CN110054205A - Cesium iodide is nanocrystalline and its preparation method and application - Google Patents
Cesium iodide is nanocrystalline and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to technology of quantum dots fields, and it is nanocrystalline and preparation method thereof specifically to provide a kind of cesium iodide.The nanocrystalline preparation method of the cesium iodide at least includes the following steps: caesium source precursor solution being reacted 5~12min with propiodal precursor solution at 165~195 DEG C, reaction terminates quenching immediately and handles, and it is nanocrystalline to obtain cesium iodide；Caesium source precursor solution, propiodal precursor solution are insoluble oxygen molecule, hydrone.The ionic cesium iodide that the preparation method has synthesized different-shape is nanocrystalline, and the cesium iodide obtained is nanocrystalline without other phases or impurity, also the not presence of by-product, purity is up to 99.9% or more, optical transition ability more better than its block materials and efficiency, while block scintillator material shortcoming slow on the reaction time can be also made up to a certain extent.
Description
Technical field
The invention belongs to technology of quantum dots fields, and in particular to a kind of cesium iodide is nanocrystalline and its preparation method and application.
Background technique
In the society of current development in science and technology, nano material all plays increasingly important role in every field.
In in the past few decades, in the research in relation to nanometer scope material, metal nano material, semiconductor nano material and magnetism are received
Rice material is to be studied most nano materials.Wherein, semiconductor nano is also referred to as quantum dot, its radius be less than or
It is approximately equal to bohr exciton radii.In quanta point material, most classic is cadmium selenide (CdSe), cadmium telluride (CdTe) and vulcanization
Cadmium (CdS) etc. not only promotes the development of basic research to their exploration, while also having in terms of technical application important
Meaning.Up to now, the fluorescent emission of these types of quantum dot is still inhaled dependent on the size of its size and the characteristic distributions of size
Draw many researchers.This is mainly due to nanocrystalline quantum confined effects to play a role.These traditional binary are polynary
For metal chalcogenide compound due to the effect of quantum size effect, optical property improves a lot to its block materials.Except this
Except, also have multifunction surface chemical property and free colloidal state, can be dispersed in well various solvents and
In matrix, finally compatibly apply in different training equipments.For metallic nano crystal, many physics of itself are joined
It is several all to have an impact to its property, such as size, shape, element composition and crystal structure, change any one parameter and all may be used
To be changed to its property, at the same nanocrystalline variation flexibility and range be for specific parameter it is very sensitive, than
Such as in the application in terms of local surface plasma resonance (LSPR) and Surface enhanced Raman scattering (SERS), there is research to send out
It is existing, it is nanocrystalline for golden (Au) and silver-colored (Ag)；For, pattern and structure play ten to the quantity of LSPR, position and intensity
Divide important role.In terms of catalytic applications, there is research surface, improves the lively type of metallic nano crystal by reducing size.
In recent years, the comparison that magnetic nano-particle is studied in the application for including chemistry, biomedical, electronics and material engineering is more,
For magnetic nano-particle, they have special paramagnetic properties, and because there is excessive atom on surface, but only
The unsaturation that a small amount of ligancy can cause magnetic moment to be distributed, the track and spin moment of particle all improve a lot.Magnetic Nano
By the adjusting in size, can physics to its tobacco tar and chemical property regulate and control.These are different from block material
The property of material, so that magnetic Nano material is widely used in cancer diagnosis, giant magnetoresistance, magnetic liquid, magnetic recording, soft
The fields such as magnetic refrigeration and magnetic-optic devices.
Scintillator is that one kind can convert a branch of UV, visible light diffusing scattering from X-ray, gamma-rays etc. for high-energy photon
(UV-vis) light of range.In addition, the charged particle such as electronics, proton or heavier ion that accelerate, even neutron are ok
It is deposited on by their detection energy and is again converted to glisten together under the interaction of scintillator matrix.Due to this spy
Property, scintillator material is applied to spectrum or energy converter etc..Flashing is a kind of common phenomenon, in gas, liquid
It is likely to occur in body and solid.There are two types of important scintillator materials in solids, are solid inorganic flashing respectively
Body material and SOLID ORGANIC scintillator material.Wherein, the large percentage that inorganic scintillator material accounts in practical application and development,
Such as caesium iodide scintillator and nanometer scintillator.As it is previously noted that measure scintillator material a performance be die-away time, decline
Subtract that the time is shorter, it is better to the detectability of ray.This type scintillator has very much, but has certain drawbacks, such as
Barium fluoride, cupric iodide etc., although and the scintillation material decayed fastly, the emission wavelength of blue exterior domain and growth size
Limitation brings many inconvenience to detection.And this scintillator material of cesium iodide, the cubic system with high degree of symmetry, easily
In the growth of large size single crystal, die-away time is also shorter (being less than 10ns), so having largely about pure cesium iodide and doping
The research of the caesium iodide scintillator of other elements.For pure caesium iodide scintillator material, it is considered that be that there are two shine
Component, a main emission wavelength, that is, fast component, a slow component.Fastly, the ratio of component is smaller slowly, and the performance of material is better.
