CN106544026B - A kind of alkali metal-rare earth fluorine sulfide NaLaF2S and its synthetic method - Google Patents
A kind of alkali metal-rare earth fluorine sulfide NaLaF2S and its synthetic method Download PDFInfo
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Abstract
The present invention relates to a kind of alkali metal-rare earth fluorine sulfide NaLaF2S and its synthetic method, it is characterised in that the molecular formula of alkali metal rare earth fluorine sulfide is NaLaF2S；It is La according to the ratio between amount of substance by analyzing pure grade lanthanum oxide powder and sodium fluoride3+:Na+=1.0:(4.0~6.0) synthesis.When synthesis under the conditions of certain synthesis temperature and shorter soaking time, using lanthana and sodium fluoride as raw material, with CS2For sulfiding gas, NaLaF can be easily synthesized2S compound.Meanwhile simple process, it is suitable for large scale preparation alkali metal rare earth fluorine sulfide, has broad application prospects.
Description
Technical field
The invention belongs to new material technology fields, are related to a kind of alkali metal-rare earth fluorine sulfide NaLaF2S and its synthesis side
Method.
Background technique
" transition metal-rare earth fluorine sulfide " can be used as a new class of advanced rare-earth pigment compound and luminous host material
Material, since preparation needs hot conditions and is difficult to synthesize, this kind of current document report of compound is few.Current class reported in the literature
There was only a few like compound, mainly ' the alkaline-earth metal-rare earth fluorine vulcanization of alkaline-earth metal and the formation of light rare earth fluorine sulfide
Object ', including Ce2SrF4S2、Ce2CaF4S2(it is detailed in document: A.Demourgues, A.Tressauda, H.Laronzea,
P.Macaudiére,Rare earth fluorosulfides LnSF and Ln2AF4S2as new colour
Pigments, Journal of Alloys and Compounds, 2001, Vol.323-324:223-230.)；Y2(Ca,Sr)
F4S2(it is detailed in document Yun-Chen Wu, Yi-Chin Chen, Teng-Ming Chen, Chi-Shen Lee, Kuo-Ju
Chenc,Hao-Chung Kuo,Crystal structure characterization,optical and
photoluminescent properties of tunable yellow-to orange-emitting Y2(Ca,Sr)
F4S2:Ce3+phosphors for solid-state lighting,Journal of Materials Chemistry,
2012,Vol.22:8048-8057.)；And Sm2CaF4S2(it is detailed in document A.Demourgues, A.Tressauda,
H.Laronzea,P.Gravereau,P.Macaudiére,Preparation and structural properties of
new series of mixed-anion compounds:rare earth fluorosulfides,Journal of
Fluorine Chemistry,2001,Vol.107(2):215–221.).Alkaline-earth metal and being formed by of light rare earth fluorides
Close object such as CeSrF4S2、CeCaF4S2Preparation process is complicated, needs slowly to be warming up to 1200 DEG C with the heating rate of 15 DEG C/h,
It is slow cooling to room temperature with the rate of temperature fall of 5 DEG C/h, pure phase CeSrF can just be obtained by being annealed at 1100 DEG C4S2、
CeCaF4S2, preparation temperature is high and condition is harsh.And alkali metal and rare earth fluorine sulfide are formed at present new compound there is not yet
Document report, this kind of ' alkali metal-rare earth fluorine sulfide ' be expected with and alkaline-earth metal-rare earth fluorine sulfide have different knots
Structure and property, to be expected to become basis material a new class of, that different-waveband is luminous.
Summary of the invention
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of alkali metal-rare earth fluorine sulfide NaLaF2S and
Its synthetic method.
Technical solution
A kind of alkali metal rare earth fluorine sulfide NaLaF2S, it is characterised in that the molecular formula of alkali metal rare earth fluorine sulfide is
NaLaF2S；It is La according to the ratio between amount of substance by analyzing pure grade lanthanum oxide powder and sodium fluoride3+:Na+=1.0:(4.0~
6.0) it synthesizes；The lanthana molecular formula: La2O3；The sodium fluoride molecular formula: NaF.
