CN106629808B - A kind of solution growth samarium oxychloride is nanocrystalline and its method - Google Patents
A kind of solution growth samarium oxychloride is nanocrystalline and its method Download PDFInfo
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Abstract
The present invention relates to a kind of solution growth samarium oxychloride is nanocrystalline and its method, belong to inorganic ternary rare earth compound nano crystalline substance materials synthesis field.First according to 1：The molar ratio of (1~10), samarium source and chlorine source presoma are disperseed in a solvent, reach uniform mixing by stirring.Then under protective atmosphere, more than 200 degrees Celsius are warming up to, by certain soaking time, completes the nanocrystalline growth of samarium oxychloride.Then, can to obtain samarium oxychloride by centrifugation nanocrystalline.The samarium oxychloride that is grown is nanocrystalline to have complete cuboid pattern, and thickness is about 20 nanometers, meanwhile, there is good monodispersity.The present invention is nanocrystalline using solwution method synthesis samarium oxychloride, low with reaction temperature, easy to operate, is easy to control, and the nanocrystalline purity of prepared samarium oxychloride is high, without any observable impurities phase.Important material platform is provided for the nanocrystalline physicochemical properties of further research samarium oxychloride.
Description
【Technical field】
The invention belongs to inorganic ternary rare earth compound nano crystalline substance materials synthesis field, and in particular to a kind of solution growth
Samarium oxychloride is nanocrystalline and its method.
【Background technology】
Rare earth element causes rare earth based compound to have abundant physical chemistry due to its special 4f electron orbit
Matter, such as catalytic performance, optical property, magnetic performance etc..The oxyhalide tool of rare-earth-based has been widely used, including as fluorescence
Powder (Frank E.Swindells, Lanthanum Oxychloride Phosphors [J], Journal of
Electrochemical Society, 1954,101:415-418), scintillator (Yetta D.Eagleman, Edith
Bourret-Courchesne, Stephen E.Derenzo, Room-temperature scintillation
Properties of cerium-doped REOX (RE=Y, La, Gd, and Lu；X=F, Cl, Br, and I) [J],
Journal of Luminescence, 2011,131 (4)：669-675), ion conductor (K.Okamoto, N.Imanaka, and
G.Adachi,Chloride Ion Conduction in Rare Earth Oxychlorides[J],Solid State
Ionics,2002,154-155:577-580), catalyst (Simon G.Podkolzin, Eric E.Stangland, Mark
E.Jones, Elvira Peringer, Johannes A.Lercher, Methyl Chloride Production from
Methane over Lanthanum-Based Catalysts [J], Journal of American Chemical
Society,2007,129(9)：2569-2576) etc..These purposes cause rare earth oxychloride to have important commercial value.
Samarium oxychloride (SmOCl) compound is one kind of rare earth oxychloride family.It belongs to tetragonal crystal system, space group
For P4/nmn (129).Cell parameter is respectively：A, b, c are respectivelyWithFrom crystal structure
See, samarium oxychloride is a kind of lamellar compound.Rare earth samarium element and oxygen element form stronger chemical bonding, between chlorine element by
Independent one layer is formed in stronger chemical bonding.
For preparation method, the oxyhalide of rare-earth-based uses traditional solid phase reaction, generally requires higher temperature,
Such as 900 degrees Celsius.But traditional solid phase reaction can not obtain the rare earth oxychloride of nanoscale.For rare earth oxyhalogen
The research of the synthetic method of compound, major limitation is in terms of block materials and film so far.Nanometer on rare earth oxychloride
Investigation of materials, only fragmentary report.For example tight pure China et al. uses (La (CCl3COO)3) single source presoma is in octadecylene and length
By thermal decomposition in chain amine aqueous solution, zirconyl oxyhalides lanthanum is prepared for.Sarbajit Banerjee et al. are reported using LnCl3And Ln
(OiPr)3Nanocrystalline (the Kenneth R.Kort and Sarbajit of LnOCl (Ln=La, Ce, Gd, Dy, Er, Yb) are synthesized
Banerjee,Shape-controlled synthesis of well-defined matlockite LnOCl(Ln:La,
Ce,Gd,Dy)nanocrystals by a novel non-hydrolytic approach[J],Inorganic
Chemistry,2011,50(12):, but single source presoma and Ln (O 5539-5544)iPr)3Synthesis is general very complicated, causes into
This is excessive.
