CN108559507A - A kind of preparation method of zinc doping Luetcium aluminum garnet - Google Patents
A kind of preparation method of zinc doping Luetcium aluminum garnet Download PDFInfo
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- CN108559507A CN108559507A CN201810788756.5A CN201810788756A CN108559507A CN 108559507 A CN108559507 A CN 108559507A CN 201810788756 A CN201810788756 A CN 201810788756A CN 108559507 A CN108559507 A CN 108559507A
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- aluminum garnet
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- luetcium aluminum
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7706—Aluminates
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
- C01F17/32—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 oxide or hydroxide being the only anion, e.g. NaCeO2 or MgxCayEuO
- C01F17/34—Aluminates, e.g. YAlO3 or Y3-xGdxAl5O12
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to luminescent material technical fields, and in particular to a kind of preparation method of zinc doping Luetcium aluminum garnet includes the following steps:Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 20 50min, mixture is obtained after drying;Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generates, then passes to ammonia until precipitation no longer generates, absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;Step 5, by 4 8h of mixed precipitation freeze-day with constant temperature, it is cooling after ball mill grinding at powder, then calcine 2 4h, obtain zinc doping Luetcium aluminum garnet.The present invention solves the technological gap of zinc doping Luetcium aluminum garnet, provides the doping way of new Luetcium aluminum garnet.
Description
Technical field
The invention belongs to luminescent material technical fields, and in particular to a kind of preparation method of zinc doping Luetcium aluminum garnet.
Background technology
Lu2O3-Al2O3System is with Y2O3-Al2O3Grow up based on system.Due to Y2O3-Al2O3It is deposited in system
In such as YAG (yttrium-aluminium-garnet, Y3Al5O12) and YAP (yttrium aluminate, YAlO3) both phases, since they have good materialization
Property and optical property become most common host material.People are prepared by adulterating the active ions such as Nd, Yb and Ce
High performance laser or scintillation material.Such as common Nd:YAG and Yb:YAG laser crystal, Ce:YAP scintillation crystals.People at present
Also Ce is being had studied:YAG and Yb:The scintillation properties of YAG.But with the development of science and technology, YAP and YAG is relatively low due to density
And cascade unit is larger, cannot be satisfied the requirement of minimonitor, therefore people Lu3+Ion replaces Y3+Ion obtains Lu2O3-
Al2O3System.Research finds such as to mix Cerium aluminate lutetium (i.e. Ce:LuAlO3) scintillation crystal density up to 8.34g/cm3, it is people
One of highest material of density in the medical scintillator studied.And with reference to the sudden strain of a muscle of the active ions YAG crystal such as doping Yb and Ce
Bright and laser activity development, has important role to the preparation of lutetium aluminum carbuncle crystal in practical application.
Relevant research domestic at present be mainly silicate silicic acid lutetium crystalline ceramics preparation, though achieve relatively
High transparency, but refraction and absorption due to the crystal boundary of polycrystalline structure ceramic body to light, optical characteristics come relative to crystal
Say or have larger gap.And domestic related crystalline research then concentrates on the growth of lutetium aluminate crystal, but due to Lu2O3-
Al2O3System exists simultaneously three kinds of phases, and aluminic acid lutetium is mutually a kind of high-temperature stable phase, and compares and belong to thermodynamics at room temperature not
Stable phase, is usually easy to be formed other phases in growth and is difficult to grow large-size crystals, and be easy to crack.
Invention content
For the problems of the prior art, the present invention provides a kind of preparation method of zinc doping Luetcium aluminum garnet, solves
The technological gap of zinc doping Luetcium aluminum garnet provides the doping way of new Luetcium aluminum garnet.
To realize the above technical purpose, the technical scheme is that:
A kind of preparation method of zinc doping Luetcium aluminum garnet, includes the following steps:
Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 20-
50min obtains mixture after drying;
Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;
Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;
Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generate, then pass to ammonia until
Precipitation no longer generates, and absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;
Step 5, by mixed precipitation freeze-day with constant temperature 4-8h, it is cooling after ball mill grinding at powder, then calcine 2-4h, obtain zinc
Adulterate Luetcium aluminum garnet.
The molar ratio of three two lutetiums of oxidation and alundum (Al2O3) in the step 1 is 3: 5.
A concentration of 30-150g/L of three two lutetiums of oxidation in absolute ethyl alcohol in the step 1, the frequency of the ultrasonic cleaning
Rate is 40-60kHz, and the drying temperature is 60-70 DEG C.
The mass concentration of hydrochloric acid is 10-20%, the pH most 3-4. of the mixed liquor in the step 2
The addition of zinc chloride in the step 3 is the 6-10% of three oxidations, two lutetium mole.
The addition of hydroxypropyl cellulose in the step 3 is the 10-15% of three oxidations, two lutetium mole.
The speed that is passed through of carbon dioxide in the step 4 is 5-10mL/min.
The supersonic frequency of ultrasound filtration in the step 4 is 40-50kHz, and temperature is 40-70 DEG C.
Freeze-day with constant temperature temperature in the step 5 is 200-250 DEG C.
