Immersion liquid

FIELD: chemistry.

SUBSTANCE: invention relates to an immersion liquid which can be used in optical instrument-making for investigating optical parameters of inorganic materials and optical components, including large, irregularly shaped articles. The immersion liquid for optical investigation contains 97-99 wt % meta-bis(meta-phenoxyphenoxy)benzene and 1-3 wt % 2-naphthol. To reduce viscosity and surface tension, the immersion liquid may further contain 0.1-3 wt % dibutyl sebacate per 100 wt % of said composition.

EFFECT: disclosed immersion liquid is nontoxic, has a good refraction index nD>1,6 and high adhesion to inorganic optical materials, which enables to deposit on the entire surface of the investigated substrate or part thereof a thin immersion layer and use thereof for effective quality control of large optical articles without immersion in a cell with an immersion liquid.

2 cl, 2 dwg, 2 tbl, 2 ex

 

The invention relates to applied chemistry and can be used as an immersion liquid in an optical instrument for monitoring optical parameters of inorganic materials and optical components, including large complex-shaped products.

Known immersion liquid on the basis of white phosphorus, methylene iodide, organic solvents β-bromonaphtalene, bromoform, decaline, tetraline, which have a high refractive index (1.5) (Handbook of chemistry, I. 4, M-L.: Chemistry, S. 821). The disadvantages of these fluids is their high toxicity, extreme toxicity, explosiveness and high cost.

Known with high refraction liquids Meirovitch (Geological dictionary. - M.: Nedra. Edited by K. N. Paffenholz and others, 1978, T. 1, 486 C.) selenium Se, sulphide of arsenic As2S3, bromide arsenic AsBr3and methylene iodide CH2I2and the immersion liquid based on methylene iodide CH2I2containing white phosphorus bromide arsenic AsBr3the sulphide of arsenic As2S3, sulfur, tin iodide SnI4and antimony iodide SbI3. These fluids are highly toxic and rapidly decompose under the action of light.

Known more cheap and safe liquid on the basis of the iodides of the metals. For example, an aqueous solution jodidamente and cadmium chloride and zinc, with a maximum refractive index of n D=1.625 (USSR Author's certificate N 948994, NC: C09K 3/00 and G01M 11/00, published 07.08.1982). But when a sufficient stability of this liquid it is not possible to obtain a higher refractive indices simultaneously with large viscosities.

Known less stable fluid in the form of an aqueous solution of iodide of zinc with a refractive index of nD=1.64 (RF Patent No. 2051940, NC: C09K 3/00, G02B 1/06 and G01M 1/00, published 10.01.1996), the viscosity of which is achieved large values of (8.1 relative to water). But the downside of this fluid is the fragility maintain its high optical properties. After a few days in liquid complexes are formed, changing its optical properties.

Known technical solutions closest to destination and technical nature of the claimed object is immersion liquid for optical studies containing iodide of cadmium CdI2the sodium iodide NaI and water that is described in the patent of the Russian Federation 2134708, NC: C09K 3/00 and G02B 1/06 published 20.08.1999. The patent States that liquid stable, low-toxic, easily washed off with water, has a high refractive index. At the maximum refractive index of nD=1,66 density of the liquid is equal 2,787, and the relative viscosity has a value of 7.7.

Immersion liquid, which can be used to control Krupnov baranich parts of the modern single crystals, optical glasses or ceramics (such as optical parts made of synthetic sapphire, alumomagnesium spinel, yttrium aluminium garnet, various glasses, and others), must meet the following requirements:

1) have a high (n>1,6) refractive index and high transparency in the visible part of the spectrum;

2) to have high adhesion to the surface of the inorganic optical materials;

3) immersion liquid and its components must be non-toxic;

4) possess a high boiling point and low vapor at room temperature.

Immersion liquid, is described in the patent of the Russian Federation 2134708, has significant drawbacks - high toxicity (the presence in its composition of iodide of cadmium CdI2), it also allows you to get a thin layer on the surface of the test object with the necessary uniformity and stability properties at the time of testing (due to water evaporation).

The present invention is to create a non-toxic with high refraction immersion liquid having a high adhesion to inorganic optical materials. This allows you to get on the surface of the tested materials and products thin layers immersion without putting large items in the cuvette with the immersion liquid. The absence of toxic components PR the environmental safety of the proposed use of the immersion liquid.

New immersion liquid to control large with high refraction of optical materials and products contains high-boiling, viscous organic compounds.

The technical result is achieved by using as the immersion liquid mixture of meta-bis (meta, phenoxyphenoxy) benzene with 2-naphthol. The chemical composition of the immersion liquid (wt.%):

meta-bis(meta, phenoxyphenoxy)benzene97-99;
2-naphthol1-3

To reduce the thickness of the layer of immersion that is applied to the material, it is necessary to reduce the viscosity and surface tension of the liquid without changing its refractive index. For this purpose, the composition of the immersion liquid may additionally be injected 0.1 to 3 wt.% dibutylsebacate (over 100%).

