CN108149323A - Prepare ruby method - Google Patents

Prepare ruby method Download PDF

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Publication number
CN108149323A
CN108149323A CN201711278549.7A CN201711278549A CN108149323A CN 108149323 A CN108149323 A CN 108149323A CN 201711278549 A CN201711278549 A CN 201711278549A CN 108149323 A CN108149323 A CN 108149323A
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CN
China
Prior art keywords
ruby
raw material
melt
arc
anode
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711278549.7A
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Chinese (zh)
Inventor
王晶晨
郭科宏
钟贵全
陈珊
侯傲
吴道洪
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Shenwu Technology Group Corp Co Ltd
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Shenwu Technology Group Corp Co Ltd
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Priority to CN201711278549.7A priority Critical patent/CN108149323A/en
Publication of CN108149323A publication Critical patent/CN108149323A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003Heating or cooling of the melt or the crystallised material
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B11/00Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/005Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method by irradiation or electric discharge
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/20Aluminium oxides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention discloses preparing ruby method, including:(1) ruby raw material is prepared, and the raw material is placed between cathode and anode, and a part for the anode is embedded in the bottom of the raw material;(2) with untransferable arc to being heated at the top of the raw material, the direction for making the raw material along the cathode to the anode melts to the melt to be formed and the positive contact;(3) melt is heated with transferred arc or conjunct arc;(4) stop heating, cool down the melt, to obtain the ruby.Nature volcano magma phenomenon can fully being simulated, and can further reduce the cost using this method using this method, improving preparation efficiency, the ruby being prepared with the ruby generated naturally with can compare favourably.