Technique due to preparing raw material and preparation used is also not quite similar, and the performance that difference studies obtained pure cesium iodide also has
Difference.In the research of pure cesium iodide crystal, following problem to be resolved is always existed: although (1) big cesium iodide block
Body material has good optical property, but bigger monocrystalline cesium iodide material is very fragile, is easy to be compromised；(2)
Bigger crystal growth is expensive, and the time of consumption is long, and the growth of high quality also will receive limitation；(3) right
For the inorganic cesium iodide material of particle shape, size and scalability are relatively good, but they are in organic solvent and polymerization
The solubility of object matrix is relatively low；(4) as the cesium iodide material as made from gel method, due to being gel state, translucency is not
It is that very well, its luminescent properties can be seriously affected.In addition, the transparent cesium iodide as made from sol-gal process is nanocrystalline, it is made into
Film rear surface is not very smooth, and particle uniformity is poor, and in practical applications, to the thickness of film, flatness,
Particle size and uniformity have very high requirement.
Summary of the invention
There is, photism low with solubility in organic solvent and polymer substrate when preparing cesium iodide for current gel method
Can be bad, particle uniformity is poor and excessively fragile the problems such as, the present invention provides a kind of preparation method that cesium iodide is nanocrystalline.
And by the cesium iodide that above-mentioned preparation method obtains it is nanocrystalline and its application.
For achieving the above object, technical scheme is as follows:
A kind of preparation method that cesium iodide is nanocrystalline, at least includes the following steps: by body before caesium source at 165~195 DEG C
Liquid solution reacts 5~12min with propiodal precursor solution, and reaction terminates quenching immediately and handles, and it is nanocrystalline to obtain cesium iodide；
Caesium source precursor solution, propiodal precursor solution are insoluble oxygen molecule, hydrone.
Correspondingly, a kind of cesium iodide is nanocrystalline, and the cesium iodide is nanocrystalline nanocrystalline using cesium iodide as described above
Preparation method is prepared, and the nanocrystalline cesium iodide is during ball shaped nano is brilliant, hexagonal plate is nanocrystalline, cube bulk is nanocrystalline
It is any.
And the nanocrystalline application in imaging of medical, electron emitter imaging field of cesium iodide.
The beneficial effect of the nanocrystalline preparation method of cesium iodide of the present invention is:
Compared with the existing technology, the nanocrystalline preparation method of cesium iodide of the invention has synthesized the ionic of different-shape
Cesium iodide is nanocrystalline, and the cesium iodide obtained is nanocrystalline without other phases or impurity, the also not presence of by-product, purity
Up to 99.9% or more.In preparation method preparation process of the invention, have simple process, nanocrystalline morphology controllable etc. excellent
Gesture.
Cesium iodide provided by the invention is nanocrystalline to be used as nanometer scintillator, three-dimensional confinement effect and electrons and holes wave
Preferably overlapping occurs for function, has optical transition ability more better than its block materials and efficiency, while also can be in certain journey
Block scintillator material deficiency slow on the reaction time is made up on degree.Therefore, imaging of medical, electronics hair be can be widely applied to
The fields such as beam imaging.
Detailed description of the invention
It to describe the technical solutions in the embodiments of the present invention more clearly, below will be to needed in the embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for ability
For the those of ordinary skill of domain, without creative efforts, it can also be obtained according to these attached drawings other attached
Figure.
