CN107446580A - A kind of preparation method of oxysulfide luminescent powder - Google Patents
A kind of preparation method of oxysulfide luminescent powder Download PDFInfo
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- CN107446580A CN107446580A CN201710656492.3A CN201710656492A CN107446580A CN 107446580 A CN107446580 A CN 107446580A CN 201710656492 A CN201710656492 A CN 201710656492A CN 107446580 A CN107446580 A CN 107446580A
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Abstract
The present invention relates to a kind of preparation method of oxysulfide luminescent powder, the chemical composition formula of the oxysulfide luminescent powder is：R2(1‑x)M2xO2S, wherein R are at least one of Y, Gd, La, Lu, at least one of M Pr, Ce, Tb, Eu, Yb, Nd, Er, Ho, 0≤x ＜ 1, it is preferable that 1 × 10‑6≤x≤5×10‑2, the synthetic method comprises the following steps：（1）By R2O3The M stoichiometrically matched2O3Mixture be dissolved in nitric acid and be made into rare earth nitrate solution；（2）By the rare earth nitrate solution and precipitant mix of gained, precipitation suspension is obtained, precursor powder will be obtained after precipitation separation, washing, drying；（3）The precursor powder of gained is vulcanized in sulfur-bearing atmosphere in 600~1300 DEG C, obtains the oxysulfide luminescent powder.Present invention process is simple and easy, and reaction efficiency is high, can obtain high-purity, ultra-fine, the oxysulfide luminescent powder of high-specific surface area and high sintering activity.
Description
Technical field
The present invention relates to a kind of synthetic method of oxysulfide luminescent powder, belong to field of ceramic preparation.
Background technology
Rare earth oxysulfide phosphor and ceramic scintillator are widely used in its excellent optical property and density feature
The fields, wherein Gd such as medical imaging, national defence safety check, industrial nondestructive testing2O2S:Pr is a sudden strain of a muscle general in current medical x-CT
Bright body, High Light Output (1.8xCdWO is collected with it4), low twilight sunset (<100ppm@100ms), and high density (7.34g/cm3) etc. it is excellent
Performance is.The synthesis of rare-earth oxide sulfate is significant for preparing high performance ceramic scintillator.GOS dodges at present
Bright body is controlled by Siemens, the company of Hitachi, Toshiba tri- substantially, and each family of powder synthetic technology is different, wherein
Using sulphite precipitation reducing process (Sulfite precipitation reduction), Hitachi is then used Siemens
Oxalate precipitation combination flux growth metrhod, and Toshiba then uses rare earth oxide and flux growth metrhod.However, traditional sulphite
Precipitation method reaction efficiency is low, and heating causes SO2Volatilization pollution environment；And oxysulfide particle prepared by traditional flux growth metrhod
Thick, specific surface area is low, and sintering activity is poor.
The content of the invention
To overcome the reaction efficiency in traditional sulphite precipitation low and SO caused by heating2Volatilization pollution environment is asked
Topic, and oxysulfide particle prepared by traditional flux growth metrhod are thick, and specific surface area is low, the problem of sintering activity difference, this hair
Bright to provide a kind of reaction efficiency high, environment-friendly, and the oxysulfide particle of gained is high-purity, ultra-fine, high-specific surface area and high fever
The synthetic method of the oxysulfide luminescent powder of activity, and the oxysulfide luminescent powder synthesized by the synthetic method are tied, by
Oxysulfide ceramic scintillator prepared by the oxysulfide luminescent powder.
On the one hand, the present invention provides a kind of synthetic method of oxysulfide luminescent powder, the oxysulfide luminescent powder
Chemical composition formula be：R2(1-x)M2xO2S, wherein R are at least one of Y, Gd, La, Lu, M Pr, Ce, Tb, Eu, Yb,
At least one of Nd, Er, Ho, 0≤x ＜ 1, it is preferable that 0 ＜ x ＜ 1, it is highly preferred that 1 × 10-6≤x≤5×10-2,
The synthetic method comprises the following steps：
(1) by R2O3The M stoichiometrically matched2O3Mixture be dissolved in nitric acid and be made into rare earth nitrate solution；
(2) by the rare earth nitrate solution and precipitant mix of gained, precipitation suspension is obtained, by precipitation separation, washing, is dried
After obtain precursor powder；
(3) precursor powder of gained is vulcanized in sulfur-bearing atmosphere in 600~1300 DEG C, obtains the oxysulfide hair
Light powder.
