Method of coloring fianites

FIELD: jewelry industry; optics.

SUBSTANCE: proposed method is used for coloring fianites (man-made diamonds) in green, blue and brownish-yellow colors; proposed method may be also used in optics for production of colored light filters withstanding temperatures above 1000°C. Proposed method includes preliminary application of cobalt on fianite surface to be colored and at least one metal whose oxide is liable to spinelle-forming with oxide of bivalent cobalt, iron and/or aluminum, for example. Then material is subjected to heat treatment in oxygen-containing atmosphere at temperature above 1000°C but not exceeding the fianite melting point. The procedure is continued for no less than 3 h. Coat is applied by thermal spraying of metals in vacuum. Said metals may be applied in turn and simultaneously. For obtaining bluish-green color of fianite, cobalt and aluminum are applied at atomic ratio of 1:1 to 1:2. For obtaining yellowish-green color, cobalt, aluminum and iron are applied at atomic ratio of 1:1 :0.1-0.2. For obtaining yellowish-brown color, cobalt and iron are applied at ratio of 1:1 to 1:2.

EFFECT: enhanced resistance to high temperature and chemical action.

7 cl, 11 ex

 

The invention relates to the field of processing synthetic refractory shaped crystals, in particular of pave rhinestone (crystal based on zirconium dioxide and/or hafnium, stabilized by yttrium oxide). The invention can be used in the jewelry industry for dyeing inserts, imitating precious stones, green, blue, and brown-yellow color and optics for color filters that can withstand temperatures above 1000°C.

Known way to change the color of gemstone jewelry [U.S. Patent No. 5981003, IPC And 44 C 17/00, op. 09.11.99, No. 6146723, IPC A 01 N 1/00 A 01 N 3/00, A 41 G 3/00, A 41 G 5/00, B 44 F 7/00, op. 14.11.00], which consists in applying on a faceted crystal transparent coating of permanent water color ink, soluble in alcohol, which you can change the color of the stones.

The method allows to obtain jewelry stones, including rhinestone beads, any color.

The disadvantage of this method is the instability of the resulting color, grated in the process of wearing, soluble in alcohol and decomposing at elevated temperatures. As a result, when manufacturing jewellery, founding together with inserts, color is not saved. The method cannot be applied in the manufacture of filters used at high temperatures.

Known method for improving the quality of precious stones [Pat the NT of the Russian Federation No. 2083149, IPC And 44 With 17/00, op. 10.07.97], which consists in alloying stones from aqueous solutions of soluble salts containing the ions of the p-, d-elements, such as bismuth, lead, neodymium, chromium, at concentrations of 0.0001 0.002 wt.% by irradiation optical quantum generator with an energy of about 1 j in the free-running mode with a pulse duration of 0.001 and with varying frequency radiation.

When 10-fold exposure rhinestone beads in an aqueous solution of divalent Nickel sulfate and ferric nitrate neodymium is achieved purple crystals.

The disadvantages of this method are the complexity and high cost of the necessary equipment, as well as the impossibility of obtaining a wide range of blue-green and yellow-brown color.

There is a method of imparting colors of precious natural stones [U.S. patent No. 6872422, IPC 23 16/00 C, With 30 In 29/10, published. 29.03.05], which includes a coating of a precious stone one or more dye layers in a thin film and subsequent heat treatment at a temperature of from 700°With up to 1200°C for from 30 minutes to 10 hours in air or in oxygen atmosphere. When precious stones are Topaz and sapphire, i.e. stones, which include aluminum, forming spieleabend oxides with transition metals. In the coloring layers are layers of cobalt, cobaltates the materials, iron, ferrous materials, chromium, chromium materials in any combination in order to obtain stones of different colors and shades.

A known method can be painted precious natural stones, namely, topazes and sapphires in blue, green, yellow-orange and orange-red color, getting chemical and temperature-resistant color.

The known method is not suitable for dyeing synthetic stones, including pave rhinestone. The application of this method for coloring pave rhinestone will not allow you to get the blue-green range of coloring pave rhinestone due to the formation of unstable coloring films with recommended coloring layers and modes of treatment.

The closest technical solution to the claimed invention is a method of dyeing crystal jewellery [Copyright certificate №768455, IPC B 01 J 17/34, And 44 C 17/00, op. 07.10.80], which includes coating the surface of the crystal transition element of the iron subgroup or group of rare earth metal deposition and subsequent heat treatment for the solid-phase chemical reactions with the formation of the colored layer.

