JP6570688B2 - 分子クラスタ化合物からの金属酸化物ナノ粒子の合成 - Google Patents
分子クラスタ化合物からの金属酸化物ナノ粒子の合成 Download PDFInfo
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- JP6570688B2 JP6570688B2 JP2018055987A JP2018055987A JP6570688B2 JP 6570688 B2 JP6570688 B2 JP 6570688B2 JP 2018055987 A JP2018055987 A JP 2018055987A JP 2018055987 A JP2018055987 A JP 2018055987A JP 6570688 B2 JP6570688 B2 JP 6570688B2
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- 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
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02565—Oxide semiconducting materials not being Group 12/16 materials, e.g. ternary compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G11/00—Compounds of cadmium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G13/00—Compounds of mercury
- C01G13/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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Description
本発明の方法は、IIB族金属酸化物ナノ粒子:ZnO、CdO及びHgO、それらのドープされた種及び合金種の合成を述べるものである。ある実施形態では、金属酸化物(M1O)ナノ粒子は、II−VIクラスタの存在下で成長し、ここで、II=M1であり、VI=Oである。本明細書で使用されているように、II=M1なる表現は、分子クラスタに含まれるMが、酸化物MOに含まれているものと同じMであることを意味している。非限定的な例では、ZnOナノ粒子は、ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)(diaquabis[2-(methoximino)propanato]zinc(II))、[Zn(OC(O)C(Me)N(OMe))2]・2H2Oのような、亜鉛と酸素を含むクラスタ化合物の存在下で成長する。
好ましい実施形態では、予め作製されたクラスタ化合物が高沸点溶媒と混合される。別の好ましい実施形態では、適切な前駆体が溶媒に加えられて、インサイチューで分子クラスタが形成される。反応溶液が非配位性である場合には、キャッピング剤が反応溶液に加えられる。幾つかの実施形態では、更なる金属前駆体及び酸化物前駆体が、別個の前駆体又は単一源の前駆体の何れかの形態として加えられる。金属及び酸化物前駆体に対する分子クラスタ材料のモル比は、適切な任意なものであってよい。好ましくは、モル比は、1:0(つまり、金属及び酸化物前駆体が存在しない)乃至1:10,000の範囲、より好ましくは1:0乃至1:1,000の範囲、最も好ましくは1:0乃至1:250の範囲にある。随意選択的に、活性化剤が反応溶液に加えられて、クラスタの分解温度が下げられる。
調整方法は、II−VI分子クラスタ化合物の存在下でIIB族金属酸化物ナノ粒子を成長させることを含む。適切な分子クラスタ化合物の例とそれらの合成については、米国特許第7,803,423号に記載されており、当該特許の内容の全体は、引用を以て本明細書の一部となる。
IIB族金属(M)前駆体は、有機金属化合物、無機塩、配位化合物、又は元素源を含んでよいが、これらに限定されない。例としては、ZnEt2、CdMe2、HgMe2などの式MR2(R=アルキル又はアリール)である有機金属化合物、フッ化物、塩化物、臭化物、ヨウ化物、硝酸塩(M(NO3)2のような無機塩、アセチルアセトン(M(CH3C(O)CHC(O)CH3)2)、シュウ酸塩(MC2O4)、水酸化物(MG(OH)2)、メトキシ(M(OCH3)2、ステアレート(M(CH3(CH2)15CH2CO2)2)等の脂肪酸のような配位化合物、Zn、Cd、Hgのような元素源がある。
金属前駆体が酸素源としても働く場合(例えば、金属前駆体がステアリン酸金属のような脂肪酸である場合)、酸素を含む更なる前駆体は必要とされないだろう。IIB族金属前駆体が酸素を含んでいない場合、金属前駆体が酸素前駆体と共に加えられてよい。酸素前駆体としては、過酸化物、塩基、無機塩、配位化合物、アルコール、又は酸素元素がこれらに限定されない。より具体的例には、H2O2のような過酸化物、NaOH等の水酸化物のような塩基、Na2Oのような無機塩、NO2のような配位化合物、第一級アルコール、第二級アルコール又は第三級アルコールのようなアルコールがある。