A kind of method that the present invention is directly vulcanized using presoma, i.e., the rare earth required for being obtained using coprecipitation technology are sunk
Shallow lake presoma, then directly vulcanized using sulphur source and obtain oxysulfide luminescent powder.Present invention process is simple and easy, reaction efficiency
Height, high-purity, ultra-fine, the oxysulfide luminescent powder of high-specific surface area and high sintering activity can be obtained.
It is preferred that in step (1), the concentration of nitric acid is 30~90%, in the rare earth nitrate solution, R ions
Concentration is 0.001~10mol/L.
It is preferred that in step (2), the precipitating reagent is oxalic acid, ammonium oxalate, ammoniacal liquor, ammonium hydrogen carbonate, ammonium carbonate, hydroxide
At least one of sodium, potassium hydroxide.
It is preferred that the mol ratio of precipitating reagent and all metal ions in rare earth nitrate solution is 0.5：1~5：1.
It is preferred that in step (2), drying temperature is 40~120 DEG C.
It is preferred that in step (3), the sulfur-bearing atmosphere is SO2、H2S or Ar gas steams as the sulphur simple substance that carrier gas carries
At least one of gas.
It is preferred that in step (3), 0.5~8 hour is incubated in 600~1300 DEG C.
On the other hand, the present invention also provides a kind of oxysulfide luminescent powder synthesized by above-mentioned synthetic method, the sulphur
The particle size of oxide luminescent powder is less than 10 μm, specific surface area 5m2/ more than g.
Another further aspect, the present invention also provide a kind of oxysulfide ceramic scintillator, and its above-mentioned oxysulfide luminescent powder burns
Tie and obtain.
The preparation method of oxysulfide provided by the invention, it is the characteristics of its technique：
(1) have technique simple using the direct vulcanization method of presoma, settle at one go, the advantages of energy-conserving and environment-protective；
(2) there is higher specific surface area and purity, higher burning using the oxysulfide powder of the technology of the present invention route synthesis
Knot activity so that the powder that obtains of the technique by without pressure pre-burning and high temperature insostatic pressing (HIP) or independent hot pressed sintering relatively low
At a temperature of can realize complete densification.
Brief description of the drawings
Fig. 1 is the XRD spectrum of oxysulfide powder prepared by the present invention, and it is the single side of oxysulfide six to show product
Phase；
Fig. 2 is the shape appearance figure of the typical oxysulfide obtained using present invention process, and powder granule is with spherical shape
Looks.
Embodiment
The present invention is further illustrated below in conjunction with accompanying drawing and following embodiments, it should be appreciated that accompanying drawing and following embodiments
The present invention is merely to illustrate, is not intended to limit the present invention.
The present invention provides a kind of synthetic method of oxysulfide luminescent powder.The chemical composition of the oxysulfide luminescent powder
It can be expressed as with formula：R2(1-x)M2xO2One or more combinations in S, R Y, Gd, La, Lu, M Pr, Ce, Tb, Eu, Yb,
One or more in Nd, Er, Ho, 0≤x ＜ 1, it is preferable that 0 ＜ x ＜ 1, it is highly preferred that 1 × 10-6≤x≤5×10-2, enter
One step preferably, 2 × 10-6≤x≤5×10-3.A kind of method that the present invention is directly vulcanized using presoma, i.e., using co-precipitation
Technique obtains required rare-earth precipitation presoma, is then directly vulcanized using sulphur source and obtains oxysulfide luminescent powder.Hereinafter, make
For example, the method for illustrating the present invention.
First, by R2O3The M stoichiometrically matched2O3Mixture be dissolved in nitric acid and be made into rare earth nitrate solution.
