CN106517295A - Method for synthesizing high-stability gamma-Pr2S3 powder - Google Patents
Method for synthesizing high-stability gamma-Pr2S3 powder Download PDFInfo
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- CN106517295A CN106517295A CN201610905618.1A CN201610905618A CN106517295A CN 106517295 A CN106517295 A CN 106517295A CN 201610905618 A CN201610905618 A CN 201610905618A CN 106517295 A CN106517295 A CN 106517295A
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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
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Abstract
The invention relates to a method for synthesizing high-stability gamma-Pr2S3 powder. By virtue of the method, high-purity gamma-Pr2S3 powder with a cubic structure within a temperature range from the room temperature to 1340 DEG C and stable thermodynamics performance at a relatively low preparation temperature and a relative short temperature maintenance time can be obtained. The problems that the vulcanizing temperature is high, the time is long, the cost is high, or the product stability is low, the purity is low, and carbon pollution and sulfur oxide impurities are easily produced in the prior art are solved. Gamma-phase Pr2S3 belongs to a stable phase at a temperature higher than 1340 DEG C, so that praseodymium sulfide powder prepared by virtue of the method can stably preserve a gamma-phase structure in a whole temperature range. Meanwhile, the method is simple in process, low in cost and applicable to the large-scale preparation of high-stability high-purity gamma-phase praseodymium sulfide, and has wide application prospects.
Description
Technical field
The invention belongs to new material technology field, is related to a kind of synthesizing high-stability γ-Pr2S3The method of powder, specifically relates to
And a kind of Fast back-projection algorithm high-stability gamma-phase praseodymium sulfide (γ-Pr2S3) raw powder's production technology.γ-Pr obtained by the method2S3
Powder can remain Emission in Cubic in the range of total temperature, have very high thermodynamic stability, be applied to prepare γ-Pr2S3Polycrystalline material
Material, thermoelectric material.
Background technology
Sulfuration praseodymium compound co-exists in 3 kinds of crystal phase structures i.e.：α phases, β phases and γ phases, wherein α-Pr2S3Belong to rhombic system,
Space group is (D2h 16- Pnma), it is ambient stable phase；β-Pr2S3For tetragonal, space group is (D4h 20-I41/ acd) molecular formula
Writing Pr10S15-xOxThe oxysulfide of (0≤x≤1), substantially praseodymium, β-Pr2S3Thermodynamically stable scope be 925 DEG C～1340
℃；γ-Pr2S3For body-centered cubic structure, space group isBelong to the Th with metal cavity3P4Structure, which is in temperature
It is stable phase when degree is higher than 1340 DEG C.In actual technology application, γ phases praseodymium sulfide is with even more important with β phases compared with α phases
Application background, γ-Pr2S3Belong to typical high-melting-point (1800 DEG C) rare earth chalcogen compound, with outstanding physical chemistry
Can, there is important technology application prospect in technical fields such as thermoelectric material, magnetic material, senior pigment；Additionally due to γ-
Pr2S3Cubic structure and Pr-S chemical bonds in infrared region without absorption so that the material can be prepared into red by hot pressed sintering
Outer optical clear ceramics, without causing infrared light scattering to cause transmitance to decline or devitrification because of optical anisotropy.
Therefore, prepare praseodymium sulfide powder and control its phase structure for γ phases, particularly prepare the γ with high thermodynamic stability-
Pr2S3Practical application development of the powder to the material is significant.
