JP6810534B2 - ナノ粒子組成物およびその製法並びに使用法 - Google Patents
ナノ粒子組成物およびその製法並びに使用法 Download PDFInfo
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- JP6810534B2 JP6810534B2 JP2016083675A JP2016083675A JP6810534B2 JP 6810534 B2 JP6810534 B2 JP 6810534B2 JP 2016083675 A JP2016083675 A JP 2016083675A JP 2016083675 A JP2016083675 A JP 2016083675A JP 6810534 B2 JP6810534 B2 JP 6810534B2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
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- OGBUMNBNEWYMNJ-UHFFFAOYSA-N batilol Chemical class CCCCCCCCCCCCCCCCCCOCC(O)CO OGBUMNBNEWYMNJ-UHFFFAOYSA-N 0.000 description 6
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Chemical class CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
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Description
本件特許出願は、2006年1月12日付で出願された、米国仮特許出願第60/758,307号に基く優先権を請求するものである。
本件特許出願の趣旨達成に係る努力は、部分的にザナショナルサイエンスファウンデーション(The National Science Foundation)からの承諾(NSF/DMI 0115532)によって支援されたものであった。該政府は、本件特許出願から発生するあらゆる特許において、幾分かの権利を持つことができる。
長年に渡り、潤滑剤、被覆、または送出メカニズム(delivery mechanism)として使用できる、ナノ粒子の開発のために、かなりの努力がはらわれてきた。ナノ粒子組成物を改善する新たな方法、その製造方法、並びにその使用法が、探し求められている。
一局面においては、組成物が記載され、該組成物は、固体潤滑剤ナノ粒子および有機媒体を含有する。
あらゆる態様を詳細に説明する前に、本発明は、その応用において、以下の説明において示される、あるいは以下の図面において例示される成分、部材の構成および配列の詳細に限定されるものではないことを理解すべきである。本発明では、その他の態様も可能であり、また本発明は、様々な方法で実施し、あるいは実行することができる。また、本明細書で使用する語法並びに述語は、説明のためのものであり、本発明の限定を意味するものではないと理解すべきである。
実施例1:
ボールミル微粉砕を、焼入れステンレススチール製バイアルおよびボールを用いて、スペックス(SUPEX) 8000D装置内で行った。MoS2(アルファエーサー(Alfa Aesar)製、純度:98%;平均粒径:700nm)およびカノーラオイル(クリスコ(Crisco)製)を、1部のMoS2(10g)対2部(20g)のカノーラオイルなる比で、出発物質として使用した。ボール対粉末比は、2:1であった。換言すれば、該容器内のボールの質量は、2質量%であり、また該MoS2サンプルの質量は、1質量%であった。MoS2は、空気中で48時間ボールミル微粉砕処理し、次いでカノーラオイル中で、室温にて48時間、微粉砕処理した。得られたナノ粒子は、ボールミル微粉砕処理後、約50nmなる粒径のものであった。以下の表1に、微粉砕処理条件および得られた粒子の形態をまとめた。該ボールミル微粉砕されたナノ粒子の形状に及ぼす、微粉砕用媒体の強力な効果の存在が観測された。乾式微粉砕は、該粒子サイズが、ミクロンサイズからナノメータサイズに減じられた際に、面の挫屈および折畳みを示した。しかし、ここで使用した該乾式微粉砕条件は、数個のナノ粒子を埋設した微細クラスタを生成した。他方で、湿式微粉砕は、挫屈を示さなかったが、解凝集を示した。