Description

Prepare ruby method
Technical field
The invention belongs to Material Field, in particular to preparing ruby method.
Background technology
Corundum (α-Al2O3) because it is doped with a small amount of Cr2O3And take on a red color, it is referred to as ruby crystal.It is closed since artificial Since being found into ruby crystal, ruby crystal because its output in visible range, line width is relatively narrow, fluorescence lifetime is long, quantum Efficient, pump absorption bandwidth, the features such as position is superior, in addition high temperature resistant, hard, long lifespan, thermal conductivity is good, chemical property is steady The excellent physical and chemical performance such as fixed plays the effect to become more and more important in fields such as optics, industry, decoration, medical instruments.
The main method for preparing ruby crystal at present has:Flame melt method, fluxing agent melt method, czochralski method, hydro-thermal method and light Learn float-zone method.Flame melt method and hydro-thermal method are due to the limitation of its process conditions, it is difficult to grow high quality, large-sized crystal;It carries Although daraf(reciprocal of farad) is the common methods for growing crystal, but Al2O3Fusing point be about 2000 DEG C, common crucible can not bear as This high temperature, high temperature easily make crucible melt and influence its quality;Floating zone method is a kind of fast-growth small-sized crystals Technology, have the characteristics that the speed of growth is fast, growth temperature is wide, without crucible, but its reaction time is longer.Fluxing agent melt Method can pollute crystal using crucible and fluxing agent.
Therefore, the method for preparing ruby crystal is further improved.
Invention content
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, the present invention One purpose is that proposition prepares ruby method, and this method can fully simulate nature volcano magma phenomenon, and use This method can further reduce the cost, and improve preparation efficiency, the ruby being prepared with can be with the ruby that generates naturally It compares favourably.
According to an aspect of the present invention, the present invention propose it is a kind of prepare ruby method, including:
(1) ruby raw material is prepared, and the raw material is placed between cathode and anode, and the one of the anode It is partially buried in the bottom of the raw material;
(2) with untransferable arc to being heated at the top of the raw material, make the raw material along the cathode to the anode Direction melt to the melt to be formed and the positive contact;
(3) melt is heated with transferred arc or conjunct arc;
(4) stop heating, cool down the melt, to obtain the ruby.
The above embodiment of the present invention prepares ruby method, first with untransferable arc to be located at cathode and anode it Between prepare and heated at the top of ruby raw material, the direction of raw material from cathode to anode is made to start to melt and formed melt, After when melt and being embedded in the positive contact of raw material bottom, then using transferred arc or conjunct arc continue to heat melt, heating is abundant Stop heating and cooling down afterwards, finally obtain ruby.The ruby method for preparing of the above embodiment of the present invention combines profit as a result, Raw material is heated with untransferable arc and transferred arc or conjunct arc, efficiently solves that raw material is non-conductive can not to generate electric arc Problem.And ruby method is prepared using the present invention can fully simulate nature volcano magma phenomenon, and it is relatively low into Originally the comparable ruby of ruby quality with generating naturally and in the shorter time is synthesized.
It prepares ruby method in addition, according to the above embodiment of the present invention and can also have the following additional technology special Sign:
In some embodiments of the invention, in step (2), with untransferable arc to the center at the top of the raw material It is heated.It is possible thereby to the fraction region of donor center is only made to form melt, and surrounding raw material does not melt, and then can keep away Exempt from high-temperature fusant contact container, reach certain heat insulation.
In some embodiments of the invention, in step (3), the melt is heated with conjunct arc.Thus, it is possible to The top and bottom of melt heat simultaneously so that raw material can be melted preferably, and then effectively improve ruby Quality.
In some embodiments of the invention, the heating carries out under an inert atmosphere.Thus, it is possible to it effectively avoids Impurity is introduced in heating process.
In some embodiments of the invention, the inert atmosphere is argon gas atmosphere.Thus, it is possible to it effectively avoids heating Impurity is introduced in the process.
In some embodiments of the invention, the anode is tungsten alloy anode.It is possible thereby to it avoids preparing ruby During anode melting enter melt so that pollute ruby.
In some embodiments of the invention, the raw material includes the aluminium oxide of 98-98.5 weight % and 1.5-2 weight % Chromium oxide.Thus, it is possible to make the ruby finally obtained that there is higher quality.
In some embodiments of the invention, it is described to be cooled to natural cooling or quenching cooling.Thus, it is possible to final To ruby.
In some embodiments of the invention, it prepares ruby method to be constrained by raw material itself, make heated There was only the fraction zone melting of donor center in journey, peripheral part is non-fusible.Thereby, it is possible to fully simulate nature volcano magma Phenomenon, and then synthesize the comparable ruby of ruby quality with generating naturally.
Description of the drawings
Fig. 1 is according to an embodiment of the invention to prepare ruby method flow diagram.
Fig. 2 is according to an embodiment of the invention to prepare ruby method schematic diagram.
Specific embodiment
The embodiment of the present invention is described below in detail, the example of the embodiment is shown in the drawings, wherein from beginning to end Same or similar label represents same or similar element or the element with same or like function.Below with reference to attached The embodiment of figure description is exemplary, it is intended to for explaining the present invention, and is not considered as limiting the invention.
According to an aspect of the present invention, the present invention propose it is a kind of prepare ruby method, including:(1) system is prepared Standby ruby raw material, and raw material is placed between cathode and anode, and a part for anode is embedded in the bottom of raw material;(2) with Untransferable arc makes direction of the raw material along cathode to anode melt to the melt to be formed and is connect with anode to being heated at the top of raw material It touches;(3) melt is heated with transferred arc or conjunct arc;(4) stop heating, cool down melt, to obtain ruby.
The above embodiment of the present invention prepares ruby method, first with untransferable arc to be located at cathode and anode it Between prepare and heated at the top of ruby raw material, the direction of raw material from cathode to anode is made to start to melt and formed melt, When melt and be embedded in raw material bottom positive contact after, then using transferred arc or conjunct arc continue to melt heat, when heating is filled Stop heating and cooling down after point, finally obtain ruby.The ruby method for preparing of the above embodiment of the present invention combines as a result, Untransferable arc and transferred arc is utilized or conjunct arc heats raw material, efficiently solves that raw material is non-conductive can not to generate electric arc The problem of.And the use present invention prepares ruby method and can fully simulate nature volcano magma phenomenon, and relatively low Synthesis and the comparable ruby of ruby quality generated naturally in cost and shorter time.
