CN101239398A - Method for preparing yttrium-gadolinium-europium nano powder by coprecipitation method - Google Patents
Method for preparing yttrium-gadolinium-europium nano powder by coprecipitation method Download PDFInfo
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- CN101239398A CN101239398A CNA2008100107056A CN200810010705A CN101239398A CN 101239398 A CN101239398 A CN 101239398A CN A2008100107056 A CNA2008100107056 A CN A2008100107056A CN 200810010705 A CN200810010705 A CN 200810010705A CN 101239398 A CN101239398 A CN 101239398A
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Abstract
A method for preparing Yttrium-Gadolinium-Europium nano powder by using coprecipitation method is provided, relating to a preparing method of a chemical industry raw material. The method comprises following steps: 1) weighting rare-earth oxide Y2O3, Gd2O3 and Eu2O3 according to components ratio of (Y<1-x>Gd<0.3>Eu<x>)2O3, and dissolving them in thick hydrochloric acid, adding distilled water to prepare rare earth liquor; preparing aqueous ammonia as a precipitating agent; 2) dropping aqueous ammonia as a precipitating agent into prepared rare earth liquor to obtain a precursor which is cleaned, suction filtered, dried after time limitation, and the precursor powder is obtained by screening; 3) roasting the precursor powder, ball milling same to obtain a powder sample. The invention prepares powder by using wet chemical coprecipitation method, the obtained (Y, Gd)2O3:Eu3+ powder has good dispersibility, and the average primary grain diameter is 20nm. The preparing method is provided with a simple technique, a short period, a low cost, and is suitable for lot production.
Description
Technical field
The present invention relates to a kind of preparation method of industrial chemicals, particularly relate to the preparation method of a kind of nuclear medicine technology, X-ray detector, the required crucial powder body material of Non-Destructive Testing core material scintillating ceramic.
Background technology
In the nuclear medicine technology, scintillator is important optical function material, mainly comprises inorganic scintillation crystal and scintillating ceramic.The preparation of inorganic scintillating ceramic need have the nano-powder of superperformance, to reducing sintering temperature, realizing that uniform crystal particlesization plays an important role.Mix easily evenly in the powder preparation process, technology is simple, and advantages such as with low cost and good mechanical processability have become the first-selected object of X-CT with the flash detection material.
(Y, Gd)
2O
3: Eu
3+By host material Y
2O
3, Gd
2O
3With luminous active ions Eu
3+Form, belong to cubic crystal structure, optical isotropy has high density (5.92g/cm
3), short die-away time (＜10
-3S), short persistence advantages such as (＜0.01%) is a kind of high efficiency X ray luminous material.In recent years (Y, Gd)
2O
3: Eu
3+Powder has been applied in the nuclear medicine field through the crystalline ceramics and the photomultiplier composition electrooptical device of the preparation of special sintering technology, but the powder of its preparation good characteristic reduces preparation cost, realizes that simple process is the problem that the new material research field need solve always.
Preparation yittrium oxide and yttria-base powder mainly contain firing method, microemulsion method, chemical vapour deposition technique etc. both at home and abroad at present.The synthetic Y of firing method in the above-mentioned powder synthetic method
2O
3: the Eu powder granule is big, reunion is serious, and the luminescent properties of powder is poor; The Y of microemulsion method preparation
2O
3The particle diameter of powder is little, but complex process, the cost height yields poorly, and is not suitable for suitability for industrialized production; Chemical vapour deposition technique production equipment costliness is difficult to realize industrialization.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing yttrium-gadolinium-europium nano powder by coprecipitation method, this method by with ammoniacal liquor be that the coprecipitation of precipitating reagent prepares that a kind of particle diameter is little, good dispersion (Y, Gd)
2O
3: Eu
3+Nano-powder, the powder granularity narrowly distributing that makes, active strong, doping with rare-earth ions is even, is beneficial to reduce its sintering character, low production cost, is easy to realize industrialization.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of preparing yttrium-gadolinium-europium nano powder by coprecipitation method, this method comprises the steps:
1) configuration of solution: by (Y
1-xGd
0.3Eu
x)
2O
3Component takes by weighing rare earth oxide Y
2O
3, Gd
2O
3, Eu
2O
3, and it is dissolved in the concentrated hydrochloric acid, add distilled water, be configured to the earth solution that concentration is 0.01～1mol/L; Precipitating reagent ammoniacal liquor is configured to the weak aqua ammonia that concentration is 0.1～6mol/L;
2) preparation of presoma: above-mentioned precipitating reagent ammoniacal liquor is added drop-wise in the earth solution that configures, the precursor precipitate that obtains is behind timeliness 0～4h, clean with distilled water and absolute ethyl alcohol, suction filtration, place precursor precipitate drying box dry again, baking temperature is 70～130 ℃, and be 8～24h drying time, again through sieve precursor powder;
3) preparation of powder:, can make powder sample behind the ball milling with the above-mentioned precursor powder calcining that makes.