適切な溶媒には、ホスフィン(例えばTOP)、ホスフィンオキシド(例えばTOPO)又はアミン(例えばHDA)のようなルイス塩基型の配位性溶媒、或いは、アルカン、アルケン(例えば1−オクタデセン)、又は伝熱流体(例えばサーミノール(登録商標)66)のような非配位性有機溶媒がある。
随意選択的に、QD合成は活性化剤の存在下で進行して、分子クラスタ化合物の分解温度が下げられて、より低温でナノ粒子成長が促進される。当業者に知られた任意の活性化剤が使用されてよく、オクタノールのようなアルコール、HDAやオクチルアミンのようなアミンなどがあるが、これらに限定されない。好ましい実施形態では、活性化剤はHDAである。
この亜鉛クラスタを、ほぼ米国特許第7,588,828号に記載されたようにして調製した。当該特許は、引用を以て本明細書の一部となる。ピルビン酸ナトリウム(6.8g、62mmol)とメトキシルアミン塩酸塩(5.12g、61mmol)とを50mLの水に混合し、白色の濁った懸濁液を形成した。炭酸ナトリウム(3.2g、30mmol)を少しずつ加えると、ガスが放出した。ガスの放出が終わると、澄んだ溶液が残った。硝酸亜鉛六水和物(4.46g、15mmol)を加えて、溶液を24時間撹拌した。なお、最初の7時間については、溶液は5℃で冷たく維持された。遠心分離によって白い固体を収集し、アセトンで洗浄し、真空乾燥機で一晩乾燥させた。収量:1.12g。
HDA(10g、41mmol)を真空下で120℃で脱ガスした。ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)クラスタ(100mg、0.30mmol)を加えると、直ちに溶解して、澄んだ溶液が形成された。150℃に昇温して、30分間維持した。200℃に昇温して、30分間維持した後、溶液を室温に冷ました。白い固体の生成物を、メタノールで析出して、遠心分離で単離した。UVabsは、約355nmであり、PLmax=370nmであった(図1)。透過型電子顕微鏡(TEM、図2)像は、直径が<10nmである擬球形の粒子を示しており、それらは、量子ドット形態のナノ粒子に合致している。
HDA(7g、29mmol)及びTOPO(3g、7.8mmol)を真空下で1時間、110℃で脱ガスした。ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)クラスタ(100mg、0.30mmol)を加えて、溶液を200℃に加熱した。35分後、温度を75℃に下げて、溶液を2時間半アニールして、その後、一晩で室温に冷却した。溶液を80℃に再加熱し、酢酸亜鉛(II)(100mg、0.55mmol)を加えた。180℃に昇温して、30分間維持した。1−オクタノールの1−オクタデセン溶液(3.05M、2mL、6.1mmol)をゆっくり注入した。その添加を完了すると、温度を30分間維持し、その後、溶液を室温に冷ました。白い固体の生成物を、メタノールで析出して、遠心分離で単離した。UVabsは、約335nmであった(図3)。
HDA(7g、29mmol)及びTOPO(3g、7.8mmol)を真空下で30分間、110℃で脱ガスした。70℃で、ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)クラスタ(200mg、0.60mmol)及び酢酸亜鉛(II)(200mg、1.1mmol)を加えて、引き続き、溶液を20分間で200℃に加熱した。1−オクタノール(1.7mL、13mmol)を液滴で、1分間を超えて注入した。添加が完了すると、温度を40分間維持し、その後、溶液を70℃に冷ました。白色/黄色の固体の生成物を、メタノールで析出して、遠心分離で単離した。UVabsは、約338nmであった(図5)。X線回折(XRD)パターン(図5)は、紅亜鉛鉱相ZnOナノ粒子と合致している。注意:低角(2θ<30°)反射は、キャッピング剤に対応している。
HDA(7g、29mmol)及びTOPO(3g、7.8mmol)を真空下で30分間、110℃で脱ガスした。70℃で、ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)クラスタを加えて、引き続いて、20分間で溶液を200℃に加熱した。温度を40分間維持し、その後、溶液を70℃に冷ました。白い固体の生成物を、メタノールで析出して、遠心分離で単離した。UVabsは、約335nmであった(図6)。
Claims (12)
- IIB族金属酸化物結晶コアと、
IIB族金属オキシマト分子クラスタ化合物と、
を含んでおり、
IIB族金属酸化物結晶コアは、IIB族金属オキシマト分子クラスタ化合物に配置されている、ナノ粒子。 - IIB族金属酸化物結晶コアに配置された半導体材料の1又は複数の層を更に含む、請求項1に記載のナノ粒子。
- 半導体材料は、MgS、MgSe、MgTe、CaS、CaSe、CaTe、SrS、SrSe、SrTe、ZnO、ZnS、ZnSe、ZnTe、CdO、CdS、CdSe、CdTe、HgO、HgS、HgSe、HgTe、Zn3N2、Zn3P2、Zn3As2、Cd3N2、Cd3P2、Cd3As2、BN、BP、AlN、AlP、AlAs、AlSb、GaN、GaP、GaAs、GaSb、InN、InP、InAs、InSb、B4C、Al4C3、Ga4C、Al2S3、Al2Se3、Al2Te3、Ga2S3、Ga2Se3、Ga2Te3、In2S3、In2Se3、In2Te3、PbS、PbSe、PbTe、SnS、SnSe、SnTe、NiS、CrS、CuInS2、CuInSe2、AgInS2、又はそれらのドープされた材料からなる群から選択される、請求項2に記載のナノ粒子。