This method is successfully applicable for dyeing Topaz, corundum, quartz and some other natural and synthetic stones, which include aluminum, obrazowe the spinel with oxides of transition metals, or silicon, forming a transition metal silicon compound. The method allows to paint these stones in yellow-orange color during the deposition of iron and blue-green color during the deposition of cobalt.

However, this method is unable to obtain a stable blue-green, light yellow and brown color of rhinestone beads. For example, the deposition of cobalt or iron on the surface of the cubic Zirconia and the subsequent heat treatment results in turbid coating resistant to abrasion.

The technical problem to address with the inventive method, is to develop technologies coloring pave rhinestone (crystal based on zirconium dioxide and/or hafnium, stabilized by yttrium oxide), producing resistant to high temperatures and chemical attack of the reproducible color in the blue-green (from light blue to dark blue, from pale green to dark-green and green-blue and yellow-brown (from light to dark tea brown and black) colors.

The essence of the invention is a method comprising coating the surface of the crystal transition element of the iron subgroup metal deposition and subsequent heat treatment, according to the invention is applied cobalt and at least one metal oxide which is able to spin is neobrazovannie with oxide of divalent cobalt, for example, iron and/or aluminum, the heat treatment is carried out in an oxygen-containing atmosphere at a temperature of from 1000°With up to a temperature not exceeding the melting temperature of cubic Zirconia, at least 3 hours.

In the particular case of the implementation of the proposed method the coating is applied by thermal spraying of metals in vacuum.

In the particular case of the implementation of the proposed method mentioned metals is applied alternately.

In the particular case of the implementation of the proposed method mentioned metals can cause at the same time.

In the particular case of the implementation of the proposed method to obtain a cubic Zirconia color blue-green spectrum is applied cobalt and aluminum atomic ratio of from 1:1 to 1:2.

In the particular case of the implementation of the proposed method to obtain a cubic Zirconia color yellow-green spectrum is applied cobalt, aluminum and iron, with the atomic ratio of 1:1:0,1-0,2.

In the particular case of the implementation of the proposed method to obtain a cubic Zirconia color yellow-brown scales applied cobalt and iron in atomic ratio of from 1:1 to 1:2.

When implementing the method in the specified set of features is achieved stable reproducible color rhinestone beads in blue-green and yellow-brown tones.

It was established experimentally that in order to obtain transparent coloured and strongly linked with the surface of the cubic Zirconia film is necessary is IMO at least two metals, oxidized during the heat treatment. One of the metals must be cobalt, only because it is capable of forming the transition layer is firmly adhered to the surface of cubic Zirconia. Other damage metals are metals that form with cobalt at the heat treatment in an oxygen-containing atmosphere colored complex spieleabend oxides with the General formula(IU)2About4where Me is one or more metals that form oxides with the formula IU2About3resistant at temperatures above 1000°C. satisfy This condition, for example, iron and aluminum as oxides of aluminum and iron is capable of spinlooptime with oxide of divalent cobalt.

When applied to the surface of the cubic cobalt and at least one metal oxide which is capable of spinlooptime with oxide of divalent cobalt in the solid-phase chemical reactions occurring during thermal treatment, forms a transparent painted film firmly adhered to the surface of cubic Zirconia and give it the desired color. Painted film of spieleubersicht oxide has a melting temperature higher than the melting point of the cubic Zirconia and is not soluble in concentrated acids.

The proposed mode of treatment is determined by the fact that at temperatures below 600-700°With chemicas the second reaction on the surface of the cubic Zirconia is not happening. In the range from 700°With up to 1000°With color film strongly influenced by the inhomogeneity of the temperature field in the furnace, which does not allow to obtain a reproducible color. When the holding temperature of from 1000°and to a temperature not exceeding the melting point of the cubic Zirconia, color cubic Zirconia is determined only by the number and ratio of deposited metals and the thickness of the dye film, and a dye film obtained is transparent and is firmly adhered to the surface of cubic Zirconia.

If the shutter speed is less than three hours coloring film turn cloudy due to incomplete reaction.

The inventive method is as follows. Pre-polished product from a colorless cubic Zirconia, such as jewelry faceted box, carefully cleaned. On the rear surface (the pavilion) paste is applied by thermal spraying in vacuum cobalt and, for example, iron and/or aluminum. Moreover, the deposition of metals may be performed serially or in parallel. The use of thermal spraying in a vacuum provides a smooth painted surface, do not require further polishing. The thickness of the dye film set amount of sprayed metal with precision weighing not worse than 0.2 mg in weight from 5 to 150 mg. Heat treatment is carried out in three stages: heating, the extract is cooled, endurance exercise at least 3 hours at a temperature of from 1000°With up to a temperature not exceeding the melting temperature of cubic Zirconia depending on the desired color of rhinestone beads.

