CN111575795A - Preparation method of blue morusite - Google Patents
Preparation method of blue morusite Download PDFInfo
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- CN111575795A CN111575795A CN202010412602.3A CN202010412602A CN111575795A CN 111575795 A CN111575795 A CN 111575795A CN 202010412602 A CN202010412602 A CN 202010412602A CN 111575795 A CN111575795 A CN 111575795A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
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Abstract
The invention discloses a preparation method of blue morusite, which realizes the preparation of the blue morusite by doping metallic aluminum or aluminum-containing compounds, controls the uniformity of the doped metallic aluminum by combining a secondary crystallization method with an inner crucible device to obtain the blue morusite with uniform color, firstly, high-purity silicon carbide powder and the doped metallic aluminum or aluminum-containing compounds are fully mixed, then, polycrystalline morusite is selected as seed crystal in a crystal growth furnace to carry out physical vapor transport method to grow the doped polycrystalline morusite, the polycrystalline morusite is taken out and crushed and put into the inner crucible, high-purity silicon carbide powder is put into the bottom of an outer crucible, single-crystal morusite is selected as seed crystal to carry out physical vapor transport method growth again to obtain the blue morusite with uniform color, the aluminum and the silicon carbide powder are combined in the first growth, the aluminum is slowly released along with the gasification of the silicon carbide in the second growth process, thereby achieving the purpose of uniformly entering the mosang stone and realizing the uniformity control of the color.
Description
Technical Field
The invention relates to a preparation method of morusite, in particular to a preparation method of blue morusite.
Background
Morusite, also known as a silicon carbide gemstone, also known as carbo-silica, has been found to date for over 100 years, with natural Morusite being first discovered in 1905. The mosang stone is an inorganic compound, has a chemical formula of SiC, is constructed by a silicon carbon tetrahedron, has strong covalence, has the characteristics of high melting point and high hardness, has the hardness equivalent to that of diamond, and is corrosion-resistant and radiation-resistant. Because of the high melting point, the thermal stability is good, and the general temperature can not damage the crystal structure of the mozzarella.
Diamond is a well-known precious ornament, but natural diamond is scarce in stock and thus can be expensive, and artificial diamond cannot obtain products with larger size and cannot meet the requirements of productization, so people are continuously looking for substitutes for diamond, such as glass, spinel, sapphire, zircon and the like. However, the glass has low refractive index, no natural fire, poor polishing effect and low zircon hardness, and although the processing is easy, the glass cannot be made into sharp edges and corners and is easy to wear, and other substitutes have different problems to a greater or lesser extent until moyashi is found. Because of the difficulty in producing high quality morusite, until 1998, morusite has not begun to be used as a substitute for diamond, and the products of morusite gemstones are now widely distributed in the market, and the general public would like to accept such diamond-like but extremely inexpensive jewelry. High-purity morusite is nearly colorless and transparent, but the preparation difficulty is also great. Different colours of morganite can often be obtained by deliberate doping. The transparency of the mozzarella is excellent, and the current preparation technology can obtain the mozzarella with large size and high quality.
The currently common method for preparing morusite is a physical vapor transport method. The basic process is to put silicon carbide powder as raw material into a sealed cylindrical graphite crucible, and a circular Mosang stone wafer as seed crystal is fixed in the upper cover of the crucible. The graphite crucible is put into a crystal growth furnace and heated to above 2000 ℃, silicon carbide powder in a high-temperature region is sublimated to generate gas-phase molecules, and the gas-phase molecules are transmitted to the surface of the morusite seed crystals in a low-temperature region under the action of temperature gradient to deposit, crystallize and grow into large-size morusite crystals. The grown large-size morusite crystal is processed by gemstones, and finally morusite with different shapes and sizes is obtained.