- キャッピングリガンドを含む最外層を更に含んでおり、当該キャッピングリガンドは、ホスフィン、ホスフィンオキシド、アルキルホスホン酸、アルキルアミン、アリールアミン、ピリジン、チオール、長鎖脂肪酸及びチオフェンからなる群から選択される、請求項1に記載のナノ粒子。
- 溶媒と、
複数のナノ粒子と、
を含んでおり、当該複数のナノ粒子の各々は、
IIB族金属酸化物結晶コアと、
IIB族金属オキシマト分子クラスタ化合物と、
を含んでおり、
IIB族金属酸化物結晶コアは、IIB族金属オキシマト分子クラスタ化合物上に配置されている、インク組成物。 - IIB族金属オキシマト分子クラスタ化合物のIIB族金属とIIB族金属酸化物結晶コアのIIB族金属は、同じである、請求項5に記載のインク組成物。
- IIB族金属オキシマト分子クラスタ化合物のIIB族金属は、IIB族金属酸化物結晶コアのIIB族金属と同じではない、請求項5に記載のインク組成物。
- ホスフィン、ホスフィンオキシド、アルキルホスホン酸、アルキルアミン、アリールアミン、ピリジン、チオール、長鎖脂肪酸及びチオフェンからなる群から選択されるキャッピングリガンドからなる最外層を更に含む、請求項5に記載のインク組成物。
- IIB族金属オキシマト分子クラスタ化合物は、亜鉛オキシマト分子クラスタ化合物である、請求項5に記載のインク組成物。
- 亜鉛オキシマト分子クラスタ化合物は、ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)である、請求項9に記載のインク組成物。
- IIB族金属オキシマト分子クラスタ化合物は、亜鉛オキシマト分子クラスタ化合物である、請求項1に記載のナノ粒子。
- 亜鉛オキシマト分子クラスタ化合物は、ジアクアビス[2−(メトキシイミノ)プロパナト]亜鉛(II)である、請求項11に記載のナノ粒子。
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KR20220003356A (ko) | 2020-07-01 | 2022-01-10 | 삼성전자주식회사 | 발광 소자 및 이를 포함하는 표시 장치 |
KR20220022517A (ko) * | 2020-08-18 | 2022-02-28 | 삼성디스플레이 주식회사 | 반도체 나노입자 및 이를 포함한 전자 장치 |
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CN1894799A (zh) | 2003-09-05 | 2007-01-10 | 点度量技术有限公司 | 具有纳米级外延过生长的量子点光电器件以及制造方法 |
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JP5388099B2 (ja) * | 2007-12-28 | 2014-01-15 | 国立大学法人大阪大学 | コアシェル型量子ドット蛍光微粒子 |
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US20120251450A1 (en) | 2011-04-04 | 2012-10-04 | Alex Punnoose | Nanoparticles that preferentially associate with and kill diseased cells for diagnostic and therapeutic applications |
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JP6313860B2 (ja) | 2018-04-18 |
EP3044287A1 (en) | 2016-07-20 |
TW201641428A (zh) | 2016-12-01 |
CN108751248B (zh) | 2021-02-26 |
TW201514101A (zh) | 2015-04-16 |
TWI655156B (zh) | 2019-04-01 |
KR101788241B1 (ko) | 2017-10-19 |
WO2015036762A1 (en) | 2015-03-19 |
US20150076494A1 (en) | 2015-03-19 |
CN105705611B (zh) | 2018-06-29 |
CN108751248A (zh) | 2018-11-06 |
EP3044287B1 (en) | 2018-09-12 |
TWI557076B (zh) | 2016-11-11 |
KR20170117619A (ko) | 2017-10-23 |
KR101883891B1 (ko) | 2018-08-30 |
CN105705611A (zh) | 2016-06-22 |
TWI661993B (zh) | 2019-06-11 |
JP2018135266A (ja) | 2018-08-30 |
KR20160055237A (ko) | 2016-05-17 |
TW201827344A (zh) | 2018-08-01 |
JP2016539908A (ja) | 2016-12-22 |
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