CN110184648A - Prepare method of the rear-earth-doped sodium yttrium tungstate crystal for quantitative calibration substance - Google Patents
Prepare method of the rear-earth-doped sodium yttrium tungstate crystal for quantitative calibration substance Download PDFInfo
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- CN110184648A CN110184648A CN201910645710.2A CN201910645710A CN110184648A CN 110184648 A CN110184648 A CN 110184648A CN 201910645710 A CN201910645710 A CN 201910645710A CN 110184648 A CN110184648 A CN 110184648A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
- C30B15/20—Controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
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Abstract
The invention discloses a kind of methods for preparing rear-earth-doped sodium yttrium tungstate crystal and being used for laser crystal LA-ICP-MS micro-zone analysis quantitative calibration substance, specially first prepare Na2CO3、Y2O3、WO3With other RE oxide powder mixtures, then raw material is fully ground after dehydrated alcohol being added, raw material is transferred in crucible later, it is placed in the sintering of Muffle furnace high temperature, carry out high temperature solid state reaction, crystal growth finally is completed in micro- drop-down crystal growing furnace, obtains rear-earth-doped sodium yttrium tungstate crystal.Gained crystalline material compactness of the invention is good, and the rare earth element distribution uniformity of transparent color and luster, no color differnece, doping is good, can be used as the LA-ICP-MS micro-zone analysis quantitative calibration substance of rear-earth-doped laser crystal material.
Description
Technical field
The present invention relates to microelement micro-zone analysis chemical fields, and in particular to a kind of to prepare rear-earth-doped Yttrium Tungstate sodium crystalline substance
The method that body and the LA-ICP-MS for being used for laser crystal material quantify micro-zone analysis.
Background technique
Laser crystal is the core component of laser, its work can be improved in doping with rare-earth ions in laser crystal
Performance.It can be laser crystal if the concentration and distributed intelligence of rare earth ion in laser crystal can be determined accurately
Detection and production provide scientific basis.
The quantitative correction of rare earth element is the key technical problem of impact analysis result in laser crystal, and emphasis is to develop
With the LA-ICP-MS quantitative correction standard of crystal prototype Matrix Match.However, also lacking this kind of standard substance/reference both at home and abroad
Substance, current research work can only be by the silicate calibration standards (such as NIST SRM 610) of non-Matrix Match for quantitative
Correction, inevitably introduces systematic error.As it can be seen that it is micro to carry out rare earth in laser crystal sample using LA-ICP-MS
The key scientific problems of the accurate micro-zone analysis of element are to prepare quantitative with the LA-ICP-MS microcell of laser crystal Matrix Match
Analysis correction standard.
Summary of the invention
In view of the above problems, the present invention passes through crystal growing furnace (i.e. micro- decline crystal growing furnace) synthetic rare earth doped wolframic acid
Yttrium sodium crystal.Crystal compactness obtained by this method is good, and the rare earth element distribution uniformity of transparent color and luster, no color differnece, doping is good
It is good, it can be used as the LA-ICP-MS micro-zone analysis quantitative calibration substance of rear-earth-doped laser crystal material.
In order to achieve the above objectives, the technical solution adopted by the present invention the following steps are included:
(1) Na is prepared2CO3、Y2O3、WO3Other RE oxide powder mixtures in addition to yttrium, are placed in mortar, add
Mixture of powders is fully ground after entering dehydrated alcohol；
(2) powder sample obtained by step (1) is transferred in crucible, Muffle furnace calcining is put into, with the liter of 5~10 DEG C/min
Warm rate is from room temperature to 600~800 DEG C, constant temperature preset time；1000~1200 DEG C are warming up to identical rate again, perseverance
Warm 12~24 hours completion high temperature solid state reactions, are finally cooled to room temperature；
(3) by the sample that step (2) has been calcined be transferred to it is micro- drop-down crystal growing furnace crucible in, by shove charge, heating,
Seeding isodiametric growth, pulls, cooling step completion crystal growth, obtains rear-earth-doped sodium yttrium tungstate crystal, is used for laser crystal
LA-ICP-MS micro-zone analysis quantitative calibration substance.
Preferably, the ratio of other rare earth oxides doping in the step (1) in addition to yttrium is 0.01%~0.1%.
Preferably, the dehydrated alcohol of submergence mixture of powders is added in the step (1) into mortar.