Fig. 1 is the nanocrystalline XRD spectrum of the cesium iodide that is prepared of the embodiment of the present invention 1,2,3；
Fig. 2 is nanocrystalline transmission electron microscope (TEM) figure of the spherical cesium iodide that is prepared of the embodiment of the present invention 1；
Fig. 3 is the nanocrystalline high resolution TEM (HRTEM) of the spherical cesium iodide that is prepared of the embodiment of the present invention 1
Figure；
Fig. 4 is nanocrystalline TEM, HRTEM figure of the hexagonal plate cesium iodide that is prepared of the embodiment of the present invention 2；
Fig. 5 is nanocrystalline TEM, HRTEM figure of the cubic block cesium iodide that is prepared of the embodiment of the present invention 3.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, not
For limiting the present invention.
Present example provides a kind of preparation method that cesium iodide is nanocrystalline.The preparation method at least includes the following steps:
Caesium source precursor solution is reacted into 5~12min with propiodal precursor solution at 165~195 DEG C, reaction terminates vertical
I.e. quenching is handled, and it is nanocrystalline to obtain cesium iodide；
Caesium source precursor solution, propiodal precursor solution are insoluble oxygen molecule, hydrone.
Preparation method technical solution of the invention is further explained in detail below.
Above-mentioned caesium source precursor solution is the caesium source precursor solution of octadecene and oleic acid, that is, solvent is 18
The mixture of carbene and oleic acid, solute are the substance containing caesium.
Preferably, in the precursor solution of the caesium source, the volume ratio of octadecene and oleic acid mixture is (28~35): 1.
Caesium source is dissolved in the in the mixed solvent obtained under the proportion by octadecene and oleic acid, caesium source solution rate is fast, can obtain
Good oil-phase solution.
Preferably, caesium source is cesium carbonate.
It other side reactions occurs and is preparing cesium iodide nanometer to avoid cesium carbonate from being dissolved in octadecene and oleic acid
There is side reaction during brilliant, need before octadecene, oleic acid to be to cesium iodide dissolution, is dried, deoxygenation processing, mentions
The purity of high octadecene and oleic acid reduces a possibility that side reaction occurs.
Preferably, the solute of the propiodal precursor solution is diiodinating germanium, sodium iodide, potassium iodide, calcium iodide, tetraiodide
Any one of tin, these types of propiodal is soluble, and will not introduce other side reaction product impurity；The propiodal precursor is molten
The solvent of liquid is the mixture of oleic acid, oleyl amine, octadecene, using oleic acid, oleyl amine and octadecene as propiodal precursor solution
Solvent obtain oil-phase solution so that propiodal is dissolved in wherein, avoid introducing the other compositions such as water.
Preferably, in the solvent of propiodal precursor solution, according to volume ratio, the oleic acid: oleyl amine: octadecene=1:1:
(18~22).
Nanocrystalline if necessary to obtain cube block-like cesium iodide, then the solvent of propiodal precursor solution is in addition to oleic acid, oil
It further include tri octyl phosphine, and the volume ratio of the tri octyl phosphine and the octadecene is (1.8 except amine and octadecene
~2.5): 1.Into propiodal precursor solution add tri octyl phosphine after, be conducive to hexagonal plate cesium iodide it is nanocrystalline into
The cesium iodide that one step generates cubic block is nanocrystalline.
According to above-mentioned caesium source precursor solution and the component of propiodal precursor solution, according to molar ratio, body before the caesium source
The ratio of iodine is (4.0~5.0): (3.0~9.5) in cesium element and the propiodal precursor in liquid solution.In aforementioned item
Under part, with propiodal input amount increase and the extension in reaction time, the cesium iodide of generation it is nanocrystalline can by spherical shape by
Crossfade into hexagonal plate, cube bulk.Such as when the mole of cesium element and the mole ratio of iodine are 4.6:3.06, instead
5min is answered, it is nanocrystalline to obtain spherical cesium iodide；And if the molar ratio of the two is about 4.6:6.13, the reaction time extends to
It is nanocrystalline then to generate hexagonal plate cesium iodide by 10min or so；The two molar ratio is about 4.6:9.19, and the reaction time extends to
10min or so, and when containing in propiodal precursor solution tri octyl phosphine, it is nanocrystalline that blocky cesium iodide can be obtained cube.
In the present invention, quenching processing can effectively solve to generate the nanocrystalline partial size of cesium iodide is inhomogenous, surface irregularity
The problems such as.
Preferably, quenching processing is water-bath or oil bath.