The γ phase praseodymium sulfide raw powder's production technologies reported for work at present include three kinds of methods, and first method is that element is directly closed
Into method [John B.Gruber, Ramon Burriel, Edgar F.Westrum, Jr.W.Plautz, G.Metz, and Xiao-
Xia Ma, etal, Thermophysical properties of the lanthanide
sesquisulfides.II.Schottky contributions and magnetic and electronic
properties ofγphase Pr2S3, Tb2S3,and Dy2S3, Journal of Chemistry Physics, 1991,95
(3):1964-1972], the method is mainly mixed in quartz ampoule using metal Pr powder and S simple substance powder reacts 6 at 600 DEG C
Hour, after again at 900 DEG C be incubated 3 days, then quartz ampoule is opened, will reaction half product take out and grind to form 200 mesh or so
Powder, then cold pressing plate, in 1500 DEG C, H29 hours are incubated in S atmosphere, γ-Pr can be obtained2S3；Second method is dilute
Native oxide curative method [Yuan Haibin, Synthesis of rare earth sulfides and their UV-vis
Absorption spectra, Journal of Rare Earths, 2009,27 (2):308-311；Shinji Hirail,
Preparations ofγ-Pr2S3andγ-Nd2S3Powders by Sulfurization of Pr6O11and
Nd2O3Powders Using CS2Gas and their Sintering, Journal of the Japan Institute
Metals,2003,67(1):15-21], the method is by the oxide of praseodymium such as Pr2O3Or Pr6O11In CS2When carrying out long under atmosphere
Between high-temperature gas-solid vulcanization reaction, finally obtain rare-earth sulfide, the curing temperature of this method is generally left at 900～1300 DEG C
The right side, and subsequently need to process at 1500～1700 DEG C, and the γ-Pr for synthesizing2S3Product stability is poor, purity is low, usually contains
Oxide, oxysulfide and β phases；The third method is complex presoma thermal decomposition method [GUO Pengjiang, JIAO
Baojuan, Thermal decomposition of Pr [(C5H8NS2)3(C12H8N2)],Science in China Ser.B：
Chemistry, 2005,48：Supp.83-87], the method synthesizes the sulfur-bearing of praseodymium but the complex without oxygen atom in advance
Such as Pr [(C5H8NS2)3(C12H8N2)], heat point is then carried out in a low temperature of 250 DEG C～400 DEG C and in inert gas atmosphere
Solution, it is possible to obtain nano level γ-Pr2S3Powder, but the major defect of the method is the γ-Pr for preparing2S3Contain in product powder
Substantial amounts of carbon, powder are presented black；4th kind of method is that [Tao rising star, Huang Jinfu, Pei Lizhai, Zhang Qianfeng, binary are dilute for solvent-thermal method
The solvent-thermal process of native sulfide and sign, rare metal and hard alloy, 2013,41 (4):21-25], the method is similar to matching somebody with somebody
Position compounds precursors thermal decomposition method, difference is all to put the actual raw material of the sulfur-bearing complex of the praseodymium that can synthesize
In reactor, such as praseodymium nitrate, adjacent phenanthrene quinoline, sodium diethyldithiocarbamate are mixed in ethanol respectively, after be placed in
The interior held for some time at 180 DEG C of water heating kettle, synthesizes γ-Pr using the method treated different things alike2S3Powder, but the method synthesis
The many oxycompounds of praseodymium sulfide product and oxysulfide, stability and purity it is relatively low.
Obvious existing synthetically prepared γ-Pr2S3There are different defects in the method for powder, such as to process equipment and bar
Part requires harsh, and curing temperature height, time length, relatively costly, or product stability is low, purity is low.Therefore, develop high steady
Qualitative and highly purified γ-Pr2S3Development of the synthetically prepared technology of powder to praseodymium sulfide material is significant.
The content of the invention
Technical problem to be solved
In place of the deficiencies in the prior art, the present invention proposes a kind of synthesizing high-stability γ-Pr2S3The side of powder
Method
Technical scheme
A kind of synthesizing high-stability γ-Pr2S3The method of powder, it is characterised in that step is as follows：
The preparation of step 1, presoma powder：
The concentrated solution of NaCl, NaBr or NaI is made at 25 DEG C using deionized water, concentration is 3.0～6.0mol L-1；
By in concentrated solution injection analysis pure level praseodymium carbonate powder, with magnetic stirrer to uniform, it is subsequently placed in 70
Be dried in～90 DEG C of vacuum drying chamber 12h remove moisture, grind to form the powder of 200～300 mesh after taking-up, obtain praseodymium carbonate with
NaCl, NaBr or NaI presoma powder；
The molecular formula for analyzing pure level praseodymium carbonate：Pr2(CO3)3；
The pure level praseodymium carbonate powder of the analysis is Pr with the ratio of the amount of the material of NaCl, NaBr or NaI3+:Na+=1.0:
(1.0～2.0)；
Step 2, γ-Pr2S3The preparation of powder：Presoma powder is placed in atmosphere tube type stove, flow be 30～
Under the Ar gas shieldeds of 50mL/min, heated up with 5 DEG C/min of the rate of heat addition；
When tubular type furnace temperature rises to 650 DEG C, mixed gas that flow is 30～50mL/min are passed through as shielding gas
Body, continue to make tube furnace be warming up to 750～900 DEG C, be incubated 90～200min, after insulation terminates, tube furnace natural cooling；
When furnace temperature is less than 650 DEG C, Ar gas that flow is 30～50mL/min is passed through as protective gas；
Green powder is taken out upon cooling to room temperature, and deionized water and washes of absolute alcohol powder are each 1 time successively, then
Again powder is put in vacuum drying chamber, under 60 DEG C, vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried powder i.e.
