Antireflection optical multi-layer coating

 

The invention relates to the manufacture of optical elements, reflective interference filters and surface treatment of glass, and more particularly to layered products, including the basis of glass and multilayer coating of the specified material having a different composition from organic material, oxides, metals and nonmetals, caused mainly by deposition from the gaseous environment. Antireflection optical multi-layer coating is made with alternating layers with high and low refractive indices. At least one of the alternating layers are made of nanostructured carbon, which is composite and contains distributed in the volume of pores with a size of 1-10 nm in the total amount of 10-60%, or multi-layer, made of amorphous carbon sp and/or sp2 and/or sp3-hybridized States, and nanostructured carbon layer additionally contains related atoms from the series: hydrogen, oxygen, fluorine, nitrogen. The proposed solution allows to obtain more functional, technological interference coating on equal substrates, smaller thickness and without increasing the reflectance. Coating the nature of geloina structure consists of one carbon material, what determines the absence of diffusion processes on the boundary components of the nanolayers. 1 S. and 2 C.p. f-crystals, 10 ill.

The invention relates to the manufacture of optical elements, reflective interference filters and surface treatment of glass, and more particularly to layered products, including the basis of glass and multilayer coating of the specified material having a different composition from organic material, oxides, metals and nonmetals, caused mainly by deposition from the gaseous environment.

The level of this technology characterize multilayer antireflection coating formed on optical substrates, lenses, prisms and glass for the Windows of the buildings, which are applied directly or on the metallic functional layer, which provides high heat reflecting capacities, and contain alternating layers of low and high refractive indices, which reduces the reflection from the coating as a whole (see US patents 6172812, G 02 In 005/28, 2001; 6238781, 32 In 017/04, 2001; 6280848, 32 In 017/06, 2001; 5306547, NAT. class. 428/213, 1994; 4985312, 428/627, 1991).

These analogues aimed at addressing targets to achieve private effect and are not universal Kaiku matching characteristics of the proposed coating is described in patent US 6139968, 32 In 017/00, 2000, multilayer ar coating (see Fig.1), is performed on the substrate P with alternating layers of A titanium oxide having a high refractive index and layers with a low refractive index of SiO2, MgO, Al2O3etc. This coating contains more than 30 alternating layers, which provides 3% reflection and 97% transmittance of incident light.

Known coating can be deposited on glass, plastic, semiconductor and metal substrate is used as an anti-reflective and anti-reflective coatings for displays, light-emitting devices, solar cells, optical filters and the like.

A disadvantage of the known antireflection coating is the technological complexity of manufacturing the layered structure of different physical characteristics and optical parameters of materials to achieve high reflectivity, which defines a relatively large thickness of the multilayer coating, limiting the practical application of performance and consumer cost.

Objective behind the present invention is the elimination of the marked shortage, and the thickness without increasing its reflectivity.

The required technical result is achieved by the fact that in the known optical multilayer antireflection coating with alternating layers with high and low refractive indices, according to the invention at least one of the alternating layers are made of nanostructured carbon, that is, a multilayer or composite, which contains distributed in the volume of pores with a size of 1-10 nm in the total amount of 10-60% and is made of amorphous carbon sp and/or sp2 and/or sp3-hybridized States, and nanostructured carbon layer additionally contains related atoms from the series: hydrogen, oxygen, fluorine, nitrogen.

Distinctive features provide nanostructured carbon layer refractive indices of 2.6 or 1.2, which are respectively more and less range (2,4-1,4) refractive indices of the materials, which allows to significantly reduce the overall thickness of the antireflection multilayer coatings in comparison with the known prototype, with equal bandwidth, the minimum reflection coefficient.

The execution layer antireflection multilayer coatings of nanostructured carbon in the form of cher the e and the volume of pores with a size of 1-10 nm in the total amount of 10-60% provides increase or decrease the total refractive index of the coating as a whole for the limit values of known materials, that can multiply to reduce the thickness of the coating, reducing its value when expanding technological possibilities of use.