A kind of alkali metal rare earth fluorine sulfide NaLaF2The synthetic method of S, it is characterised in that steps are as follows:
The preparation of step 1, presoma powder:
It is La according to the ratio between amount of substance at 25 DEG C3+:Na+=1.0:(4.0~6.0), pure grade lanthana powder will be analyzed
Body and sodium fluoride, which are placed in mortar to be fully ground, makes its mixing, obtains the presoma powder that lanthana is mixed with NaF；
The lanthana molecular formula: La2O3；The sodium fluoride molecular formula: NaF；
Step 2, NaLaF2The preparation of S compound powder:
Presoma powder is placed in atmosphere tube type furnace, under the Ar protection that flow is 30mL/min, with the rate of heat addition 5
DEG C/min heating；
When tubular type furnace temperature rises to 700 DEG C, it is passed through the Ar gas and CS that flow is 30mL/min2Mixed gas, continue
So that tube furnace is warming up to 750~850 DEG C, and keeps the temperature 120-180min；Wherein mixed gas volume ratio is
After heat preservation, CS is closed2Gas, being passed through flow is the Ar gas of 30mL/min as protective gas, to tube furnace
Cooled to room temperature takes out powder, successively uses deionized water and washes of absolute alcohol powder each 1 time, then again puts powder
Enter in vacuum oven, at 60 DEG C, vacuum degree 5Pa, keep being dried for 3 hours, taking out dry powder is to prepare
NaLaF2S powder.
The pure grade lanthanum oxide powder of analysis is 200~300 mesh.
Beneficial effect
A kind of alkali metal proposed by the present invention-rare earth fluorine sulfide NaLaF2S and its synthetic method, it is characterised in that alkali gold
The molecular formula for belonging to rare earth fluorine sulfide is NaLaF2S；By analyzing pure grade lanthanum oxide powder and sodium fluoride, according to the ratio between the amount of substance
For La3+:Na+=1.0:(4.0~6.0) synthesis.When synthesis under the conditions of certain synthesis temperature and shorter soaking time, with
Lanthana and sodium fluoride are raw material, with CS2For sulfiding gas, NaLaF can be easily synthesized2S compound.Meanwhile technique letter
It is single, it is suitable for large scale preparation alkali metal rare earth fluorine sulfide, has broad application prospects.
Specific embodiment
Now in conjunction with embodiment, the invention will be further described:
Embodiment one:
The preparation of step 1 presoma powder:
16.3 grams of the analysis pure zirconia lanthanum powder of 200 mesh and 8.4 grams of the pure sodium fluoride of analysis of 200 mesh are weighed respectively, so that
The ratio between the amount of the two substance meets La3+:Na+=1.0:4.0.At 25 DEG C, by weighed NaF and La2O3It is placed in mortar and fills
Divide grinding to be uniformly mixed it, lanthana and the mixed uniformly presoma powder of NaF can be obtained.
Step 2NaLaF2The preparation of S compound powder:
It is placed in prepared by step 1 in atmosphere tube type furnace for 24.7 grams of presoma powder, is protected in the Ar that flow is 30mL/min
Under shield, with 5 DEG C/min of rate of heat addition heating, when tubular type furnace temperature rises to 700 DEG C, the gas being passed through is changed to Ar gas and CS2
Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio isContinue to be warming up to tube furnace
750 DEG C, and keep the temperature 180min.After heat preservation, CS is closed2Mixed gas is still used instead the Ar gas of 30mL/min flow by gas
Powder is taken out to tube furnace cooled to room temperature as protective gas, successively uses deionized water and washes of absolute alcohol powder
Each 1 time, then powder is put into vacuum oven again, at 60 DEG C, vacuum degree 5Pa, keeps being dried for 3 hours, take out
Dry powder is the NaLaF prepared2S powder.
Embodiment two:
The preparation of step 1 presoma powder:
9.78 grams of the analysis pure zirconia lanthanum powder of 300 mesh and 7.56 grams of the pure sodium fluoride of analysis of 300 mesh are weighed respectively, so that
The ratio between the amount of the two substance meets La3+:Na+=1.0:6.0.At 25 DEG C, by weighed NaF and La2O3It is placed in mortar and fills
Divide grinding to be uniformly mixed it, lanthana and N can be obtainedaThe mixed uniformly presoma powder of F.
