CN108475580A - 多晶介电体薄膜及电容元件 - Google Patents
多晶介电体薄膜及电容元件 Download PDFInfo
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- CN108475580A CN108475580A CN201780006873.5A CN201780006873A CN108475580A CN 108475580 A CN108475580 A CN 108475580A CN 201780006873 A CN201780006873 A CN 201780006873A CN 108475580 A CN108475580 A CN 108475580A
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- Prior art keywords
- thin film
- film
- dielectric body
- body thin
- polycrystalline dielectric
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- 239000010409 thin film Substances 0.000 title claims abstract description 57
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- 229910052746 lanthanum Inorganic materials 0.000 claims description 5
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- 239000010408 film Substances 0.000 description 77
- 238000000034 method Methods 0.000 description 26
- 150000002500 ions Chemical class 0.000 description 25
- 239000000758 substrate Substances 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 17
- 238000000407 epitaxy Methods 0.000 description 16
- 239000000843 powder Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000010586 diagram Methods 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000003990 capacitor Substances 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 150000004706 metal oxides Chemical class 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 229910001427 strontium ion Inorganic materials 0.000 description 5
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 5
- 238000005266 casting Methods 0.000 description 4
- 238000000224 chemical solution deposition Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910001422 barium ion Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 238000001683 neutron diffraction Methods 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 150000002831 nitrogen free-radicals Chemical class 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000012552 review Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000013077 target material Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229940068984 polyvinyl alcohol Drugs 0.000 description 1
- 235000019422 polyvinyl alcohol Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 210000003462 vein Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/0647—Boron nitride
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Abstract
本发明提供介电损失tanδ小的多晶介电体薄膜及电容元件。是主要组成为钙钛矿型氮氧化物的多晶介电体薄膜。钙钛矿型氮氧化物以组成式AaBbOoNn(a+b+o+n=5)表示,a/b>1且n≥0.7。
Description
技术领域
本发明涉及多晶介电体薄膜及电容元件。
背景技术
近年来,伴随数字装置的小型化、高性能化,需要使用了高性能的介电体薄膜的电容元件。
以往,就介电体薄膜而言,广泛采用使用了金属氧化物材料的薄膜。但是,金属氧化物材料制得的介电体薄膜的特性改善已逐渐逼近极限,需要有更高特性的新材料。新材料的候选者之一可列举钙钛矿(perovskite)结晶结构中的氧八面体中的一部分氧原子置换成氮原子而成的金属氮氧化物材料。但是难以获得具有金属氮氧化物材料的介电体薄膜。
例如,专利文献1及专利文献2记载了制作钙钛矿型氮氧化物ABO2N粉末的方法。但是,专利文献1及专利文献2中针对获得使用钙钛矿型氮氧化物ABO2N的薄膜,没有任何揭示。
又,非专利文献1及非专利文献2记载了制作由钙钛矿型氮氧化物ABO2N构成的薄膜。但非专利文献1及非专利文献2获得的薄膜是磊晶膜(epitaxial film)。
磊晶膜是利用磊晶生长制得的薄膜。磊晶生长是一种薄膜结晶生长技术,是指在成为基板的结晶上进行结晶生长,整齐地排列在基底的基板的结晶面的结晶生长。
磊晶膜有制造非常耗时的缺点。非专利文献1中记载了制造厚度20nm以下的磊晶膜要耗费530小时以下的长时间。
[先前技术文献]
[专利文献]
专利文献1:日本特开昭61-122108号公报
专利文献2:日本特开2013-001625号公报
[非专利文献]
非专利文献1:Scientific Reports 4.DOI:10.1038/srep04987
非专利文献2:KAST平成25年度研究概要第32-33页
发明内容
(发明要解决的技术问题)
本发明是鉴于如此的实情而做出的,目的在于提供制造效率高、介电损失小的多晶介电体薄膜及电容元件。
(用于解决技术问题的手段)
本发明的多晶介电体薄膜的主要组成是钙钛矿型氮氧化物,其特征为:该钙钛矿型氮氧化物以组成式AaBbOoNn(a+b+o+n=5)表示,
a/b>1,且
n≥0.7。
本发明的多晶介电体薄膜通过具有上述特征,可减小介电损失。
本发明的多晶介电体薄膜优选为,前述A是选自Sr、Ba、Ca、La、Ce、Pr、Nd、Na中的1种以上的元素,前述B是选自Ta、Nb、Ti、W中的1种以上的元素。
本发明的多晶介电体薄膜优选具有BO4N2的八面体结构且该八面体结构中的N的配置以cis型为主。
本发明的电容元件具有前述多晶介电体薄膜。
附图说明
图1是本发明的一个实施方式的薄膜电容器的概略图。
图2A是表示N的配置为cis型(顺式型)时的示意图。
图2B是表示N的配置为trans型(反式型)时的示意图。