The nanocrystalline preparation method of cesium iodide provided by the invention, it is nanocrystalline at the ionic cesium iodide of different-shape,
And obtain cesium iodide it is nanocrystalline without other mutually or impurity, the also not presence of by-product, purity be up to 99.9% and
More than.In preparation method preparation process of the invention, have production process safe and reliable, process conditions are simple and easy to control, are produced into
The advantages such as this low, nanocrystalline morphology controllable are suitable for industrialization large-scale production.
The nanocrystalline purity is high of cesium iodide that above-mentioned preparation method obtains, morphology controllable can be used as a nanometer scintillator, thirdly
It ties up confinement effect and preferably overlapping occurs for electrons and holes wave function, there is optical transition energy more better than its block materials
Power and efficiency, while block scintillator material deficiency slow on the reaction time can be also made up to a certain extent.It therefore, can be with
It is widely used in the fields such as imaging of medical, electron emitter imaging, particle physics.
More effectively to illustrate technical solution of the present invention, technical side of the invention is illustrated below by specific embodiment
Case.
Embodiment 1
A kind of preparation method that spherical shape cesium iodide is nanocrystalline, comprising the following steps:
(1) the removal of impurities processing of solvent: 50mL octadecene is placed in single necked round bottom flask, is sealed with rubber plug, is then put
In 140 DEG C of oil bath, a syringe needle is inserted on rubber plug, syringe needle is connected with biexhaust pipe, in this 140 DEG C of oil bath items
It carries out filling under part and is vacuum-treated 30min, argon gas is passed through after exhausting, while inserting the protection balloon for being full of argon gas on rubber plug, with
Antiaircraft gas and water or other impurities enter.Oleic acid, oleyl amine use same processing means, in case using below.
(2) preparation of caesium source precursor solution: 0.015g cesium carbonate is put into the closed three neck round bottom of side port,
Then it connecting on condenser pipe, condenser pipe is connect with biexhaust pipe, and interface all uses vacuum grease lubrication, to guarantee airtightness,
Then the round-bottomed flask for filling cesium carbonate is subjected to vacuumize process, removes the ingredients such as the empty gas and water in flask, is filled with argon repeatedly
Gas, and vacuumize process, it is ensured that eliminate air, moisture.After exhausting by have already passed through drying process 3mL octadecene and
0.1mL oleic acid three-neck flask side port be added, and by the solution in flask be heated to 150 DEG C until cesium carbonate be completely dissolved,
To the last become colorless transparent solution, this solution is as the caesium source precursor solution in synthesis, for use.
(3) preparation of propiodal precursor solution: weighing the diiodinating germanium of 0.01g in the balance in glove box, to be placed in glass small
In bottle, taking-up is closed with rubber plug and is protected with argon gas ball, oleic acid, each 0.2mL of oleyl amine after addition is dried, octadecene
2mL is placed it in oil bath and is heated to 100 DEG C until it is dissolved as colorless and transparent solution, this solution is as the iodine in synthesis
Source precursor solution, for use.
(4) the caesium source precursor solution that step (2) obtains is heated to 180 DEG C by, propiodal prepared by later step (3)
Precursor solution is rapidly injected in the caesium source precursor solution for being heated to 180 DEG C, isothermal reaction 5min, uses water-bath quenching immediately
Three-neck flask.
(5) reaction solution that obtains cold bath quenching is collected in 50mL centrifuge tube, centrifugal speed 8000r/min, from
Heart 8min, it is nanocrystalline in centrifugation bottom of the tube and wall to have obtained cesium iodide, takes cesium iodide nanocrystalline, and receive to the cesium iodide of acquisition
5mL n-hexane is added in meter Jing Zhong, with ultrasonic machine ultrasound, makes cesium iodide is nanocrystalline to be uniformly dispersed in wherein, centrifuge separation, again
Ultrasound, dispersion, centrifugation are carried out using n-hexane, is dispersed in n-hexane for the cesium iodide finally obtained is nanocrystalline.
Embodiment 2
A kind of preparation method that hexagonal plate cesium iodide is nanocrystalline, comprising the following steps:
(1) the removal of impurities processing of solvent: 50mL octadecene is placed in single necked round bottom flask, is sealed with rubber plug, is then put
In 140 DEG C of oil bath, a syringe needle is inserted on rubber plug, syringe needle is connected with biexhaust pipe, in this 140 DEG C of oil bath items
It carries out filling under part and is vacuum-treated 30min, argon gas is passed through after exhausting, while inserting the protection balloon for being full of argon gas on rubber plug, with
Antiaircraft gas and water or other impurities enter.Oleic acid, oleyl amine use same processing means, in case using below.
