CN104310454A - Process method of rare earth oxysulfide by using alkali chloride - Google Patents
Process method of rare earth oxysulfide by using alkali chloride Download PDFInfo
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- CN104310454A CN104310454A CN201410504355.4A CN201410504355A CN104310454A CN 104310454 A CN104310454 A CN 104310454A CN 201410504355 A CN201410504355 A CN 201410504355A CN 104310454 A CN104310454 A CN 104310454A
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- rare
- mol
- alkali metal
- rare earth
- earth oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/288—Sulfides
- C01F17/294—Oxysulfides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a process method of rare earth oxysulfide by using an alkali chloride. The method comprises the following steps: (1) weighing required materials RE2O2S (wherein RE is one of rare earth elements Y, La, Gd and Sm), Na2CO3, sublimed sulfur and alkali chloride AMCl (wherein AM is one of alkali metal elements Li, Na or K) according to a stoichiometric ratio and uniformly mixing the weighed materials; (2) putting the uniformly mixed materials into inner and outer crucibles, and filling high-temperature powder in the gap between the two crucibles and compacting, where each of the two crucibles has a cover; (3) raising the temperature of the crucibles with the mixed material to 1100-1250 DEG C in a gradient way, sintering for 3-5 hours and then cooling to room temperature along with a furnace; (4) washing the sintered product with hot water, stirring, and carrying out suction filtration; and (5) drying the washed product into a constant-temperature blowing drying box to obtain the rare earth oxysulfide. By taking RE2O3, Na2CO3, sublimed sulfur and alkali chloride AMCl as raw materials, the rare earth oxysulfide is prepared by using a sulfur melting method. The preparation method of the rare earth oxysulfide is simple and easy to operate and the rare earth oxysulfide can be used in the fields of light-emitting materials and photoabsorption materials and the like.
Description
Technical field
The present invention relates to the processing method that a kind of alkali metal chloride prepares rare-earth oxide sulfate, the sulphur particularly relating to rare-earth oxide sulfate melts method preparation and modification, and the preparation of narrow size distribution rare-earth oxide sulfate and optimization.
Background technology
Rare-earth oxide sulfate has higher chemical stability and thermostability, water insoluble, and fusing point is up to 2000 ~ 2200 DEG C; Energy gap is 4.6 ~ 4.8eV, is suitable for dopant ion; Its maximum phonon energy is 520cm
-1, be suitable for the substrate material as luminescent material, there is very high photoabsorption and energy transfer efficiency.Hexagonal Ln
2o
2the maximum feature of S crystalline structure has more spacious space structure, allows a certain amount of positively charged ion and anion vacancy to be formed and a certain amount of gap ion enters, and crystalline structure remains unchanged substantially.Wherein La
2o
2s, Y
2o
2s and Gd
2o
2s as the substrate material of luminescent material, by doping Eu
3+, Tb
3+, Ce
3+deng light emitting ionic ultraviolet and vacuum ultraviolet-excited under there is good luminescent properties, and Sm
2o
2s, as optical absorbing material, has good optical absorption characteristics to 1.06 μm and 1.54 μm of laser.Therefore, rare-earth oxide sulfate is widely used as optical material.The main preparation method of rare-earth oxide sulfate is that sulphur melts method, and be applicable to industrial mass production, crystal perfection, luminescent properties is better than product prepared by additive method.But sulphur melts the fusing assistant consumption of method and kind is not fixed, and goes back the scope that neither one is clear and definite.Current sulphur melts the standby rare-earth oxide sulfate of legal system, and the particle of product is comparatively large, need ball milling, luminescent properties is reduced greatly, and the distribution of sizes of particle remains to be further improved.Therefore optimize sulphur and melt the technological process of legal system for rare-earth oxide sulfate, the physical property of particle improving rare-earth oxide sulfate is very important.
Summary of the invention
The technical problem to be solved in the present invention overcomes above-mentioned defect, and melting method by the sulphur that alkali metal chloride AMCl is auxiliary, to prepare chemical formula be RE
2o
2the rare-earth oxide sulfate of S.
For solving the problem, the present invention adopts following technical scheme to be:
Alkali metal chloride prepares a processing method for rare-earth oxide sulfate, it is characterized in that, in described alkali metal chloride AMCl, AM is the one in alkali metal Li, Na or K; Described rare-earth oxide sulfate chemical formula is RE
2o
2in S, RE is the one in rare earth element y, La, Gd or Sm; Described chemical formula is RE
2o
2it is standby that the rare-earth oxide sulfate of S melts legal system by sulphur, and its preparation process is as follows:
1. required material RE is stoichiometrically taken
2o
2s (wherein RE is the one in rare earth element y, La, Gd or Sm), Na
2cO
3, sublimed sulphur and alkali metal chloride AMCl (wherein AM is the one in alkali metal Li, Na or K), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. crucible gradient increased temperature to 1100 ~ 1250 DEG C of compound will be housed, sintering 3h ~ 5h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, can rare-earth oxide sulfate be obtained.