The refractive index of the immersion liquid in the visible part of the spectrum is 1,63-1,64. Both fluids are characterized by high evaporating temperatures (Tinstrumentation·(1)>360°C; Tinstrumentation·(2)>290°C) and low values of the elasticity of steam (≤5 10-7mm Hg) at room temperature, which determines the absence of evaporation of the immersion liquid. This ensures the stability properties of the layer immersion the first liquid and the absence of unpleasant odors and toxic fumes in the process of testing optical materials. The introduction of the material 2-naphthol stabilizes the structure and properties of the material.

The mere fact that the introduction of the immersion liquid aromatic hydrocarbons does not provide a significant increase in the refractive index of the liquid. So, for example, U.S. patent No. 4465621 describes the immersion liquid, consisting of butyl benzyl phthalate, mixed with diallylphthalate and/or chlorinated paraffin, and having a refractive index in the visible part of the spectrum only 1,49-1,53.

In the description of U.S. patent No. 4832855 immersion liquid based on dialkylamide ester of phthalic acid and chlorinated paraffin has a refractive index to the visible part of the spectrum in the range 1,50-1,60. However, in the examples described in this patent, the values of the refractive index of the immersion liquid does not exceed 1,52.

To obtain a thin layer on the surface of the test material immersion liquid is applied by brush or swab, and when diluted volatile solvent (e.g. acetone) by spraying. After applying a layer of immersion liquid on the ground or frosted surface of the test specimen while scanning can be defined inclusions, bubbles, cords and other defects in the material volume.

Developed immersion liquid may also be used in mi is roscopy when creating immersion lenses.

In Fig.1 shows a photograph of a polished slice of a crystal of gallium-scandium-gadolinium garnet without immersion liquid.

In Fig.2 shows a photograph of a polished slice of a crystal of gallium-scandium-gadolinium garnet coated with a new layer of immersion liquid.

Example 1

Manufactured immersion liquid by mixing at room temperature components under item 1 of the formula at different ratios. Chemical composition and properties of liquids are given in table 1. Without additives modifying component (2-naphthol) the main component of the immersion fluid - meta-bis(meta-phenoxyphenoxy) benzene - prone to spontaneous crystallization transition in the gel state and the loss of high optical homogeneity. The introduction of the immersion liquid 1-3 wt.% 2-naphthol stabilize its structure and allows to obtain a highly homogeneous transparent viscous composition having a high refractive index (nD>1,6). Experiments have also shown that the introduction of the immersion liquid than 3 wt.% 2-naphthol leads to its dimness.

Table 1
Chemical composition and properties of the immersion fluid.
Chemical composition, wt.%The properties of the immersion liquid
meta-bis(meta-phenoxyphenoxy)benzene2-naphtholAppearanceThe refractive index, nDViscosity, SP
1100,0-Inhomogeneous gel-like substance--
299,01,0Viscous transparent liquid1,6333600
398,02,0Viscous transparent liquid1,6363480
497,03,0Viscous transparent liquid1,6403410
596,04,0 Turbid liquid--

Example 2

Manufactured immersion liquid by mixing at room temperature components under item 2 formulas for different ratios. Chemical composition and properties of the fluids are shown in table 2.

Table 2
Chemical composition and properties of the immersion fluid.
Chemical composition, wt.%The properties of the immersion liquid
meta-bis(meta-phenoxyphenoxy)benzene2-naphtholDibutylsebacate (over 100%)The refractive index of nDViscosity, SP
199,01,0-1,6333600
299,01,021,6332400
399,01,031,6331300
499,01,041,623700

The table shows that the introduction of the immersion liquid supplements dibutylsebacate up to 3 wt.% (over 100%) leads to a significant reduction of its viscosity, the value of the refractive index is almost unchanged. The introduction of this additive in the amount of more than 3 wt.% leads to an undesirable decrease of the refractive index of the immersion liquid.

Example 3

Developed immersion liquid can be used to control the optical homogeneity of products made of different optical materials. As a subject was selected crystal gallium-scandium-gadolinium garnet (GSGG). From crystal boules GSGG having a cylindrical shape, cut the sample in the form of a plate thickness of 3 mm, the Opposite ends of the sample were polished. Immersion composition was applied with a swab on the polished end surface of the sample crystal. The sample was placed between crossed Polaroids, allowing to visually observe the distortion of analogo front, due to the presence in the sample of the external phase, smiley or stress.

Comparison of the images shown in Fig.1 and 2, demonstrates the high effectiveness of the developed immersion fluid for quality control of optical elements.

1. Immersion liquid for optical studies with meta-bis(meta-phenoxyphenoxy)benzene and 2-naphthol in the following ratio, wt. %:

meta-bis(meta-phenoxyphenoxy)benzene97-99
2-naphthol1-3

2. Immersion liquid under item 1, characterized in that it further contains 0.1 to 3 weight. % dibutylsebacate in excess of 100 weight. % the composition of the immersion liquid on p. 1.



 

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