The implementation of the nanostructured layer of amorphous carbon SP and/or s2 and/or s3-hybridized state allows to simplify the technology of manufacture of antireflection coatings by plasma deposition from the gas phase, characterized by the constancy of performance of the assignment with different physical modes of operation of the coating, since the whole multilayer structure is composed of one carbon material, which determines the absence of diffusion processes on the boundary of the nanolayers.

Execution of nanostructured (s) layer (s) antireflection coating comprising atoms of hydrogen, oxygen, fluorine, nitrogen, which precipitated from the gas phase with a pre-selected quantitative ratio with carbon allows for more control values of the refractive index.

The invention allows thus to expand the technological capabilities of manufacturing antireflection coating with an adjustable value in more or less well-known range of values of the coefficient of prelamin is my energy and reducing its thickness, it can be used for coating of deformable surfaces, in particular, a flexible film substrate materials.

The new coating is characterized by a decrease in roughness and, most importantly, a manifestation of the bactericidal properties, which extends the operational capabilities and the scope of its use.

Therefore, every significant topic are needed, and their combination is sufficient to achieve the novelty of quality as a new effect of amounts that are not inherent characteristics of dissociation.

The invention is illustrated in the drawing, which schematically:

in Fig.1 - coating of the prototype with alternating layers a and b;

in Fig.2 - technology installation;

in Fig.3 - proposed floor with a multilayered nanostructure layer; and

in Fig.4 - the same, with nanocomposite structure layer In;

in Fig.5 is a graph of the dependence of the reflection coefficient of the proposed coverage from the angle of incidence of the x-ray beam;

in Fig.6 is the same as for the proposed coverage with different periods;

in Fig.7 is a graph of the spectral dependence of the refractive index of nanostructured carbon layers In different thicknesses;

in Fig.8 - dispersive dependence of the coefficient prelamin.10 - the spectral dependence of the reflection coefficient of the coating according to the invention from the wavelength of the incident light.

Experimental setup (Fig.2) includes placed in the vacuum chamber 1 and provided with flaps 2 magnetrons source 3 with a graphite target and ion-beam source 4 mounted on the holder 5 of the processed products, which is connected with the motor 6, the rotation and connected to the RF generator 7. The camera 1 has a detachable Windows 8 and communicates with the system 9 hasenpusch.

Below are examples of specific performance of the proposed coatings on flat glass substrate P.

The processed substrate P through the split window 8 strengthen on the holder 5, after which the chamber 1 is pressurized and vacuum to a residual pressure of 10-5mm RT.article.

Further through the system 9 hasenpusch in the camera 1 serves oxygen to a pressure of 10-1mm RT.article and in the plasma of high-frequency electric discharge excited by a generator 7, carry out the cleaning of the surface of the substrate from residual contamination within 10 minutes. The constant bias voltage on the substrate 200 C.

After completion of the cleaning process chamber 1 is again vacuum to a pressure of 10-5mm RT.article and nabusog source 4 and a magnetron sputtering source 3. The partial pressure of cyclohexane and argon equal to 8 x 10-2mm RT.article.

Then include the sources 3 and 4, set operating parameters, which provide a predetermined difference in the densities of the formed structural layer nanofilms C. Next, open valve 2 sources 3, 4, and simultaneously include the electric motor 6, which make the required number of turns of the holder 5 with the processed substrate P.

After forming the deposition of the coating on the substrate P of the set thickness off the sources 3, 4, the generator 7 and the motor 6, the rotation of the holder 5, the valve 2 will return to its original position, the camera 1 is reported with the atmosphere, and then through the window 8 remove the processed product.

Layers of type a is obtained by precipitation from only one source, 3 or 4, in the described example of the source 3 magnetron sputtering.

Change the thickness of the deposited in the chamber 1 of the layers a and b is provided by regulation of the speed of rotation of the holder 5 so that the passage of the substrate P on the sources 3 and 4 was formed layer And, At a given thickness.