Preferably, muffle furnace is specifically set in the step (2) are as follows: with the heating rate of 5 DEG C/min from room temperature liter
1000 DEG C are warming up to from 700 DEG C to 700 DEG C, constant temperature 6 hours, then with same 5 DEG C/min, constant temperature 12h is finally cooled to room
Temperature.
Preferably, step (2) the high temperature solid phase reaction are as follows:
Na2CO3+xRE2O3+(1-x)Y2O3+4WO3=2NaRExY(1-x)(WO4)2+CO2↑。
Preferably, micro- drop-down crystal growing furnace program setting in the step (3) are as follows: heating power from 0W to 1500~
1800W, heat up 8~12h of used time, and then program-controlled increase heats up power to 2000W, 1~5h of used time, when micro- lower crystal pulling is raw again
When at thering is melt liquid to occur in the crucible of furnace, stop program-controlled heating, with NaY (WO4)2Seed crystal carries out seeding；When crystal growth,
Make 24~48h of isodiametric growth of crystal with the program-controlled increase power of the rate of 1~3W/h；Complete to melt crystallization in crucible, crystal is drawn
It is de-；Cooling process setting are as follows: 2000~2500W to 0W, 20~30h of used time.
Preferably, micro- decline crystal growing furnace program setting in the step (3) are as follows: heating power is used from 0W to 1700W
When 10h, after seeding process power rises to 1800W, set program-controlled heating power again from 1800W to 2000W, used time 2h works as function
When rate is 1960W, liquid stream appearance is observed, has stopped program-controlled heating, carried out seeding with seed crystal；When crystal growth, with 1.3W/h
The program-controlled increase power of rate make isodiametric growth of crystal 48h；Complete to raw material flow in crucible, crystal pulls；Cooling process setting are as follows:
2050W to 1300W, used time 10h, 1300W to 0W, used time 10h.
Preferably, the rear-earth-doped sodium yttrium tungstate crystal synthesized in the step (3) is strip, length is 10~
30mm, width are 1~5mm.
Preferably, the rear-earth-doped sodium yttrium tungstate crystal length synthesized in the step (3) is 25mm, width 3mm.
The technical solution adopted in the present invention compared with prior art, at least has the advantage that
1, rear-earth-doped sodium yttrium tungstate crystal matrix composition prepared by the present invention is Yttrium Tungstate sodium, is not avoided because of matrix not
Fit over caused error in LA-ICP-MS detection.
2, present invention gained crystalline material compactness is good, and laser ablation pit edge does not have apparent avalanche and melting existing
As.
3, rare earth element distribution uniformity is good in rear-earth-doped sodium yttrium tungstate crystal prepared by the present invention, meets as school
The requirement of quasi- substance.
Detailed description of the invention
Fig. 1 is the pictorial diagram of rear-earth-doped sodium yttrium tungstate crystal in embodiment 1.
Fig. 2 is the XRD diagram of rear-earth-doped sodium yttrium tungstate crystal in embodiment 1.
Fig. 3 is rare earth element LA-ICP-MS line scanning signal representative in rear-earth-doped sodium yttrium tungstate crystal in embodiment 1
Figure.
Specific embodiment
Below by embodiment, the present invention is further illustrated, but not limited to this.
Embodiment 1
It is a kind of prepare rear-earth-doped sodium yttrium tungstate crystal be used for laser crystal material LA-ICP-MS micro-zone analysis it is fixed
The method for measuring calibration substance, the specific steps are as follows:
(1) lanthana, cerium oxide, praseodymium oxide are respectively weighed and respectively weighs 0.0016g, respectively weigh neodymia, samarium oxide
0.0017g respectively weighs europium oxide, gadolinium oxide, terbium oxide, dysprosia 0.0018g, respectively weighs holimium oxide, erbium oxide, thulium oxide
0.0019g respectively weighs ytterbium oxide, luteium oxide 0.0020g, weighs yttrium oxide 1.1132g, weighs natrium carbonicum calcinatum 0.5352g, claims
Take tungstic acid 4.6370g；Load weighted drug is ground into 1h, when grinding can drip few drops of alcohol into agate mortar, guarantee
It is abundant that drug grinds mixing；
(2) drug being fully ground is transferred in clean corundum crucible, then carries out high-temperature calcination with Muffle furnace, completed
High temperature solid state reaction.Muffle furnace setting are as follows: 700 DEG C are risen to 5 DEG C/min, constant temperature 12 hours, then with same 5 DEG C/min
It is warming up to 1000 DEG C from 700 DEG C, constant temperature 12 hours, is finally cooled to room temperature removing pharmaceutical producs；
(3) drug calcined is transferred to shove charge in the crucible of micro- drop-down crystal growing furnace, carries out crystal growth operations, it is micro-
Decline crystal growing furnace program setting: setting temperature programming power is from 0W to 1700W, and heat up 10h, and seeding process power rises to
After 1800W, program-controlled heating is set again from 1800W to 2000W, used time 2h has observed that liquid stream goes out when power is 1960W
It is existing, stop program-controlled heating, removes seeding with seed crystal.When crystal growth, keep crystal isometrical with the program-controlled increase power of the rate of 1.3W/h
Grow 48h.Complete to raw material flow in crucible, crystal pulls.Cooling process is set as 2050W to 1300W, used time 10h；1300W is arrived
0W, used time 10h.
