Method of modification of the hydrophobic surfaces

FIELD: medical and biological instrumentation industry; methods of modification of the hydrophobic surfaces.

SUBSTANCE: the invention is pertaining to the method of modification of hydrophobic surfaces and may be used for upgrading the hydrophobic surfaces used in the scanning probe microscopy, in the immune-enzyme analysis, at development of the biochips. The method of modification of hydrophobic surfaces includes deposition on the surface of the modifying monolayer of the complex composition molecules containing the functional group, the section forming the hydrogenous ties and the hydrophobic section. At that as the functional group the molecule contains, at least, one group sampled from the following row:NH2, СООН, СНО,ONH2, SH; as the section forming the hydrogen ties the molecule contains the fragments -NH(CH2)nCO- ,where п=1-5, and as the hydrophobic section the molecule contains the fragment -(СН2)n , where n=5-12, or the similar fragment with one or several insertions of the heteroatoms sampled from the row of O, S, NH. In particular, such molecules may have the following composition[Gly4-NHCH2]2C10H20. The invention allows to ensure the high quality evenness of the modified surfaces, reproducibility of their properties and reduction of the time interval of the modification.

EFFECT: the invention ensures the high quality evenness of the modified surfaces, reproducibility of their properties and reduction of the time interval of the modification.

2 cl, 3 dwg

 

The invention relates to a method of modifying a hydrophobic surfaces, in particular of surface modification of high-oriented pyrolytic graphite (HOPG), and may find applications in scanning probe microscopy, immunoassay analysis, creating biochips, as well as to impart hydrophobic surfaces other surface properties.

There is a method of modifying a hydrophobic surface, disclosed in the article:

"Manipulation and Overstretching of Genes on Solid Substrates" Nikolai Severin, Jolrg Barner, Tony A.Kalachev, and Julrgen P.Rabe, NANO LETTERS, 2004, Vol.4, No. 4, 577-579.

The authors modified HOPG surface by depositing a monolayer of octadecylamine and dodecylamine from chloroform or benzene using spinner.

The disadvantages of the method include the fact that damage to the monolayer contains water-insoluble molecules, between which there is only hydrophobic interactions, respectively, the modified surface exhibits hydrophobic properties. For applying a monolayer of octadecylamine and dodecylamine to the surface requires a special device - spinner. In addition, alkali on the surface form a lamella that demonstrates the heterogeneity of the monolayer.

The closest to the invention is a method of modifying a hydrophobic surface by applying to the surface of the monolayer of polymer molecular is, containing hydrophilic side chains and hydrophobic side chains (US 6759388, published. 06.07.2004). The polymer is a mixture of molecules of different molecular weight, and very large. First, it is not possible to obtain a surface with high smoothness, as in the known method, the roughness of the modified surface is 7-12 angstroms (in the claimed method - 1-2 Angstrom). Secondly, the volatility of the molecular structure of the polymer is not possible to obtain the same surface in the same conditions. In addition, the modification time of the molecules of the polymer is large - hours (in the claimed method.

The technical result of the claimed method is to provide high smoothness of the surface, the reproducibility of the properties of modified surfaces and reducing the time of the modification.

The technical result is achieved by the method of modifying a hydrophobic surface, comprising coating the surface modifier of the monolayer, according to which is applied a monolayer of molecules of complex composition, containing functional group, area, forming hydrogen bonds, and hydrophobic region, thus:

as the functional group of the molecule contains at least one group selected from NH2, COOH, Cho, ONH2SH, as the site, forming hydrogen of light and - fragments-NH(CH2)nCO-, where n=1-5, and as the hydrophobic site of the molecule contains a fragment -(CH2)nor fragment(CF2)n-where n=5-12, or the same fragment with one or more inserts heteroatoms such as O, S, NH.

In the best embodiment of the invention is applied to the monolayer of molecules characterized by the formula [Gly4-NHCH2]2C10H10where Gly is a glycine residue.

In the private embodiment of the invention, the monolayer is applied to the surface of high-oriented pyrolytic graphite.

The essence of the proposed method is the use of individual molecules of a substance having the composition of a hydrophobic part and a hydrophilic part that carries the desired functional group (NH2, COOH, etc) and at the same time with the plot (part), capable of forming intermolecular hydrogen bonds.

The hydrophobic portion of the molecule interact with the hydrophobic surface, and the portion of the molecule that can form intermolecular hydrogen bonds, provides interaction between neighboring molecules. Thus, the hydrophobic surface is formed monomolecular film, in which each molecule interacts with neighboring in the monolayer molecules (through the formation of hydrogen-bonding and hydrophobic surface (through the Hydra is falnoga interaction), moreover, the orientation of the molecules in the layer (in the film) is strictly determined by these interactions, so that the functional group exposed at the opposite surface direction and available for further use.