The colored morusite is usually prepared by adding a doping substance into the raw materials, and the doping substance enters the interior of the morusite during the growth process to form the colored morusite. However, the method for preparing the colored morusite cannot control the release speed of the doping substance, so that the obtained morusite crystal has poor color uniformity, the doping substance is released more at the initial growth stage, the color of the region close to the seed crystal is darker, and the doping substance is almost released to the end of the later growth stage, so that the color of the morusite is very light. How to obtain the morusite with uniform color becomes a big problem of rapid marketization of the colorful morusite.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems, the invention provides a preparation method of blue morusite, which comprises the steps of doping metal aluminum or an aluminum-containing compound to prepare the blue morusite, controlling the uniformity of the doped metal aluminum by combining a secondary crystallization method with an inner crucible device to obtain the blue morusite with uniform color, fully mixing high-purity silicon carbide powder with the doped metal aluminum or the aluminum-containing compound, selecting polycrystalline morusite as a seed crystal in a crystal growth furnace to carry out a physical vapor transport method to grow the doped polycrystalline morusite, taking out the polycrystalline morusite, breaking the polycrystalline morusite, putting the polycrystalline morusite into an inner crucible, putting high-purity silicon carbide powder at the bottom of an outer crucible, selecting single-crystal morusite as the seed crystal to carry out physical vapor transport method again to grow the single-crystal morusite, and obtaining the blue morusite with uniform color.
The technical scheme is as follows: in order to solve the technical problems, the invention adopts the technical scheme that:
an effective preparation method of blue morusite comprises the following steps:
uniformly mixing high-purity silicon carbide powder and a doped metal aluminum or aluminum-containing compound, putting the mixture into a high-purity graphite crucible, fixing the Moraxel polycrystal serving as a seed crystal on the inner side of a graphite crucible cover, sealing the graphite crucible, putting the graphite crucible into a crystal growth furnace, and growing by adopting a physical vapor transport method;
step (2), after cooling, taking out the mullite polycrystal doped with the metallic aluminum, crushing and grinding the polycrystal into small crystal grains, putting the small crystal grains into a high-purity graphite inner crucible, covering a graphite crucible cover with micropores, putting the graphite inner crucible into the center of the bottom of a high-purity graphite outer crucible, and putting high-purity silicon carbide powder into the high-purity graphite outer crucible to surround the graphite inner crucible;
step (3), selecting single crystal morusite as seed crystal, fixing the seed crystal on the inner side of a graphite outer crucible cover, sealing the graphite outer crucible, and putting the graphite outer crucible into a crystal growth furnace;
and (4) growing crystals by adopting a physical vapor transport method to obtain the blue morusite.
Further, in the step (1), the doped metal aluminum or aluminum-containing compound is one or more of elemental metal aluminum, aluminum nitride or aluminum phosphide.
Further, in the step (1), the uniform mixing mode is a ball milling method.
Further, in the step (1), the seed crystal is fixed by bonding or mechanical fixing.
Further, in the step (2), the temperature reduction speed is 20-50 ℃ per hour.
Further, in the step (2), the pulverization is performed by a mechanical method.
Further, in the step (2), the micropore size of the graphite inner crucible cover is 10-50 microns.
Further, in the step (3), the material of the single crystal morusite is 4H-, 6H-, 15R-or other alpha-type morusite.
Has the advantages that: the preparation of the blue morusite is realized by doping metallic aluminum or an aluminum-containing compound, and the uniformity of the doped metallic aluminum is controlled by combining a secondary crystallization method and an inner crucible device, so that the blue morusite with uniform color is obtained. The method can obtain the blue morusite with different color depths by controlling the content of the doped metal aluminum, and has simple and controllable operation.
Drawings
FIG. 1 is a schematic view of a growth crucible of the present invention;
FIG. 2 is a top view of the inner crucible cover of the present invention.
The method comprises the following steps of 1, seed crystal, 2, a high-purity graphite crucible, 3, micropores, 4, a high-purity graphite inner crucible, 5, small crystal grains, 6 and high-purity silicon carbide powder.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to specific examples. The following examples are illustrative only and are not to be construed as limiting the invention.
Aiming at the difficulties in the prior art, the invention provides a preparation method of blue morusite, which comprises the steps of doping metallic aluminum or an aluminum-containing compound to prepare the blue morusite, controlling the uniformity of the doped metallic aluminum by combining a secondary crystallization method with an inner crucible device to obtain the blue morusite with uniform color, fully mixing high-purity silicon carbide powder with the doped metallic aluminum or the aluminum-containing compound, then selecting the polycrystalline morusite as a seed crystal in a crystal growth furnace to grow the doped polycrystalline morusite by a physical vapor transport method, taking out the polycrystalline morusite to break, putting the polycrystalline morusite into an inner crucible, putting high-purity silicon carbide powder at the bottom of an outer crucible, selecting the single-crystal morusite as the seed crystal, and growing the single-crystal morusite again by the physical vapor transport method to obtain the blue morusite with uniform color.