For the γ-Pr for preparing2S3Powder；
The mixed gas are Ar gas and CS2Or H2The mixed gas of S, mixed gas volume ratio are Ar:CS2Or Ar:H2S
For 1:1.
It is described to analyze pure level praseodymium carbonate powder for 200～300 mesh.
Beneficial effect
A kind of synthesizing high-stability γ-Pr proposed by the present invention2S3The method of powder, it is in relatively low preparation temperature, shorter
Under the conditions of temperature retention time, it is possible to obtain under the temperature range of room temperature～1340 DEG C cubic structure, thermodynamically stable high-purity γ-
Pr2S3Powder.Curing temperature height, time length, high cost in prior art is solved, or product stability is low, purity is low, easy
In there are problems that carbon pollution and oxysulfide.Due to γ phases Pr2S3Belong to stable phase when temperature is higher than 1340 DEG C, because
Praseodymium sulfide powder prepared by this present invention is the praseodymium sulfide powder that can stably remain γ phase structures in the range of total temperature.Together
When, its process is simple, low cost are suitable for preparing the high high-purity gamma phase praseodymium sulfide of stability on a large scale, with wide application
Prospect.
Specific embodiment
In conjunction with embodiment, the invention will be further described：
Embodiment 1:
The preparation of step 1 presoma powder：Ratio according to the amount of material is Pr3+:Na+=1.0:2.0 weigh 200 mesh respectively
The pure level praseodymium carbonate (molecular formula of analysis：Pr2(CO3)3) 11.55 grams and 5.85 grams of NaCl of powder.At 25 DEG C, will be weighed
NaCl adds 17ml deionized waters to make concentration for 6.0mol L-1Concentrated solution；Made NaCl solution is injected into praseodymium carbonate powder again
In body, with magnetic stirrer to uniform；Then the mixture of NaCl and praseodymium carbonate is placed at 90 DEG C of vacuum drying chamber
In be dried 12h and remove moisture, and after taking out, grind to form the powder of 200 mesh, you can obtain praseodymium carbonate it is mixed uniformly with NaCl before
Drive 17.4 grams of body powder.
Step 2 γ-Pr2S3The preparation of powder：Presoma powder prepared by step 1 is placed in atmosphere tube type stove, in flow
Under for the Ar protections of 50mL/min, heated up with 5 DEG C/min of the rate of heat addition, when tubular type furnace temperature rises to 650 DEG C, by the gas being passed through
Structural reform is Ar gas and CS2Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio is Ar:CS2(or H2S)=1:
1, continue to make tube furnace be warming up to 850 DEG C, be incubated 90min, after insulation terminates, tube furnace natural cooling, and treat that furnace temperature is less than 650
DEG C when, mixed gas are still used the Ar gas of 50mL/min same traffics instead as protective gas, treat that tube furnace naturally cools to room
Temperature, takes out green powder, and deionized water and washes of absolute alcohol powder are each 1 time successively, powder is put into vacuum again then and is done
In dry case, under 60 DEG C, vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried 19.2 grams of powder, as prepares
γ-Pr2S3Powder.
Embodiment 2:
The preparation of step 1 presoma powder：Ratio according to the amount of material is Pr3+:Na+=1.0:1.0 weigh 200 mesh respectively
The pure level praseodymium carbonate (molecular formula of analysis：Pr2(CO3)3) 16.1 grams and 4.1 grams of NaCl of powder.At 25 DEG C, will be weighed
NaCl adds 23ml deionized waters to make concentration for 3.0mol L-1Solution；Again NaCl solution is injected in praseodymium carbonate powder,
With magnetic stirrer to uniform；Then NaCl is placed in 70 DEG C of vacuum drying chamber with the solidliquid mixture of praseodymium carbonate
It is dried 12h and removes moisture, and after taking out, grind to form the powder of 300 mesh, you can obtains praseodymium carbonate and the mixed uniformly forerunners of NaCl
20.2 grams of body powder.