Block samarium oxychloride compound is generated usually using samarium oxide and ammonium chloride in 850-950 degrees Celsius of reaction, is obtained
The samarium oxychloride obtained is polycrystalline material (JormaJoni Korventausta,Ralf-Johan
EijaPierre Porcher,Host anion effect on the energy level scheme of
Sm3+In SmOX (X=F, Cl and Br) [J], Journal of Luminescence, 1997,72-74:204-207).This
Outside on samarium oxychloride is nanocrystalline and preparation method research, there is no any report also so far.
【The content of the invention】
It is an object of the invention to overcome existing the defects of reporting for work without any samarium oxychloride Syntheses technology, there is provided one
Kind of solution growth samarium oxychloride is nanocrystalline and its method, using samarium source and chlorine source, greatly reduces the original needed for reaction synthesis
Expect cost, while it is nanocrystalline to be made samarium oxychloride, for faced blocks samarium oxychloride, increases specific surface area, beneficial to raising
The performance of samarium oxychloride compound.
In order to achieve the above object, the present invention adopts the following technical scheme that：
Comprise the following steps：
Step 1：Samarium source and chlorine source are added in solvent, obtain mixed solution；Mole wherein between samarium source and chlorine source
Than for 1：(1~10)；
Step 2：Under lasting stirring and protective atmosphere, mixed solution is warming up to more than 200 DEG C and is reacted, completed
Nanometer crystals growth, product is nanocrystalline by separation acquisition samarium oxychloride.
Further, the samarium source in step 1 includes acetylacetone,2,4-pentanedione samarium, isopropoxy samarium or acetic acid samarium.
Further, the chlorine source in step 1 includes ammonium chloride, hexadecyltrimethylammonium chloride, tetradecyltrimethylammonium
One kind in ammonium chloride, cetalkonium chloride, cetylpyridinium chloride and octyltrimethylammonium chloride.
Further, the solvent in step 1 includes：Octadecylene, oleyl amine, oleic acid, lauryl amine, cetylamine, octadecylamine, ten
One or any two or more mixture in eight alkyl tertiary amines and trioctylamine.
Further, it is to carry out continuing stirring by 50~1500 revs/min of magnetic agitation in step 2；Protect gas
Atmosphere is nitrogen or argon gas.
Further, the heating rate of mixed solution is 2~20 DEG C/min in step 2.
Further, mixed solution is reacted from room temperature to 200~320 DEG C in step 2, is cooled to after reaction
Room temperature carries out product separation again.
Further, the reaction time is 2~500 minutes in step 2.
Further, product obtains chlorine by the centrifugation that centrifugation rate is 2000~10000 revs/min in step 3
Samarium oxide is nanocrystalline.
Further, it is cuboid pattern that the samarium oxychloride is nanocrystalline, and thickness is 5~40 nanometers, 10~60 nanometers of width,
Length is 15~100 nanometers.
Compared with prior art, the present invention has technique effect beneficial below：
First samarium source and chlorine source are put into solvent in the present invention, make them fully dispersed by stirring；Reaction solution system
As temperature rises, Sm atom and chlorine atom obtain sufficiently high thermal energy, across potential barrier, form substantial amounts of samarium oxychloride nucleus；
Samarium oxychloride nucleus is gradually grown up by competition, some nucleus, and some fades away, and completes nucleus maturing process；Finally, grow up
Crystal consume small crystal nucleus in reaction system, reach a kind of dynamic equilibrium, complete crystal growth；The present invention uses solution
Method, the characteristics of reaction using samarium source and chlorine source in high boiling solvent, by being nucleated, curing, nuclei growth three phases, is completed
The nanocrystalline growth of samarium oxychloride, is then simply centrifuged, you can the samarium oxychloride for preparing pure phase is nanocrystalline.This
Invention raw material sources are extensive, and reaction is gentle, and traditional solid-phase sintering method compares, and required reaction temperature is very low, at 200 DEG C
It can react above；Product purity is very high, and no any impurity mutually occurs, reaction yield 100%, and no any impurity material produces.
