Method of producing nanocomposite based on liquid crystal polymer matrix and inorganic semiconductor

FIELD: chemistry.

SUBSTANCE: invention relates to polymer composite materials, particularly a method of producing a nanocomposite based on a liquid crystal polymer and an inorganic semiconductor which can be widely used in laboratory experiments and in industry. The invention discloses a method of producing a nanocomposite which involves mechanical treatment of a solution of a liquid crystal polymer of the type poly-4-(n-acryloyloxyalkoxy)benzoic acid of formula: , where n=3-12, until interchain bonds of the polymer break.The solution is mixed with nanoparticles of the inorganic semiconductor coated with a low-molecular weight organic ligand which contains the same functional group as the polymer and is selected from a group of fatty acids. The obtained mixture is held, chemically bonded nanoparticles are formed and separated and the solvent is distilled off. The inorganic semiconductor used is cadmium selenide, cadmium sulphide or lead sulphide. The fatty acid used is oleic or palmic or linoleic acid.

EFFECT: disclosed method enables to obtain nanocomposites based on liquid crystal polymers which contain nanoparticles of inorganic semiconductors which are included in the volume of the composite in an ordered manner.

2 cl, 4 dwg, 3 ex

 

The invention relates to methods of preparation of polymer composite materials, and specifically to methods for mixed compositions of polymers with inorganic semiconductors, and more specifically to the nanocomposites based on the polymer liquid crystal matrix and nanoparticles of inorganic semiconductors, and can be used in laboratory research and in industry, manufacturing of polymer composite nanomaterials.

Known methods for producing compositions of polymers with nanoparticles due to direct surface modification of the nanoparticles in a variety of ways, including hydrophobic interaction of polymers with ligands on the surface of the nanoparticles.

Thus, a sufficiently uniform coating of the nanoparticles, macromolecules can be achieved due to the interaction aktiline groups trioctylphosphine acting as a ligand on the surface of the nanoparticles with hydrophobic amorphous areas of amphiphilic polymers described in the works of Gao X, Yang L, Petros JA, Marshall FF, Simons JW, Nie S. In vivo molecular and cellular imaging with quantum dots. Curr Opin Biotechnol 2005; 16:pp.63-72; and Yu WW, Chang E, Falkner JC, Zhang JY, Al-Somali AM, Sayes CM, et al. Forming biocompatible and nonaggregated nanocrystals in water using amphiphilic polymers. J Am Chem Soc 2007;129: 2871-9.

In the work Dubertret B, Skourides P, Norris DJ, Noireaux V, Brivanlou AH, Libchaber A. In vivo imaging of quantum dots encapsulated in phospholipid micelles. Science 2002;298:1759-62 described method of encapsulating nanocast is in a hydrophobic membrane, consisting in the creation of micelles consisting of a mixture of 1,2-dipalmitoyl-glycero-3-phosphoethanolamine-N-methoxy (polyethylene glycol) and 1,2-dipalmitoyl-glycero-3-phospholine. This mixture is characterized by a very complex phase condition, which depends on the composition of the mixture. For example, if 40% of the polymer content of the lipid is formed grafted polymer micelle, forming a hydrophobic coating on the surface of the nanoparticles.

Known methods of creating polymer multidentate ligand coatings on the surface of the nanoparticles, which uses amorphous polymers, characterized by a high density of functional groups. In the work Potapova I, Mruk R, Hubner C, Zentel R, Basche T, A. Mews CdSe/ZnS nanocrystals with dye-functionalized polymer ligands containing many anchor groups. Angew Chem Int Ed 2005; 44:243 7-40 in the conditions of multi-stage reaction of ligand exchange copolymer is a polymer based on poly(N-cryoelectronic) with the amine groups in the side chains of the macromolecules were synthesized chelate complexes with the surface of the semiconductor nanocrystals.

In the work Querner, Benedetto A, Demadrille R, Rannou P, Reiss P. Carbodithioate-containing oligo - and polythiophenes for nanocrystals'surface functionalization. Chem Mater 2006; 18:4817-26 was reported about the method of direct exchange with the mixture of the semiconductor nanoparticles with polymers, such as polythiophenes, for the formation of chelate groups between the surface of nanoparticles and carbothioate groups present in the polymer organic ligand.

The method of "direct polymerization from the surface of the nanoparticles, when the polymerization catalysts are composed of a ligand on the surface, has significant limitations.

