Composite artificial colored gem and preparation method thereof

Abstract

The invention relates to a composite artificial colored gemstone and a preparation method thereof. A gemstone and a gemstone B with different colors grow by adopting a Bridgman-Stockbarger method. Comprising the following steps: (1) calculating and accurately weighing raw materials according to the stoichiometric ratio of a gem A, and then uniformly mixing; (2) firstly putting a gem B with a proper size into a crucible, then putting the raw materials uniformly mixed in the step (1) into the crucible, covering a crucible cover, closing a furnace door, vacuumizing, and filling protective gas to standard atmospheric pressure; 3) turning on a heating power supply to heat and keep constant temperature to remove moisture and air in the raw materials, then heating to the melting point of the raw materials, and keeping constant temperature to completely melt the raw materials; slowly descending the crucible, and carrying out gemstone composite growth; 4, the temperature is slowly reduced to the room temperature after growth is finished, and the furnace is opened. The method has the advantages that the high-quality, large-size and multi-color composite gemstone can be rapidly grown, the problems that an existing gemstone is single in color and small in size can be effectively solved, and the grown gemstone is stable in composite interface and not prone to cracking and has good economic value.

Description

Technical Field

[0001] The invention relates to a composite gemstone and a preparation method thereof, in particular to a composite artificial colored gemstone and a preparation method thereof, belonging to the technical field of crystal material preparation. Background Art

[0002] In the prior art, the main methods for growing colored gemstones include flame method, Czochralski method, hydrothermal method, etc., but the grown gemstones are mostly single color and small in size. Inlay and other processes are often used to diversify the colors, but due to the high hardness of gemstones, the processing cost is high.

[0003] Consider using the crucible descent method to prepare colored gemstones. The crucible descent method is often used for single crystal growth, usually to produce large-sized single crystals. The material for single crystal growth is placed in a cylindrical crucible, slowly descends, and passes through a heating furnace with a certain temperature gradient. The furnace temperature is controlled to be slightly higher than the melting point of the material. According to the properties of the material, the heating device can be a resistance furnace or a high-frequency furnace. When passing through the heating area, the material in the crucible is melted. When the crucible continues to descend, the temperature at the bottom of the crucible first drops below the melting point and begins to crystallize. The single crystal continues to grow as the crucible descends. Summary of the invention

[0004] The present invention provides a composite artificial colored gemstone and a preparation method thereof, the purpose of which is to overcome the above-mentioned deficiencies in the prior art and realize the artificial preparation of the composite colored gemstone.

[0005] The technical solution of the present invention is: a composite artificial colored gemstone, which is composed of A gemstone and B gemstone of different colors and is grown by a crucible descent method.

[0006] A method for preparing a composite artificial colored gemstone comprises the following steps: Step 1) Calculate and accurately weigh each raw material according to the stoichiometric ratio of gemstone A, and then mix them evenly; Step 2) Place the B gemstone of appropriate size in the crucible, then put the mixed raw materials in step 1) into the crucible, cover the crucible, close the furnace door and evacuate to 0-10 -2 Pa, fill the protective gas to standard atmospheric pressure; Step 3) Turn on the heating power and raise the temperature to 200°C, keep the temperature constant for (1-5) hours to remove moisture and air in the raw materials, then raise the temperature to the melting point of the raw materials and keep the temperature constant for (5-10) hours to completely melt the raw materials; slowly lower the crucible at a speed of (0.2-2) mm / h to carry out gem composite growth; Step 4) After the growth is completed, the temperature is slowly cooled to room temperature at (10-40)℃ / h, and the furnace is opened to obtain a composite artificial colored gemstone.

[0007] Preferably, the A gemstone and the B gemstone are ruby ​​and colorless sapphire respectively, the doping concentration of chromium ions in the ruby ​​is 1%, and the colorless sapphire is Al2O3 crystal.

