CN105647279A - Application of beta-cyclodextrin and nitroferrocene composite solution in micro-contact printing - Google Patents

Application of beta-cyclodextrin and nitroferrocene composite solution in micro-contact printing Download PDF

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Publication number
CN105647279A
CN105647279A CN201511001619.5A CN201511001619A CN105647279A CN 105647279 A CN105647279 A CN 105647279A CN 201511001619 A CN201511001619 A CN 201511001619A CN 105647279 A CN105647279 A CN 105647279A
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China
Prior art keywords
beta
cyclodextrin
nitro
ferrocene
solution
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Granted
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CN201511001619.5A
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Chinese (zh)
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CN105647279B (en
Inventor
苏炜
李培源
陈今浩
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Guangxi Beibu Gulf Grain And Oil Technology Research Co ltd
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Guangxi Teachers College
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/14—Printing inks based on carbohydrates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M1/00—Inking and printing with a printer's forme
    • B41M1/12—Stencil printing; Silk-screen printing
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D11/00—Inks
    • C09D11/02—Printing inks
    • C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
    • C23C18/28—Sensitising or activating
    • C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper using reducing agents
    • C23C18/405—Formaldehyde

Abstract

The invention discloses an application of a beta-cyclodextrin and nitroferrocene composite solution in micro-contact printing. The beta-cyclodextrin and nitroferrocene composite solution is used in micro-contact printing as a printing agent, the pattern of a PDMS stamper is transferred to a carboxylated polypropylene substrate, and a chemical plating method is carried out to obtain an exquisite metal pattern on the polypropylene substrate. Production of the metal pattern on the surface of the polypropylene substrate commonly used in the electronic industry through using the beta-cyclodextrin and nitroferrocene composite solution as micro-contact printing ink provides a new idea for the micro-contact printing industry.