Sintering temperature in the step 5 is 900-1100 DEG C.
Three two lutetiums of oxidation and alundum (Al2O3) are carried out cleaning mixing by step 1, by the ultrasonic cleaning of absolute ethyl alcohol, by table
Face organic impurities removal, while can utilize clutch that can be thoroughly mixed solid, obtain mixture;
Alundum (Al2O3) and three oxidation two lutetiums acidifications are formed acid solution, while three two lutetiums of oxidation are converted into lutetium by step 2
Ion, alundum (Al2O3) are converted into aluminium ion, by the mixing of ionic nature, to increase phase mixcibility of the lutetium with aluminium.
Step 3 is added zinc chloride as soluble dopant into solution, plays Ar ion mixing doping effect, adopts simultaneously
It uses hydroxypropyl cellulose to be added as dispersant into mixed liquor, promotes the dispersibility and toughness of solution.
Step 4 can form aeration reaction by the aeration reaction of carbon dioxide, and metal ion is formed carbonic acid precipitation, and
And using hydroxypropyl cellulose dispersibility and precipitation itself porosity, formed mixing package, be passed through ammonia adjust pH until
It is in alkalinity completely, finally by the mode of ultrasound filtration by Precipitation, while ultrasound can utilize clutch that can will wrap up property
Precipitation smash again, carry out depth mixing, additionally it is possible to reduce washing difficulty;Absolute ethyl alcohol washing can be by hydroxypropyl cellulose
Dissolving removal, and precipitation is not destroyed, while dissolved hydroxypropyl cellulose can recycle reuse.
Step 5 converts carbonate to oxide, and the effect being thoroughly mixed using it by the way of freeze-day with constant temperature,
Being sufficiently mixed for oxide can be formed, ball mill grinding calcines to form zinc doping Luetcium aluminum garnet.
From the above, it can be seen that the present invention has following advantages:
1. the present invention solves the technological gap of zinc doping Luetcium aluminum garnet, the doping side of new Luetcium aluminum garnet is provided
Formula solves Luetcium aluminum garnet grain forming energy force difference, problem easy to crack.
2. material prepared by the present invention not only improves transparency, material granule tight type, while also improving are promoted
Stability and mechanical strength are learned, zinc ion fills up internal crystal gap and stomata, improves overall performance, particle diameter distribution very well
It is narrow.
3. the present invention is used as dopant using zinc, can improving laser export, and stability is good, physics, biology,
The various fields such as OCT, laser spectroscopy, optic communication and Laser focus tool has been widely used.
Specific implementation mode
The present invention will be described in detail in conjunction with the embodiments, but does not do any restriction to the claim of the present invention.
Embodiment 1
A kind of preparation method of zinc doping Luetcium aluminum garnet, includes the following steps:
Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 20min,
Mixture is obtained after drying;
Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;
Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;
Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generate, then pass to ammonia until
Precipitation no longer generates, and absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;
Step 5, by mixed precipitation freeze-day with constant temperature 4-8h, it is cooling after ball mill grinding at powder, then calcine 2-4h, obtain zinc
Adulterate Luetcium aluminum garnet.
The molar ratio of three two lutetiums of oxidation and alundum (Al2O3) in the step 1 is 3: 5.
A concentration of 30g/L of three two lutetiums of oxidation in absolute ethyl alcohol in the step 1, the frequency of the ultrasonic cleaning are
40kHz, the drying temperature are 60 DEG C.
The mass concentration of hydrochloric acid is 10% in the step 2, the pH most 3. of the mixed liquor
The addition of zinc chloride in the step 3 is the 6% of three oxidations, two lutetium mole.
The addition of hydroxypropyl cellulose in the step 3 is the 10% of three oxidations, two lutetium mole.
The speed that is passed through of carbon dioxide in the step 4 is 5mL/min.
The supersonic frequency of ultrasound filtration in the step 4 is 40kHz, and temperature is 40 DEG C.
Freeze-day with constant temperature temperature in the step 5 is 200 DEG C.
Sintering temperature in the step 5 is 900 DEG C.
Embodiment 2
A kind of preparation method of zinc doping Luetcium aluminum garnet, includes the following steps:
Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 50min,
Mixture is obtained after drying;
Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;
Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;
Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generate, then pass to ammonia until
Precipitation no longer generates, and absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;
Step 5, by mixed precipitation freeze-day with constant temperature 8h, it is cooling after ball mill grinding at powder, then calcine 4h, obtain zinc doping
Luetcium aluminum garnet.
The molar ratio of three two lutetiums of oxidation and alundum (Al2O3) in the step 1 is 3: 5.
A concentration of 150g/L of three two lutetiums of oxidation in absolute ethyl alcohol in the step 1, the frequency of the ultrasonic cleaning
For 60kHz, the drying temperature is 70 DEG C.
The mass concentration of hydrochloric acid is 20% in the step 2, the pH most 4. of the mixed liquor
The addition of zinc chloride in the step 3 is the 10% of three oxidations, two lutetium mole.