图3A是表示N的配置为cis型时的示意图。
图3B是表示N的配置为trans型时的示意图。
图4是由CaTaO2N构成的磊晶膜的XRD图的概略图。
具体实施方式
以下基于实施方式说明本发明。
本实施方式的薄膜电容器的示意图如图1所示。图1所示的薄膜电容器1,在基板11上按顺序形成下部电极12、多晶介电体薄膜13,且在多晶介电体薄膜13的表面具备上部电极14。
基板11的材质无特殊限制,使用单晶硅基板作为基板11的话,取得容易性及成本性优良。当重视挠性时,也可使用镍箔作为基板。
下部电极12及上部电极14的材质无特殊限制,发挥作为电极的功用即可。例如可列举Pt、Ag、Ni等。下部电极12的厚度优选为0.01~10μm。上部电极14的厚度优选为0.01~10μm。
多晶介电体薄膜13是主要组成为钙钛矿型氮氧化物的多晶介电体薄膜。
前述钙钛矿型氮氧化物能以组成式AaBbOoNn(a+b+o+n=5)表示。A为前述钙钛矿型氮氧化物的A位点(A-site)离子即可。B为前述钙钛矿型氮氧化物的B位点(B-site)离子即可。
A优选为选自Sr、Ba、Ca、La、Ce、Pr、Nd、Na中的1种以上的元素。若使用选自Sr、Ba、La、Nd中的1种以上的元素的话,可获得高电容,故更佳,使用Sr的话最佳。B优选为选自Ta、Nb、Ti、W中的1种以上的元素。使用选自Ta、Ti中的1种以上的元素的话,可获得非均相少的多晶介电体薄膜13,故更佳,使用Ta最佳。
进一步,优选a/b>1且n≥0.7。又,a/b更优选为a/b≥1.05。n更优选为n≥0.8。a/b及n通过为上述范围内,可使tanδ为良好。
又,前述钙钛矿型氮氧化物,其A位点离子的平均价数及B位点离子的平均价数的合计为6.7~7.3价。平均价数的合计优选为7价。
在此,平均价数是将存在于A位点及B位点的离子的价数根据其存在比平均化得到的值。例如,针对A位点上Sr与La以4∶1的比存在且B位点上Ta与Ti以4∶1的比存在的情形叙述。Sr离子的价数为2,La离子的价数为3。因此,令其平均价数为α时,α可由下式(1)算出。又,Ta离子的价数为5,Ti离子的价数为4。因此,令其平均价数为β时,β可由下式(2)算出。并且,α=2.2、β=4.8。然后,平均价数的合计(α+β)成为7。
α=(Sr离子的价数)×(Sr离子的存在比)+(La离子的价数)×(La离子的存在比)
=2×4/5+3×1/5
=2.2…式(1)
β=(Ta离子的价数)×(Ta离子的存在比)+(Ti离子的价数)×(Ti离子的存在比)
=5×4/5+4×1/5
=4.8…式(2)
又,本申请的平均价数的合计的计算中,富含A位点或是富含B位点时,亦即a/b≠1时,亦以a/b=1来处理。例如上述情形中,即使a/b=1.2的情况下,平均价数的合计也为2.2+4.8=7。
以下,举钙钛矿型氮氧化物为SraTabOoNn的情形为例说明,但A位点元素及/或B位点元素为不同元素的情形亦可套用。
在多晶介电体薄膜13中,优选具有BO4N2的八面体结构且前述八面体结构中的N的配置以cis型为主。
在此,氮(N)取顺式(cis)配置的结构,是如图2A所示的2个N彼此位于相邻位置的结构。相对于此,N取反式(trans)配置的结构,是如图2B所示的2个N彼此位于不相邻位置的结构。
针对N取cis配置的情形及N取trans配置的情形,分别显示多个八面体结构相连的情形的图是图3A及图3B。由图3A可知,N取cis配置时,结晶从c轴方向观察是曲曲折折地延伸。相对于此,由图3B可知,N取trans配置时,结晶是沿c轴方向一直线地延伸。且,N取trans配置时比起N取cis配置时的c轴较长。
本实施方式的多晶介电体薄膜中,N取cis配置为主的情况可利用中子衍射确认。即使不进行中子衍射,若ABO2N为多晶体,则可知N取稳定的cis配置。另一方面,欲获得trans配置的ABO2N时,需如非专利文献1那样,在基板上使其进行磊晶生长等而对于ABO2N的单晶施加基板应力,trans配置需要准备稳定且特殊的状态。但,cis配置为主的多晶体中,通常trans配置不会完全成为0。即使cis配置稳定,仍有时会因热运动等造成一部分的N的排列混乱并取trans配置的情形。如此的情形下,就全体数目而言,cis配置为优势,故在中子衍射中,由位点的存在机率得知为cis配置的结果。
