CN109279645A - A kind of cubic phase CaGa2O4The high temperature and high pressure preparation process of compound - Google Patents
A kind of cubic phase CaGa2O4The high temperature and high pressure preparation process of compound Download PDFInfo
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- CN109279645A CN109279645A CN201811413778.XA CN201811413778A CN109279645A CN 109279645 A CN109279645 A CN 109279645A CN 201811413778 A CN201811413778 A CN 201811413778A CN 109279645 A CN109279645 A CN 109279645A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/30—Three-dimensional structures
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
A kind of cubic phase CaGa of the invention2O4The high temperature and high pressure preparation process of compound belongs to the technical field of luminescent material preparation.Preparation method is that CaGa is made in the technical process using Paris white and gallium oxide powder as raw material, through mixing briquetting, assembling, high temperature and pressure synthesis, cooling release2O4Material；The high temperature and pressure synthesis, is to carry out in high temperature high pressure device, in the case where pressure is 5.0GPa, temperature is 1323~1673K heat-insulation pressure keeping 15~30 minutes.The method of the present invention has prepared the CaGa with face-centered cubic crystal structure2O4；It is to be carried out in no modifying agent environment anhydrous, product purity is high；Used high-temperature high-pressure apparatus is largely used to produce diamond at home at present, easy to operate, is conducive to implement quickly and be mass produced.
Description
Technical field
The invention belongs to the technical fields of luminescent material preparation.More particularly to the cubic phase of calcium gallium oxide, with calcium carbonate
(CaCO3), gallium oxide (Ga2O3) it is raw material, CaGa is prepared using high temperature and pressure synthetic technology2O4The method of cubic phase.
Background technique
With society be constantly progressive, scientific and technological rapid development, luminescent material early have become extensive use in occupy it is important
A kind of material of status.Now with the emergence of advanced luminescent material, huge push away is played to modern industrial technology progress
Movement is used.Especially electroluminescent has the characteristics that low energy consumption, small size, surface are shown, is that instrument and meter illuminates, plane is shown
The important source material of device manufacture.Calcium gallium oxide (CaGa2O4) there is very high chemical stability, and show good hold
Long luminescent properties are very promising electroluminescent materials.
The α-and β-CaGa of existing crystal structure report at present2O4, orthorhombic system is belonged to, space group is respectively Pna21With
P21/c.The HP-CaGa of report in 19802O4, there is inverse spinel structure, belong to rhombic system, space group Pnam.Due to same
A kind of material has different crystal structures, can show different physics, chemical property, therefore with brand-new crystal structure
Material is very likely to generate new light, electrical effect, this has the developmental research of luminescent material and potential application important
Meaning.The present invention prepares the cubic phase calcium gallium oxide (CaGa of new construction by high temperature and high pressure method2O4), there is spinelle
Structure belongs to cubic system, space group Fd-3m.The discovery of this new construction calcium gallium oxide enriches this type oxide
Type has established experiment basis to excavate more excellent performance of luminescent material.
Summary of the invention
The technical problem to be solved by the present invention is to the methods using new synthesis calcium gallium oxide --- high temperature and pressure preparation
Method, this method pass through control pressure, dwell time and synthesis temperature mainly to regulate and control cube phase structure of calcium gallium oxide
It is formed, prepares the calcium gallium oxide with brand-new structure, and this method is easy to implement.
Calcium gallium oxide new construction phase of the invention, component is CaGa2O4, structure is face-centred cubic structure.
The specific technical solution of cubic phase calcium gallium oxide preparation of the invention is as described below.
A kind of cubic phase CaGa2O4The high temperature and high pressure preparation process of compound is with Paris white and gallium oxide powder for original
CaGa is made in material, the technical process through mixing briquetting, assembling, high temperature and pressure synthesis, cooling release2O4Material；It is characterized in that,
The mixing briquetting is to mix Paris white and gallium oxide powder at 1: 1 in molar ratio, is pressed into block by synthetic cavity size
Shape；The assembling is that boron nitride (BN) pipe will be first wrapped up outside bulk sample, is reloaded into graphite-pipe heating container, is finally putting into
In pyrophyllite synthetic cavity；The high temperature and pressure synthesis, is carried out in high temperature high pressure device, is 5.0GPa, temperature in pressure
Degree is heat-insulation pressure keeping 15~30 minutes under 1323~1673K；Described cooling release is off cooled to room temperature after heating
Release afterwards.
The CaCO3, being preferably selected purity is 99.99%, and granularity is 1~5 micron；The Ga2O3, it is preferably selected
Purity is 99.99%, and granularity is 1~5 micron.