For example, anionic or free-radical polymerization incompatible with the chemistry and structure of the nanoparticles. However, in the works of Farmer SC, Patten THOSE. Photoluminescent polymer/quantum dot composite nanoparticles. Chem Mater 2001; 13:3920-6 and Werne T, Patten THOSE. Preparation of structurally well-defined polymer-nanoparticle hybrids with controlled/living radical polymerizations J Am Chem Soc 1999; 121:7409-10 describes how the implementation of the graft polymerization on the surface of the nanoparticles by the mechanism controlled radical polymerization atom transfer and polymerization disclosure cycle, which allows to obtain nanoparticles coated with a polymer "cloud."

The same method, but using a metathesis reaction to obtain nanocomposites nanocomposite on the basis of cadmium selenide and polyolefins described in Skaff H, Ilker MF, Coughlin S, Emrick T. Preparation of cadmium selenide-face composites from functional phosphine oxides and ruthenium-based metathesis. J Am Chem Soc 2002; 124:5729-33.

There are a number of other methods of obtaining compositions of the nanoparticles with polymers, and all of the described methods offer the use of amorphous polymers as coatings or matrices nanoparticles.

Basic common disadvantage of the above methods is the inability to obtain nanocomposites, in which nanoparticle localise the van inside the polymer matrix.

A method of obtaining mixtures of liquid crystalline polymer with quantum dots of cadmium selenide in which the solution of the selenide of cadmium concentration of 10 mg/ml was added dropwise to the polymer solution concentration of 50 mg/ml under stirring at room temperature for 15-20 minutes, planted composite, infusing a solution of 3-fold volume of hexane, washed with hexane and the precipitate is dried under vacuum.

The disadvantage of this method is the absence of operation of the preliminary machining of polymer solution, which contributes to the destruction of cross-links links, which in turn determines the content of nanoparticles in the composite material.

The closest in technical essence to the proposed technical solution is described in the work of E.B. Burmatov, D.A., Pbulk, M.V. Burmatov. New polymer liquid crystal CdS nanocomposites, forming a chiral nematic phase. High-molecular compounds. Series B, 2007, vol 49, No. 2, s-380 and includes a modification of the liquid crystal polymer environment by introducing in the original polymer of at least one semiconductor element with the formation of chemical bonds this item with the molecules of the polymer, the synthesis of semiconductor nanoparticles in a modified polymer medium by passing through it a gas phase containing the rest of the s chemical elements of the semiconductor, and the increasing size of the nanoparticles in the environment to education adsorption links, polymer molecules with the surface of the nanoparticles.

The disadvantage of this method is the destruction of the liquid crystalline phase of the polymer in the inclusion of nanoparticles of semiconductor elements in the polymer matrix at a concentration close to 10% wt., and the lack of organization of the nanoparticles in the polymeric matrix.

The objective of the proposed technical solution is to develop a method of obtaining nanocomposites nanocomposite based on liquid crystal (LC) polymers with ordered structural organization of nanoparticles of inorganic semiconductors volume of the composite when the concentration of the nanoparticles in the composite more than 10% wt.

The solution of this problem is achieved in that in the method of obtaining nanocomposites nanocomposite based on liquid crystal polymer matrix and inorganic semiconductor, comprising the binding molecules of the polymer with the surface of the nanoparticles of inorganic semiconductor, a solution of a liquid crystal polymer of a number of poly-4-(acryloyloxyhexyloxy)benzoic acid of General formula:

,

where n=3-12,

the molecular mass Mw=3 0000-40000,

mechanically treated to the destruction of the cross-links of links of the polymer, followed by mixing with the nanoparticles reorgan the ical semiconductor, selected from the group comprising cadmium selenide, cadmium sulfide or lead sulfide, pre-coated low-molecular organic ligand containing the same as the polymer, a functional group selected from the group of fatty acids, further maintaining the liquid mixture to the displacement of the ligands with the formation of chemically related nanoparticles, by selecting them from the solution and distillation of the solvent. As fatty acids are used oleic or palmitic, or linoleic acid.

The essence of the method consists in creating such a mode of processing of the initial liquid crystal polymer in solution, which provides steric availability and reactivity of the surface of the nanoparticles, modified with low molecular weight ligands, functional groups of the macromolecules of the polymer located in strict accordance with the structure of an LCD phase polymer.