本实施方式的多晶介电体薄膜是和磊晶膜不同种类的薄膜。在此,以特定基板制作钙钛矿型氮氧化物是SraTabOoNn的磊晶膜时,N取trans配置。
为了确认本实施方式的多晶介电体薄膜不是磊晶膜,测出钙钛矿型氮氧化物是SrTaO2N的磊晶膜的XRD数据,和本实施方式的多晶介电体薄膜的XRD数据比较,确认并非共同峰即可。又,图4是钙钛矿型氮氧化物是CaTaO2N的磊晶膜的XRD数据。和图4一样准备SrTaO2N的磊晶膜的XRD数据即可。又,薄膜为多晶膜的情况可由XRD数据有峰且来自其峰的结晶面并非只是特定的结晶面来确认。
多晶介电体薄膜13是多晶膜的一种,也是介电体薄膜的一种。多晶介电体薄膜13的厚度无特殊限制,优选为10nm~1μm。
薄膜电容器1的制造方法
其次,针对薄膜电容器1的制造方法说明。以下针对A位点原子为Sr、B位点原子为Ta的情形说明,但使用其他种类的原子的情形亦同。
最终成为多晶介电体薄膜13的薄膜的成膜方法无特殊限制。例如,可例示真空蒸镀法、溅镀法、PLD法(脉冲激光蒸镀法)、MO-CVD(有机金属化学气相沉积法)、MOD(有机金属分解法)、溶胶凝胶法、CSD(化学溶液沉积法)等。又,成膜时使用的原料中有时会含有少量的杂质、副成分,但若是未大幅损及薄膜性能的程度的量,则无特别问题。又,本实施方式的多晶介电体薄膜13也可在无大幅损及性能的程度下含有少量杂质、副成分。
上述成膜方法中,若以PLD法、溅镀法及CSD法等方法成膜,则最终获得的薄膜容易成为多晶膜。又,针对本实施方式的多晶介电体薄膜13,若以PLD法、溅镀法及CSD法等方法成膜,容易成为N取cis配置的结构。也可利用CVD法合成,但是因为成分元素数多,PLD法、溅镀法的组成控制性较高。在本实施方式中,针对利用PLD法进行的成膜方法说明。
首先,准备单晶硅基板作为基板11。然后,在单晶硅基板上按SiO2、TiOx、Pt顺序成膜,并形成由Pt构成的下部电极12。形成下部电极12的方法无特殊限制。例如可列举溅镀法、CVD等。
然后,在下部电极12上以PLD法形成金属氧化物薄膜。又,为了使下部电极12的一部分露出,使用金属掩模形成有部分未形成薄膜的区域。
PLD法中,首先将含有作为目的的多晶介电体薄膜的构成元素的靶材设置于成膜室内。然后,在靶材的表面上照射脉冲激光。利用脉冲激光的强能量,使靶材表面瞬间蒸发。并且,使蒸发物沉积在以面向靶材的方式配置的基板上而成为金属氧化物薄膜。
靶材的种类无特殊限制,除了含有制作的多晶介电体薄膜的构成元素的金属氧化物烧结体以外,还可使用合金、氮化物烧结体、金属氮氧化物烧结体等。又,在靶材中,优选各元素平均分布,但是在不影响获得的多晶介电体薄膜的质量的范围内,分布也可以有不均匀。再者,靶材不一定是1个,也可以准备多个含有多晶介电体薄膜的构成元素的一部分的靶材用于成膜。靶材形状亦无限制,制成适合使用的成膜装置的形状即可。例如,可通过调整成膜条件(氧气压力、氮气压力、成膜室的大小及气体导入管的位置等),以控制最终获得的多晶介电体薄膜的a/b。例如靶材的a/b若大,则可增大所成的膜中的a/b。又,不只是靶材a/b,成膜条件亦重要。原因在于,因为脉冲激光而从靶材蒸发的金属元素会受到构成成膜室中的气体环境的元素的影响,并到达基板的成膜面。
例如,当最终获得的多晶介电体薄膜的组成为SraTabOoNn时,则准备含Sr2Ta2O7的烧结体作为靶材。然后,通过调整成膜条件(例如氧气压力、氮气压力、成膜室的大小及气体导入管的位置等),可控制最终获得的多晶介电体薄膜的a/b。
又,PLD法的情形中,为了使成膜的金属氧化物薄膜结晶化,优选在成膜时将基板11以红外线激光加热。基板11的加热温度依金属氧化物薄膜及基板11的构成元素及组成等而改变,例如以成为600~800℃的方式加热并进行成膜。通过使基板11的温度为适温,金属氮氧化物薄膜容易结晶化,同时,可防止冷却时产生的裂痕的发生。
在成膜中,通过导入氮自由基并进行氮化处理,可获得由钙钛矿型氮氧化物构成的多晶介电体薄膜13。
最后,通过在多晶介电体薄膜13上形成上部电极14,可制造薄膜电容器1。又,上部电极14的材质无特殊限制,可使用Ag、Au、Cu等。又,上部电极14的形成方法亦无特殊限制。例如可以利用溅镀法形成。