Thus for the experiments were made carbon double-layer interference coating on the substrate P (Fig.3, 4), where the layer And carbon across the ois coatings have different thickness and a large number of nanostructured carbon films with different parameters, applied consistently with the carbon layers A.

Carbon is a unique element whose atom may form a chemical bond with different types of hybridization, which ensures the existence of materials that consists of only carbon atoms, but with entirely different structures: graphite, sp2-hybridization links carbon atoms; diamond, s3-hybridization links carbon atoms and carbin, SP-hybridization links carbon atom.

Each of these materials has the inherent physical properties, in particular the density of diamond is 3.5 g/CC, and the density of graphite of 2.26 g/cubic cm

When the deposition on the substrate P amorphous carbon ion-plasma method it is possible to provide simultaneous existence in one nanostructured layer of carbon atoms with different types of hybridization in different proportions. As a result, the density of the material layers, and hence the refractive index of amorphous carbon can be controlled by simply changing the percentages between the various hybridized to its conditions.

Unequivocal proof that manufactured nanostructured layer interference coatings shiny 243 nm, 241 nm and 240 nm when the thickness of its constituent films of 5.4 nm and 4.6 nm and 3.6 nm, respectively in a, b, C) from the angle of incidence of the x-ray beam at a wavelength of 0,154 nm, as in the graphs of Fig.5 peaks are present.

The coating of the carbon films produced in the following way. On a quartz substrate P to form two layers in the thickness of 4.7 nm (period patterns with a thickness of 9.4 nm), each of which represents a multi-layer (50 layers) structure of amorphous carbon obtained ion deposition from the gas phase. Then top form similar to the alternating two-layer structure 70 components of the carbon layers with total thickness of 4.7 nm and 2.3 nm (period patterns with a thickness of 7.0 nm), respectively. This is achieved by reducing the partial pressure of cyclohexane to 6X10-4mm RT.article at a constant partial pressure of argon.

When the value of the angles corresponding to the first Bragg peak (Fig.6), the observed maxima of the reflection from the first and second multi-layered structure of the coating. In the second order interference is observed Bragg peak only from the second structure. The practical absence of the Bragg peak from the first multilayer structure is explained by the suppression of the reflection x-ray the interference of the Bragg peak from the first multilayer structure again observed, but disappears Bragg peak from the second multilayer structure. This is confirmed by the ratio of layer thicknesses as 2:1.

Thus, for example, perform a two-layer interference coatings, nanostructured layers which are layered carbon, illustrates the practical implementation of the invention. Repeating the deposition process of the amorphous carbon, you can get any number of such layers in an interference coating that performs the functions of optical enlightening on the substrate P.

At the same time revealed the spectral dependence of the refractive index of the thickness of the formed carbon film (Fig.7), where the thickness of the amorphous carbon layers with 50 films is: a - 200 nm, b - 75 nm, 50 nm, 25 nm, d - 10 nm, s - 4,8 nm. From these graphs it follows that changed not only the absolute values of the refractive indices of the samples, but also the nature of the spectral dependence. Layers with a thickness of more than 50 nm have a strong dispersion curves of the refractive index of the incident energy (a, b, C), while at smaller thicknesses, this dependence becomes weak (g, d) and almost disappears at a thickness of 10 nm. Therefore, if carbon layers of nanometer taxefficient of refraction will be absent (e), what is important when using it and the quality of the interference coating.

To obtain the coating film of amorphous carbon may, for example, by physical sputtering of a solid target, but is more variable and technological represented his deposition in the plasma electric gas discharge of the gaseous carbon-containing environment, because it greatly enhances the properties of the layers In amorphous carbon in the process of their formation. First of all you can use carbon compounds with different types of hybridization chemical bonds of carbon atoms with hydrogen, for example, acetylene (SP-hybridization), benzene (s2-hybridization), cyclohexane and methane (s3-hybridization).

