプレート上に90sec保持した後、1atm-O2雰囲気中で600℃,3min焼結し、厚さ250nmのPZO膜を形成した。
(3)1.4mol/kg濃度の1.3PbZrO3形成用MOD溶液(豊島製作所製Lot.00050667-1),エタノール,2nブトキシエタノールを合わせて1000ml(それぞれ1:1:1の割合で混合)とし、その中に、ポリビニルピロリドン(日本触媒K-30)という白色粉末を20g添加し、撹拌溶解したものをPZO-400nmの原料溶液とした、この溶液3mlを6inウェハ上に滴下し、1000rpmで10sec回転塗布した後、150℃ホットプレート上に30sec保持、次に250℃ホットプレート上に90sec保持した後、1atm-O2雰囲気中で600℃,3min焼結し、厚さ400nmのPZO膜を形成した。
装置 : RFマグネトロンスパッタリング装置
パワー : 1500W
ガス : Ar/O2
圧力 : 0.14Pa
温度 : 600℃
成膜速度 : 0.63nm/秒
成膜時間 : 1.3分
サンプル1(実施例): 50nm なし
サンプル2(実施例): 250nm なし
サンプル3(実施例): 400nm なし
サンプル4(実施例): 50nm 1000nm(総膜厚1050nm)
サンプル5(実施例):250nm 2500nm(総膜厚2750nm)
サンプル6(実施例):400nm 4000nm(総膜厚4400nm)
サンプル7(比較例): なし 1000nm
サンプル8(比較例): なし 2500nm
サンプル9(比較例): なし 4000nm
12 ZrO2膜
13 Pt膜
14 Sr(Ti0.8Ru0.2)O3膜(STRO膜)
15 PbZrO3膜(PZO膜)とPb(Zr0.55Ti0.45)O3膜(PZT膜)を順に積層した積層膜
16 PZO膜
17 Pb(Zr0.55Ti0.45)O3膜(PZT膜)
103 下部電極
104 PbZrO3膜(PZO膜)
105 PZT膜
106 酸化膜
Claims (10)
- Sr(Ti,Ru)O 3 膜と、
前記Sr(Ti,Ru)O 3 膜上に形成されたPb(Zr1−ATiA)O3膜と、
前記Pb(Zr1−ATiA)O3膜上に形成されたPb(Zr1−xTix)O3膜と、
を具備し、
前記A及び前記xは下記式1〜式3を満たすことを特徴とする強誘電体セラミックス。
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3 - 請求項1において、
前記Aが0であり、
前記Pb(Zr1−ATiA)O3がPbZrO3膜であることを特徴とする強誘電体セラミックス。 - 請求項1または2において、
前記Pb(Zr1−ATiA)O3膜は電極膜上に形成されていることを特徴とする強誘電体セラミックス。 - 請求項3において、
前記電極膜は酸化物または金属からなることを特徴とする強誘電体セラミックス。 - 請求項3において、
前記電極膜はPt膜またはIr膜であることを特徴とする強誘電体セラミックス。 - 請求項3乃至5のいずれか一項において、
前記電極膜はZrO2膜上に形成されていることを特徴とする強誘電体セラミックス。 - 請求項6において、
前記ZrO 2 膜はSi基板上に形成されていることを特徴とする強誘電体セラミックス。 - Sr(Ti,Ru)O 3 膜を形成するステップと、
前記Sr(Ti,Ru)O 3 膜上にPb(Zr 1−A Ti A )O 3 膜を形成するステップと、
前記Pb(Zr 1−A Ti A )O 3 膜上にPb(Zr 1−x Ti x )O 3 膜を形成するステップと、を具備し、
前記A及び前記xは下記式1〜式3を満たすことを特徴とする強誘電体セラミックスの製造方法。
0≦A≦0.1 ・・・式1
0.1<x<1 ・・・式2
A<x ・・・式3 - 請求項8において、
前記Aが0であり、
前記Pb(Zr1−ATiA)O3膜がPbZrO3膜であることを特徴とする強誘電体セラミックスの製造方法。 - 請求項8または9において、
前記Pb(Zr1−ATiA)O3膜を形成するステップでは、Pb(Zr1−ATiA)O3の前駆体溶液を基板上に塗布し、5atm以上の酸素雰囲気で結晶化を行うことにより前記Pb(Zr 1−A Ti A )O 3 膜が形成されることを特徴とする強誘電体セラミックスの製造方法。
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