以上已针对本发明的实施方式说明,但本发明不受如此的实施方式的任何限定,在不脱离本发明要旨的范围内当然能以各种不同的方式实施。
又,本发明的电容元件是利用介电性的元件,包括电容器(condenser)、热阻器、滤波器、双工器、共振器、发信器、天线、压电元件、晶体管、强介电体内存等。本实施方式的多晶介电体薄膜适合使用于特别要求介电损失小的电容元件。
[实施例]
以下针对本发明进一步基于详细的实施例说明,但本发明不限于此等实施例。
实验例1
首先,准备SrCO3粉末及Ta2O5粉末作为当作成膜用靶材使用的Sr2Ta2O7烧结体的原料。称量SrCO3粉末及Ta2O5粉末,使Sr/Ta的摩尔比成为1。
然后,对于SrCO3粉末及Ta2O5粉末,以使用乙醇溶剂的湿式球磨机混合16小时,获得混合浆料。
然后,将前述混合浆料以恒温干燥机于80℃进行12小时干燥,获得混合物。
然后,将前述混合物以乳钵轻轻地粉碎,放入陶瓷制的坩埚。然后使用电炉,于大气环境中于1000℃进行2小时热处理,获得预烧物。
然后对于前述预烧物,再次以使用乙醇溶剂的湿式球磨机混合16小时,获得预烧后浆料。
将获得的预烧后浆料于恒温干燥机于80℃干燥12小时,获得预烧后混合物。
对于前述预烧后混合物,添加聚乙烯醇溶液作为黏结剂,混合并获得造粒物。聚乙烯醇溶液的添加量相对于粉碎物100重量%为0.6重量%。
将前述造粒物成形为直径约23mm、高度约9mm的圆柱形状,获得成形物。成形方法为CIP成形。
对于前述成形物,使用电炉于大气环境中于1400℃煅烧2小时,获得烧结物。进一步,将前述烧结物的顶面及底面进行镜面研磨,获得高度5mm的成膜靶材。又,确认获得的成膜靶材的相对密度为96~98%。
将依上述方式获得的成膜用靶材设置于成膜装置,并设置硅基板成为面向成膜用靶材。该硅基板是使用在表面具有Pt膜作为下部电极的硅基板。
实验例1中,以PLD法成膜为厚200nm。通过调整此时的成膜条件(氧气压力、氮气压力等)以控制最终获得的多晶介电体薄膜的a/b。在成膜中,通过导入氮自由基并进行氮化处理,以获得多晶介电体薄膜。又,成膜时所耗费时间为0.5~2小时。
使用理学公司制全自动水平型多目的X射线衍射装置SmartLab测定实验例1获得的薄膜样本的XRD图。确认实验例1的实施例皆非磊晶膜。又,使用LECO公司制TC600利用脉冲加热熔融萃取法(红外线吸收法)对所获得的薄膜样本的o及n进行定量。又,由XPS的化学偏移判定Sr离子及Ta离子的价数,并确认价数和原料一样。具体而言,Sr离子的价数为2,Ta离子的价数为5。又,a/b的值及n的值是利用由脉冲加热熔融萃取法定量的值算出。
又,从针对实验例1获得的薄膜样本的XRD图中,确认了实验例1的实施例皆为多晶膜。即,确认了薄膜结晶化且成为多晶薄膜。又,确认了获得的多晶薄膜并非对特定面取向的取向膜。其成为cis配置是稳定的状态。又,图3A未图示Ta-N链,但ABO2N的cis型结构中,Ta-N链连成曲曲折折状。
然后,在实验例1获得的薄膜样本上使用蒸镀形成Ag电极,并测定介电损失(tanδ)。
介电损失的测定是利用阻抗分析仪(安捷伦科技公司制)4294A,以测定电压100mV、测定频率1MHz进行。本实验例中,tanδ为10%以下时评为良好。结果示于表1。
[表1]
A位点 | B位点 | a/b | n | tanδ(%) | |
比较例1 | Sr | Ta | 0.7 | 0.8 | 40 |
比较例2 | Sr | Ta | 0.9 | 0.8 | 16 |
实施例1 | Sr | Ta | 1.1 | 0.8 | 1 |
依据表1,a/b大于1的实施例1,介电损失为1%以下。相对于此,a/b为1以下的比较例1、2,介电损失超过1%。
依据表1,a/b越高,则tanδ越接近0%。此是ABO2N特有的现象。依理论计算,推测当出现阴离子缺陷时,容易通过A位点成为缺陷而补偿。但A位点若成为缺陷,据认为介电性降低,tanδ上升。而据认为通过提高a/b,含有比起化学计量(a/b=1)更多的A位点元素,则不易发生A位点缺陷,可减小tanδ。
实验例2