The pictorial diagram of rear-earth-doped sodium yttrium tungstate crystal manufactured in the present embodiment is as shown in Figure 1, it is found that obtained dilute
Soil doping sodium yttrium tungstate crystal uniform color, without apparent color difference.
The XRD diagram of rear-earth-doped sodium yttrium tungstate crystal manufactured in the present embodiment is as shown in Fig. 2, as can be seen from Figure 2, synthetic crystal
Matrix chemical composition be Yttrium Tungstate sodium.
LA-ICP-MS test: sanding and polishing after the crystal target of synthesis is carried out after each index tuning of instrument is normal
Analysis test is degraded in the line scanning of synthetic crystal sample.When analysis is degraded in line scanning, laser ablation spot diameter is 60 μm, line scanning speed
Rate is 10 μm of s-1, gas background acquisition time is 20s, and sample signal acquires 160s, the rare earth-doped calcium tungstate crystal of acquisition
LA-ICP-MS line scanning signal figure as shown in figure 3, each rare earth element signal curve is smooth as can be seen from Figure 3, each rare earth element warp
The relative standard deviation of elemental signals intensity rate after Internal standard correction methods shows artificial schellite crystals element less than 10%
Distribution uniformity is good.
Embodiment 2
It is a kind of prepare rear-earth-doped sodium yttrium tungstate crystal be used for laser crystal material LA-ICP-MS micro-zone analysis it is fixed
The method for measuring calibration substance, the specific steps are as follows:
(1) lanthana, cerium oxide, praseodymium oxide are respectively weighed and respectively weighs 0.0048g, respectively weigh neodymia, samarium oxide
0.0051g respectively weighs europium oxide, gadolinium oxide, terbium oxide, dysprosia 0.0054g, respectively weighs holimium oxide, erbium oxide, thulium oxide
0.0057g respectively weighs ytterbium oxide, luteium oxide 0.0060g, weighs yttrium oxide 1.1132g, weighs natrium carbonicum calcinatum 0.5352g, claims
Take tungstic acid 4.6370g；Load weighted drug is ground into 1h, when grinding can be added into agate mortar submerges above-mentioned drug
Dehydrated alcohol, grind one and a half hours, guarantee drug grinding mixing it is abundant；
(2) drug being fully ground is transferred in clean corundum crucible, then carries out high-temperature calcination with Muffle furnace, completed
High temperature solid state reaction.Muffle furnace setting are as follows: 750 DEG C are risen to 8 DEG C/min, constant temperature 12 hours, then with same 8 DEG C/min
It is warming up to 1100 DEG C from 750 DEG C, constant temperature 14 hours, is finally cooled to room temperature removing pharmaceutical producs；
(3) drug calcined is transferred to shove charge in the crucible of micro- drop-down crystal growing furnace, carries out crystal growth operations, it is micro-
Decline crystal growing furnace program setting: setting temperature programming power is from 0W to 1600W, and heat up 9h, and seeding process power rises to
After 1800W, program-controlled heating is set again from 1800W to 2000W, and used time 2h is molten when having in the crucible that micro- lower crystal pulling generates furnace
It is current to melt liquid discharge, stops program-controlled heating, with NaY (WO4)2Seed crystal removes seeding.When crystal growth, with the program-controlled increasing of the rate of 2W/h
Power is added to make isodiametric growth of crystal 36h.Complete to melt crystallization in crucible, crystal pulls.Cooling process is set as 2250W and arrives
Rear-earth-doped sodium yttrium tungstate crystal is made in 0W, used time 36h, and the LA-ICP-MS for laser crystal material quantifies micro-zone analysis.