The present invention synthesizes samarium oxychloride using samarium source simple and easy to get and chlorine source and greatly reduces the required cost of material of reaction synthesis,
With important economic value, involved whole growth and separation process fast and easy, technique are simple.
Further, the solvent boiling point used in the present invention is higher, can react at a higher temperature, improves crystalline
Amount.
The nanocrystalline habit of samarium oxychloride that the present invention is grown is rectangular shape, and crystallization is complete, and Size Distribution is equal
One.For its nanocrystalline opposite micron-sized block materials of samarium oxychloride of the present invention, its size greatly reduces, and specific surface area is significantly
Increase, is expected to strengthen in terms of photocatalysis performance, for explore samarium oxychloride it is nanocrystalline potential physical chemistry feature
Important material support is provided etc. performance.
【Brief description of the drawings】
Fig. 1 is the nanocrystalline X-ray spectrum of samarium oxychloride of the present invention.
Fig. 2 is the nanocrystalline transmission electron microscope figure of the samarium oxychloride of the present invention.
Fig. 3 is the nanocrystalline X-ray diffraction spectrum of the samarium oxychloride grown under the conditions of 200 DEG C.
Fig. 4 is the nanocrystalline X-ray diffraction spectrum of the samarium oxychloride grown under the conditions of 280 DEG C.
【Embodiment】
Samarium oxychloride nanometer crystals growth is related to following process.First, samarium source and chlorine source are put into high boiling solvent
In, by magnetic agitation, make them fully dispersed.Reaction solution system rises with temperature, and Sm atom and chlorine atom obtain foot
Enough high thermal energy, across potential barrier, forms substantial amounts of samarium oxychloride nucleus.Samarium oxychloride nucleus is gradual by competition, some nucleus
Grow up, some fades away, and as big nucleus " consumes " small crystal nucleus, here it is nucleus " maturing process ".Finally, the crystalline substance grown up
Body consumes the small crystal nucleus in reaction system, and reaches a kind of dynamic equilibrium, that is, completes crystal growth.The present invention is required
Samarium source and chlorine source and high boiling solvent, are conventional chemical medicines.Required purity requirement is not high, is the pure rank of analysis.
Specific method of the present invention comprises the following steps：
Step 1：The use of high boiling solvent is reaction transmitting medium according to certain molar ratio, samarium source and chlorine source are reaction
Raw material, the predecessor in samarium source, chlorine source is added in high boiling solvent, obtains a kind of mixed solution；Both samarium source and chlorine source it
Between the scope that can adjust of molar ratio be 1：The ratio of (1~10), samarium source and solvent is 0.2mmol：10mL.Samarium source is acetylacetone,2,4-pentanedione
Any one in samarium, isopropoxy samarium, acetic acid samarium；Chlorine source is ammonium chloride, hexadecyltrimethylammonium chloride, myristyl three
One in ammonio methacrylate, cetalkonium chloride, cetylpyridinium chloride and octyltrimethylammonium chloride
Kind；High boiling solvent includes：Octadecylene, oleyl amine, oleic acid, lauryl amine, cetylamine, octadecylamine, octadecyl tertiary amine and trioctylamine
In one or any two or more mixture.
Step 2：The obtained mixed solution of step 1 is put into reaction vessel, excluding reaction with vacuum pump first holds
Air in device, then by the use of inert gas as protective gas into line replacement, is persistently passed through inert gas to reaction vessel, is formed
Protective atmosphere.Inert gas is any one of high pure nitrogen and argon gas.
Step 3：Reaction vessel is put into heating unit, magnetic agitation is carried out with 50~1500 revs/min of rotating speed,
The temperature of reaction system rises to reaction temperature from room temperature using heating rate as 2~20 DEG C/min, such as more than 200 degree, preferably
200~320 DEG C, and 2~500 minutes are kept the temperature, room temperature is then cooled to, completes nanometer crystals growth.Product is passed through to centrifuge speed
Rate is 2000~10000 revs/min of centrifugation, obtains the samarium oxychloride nanocrystalline powder of white.
Unnecessary chlorine source cannot participate in reaction in the present invention, just separates, can reuse after centrifuging in the solution.
