CN105239161B - The preparation method of ruby crystal - Google Patents
The preparation method of ruby crystal Download PDFInfo
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- CN105239161B CN105239161B CN201510679822.1A CN201510679822A CN105239161B CN 105239161 B CN105239161 B CN 105239161B CN 201510679822 A CN201510679822 A CN 201510679822A CN 105239161 B CN105239161 B CN 105239161B
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Abstract
The invention belongs to technical field of inorganic composite material preparation, a kind of preparation method of ruby crystal are in particular disclosed, including step：A, Al is weighed respectively2O3And Cr2O3, and mix and be put into arc discharge device, the arc discharge device is equipped with cathode and anode, the Al2O3And Cr2O3It is placed on the centre of the cathode and anode；B, the arc discharge device is vacuumized, and is passed through argon gas；C, the arc discharge device is opened, adjusts size of current, the arc discharge device is made to discharge；D, electric discharge terminates, and ruby crystal is made.The preparation method of ruby crystal according to the present invention not only has that reaction speed is fast, generated time is short, the advantages such as simple for process, easy to operate, at low cost, and the ruby crystal being prepared through this method also has the characteristics that purity is high, high-quality, various colors.
Description
Technical field
The invention belongs to technical field of inorganic composite material preparation, in particular, being related to a kind of preparation of ruby crystal
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.
Invention content
To solve the above-mentioned problems of the prior art, the present invention provides a kind of preparation methods of ruby crystal, should
Method is prepared based on arc process, can prepare mass height, large scale, the ruby crystal more than color category, and react
Time substantially shortens.
In order to reach foregoing invention purpose, present invention employs following technical solutions：
A kind of preparation method of ruby crystal, including step：A, Al is weighed respectively2O3And Cr2O3, and mix and be put into electricity
In arc discharging apparatus；Wherein, the arc discharge device is equipped with opposite cathode and anode, the Al2O3And Cr2O3It is placed on
The centre of the cathode and anode；B, the arc discharge device is vacuumized, and is passed through argon gas；C, the electric arc electric discharge is opened
Device adjusts size of current, and the arc discharge device is made to discharge；D, electric discharge terminates, and ruby crystal is made.
Further, the Al2O3And Cr2O3After mixing, then ground, tabletting, obtain the green compact of a diameter of 15mm, institute
Green compact is stated to be put into the copper crucible of the arc discharge device.
Further, the cathode of the arc discharge device is tungsten filament, and the anode is selected from copper crucible, aluminium earthenware
Any one in crucible, golden crucible, platinum crucible；Wherein, the Al2O3And Cr2O3It is placed in the anode.
Further, the Cr2O3With Cr2O3Mass ratio be 0.1~2:99.9~98.
Further, in the step C, size of current is 50A~200A.
Further, in the step C, the reaction time is 0.5min~5min.
Further, during opening the arc discharge device and terminating to electric discharge, to the arc discharge device
In be passed through cooling water.
Further, in the step B, the arc discharge device is evacuated to 100Pa, then put to the electric arc
The air pressure for being passed through argon gas to the arc discharge device in electric installation is more than 101kPa.
Ruby crystal has been prepared by the arc process using inert gases such as argon gas as atmosphere in the present invention, with existing skill
Many preparation methods in art are compared, and the present invention has the advantages that：
(1) reaction speed is fast, and generated time is short：The present invention is exceedingly fast using plasma direct-current discharge, heating rate, can wink
Between make Al2O3And Cr2O3As molten condition, and Al is completed within tens of seconds2O3And Cr2O3Fusion；Meanwhile cooling velocity is fast,
Room temperature is down in several minutes so that entire generated time is no more than 5min.
(2) product purity is high, high-quality：The plasma that electric arc generates is pure, will not introduce any impurity, due to
Its temperature is high, does not need to any cosolvent, additive, catalyst, product quality stability and favorable reproducibility.