Compound experiment of the invention can be completed on domestic DS029B type cubic hinge press.Experiment shows synthesis temperature
Height be influence CaGa2O4An important factor for cubic phase and its purity.It can be seen that by embodiment, optimum material proportion is carbonic acid
Calcium powder and gallium oxide powder molar ratio are 1: 1, and best synthesis pressure is 5.0GPa, optimum synthesising temperature 1623K, heat-insulation pressure keeping 30
Minute.
The present invention is also claimed by a kind of calcium gallium oxide of the preparation method preparation of made of new structural material calcium gallium oxide,
It is characterized in that having face-centered cubic crystal structure.
The beneficial effects of the invention are that first, it is prepared using the method for high temperature and pressure with face-centered cubic crystal structure
CaGa2O4, it is a kind of material of new crystal structure, to CaGa2O4The developmental research and application of luminescent material have certain meaning
Justice.Second, the present invention is entirely to carry out in no modifying agent environment, can fundamentally avoid unnecessary impurity anhydrous
Occur, resulting cubic phase calcium gallium oxide purity is high.Third, this method production cubic phase calcium gallium oxide used by height
High-temperature high-pressure apparatus is largely used to produce diamond at home at present, easy to operate, can implement to produce quickly with its production
Industry, and the cubic phase calcium gallium oxide of high-quality can be obtained.
Detailed description of the invention
Attached drawing 1 is that the embodiment of the present invention 1 prepares CaGa2O4X-ray diffraction pattern.
Attached drawing 2 is that the embodiment of the present invention 2 prepares CaGa2O4X-ray diffraction pattern.
Attached drawing 3 is that the embodiment of the present invention 3 prepares CaGa2O4X-ray diffraction pattern.
Attached drawing 4 is that the embodiment of the present invention 4 prepares CaGa2O4X-ray diffraction pattern.
Attached drawing 5 is that the embodiment of the present invention 5 prepares CaGa2O4X-ray diffraction pattern.
Specific embodiment
Following embodiment is completed on domestic DS029B type cubic hinge press.Embodiment 1 is preferred processing condition
Under prepare the CaGa of the good cubic structure of crystallization degree2O4.Embodiment 3~5 illustrates as a comparison case in higher synthesis temperature
Under be that cubic crystal structure CaGa cannot be made2O4's.
Embodiment 1
By analytically pure Paris white (CaCO3) and gallium oxide powder (Ga2O3) be sufficiently mixed at 1: 1 in molar ratio, powder is molded
Afterwards, sample is fitted into high temperature and pressure cavity.Make heating tube with graphite in assembling cavity, does insulation tube, synthesis pressure with pyrophillite
Power is 5.0GPa, temperature 1623K, the pressure-maintaining and heat-preservation time 30 minutes, stops release after sample cooled to room temperature after heating, this
Under the conditions of the calcium gallium oxide (CaGa for preparing2O4) there is cubic structure, crystallization degree is best, only minimal amount of unreacted
Miscellaneous phase.Specific X-ray diffraction patterns are shown in Fig. 1.
The relatively optimal 1623K of synthesis temperature floats up and down 50K, remaining condition is constant, and can also synthesize has cube
The CaGa of structure2O4, and there is good crystallinity.
Embodiment 2
It using former material feed powder same as Example 1, is sufficiently mixed at 1: 1 in molar ratio, uses embodiment 1 after powder is molded
Assembling, synthesis pressure 5.0GPa, temperature 1323K, the pressure-maintaining and heat-preservation time 15 minutes, stop heating after sample naturally cool to
Release after room temperature, the compound component of this condition preparation include CaGa2O4Cubic phase, but also contain the impurity phase of other generations.Tool
The X-ray diffraction patterns of body are shown in Fig. 2.
Embodiment 3
Using assembling and former material feed powder same as Example 1, synthesis pressure 5.0GPa, temperature 1823K, pressure-maintaining and heat-preservation
Time 30 minutes, stopping release after sample cooled to room temperature, the compound main component that this condition is prepared after heating was
Predecessor Ga2O3Phase also contains the impurity phase of other generations.Specific X-ray diffraction patterns are shown in Fig. 3.
Embodiment 4
Using assembling and former material feed powder same as Example 1, synthesis pressure 5.0GPa, temperature 1923K, pressure-maintaining and heat-preservation
Time 30 minutes, stop release after sample cooled to room temperature after heating, the compound main component that this condition is prepared is still
For predecessor Ga2O3Phase.Specific X-ray diffraction patterns are shown in Fig. 4.
Embodiment 5
Using assembling and former material feed powder same as Example 1, synthesis pressure 5.0GPa, temperature 2123K, pressure-maintaining and heat-preservation
Time 30 minutes, stopping release after sample cooled to room temperature, the compound main component that this condition is prepared after heating was
Impurity phase.Specific X-ray diffraction patterns are shown in Fig. 5.