予言的実施例:
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1.固体潤滑剤ナノ粒子と;
有機媒体と、
を含むことを特徴とする、組成物。
2.前記固体潤滑剤ナノ粒子が、ボールミルで微粉砕されたナノ粒子、化学機械的に微粉砕されたナノ粒子、またはこれらの組合せを含む、前記1記載の組成物。
3.前記組成物が、ナノ粒子を主成分とする潤滑剤である、前記1記載の組成物。
4.前記有機媒体が、オイル系媒体、グリース系媒体、アルコール系媒体、またはこれらの組み合わせを含む、前記1記載の組成物。
5.前記有機媒体が、複合オイル、カノーラオイル、植物油、大豆油、コーン油、菜種油のエチルおよびメチルエステル、蒸留モノグリセライド、モノグリセライド、ジグリセライド、モノグリセライドの酢酸エステル、モノグリセライドの有機酸エステル、ソルビタン、脂肪酸のソルビタンエステル、脂肪酸のプロピレングリコールエステル、脂肪酸のポリグリセロールエステル、炭化水素油、n-ヘキサデカン、リン脂質、またはこれらの組合せを含む、前記1記載の組成物。
6.前記有機媒体が、複合油を含む、前記1記載の組成物。
7.前記ナノ粒子が、モリブデンジスルフィド、タングステンジスルフィド、グラファイト、ポリテトラフルオロエチレン、フッ化セリウム、酸化亜鉛、窒化ホウ素、六方晶系窒化ホウ素、硫酸銀、ヨウ化カドミウム、ヨウ化鉛、フッ化バリウム、硫化錫、リン酸亜鉛、銀、鉛、ニッケル、硫化亜鉛、マイカ、硝酸ホウ素、ホウ砂、フッ化炭素、挿入グラファイト、リン化亜鉛、銅、ホウ素、またはこれらの組合せを含む、前記1記載の組成物。
8.更に、ミクロンサイズの粒子をも含む、前記1記載の組成物。
9.更に、乳化剤をも含む、前記1記載の組成物。
10.前記乳化剤が、約2〜約7なる範囲の親水-親油バランス値を持つ、前記9記載の組成物。
12.更に、基剤をも含む、前記1記載の組成物。
13.前記基剤が、オイル、グリース、スプレイ、プラスチック、ゲル、またはこれらの組合せを含む、前記12記載の組成物。
14.前記基剤が、炭化水素油、植物油、コーン油、ピーナッツ油、カノーラオイル、大豆油、鉱油、パラフィンオイル、合成油、石油ゲル、石油グリース、炭化水素ゲル、炭化水素グリース、リチウムを主成分とするグリース、フルオロエーテルを主成分とするグリース、エチレンビステアラミド、ワックス、シリコーン、またはこれらの組合せを含む、前記12記載の組成物。
15.質量基準で、約1部またはそれ未満の乳化剤に対して、約1部の有機媒体を有する、前記1記載の組成物。
16.質量基準で、約0.4部またはそれ未満の乳化剤に対して、約1部の有機媒体を有する、前記1記載の組成物。
17.約3部の有機媒体に対して、約1部の固体潤滑剤ナノ粒子を有する、前記1記載の組成物。
18.約4部の有機媒体に対して、約1部の固体潤滑剤ナノ粒子を有する、前記1記載の組成物。
19.約8部の有機媒体に対して、約3部の固体潤滑剤ナノ粒子を有する、前記1記載の組成物。
20.約4部の有機媒体に対して、約2部の固体潤滑剤ナノ粒子を有する、前記1記載の組成物。
22.前記固体潤滑剤ナノ粒子が、閉鎖型構成体を含む、前記1記載の組成物。
23.前記固体潤滑剤ナノ粒子が、開放型構成体を含む、前記1記載の組成物。
24.最終用途の部品としての対象を、前記1記載の組成物で潤滑処理または被覆する工程を含むことを特徴とする、該対象を潤滑処理または被覆する方法。
25.前記対象が、境界潤滑レジームを含む、前記24記載の方法。
26.前記方法を、機械的用途、製造用途、鉱業的用途、航空宇宙産業用途、および自動車産業用途を含む用途において使用する、前記24記載の方法。