The addition of hydroxypropyl cellulose in the step 3 is the 15% of three oxidations, two lutetium mole.
The speed that is passed through of carbon dioxide in the step 4 is 10mL/min.
The supersonic frequency of ultrasound filtration in the step 4 is 40-50kHz, and temperature is 70 DEG C.
Freeze-day with constant temperature temperature in the step 5 is 250 DEG C.
Sintering temperature in the step 5 is 1100 DEG C.
Embodiment 3
A kind of preparation method of zinc doping Luetcium aluminum garnet, includes the following steps:
Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 40min,
Mixture is obtained after drying;
Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;
Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;
Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generate, then pass to ammonia until
Precipitation no longer generates, and absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;
Step 5, by mixed precipitation freeze-day with constant temperature 6h, it is cooling after ball mill grinding at powder, then calcine 3h, obtain zinc doping
Luetcium aluminum garnet.
The molar ratio of three two lutetiums of oxidation and alundum (Al2O3) in the step 1 is 3: 5.
A concentration of 80g/L of three two lutetiums of oxidation in absolute ethyl alcohol in the step 1, the frequency of the ultrasonic cleaning are
50kHz, the drying temperature are 65 DEG C.
The mass concentration of hydrochloric acid is 15% in the step 2, the pH most 4. of the mixed liquor
The addition of zinc chloride in the step 3 is the 8% of three oxidations, two lutetium mole.
The addition of hydroxypropyl cellulose in the step 3 is the 13% of three oxidations, two lutetium mole.
The speed that is passed through of carbon dioxide in the step 4 is 8mL/min.
The supersonic frequency of ultrasound filtration in the step 4 is 40-50kHz, and temperature is 60 DEG C.
Freeze-day with constant temperature temperature in the step 5 is 230 DEG C.
Sintering temperature in the step 5 is 1000 DEG C.
Performance detection
Embodiment 1 | Embodiment 2 | Embodiment 3 | |
Transparency | 90% | 92% | 95% |
Particles | 10-50μm | 30-60μm | 10-20μm |
Density | 6.78g/cm3 | 6.80g/cm3 | 6.81g/cm3 |
Dispersibility | Well | Well | Well |
In conclusion the present invention has the following advantages:
1. the present invention solves the technological gap of zinc doping Luetcium aluminum garnet, the doping side of new Luetcium aluminum garnet is provided
Formula.
2. material prepared by the present invention not only improves transparency, material granule tight type, while also improving are promoted
Stability and mechanical strength are learned, zinc ion fills up internal crystal gap and stomata, improves overall performance, particle diameter distribution very well
It is narrow.
3. the present invention using zinc be used as dopant, can improving laser export, in physics, biology, OCT, laser spectrum
The various fields such as, optic communication and Laser focus tool has been widely used.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical solution described in inventive embodiments.It will be understood by those of ordinary skill in the art that still can be carried out to the present invention
Modification or equivalent replacement, to reach identical technique effect;As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of zinc doping Luetcium aluminum garnet, it is characterised in that:Include the following steps:
Step 1, three high-purity two lutetiums of oxidation and alundum (Al2O3) powder are added in absolute ethyl alcohol and are cleaned by ultrasonic 20-50min, dried
Mixture is obtained after dry;
Step 2, it feeds the mixture into hydrochloric acid solution, stirs to being completely dissolved, obtain mixed liquor;
Step 3, zinc chloride and hydroxypropyl cellulose are added and are stirred evenly into mixed liquor, obtain dispersion mixing liquid;
Step 4, carbon dioxide is slowly introducing dispersion mixing liquid, until precipitation no longer generates, then passes to ammonia until precipitation
It no longer generates, absolute ethyl alcohol repeatedly washs after ultrasound filtration, and drying obtains mixed precipitation;
Step 5, by mixed precipitation freeze-day with constant temperature 4-8h, it is cooling after ball mill grinding at powder, then calcine 2-4h, obtain zinc doping
Luetcium aluminum garnet.
2. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 1
In three oxidation two lutetiums and alundum (Al2O3) molar ratio be 3:5.
3. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 1
In three oxidation a concentration of 30-150g/Ls of two lutetiums in absolute ethyl alcohol, the frequency of the ultrasonic cleaning is 40-60kHz, described
Drying temperature is 60-70 DEG C.
4. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 2
The mass concentration of middle hydrochloric acid is 10-20%, the pH most 3-4 of the mixed liquor.
5. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 3
In zinc chloride addition be three oxidations, two lutetium mole 6-10%.
6. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 3
In hydroxypropyl cellulose addition be three oxidations, two lutetium mole 10-15%.
7. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 4
In carbon dioxide be passed through speed be 5-10mL/min.
8. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 4
In ultrasound filtration supersonic frequency be 40-50kHz, temperature be 40-70 DEG C.
9. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 5
In freeze-day with constant temperature temperature be 200-250 DEG C.
10. a kind of preparation method of zinc doping Luetcium aluminum garnet according to claim 1, it is characterised in that:The step 5
In sintering temperature be 900-1100 DEG C.
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Application publication date: 20180921 |