In order to solve the technical problems, the invention adopts the technical scheme that: as shown in fig. 1-2, a method for preparing blue morganite comprises the following steps:
uniformly mixing high-purity silicon carbide powder 6 and a doped metal aluminum or aluminum-containing compound, putting the mixture into a high-purity graphite crucible 2, fixing the mullite polycrystal as a seed crystal 1 on the inner side of a graphite crucible cover, sealing the graphite crucible, putting the graphite crucible into a crystal growth furnace, and growing by adopting a physical vapor transport method.
According to the specific embodiment of the invention, the purity of the silicon carbide powder is not less than 99.99%. According to some specific embodiments of the present invention, the doped metallic aluminum or aluminum-containing compound is one or more of elemental metallic aluminum, aluminum nitride or aluminum phosphide. According to some specific embodiments of the present invention, the seed crystal is fixed by bonding or mechanical fixing.
And (2) after cooling, taking out the mullite polycrystal doped with the metal aluminum, crushing and grinding the polycrystal into small crystal grains 5, putting the small crystal grains into a high-purity graphite inner crucible 4, covering a graphite crucible cover with micropores 3, putting the graphite inner crucible into the center of the bottom of a high-purity graphite outer crucible, and putting high-purity silicon carbide powder into the high-purity graphite outer crucible to surround the graphite inner crucible.
According to a specific embodiment of the present invention, the cooling rate is 20 ℃ to 50 ℃ per hour. The crushing mode is a mechanical method. According to specific embodiments of the present invention, the graphite inner crucible cover has a pore size of 10-50 microns.
And (3) selecting single crystal morusite as seed crystal, fixing the seed crystal on the inner side of the graphite outer crucible cover, sealing the graphite outer crucible, and putting the graphite outer crucible into a crystal growth furnace.
And (4) growing crystals by adopting a physical vapor transport method to obtain the blue morusite.
Detailed description of the preferred embodiment 1
According to the preparation method of the blue morusite, the blue morusite is prepared by doping metallic aluminum or an aluminum-containing compound, and the uniformity of the doped metallic aluminum is controlled by combining a secondary crystallization method and an inner crucible device, so that the blue morusite with uniform color is obtained. The preparation method comprises the following specific steps:
uniformly mixing high-purity silicon carbide powder and metal-doped aluminum nitride, putting the mixture into a high-purity graphite crucible, fixing the mullite polycrystal serving as a seed crystal on the inner side of a graphite crucible cover, sealing the graphite crucible, putting the graphite crucible into a crystal growth furnace, and growing the crystals by adopting a physical vapor transport method; the uniform mixing mode is a ball milling method; the seed crystal is fixed in an adhering way.
Step (2), after cooling, taking out the aluminum-doped mullite polycrystal, crushing and grinding the polycrystal into small crystal grains, putting the small crystal grains into a high-purity graphite inner crucible, covering a graphite crucible cover with micropores, wherein the micropore size is 10 microns, putting the graphite inner crucible into the center of the bottom of a high-purity graphite outer crucible, and putting high-purity silicon carbide powder into the high-purity graphite outer crucible to surround the graphite inner crucible; the crushing mode is a mechanical method; the cooling speed is 20 ℃ per hour.
Step (3), selecting single crystal morusite as seed crystal, fixing the seed crystal on the inner side of a graphite outer crucible cover, sealing the graphite outer crucible, and putting the graphite outer crucible into a crystal growth furnace; the single crystal morusite is made of 4H-type morusite.
And (4) growing crystals by adopting a physical vapor transport method to obtain the blue morusite.
The blue morusite grown by the process has the advantages of uniform color, good transparency and good crystallization quality.
Specific example 2
The difference from the specific example 1 is that in the step (1), the aluminum-containing compound is elemental metal aluminum; the seed crystal is fixed mechanically; in the step (2), the cooling speed is 50 ℃ per hour; the micropore size of the graphite inner crucible cover is 50 microns. In the step (3), the single crystal moyaite is 6H-type moyaite.