That is, M2O3Account for M2O3And R2O3Material amount sum ratio (i.e. mol ratio) can be 1 × 10-6To 5 × 10-2Between.R2O3It is commercially available
From commercialization, its purity can be more than 4N.M2O3Commercialization is purchased from, its purity can be more than 4N.Nitric acid used can be dust technology,
Such as its concentration can be 30%~90%.R2O3And M2O3The gross mass of mixture and the volume ratio of nitric acid can be 1g：(1~5)
mL.In one example, the ratio of nitric acid and RE oxide powder is about 1.5ml (65% nitric acid)：1g oxides.It is being formulated
Rare earth nitrate solution in, the concentration of R ions can be 0.001~10mol/L, and the concentration of M ions can be 0.001~10mol/
L.Contain rare earth nitrades in rare earth nitrate solution, and can contain and react remaining nitric acid (that is, nitric acid typically can be excessively), sink
Shallow lake agent is preferential after adding to neutralize excessive nitric acid.Rare earth nitrades are dissolved in into water compared to directly, and to be configured to rare earth nitrades molten
Rare earth oxide is dissolved in nitric acid and is made into rare earth nitrate solution by liquid, the present invention, can save cost.The nitrate that cause is bought is all
It is not high with respect to cost performance containing the different degrees of crystallization water.
Then, using coprecipitation technology, R is prepared2(1-x)M2xO3Presoma.Specifically, by rare earth nitrate solution
Mixed under agitation with precipitating reagent, precipitation (such as white precipitate) is generated with reaction.Reaction temperature can be RT (room temperature)~100
℃.Reaction time can be 1~1000 minute.In the present invention, precipitating reagent can be oxalic acid, ammonium oxalate, or alkaline precipitating agent, example
Such as the one or more combination in ammoniacal liquor, ammonium hydrogen carbonate, ammonium carbonate, sodium hydroxide, potassium hydroxide, urea.Precipitating reagent can be made into
Mixed after the aqueous solution with rare earth nitrate solution.The concentration of the precipitating reagent aqueous solution can be 0.1~10mol/L.Rare earth nitrades are molten
The order by merging of liquid and precipitating reagent is unlimited, such as can add rare earth nitrate solution into precipitating reagent, or precipitating reagent is added
Into rare earth nitrate solution.It during mixing, can directly mix, can also be mixed by the way of being added dropwise (positive to drip anti-drop drop altogether
).The mol ratio of precipitating reagent and all metal ions in rare earth nitrate solution can be 0.5：1~10：1, preferably 1：1
~5：1, more preferably 3:1~6:1, further preferred 3.5:1~4.5:1.When using alkaline precipitating agent, the dosage of precipitating reagent can
To make the pH of mixed solution be 7.0~14.0, preferably 8.0~12.By the precipitation separation of gained, washing, dry, obtain presoma
Powder.Such as the precipitation of gained can be filtered, the filtration cakes torrefaction washed after being washed with alcohol.Drying temperature can be 40~120 DEG C.
The precursor powder of gained is directly vulcanized, you can obtain oxysulfide luminescent powder.Sulphur source can be simple substance
One or more combinations in sulphur, hydrogen sulfide or sulfur dioxide, for the angle of environmental protection, preferably sulphur simple substance, other two gas
Body is poisonous and harmful.Gas cure method can be used in the present invention.Specifically, lead into the container equipped with precursor powder
Enter sulfurous gas.Sulfurous gas can be SO2、H2The sulphur simple substance steam that S or Ar gas carries as carrier gas.Curing temperature can be
600~1300 DEG C, preferably 800~1200 DEG C.Soaking time can be 0.5~8 hour.It is in the present invention, precursor powder is straight
Capable vulcanization is tapped into, without being calcined before vulcanization, so can not only simplify technique, and vulcanize the oxysulfide phase obtained
Purity is high, and particle is relatively thinner.
In sulfidation, caused tail gas can use the absorption tower containing NaOH to fully absorb, without being emitted into air
Middle pollution environment.
Oxysulfide luminescent powder produced by the present invention has high-purity, understands that its purity can be more than 99.5% by XRD,
Its pattern is spherical, and has thinner particle size, such as d<10 μm, or even d<500nm, and higher specific surface area
(SSA>5m2/g)。
Moreover, oxysulfide luminescent powder produced by the present invention has high sintering activity, by quiet without pressure pre-burning combination heat etc.