Claims (4)
1. a kind of cubic phase CaGa2O4The high temperature and high pressure preparation process of compound, be using Paris white and gallium oxide powder as raw material,
CaGa is made in technical process through mixing briquetting, assembling, high temperature and pressure synthesis, cooling release2O4Material；It is characterized in that, described
Mixing briquetting, be to mix Paris white and gallium oxide powder at 1: 1 in molar ratio, be pressed into bulk by synthetic cavity size；
The assembling is that first will wrap up boron nitride tube outside bulk sample, is reloaded into graphite-pipe heating container, is finally putting into pyrophyllite conjunction
At in cavity；The described high temperature and pressure synthesis, is carried out in high temperature high pressure device, pressure be 5.0GPa, temperature 1323
Heat-insulation pressure keeping 15~30 minutes under~1673K；Described cooling release is off release after cooled to room temperature after heating.
2. a kind of cubic phase CaGa according to claim 12O4The high temperature and high pressure preparation process of compound, which is characterized in that
The described high temperature and pressure synthesis, is the synthesis temperature 1623K at pressure 5.0GPa, heat-insulation pressure keeping 30 minutes.
3. a kind of cubic phase CaGa according to claim 1 or 22O4The high temperature and high pressure preparation process of compound, feature exist
In the CaCO3, purity 99.99%, granularity is 1~5 micron；The Ga2O3, purity 99.99%, granularity 1
~5 microns.
4. a kind of cubic phase CaGa of claim 12O4Calcium gallium oxide made from the high temperature and high pressure preparation process of compound,
It is characterized in that there is face-centered cubic crystal structure.
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| CN201811413778.XA CN109279645A (en) | 2018-11-26 | 2018-11-26 | A kind of cubic phase CaGa2O4The high temperature and high pressure preparation process of compound |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498903A (en) * | 2020-04-22 | 2020-08-07 | 吉林大学 | Rhombohedral phase lead-tantalum oxide and high-temperature high-pressure preparation method thereof |
| CN114671461A (en) * | 2022-05-17 | 2022-06-28 | 长春理工大学 | High-temperature high-pressure preparation method of spinel structure metal oxide negative electrode material containing oxygen vacancies |
Citations (5)
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|---|---|---|---|---|
| JPS4633266Y1 (en) * | 1968-10-26 | 1971-11-17 | ||
| US20060112873A1 (en) * | 2003-01-29 | 2006-06-01 | Tdk Corporation | Magnetic garnet single crystal film formation substrate, optical element and production method of the same |
| CN103094537A (en) * | 2011-11-07 | 2013-05-08 | 三星Sdi株式会社 | Electrode active material, preparation method thereof, and electrode and lithium battery containing the same |
| CN103198912A (en) * | 2013-04-12 | 2013-07-10 | 吉林大学 | High-temperature and high-pressure preparation method of cubic-phase scandium germanium oxide |
| CN103214244A (en) * | 2013-04-27 | 2013-07-24 | 武汉虹信通信技术有限责任公司 | Microwave dielectric ceramics and preparation method thereof |
-
2018
- 2018-11-26 CN CN201811413778.XA patent/CN109279645A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4633266Y1 (en) * | 1968-10-26 | 1971-11-17 | ||
| US20060112873A1 (en) * | 2003-01-29 | 2006-06-01 | Tdk Corporation | Magnetic garnet single crystal film formation substrate, optical element and production method of the same |
| CN103094537A (en) * | 2011-11-07 | 2013-05-08 | 三星Sdi株式会社 | Electrode active material, preparation method thereof, and electrode and lithium battery containing the same |
| CN103198912A (en) * | 2013-04-12 | 2013-07-10 | 吉林大学 | High-temperature and high-pressure preparation method of cubic-phase scandium germanium oxide |
| CN103214244A (en) * | 2013-04-27 | 2013-07-24 | 武汉虹信通信技术有限责任公司 | Microwave dielectric ceramics and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| BILJANA LAZIC´ ET AL.: "Rietveld Analysis of a High Pressure Modification of Monocalcium Oxogallate (CaGa2O4)", 《Z. ANORG. ALLG. CHEM.》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111498903A (en) * | 2020-04-22 | 2020-08-07 | 吉林大学 | Rhombohedral phase lead-tantalum oxide and high-temperature high-pressure preparation method thereof |
| CN114671461A (en) * | 2022-05-17 | 2022-06-28 | 长春理工大学 | High-temperature high-pressure preparation method of spinel structure metal oxide negative electrode material containing oxygen vacancies |
| CN114671461B (en) * | 2022-05-17 | 2023-11-17 | 长春理工大学 | High-temperature high-pressure preparation method of spinel-structure metal oxide anode material containing oxygen vacancies |
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