In order to conserve power and extend the service life of the furnace, it is advisable to limit the temperature of the heat treatment 1300°C.

Example 1.

As the sample was used jewelry box from colorless cubic Zirconia with a pre-treated surface. Thermal spraying in vacuum on the rear surface (the pavilion) insert caused a layer of cobalt thickness of 7.8 nm and a layer of aluminum of a thickness of 23 nm (atomic ratio 1:2). The thickness of the metal layers is a calculated value, it asked a number of sprayed metal. The heat treatment is conducted in air, the heating is carried out in a furnace with a heating rate of 10°C/min up to 1100°C, held at this temperature for 3 hours, cooled at a rate of 10°C/min to 100°C, after which the sample was taken out from the oven.

The treated sample has a uniform pale sky-blue colour, resistant to abrasion, exposure to concentrated acids and high temperatures.

Example 2.

The sample, as in example 1. But the thickness of the layer of cobalt 33 nm, and a layer of aluminium of a thickness of 100 nm. Exposure was carried out at a temperature of 1050°C for 5 hours. The treated sample has a uniform steady intense the ate blue color.

Example 3.

The sample, as in example 1. The thickness of the layer of cobalt 6.7 nm, and a layer of iron - 14 nm (atomic ratio 1:2). Heat treatment as in example 1. The treated sample has a uniform steady bright tea color.

Example 4.

The sample, as in example 1. A layer of cobalt thickness of 6 nm. Heat treatment as in example 1. The treated sample has a dirty-green color, coloring film loose, easily removed by abrasion.

Example 5.

The sample, as in example 1. The thickness of the layers of cobalt and aluminum, as in example 1 (atomic ratio 1:2). The heat treatment is conducted in air, the heating is carried out in a furnace to 650°C, kept at this temperature for 5 hours. The treated sample has a dirty-green color, coloring film loose, easily removed by abrasion.

Example 6.

The sample, as in example 1. Processed 10 samples. The thickness of the layers of cobalt and aluminum, as in example 1 (atomic ratio 1:2). Exposure was carried out for 3 hours at a temperature of 1350°C. the Treated samples have a uniform steady pale sky-blue colour. However, of the ten processed samples have two cracks.

Example 7.

Same as in example 1, but the thickness of the layers of cobalt and aluminum are 33 and 50 nm, respectively (atomic ratio 1:1). The treated sample has a uniform stable intensive the Yu emerald-green color.

Example 8.

Same as in example 2, but the exposure was carried out for 1 hour at a temperature of 1100°C. the Treated sample is turbid, blue, easily removed from the Erasure color.

Example 9.

Same as in example 2, but the exposure was carried out for 5 hours at a temperature of 950°C. was Treated with 10 stones, located in different parts of the furnace. The treated samples have different color shade between green and blue.

Example 10.

The sample, as in example 1. On the surface of the paste layer applied cobalt thickness of 7.8 nm, a layer of aluminum of a thickness of 23 nm and the iron layer thickness of 2 nm (atomic ratio 1:1:0,2). The heat treatment is conducted as in example 1. The treated sample has a uniform steady bright yellow-green color.

Example 11

As the sample was used plane-parallel disk of cubic thickness of 3 mm On a thoroughly cleansed the surface of the disk caused the cobalt and iron in atomic ratio of 1:2, number of sprayed material is two times more than in example 3. The treated sample has a brownish color and has properties of a neutral density filter with a transmittance of about 5% over the entire visible range. The filter does not change its properties to 1100°C.

1. The method of staining rhinestone beads, characterized in that on the surface is pre-applied in the form coated with the cobalt and I, at least one metal oxide which is capable of spinlooptime with oxide of divalent cobalt, such as iron and/or aluminum, and then in an oxygen-containing atmosphere are heat treated at temperatures above 1000°With, but not exceeding the melting point of the cubic Zirconia, at least 3 hours

2. The method according to claim 1, characterized in that the coating is applied by thermal spraying of metals in vacuum.

3. The method according to claim 1 or 2, characterized in that the said metal is applied alternately.

4. The method according to claim 1 or 2, characterized in that the said metal is applied at the same time.

5. The method according to claim 1, characterized in that cause cobalt and aluminum atomic ratio of from 1:1 to 1:2.

6. The method according to claim 1, characterized in that cause cobalt, aluminum and iron, with the atomic ratio of 1:1:0,1-0,2.

7. The method according to claim 1, characterized in that cause cobalt and iron with an atomic ratio of from 1:1 to 1:2.



 

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