The ruby method for preparing of the above embodiment of the present invention is described in detail below with reference to Fig. 1-2.
S100:Pretreatment
According to an embodiment of the invention, ruby raw material is prepared, and raw material is placed between cathode and anode, and A part for anode is embedded in the bottom of raw material.Be conducive to subsequently heat ruby raw material as a result,.
According to a particular embodiment of the invention, the aluminium oxide of 98-98.5 weight % can be included by preparing ruby raw material With the chromium oxide of 1.5-2 weight %.Using the aluminium oxide and chromium oxide of aforementioned proportion raw material is configured, and be not introduced into other in the present invention Impurity component, thus, it is possible to make the ruby finally obtained that there is higher quality.
According to a particular embodiment of the invention, anode can be tungsten-copper alloy anode, and the copper content of alloys in common use is 10- 50%.Alloy is produced with powder metallurgy process, has good electrical and thermal conductivity, preferable elevated temperature strength and certain plasticity. At very high temperatures, such as 3000 DEG C or more, the copper in alloy is liquefied evaporation, largely absorbs heat, reduction material surface temperature Degree.Gun body anode and cathode in the present invention is protected by water cooling, and maximum temperature is no more than 1000 DEG C.It is suitable by selecting in the present invention Tungsten alloy can make anode have the fusing point far above aluminium oxide and chromium oxide, as a result, when aluminium oxide and chromium oxide as anode Will not cause too much influence to anode after melting, so as to avoid prepare ruby anodic be fusing into melt into And pollute ruby.
S200:Raw material is heated with untransferable arc
According to an embodiment of the invention, with untransferable arc to being heated at the top of raw material, make raw material along cathode to anode Direction melt to the melt and positive contact to be formed.
Be mainly aluminium oxide and chromium oxide due to preparing ruby raw material, be non-conducting material, anode and cathode it Between can not generate electric arc, therefore transferred arc or conjunct arc can not be used to heat it.The present inventor passes through pre- First using untransferable arc, it can effectively realize that the heating to non-conductive ruby raw material melts, and aluminium oxide can be made after melting For conducting medium, and then realize that subsequent transfer arc or conjunct arc heat melt.
According to a particular embodiment of the invention, heating can carry out under an inert atmosphere.Thus, it is possible to it effectively avoids Impurity is introduced in heating process.Specifically, it is prepared prepared after ruby raw material is placed between cathode and anode, it can be with It first vacuumizes, then is passed through inert gas, reaction atmosphere is made to become the inert atmosphere for being not susceptible to reaction, then using untransferable arc Raw material is heated.According to a particular embodiment of the invention, inert atmosphere can be argon gas atmosphere.
According to a particular embodiment of the invention, the center at the top of raw material can be heated with untransferable arc. Since the fusing point of aluminium oxide and chromium oxide is above 2000 DEG C, common refractory brick material is unable to reach so high high temperature resistant Performance.Inventors be surprised to learn that being heated by using untransferable arc to the center at the top of raw material, raw material can be made to exist Start to melt on cathode to the direction of anode, and only the fraction region of heart position forms melt, periphery raw material in the feed It does not melt, and then melt is made to be surrounded by aluminium oxide and chromium oxide powder, until melt and positive contact, it is possible thereby to utilize oxidation The heat-barrier material of aluminium and chromium oxide powder as melt, and then can save and refractory brick is set in container inner wall, it not only reduces Cost, while the refractory brick of setting can also be avoided to melt at high temperature and pollute ruby.
According to a particular embodiment of the invention, by take the above method make furnace interior donor center position small portion Divide and form melt, peripheral part is non-fusible, can fully simulate nature volcano magma phenomenon, and then the ruby and nature generated The ruby of generation is quite similar.
S300:Melt is heated with transferred arc or conjunct arc
According to an embodiment of the invention, melt is heated with transferred arc or conjunct arc.It is according to the present invention specific Embodiment when carrying out being heated to the melt contacts to be formed to anode to raw material using untransferable arc, can utilize melt oxidation Aluminium further heats melt using transferred arc or conjunct arc, melt is made more to stablize as conducting medium.Lead to as a result, The electric conductivity for efficiently using melt is crossed, realizes that untransferable arc switches to transferred arc or conjunct arc, and then melt can be enable to obtain To abundant heating, and then further improve ruby quality.
According to a particular embodiment of the invention, conjunct arc may be used to heat melt.Thus, it is possible to use joint Arc to the top and bottom of melt heat simultaneously so that raw material can be melted preferably, and then effectively improve red treasured Stone quality.
S400:Stop heating and cool down melt
According to an embodiment of the invention, stop heating, cool down melt, to obtain ruby.Thus, it is possible to it finally makes It is standby to obtain ruby.
According to a particular embodiment of the invention, cooling can be natural cooling or quenching cooling.Thus, it is possible to effective To ruby.
In conclusion the ruby method for preparing by using the above embodiment of the present invention at least has following beneficial effect One of fruit:
1st, aluminium oxide and chromium oxide are used as raw material, and raw material is heated using plasma arc under an inert atmosphere, Other impurity are not introduced in preparation process, and then can be in relatively low cost and the higher red treasured of synthesis quality in the shorter time Stone.
2nd, raw material is heated using untransferable arc and conjunct arc, generated time is short, efficient.
3rd, it is constrained by raw material itself, makes the fraction zone melting for there was only donor center in heating process, surrounding Part is non-fusible, can fully simulate nature volcano magma phenomenon, make the ruby of generation with the ruby generated naturally very It is similar.
4th, furnace body does not have heat resisting brick, and then can melt pollution ruby to avoid heat-resisting peritectic.
In the description of this specification, reference term " one embodiment ", " example ", " is specifically shown " some embodiments " The description of example " or " some examples " etc. means specific features, structure, material or the spy for combining the embodiment or example description Point is contained at least one embodiment of the present invention or example.In the present specification, schematic expression of the above terms are not It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be any It is combined in an appropriate manner in a or multiple embodiments or example.In addition, without conflicting with each other, the technology of this field Different embodiments or examples described in this specification and the feature of different embodiments or examples can be combined by personnel And combination.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example Property, it is impossible to limitation of the present invention is interpreted as, those of ordinary skill in the art within the scope of the invention can be to above-mentioned Embodiment is changed, changes, replacing and modification.