Described step is middle mol (Na 1.
2cO
3): mol (RE
2o
3)=1.5 ~ 2, mol (sublimed sulphur): mol (RE
2o
3)=3.5 ~ 4.5, mol (AMCl): mol (RE
2o
3)=0.25 ~ 1.
Described step 3. middle gradient increased temperature system is warmed up to 300 ~ 400 DEG C with temperature rise rate 2 ~ 3 DEG C/min, and be incubated 1h ~ 2h, is then warmed up to 1100 ~ 1250 DEG C with temperature rise rate 3 ~ 5 DEG C/min, and is incubated 3h ~ 5h.
Rare-earth oxide sulfate of the present invention is with RE
2o
3(wherein RE is the one in rare earth element y, La, Gd or Sm), Na
2cO
3, sublimed sulphur and alkali metal chloride AMCl (wherein AM is the one in alkali metal Li, Na or K) be raw material, adopt sulphur to melt legal system standby, preparation synthetic method is simple, easy to operate.
The rare-earth oxide sulfate La of the present invention's synthesis
2o
2s, Y
2o
2s and Gd
2o
2s as the substrate material of luminescent material, by doping Eu
3+, Tb
3+or Ce
3+deng light emitting ionic ultraviolet and vacuum ultraviolet-excited under there is good luminescent properties, and Sm
2o
2s is as optical absorbing material, to 1.06 μm and 1.54 μm of laser, there is good optical absorption characteristics, it is by the selection to alkali metal chloride kind and consumption, adopts sulphur to melt method and prepares the narrow rare-earth oxide sulfate of size distribution, thus may be used for the field such as luminescent material and light absorbing material.In addition, this invention exploits a kind of novelty teabag of alkali metal chloride, reduce the particle distribution range of rare-earth oxide sulfate, make product not need ball milling, reduce production cost.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
It is RE that the sulphur that the present invention's alkali metal chloride is assisted melts method synthetic chemistry formula
2o
24 specific embodiments of the rare-earth oxide sulfate of S (wherein RE is the one in rare earth element y, La, Gd or Sm) are as shown in table 1:
Table 1
Embodiment 1
#:
Raw material composition is as in table 11
#shown in, concrete preparation method comprises the following steps:
1. 18.672g Y is taken by weight
2o
3, 13.146g Na
2cO
3(mol (Na
2cO
3): mol (Y
2o
3)=1.5), 9.280g sublimed sulphur (mol (sublimed sulphur): mol (Y
2o
3)=3.5) and 0.876gLiCl (mol (LiCl): mol (Y
2o
3)=0.25), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. the crucible that compound is housed is warmed up to 300 DEG C with temperature rise rate 2 DEG C/min, and is incubated 1h, be then warming up to 1100 DEG C with temperature rise rate 3 DEG C/min, sintering 3h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, obtain rare-earth oxide sulfate.
As follows to the test result of this rare-earth oxide sulfate:
By process 5. in dry after powder carry out crystal species analysis with X-ray diffractometer (XRD, D/Max2500), result display main diffraction peak position all with six side Y
2o
2s-phase is corresponding, and does not have the peak of other material phases; Carry out granule-morphology analysis by scanning electronic microscope (SEM, JEOL-6310), and adopt software to carry out particle size statistics, result display even particle distribution, average particle size particle size is 3 μm.
Embodiment 2
#:
1. 19.060g La is taken by weight
2o
3, 10.541g Na
2cO
3(mol (Na
2cO
3): mol (La
2o
3)=1.7), 7.034g sublimed sulphur (mol (sublimed sulphur): mol (La
2o
3)=3.75) and 1.709gNaCl (mol (NaCl): mol (La
2o
3)=0.5), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. the crucible that compound is housed is warmed up to 330 DEG C with temperature rise rate 2.5 DEG C/min, and is incubated 1.5h, be then warming up to 1150 DEG C with temperature rise rate 3.5 DEG C/min, sintering 4h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, obtain rare-earth oxide sulfate.
As follows to the test result of this rare-earth oxide sulfate:
By process 5. in dry after powder carry out crystal species analysis with X-ray diffractometer (XRD, D/Max2500), result display main diffraction peak position all with six side La
2o
2s-phase is corresponding, and does not have the peak of other material phases; Carry out granule-morphology analysis by scanning electronic microscope (SEM, JEOL-6310), and adopt software to carry out particle size statistics, result display even particle distribution, average particle size particle size is 2.3 μm.
Embodiment 3
#:
Form as in table 13
#shown in, concrete preparation method comprises the following steps:
1. 19.151gGd is taken by weight
2o
3, 10.639g Na
2cO
3(mol (Na
2cO
3): mol (Gd
2o
3)=1.9), 7.200g sublimed sulphur (mol (sublimed sulphur): mol (Gd
2o
3)=4.25) and 2.954gKCl (mol (KCl): mol (Gd
2o
3)=0.75), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. the crucible that compound is housed is warmed up to 360 DEG C with temperature rise rate 3 DEG C/min, and is incubated 2h, be then warming up to 1200 DEG C with temperature rise rate 4 DEG C/min, sintering 5h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, obtain rare-earth oxide sulfate.
