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8 protocols using sip6831

1

Fabrication of ZrO2 Nanocomposite Materials

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ZrO2 nanocomposites were prepared from a solution with 30 wt% 10 nm ZrO2 NPs dispersed in MIBK, which were purchased from Ditto Technology (DT-ZROSOL-30MIBK (N10)). Dipentaerythritol penta-/hexa-acrylate and 1-hydroxycyclohexyl phenyl ketone were purchased from Sigma‒Aldrich and used as a monomer and a photoinitiator, respectively. MIBK, MEK, and acetone were purchased from Duksan General Science. h-PDMS, a vinylmethyl copolymer (VDT-731), a platinum catalyst (SIP6831.2), and a siloxane-based silane reducing agent (HMS-301) were purchased from Gelest. 2,4,6,8-Tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane and toluene, which were used as a modulator and a solvent, were purchased from Sigma‒Aldrich and Samchun Chemicals, respectively. PDMS, a silicone elastomer base, and a silicone elastomer curing agent were purchased from Dow Corning (SYLGARD™ 184 Silicone Elastomer Kit). The trichloro(1H,1H,2H,2H-perfluorooctyl)silane used for hydrophobic coating was purchased from Sigma‒Aldrich. toluene and n-hexane were purchased from Samchun Chemicals.
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2

Silicone Gel Fabrication and Characterization

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Silicone gels are made following the recipe in [29 ]. In brief, we mix divinyl-terminated polydimethylsiloxane (DMS-V31, Gelest), a cross-linker (HMS-301, Gelest) and a catalyst (SIP6831.2, Gelest). The mixture is thoroughly degassed, and then cured in an oven at 40°C for at least 24 hours. The gels’ Young moduli, E, are tuned by changing the ratio of divinyl-terminated chains to cross-linker in the mixture, while keeping the concentration of catalyst at 0.0019% by volume. The stiffness of the gels are measured by indentation experiments (e.g. [9 ]). Other mechanical properties of the gels are demonstrated in the Supplemental information.
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3

Fabrication of PDMS-based Microfluidic Devices

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All commercial reagents were obtained from Aldrich Chemical Co. and used without further purification unless otherwise specified. Hard PDMS components: (7.0-8.0% vinylmethylsiloxane)-dimethylsiloxane copolymer (VDT-731), platinum-divinyltetramethyldisiloxane (SIP6831.2), 1,3,5,7-tetravinyl-1,3,5,7-tetramethylcyclotetrasiloxane (SIT7900.0), and (25-30% methylhydrosiloxane)-dimethylsiloxane copolymer (HMS-301) were purchased from Gelest. The soft PDMS elastomer kit (Sylard 184) was ordered from Dow corning. The alkanethiol solution was prepared by dissolving 1-octadecylthiol in ethanol to obtain a concentration of 5mM. The amine backfilling solution was prepared by dissolving 10 mg ml−1 3,6-diaminoacridine hydrochloride in a mixture of ethanol and diacetone alcohol and then immediately filtered through 0.22 μm syringe filters before use.
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4

Nanoscale Soft-Mold Fabrication via SAM

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The master mold was coated by liquid-phase SAM to improve mold release in a solution mixture of a 1000:1 volume ratio of hexane and (heptadecafluoro-1,1,2,2-tetra-hydodecyl)trichlorosilane (H5060.1, JSI silicone) for 10 min. h-PDMS solution was prepared by mixing 3.4 g of vinylmethyl copolymers (VDT-731, Gelest), 18 μL of platinum-catalyst (SIP6831.2, Gelest), 0.1 g of modulator (2,4,6,8-Tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, Sigma-aldrich), 2 g of toluene and 1 g of siloxane-based silane reducing agent (HMS-301, Gelest). The h-PDMS was spin-coated on the master mold at 3000 rpm for 50 s, then baked at 70 °C for 2 h. A degassed mixture of a 10:1 weight ratio of PDMS (Sylgard 184 A, Dow corning) and its curing agent (Sylgard 184 B, Dow corning) was poured on the h-PDMS layer, then baked at 100 °C for 2 h. The soft-mold was released from the master mold, then coated with vapor-phase SAM by a typical vaporizing process using (tridecafluoro-1,1,2,2-tetrahydrooctyl)trichlorosilane (SIT8174.0, Gelest) for 30 min at 5 Torr followed by DI water for 10 min at 10 Torr. The 3 μL of NPC was dropped on a glass substrate, then it was covered by the soft-mold. UV light was illuminated for 5 min at 2 bar to harden the NPC (Nanosis 820, NND). The soft-mold was released to complete the replication process.
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5

