CN101463478A - Preparation of double-layer nanometer film composed of multi-alkyl cyclopentane and self-assembled membrane - Google Patents
Preparation of double-layer nanometer film composed of multi-alkyl cyclopentane and self-assembled membrane Download PDFInfo
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- CN101463478A CN101463478A CN 200710307292 CN200710307292A CN101463478A CN 101463478 A CN101463478 A CN 101463478A CN 200710307292 CN200710307292 CN 200710307292 CN 200710307292 A CN200710307292 A CN 200710307292A CN 101463478 A CN101463478 A CN 101463478A
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- assembled
- coupling agent
- polyalkylcyclopentane
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- RGSFGYAAUTVSQA-UHFFFAOYSA-N pentamethylene Natural products C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 title claims description 25
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 title claims description 24
- 239000012528 membrane Substances 0.000 title claims 2
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 14
- 238000004528 spin coating Methods 0.000 claims abstract description 8
- 239000007822 coupling agent Substances 0.000 claims abstract 2
- 239000013545 self-assembled monolayer Substances 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000002094 self assembled monolayer Substances 0.000 claims description 20
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000003921 oil Substances 0.000 claims description 4
- 150000001282 organosilanes Chemical class 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 150000002430 hydrocarbons Chemical group 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 235000012431 wafers Nutrition 0.000 claims 3
- -1 n-dodecyl Chemical group 0.000 claims 2
- 150000003376 silicon Chemical class 0.000 claims 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 abstract description 6
- 239000002120 nanofilm Substances 0.000 abstract 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 10
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 6
- 239000000314 lubricant Substances 0.000 description 6
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 230000033444 hydroxylation Effects 0.000 description 4
- 238000005805 hydroxylation reaction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000077 silane Inorganic materials 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- BNCXNUWGWUZTCN-UHFFFAOYSA-N trichloro(dodecyl)silane Chemical compound CCCCCCCCCCCC[Si](Cl)(Cl)Cl BNCXNUWGWUZTCN-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 3
- 238000000682 scanning probe acoustic microscopy Methods 0.000 description 3
- 229910016569 AlF 3 Inorganic materials 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 241000252506 Characiformes Species 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
本发明公开了一种多烷基环戊烷和自组装膜组成的双层纳米膜的制备方法。本发明用普通硅烷偶联剂或全氟硅烷偶联剂在羟基化的单晶硅表面利用气相法制备单分子自组装膜，然后用旋涂方法再在自组装单分子表明形成一层流动性的多烷基环戊烷，而制备成由MAC和自组装单分子膜组成的纳米双层膜。The invention discloses a preparation method of a double-layer nano-film composed of polyalkylcyclopentane and a self-assembled film. The present invention uses common silane coupling agent or perfluorosilane coupling agent to prepare monomolecular self-assembled film on the surface of hydroxylated single crystal silicon by gas phase method, and then forms a layer of fluidity on self-assembled monomolecular surface by spin coating method. The polyalkylcyclopentane was prepared into a nano-bilayer film composed of MAC and self-assembled monomolecular film.
Description
Technical field
The present invention has narrated the preparation method of the double-layer nanometer film of a kind of multi-alkyl cyclopentane and self-assembled film composition.
Background technology
Because excellent performance and low cost, microelectromechanical systems (being called for short MEMS) and hard disc of computer industry obtained development rapidly in the past in 20 years, and had obtained being extensive use of.But adherent phenomenon and friction problem have a strong impact on the yield rate of MEMS, and can directly cause the inefficacy of micro element, self-assembled monolayer (SAMs) with the substrate combination firmly, low surface energy and good lubrication are arranged, yet wearing and tearing easily take place and lose lubrication in SAMs in the device operational process.As for hard disc of computer, method commonly used at present is earlier at magnetic storage layer surface preparation hard diamond-like carbon film or CN
xProtective layer again at protective layer surface-coated lubricant film as thin as a wafer, selects for use PFPE (PFPE) lubricating oil to prepare the disk protect lubricant film usually.But PFPE is with magnetic head common used material Al
2O
3Chemical action can take place in friction process produce Lewis acid AlF
3, AlF
3Catalyzed degradation PFPE conversely then.Multi-alkyl cyclopentane (MAC) steam forces down, chemical stability is good, tribological property is good, is lubricant for magnetic recording medium such as extremely promising novel disk, tape.Therefore, MAC is well combined the lubrication problem that is expected to solve MEMS and hard disc of computer with self-assembled film.