Claims (9)
- It prepares rear-earth-doped sodium yttrium tungstate crystal 1. a kind of and is used for laser crystal LA-ICP-MS micro-zone analysis quantitative calibration object The method of matter, which comprises the following steps:(1) Na is prepared2CO3、Y2O3、WO3Other RE oxide powder mixtures in addition to yttrium, are placed in mortar, and nothing is added Mixture of powders is fully ground after water-ethanol；(2) powder sample obtained by step (1) is transferred in crucible, is put into Muffle furnace calcining, with the heating speed of 5~10 DEG C/min Rate is from room temperature to 600~800 DEG C, constant temperature preset time；1000~1200 DEG C are warming up to identical rate again, constant temperature 12 ~24 hours completion high temperature solid state reactions, are finally cooled to room temperature；(3) sample that step (2) has been calcined is transferred in the crucible of micro- drop-down crystal growing furnace, by shove charge, heats up, draws Crystalline substance isodiametric growth, pulls, cooling step completion crystal growth, obtains rear-earth-doped sodium yttrium tungstate crystal, is used for laser crystal LA-ICP-MS micro-zone analysis quantitative calibration substance.
- 2. preparation method as described in claim 1, which is characterized in that other rare-earth oxidations in the step (1) in addition to yttrium The ratio of object doping is 0.01%~0.1%.
- 3. preparation method as described in claim 1, which is characterized in that submergence powder is added in the step (1) into mortar The dehydrated alcohol of mixture.
- 4. preparation method as described in claim 1, which is characterized in that muffle furnace is specifically set in the step (2) are as follows: 700 DEG C are risen to from room temperature with the heating rate of 5 DEG C/min, constant temperature 6 hours, then be warming up to same 5 DEG C/min from 700 DEG C 1000 DEG C, constant temperature 12h is finally cooled to room temperature.
- 5. preparation method as described in claim 1, which is characterized in that step (2) the high temperature solid phase reaction are as follows:Na2CO3+xRE2O3+(1-x)Y2O3+4WO3=2NaRExY(1-x)(WO4)2+CO2↑。
- 6. preparation method as described in claim 1, which is characterized in that micro- drop-down crystal growing furnace program in the step (3) Setting are as follows: heating power is from 0W to 1500~1800W, and heat up 8~12h of used time, and then program-controlled increase heating power arrives again 2000W, 1~5h of used time stop program-controlled heating, use NaY when having melt liquid to occur in the crucible that micro- lower crystal pulling generates furnace (WO4)2Seed crystal carries out seeding；When crystal growth, with the program-controlled increase power of the rate of 1~3W/h make isodiametric growth of crystal 24~ 48h；Complete to melt crystallization in crucible, crystal pulls；Cooling process setting are as follows: 2000~2500W to 0W, 20~30h of used time.
- 7. preparation method as claimed in claim 6, which is characterized in that micro- decline crystal growing furnace program in the step (3) Setting are as follows: for heating power from 0W to 1700W, used time 10h after seeding process power rises to 1800W, sets program-controlled heating function again Rate is from 1800W to 2000W, used time 2h, when power is 1960W, has observed liquid stream appearance, has stopped program-controlled heating, use seed crystal Carry out seeding；When crystal growth, isodiametric growth of crystal 48h is made with the program-controlled increase power of the rate of 1.3W/h；To raw material in crucible It has been flowed that, crystal pulls；Cooling process setting are as follows: 2050W to 1300W, used time 10h, 1300W to 0W, used time 10h.
- 8. preparation method as described in claim 1, which is characterized in that the rear-earth-doped Yttrium Tungstate synthesized in the step (3) Sodium crystal is strip, and length is 10~30mm, and width is 1~5mm.
- 9. preparation method as claimed in claim 8, which is characterized in that the rear-earth-doped Yttrium Tungstate synthesized in the step (3) Sodium crystal length is 25mm, width 3mm.
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Cited By (2)
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| CN111501089A (en) * | 2020-04-17 | 2020-08-07 | 江苏师范大学 | Mixed rare earth-transition element doped up-conversion laser crystal and preparation method thereof |
| CN114908422A (en) * | 2022-06-29 | 2022-08-16 | 合肥工业大学 | Strontium-doped lanthanum hexaboride single crystal and preparation method thereof |
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| CN114908422B (en) * | 2022-06-29 | 2024-06-14 | 合肥工业大学 | Strontium doped lanthanum hexaboride monocrystal and preparation method thereof |
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