Description

Utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing
Technical field
The invention belongs to modern electronic technology field, utilize beta-cyclodextrin and nitro ferrocene as the application of composite green Environment-friendlyink ink in micro-contact printing in particular to a kind of.
Background technology
Surface micro-constructing technology embody just gradually in significant application value, particularly microcontact printing techniques, its can in little size micro-patterning, in multiple field, particularly modern electronic technology field is significant. Current alternative micro-contact printing ink is less, has also limited to the material that surface can carry out micro-contact printing, and a large amount of materials cannot prepare picture on surface by the method for micro-contact printing. Thus develop new, stable ink to have a very big significance.
In order to adapt to a new generation's ink for the requirement of environmental protection and HUMAN HEALTH, it is necessary to develop the application of cyclodextrin in micro-contact printing further. Cyclodextrin is nontoxic, has good human compatibility. Beta-cyclodextrin and nitro ferrocene composite solution stable performance, quality of forming film height, it is possible to be applied to the micro-contact printing of surfaces of various materials as a kind of stable ink. Current beta-cyclodextrin and nitro ferrocene composite solution have no report as the application of micro-contact printing ink.
Summary of the invention
It is an object of the invention to provide and a kind of utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, using print paste as micro-contact printing of beta-cyclodextrin and nitro solution of ferrocene, by the design transfer of PDMS seal to carboxylated polypropylene substrate, then in polypropylene substrate, obtain exquisite metal pattern by the method for electroless plating.
In order to realize the object according to the present invention and other advantage, it provides utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, comprising:
Step one, obtains beta-cyclodextrin water dissolution the beta-cyclodextrin aqueous solution that concentration is 3-6g/L, and adds nitro ferrocene in the gained beta-cyclodextrin aqueous solution, and 20KHz ultrasonic concussion 30-60min obtains beta-cyclodextrin and nitro ferrocene composite solution;
Step 2, is soaked in 30-40s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 30-60s, is placed in carboxylated polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 10-20s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern;
Step 3, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern210-30s in solution, puts into the solution for electroless copper and carries out electroless plating after taking-up, the time is 1-10min, after polypropylene substrate being taken out, can obtain metallic copper pattern in polypropylene substrate.
Preferably, described utilizing beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, this nitro ferrocene structural formula is as follows:
Preferably, described utilizing beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, in step one, the usage ratio of the beta-cyclodextrin aqueous solution and nitro ferrocene is, adds 0.8g nitro ferrocene in often liter of beta-cyclodextrin aqueous solution.
Preferably, described utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, polypropylene substrate is carried out carboxylated method is: at the isopropanol water solution of 45-55%, polypropylene substrate is soaked 30-60min, under 55-65 DEG C of condition, 15-20min is soaked again with 2-3mol/L sulfuric acid, 60-65 DEG C of vacuum-drying, obtains carboxyted polypropylene substrate.
Preferably, described utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, in step 3, the solution for electroless copper is made up of the distilled water of 4-6wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and surplus.
The present invention at least comprises following useful effect:
1. by beta-cyclodextrin and nitro ferrocene composite solution are prepared metal pattern as micro-contact printing ink at the polypropylene-base basal surface that electron trade is conventional, for micro-contact printing industry provides new approaches.
2. the hydrophobic cavities of inside " V " font of beta-cyclodextrin applicable accommodation nitro ferrocene molecule enters and is fixed on beta-cyclodextrin molecule inside.
3. nitro has electron attraction, increases the positive polarity of iron, effectively improves the coordination keying action of the carboxyl of iron and substrate surface, makes the pattern of printing and substrate combine tightr.
4. beta-cyclodextrin has good biocompatibility, and iron is one of element indispensable in human body, it is possible to meet a new generation's ink for the requirement of environmental protection and HUMAN HEALTH.
Embodiment
The present invention is described in further detail below, to make those skilled in the art can implement according to this with reference to specification sheets word.
Utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, comprising:
Step one, substrate is carboxylated, and the isopropanol water solution of polypropylene substrate 45-55% is soaked 30-60min, under 55-65 DEG C of condition, 15-20min is soaked again with 2-3mol/L sulfuric acid, cleaning with water subsequently, 60-65 DEG C of vacuum-drying, obtains carboxyted polypropylene substrate.
Step 2, prepare beta-cyclodextrin and nitro ferrocene composite solution, beta-cyclodextrin water dissolution is obtained the beta-cyclodextrin aqueous solution that concentration is 3-6g/L, often liter of beta-cyclodextrin aqueous solution adds 0.8g nitro ferrocene, the ultrasonic 30-60min of 20kHz, obtaining beta-cyclodextrin and the nitro ferrocene composite solution of evenly dispersion, wherein, the structural formula of nitro ferrocene is:
Step 3, micro-contact printing, is soaked in 30-40s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 30-60s, is placed in carboxyted polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 10-20s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern.
Step 4, electroless plating, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern210-30s in solution, is put in after taking-up in the chemical bronze plating liquid being made up of the distilled water of 4-6wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and surplus and carries out electroless plating, and the time is 1-10min. Exquisite metallic copper pattern can be obtained in polypropylene substrate after taking-up.