The result of this treatment, the polymer in solution, it is possible to carry out the substitution reaction of molecules of low molecular weight ligand molecules of the polymer, ensuring the formation of chemical bonds between the polymer molecule and the surface of the nanoparticles.

The first feature is that the solution is a liquid crystal polymer, the molecules of which include at least ar is a functional group, capable of forming a chemical bond with the surface of inorganic nanoparticles, after dissolution of the polymer is subjected to mechanical treatment in terms of long-term mixing (at least 2 hours) or ultrasonic mixing for breaking cross-links links.

The lack of long-term mechanical effects leads to the impossibility of breaking most of the cross-links the links that you need to ensure reaction between the functional groups of the polymer and the surface of the nanoparticles, allowing the implementation of more than 10% wt. the nanoparticles in the composition of the material.

The second feature is that the nanoparticles pre-covered with a sheath of low molecular weight organic ligands containing the same functional group as liquid crystal polymer. Otherwise, it is impossible to carry out the substitution reaction of low molecular weight ligand polymer due to the formation of chemical bonds between the surface of the nanoparticles and the functional group of the polymer is localized in the volume of polymer in strict accordance with the structure of the LCD - phase.

The following examples illustrate the proposed solution, but in no way limit its scope.

Obtaining a small molecule ligand substituted for pressurizat sudnikovich nanoparticles

Synthesis of semiconductor nanoparticles is carried out according to the method described in Y. Yin, Alivisatos A.P. Colloidal nanocrystal synthesis and the organic-inorganic interface, Nature, vol. 437, No. 7059, p.664-670, 2005.

For example, to obtain the selenide of cadmium in the flask Slanka to 0,83 g (3.0 mmol) of N-tetradecyl phosphonic acid and 7 g of oxide though add cadmium oxide CdO (Aldridge) in an amount of 0.23, the System vacuum, then filled with argon and incubated for 1 hour at 80°C.

In a separate volume dissolve 0.18 g (4.7 mmole) of selenium in 20 ml though. The mixture of cadmium is heated to 340°C until complete complexation of cadmium with N-tetradecyl phosphonic acid, which is fixed on the discoloration of the original dark-red solution, and then cooled to 300°C.

With vigorous stirring in a flask inject 6 ml of selenium with though. After thorough mixing for 1.5 hours at 300°C. the remaining solution of selenium in the amount of 14 ml slowly (at a rate of 10 ml/h) is injected by means of a reciprocating pump.

Nanoparticles clean planting in excess of acetone and centrifugation for 4 minutes. The mother liquor is decanted.

Replacement of low molecular weight ligand though (TOF) by adding 4 mmol of oleic acid, dissolved in heptane heated to 40°C 0.5% Sol nanoparticles with intense peremeci the years. Nanoparticles are planting in excess of a mixture of acetone with methanol and centrifugation for 4 minutes. The mother liquor is decanted.

The CdSe nanoparticles with replaced shell dissolved in hexane. The degree of substitution of low molecular weight ligand controlled by changing the characteristic bands 1378 cm-1/ 1464 cm-1in the IR spectra (figure 1). When casting this part of the spectrum to the baseline are selected relative values D intensity of the bands. Given that net TOF ratio 1378 cm-1/ 1464 cm-1is MX 0.317, you can calculate the molar proportion according to the following formula:

Tomix=x·Koleic acid+ (1-x)·KTOF,

where Koleic acid=D1387/D1464=0,107 (value for oleic acid), KTOR TOF=MX 0.317, then the contents of the PF after substitution will be 15 mol%. and the degree of substitution is 85%.

Substitution of low molecular weight ligands for the sulphides of cadmium and lead, as well as nanorods on their basis, spend the same way.

Obtaining nanocomposites

An essential element of this method is machining of polymer solution under conditions of long-term stirring or ultrasonic treatment for destruction of cross-links links. Nanoparticles were pre-coated with low molecular weight organic shell l is gandow, containing the same functional group as liquid crystal polymer, and dispersed (dissolved) in an organic solvent. In a pre-prepared polymer solution under continuous stirring dropwise added slowly Sol (solution) nanoparticles. In conditions of continuous mixing carry out the substitution of molecules of low molecular weight ligand molecules of the polymer, which form a chemical bond with the surface of the nanoparticles. The resulting mixed solution is added in excess amount precipitator (more than threefold), resulting in a precipitate of a polymer composite with related nanoparticles. The solvent is decanted, the residue is further treated by the precipitator, and then dried.