Claims (9)

1. a kind of prepare ruby method, which is characterized in that including:
(1) ruby raw material is prepared, and the raw material is placed between cathode and anode, and a part for the anode It is embedded in the bottom of the raw material;
(2) with untransferable arc to being heated at the top of the raw material, make the raw material along the cathode to the side of the anode To melting to the melt to be formed and the positive contact;
(3) melt is heated with transferred arc or conjunct arc;
(4) stop heating, cool down the melt, to obtain the ruby.
2. according to claim 1 prepare ruby method, which is characterized in that in step (2), with untransferable arc to institute It is heated the center for stating the top of raw material.
3. according to claim 2 prepare ruby method, which is characterized in that in step (3), with conjunct arc to described Melt is heated.
4. according to claim 1 prepare ruby method, which is characterized in that it is described heating be under an inert atmosphere into Capable.
5. according to claim 4 prepare ruby method, which is characterized in that the inert atmosphere is argon gas atmosphere.
6. according to claim 1 prepare ruby method, which is characterized in that the anode is tungsten alloy anode.
7. according to claim 1 prepare ruby method, which is characterized in that the raw material includes 98-98.5 weights Measure the aluminium oxide of % and the chromium oxide of 1.5-2 weight %.
8. according to claim 1 prepare ruby method, which is characterized in that described to be cooled to natural cooling or quench Fire cooling.
9. according to claim 1 prepare ruby method, which is characterized in that is constrained, made by raw material itself There was only the fraction zone melting of donor center in heating process, peripheral part is non-fusible.
CN201711278549.7A 2017-12-06 2017-12-06 Prepare ruby method Pending CN108149323A (en)

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CN201711278549.7A CN108149323A (en) 2017-12-06 2017-12-06 Prepare ruby method

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CN201711278549.7A CN108149323A (en) 2017-12-06 2017-12-06 Prepare ruby method

Publications (1)

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CN108149323A true CN108149323A (en) 2018-06-12

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Country Status (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110853472A (en) * 2019-12-11 2020-02-28 武汉科技大学 Simulation method of in-board volcano effect

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110853472A (en) * 2019-12-11 2020-02-28 武汉科技大学 Simulation method of in-board volcano effect

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