The present invention is further detailed below in conjunction with instantiation.
Embodiment 1
Measure 10 milliliters of oleyl amines to be put into 50 milliliters of there-necked flask, sequentially add acetic acid samarium and cetyl trimethyl chlorination
Each 0.2 mM of ammonium, the molar ratio of acetic acid samarium and hexadecyltrimethylammonium chloride is 1 at this time:1, acetic acid samarium and solvent oleyl amine
Ratio be 0.2mmol：10mL；1500 revs/min of magnetic agitation so that acetic acid samarium and hexadecyltrimethylammonium chloride are fully
It is dispersed in oleyl amine.The air in there-necked flask is taken out, is replaced with high-purity argon gas, then persistently leads to argon gas, is formed to reaction system
Protective atmosphere.Since room temperature, 320 DEG C are risen to 10 DEG C/min of heating rate, then keeps the temperature 60 minutes at 320 DEG C, then
Reaction system cools to room temperature.By reaction solution using centrifuging, centrifugation rate is 8600 revs/min, obtains the chlorine of white
Samarium oxide is nanocrystalline.
As shown in Figure 1, the resulting product has very strong X-ray diffraction peak, indicate good crystallinity.By and thing
00-012-0790 in phase data storehouse compares, and the resulting product and 00-012-0790 fit like a glove.It imply that and obtained
Product be pure samarium oxychloride.Transmission electron micrograph is shown shown in Fig. 2, and the samarium oxychloride obtained is cuboid,
About 40 nanometers and 80 nanometers respectively of about 20 nanometers of thickness, width and length.
Embodiment 2
Measure 5 milliliters of oleic acid respectively and 5 milliliters of octadecylenes are put into 50 milliliters of there-necked flask, sequentially add acetylacetone,2,4-pentanedione samarium
0.2 mM and 0.4 mM of octyltrimethylammonium chloride, 100 revs/min of magnetic agitation so that acetylacetone,2,4-pentanedione samarium and octyl group
Trimethyl ammonium chloride is sufficiently dispersed in solution.The air in there-necked flask is taken out, is replaced with high pure nitrogen, then persistently leads to nitrogen
Gas, protective atmosphere is formed to reaction system.Since room temperature, 200 DEG C are risen to 5 DEG C/min of heating rate, it is then warm herein
Degree insulation 2 minutes, following reaction system cools to room temperature.By reaction solution using centrifuge, centrifugation rate for 10000 turns/
Minute, the samarium oxychloride for obtaining white is nanocrystalline.
As shown in figure 3, the resulting product also has X ray diffracting characteristic peak.By with the 00- in thing phase data storehouse
012-0790 compares, and the diffraction maximum in the resulting product and 00-012-0790 is coincide, and occurs without impurity peaks.Penetrated by X
, although the samarium oxychloride obtained is nanocrystalline smaller, has there is the nanocrystalline spy of samarium oxychloride in line diffraction spectrum analysis
Levy peak.
The samarium oxychloride that the present embodiment is obtained is cuboid, about 5 nanometers of thickness, width and length respectively about 10 nanometers and
15 nanometers.
Embodiment 3
Measure 5 milliliters of octadecylamines respectively and 5 milliliters of octadecyl tertiary amines are put into 50 milliliters of there-necked flask, sequentially add different
1 mM of 0.2 mM of propoxyl group samarium and cetalkonium chloride, 1000 revs/min of magnetic agitation so that different
Propoxyl group samarium and cetalkonium chloride are sufficiently dispersed in solution.The air in there-necked flask is taken out, with height
Pure argon is replaced, and then persistently leads to argon gas, and protective atmosphere is formed to reaction system.Since room temperature, with 15 DEG C/min of heating
Speed rises to 280 DEG C, and then in this temperature 500 minutes, following reaction system cools to room temperature.By reaction solution use from
The heart separates, and centrifugation rate is 5000 revs/min, and the samarium oxychloride for obtaining white is nanocrystalline.The oxychloride that the present embodiment is obtained
Samarium is about 60 nanometers and 100 nanometers respectively of cuboid, about 40 nanometers of thickness, width and length.