27.前記方法を、薬学的用途、医学的用途、歯科学的用途、化粧学的用途、食物製品用途、栄養学的用途、健康関連用途、バイオ-燃料用途、およびこれらの組合せを含む用途において利用する、前記24記載の方法。
28.前記対象が、機械器具、軸受、ギア、カムシャフト、ポンプ、トランスミッション、ピストンリング、エンジン、発電機、ピン-ジョイント、航空宇宙学的システム、採掘装置、製造装置、無機-有機資材、またはこれらの組合せを含む、前記24記載の方法。
29.前記組成物を、潤滑剤、グリース、ゲル、スプレイ、配合プラスチック部品、ペースト、粉末、エマルション、分散物、またはこれらの組合せに添加する、前記24記載の方法。
30.前記対象の潤滑処理が、固体潤滑剤ナノ粒子および有機媒体を含む前記組成物を、送出メカニズムとして使用することを含む、前記24記載の方法。
32.前記方法を、無機-有機資材用途を包含する用途において利用する、前記30記載の方法。
33.前記無機-有機資材用途が光学、エレクトロニクス、イオニックス、メカニックス、エネルギー、環境、生物学、医薬、知能膜、分離デバイス、機能性知能被膜、光起電力電池および燃料電池、光触媒、ニュー触媒、センサ、知能マイクロエレクトロニクス、マイクロ-オプティカルおよびフォトニック部品およびナノフォトニックス用のシステム、革新的化粧料、活性分子のターゲティング、撮像、これを用いた治療、およびその制御放出を組合わせた、インテリジェント治療媒介体、および自動車または包装産業用の、ナノセラミック-ポリマー複合体を包含する、前記32記載の方法。
34.層状に形成された材料を含むことを特徴とする、ナノ粒子。
35.前記層状に形成された材料が、カルコゲナイドを含む、前記34記載の組成物。
36.前記層状に形成された材料が、モリブデンジスルフィド、タングステンジスルフィド、グラファイト、挿入グラファイト、またはこれらの組合せを含む、前記34記載の組成物。
37.更に、ポリテトラフルオロエチレン、窒化ホウ素、六方晶系窒化ホウ素、またはこれらの組合せをも含む、前記34記載の組成物。
38.更に、軟質金属、銀、鉛、ニッケル、銅、フッ化セリウム、酸化亜鉛、硫酸銀、ヨウ化カドミウム、ヨウ化鉛、フッ化バリウム、硫化錫、リン酸亜鉛、硫化亜鉛、マイカ、硝酸ホウ素、ホウ砂、フッ素化炭素、リン化亜鉛、ホウ素、またはこれらの組合せをも含む、前記37記載の組成物。
39.層状に形成された材料を、微粉砕する工程を含むことを特徴とする、ナノ粒子の製造方法。
40.前記微粉砕工程が、ボールミル微粉砕、化学機械的微粉砕、またはこれらの組合せを含む、前記39記載の方法。
42.前記粒子が、約100nmまたはそれ未満の平均サイズにまで微粉砕される、前記39記載の方法。
43.前記層状に形成された材料が、カルコゲナイドを含む、前記39記載の方法。
44.前記層状に形成された材料が、モリブデンジスルフィド、タングステンジスルフィド、グラファイト、挿入グラファイト、またはこれらの組合せを含む、前記39記載の方法。
45.更に、ポリテトラフルオロエチレン、窒化ホウ素、六方晶系窒化ホウ素、またはこれらの組合せと共に、前記層状に形成された材料を、微粉砕する工程を含む、前記39記載の方法。
46.更に、軟質金属、銀、鉛、ニッケル、銅、フッ化セリウム、酸化亜鉛、硫酸銀、ヨウ化カドミウム、ヨウ化鉛、フッ化バリウム、硫化錫、リン酸亜鉛、硫化亜鉛、マイカ、硝酸ホウ素、ホウ砂、フッ化炭素、リン化亜鉛、ホウ素、またはこれらの組合せと共に、前記層状に形成された材料を微粉砕する工程を含む、前記45記載の方法。
47.前記ボールミル微粉砕が、高エネルギーボールミル微粉砕、中エネルギーボールミル微粉砕、またはこれらの組合せを含む、前記40記載の方法。
48.前記ボールミル微粉砕が、前記層状に形成された材料を、真空中で、ガス中で、液体中で、第二の固体の存在下で、またはこれらの組合せで微粉砕する工程を含む、前記40記載の方法。
49.前記ボールミル微粉砕が、前記の層状に形成された材料を、空気中で、アルコール中で、オイル中で、またはこれらの組合せの下で微粉砕する工程を含む、前記48記載の方法。