Preparation of liquid-crystalline polymer

The solution is a liquid crystal polymer for breaking cross-links links machine:

1) in the conditions of long-term mixing (≥2 hours) solution of the polymer in tetrahydrofuran Teflon magnetic maslinica at 300-500 rpm (as described in examples 1, 3)

2) or ultrasonic agitation using an ultrasonic processor UP400S (400 W, 24 kHz) (Hielscher Ultrasonics, Germany) (example 2)

Example 1

150 ml of the solution prepared as described above, the polymer is poly-4-(acryloyloxyhexyloxy)benzo who Inoi acid with a concentration of 1.5 wt.%. in tetrahydrofuran are placed in a conical flask with reflux condenser and Teflon maslinica.

The solution thermostatic at 45°C in an atmosphere of argon while stirring at a speed of 400 rpm for 24 hours. Then add 5 ml of Zola nanoparticles of cadmium selenide CdSe (concentration of 8 wt.%. in toluene)and the mixture is stirred for further 30 minutes

The solvent is distilled off on a rotary evaporator and the residue - nanocomposite - dried under low vacuum for 24 hours.

Get the nanocomposite with the content of inorganic semiconductors volume of the composite 15% wt., orderly distributed in the volume of the composite, as shown by the data of small-angle (left 2) and wide angle (right 2) x-ray scattering. Anisotropy of small-angle scattering reflex from inorganic semiconductor match the orientation of the smectic layers in the polymer matrix.

Example 2

80 ml of the polymer solution of poly-4-(acryloyloxyhexyloxy)benzoic acid with a concentration of 1.5 wt.%. in tetrahydrofuran in a glass round bottom flask placed in an ultrasonic bath with an operating frequency of 24 kHz and a power generator 400 watts. The solution is incubated at room temperature for 60 minutes, after which it add 5 ml of Zola nanoparticles of lead sulfide PbS (concentration of 6 wt.%. in toluene) and the mixture videri is up another 2 minutes

The solvent is distilled off on a rotary evaporator, and the residue, representing the nanocomposite, dried under low vacuum for 24 hours.

Get nanocomposite containing 20 wt.%, in which the nanoparticles are distributed in an orderly fashion in the volume of the composite, as shown by the data of electron microscopy figure 3.

Example 3

100 ml of the polymer solution of poly-4-(acryloyloxyhexyloxy)benzoic acid with a concentration of 1.0% by weight. in tetrahydrofuran are placed in a conical flask with reflux condenser and Teflon maslinica.

The solution thermostatic at 45°C in an atmosphere of argon while stirring at 500 rpm for 18 hours. Then add 3 ml of Zola nanorods cadmium sulfide CdS (concentration 10% by weight. in toluene)and the mixture is stirred for further 30 minutes

The degree of displacement of ligands and formation of chemical bonds between polymer molecules and the surface of the nanoparticles is controlled by IR-spectroscopy on the characteristic bands in the absorption spectrum of the composite.

The solvent is distilled off on a rotary evaporator, and the residue, representing the nanocomposite, dried under low vacuum for 24 hours.

The obtained nanocomposite with the content of the nanoparticles 23% wt. in the composite, as shown by the electron microscopy data in figure 4.

Thus, the proposed sposobnost to obtain nanocomposites based on liquid crystal polymers, containing orderly included nanoparticles of inorganic semiconductors volume of the composite in amounts of more than 10% wt.

1. The method of obtaining nanocomposites nanocomposite based on liquid crystal polymer matrix and inorganic semiconductor, comprising the binding molecules of the liquid crystal polymer with the surface of the nanoparticles of inorganic semiconductor, characterized in that a solution of a liquid crystal polymer of a number of poly-4-(n-acryloyloxyhexyloxy)benzoic acid of General formula:

where n=3-12,
mechanically treated to the destruction of the cross-links of links of the polymer, followed by mixing with nanoparticles of inorganic semiconductor selected from the group comprising cadmium selenide, cadmium sulfide or lead sulfide, pre-coated low-molecular organic ligand containing the same as the polymer, a functional group selected from the group of fatty acids, further maintaining the liquid mixture to the displacement of the ligands with the formation of chemically related nanoparticles, by selecting them from the solution and distillation of the solvent.

2. The method of obtaining nanocomposites nanocomposite according to claim 1, characterized in that the fatty acids used oleic or palmitic, or linoleic acid.