将SrCO3粉末及Ta2O5粉末替换为使用La2O3粉末及TiO2粉末,除此以外和实验例1同样进行,制作实施例11及比较例11的薄膜样本,并进行各种测定。进一步,使用BaO粉末及Ta2O5粉末,除此以外,和实验例1同样进行,制作实施例12及比较例12的薄膜样本,并进行各种测定。进一步,使用Nd2O3粉末及TiO2粉末,除此以外,和实验例1同样进行,制作实施例13及比较例13的薄膜样本,并进行各种测定。结果示于表2。又,针对实验例2获得的实施例的薄膜样本进行XRD测定。依照XRD测定,确认了实施例2的实施例及比较例也皆非磊晶膜而是多晶薄膜。进而,确认了N的配置为cis型。又,关于实施例11及比较例11,从XPS的化学偏移判定La离子及Ti离子的价数,并确认了价数和原料一样。具体而言,La离子的价数为3,Ti离子的价数为4。关于实施例12及比较例12,从XPS的化学偏移判定Ba离子及Ta离子的价数,并确认了价数和原料一样。具体而言,Ba离子的价数为2,Ta离子的价数为5。进而,关于实施例13及比较例13,从XPS的化学偏移判定Nd离子及Ti离子的价数,并确认了价数和原料一样。具体而言,Nd离子的价数为3,Ti离子的价数为4。
[表2]
A位点 | B位点 | a/b | n | tanδ(%) | |
比较例11 | La | Ti | 0.90 | 0.9 | 50 |
实施例11 | La | Ti | 1.25 | 0.9 | 1 |
比较例12 | Ba | Ta | 0.80 | 1.0 | 48 |
实施例12 | Ba | Ta | 1.30 | 1.0 | 5 |
比较例13 | Nd | Ti | 0.90 | 0.8 | 53 |
实施例13 | Nd | Ti | 1.20 | 0.8 | 9 |
依表2,a/b比1大的实施例11,介电损失为1%以下。反观a/b为1以下的比较例11,介电损失超过1%。
实验例3
针对实施例1(n=0.8),使n值变化,获得实施例21及比较例21、22。结果示于表3。
[表3]
A位点 | B位点 | a/b | n | tanδ(%) | |
比较例21 | Sr | Ta | 1.1 | 0.5 | 40 |
比较例22 | Sr | Ta | 1.1 | 0.6 | 18 |
实施例21 | Sr | Ta | 1.1 | 0.7 | 4 |
实施例1 | Sr | Ta | 1.1 | 0.8 | 1 |
依表3,n≥0.7的实施例,tanδ为10%以下,成为介电损失优良的多晶介电体薄膜。反观n<0.7的比较例21、22,tanδ超过10%,是恶化的。
推测n<0.7时,不会充分地构成Ta-N链相连成曲曲折折状的结构,故tanδ恶化。
【符号说明】
1 薄膜电容器
11 基板
12 下部电极
13 多晶介电体薄膜
14 上部电极
Claims (4)
1.一种多晶介电体薄膜,其主要组成是钙钛矿型氮氧化物,其特征为:
该钙钛矿型氮氧化物以组成式AaBbOoNn表示,其中,
a+b+o+n=5,
a/b>1,且
n≥0.7。
2.如权利要求1所述的多晶介电体薄膜,其中,
所述A是选自Sr、Ba、Ca、La、Ce、Pr、Nd、Na中的1种以上的元素,且
所述B是选自Ta、Nb、Ti、W中的1种以上的元素。
3.如权利要求1或2所述的多晶介电体薄膜,其中,
所述多晶介电体薄膜具有BO4N2的八面体结构,且所述八面体结构中的N的配置为cis型。
4.一种电容元件,其具有如权利要求1~3中任一项所述的多晶介电体薄膜。
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EP3392889A1 (en) | 2018-10-24 |
JPWO2017135294A1 (ja) | 2018-11-29 |
US10611693B2 (en) | 2020-04-07 |
TW201930182A (zh) | 2019-08-01 |
CN108475580B (zh) | 2020-06-02 |
TWI692438B (zh) | 2020-05-01 |
JP6866852B2 (ja) | 2021-04-28 |
TW201728528A (zh) | 2017-08-16 |
EP3392889A4 (en) | 2019-08-14 |
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