(3) product colour enriches：By adjusting Cr2O3Quality and the reaction time, rose-red, pink, deep can be obtained
The product of the multiple colors such as red, scarlet.
(4) it is highly practical, it is at low cost：Present invention process is simple, easy to operate, at low cost, and entire reaction process is nontoxic, nothing
It is harmful, pollution-free.
Description of the drawings
What is carried out in conjunction with the accompanying drawings is described below, above and other aspect, features and advantages of the embodiment of the present invention
It will become clearer, in attached drawing：
Fig. 1 is the XRD diagram piece of 3 ruby crystal according to an embodiment of the invention；
Fig. 2 is the section SEM pictures of 3 ruby crystal according to an embodiment of the invention.
Specific embodiment
Hereinafter, with reference to the accompanying drawings to detailed description of the present invention embodiment.However, it is possible to come in many different forms real
The present invention is applied, and the present invention should not be construed as limited to the specific embodiment illustrated here.On the contrary, provide these implementations
Example is in order to explain the principle of the present invention and its practical application, so as to make others skilled in the art it will be appreciated that the present invention
Various embodiments and be suitable for the various modifications of specific intended application.
The preparation method of ruby crystal according to an embodiment of the invention includes the following steps：
In step 1, Al is weighed respectively2O3And Cr2O3, ground after mixing, and the pressure of a diameter of 15mm is pressed into mold
Base.
Usually, Cr is controlled2O3Dosage for its quality be Al2O3And Cr2O3The 0.1%~2% of gross mass, that is,
It says, Cr2O3And Al2O3Mass ratio be 0.1~2:99.9~98.
In step 2, green compact is put into the copper crucible in arc discharge device；Specifically, the arc discharge device
Using copper crucible as anode, using tungsten filament as cathode, that is to say, that by Al in step 12O3And Cr2O3Obtained green compact is positioned over
Between cathode and anode.
What deserves to be explained is because temperature of the arc discharge device in electric discharge is higher, generally using tungsten filament as cathode,
But the present invention is not restricted to this, other higher melting-point metals etc.；And anode is also not limited to the copper in the present embodiment
Crucible processed can also be aluminium crucible, golden crucible, platinum crucible etc..
In step 3, cooling water is passed through into arc discharge device, and be evacuated to 10-3Atmospheric pressure (about 100Pa
Left and right), then be filled with air pressure in argon gas to device thereto and be more than an atmospheric pressure (101kPa or so)；Usually, holding meanss
Middle air pressure is slightly above an atmospheric pressure.
In step 4, arc discharge device is opened, setting electric current is 50A~200A, reacts 0.5min~5min, makes electricity
Arc discharging apparatus discharges.
In step 5, electric discharge terminates, and closes power supply, adjusts pressure to normal pressure (atm higher), stops being passed through
Cooling water, ruby crystal made from taking-up.
Hereinafter, by detailed retouch is carried out to the preparation method of ruby crystal according to the present invention with reference to specific embodiment
It states, for convenience of being compared to the experiment parameter of each embodiment, analysis in table form compares each embodiment；Embodiment 1-4
In comparing result under different experiments parameter it is as shown in table 1.
Table 1 according to an embodiment of the invention 1-4 experiment parameter comparison
Wherein, in table 1, " mass ratio " refers to Cr2O3With Al2O3Mass ratio.
X-ray diffraction (hereinafter referred to as XRD) characterization has been carried out to the ruby crystal that above-described embodiment 3 is prepared,
XRD diagram piece is as shown in Figure 1；And scanning electron microscope (hereinafter referred to as SEM) characterization, section SEM pictures such as Fig. 2 are carried out to its section
It is shown.