Densification completely individually can be achieved in pressure using heat pressing process.In one example, by oxysulfide powder and low melting point
Sintering aid mixing, ball milling, obtain mixed powder, the low melting point sintering aid can be LiF, Li2GeF6、LiBF4、Li2B4O7
At least one of.The addition of the low melting point sintering aid is 0.01wt%~5wt% of oxysulfide powder.Ball milling
When, ball-milling medium is aluminum oxide or zirconia ball, and solvent is water or ethanol, and ball milling pearl material is than 1:1~10:1, rotating speed 50rpm
~500rpm, 1~50 hour duration.Then, gained mixed powder is molded, obtains biscuit.Shaping can be to carry out successively
Dry-pressing formed and cold isostatic compaction, wherein dry-pressing formed pressure is 20~50Mpa, cold isostatic compaction pressure is 100~
200Mpa.Biscuit is subjected to pressureless sintering under vacuum or protective atmosphere, sintering temperature can be 1100~1500 DEG C, soaking time
It can be 1~10 hour, obtain pre-sintered body.Gained pre-sintered body is subjected to HIP sintering, sintering temperature under protective atmosphere
Degree can be 1100~1500 DEG C, and pressure can be 100~250Mpa, and soaking time can be 1~20 hour, obtain oxysulfide ceramics
Scintillator.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by this paper explanation
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Method of testing：
Purity：XRD X-ray diffractometers；
Particle diameter：LPS laser particle analyzers；
Specific surface area：BET nitrogen adsorption methods.
Embodiment 1
Weigh 50g Gd2O3, 0.1g Pr6O11With 0.01g CeO2, it is dilute that mixing adds acquisition in 30mL nitric acid (concentration 68%)
Native nitrate solution.Above-mentioned rare earth nitrate solution is added in 45mL ammoniacal liquor (concentration 2mol/l), makes the pH of mixed solution
For 10, reacted about 0.5 hour in room temperature~50 degree, you can there is white precipitate, the white suspension solution is filtered repeatedly, in
100 degree of drying, produce presoma.Presoma is placed in 850 DEG C of tube furnaces again, is passed through H2S gases, continue 3h, produce
Gd2O2S:Pr, Ce pure phase luminescent powder.
Fig. 1 shows the XRD spectrum of oxysulfide powder made from embodiment 1, and it is single oxysulfide six to show product
Fang Xiang.Fig. 2 is the shape appearance figure for the oxysulfide that embodiment 1 obtains, it can be seen that powder granule is with spherical pattern.Through
Test, the purity of the oxysulfide powder of gained is 100%, average grain diameter 30nm, specific surface area 10m2/g。
Embodiment 2：
Weigh 50g Gd2O3, 0.15g Pr6O11With 0.02g CeO2, it is dilute that mixing adds acquisition in 30mL nitric acid (concentration 68%)
Native nitrate solution.Above-mentioned rare earth nitrate solution is added in 50ml ammonium hydrogen carbonate (concentration 1.5mol/l), makes mixing molten
The pH of liquid is 9, is reacted about 0.5 hour in room temperature~40 degree, you can white precipitate occur, the white suspension solution is taken out repeatedly
Filter, in 100 degree of drying, produce presoma.Presoma is placed in 900 DEG C of tube furnaces again, is passed through SO2Gas, continue 3h, produce
Gd2O2S:Pr, Ce pure phase luminescent powder.XRD is shown as pure phase (substantially with embodiment 1), and granularity about 100nm, specific surface area is about
8m2/g。
Embodiment 3：
Weigh 50g Gd2O3, 0.8Pr6O11With 0.015g CeO2, mixing, which adds, obtains rare earth in 50mL nitric acid (concentration 68%)
Nitrate solution.Above-mentioned rare earth nitrate solution is added in 100g urea (concentration 3mol/l), the pH for making mixed solution is
9, reacted about 6 hours in 85-90 degree, you can there is white precipitate, the white suspension solution is filtered repeatedly, dried in 100 degree,
Produce presoma.Again by presoma and sulphur powder in 1100 DEG C of tube furnaces under inert atmosphere Ar gas shieldeds, sustained response 3h, i.e.,
Obtain Gd2O2S:Pr, Ce pure phase luminescent powder.XRD is shown as pure phase (substantially with embodiment 1), and granularity about 500nm, specific surface area is about
5m2/g。
Claims (9)
- A kind of 1. synthetic method of oxysulfide luminescent powder, it is characterised in that the chemical group of the oxysulfide luminescent powder It is into formula：R2(1-x)M2xO2S, wherein R are at least one of Y, Gd, La, Lu, M Pr, Ce, Tb, Eu, Yb, Nd, Er, Ho At least one of, 0≤x ＜ 1, it is preferable that 1 × 10-6≤x≤5×10-2,The synthetic method comprises the following steps：（1）By R2O3The M stoichiometrically matched2O3Mixture be dissolved in nitric acid and be made into rare earth nitrate solution；（2）By the rare earth nitrate solution and precipitant mix of gained, precipitation suspension is obtained, by precipitation separation, washing, is dried After obtain precursor powder；（3）The precursor powder of gained is vulcanized in sulfur-bearing atmosphere in 600~1300 DEG C, obtains the oxysulfide hair Light powder.