As shown in figure 4, the X-ray diffraction peak of the resulting product is very sharp.By with the 00- in thing phase data storehouse
012-0790 compares, and all diffraction maximums in the resulting product and 00-012-0790 are coincide, and free from admixture peak occurs.
Embodiment 4
Measure 5 milliliters of oleic acid respectively and 5 milliliters of oleyl amines are put into 50 milliliters of there-necked flask, sequentially add acetylacetone,2,4-pentanedione samarium
0.2 mM and 0.6 mM of ammonium chloride, 800 revs/min of magnetic agitation so that acetylacetone,2,4-pentanedione samarium and ammonium chloride fully divide
Dissipate in the solution.The air in there-necked flask is taken out, is replaced with high-purity argon gas, then persistently leads to argon gas, is formed and protected to reaction system
Protect atmosphere.Since room temperature, 300 DEG C are risen to 5 DEG C/min of heating rate, then in this temperature 300 minutes, then
Reaction system cools to room temperature.By reaction solution using centrifuging, centrifugation rate is 2000 revs/min, obtains the chlorine of white
Samarium oxide is nanocrystalline.The samarium oxychloride that the present embodiment is obtained is cuboid, about 35 nanometers of thickness, width and length respectively about 50
Nanometer and 90 nanometers.
Embodiment 5
Measure 2 milliliters of lauryl amines respectively and 8 milliliters of octadecylamines are put into 50 milliliters of there-necked flask, sequentially add acetylacetone,2,4-pentanedione
2 mMs of 0.2 mM of samarium and cetalkonium chloride, 500 revs/min of magnetic agitation so that acetylacetone,2,4-pentanedione
Samarium and cetalkonium chloride are sufficiently dispersed in solution.The air in there-necked flask is taken out, uses high-purity argon gas
Displacement, then persistently leads to argon gas, and protective atmosphere is formed to reaction system.Since room temperature, with 20 DEG C/min of heating rate liter
To 260 DEG C, then in this temperature 30 minutes, following reaction system cools to room temperature.Reaction solution is used and is centrifuged,
Centrifugation rate is 6000 revs/min, and the samarium oxychloride for obtaining white is nanocrystalline.The samarium oxychloride that the present embodiment is obtained is rectangular
About 40 nanometers and 45 nanometers respectively of body, about 20 nanometers of thickness, width and length.
Embodiment 6
10 milliliters of cetylamines are measured respectively to be put into 50 milliliters of there-necked flask, sequentially add 0.2 mM of isopropoxy samarium
With 0.8 mM of cetylpyridinium chloride, 50 revs/min of magnetic agitation so that isopropoxy samarium and hexadecyl pyrrole
Pyridine is sufficiently dispersed in solution.The air in there-necked flask is taken out, is replaced with high-purity argon gas, then persistently leads to argon gas, to reaction
System forming protective atmosphere.Since room temperature, 240 DEG C are risen to 2 DEG C/min of heating rate, then in this temperature 150
Minute, following reaction system cools to room temperature.By reaction solution using centrifuging, centrifugation rate is 7000 revs/min, is obtained
The samarium oxychloride of white is nanocrystalline.The samarium oxychloride obtained is cuboid, about 20 nanometers of thickness, width and length respectively about 35
Nanometer and 50 nanometers.
Embodiment 7
Measure 4 milliliters of lauryl amines, 4 milliliters of cetylamines and 2 milliliters of trioctylamines respectively to be put into 50 milliliters of there-necked flask, successively
Add 1.6 mMs of 0.2 mM of acetic acid samarium and tetradecyl trimethyl ammonium chloride, 1200 revs/min of magnetic agitation so that second
Sour samarium and tetradecyl trimethyl ammonium chloride are sufficiently dispersed in solution.The air in there-necked flask is taken out, is put with high pure nitrogen
Change, subsequent maintaining nitrogen purge, protective atmosphere is formed to reaction system.Since room temperature, risen to 12 DEG C/min of heating rate
210 DEG C, then in this temperature 200 minutes, following reaction system cools to room temperature.Reaction solution is used and is centrifuged,
Centrifugation rate is 4000 revs/min, and the samarium oxychloride for obtaining white is nanocrystalline.The samarium oxychloride obtained is cuboid, thickness
About 20 nanometers, about 30 nanometers and 40 nanometers respectively of width and length.