 

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17 cl, 11 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: alunite-type compound particles represented by the general formula (I) and featuring specific value for D75/D25, where D25 is diametre of particles comprising 25% of the total particle amount, and D75 is diametre of particles comprising 75% of the total particle amount at integral curve of particle size dispersion measured by laser beam diffraction method: Ma[Al1-xM'x]3(SO42-)y(OH)z·mH2O (I), where M is at least one cation selected out of group including Na+, K+, NH4+ and H3O+, M' is at least one cation selected out of group including Cu2+, Zn2+, Ni2+, Sn4+, Zr4+ and Ti4+, and a, m, x, y and z comply with the following: 0.8 ≤ a ≤ 1.35, 0 ≤ m ≤ 5, 0 ≤ x ≤ 0.4, 1.7 ≤ y ≤ 2.5, and 4 ≤ z ≤ 7 respectively.

EFFECT: claimed particles of small mean particle size, spherical, disc or hexagonal form and extremely narrow size dispersion.

FIELD: chemistry.

SUBSTANCE: invention relates to a thermosetting resin composition for protective coating semiconductor devices from the effect of the environment. The composition contains epoxy resin - ED-20, filler, polymerisation catalyst - boron compound and a mixture of mono-, di- and polysulphides of 2-tert-butylphenol having the structure:

n=1÷4

in amount of 2.4-4.0% of the mass of the epoxy resin. Proposed also is a method of making a protective coating for semiconductor devices.

EFFECT: invention enables protection of semiconductor articles and microcircuit chips from external effects, including radiation exposure.

2 cl, 2 ex, 2 tbl

FIELD: chemistry, medicine.

SUBSTANCE: invention refers to the new particles of the basic aluminium salt containing the anion of the organic acid and having the following formula (I): Ma[Al1-xM'x]bAzBy(OH)n·mH2O (where M is at least one cation selected from the Na+, K+, NH4+ and H3O+; M' is at least one metal cation selected from the Cu2+, Zn2+, Ni2+, Zr4+, Fe2+, Fe3+ and Ti4+; A is at least one anion of the organic acid selected from the anions of oxalic, citric, malic, tartaric, glyceric, gallic and lactic acids; B is at least one anion of the inorganic acid selected from the sulphate (SO42-), phosphate (PO43-), and nitrate ions (NO31-); and a, b, m, n, x, y and z meet the conditions 0.7≤a≤1.35; 2.7≤b≤3.3; 0≤m≤5; 4≤n≤7; 0≤x≤0.6; 1.7≤y≤2.4 and 0.001≤z≤0.5 respectively). The particles have the form of the grains, paired particles, rectangular parallelepipeds, disks (having the form of the Go stones), hexagonal plates, rice grains or cylinders with their diametre being constant. The invention refers also to the method of these particles preparation, to the additive to the polyethylene or polypropylene, to polymer resin containing these particles, to the polymer resin composition containing the additive with mass ratio additive/polyethylene or polypropylene (0.5-90):100, to the adsorbent consisting of these particles, to the colorant carrier and to the UV light absorber consisting of the particles of basic aluminium salt.

EFFECT: enhancing of the transparency and tensile strength.

20 cl, 16 ex, 12 tbl, 32 dwg

FIELD: chemistry.

SUBSTANCE: present invention refers to fibre dull polish ensured by mixed mineral additives in raised polymer thermoplastic compositions. Associated mineral additives contain at least two mineral additives chosen from the group containing zinc sulphide, titanium dioxide, barium sulphate, silicon dioxide, alumina, kaolin, calcium carbonate, calcium sulphate, mat clay. The polymer composition for product spinning as filaments, fibres, filament fibres contains associated mineral additives 2 wt % to 4 wt %.

EFFECT: high dulling factor of thermoplastic polymers.

16 cl, 2 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: moulding from polymethymethacrylate matrix contains a soluble fluorescent dye and a light diffusing agent with a difference of the refractive index of light and the refractive index of polymethylmethacrylate matrix from +/- (0.003 to 0.2) and an additional white pigment, containing a difference of the refractive index of light and refractive index of polymethylmethacrylate matrix from + (0.4 till 1.5) on the concentration from 0.001 to 0.1 wt %. The moldings proposed can be used for car bodies, furniture, index boards and devices of illuminated signs.

EFFECT: obtaining molding with improved brightness of colour.

22 cl, 2 tbl

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