The method of aforesaid a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method, it is with Eu
2O
3The Eu that form is mixed up
3+Doping content be 1mol%～10mol%.
The method of aforesaid a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method, it is when titration, and environment temperature is 0～20 ℃, and rate of titration is 1～5ml/min, and the precipitation pH value of back regulation system fully is 7～12.
The method of aforesaid a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method adopts weak reducing atmosphere during its calcining, and calcining heat is 500～1000 ℃, and temperature retention time is 1～6h.
Advantage of the present invention and effect are:
1. precursor precipitate of the present invention in calcination process, just had when calcining heat is 600 ℃ pure crystalline phase (Y, Gd)
2O
3: Eu
3+Form, during to 700 ℃, pure crystalline phase (Y, Gd)
2O
3: Eu
3+Be completed into, its crystallization temperature is low, no dephasign, better crystallinity degree.
2. preparation technology of the present invention is simple, and the cycle is short, and cost is low, is suitable for dropping into producing in batches.
The present invention preparation (Y, Gd)
2O
3: Eu
3+Powder granule is reunited less, good dispersion, and almost spherical, average grain diameter are 20nm.
Description of drawings
Fig. 1 be average grain diameter of the present invention be about 20nm (Y, Gd)
2O
3: Eu
3+The SEM figure of powder;
Fig. 2 be average grain diameter of the present invention be about 20nm (Y, Gd)
2O
3: Eu
3+The TEM figure of powder;
Fig. 3 be the present invention (Y, Gd)
2O
3: Eu
3+The SEAD style figure of powder;
Fig. 4 is Eu of the present invention
3+Doping content to the swash figure of powder luminescent properties influence.
The specific embodiment
Accompanying drawing of the present invention be under electron microscope to the present invention (Y, Gd)
2O
3: Eu
3+The photo that powder scans, literal wherein are not very clear, but do not influence the understanding to technical solution of the present invention.
Below the present invention is described in detail.
The present invention includes and be prepared as follows step:
1. the configuration of solution: by (Y
1-xGd
0.3Eu
x)
2O
3Component takes by weighing Y
2O
3(99.9%), Gd
2O
3(99.9%), Eu
2O
3(99.9%), through the concentrated hydrochloric acid dissolving, is made into the earth solution that concentration is 0.01～1mol/L.It is 0.1～6mol/L that the concentration of precipitating reagent ammoniacal liquor is joined.
2. the preparation of presoma: above-mentioned precipitating reagent is added drop-wise in the earth solution that configures, temperature is 0～20 ℃, rate of addition is 1～5ml/min, the pH value of regulation system is 7～12, the precursor precipitate timeliness 0～4h that obtains, clean for several times with distilled water and absolute ethyl alcohol, suction filtration places precursor precipitate drying box at 70～130 ℃ of drying 8～24h.
3. calcining: the precursor powder that drying is good is pulverized, placed 500～1000 ℃ horse expense stove to calcine 1～4h.
As shown in the figure, the powder dispersity of the present invention's preparation is good, almost spherical; Its (Y, d)
2O
3: Eu
3+Sample belongs to body-centered cubic structure; Eu
3+Doping content the powder luminescent properties is had influence, i.e. Eu
3+Optimum doping concentration be 5～7mol%, the place has the strongest relative glow peak at the 612nm wavelength.
Embodiment 1:
0.281g Y
2O
3, 0.213g Gd
2O
3With 0.021g Eu
2O
3Mixing also is dissolved in concentrated hydrochloric acid, and adding distilled water is made into and contains the solution that rare earth ion is 0.05mol/L.The concentration that is made into ammoniacal liquor is 1mol/L, ammoniacal liquor is splashed in the earth solution that has prepared, and speed 2ml/min is until PH=7～8, and use magnetic stirrer, titration to finish back timeliness 30min, suction filtration, clean three times with distilled water, absolute ethyl alcohol washes twice, until PH=8, placing temperature is 70 ℃ of dry 24h of drying box, grinds, and crosses 80 purpose mesh screens, place horse expense stove at 700 ℃ of calcining 2h, ball milling, obtaining primary particle size is 17nm's, spherical, reunite more serious (Y, Gd)
2O
3: Eu
3+Powder.