[0008] Preferably, the stoichiometric ratio of ruby ​​in step 1) is 1% Cr:Al2O3, and in step 2) the furnace door is closed and the vacuum is evacuated to 10 -2 Pa; in the step 3), the temperature is kept constant for 2 hours to remove moisture and air from the raw material, and the temperature is kept constant for 5 hours to completely melt the raw material, and the crucible is slowly lowered at a speed of 0.2 mm / h; in the step 4), after the growth is completed, the temperature is slowly lowered to room temperature at 20°C / h, and the furnace is opened to obtain composite artificial ruby ​​and sapphire.

[0009] Preferably, the A gemstone and B gemstone are emerald and ruby ​​respectively, the doping concentration of V2O5, Ti2O3, NiO and Co3O4 in emerald is 0.1%, and ruby ​​is Cr:Al2O3 crystal.

[0010] Preferably, in step 2), the furnace door is closed and vacuumed to 10 -1 Pa; in the step 3), the temperature is kept constant for 3 hours to remove moisture and air from the raw material, and the temperature is kept constant for 7 hours to completely melt the raw material, and the crucible is slowly lowered at a speed of 0.2 mm / h; in the step 4), after the growth is completed, the temperature is slowly lowered to room temperature at 30°C / h, and the furnace is opened to obtain composite artificial ruby ​​and emerald.

[0011] The advantages of the present invention are as follows: the method is reasonably designed, and high-quality, large-sized, and multi-color composite gemstones can be quickly grown, which can effectively solve the problems of single color and small size in existing gemstones. Moreover, the composite interface of the grown gemstones is stable and not easy to crack. The decorative effect of colorful gemstones can be achieved, and the gemstones have good economic value. DETAILED DESCRIPTION

[0012] The present invention is further described in detail below with reference to examples and specific implementation modes.

[0013] A composite artificial colored gemstone, composed of A gemstone and B gemstone of different colors, is grown by a crucible descent method, comprising the following steps: Step 1) Calculate the stoichiometric ratio of gemstone A and accurately weigh the raw materials in a glove box, then mix them evenly.

[0014] Step 2) Place the B gemstone of appropriate size in the crucible, then put the mixed raw materials in step 1) into the crucible, cover the crucible, close the furnace door and evacuate to 0-10 -2 Pa, fill with protective gas to standard atmospheric pressure.

[0015] Step 3) Turn on the heating power and raise the temperature to 200℃, and keep the temperature constant for (1-5) hours to remove moisture, air, etc. in the raw materials. Then raise the temperature to the melting point of the raw materials and keep the temperature constant for (5-10) hours to completely melt the raw materials. Slowly lower the crucible at a speed of (0.2-2) mm / h to carry out gem composite growth.

[0016] Step 4) After the growth is completed, the temperature is slowly cooled to room temperature at (10-40)℃ / h, and the furnace is opened to obtain a composite artificial colored gemstone. Example 1

[0017] A composite artificial colored gemstone consists of colorless sapphire and ruby, wherein the colorless sapphire is Al2O3 crystal and the doping concentration of chromium ions in the ruby ​​is 1%.

[0018] The preparation adopts the crucible descent method, which includes the following steps: Step 1) Calculate the stoichiometric ratio of ruby ​​(1% Cr:Al2O3) and accurately weigh the raw materials in a glove box, then mix them evenly.

[0019] Step 2) Place colorless sapphire of appropriate size in the crucible, then put the mixed raw materials in step 1) into the crucible, cover the crucible, close the furnace door and evacuate to 10 -2 Pa, fill with protective gas to standard atmospheric pressure.

[0020] Step 3) Turn on the heating power and raise the temperature to 200℃. Keep the temperature constant for 2 hours to remove moisture, air, etc. from the raw materials. Then raise the temperature to the melting point of the raw materials and keep the temperature constant for 5 hours to completely melt the raw materials. Slowly lower the crucible at a speed of 0.2mm / h to carry out gem composite growth.

[0021] Step 4) After the growth is completed, the temperature is slowly lowered to room temperature at 20°C / h, and the furnace is opened to obtain composite artificial ruby ​​and sapphire. Example 2

[0022] A composite artificial colored gemstone consists of ruby ​​and emerald, wherein the ruby ​​is a Cr:Al2O3 crystal and the doping concentration of V2O5, Ti2O3, NiO and Co3O4 in the emerald is 0.1%.