When the atom layers will be formed to contain hydrogen at a concentration that depends on the ratio s/N in the original gaseous substance that also allows us to control the values of the refractive index antireflection coating.

The layers were obtained by magnetron sputtering in different environments (Fig.8): a - C6H12/Ah=1/3; b - C6H12/Ah=1/1, b - C6H12characterized by low refractive index.

It is evident from Fig.8, which shows the dispersion Alsenoy 200 nm, obtained by magnetron sputtering, it is seen that the increase in the content With6H12leads to a decrease of the refractive index due to the high content of hydrogen (40%) and 10% by volume of pores.

The films deposited from the environment with equal content With6H12and Ah, the value of the refractive index decreases to 1.9. The lowest refractive index is 1.35 are films produced in the atmosphere With6H12. In the last two modes, the dependence of refractive index on wavelength is practically absent, which allows their use in the formation of layers In the invention.

Nanostructure composite layers obtained by the alternation of two techniques: magnetron sputtering and ion source with the formation of the two films of equal thickness. Thus the total thickness of the layer is In: a - 3,0 nm, b - 1.5 nm, 1.0 nm and a high refractive index, see Fig.9, which shows that reducing the thickness of the carbon layers in multilayer structures from 3.0 nm to 1.0 nm leads to an increase of the coefficient of refraction and the extinction of its dispersion dependence.

The maximum value of the refractive index is observed in layer thickness equal to 1.0 nm, what about the manufactured optical multilayer antireflection coating, consisting of 4 pairs of carbon alternating layers a and B. One layer pair has a refractive index equal to 1.35, and is a carbon composite containing 40% hydrogen and 10 % by volume of pores, and other nanostructured layer in the pair has a refractive index 2.48 and made of 52 carbon layer thickness of 1.0 nm.

Optical characteristics of this coating is shown in Fig.10, which shows the experimental dependence of the reflectance on the wavelength of the incident light. From this it follows that the minimum value of the refractive index of the proposed coating is 0.2%, much less than in the prototype.

In addition, the hydrogen concentration in the layer of amorphous carbon and the ratio of hybridized state can also be controlled with the help of:

- of a kind used for excitation of the plasma electric gas discharge, direct current, high frequency, electron-cyclotron, and others;

- energy ions affecting growth layer;

- pressure in the vacuum chamber;

- changes in the composition of the working gas environment;

- power deposited in the discharge;

the substrate temperature.

To control the refractive index antireflection coated is 0-60%.

To extend the control range of the refractive index of the formed coating using gaseous carbon compounds, including atoms of oxygen, fluorine and nitrogen.

Therefore, under nanostructured refers to such heterogeneous materials, which are nano-sized (1-10 nm) region different from the rest of the material properties, structure and chemical composition, localized and have clearly defined boundaries.

The main characteristic of composite nanostructured materials is that their properties are not the sum of the properties of their constituent components, i.e. are such exceptional values of the physical parameters that are absent in traditional homogeneous materials, which is defined as the novelty of quality. The present solution provides a more well-known range of refractive indices of adjacent layers of a multilayer interference coatings, namely 1,2 - 2,6 against 1.4 to 2.4 for known materials.

Comparative analysis of the proposed technical solutions to identified analogues of the prior art from which the invention not obvious to a person skilled in to prevedsomeplace conclusion on compliance with the criteria of patentability.

Claims

1. Antireflection optical multi-layer coating with alternate-sustainability of layers having high and low refractive indices, wherein at least one of the alternating layers are made of nanostructured carbon, which is a multilayer or composite containing distributed in the volume of pores with a size of 1-10 nm in the total amount of 10-60%.

2. The floor under item 1, wherein the nanostructured carbon layer is made of amorphous carbon SP and/or s2 and/or s3-hybridized States.

3. The coating on PP.1 and 2, characterized in that the nanostructured carbon layer additionally contains related atoms from the series: hydrogen, oxygen, fluorine, nitrogen.

 

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