50.前記ボールミル微粉砕が、第一ボールミル微粉砕、および少なくとも1回の、更なるその後のボールミル微粉砕処理を含む、前記40記載の方法。
52.前記ボールミル微粉砕が、空気中でのおよびその後の有機媒体中での微粉砕である、前記51記載の方法。
53.前記有機媒体が、アルコール、オイル、またはこれらの組合せを含む、前記52記載の方法。
54.前記有機媒体が、複合油、カノーラオイル、植物油、大豆油、コーン油、菜種油のエチルおよびメチルエステル、蒸留モノグリセライド、モノグリセライド、ジグリセライド、モノグリセライドの酢酸エステル、モノグリセライド有機酸エステル、ソルビタン、脂肪酸のソルビタンエステル、脂肪酸のプロピレングリコールエステル、脂肪酸のポリグリセロールエステル、炭化水素油、n-ヘキサデカン、またはこれらの組合せを含む、前記52記載の方法。
55.前記有機媒体が、複合油を含む、前記52記載の方法。
56.前記ボールミル微粉砕工程を約12〜約50時間に渡り行う、前記40記載の方法。
57.前記微粉砕工程が、酸化防止剤と共に、前記層状に形成された材料を微粉砕する工程を含む、前記39記載の方法。
58.前記微粉砕工程が、耐蝕性物質と共に、前記層状に形成された材料を微粉砕する工程を含む、前記39記載の方法。
59.前記酸化防止剤が、ヒンダードフェノール、アルキル化フェノール、アルキルアミン、アリールアミン、2,6-ジ-tert-ブチル-4-メチルフェノール、4,4'-ジ- tert-オクチルジフェニルアミン、tert-ブチルヒドロキノン、トリス(2,4-ジ-tert-ブチルフェニル)ホスフェート、ホスフィット、チオエステル、またはこれらの組合せを含む、前記57記載の方法。
60.前記耐蝕剤が、アルカリ土類金属ビスアルキルフェノールスルホネート、ジチオホスフェート、アルケニル琥珀酸半-アミド、またはこれらの組合せを含む、前記58記載の方法。
62.更に、ポリテトラフルオロエチレン、窒化ホウ素、六方晶系窒化ホウ素、またはこれらの組合せと共に、前記層状に形成された材料を、微粉砕する工程をも含む、前記61記載の方法。
63.更に、軟質金属、銀、鉛、ニッケル、銅、フッ化セリウム、酸化亜鉛、硫酸銀、ヨウ化カドミウム、ヨウ化鉛、フッ化バリウム、硫化錫、リン酸亜鉛、硫化亜鉛、マイカ、硝酸ホウ素、ホウ砂、フッ化炭素、リン化亜鉛、ホウ素、またはこれらの組合せと共に、前記層状に形成された材料を微粉砕する工程をも含む、前記62記載の方法。
64.前記基剤と乳化剤とを混合する、前記61記載の方法。
65.前記乳化剤を、前記ナノ粒子を添加する前に、前記基剤と混合する、前記64記載の方法。
66.前記混合処理が、超音波処理を含む、前記64記載の方法。
67.約0.5〜約2質量%なる範囲の量の前記ナノ粒子を、前記基剤中で超音波処理し、あるいはそこに分散させる、前記61記載の方法。
68.約0.25〜約5質量%なる範囲の量の前記ナノ粒子を、前記基剤中で超音波処理し、あるいはそこに分散させる、前記61記載の方法。
69.約0.75〜約2.25質量%なる範囲の量の前記乳化剤を、前記基剤中で超音波処理し、あるいはそこに分散させる、前記64記載の方法。
70.約0.5〜約10質量%なる範囲の量の前記乳化剤を、前記基剤中で超音波処理し、あるいはそこに分散させる、前記64記載の方法。
Claims (32)
- ナノ粒子組成物の製造方法であって、
(a)固体潤滑剤を乾式微粉砕して乾式微粉砕されたナノ粒子組成物を生成する工程であって、該ナノ粒子組成物が、500nm以下の平均粒径を有し、かつ層状材料であるナノ粒子を含む工程、及び、
(b)該ナノ粒子を、有機媒体が該ナノ粒子の少なくとも一部に挿入するまで、該有機媒体中で湿式微粉砕する工程
を含み、
該固体潤滑剤が、タングステンジスルフィド、グラファイト、窒化ホウ素、またはこれらの組合せである、製造方法。 - 有機媒体が、少なくとも1つのオイルを含む、請求項1に記載の製造方法。
- 少なくとも1つのオイルが、少なくとも1つの植物油を含む、請求項2に記載の製造方法。
- 少なくとも1つの植物油が、カノーラオイル、大豆油、コーン油、菜種油またはこれらの組合せの少なくとも1つを含む、請求項3に記載の製造方法。