[0023] The preparation adopts the crucible descent method, which includes the following steps: Step 1) Calculate the stoichiometric ratio of emerald and accurately weigh each raw material in a glove box, then mix them evenly.

[0024] Step 2) Place a ruby ​​of appropriate size in the crucible, then add the mixed raw materials in step 1) into the crucible, cover the crucible, close the furnace door and evacuate to 10 -1 Pa, fill with protective gas to standard atmospheric pressure.

[0025] Step 3) Turn on the heating power and raise the temperature to 200℃. Keep the temperature constant for 3 hours to remove moisture, air, etc. from the raw materials. Then raise the temperature to the melting point of the raw materials and keep the temperature constant for 7 hours to completely melt the raw materials. Slowly lower the crucible at a speed of 1mm / h to carry out gem composite growth.

[0026] Step 4) After the growth is completed, the temperature is slowly lowered to room temperature at 30°C / h, and the furnace is opened to obtain composite artificial ruby ​​and emerald.

[0027] The above is only a preferred embodiment of the present invention. It should be pointed out that a person skilled in the art can make several modifications and improvements without departing from the inventive concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A composite artificial colored gemstone, characterized in that: It is composed of A gemstones and B gemstones of different colors and is grown using the crucible descent method.

2. The method for preparing a composite artificial colored gemstone according to claim 1, characterized in that: The following steps are involved: Step 1) Calculate and accurately weigh each raw material according to the stoichiometric ratio of gemstone A, and then mix them evenly; Step 2) Place the B gemstone of appropriate size in the crucible, then put the mixed raw materials in step 1) into the crucible, cover the crucible, close the furnace door and evacuate to 0-10 -2 Pa, fill the protective gas to standard atmospheric pressure; Step 3) Turn on the heating power and raise the temperature to 200°C, keep the temperature constant for (1-5) hours to remove moisture and air in the raw materials, then raise the temperature to the melting point of the raw materials and keep the temperature constant for (5-10) hours to completely melt the raw materials; slowly lower the crucible at a speed of (0.2-2) mm / h to carry out gem composite growth; Step 4) After the growth is completed, the temperature is slowly cooled to room temperature at (10-40)℃ / h, and the furnace is opened to obtain a composite artificial colored gemstone.

3. The method for preparing a composite artificial colored gemstone according to claim 2, characterized in that: The gemstone A and gemstone B are ruby ​​and colorless sapphire respectively, the doping concentration of chromium ions in ruby ​​is 1%, and the colorless sapphire is Al2O3 crystal.

4. The method for preparing a composite artificial colored gemstone according to claim 3, characterized in that: In the step 1), the stoichiometric ratio of ruby ​​is 1% Cr:Al2O3, and in the step 2), the furnace door is closed and the vacuum is evacuated to 10 -2 Pa; in the step 3), the temperature is kept constant for 2 hours to remove moisture and air from the raw material, and the temperature is kept constant for 5 hours to completely melt the raw material, and the crucible is slowly lowered at a speed of 0.2 mm / h; in the step 4), after the growth is completed, the temperature is slowly lowered to room temperature at 20°C / h, and the furnace is opened to obtain composite artificial ruby ​​and sapphire.

5. The method for preparing a composite artificial colored gemstone according to claim 2, characterized in that: The A gemstone and B gemstone are emerald and ruby ​​respectively. The doping concentration of V2O5, Ti2O3, NiO and Co3O4 in emerald is 0.1%, and ruby ​​is Cr:Al2O3 crystal.

6. The method for preparing a composite artificial colored gemstone according to claim 5, characterized in that: In step 2), the furnace door is closed and vacuumed to 10 -1 Pa; in the step 3), the temperature is kept constant for 3 hours to remove moisture and air from the raw material, and the temperature is kept constant for 7 hours to completely melt the raw material, and the crucible is slowly lowered at a speed of 0.2 mm / h; in the step 4), after the growth is completed, the temperature is slowly lowered to room temperature at 30°C / h, and the furnace is opened to obtain composite artificial ruby ​​and emerald.