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (4)
1. a kind of preparation method of ruby crystal, which is characterized in that including step：
A, Al is weighed respectively2O3And Cr2O3, the Al2O3And Cr2O3After mixing, then ground, tabletting, obtain a diameter of 15mm's
Green compact, the green compact are put into the arc discharge device；Wherein, the arc discharge device is equipped with opposite cathode and sun
Pole, the cathode are tungsten filament, any one of the anode in copper crucible, aluminium crucible, golden crucible, platinum crucible；It is described
Al2O3And Cr2O3It is placed in the anode；
B, the arc discharge device is vacuumized, and is passed through argon gas；
C, the arc discharge device is opened, adjusts size of current, the arc discharge device is made to discharge；Size of current is 50A
~200A, reaction time are 0.5min~5min；
D, electric discharge terminates, and ruby crystal is made.
2. the preparation method of ruby crystal according to claim 1, which is characterized in that the Cr2O3With Al2O3Quality
The ratio between be 0.1~2:99.9~98.
3. the preparation method of ruby crystal according to claim 2, which is characterized in that opening the electric arc electric discharge dress
It puts to electric discharge during terminating, cooling water is passed through into the arc discharge device.
4. the preparation method of ruby crystal according to claim 1, which is characterized in that in the step B, by described in
Arc discharge device is evacuated to 100Pa, then is passed through argon gas to the arc discharge device into the arc discharge device
Air pressure is more than 101kPa.
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| CN105239161B true CN105239161B (en) | 2018-06-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107022792A (en) * | 2017-02-28 | 2017-08-08 | 梧州市东麟宝石机械有限公司 | A kind of artificial synthesized sapphire preparation method |
| CN107034514A (en) * | 2017-02-28 | 2017-08-11 | 梧州市东麟宝石机械有限公司 | A kind of excellent ruby preparation method of permeability |
| CN106966704A (en) * | 2017-02-28 | 2017-07-21 | 梧州市东麟宝石机械有限公司 | One kind synthesis ruby preparation method of dove blood |
| CN107829132A (en) * | 2017-10-10 | 2018-03-23 | 上海应用技术大学 | A kind of method for preparing alumina single crystal |
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|---|---|---|---|---|
| WO2005068392A1 (en) * | 2004-01-19 | 2005-07-28 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | COLORED TRANSPARENT CORUNDUM MATERIAL COMPRISING A POLYCRYSTALLINE SUB-µM STRUCTURE, AND METHOD FOR THE PRODUCTION OF MOLDED ELEMENTS FROM SAID MATERIAL |
| CN1778758A (en) * | 2005-09-29 | 2006-05-31 | 上海大学 | Preparation of Cr4+ A12O3 transparent laser ceramic materials |
| CN101306942A (en) * | 2008-06-27 | 2008-11-19 | 王昕� | Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof |
| CN102021647A (en) * | 2010-10-22 | 2011-04-20 | 北京工业大学 | Method for rapid growth of centimeter magnitude ruby crystal |
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2015
- 2015-10-19 CN CN201510679822.1A patent/CN105239161B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005068392A1 (en) * | 2004-01-19 | 2005-07-28 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | COLORED TRANSPARENT CORUNDUM MATERIAL COMPRISING A POLYCRYSTALLINE SUB-µM STRUCTURE, AND METHOD FOR THE PRODUCTION OF MOLDED ELEMENTS FROM SAID MATERIAL |
| CN1778758A (en) * | 2005-09-29 | 2006-05-31 | 上海大学 | Preparation of Cr4+ A12O3 transparent laser ceramic materials |
| CN101306942A (en) * | 2008-06-27 | 2008-11-19 | 王昕� | Fine-crystal high transparency ruby ceramic materials and low-temperature preparation thereof |
| CN102021647A (en) * | 2010-10-22 | 2011-04-20 | 北京工业大学 | Method for rapid growth of centimeter magnitude ruby crystal |
Non-Patent Citations (1)
| Title |
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| 直流电弧法合成B4C的研究;李雪飞等;《吉林师范大学学报(自然科学版)》;20070531(第2期);第47-48、52页 * |
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