Step 2 γ-Pr2S3The preparation of powder：Presoma powder prepared by step 1 is placed in atmosphere tube type stove, in flow
Under for the Ar protections of 30mL/min, heated up with 5 DEG C/min of the rate of heat addition, when tubular type furnace temperature rises to 650 DEG C, by the gas being passed through
Structural reform is Ar gas and CS2Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio is Ar:CS2=1:1, continue
Make tube furnace be warming up to 750 DEG C, be incubated 200min, after insulation terminates, tube furnace natural cooling, and when furnace temperature is less than 650 DEG C,
Mixed gas are still used the Ar gas of same traffic instead as protective gas, treat that tube furnace naturally cools to room temperature, take out green flour
Body, deionized water and washes of absolute alcohol powder are each 1 time successively, and then again powder is put in vacuum drying chamber, 60 DEG C,
Under vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried 26.5 grams of powder, the γ-Pr for as preparing2S3Powder.
Embodiment 3:
The preparation of step 1 presoma powder：Ratio according to the amount of material is Pr3+:Na+=1.0:1.5 weigh 250 mesh respectively
The pure level praseodymium carbonate (molecular formula of analysis：Pr2(CO3)3) 16.9 grams and 6.4 grams of NaCl of powder.At 25 DEG C, will be weighed
NaCl adds 22.0ml deionized waters to make concentration for 5.0mol L-1Solution；NaCl solution is injected into praseodymium carbonate powder again
In, with magnetic stirrer to uniform；Then the solidliquid mixture of NaCl and praseodymium carbonate is placed at 80 DEG C of vacuum drying
12h is dried in case and removes moisture, and grind to form the powder of 250 mesh after taking out, you can obtain praseodymium carbonate mixed uniformly with NaCl
23.3 grams of presoma powder.
Step 2 γ-Pr2S3The preparation of powder：Presoma powder prepared by step 1 is placed in atmosphere tube type stove, in flow
Under for the Ar protections of 30～50mL/min, heated up with 5 DEG C/min of the rate of heat addition, when tubular type furnace temperature rises to 650 DEG C, will be passed through
Gas be changed to Ar gas and H2The mixed gas of S, total gas flow rate are constant, and wherein mixed gas volume ratio is Ar:H2S=1:1,
Continue to make tube furnace be warming up to 800 DEG C, be incubated 120min, after insulation terminates, tube furnace natural cooling, and treat that furnace temperature is less than 650
DEG C when, mixed gas are still used the Ar gas of same traffic instead as protective gas, treat that tube furnace naturally cools to room temperature, take out green
Toner body, deionized water and washes of absolute alcohol powder are each 1 time successively, and then again powder is put in vacuum drying chamber,
60 DEG C, under vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried 27.9 grams of powder, the γ-Pr for as preparing2S3Powder
Body.
Embodiment 4:
The preparation of step 1 presoma powder：Ratio according to the amount of material is Pr3+:Na+=1.0:1.4 weigh 200 mesh respectively
The pure level praseodymium carbonate (molecular formula of analysis：Pr2(CO3)3) 13.2 grams and 8.23 grams of NaBr of powder.At 25 DEG C, will be weighed
NaBr adds 20ml deionized waters to make concentration for 4.0mol L-1Solution；Again NaBr solution is injected in praseodymium carbonate powder,
With magnetic stirrer to uniform；Then NaBr is placed in 80 DEG C of vacuum drying chamber with the solidliquid mixture of praseodymium carbonate
It is dried 12h and removes moisture, and after taking out, grind to form the powder of 200 mesh, you can obtains praseodymium carbonate and the mixed uniformly forerunners of NaBr
21.3 grams of body powder.
Step 2 γ-Pr2S3The preparation of powder：Presoma powder prepared by step 1 is placed in atmosphere tube type stove, in flow
Under for the Ar protections of 40mL/min, heated up with 5 DEG C/min of the rate of heat addition, when tubular type furnace temperature rises to 650 DEG C, by the gas being passed through
Structural reform is Ar gas and CS2Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio is Ar:CS2=1:1, continue
Make tube furnace be warming up to 850 DEG C, be incubated 180min, after insulation terminates, tube furnace natural cooling, and when furnace temperature is less than 650 DEG C,
Mixed gas are still used the Ar gas of same traffic instead as protective gas, treat that tube furnace naturally cools to room temperature, take out green flour
Body, deionized water and washes of absolute alcohol powder are each 1 time successively, and then again powder is put in vacuum drying chamber, 60 DEG C,
Under vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried 10.8 grams of powder, the γ-Pr for as preparing2S3Powder.