Summary of the invention
The object of the present invention is to provide the preparation method of the double-layer nanometer film of a kind of multi-alkyl cyclopentane and self-assembled film composition.
The present invention utilizes vapor phase process to prepare self-assembled monolayer with common silane coupling agent or perfluor silane coupling agent at hydroxylated monocrystalline silicon surface, show the multi-alkyl cyclopentane (MAC) that forms one deck flowability at self-composed monomolecular again with spin coating method then, and be prepared into the nano double tunic of forming by MAC and self-assembled monolayer.
Preparation method of the present invention comprises A and two steps of B successively:
A. the preparation of functionalization organosilane self-assembled monolayer:
The container that fills silane coupling agent is placed in the autoclave that contains the hydroxylation silicon chip that can lead to nitrogen, earlier logical high pure nitrogen displaces the air in the still, encloses container, place oil bath slowly to be heated to 150 ℃, constant temperature naturally cools to room temperature then, open container, it is ultrasonic respectively in dehydrated alcohol and acetone to take out silicon chip, to remove the silane coupling agent of physical adsorption, dries up with nitrogen and promptly gets surperficial uniform self-assembled monolayer;
B. the preparation of multi-alkyl cyclopentane liquid film on self-assembled monolayer:
The silicon chip of organosilane self-assembled monolayer with preparation, be fixed on the sol evenning machine, the hexane solution that dropwise drips 0.05% multi-alkyl cyclopentane carries out spin coating under the speed of 3000rpm on silicon chip, obtain the duplicature of different thickness by control spin coating number of times.
Silane coupling agent involved in the present invention is the hydrocarbon chain silane coupling agent of 8-18 carbon or the tri-alkoxy perfluor silane coupling agent of 6-12 carbon.
Multi-alkyl cyclopentane is the multi-alkyl cyclopentane of dodecyl replacement or the multi-alkyl cyclopentane (MAC) that 2-octyl group dodecyl replaces.
Preparation method of the present invention is simple, workable, and thickness is controlled easily.Friction, wearing test result show: prepared duplicature can significantly improve the supporting capacity and the wear resistance of self-assembled monolayer.Not only be expected to solve the problem that supporting capacity that self-assembled film exists is low and wear no resistance in microelectromechanical systems is used, and the lubricant multi-alkyl cyclopentane that is expected to now only to be used for aerospace oiling system excellent performance is used for microelectromechanical systems or hard disc of computer industry.
The present invention has following advantage:
(1) this invention adopts vapor phase process to prepare self-assembled monolayer, compare with liquid phase method, overcome liquid phase method silane coupling agent facile hydrolysis and easily formed the shortcoming of polymkeric substance, the self-assembled monolayer that forms is combined in monocrystalline silicon surface by the chemical bond formal bond fully, combination degree is more firm, and the film surface that forms is uniform and smooth.
(2) Zhi Bei double-layer nanometer film is made up of at the self-assembled monolayer that monocrystalline silicon surface forms with chemical bonding with different silane coupling agents the multi-alkyl cyclopentane of lubricity excellence, combine the two-fold advantage of bonding lubricant (SAMs) and nonbonding lubricant (mobile MAC), therefore prepared nano double tunic has better tribological property.
(3) multi-alkyl cyclopentane with excellent lubricity has improved the supporting capacity and the wear resistance of single self-assembled monolayer greatly, has greatly expanded the purposes of self-assembled monolayer and multi-alkyl cyclopentane.In order to understand the present invention better, describe by example:
Embodiment:
Embodiment 1: the preparation of multi-alkyl cyclopentane and dodecyl trichlorosilane double-layer nanometer film
Comprise two steps of A and B successively:
A. the preparation of dodecyl trichlorosilane self-assembled monolayer
(1) doing substrate with monocrystalline silicon piece, is that the vitriol oil of 70%:30% and the mixing solutions of hydrogen peroxide (Piranha solution) clean distilled water rinsing, N with volume ratio down at 90 ℃
2Air-blowing is done, and promptly gets the silicon chip of surface hydroxylation.
(2) the dodecyl trichlorosilane of getting 0.2ml adds in the Glass Containers of exsiccant 2ml, and Glass Containers is placed the autoclave of the led to nitrogen that is placed with the hydroxylation silicon chip, and logical nitrogen flooding is removed air rear enclosed container in the still.