Hereinafter the invention is described by examples with reference to figures 1-3.

Figure 1. The formula of the molecule, corresponding to one of the proposed structures of molecules.

Figure 2. The image of the HOPG surface after modification of the proposed method obtained by using atomic force microscope (AFM).

Figure 3. Image of DNA molecules adsorbed on the surface of high-oriented pyrolytic graphite (HOPG), modified the proposed method obtained using AFM.

The invention is carried out as follows.

For surface modification of high-oriented pyrolytic graphite (HOPG) was used molecules: [Gly4-NHCH2]2C10H20(figure 1), where 1 - amino group, 2-4 glycine residue, 3 - hydrocarbon chain With10H20.

This molecule in aqueous solution is folded in half and forms a molecule with the proposed in this patent structure:

- the functional part (two amino);

- polyglycidol plot (4×2 glycine residue)that can form intermolecular hydrogen bonds;

hydrophobic the plot (hydrocarbon chain With 10H20).

An example of a specific implementation.

On a fresh cleaved HOPG put a drop of the solution [Gly4-NHCH2]2With10H20dissolved in water, with a volume of 50 μl and a concentration of 0.01 mg/ml was kept for 5-10 minutes and was removed by a stream of nitrogen or compressed air.

After this procedure, the surface of the graphite is completely covered by a monolayer of [Gly4-NHCH2]2C10H20.

After incubation sizescolors HOPG at 0.01 mg/ml aqueous solution of this substance on the surface of HOPG is formed almost defect-free monolayer of these molecules (figure 2). The AFM image shows the layer formed by these molecules are also small defects in the monolayer, but their number is small. The average roughness of the surface after deposition of the monolayer [Gly4-NHCH2]2With10H20is about 0.2 nm to modification, while to the modification of the surface sizescolors HOPG has a roughness of less than 0.05 nm, which indicates the formation of a monolayer. Changing the wettability of the surface after modification it becomes more hydrophilic, which can be seen in the spreading of water droplets deposited on the modified HOPG. Before modification the surface sizescolors HOPG fully namachivayam water. A surface roughness of less than 0.2 nm, visible atomar the e steps on the HOPG crystal.

The activity of the surface after modification was verified by deposition of DNA molecules. It is known that DNA molecules are not adsorbed on the HOPG surface due to its hydrophobicity and inertia. However, after modification of the proposed method the HOPG surface acquires a positive charge and the DNA molecules with a negative charge in water, contact with it (figure 3).

For the implementation of the proposed invention in a similar way we also used the following substances:

[SH-[NH-CH2-CO]4-NHCH2]2C10H20

[COOH-[NH-CH2-CO]4-NHCH2]2C10H20

[CHO-[NH-CH2-CO]4-NHCH2]2C10H20

[ONH2-[NH-CH2-CO]4-NHCH2]2C10H20

[H-[NH-C2H4-CO]4-NHCH2]2C10H20

[H-[NH-C3H6-CO]4-NHCH2]2C10H20

[H-[NH-C4H8-CO]4-NHCH2]2C10H20

[H-[NH-C5H10-CO]4-NHCH2]2C10H20

[H-[NH-C2H4-CO]4-NHCH2]2C10H20S

[H-[NH-C2H4-CO]4-NHCH2]2C10H20NH

[H-[NH-C2H4-CO]4-NHCH2]2C10H20O

All these modifying substances allows the t to obtain the technical result because they are all individual substances (oligomers), the monolayer which provides a smooth surface (1-2 Angstrom) and the identity of samples obtained with one and the same substance under identical conditions. Modification time for all of these substances is a few minutes.

Likewise modified the surface of the mica, which was previously gidrofobizirovan using trimethylchlorosilane.

The procedure of waterproofing mica:

Svezhesmoloty the mica was aged in pairs of trimethylchlorosilane for 15-20 minutes, then was heated in an argon atmosphere to 100°and was maintained under these conditions for 10 minutes. After this procedure, the mica surface was water-resistant, i.e. hydrophobic. The procedure of modifying the hydrophobic surface of mica was completely similar to the modification of the graphite. The difference was slightly increased surface roughness of 0.2-0.4 nm. The ability to adsorb DNA molecules this surface coincides with the surface of HOPG.

It is also possible to modify the surface of the silicon and silicon oxide. The procedure is exactly the same as for mica, preliminary hydrophobization by trimethylchlorosilane. It may be of interest for microelectronics, as all technologies using silicon and silicon oxide (quartz).

You can also modify the surface of carbon nanotubes, as it is close to the surface of HOPG.

The use of water-soluble drug in contrast to solutions in benzene or chloroform more environmentally harmless and does not require special conditions (ventilation, for example).