Embodiment 1
Utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, comprising:
Step one, substrate is carboxylated, with the isopropanol water solution of 45%, polypropylene substrate is soaked 30min, then soaks 15min with 2mol/L sulfuric acid under 55 DEG C of conditions, cleans with water subsequently, and 60 DEG C of vacuum-dryings, obtain carboxyted polypropylene substrate.
Step 2, prepare beta-cyclodextrin and nitro ferrocene composite solution, beta-cyclodextrin water dissolution is obtained the beta-cyclodextrin aqueous solution that concentration is 3g/L, often liter of beta-cyclodextrin aqueous solution adds 0.8g nitro ferrocene, the ultrasonic 30min of 20kHz, obtains beta-cyclodextrin and the nitro ferrocene composite solution of evenly dispersion.
Step 3, micro-contact printing, is soaked in 30s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 30s, is placed in carboxyted polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 10s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern.
Step 4, electroless plating, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern210s in solution, is put in after taking-up in the chemical bronze plating liquid being made up of 4wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and 51wt% distilled water and carries out electroless plating, and the time is 5min. Exquisite metallic copper pattern can be obtained in polypropylene substrate after taking-up.
Embodiment 2
Utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, comprising:
Step one, substrate is carboxylated, with the isopropanol water solution of 50%, polypropylene substrate is soaked 50min, then soaks 20min with 2.5mol/L sulfuric acid under 55-65 DEG C of condition, cleans with water subsequently, and 60 DEG C of vacuum-dryings, obtain carboxyted polypropylene substrate.
Step 2, prepare beta-cyclodextrin and nitro ferrocene composite solution, beta-cyclodextrin water dissolution is obtained the beta-cyclodextrin aqueous solution that concentration is 5g/L, often liter of beta-cyclodextrin aqueous solution adds 0.8g nitro ferrocene, the ultrasonic 50min of 20kHz, obtains beta-cyclodextrin and the nitro ferrocene composite solution of evenly dispersion.
Step 3, micro-contact printing, is soaked in 35s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 40s, is placed in carboxyted polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 15s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern.
Step 4, electroless plating, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern220s in solution, is put in after taking-up in the chemical bronze plating liquid being made up of 5wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and 50wt% distilled water and carries out electroless plating, and the time is 10min. Exquisite metallic copper pattern can be obtained in polypropylene substrate after taking-up.
Embodiment 3
Utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, comprising:
Step one, substrate is carboxylated, with the isopropanol water solution of 55%, polypropylene substrate is soaked 60min, then soaks 20min with 3mol/L sulfuric acid under 55-65 DEG C of condition, cleans with water subsequently, and 65 DEG C of vacuum-dryings, obtain carboxyted polypropylene substrate.
Step 2, prepare beta-cyclodextrin and nitro ferrocene composite solution, beta-cyclodextrin water dissolution is obtained the beta-cyclodextrin aqueous solution that concentration is 6g/L, often liter of beta-cyclodextrin aqueous solution adds 0.8g nitro ferrocene, the ultrasonic 60min of 20kHz, obtains beta-cyclodextrin and the nitro ferrocene composite solution of evenly dispersion.
Step 3, micro-contact printing, is soaked in 40s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 60s, is placed in carboxyted polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 20s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern.
Step 4, electroless plating, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern230s in solution, is put in after taking-up in the chemical bronze plating liquid being made up of 6wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and 49wt% distilled water and carries out electroless plating, and the time is 10min. Exquisite metallic copper pattern can be obtained in polypropylene substrate after taking-up.
Embodiment 4
Human body normal epidermis cell HaCaT is incubated at Da Erbaike improve in Eagle's medium (DMEM) nutrient solution (containing 10% new-born calf serum), puts 37 DEG C, 5%CO2Cultivating under condition, 1��2d changes 1 nutrient solution. When cell grows to the polypropylene substrate process that logarithmic phase adds undressed polypropylene substrate respectively, embodiment 1,2 and 3 gained is printed on metallic copper pattern. Cell is placed in 37 DEG C, 5%CO with 0.25% Trypsin 96 orifice plate2Incubator is cultivated. After 2��4h, every block culture plate adds undressed polypropylene substrate respectively and embodiment 1-3 gained is printed on the polypropylene substrate of metallic copper pattern and complete culture solution cultured cells as a control group and experimental group, culture plate, as blank, is moved into 37 DEG C, 5%CO by the nutrient solution not containing cell and sample2Incubator is cultivated. After 24h, abandon nutrient solution, phosphate buffered saline buffer (PBS) washes plate 2 times, adds 2-(2-methoxyl group-4-nitrophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfonic acid benzene)-2H-tetrazolium list sodium (CCK-8) 10 �� l. Continue at 37 DEG C, 5%CO22��4h cultivated by incubator, and microplate reader 550nm place surveys each hole optical density(OD) (D value). Cell survival rate (%)=[(experimental port D value-blank well D value)/(control wells D value-blank well D value)] �� 100%, experimental result is as shown in table 1.
Table 1
As can be seen from Table 1, the cell survival rate of the polypropylene substrate of the present invention after electroless copper is obviously higher than undressed polypropylene substrate, illustrate that beta-cyclodextrin and nitro ferrocene composite solution are as micro-contact printing ink good biocompatibility, cytotoxicity is low, safety non-toxic is little to human body harm.
Although embodiment of the present invention are open as above, but listed utilization that it is not restricted in specification sheets and enforcement mode, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore claim is not being deviated from and under general concept that equivalency range limits, the present invention is not limited to specific details.