The present invention is nanocrystalline in order to grow pure samarium oxychloride, and samarium source presoma and chlorine source presoma are dispersed in boiling point
In higher solvent, it is sufficiently mixed.It is put into reaction vessel, excludes air, is protected using inert gas.By one
Fixed heating rate reaches more than 200 degrees Celsius, then keeps the temperature at this temperature, carries out nanocrystalline growth.Finally will reaction
Solution drops to room temperature, centrifuges, and obtains the powder of white.
The present invention is a kind of nanocrystalline and growing method, particularly the nanocrystalline growing method of pure phase samarium oxychloride.This hair
Bright use high boiler is reaction medium and dispersant, and samarium source presoma and chlorine source presoma are reaction raw materials (molar ratio 1：1-
10), under the protection of inert gas, by way of high-temperature heating, it is nanocrystalline that pure phase samarium oxychloride can be obtained.
The samarium oxychloride that the present invention is grown is nanocrystal, and the obtained nanocrystalline regular appearance of samarium oxychloride, has crystallized
Good, monodispersity is good.Grown it is nanocrystalline be complete cuboid pattern, its thickness is in 20 rans.The present invention uses
Solwution method synthesis samarium oxychloride is nanocrystalline, has the advantages that reaction is gentle, easy to operate and is easy to control, and traditional solid phase is burnt
Knot method compares, and required reaction temperature is very low, and product purity is very high, and no any impurity mutually occurs.For further exploring it
In various functional properties supply the test sample of high-purity, for the further nanocrystalline physicochemical properties of research samarium oxychloride
Important material platform is provided, so as to have to explore samarium oxychloride nanocrystalline middle potential photocatalysis performance, light, electricity, magnetic etc.
The physical and chemical performance of interest provides important material and supports.
Claims (10)
1. a kind of nanocrystalline method of solution growth samarium oxychloride, it is characterised in that comprise the steps of：
Step 1：Samarium source and chlorine source are added in solvent, obtain mixed solution；Molar ratio wherein between samarium source and chlorine source is
1：(1~10)；
Step 2：Under lasting stirring and protective atmosphere, mixed solution is warming up to more than 200 DEG C and is reacted, complete nanometer
Crystals growth, product is nanocrystalline by separation acquisition samarium oxychloride.
A kind of 2. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 1
In samarium source include acetylacetone,2,4-pentanedione samarium, isopropoxy samarium or acetic acid samarium.
A kind of 3. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 1
In chlorine source include ammonium chloride, hexadecyltrimethylammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecyldimethyl benzyl ammonium benzyl
One kind in ammonium chloride, cetylpyridinium chloride and octyltrimethylammonium chloride.
A kind of 4. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 1
In solvent include：One in octadecylene, oleyl amine, oleic acid, lauryl amine, cetylamine, octadecylamine, octadecyl tertiary amine and trioctylamine
Kind or any two or more mixture.
A kind of 5. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 2
In be by 50~1500 revs/min of magnetic agitation carry out continue stirring；Protective atmosphere is nitrogen or argon gas.
A kind of 6. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 2
The heating rate of middle mixed solution is 2~20 DEG C/min.
A kind of 7. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 2
Middle mixed solution is reacted from room temperature to 200~320 DEG C, and room temperature is cooled to after reaction and carries out product separation again.
A kind of 8. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 2
The middle reaction time is 2~500 minutes.
A kind of 9. nanocrystalline method of solution growth samarium oxychloride according to claim 1, it is characterised in that：Step 3
Middle product is nanocrystalline by the centrifugation acquisition samarium oxychloride that centrifugation rate is 2000~10000 revs/min.
A kind of 10. samarium oxychloride that method nanocrystalline using solution growth samarium oxychloride described in claim 1 is grown
It is nanocrystalline, it is characterised in that：The nanocrystalline samarium oxychloride is cuboid pattern, and thickness is 5~40 nanometers, and width 10~60 is received
Rice, length are 15~100 nanometers.
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Citations (2)
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| CN102583494A (en) * | 2012-02-22 | 2012-07-18 | 中国科学院宁波材料技术与工程研究所 | Method for manufacturing CeOCl nano-particles |
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