Additional interaction between the molecules by means of hydrogen bonds makes the coating more durable. So, if you are scanning using AFM DNA molecules do not move the probe, and in the following similar they can move.

The modification is achieved by simple immersion or wetting of the sample in solution and requires no additional equipment spinner or centrifuges.

The modification of the surface with the use of water-soluble molecules leads to the formation on the surface of self-organised monolayer without the formation of lamellae, and functional groups in the monolayer are oriented from the surface up to the solution. Modified surface does not introduce additional distortion in the shape of the observed DNA molecules.

The wettability or partial wettability allows to significantly extend the use of these substrates, for example, you can apply other biomolecules or viral particles, which cannot be deposited on a hydrophobic surface.

The invention is not limiting what is shown by the example, and can also be used in the following areas:

1. The surface modification of HOPG for use as a substrate for observing biopolymers and other biological objects by scanning probe microscopy.

2. The surface modification of plastic and glass for adsorption of cells or antibodies, for use in enzyme-linked immunosorbent assay.

3. When using special functional groups capable of specific binding to create biochips. I.e. from solution on the surface will be deposited only those groups that have an affinity to these functional groups.

4. The surface coating of implants for better biocompatibility.

5. To impart hydrophobic surfaces other surface properties - increase in the sorption capacity or improve the wettability. For example, in the textile industry, for better staining dyes wool or other fabrics.

1. A method of modifying a hydrophobic surface, comprising coating the surface modifying monolayer of molecules of complex composition, containing functional group, area, forming hydrogen bonds, and hydrophobic region, the functional groups of the molecule contains at least one group selected from a number of NH2, COOH, Cho, ONH2SH, is the quality of the site, forming a hydrogen bond, the molecule contains fragments-NH(CH2)nCO-, where n=1-5, and as the hydrophobic site of the molecule contains a fragment -(CH2)n-, where n=5-12, or the same fragment with one or more inserts heteroatoms selected from the series O, S, NH.

2. The method according to claim 1, characterized in that put a monolayer of molecules characterized by the formula [Gly4-NHCH2]2C10H20where Gly is a glycine residue.



 

Same patents:

FIELD: chemical industry; methods of manufacture of the composite materials on the basis of the expanded graphite.

SUBSTANCE: the invention may be used at manufacture of the adsorbents, the porous carbon carriers and the metal=containing catalytic agents. The method provides, that first prepare the 1-2 % cellulose solution in the 5-8.5 % sodium hydroxide water solution. The produced solution is mixed with the expanded graphite in the mass ratio of the graphite to the cellulose of (1-2.5) : (2-1) accordingly. The composition prepared this way is carbonize with heating rate of 4°С per a minute up to 600°С maintaining this temperature within 1 hour. To impart the composite material the catalytic and adsorption properties the cellulose solution may be added with 2-5 mass % of the modifying compound of the transition metal in terms of the metal. The invention ensures simplification of the composite material production process, the improvement of its quality due to the homogeneity of allocation of the active carbon in the lower die of the expanded graphite.

EFFECT: the invention ensures simplification of the composite material production process, the improvement of its quality.

2 cl, 2 tbl, 10 ex

FIELD: building materials industry; metallurgy industry; other industries; methods of production of the initial refractory materials and the refractory products manufactured with their usage.

SUBSTANCE: the invention is pertaining to production of the refractory products and may be used in building materials industry, metallurgy industry, other industries for production of the refractory materials and products. The refractory materials are produced by molding the composition, which contains the refractory filler and the initial refractory material with the graphite grains having the average size of 500 nanometers or less, or with the graphite grains produced by the graphitization of the carbonic carbon black. The graphite grains contain at least one component selected from the group consisting of metals, boron and silicon. The refractory materials alongside with the refractory filler may contain also the carbon grains (A), selected from the carbonic carbon black and the graphite grains produced by the graphitization of the carbonic carbon black and having absorption - DBP (x) 80 ml/100g or more; the carbon grains () selected from the carbonic carbon black and the graphite grains produced by the graphitization of carbonic carbon black, and having absorption -DBP (x) less than 80 ml/100g. The invention allows to improve the thermal impact stability of the refractory materials, their corrosion resistance and the oxidation resistance.

EFFECT: the invention ensures the improved thermal impact stability of the refractory materials, their corrosion resistance and the oxidation resistance.

19 cl, 7 ex, 2 dwg, 6 tbl

FIELD: chemical industry; other industries; methods and devices for production of the thermo-extended graphite.

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2 cl, 1 dwg, 1 tbl, 9 ex

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11 cl, 1 dwg, 4 ex

FIELD: metallurgy; semiconductor and aeronautical engineering; manufacture of electrodes, seals for aircraft engines and super clean articles.