Claims (5)

1. one kind utilizes beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing, it is characterised in that,
Step one, obtains beta-cyclodextrin water dissolution the beta-cyclodextrin aqueous solution that concentration is 3-6g/L, and adds nitro ferrocene in the gained beta-cyclodextrin aqueous solution, and 20KHz ultrasonic concussion 30-60min obtains beta-cyclodextrin and nitro ferrocene composite solution;
Step 2, is soaked in 30-40s in beta-cyclodextrin and nitro ferrocene composite solution, in N after taking-up by PDMS seal2In air-flow, dry 30-60s, is placed in carboxylated polypropylene substrate by the PDMS seal scribbling beta-cyclodextrin and nitro ferrocene composite solution, gently presses 10-20s, PDMS seal designs is transferred to polypropylene-base basal surface, obtain being printed on the polypropylene substrate of pattern;
Step 3, is soaked in 0.1g/LPdCl by the polypropylene substrate being printed on pattern210-30s in solution, puts into the solution for electroless copper and carries out electroless plating after taking-up, the time is 1-10min, after polypropylene substrate being taken out, can obtain metallic copper pattern in polypropylene substrate.
2. utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing as claimed in claim 1, it is characterised in that, this nitro ferrocene structural formula is as follows:
3. utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing as claimed in claim 1, it is characterized in that, in step one, the usage ratio of the beta-cyclodextrin aqueous solution and nitro ferrocene is, adds 0.8g nitro ferrocene in often liter of beta-cyclodextrin aqueous solution.
4. utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing as claimed in claim 1, it is characterized in that, polypropylene substrate is carried out carboxylated method is: at the isopropanol water solution of 45-55%, polypropylene substrate is soaked 30-60min, under 55-65 DEG C of condition, 15-20min is soaked again with 2-3mol/L sulfuric acid, 60-65 DEG C of vacuum-drying, obtains carboxyted polypropylene substrate.
5. utilize beta-cyclodextrin and nitro ferrocene composite solution in the application of micro-contact printing as claimed in claim 1, it is characterized in that, in step 3, the solution for electroless copper is made up of the distilled water of 4-6wt% copper sulfate, 7wt% sodium-potassium tartrate, 6wt% sodium hydroxide, 32wt% formaldehyde and surplus.
CN201511001619.5A 2015-12-28 2015-12-28 Using beta-cyclodextrin and nitro ferrocene composite solution micro-contact printing application Active CN105647279B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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JPH0952463A (en) * 1995-08-10 1997-02-25 Riso Kagaku Corp Fixing method of printing water base ink and water base ink
CN104312262A (en) * 2014-11-05 2015-01-28 广西师范学院 Application of 2-6 carboxyl phthalocyanine palladium and anthraquinone serving as micro-contact printing ink
CN104387835A (en) * 2014-11-05 2015-03-04 广西师范学院 Water-soluble double-sandwich-type La metalloporphyrin complex and application thereof in micro-contact printing technique
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