Embodiment 5:
The preparation of step 1 presoma powder：Ratio according to the amount of material is Pr3+:Na+=1.0:1.5 weigh 300 mesh respectively
The pure level praseodymium carbonate (molecular formula of analysis：Pr2(CO3)3) 7.7 grams and 7.5 grams of NaI of powder.At 25 DEG C, by weighed NaI
10.0ml deionized waters are added to make concentration for 5.0mol L-1NaI solution；Again NaI solution is injected in praseodymium carbonate powder,
With magnetic stirrer to uniform；Then NaI is placed in 75 DEG C of vacuum drying chamber with the solidliquid mixture of praseodymium carbonate
It is dried 12h and removes moisture, and after taking out, grind to form the powder of 300 mesh, you can obtains praseodymium carbonate and the mixed uniformly presomas of NaI
Powder.
Step 2 γ-Pr2S3The preparation of powder：Presoma powder prepared by step 1 is placed in atmosphere tube type stove, in flow
Under for the Ar protections of 40mL/min, heated up with 5 DEG C/min of the rate of heat addition, when tubular type furnace temperature rises to 650 DEG C, by the gas being passed through
Structural reform is Ar gas and CS2Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio is Ar:CS2=1:1, continue
Make tube furnace be warming up to 830 DEG C, be incubated 150min, after insulation terminates, tube furnace natural cooling, and when furnace temperature is less than 650 DEG C,
Mixed gas are still used the Ar gas of same traffic instead as protective gas, treat that tube furnace naturally cools to room temperature, take out green flour
Body, deionized water and washes of absolute alcohol powder are each 1 time successively, and then again powder is put in vacuum drying chamber, 60 DEG C,
Under vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried 12.6 grams of powder, the γ-Pr for as preparing2S3Powder.
Claims (2)
1. a kind of synthesizing high-stability γ-Pr2S3The method of powder, it is characterised in that step is as follows：
The preparation of step 1, presoma powder：
The concentrated solution of NaCl, NaBr or NaI is made at 25 DEG C using deionized water, concentration is 3.0～6.0mol L-1；
By in concentrated solution injection analysis pure level praseodymium carbonate powder, with magnetic stirrer to uniform, it is subsequently placed in 70～90
DEG C vacuum drying chamber in be dried 12h remove moisture, grind to form the powder of 200～300 mesh after taking-up, obtain praseodymium carbonate with
NaCl, NaBr or NaI presoma powder；
The molecular formula for analyzing pure level praseodymium carbonate：Pr2(CO3)3；
The pure level praseodymium carbonate powder of the analysis is Pr with the ratio of the amount of the material of NaCl, NaBr or NaI3+:Na+=1.0:(1.0～
2.0)；
Step 2, γ-Pr2S3The preparation of powder：Presoma powder is placed in atmosphere tube type stove, is 30～50mL/min in flow
Ar gas shieldeds under, with 5 DEG C/min of the rate of heat addition heat up；
When tubular type furnace temperature rises to 650 DEG C, mixed gas that flow is 30～50mL/min are passed through as protective gas, after
It is continuous to make tube furnace be warming up to 750～900 DEG C, 90～200min is incubated, after insulation terminates, tube furnace natural cooling；
When furnace temperature is less than 650 DEG C, Ar gas that flow is 30～50mL/min is passed through as protective gas；
Green powder is taken out upon cooling to room temperature, deionized water and washes of absolute alcohol powder are each 1 time successively, then again will
Powder is put in vacuum drying chamber, and under 60 DEG C, vacuum 5Pa, holding is dried for 6 hours, and taking-up is dried powder and as makes
For the γ-Pr for going out2S3Powder；
The mixed gas are Ar gas and CS2Or H2The mixed gas of S, mixed gas volume ratio are Ar:CS2Or Ar:H2S is 1:1.
2. synthesizing high-stability γ-Pr according to claim 12S3The method of powder, it is characterised in that：It is described to analyze pure level
Praseodymium carbonate powder is 200～300 mesh.
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| CN108715549A (en) * | 2018-06-05 | 2018-10-30 | 西北工业大学 | It is a kind of to prepare rare-earth sulfide γ-Ln2S3The method of crystalline ceramics |
| CN108715551A (en) * | 2018-06-05 | 2018-10-30 | 西北工业大学 | A kind of low-temperature sintering rare-earth sulfide γ-Ln2S3The method of infrared transparent ceramics |
| CN108715551B (en) * | 2018-06-05 | 2021-04-20 | 西北工业大学 | Low-temperature sintering rare earth sulfide gamma-Ln2S3Method for preparing infrared transparent ceramics |
| CN114870870A (en) * | 2022-04-29 | 2022-08-09 | 成都理工大学 | Magnetic environment purifying material for co-processing MO and Cr (VI) pollution and preparation method thereof |
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