- 更に、湿式微粉砕されたナノ粒子組成物を添加剤として基剤へ混ぜる工程を含み、
該基剤が有機媒体と異なるものである、請求項1〜4のいずれか1項に記載の製造方法。 - 基剤が、オイル、グリース、プラスチック、ワックス、シリコーン、またはこれらの組合せの少なくとも1つを含み、
該基剤が有機媒体と異なるものである、請求項5に記載の製造方法。 - 更に、乳化剤を基剤へ混ぜる工程を含む、請求項5又は6のいずれか1項に記載の製造方法。
- 乳化剤がリン脂質を含む、請求項7に記載の製造方法。
- 乳化剤がレシチンを含む、請求項8に記載の製造方法。
- 平均粒径が100nm以下である、請求項1〜9のいずれか1項に記載の製造方法。
- 乾式微粉砕又は湿式微粉砕がボールミル微粉砕及び/又は化学機械的微粉砕を含み、かつ、12〜50時間に渡り行われる、請求項1〜10のいずれか1項に記載の製造方法。
- ナノ粒子の少なくとも一部が有機媒体によりカプセル化又は被覆されるまで、ナノ粒子を湿式微粉砕する、請求項1〜11のいずれか1項に記載の製造方法。
- 500nm以下の平均粒径を有し、かつ層状材料である、複数のナノ粒子と、
有機媒体と、
酸化防止剤とを含み、
該有機媒体が該ナノ粒子に挿入しており、
該ナノ粒子が、タングステンジスルフィドナノ粒子、グラファイトナノ粒子、窒化ホウ素ナノ粒子、またはこれらの組合せである、組成物。 - 有機媒体が、少なくとも1つのオイルを含む、請求項13に記載の組成物。
- 少なくとも1つのオイルが、少なくとも1つの植物油を含む、請求項14に記載の組成物。
- 少なくとも1つの植物油が、カノーラオイル、大豆油、コーン油、菜種油またはこれらの組合せの少なくとも1つを含む、請求項15に記載の組成物。
- 更に基剤を含み、
該基剤が有機媒体と異なるものであり、
該有機媒体が挿入しているナノ粒子が、該基剤中に分散している、請求項13〜16のいずれか1項に記載の組成物。 - 基剤が、オイル、グリース、プラスチック、ワックス、シリコーン、またはこれらの組合せの少なくとも1つを含み、
該基剤が有機媒体と異なるものである、請求項17に記載の組成物。 - 組成物が、基剤中に分散された、該有機媒体が挿入しているナノ粒子を0.25〜5質量%含む、請求項17又は18に記載の組成物。
- 組成物が、基剤中に分散された、該有機媒体が挿入しているナノ粒子を0.5〜2質量%含む、請求項19に記載の組成物。
- 更に乳化剤を含む、請求項17〜20のいずれか1項に記載の組成物。
- 乳化剤がリン脂質を含む、請求項21に記載の組成物。
- 乳化剤がレシチンを含む、請求項22に記載の組成物。
- 0.5〜10質量%の乳化剤を含む、請求項21〜23のいずれか1項に記載の組成物。
- 0.75〜2.25質量%の乳化剤を含む、請求項24に記載の組成物。
- 平均粒径が100nm以下である、請求項13〜25のいずれか1項に記載の組成物。
- 酸化防止剤が、ヒンダードフェノール、アルキルアミン、アリールアミン、t-ブチルヒドロキノン、トリス(2,4-ジ-t-ブチルフェニル)ホスフェート、ホスフィット、チオエステルまたはこれらの組合せの少なくとも1つを含む、請求項13〜26のいずれか1項に記載の組成物。
- 更に錆止め剤を含む、請求項13〜27のいずれか1項に記載の組成物。
- 錆止め剤が、アルカリ土類金属ビスアルキルフェノールスルホネート、ジチオホスフェート、アルケニル琥珀酸半-アミド、またはこれらの組合せの少なくとも1つを含む、請求項28に記載の組成物。
- ナノ粒子が、有機媒体によりカプセル化又は被覆されている、請求項13〜29のいずれか1項に記載の組成物。
- 請求項13〜30のいずれか1項に記載の組成物を使用する方法であって、該組成物で対象を潤滑処理する工程を含む、方法。
- 請求項13〜30のいずれか1項に記載の組成物を使用する方法であって、該組成物で対象をコーティングする工程を含む、方法。
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