(3) slowly be heated to 150 ℃ in oil bath, constant temperature two hours is cooled to room temperature, takes out silicon chip in dehydrated alcohol and acetone ultrasonic 5 minutes respectively, N
2Air-blowing is done, and is self-assembled monolayer.
B. the preparation of the double-layer nanometer film of multi-alkyl cyclopentane and self assembled monolayer composition:
(1) the dose volume mass percent is the hexane solution of 0.05% multi-alkyl cyclopentane.
(2) silicon chip of dodecyl trichlorosilane self-assembled monolayer with preparation is fixed on the sol evenning machine, the hexane solution that dropwise drips 0.05% multi-alkyl cyclopentane is on silicon chip, under the speed of 3000rpm, carry out spin coating, can obtain the duplicature of different thickness by control spin coating number of times.
Embodiment 2: multi-alkyl cyclopentane and 1, H, 1H, 2H, the preparation of 2H dodecyl triethoxy perfluor silane double-layer nanometer film
Comprise two steps of A and B successively:
A.1, H, 1, H, 2H, the preparation of 2H dodecyl triethoxy perfluor silane self-assembled monolayer
(1) do substrate with monocrystalline silicon piece, hydroxylacion method is with embodiment 1.
(2) get 1 of 0.2ml, H, 1H, 2H, 2H dodecyl triethoxy perfluor silane add in the Glass Containers of exsiccant 2ml, and Glass Containers is placed the autoclave of the led to nitrogen that is placed with the hydroxylation silicon chip, and logical nitrogen flooding is removed air rear enclosed container in the still.
(3) heat treatment process of substrate and last handling process are with embodiment 1.
B. the preparation of the double-layer nanometer film of multi-alkyl cyclopentane and self assembled monolayer composition:
(1) the hexane solution compound method of multi-alkyl cyclopentane is with embodiment 1.
(2) prepare multi-alkyl cyclopentane and 1 with spin coating method, H, 1H, 2H, the method for the double-layer nanometer film that 2H dodecyl triethoxy perfluor silane is formed is with embodiment 1.
Claims (3)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710307292 CN101463478A (en) | 2007-12-18 | 2007-12-18 | Preparation of double-layer nanometer film composed of multi-alkyl cyclopentane and self-assembled membrane |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710307292 CN101463478A (en) | 2007-12-18 | 2007-12-18 | Preparation of double-layer nanometer film composed of multi-alkyl cyclopentane and self-assembled membrane |
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| Publication Number | Publication Date |
|---|---|
| CN101463478A true CN101463478A (en) | 2009-06-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710307292 Pending CN101463478A (en) | 2007-12-18 | 2007-12-18 | Preparation of double-layer nanometer film composed of multi-alkyl cyclopentane and self-assembled membrane |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102102045A (en) * | 2009-12-18 | 2011-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing metal nanoparticle-polysubstituted cyclopentane composite lubricating film |
| CN101705488B (en) * | 2009-11-09 | 2012-04-11 | 东南大学 | Surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surface |
| CN101734610B (en) * | 2009-12-15 | 2012-05-23 | 江苏大学 | Multilayer film for low load working condition of micro electro mechanical system and preparation method thereof |
| CN107557109A (en) * | 2017-09-04 | 2018-01-09 | 兰州空间技术物理研究所 | Branched-alkyl substituted silane aromatic hydrocarbon self-assembled lubricating film and preparation method thereof |
-
2007
- 2007-12-18 CN CN 200710307292 patent/CN101463478A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705488B (en) * | 2009-11-09 | 2012-04-11 | 东南大学 | Surface processing method of super-hydrophobic ice-covering-proof aluminum and steel with rough surface |
| CN101734610B (en) * | 2009-12-15 | 2012-05-23 | 江苏大学 | Multilayer film for low load working condition of micro electro mechanical system and preparation method thereof |
| CN102102045A (en) * | 2009-12-18 | 2011-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing metal nanoparticle-polysubstituted cyclopentane composite lubricating film |
| CN107557109A (en) * | 2017-09-04 | 2018-01-09 | 兰州空间技术物理研究所 | Branched-alkyl substituted silane aromatic hydrocarbon self-assembled lubricating film and preparation method thereof |
| CN107557109B (en) * | 2017-09-04 | 2020-03-17 | 兰州空间技术物理研究所 | Branched alkyl substituted silanized aromatic hydrocarbon self-assembled lubricating film and preparation method thereof |
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Open date: 20090624 |