- 2. synthetic method according to claim 1, it is characterised in that step（1）In, the concentration of nitric acid is 30~90%, In the rare earth nitrate solution, the concentration of R ions is 0.001~10mol/L.
- 3. synthetic method according to claim 1 or 2, it is characterised in that step（2）In, the precipitating reagent is oxalic acid, grass At least one of sour ammonium, ammoniacal liquor, ammonium hydrogen carbonate, ammonium carbonate, sodium hydroxide, potassium hydroxide.
- 4. synthetic method according to any one of claim 1 to 3, it is characterised in that（2）In, precipitating reagent and rare earth nitre The mol ratio of all metal ions in acid salt solution is 0.5：1~5：1.
- 5. synthetic method according to any one of claim 1 to 4, it is characterised in that step（2）In, drying temperature is 40~120 DEG C.
- 6. synthetic method according to any one of claim 1 to 5, it is characterised in that step（3）In, the sour gas Atmosphere is SO2、H2At least one of sulphur simple substance steam that S or Ar gas carries as carrier gas.
- 7. synthetic method according to any one of claim 1 to 5, it is characterised in that step（3）In, in 600~1300 DEG C insulation 0.5~8 hour.
- 8. the oxysulfide luminescent powder that a kind of synthetic method by any one of claim 1 to 7 synthesizes, its feature exist In the particle size of the oxysulfide luminescent powder is less than 10 μm, specific surface area 5m2/ more than g.
- 9. a kind of oxysulfide ceramic scintillator, it is characterised in that as the oxysulfide luminescent powder sintering described in claim 8 And obtain.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249920A (en) * | 2018-03-14 | 2018-07-06 | 上海科炎光电技术有限公司 | A kind of CT detects material with efficient nano |
| CN111439775A (en) * | 2020-06-05 | 2020-07-24 | 眉山博雅新材料有限公司 | Method for preparing GOS-doped scintillation powder |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062484A (en) * | 2015-08-04 | 2015-11-18 | 温州医科大学 | Rare earth oxysulfide upconversion nanotube and preparation method thereof |
| CN105602564A (en) * | 2016-03-03 | 2016-05-25 | 盐城工学院 | Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof |
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2017
- 2017-08-03 CN CN201710656492.3A patent/CN107446580B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062484A (en) * | 2015-08-04 | 2015-11-18 | 温州医科大学 | Rare earth oxysulfide upconversion nanotube and preparation method thereof |
| CN105602564A (en) * | 2016-03-03 | 2016-05-25 | 盐城工学院 | Zn reinforced rare earth sulfur oxide up-conversion luminescent material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108249920A (en) * | 2018-03-14 | 2018-07-06 | 上海科炎光电技术有限公司 | A kind of CT detects material with efficient nano |
| CN111439775A (en) * | 2020-06-05 | 2020-07-24 | 眉山博雅新材料有限公司 | Method for preparing GOS-doped scintillation powder |
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