As follows to the test result of this rare-earth oxide sulfate:
By process 5. in dry after powder carry out crystal species analysis with X-ray diffractometer (XRD, D/Max2500), result display main diffraction peak position all with six side Gd
2o
2s-phase is corresponding, and does not have the peak of other material phases; Carry out granule-morphology analysis by scanning electronic microscope (SEM, JEOL-6310), and adopt software to carry out particle size statistics, result display even particle distribution, average particle size particle size is 1.8 μm.
Embodiment 4
#:
Form as in table 14
#shown in, concrete preparation method comprises the following steps:
1. 19.119gSm is taken by weight
2o
3, 11.620g Na
2cO
3(mol (Na
2cO
3): mol (Sm
2o
3)=2), 7.910g sublimed sulphur (mol (sublimed sulphur): mol (Sm
2o
3)=4.5) and 4.087gKCl (mol (KCl): mol (Sm
2o
3)=1), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. the crucible that compound is housed is warmed up to 400 DEG C with temperature rise rate 2.5 DEG C/min, and is incubated 2h, be then warming up to 1250 DEG C with temperature rise rate 5 DEG C/min, sintering 4h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, obtain rare-earth oxide sulfate.
As follows to the test result of this rare-earth oxide sulfate:
By process 5. in dry after powder carry out crystal species analysis with X-ray diffractometer (XRD, D/Max2500), result display main diffraction peak position all with six side Sm
2o
2s-phase is corresponding, and does not have the peak of other material phases; Carry out granule-morphology analysis by scanning electronic microscope (SEM, JEOL-6310), and adopt software to carry out particle size statistics, result display even particle distribution, average particle size particle size is 2.0 μm.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention, to be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (3)
1. prepare a processing method for rare-earth oxide sulfate with alkali metal chloride, it is characterized in that, in described alkali metal chloride AMCl, AM is the one in alkali metal Li, Na or K; Described rare-earth oxide sulfate chemical formula is RE
2o
2in S, RE is the one in rare earth element y, La, Gd or Sm; Described chemical formula is RE
2o
2it is standby that the rare-earth oxide sulfate of S melts legal system by sulphur, and its preparation process is as follows:
1. required material RE is stoichiometrically taken
2o
2s (wherein RE is the one in rare earth element y, La, Gd or Sm), Na
2cO
3, sublimed sulphur and alkali metal chloride AMCl (wherein AM is the one in alkali metal Li, Na or K), by even for the mixing of materials weighed up;
2. in set crucible all with cover inside and outside the material that mixes being loaded, in the gap-fill high temperature resistant powder of two crucibles and compacting;
3. crucible gradient increased temperature to 1100 ~ 1250 DEG C of compound will be housed, sintering 3h ~ 5h, is then cooled to room temperature with stove;
4. the product hot wash after sintering is also stirred, suction filtration;
5. the product after washing is put into constant temperature blast drying oven to dry, can rare-earth oxide sulfate be obtained.
2. a kind of alkali metal chloride according to claim 1 prepares the processing method of rare-earth oxide sulfate, it is characterized in that, described step is middle mol (Na 1.
2cO
3): mol (RE
2o
3)=1.5 ~ 2, mol (sublimed sulphur): mol (RE
2o
3)=3.5 ~ 4.5, mol (AMCl): mol (RE
2o
3)=0.25 ~ 1.
3. a kind of alkali metal chloride according to claim 1 prepares the processing method of rare-earth oxide sulfate, it is characterized in that, described step 3. middle gradient increased temperature system is warmed up to 300 ~ 400 DEG C with temperature rise rate 2 ~ 3 DEG C/min, and be incubated 1h ~ 2h, then be warmed up to 1100 ~ 1250 DEG C with temperature rise rate 3 ~ 5 DEG C/min, and be incubated 3h ~ 5h.
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Cited By (3)
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|---|---|---|---|---|
| CN105129833A (en) * | 2015-07-13 | 2015-12-09 | 盐城工学院 | Method of preparing rare earth oxysulfide with carbon disulfide |
| CN106929018A (en) * | 2017-03-13 | 2017-07-07 | 盐城工学院 | A kind of laser protective material and preparation method thereof |
| CN110203960A (en) * | 2019-06-28 | 2019-09-06 | 南阳师范学院 | A kind of rare earth oxysulfide and preparation method thereof as lube oil additive |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105129833A (en) * | 2015-07-13 | 2015-12-09 | 盐城工学院 | Method of preparing rare earth oxysulfide with carbon disulfide |
| CN106929018A (en) * | 2017-03-13 | 2017-07-07 | 盐城工学院 | A kind of laser protective material and preparation method thereof |
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