Step 2NaLaF2The preparation of S compound powder:
It is placed in prepared by step 1 in atmosphere tube type furnace for 17.34 grams of presoma powder, is protected in the Ar that flow is 30mL/min
Under shield, with 5 DEG C/min of rate of heat addition heating, when tubular type furnace temperature rises to 700 DEG C, the gas being passed through is changed to Ar gas and CS2
Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio isContinue to be warming up to tube furnace
850 DEG C, and keep the temperature 120min.After heat preservation, CS is closed2Mixed gas is still used instead the Ar gas of 30mL/min flow by gas
Powder is taken out to tube furnace cooled to room temperature as protective gas, successively uses deionized water and washes of absolute alcohol powder
Each 1 time, then powder is put into vacuum oven again, at 60 DEG C, vacuum degree 5Pa, keeps being dried for 3 hours, take out
Dry powder is the NaLaF prepared2S powder.
Embodiment three:
The preparation of step 1 presoma powder:
13.0 grams of the analysis pure zirconia lanthanum powder of 250 mesh and 8.4 grams of the pure sodium fluoride of analysis of 250 mesh are weighed respectively, so that
The ratio between the amount of the two substance meets La3+:Na+=1.0:5.0.At 25 DEG C, by weighed NaF and La2O3It is placed in mortar and fills
Divide grinding to be uniformly mixed it, lanthana and the mixed uniformly presoma powder of NaF can be obtained.
Step 2NaLaF2The preparation of S compound powder:
It is placed in prepared by step 1 in atmosphere tube type furnace for 21.4 grams of presoma powder, is protected in the Ar that flow is 30mL/min
Under shield, with 5 DEG C/min of rate of heat addition heating, when tubular type furnace temperature rises to 700 DEG C, the gas being passed through is changed to Ar gas and CS2
Mixed gas, total gas flow rate is constant, and wherein mixed gas volume ratio isContinue to be warming up to tube furnace
800 DEG C, and keep the temperature 150min.After heat preservation, CS is closed2Mixed gas is still used instead the Ar gas of 30mL/min flow by gas
Powder is taken out to tube furnace cooled to room temperature as protective gas, successively uses deionized water and washes of absolute alcohol powder
Each 1 time, then powder is put into vacuum oven again, at 60 DEG C, vacuum degree 5Pa, keeps being dried for 3 hours, take out
Dry powder is the NaLaF prepared2S powder.
Claims (3)
1. a kind of alkali metal rare earth fluorine sulfide NaLaF2S, it is characterised in that the molecular formula of alkali metal rare earth fluorine sulfide is
NaLaF2S；It is La according to the ratio between amount of substance by analyzing pure grade lanthanum oxide powder and sodium fluoride3+:Na+=1.0:(4.0~
6.0) it synthesizes；The lanthana molecular formula: La2O3；The sodium fluoride molecular formula: NaF.
2. alkali metal rare earth fluorine sulfide NaLaF described in a kind of claim 12The synthetic method of S, it is characterised in that steps are as follows:
The preparation of step 1, presoma powder:
It is La according to the ratio between amount of substance at 25 DEG C3+:Na+=1.0:(4.0~6.0), will analyze pure grade lanthanum oxide powder and
Sodium fluoride, which is placed in mortar to be fully ground, makes its mixing, obtains the presoma powder that lanthana is mixed with NaF；
The lanthana molecular formula: La2O3；The sodium fluoride molecular formula: NaF；
Step 2, NaLaF2The preparation of S compound powder:
Presoma powder is placed in atmosphere tube type furnace, under the Ar protection that flow is 30mL/min, with 5 DEG C/min of the rate of heat addition
Heating；
When tubular type furnace temperature rises to 700 DEG C, it is passed through the Ar gas and CS that flow is 30mL/min2Mixed gas, continue to make tubular type
Furnace is warming up to 750~850 DEG C, and keeps the temperature 120-180min；Wherein mixed gas volume ratio is
After heat preservation, CS is closed2Gas, being passed through flow is the Ar gas of 30mL/min as protective gas, naturally cold to tube furnace
But to room temperature, powder is taken out, deionized water and washes of absolute alcohol powder each 1 time is successively used, powder is then put into vacuum again
It in drying box, at 60 DEG C, vacuum degree 5Pa, keeps being dried for 3 hours, taking out dry powder is the NaLaF prepared2S
Powder.
3. alkali metal rare earth fluorine sulfide NaLaF according to claim 22The synthetic method of S, it is characterised in that: the analysis
Pure grade lanthanum oxide powder is 200~300 mesh.
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