Specific example 3
The difference from the specific example 1 is that, in the step (1), the aluminum-containing compound is aluminum nitride; the seed crystal is fixed mechanically; in the step (2), the cooling speed is 42 ℃ per hour; the graphite inner crucible cover micropore size is 26 microns. In the step (3), the material of the single-crystal morusite is 15R-type morusite.
Specific example 4
The difference from the specific example 1 is that in the step (1), the aluminum-containing compound is aluminum phosphide; the seed crystal is fixed mechanically; in the step (2), the cooling speed is 38 ℃ per hour; the pore size of the graphite inner crucible cover is 31 microns.
Therefore, the invention provides an effective preparation method of blue morusite, when a graphite crucible containing an inner crucible is placed into a crystal growth furnace for morusite growth, the growth temperature is above 2000 ℃, and the growth time is longer than 60 hours, so that the blue morusite with uniform color is obtained.
In the description herein, references to the description of the terms "embodiment," "particular embodiment," "some embodiments," or the like, mean that a particular feature, material, structure, or characteristic described in connection with the embodiment or example is included in at least one embodiment of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment. Furthermore, the particular features, materials, structures, or characteristics described may be combined in any suitable manner in any one or more embodiments.
While embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (8)
1. A preparation method of blue morusite is characterized by comprising the following steps:
uniformly mixing high-purity silicon carbide powder and a doped metal aluminum or aluminum-containing compound, putting the mixture into a high-purity graphite crucible, fixing the Moraxel polycrystal serving as a seed crystal on the inner side of a graphite crucible cover, sealing the graphite crucible, putting the graphite crucible into a crystal growth furnace, and growing by adopting a physical vapor transport method;
step (2), after cooling, taking out the mullite polycrystal doped with the metallic aluminum, crushing and grinding the polycrystal into small crystal grains, putting the small crystal grains into a high-purity graphite inner crucible, covering a graphite crucible cover with micropores, putting the graphite inner crucible into the center of the bottom of a high-purity graphite outer crucible, and putting high-purity silicon carbide powder into the high-purity graphite outer crucible to surround the graphite inner crucible;
step (3), selecting single crystal morusite as seed crystal, fixing the seed crystal on the inner side of a graphite outer crucible cover, sealing the graphite outer crucible, and putting the graphite outer crucible into a crystal growth furnace;
and (4) growing crystals by adopting a physical vapor transport method to obtain the blue morusite.
2. The method of preparing blue morganite according to claim 1, wherein: in the step (1), the doped metal aluminum or aluminum-containing compound is one or more of elemental metal aluminum, aluminum nitride or aluminum phosphide.
3. The method of preparing blue morganite according to claim 1, wherein: in the step (1), the uniform mixing mode is a ball milling method.
4. The method of preparing blue morganite according to claim 1, wherein: in the step (1), the seed crystal is fixed in an adhesive or mechanical manner.
5. The method of preparing blue morganite according to claim 1, wherein: in the step (2), the cooling speed is 20-50 ℃ per hour.
6. The method of preparing blue morganite according to claim 1, wherein: in the step (2), the crushing mode is a mechanical method.
7. The method of preparing blue morganite according to claim 1, wherein: in the step (2), the micropore size of the graphite inner crucible cover is 10-50 microns.
8. The method of preparing blue morganite according to claim 1, wherein: in the step (3), the material of the single crystal morusite is 4H-, 6H-, 15R-or other alpha-type morusite.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113846383A (en) * | 2021-09-27 | 2021-12-28 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Graphite heater for simultaneously carbonizing tantalum crucibles of different sizes and using method |
| CN115434008A (en) * | 2022-09-30 | 2022-12-06 | 南通大学 | Effective control method for doping uniformity of silicon carbide single crystal grown by vapor phase method |
| WO2023035429A1 (en) * | 2021-09-13 | 2023-03-16 | 吕反修 | Method for depositing diamond film coating on surface of moissanite |
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| CN115434008A (en) * | 2022-09-30 | 2022-12-06 | 南通大学 | Effective control method for doping uniformity of silicon carbide single crystal grown by vapor phase method |
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