Fabrication of Nano-PER Structures

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h-PDMS was prepared by mixing 3.4 g of vinylmethyl copolymers (VDT-731, Gelest), 18 μL of platinum-caralyst (SIP6831.2, Gelest), 0.1 g of the modulator (2,4,6,8- tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane, Sigma-aldrich), 2 g of toluene, and 1 g of siloxane-based silane reducing agent (HMS-301, Gelest). The h-PDMS was spin-coated on the master mold at 1,000 rpm for 60 s, then baked at 70 °C for 2 h. A mixture of a 10:1 weight ratio of PDMS (Sylgard 184 A, Dow corning) and its curing agent (Sylgard 184 B, Dow corning) was poured on the h-PDMS layer and cured at 80 °C for 2 h. The cured soft mold was detached from the master mold, then used to replicate the nano-PER structure.
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6

Facile Fabrication of Hydrophobic Nanostructures

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Before replicating the nanostructures, the fabricated master mold was treated with an O2 plasma process to decontaminate it and improve hydrophilicity. The surface‐treated master mold formed a self‐assembled monolayer via a vaporized silane coupling agent (Trichloro‐1H, 1H, 2H, 2H‐Perfluorooctyl‐silane, Sigma–Aldrich) coating for 5 min at 130 °C, thereby exhibiting a hydrophobic surface, which allowed for facilitated demolding. After the surface treatment of the master mold, h‐PDMS was prepared by blending 1.7 g of vinylmethyl copolymer (VDT731, Gelest), 9 µL of platinum‐catalyst (SIP6831.2, Gelest), 0.05 g of the modulator (2,4,6,8 – tetramethyl‐ 2,4,6,8 – tetravinylcyclotetrasiloxane, Sigma–Aldrich), 1 g of toluene, and 0.5 g of siloxane‐based silane reducing agent (HMS‐301, Gelest). The h‐PDMS was spin coated on the master‐mold at 2,000 rpm for 60 s, followed by a baking process at 70 °C for 2 h to harden the h‐PDMS. Then, the PDMS mixture consisting of a 1:10 weight ratio of PDMS (Sylgard 184 A, Dow corning) and curing agent (Sylgard 184 B, Dow corning) was poured onto the h‐PDMS layer, followed by baking at 70 °C for 2 h to harden the h‐PDMS. After this process, the hardened soft mold was demolded from the master mold and used for replication.
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7

Hierarchical PDMS Replication from HSQ Molds

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Hard PDMS (hPDMS) templates were replicated from the patterned HSQ molds. Oxygen plasma-treated molds were functionalized with 1H,1H,2H,2H-perfluorodecyltriethoxysilane (MilliporeSigma) to prevent adhesion to the PDMS template. Prepolymer mixture of hPDMS, consisting of 3.4-g VDT-731 (vinylmethylsiloxane-dimethylsiloxane, Gelest), 18 μl of SIP6831.2 (platinum catalyst, Gelest), 5 μl of 2,4,6,8-tetramethyl-2,4,6,8-tetravinylcyclotetrasiloxane (MilliporeSigma), and 1.0-g HMS-301 (methylhydrosiloxane-dimethylsiloxane copolymer, Gelest) (40 (link)), was thoroughly mixed. The mixture was immediately spin-coated onto the fluorinated mold at 3000 rpm for 30 s. The mold was then brought into contact with a soft PDMS (Sylgard 184) film on a glass backing. The stack was cured at 75°C for 14 hours. Once cured, the PDMS was peeled from the mold exposing the topographical template.
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8

Fabrication of PDMS-HFBMA Bicontin uious Samples

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First, we prepare pure PDMS matrices by mixing PDMS chains (DMS-V31, Gelest) with a crosslinker (HMS-301, Gelest) and a platinum-based catalyst (SIP6831.2, Gelest) (see full recipe in [47] ). The stiffness of the matrix depends on the mass ratio between the chains and crosslinker (from 3:1 to 9:1), while keeping the catalyst concentration constant (0.0019% in volume). Once the different parts are thoroughly mixed together, we pour the mixture into a petri dish, degassed it in vacuum, and finally cure it at 60 • C for approximately 6 days. After curing, the resulting PDMS elastomer is carefully removed from the petri dish and cut into rectangular pieces (∼1cm×2cm×0.5cm).
Next, PDMS pieces are transferred into a bath of heptafluorobutyl methacrylate (HFBMA, Apollo scientific) (∼1mL HFBMA/0.5g of PDMS), in a 25mL glass bottle. This bath is then typically incubated at T swell = 60 • C in a pre-heated oven during 2.5 days. After the elastomer is saturated with the liquid, the glass bottle is brought to room temperature, at which point phase separation occurs spontaneously. The resulting phase-separated bicontiunous samples are then prepared for characterization tests.
Note that experiments with un-crosslinked PDMS are performed by preparing mixtures of PDMS chains and HFBMA liquid in glass bottles, and following the same temperature steps described above.
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