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2 tbl, 1 ex

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4 cl, 3 dwg, 1 tbl

FIELD: atomic industry; chemical industry; metallurgy; heat-and-power engineering; production of the oxidized black lead.

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22 cl, 4 dwg, 2 tbl, 2 ex

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1 ex

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17 cl, 2 dwg, 3 tbl, 5 ex

FIELD: chemical industry and special-purpose technique; manufacture of large-sized blanks of shaped articles for chemical and heat-exchange apparatus.

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3 cl, 3 ex

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EFFECT: increased covering quality due to increased strength and powdered paint adhesion with article surface to be covered.

1 tbl, 6 ex

The invention relates to a method for processing untreated metal surface

The invention relates to a device for applying liquid adhesives and sealants product and can be used in various technological processes, in particular in the manufacture of double-glazed Windows and other structural elements

FIELD: sorbents and water treatment.

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7 cl, 2 tbl, 10 ex

FIELD: chemical industry; sanitary cleaning of gas ejection.

SUBSTANCE: chemical absorber can be used for dry rendering gas mixtures harmless. Chemical absorber has timber chips processed by mixture of hydroxide water solution and sulphur-containing salt of one or more alkali metal. Degree of oxidation of sulphur in sulphur-containing salt doesn't exceed +4. Content of alkali metal hydroxide in absorber equals to 10-40 mass percent; content of sulphur is absorber equals to 1,5-6,5 mass percent. Timber chips used in absorber have thickness less or equal to 1 mm, width of 2 mm and wider and length of 50 mm and longer. To prepare chemical absorber, timber chips are soaked in hydroxide and sulfite and/or thiosulphate of alkali metal solution, kept in till swelling, impregnated and are subject to drying.

EFFECT: reduced cost.

8 cl, 3 tbl

FIELD: chemical industry; sanitary cleaning of gas ejection.

SUBSTANCE: chemical absorber has base of timber chips processed by hydroxide water solution of one and more alkali metal till achieving alkali metal content in absorber up to 10-50 mass percent. Timber chips have thickness less or equal to 1 mm, width of 2 mm and wider and length of 50 mm and longer. To prepare chemical absorber, timber chips are soaked in solution, kept in till swelling, impregnated by alkali agent and are supposed to drying till achieving humidity of 10-15 mass percent. Absorber is capable of catching HF, SO2, CO2, HCl and other sore gases.

EFFECT: reduced cost.

5 cl, 3 ex, 4 tbl

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EFFECT: possibility of producing materials at varying properties due to performance of process in wider range of polarization potentials.

4 cl, 1 tbl, 15 ex

FIELD: water treatment and sorbents.

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EFFECT: achieved combination of high sorbent capacity and good sorbent workability parameters, namely high filterability and strength caused by hardened surface layer on granules.

7 cl, 3 tbl

FIELD: liquid waste treatment.

SUBSTANCE: invention provides complexion structure containing conducting or semiconducting substrate, to which organic polymer film is grafted containing monomer selected from 4-vinylpyridine and vinylbipyridine plus cross-linking agent, namely divinylbenzene. Preparation method includes step, in which above electrically neutral organic polymer is grafted, said polymer being able of complexion ions via electropolymerization while electric grafting is performed on conducting or semiconducting substrate in presence of above cross-linking agent.

EFFECT: enhanced waste treatment efficiency.

2 tbl, 9 ex

FIELD: gas-treatment materials.

SUBSTANCE: invention relates to sorption engineering, particularly to process gas drying processes and to individual and collective respiratory apparatus protection systems. Proposed method comprises impregnation of silica gel with aqueous solution containing 380 g/L calcium chloride and 480 g/L lithium bromide at solution temperature 10-20°C and ratio of silica gel pore volume to solution volume 1:(0.9-1.0); stirring for 15-20 min; drying at 300-450°C for 0.8 h; screening and recovery of fraction with granule diameter 1.0-3.0 mm.

EFFECT: increased strength and workability of drier.

1 tbl, 3 ex

FIELD: polymeric sorbents.

SUBSTANCE: invention provides complexing sorbent containing active polymer layer condensed with complexons and immobilized on a solid support selected from the following group: .epoxated cellulose, styrene/divinylbenzene copolymers, activated with chloromethyl, hydroxymethyl, sulfone chloride groups, and sulfone group-activated phenol-formaldehyde resins. Active sorption layer contains ethylenediamine or diethylenetriamine, or triethylenetetramene, or polyethylenepolyamine with copolymers, whereas complexons are selected from group including carboxyl-containing complexons, hydroxyl-containing complexons, and phosphone-containing complexons.

EFFECT: enabled sorption of unlike-valent ions of a variety of metals from aqueous solutions within a wide pH range and regeneration of sorbent by treatment with dilute mineral acid.

18 cl, 1 dwg, 2 tbl

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