Embodiment 2:
2.042g Y
2O
3, 1.471g Gd
2O
3With 0.147g Eu
2O
3Mixing also is dissolved in concentrated hydrochloric acid, and adding distilled water is made into and contains the solution that rare earth ion is 0.1mol/L.The concentration that is made into ammoniacal liquor is 1mol/L, ammoniacal liquor is splashed in the earth solution that has prepared, and speed 2ml/min is until about PH=8, and use magnetic stirrer, titration to finish back timeliness 30min, suction filtration, clean three times with distilled water, absolute ethyl alcohol washes twice, until PH=7～8, placing temperature is 70 ℃ of dry 24h of drying box, grinds, and crosses 80 purpose mesh screens, place horse expense stove at 700 ℃ of calcining 2h, ball milling, the acquisition primary particle size is 20nm, spherical, favorable dispersibility (Y, Gd)
2O
3: Eu
3+Powder.
Embodiment 3:
0.56g Y
2O
3, 0.402g Gd
2O
3With 0.036g Eu
2O
3Mixing also is dissolved in concentrated hydrochloric acid, is rare earth ion the solution of 0.2mol/L.The concentration that is made into ammoniacal liquor is 1mol/L, ammoniacal liquor is splashed in the earth solution that has prepared, and speed 2ml/min is until about PH=8, and use magnetic stirrer, titration to finish back timeliness 30min, suction filtration, clean three times with distilled water, absolute ethyl alcohol washes twice, until PH=7～8, placing temperature is 70 ℃ of dry 24h of drying box, grinds, and crosses 80 purpose mesh screens, place horse expense stove at 700 ℃ of calcining 2h, ball milling, the acquisition diameter of particle is 25nm, spherical, favorable dispersibility (Y, Gd)
2O
3: Eu
3+Powder.
Claims (4)
1. the method for a preparing yttrium-gadolinium-europium nano powder by coprecipitation method is characterized in that, this method comprises the steps:
1) configuration of solution: by (Y
1-xGd
0.3Eu
x)
2O
3Component takes by weighing rare earth oxide Y
2O
3, Gd
2O
3, Eu
2O
3, and it is dissolved in the concentrated hydrochloric acid, add distilled water, be configured to the earth solution that concentration is 0.01～1mol/L; Precipitating reagent ammoniacal liquor is configured to the weak aqua ammonia that concentration is 0.1～6mol/L;
2) preparation of presoma: above-mentioned precipitating reagent ammoniacal liquor is added drop-wise in the earth solution that configures, the precursor precipitate that obtains is behind timeliness 0～4h, clean with distilled water and absolute ethyl alcohol, suction filtration, place precursor precipitate drying box dry again, baking temperature is 70～130 ℃, and be 8～24h drying time, again through sieve precursor powder;
3) preparation of powder:, can make powder sample behind the ball milling with the above-mentioned precursor powder calcining that makes.
2. the method for a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method according to claim 1 is characterized in that, with Eu
2O
3The Eu that form is mixed up
3+Doping content be 1mol%～10mol%.
3. the method for a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method according to claim 1 is characterized in that, during titration, environment temperature is 0～20 ℃, and rate of titration is 1～5ml/min, and the precipitation pH value of back regulation system fully is 7～12.
4. the method for a kind of preparing yttrium-gadolinium-europium nano powder by coprecipitation method according to claim 1 is characterized in that, adopts weak reducing atmosphere during calcining, and calcining heat is 500～1000 ℃, and temperature retention time is 1～6h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491749A (en) * | 2011-12-12 | 2012-06-13 | 沈阳化工大学 | Method for preparing SrZr03:Ce nanometer powder with composite coprecipitator |
-
2008
- 2008-03-20 CN CNA2008100107056A patent/CN101239398A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491749A (en) * | 2011-12-12 | 2012-06-13 | 沈阳化工大学 | Method for preparing SrZr03:Ce nanometer powder with composite coprecipitator |
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Open date: 20080813 |