(2) preparation of caesium source precursor solution: 0.015g cesium carbonate is put into the closed three neck round bottom of side port,
Then it connecting on condenser pipe, condenser pipe is connect with biexhaust pipe, and interface all uses vacuum grease lubrication, to guarantee airtightness,
Then the round-bottomed flask for filling cesium carbonate is subjected to vacuumize process, removes the ingredients such as the empty gas and water in flask, is filled with argon repeatedly
Gas, and vacuumize process, it is ensured that eliminate air, moisture.After exhausting by have already passed through drying process 3mL octadecene and
0.1mL oleic acid three-neck flask side port be added, and by the solution in flask be heated to 150 DEG C until cesium carbonate be completely dissolved,
To the last become colorless transparent solution, this solution is as the caesium source precursor solution in synthesis, for use.
(3) preparation of propiodal precursor solution: weighing the diiodinating germanium of 0.03g in the balance in glove box, to be placed in glass small
In bottle, taking-up is closed with rubber plug and is protected with argon gas ball, oleic acid, each 0.2mL of oleyl amine after addition is dried, octadecene
2mL is placed it in oil bath and is heated to 100 DEG C until it is dissolved as colorless and transparent solution, this solution is as the iodine in synthesis
Source precursor solution, for use.
(4) the caesium source precursor solution that step (2) obtains is heated to 180 DEG C by, propiodal prepared by later step (3)
Precursor solution is rapidly injected in the caesium source precursor solution for being heated to 180 DEG C, and isothermal reaction 10min is quenched with water-bath immediately
It is nanocrystalline to obtain hexagonal plate cesium iodide for cold three-neck flask.
(5) reaction solution that obtains cold bath quenching is collected in 50mL centrifuge tube, centrifugal speed 8000r/min, from
Heart 8min, it is nanocrystalline in centrifugation bottom of the tube and wall to have obtained cesium iodide, takes cesium iodide nanocrystalline, and receive to the cesium iodide of acquisition
5mL n-hexane is added in meter Jing Zhong, with ultrasonic machine ultrasound, makes cesium iodide is nanocrystalline to be uniformly dispersed in wherein, centrifuge separation, again
Ultrasound, dispersion, centrifugation are carried out using n-hexane, and is dispersed in n-hexane for the cesium iodide finally obtained is nanocrystalline.
Embodiment 3
The nanocrystalline preparation method of a kind of cube of blocky cesium iodide, comprising the following steps:
(1) the removal of impurities processing of solvent: 50mL octadecene is placed in single necked round bottom flask, is sealed with rubber plug, is then put
In 140 DEG C of oil bath, a syringe needle is inserted on rubber plug, syringe needle is connected with biexhaust pipe, in this 140 DEG C of oil bath items
It carries out filling under part and is vacuum-treated 30min, argon gas is passed through after exhausting, while inserting the protection balloon for being full of argon gas on rubber plug, with
Antiaircraft gas and water or other impurities enter.Oleic acid, oleyl amine use same processing means, in case using below.
(2) preparation of caesium source precursor solution: 0.015g cesium carbonate is put into the closed three neck round bottom of side port,
Then it connecting on condenser pipe, condenser pipe is connect with biexhaust pipe, and interface all uses vacuum grease lubrication, to guarantee airtightness,
Then the round-bottomed flask for filling cesium carbonate is subjected to vacuumize process, removes the ingredients such as the empty gas and water in flask, is filled with argon repeatedly
Gas, and vacuumize process, it is ensured that eliminate air, moisture.After exhausting by have already passed through drying process 3mL octadecene and
0.1mL oleic acid three-neck flask side port be added, and by the solution in flask be heated to 150 DEG C until cesium carbonate be completely dissolved,
To the last become colorless transparent solution, this solution is as the caesium source precursor solution in synthesis, for use.
(3) it the preparation of propiodal precursor solution: weighs the diiodinating germanium of 0.03g in the balance in glove box and is placed in and be loaded with
In the vial of 1mL tri octyl phosphine, with rubber plug closed take out and with argon gas ball protect, addition it is dried after oleic acid,
Oleyl amine each 0.2mL, octadecene 2mL, place it in oil bath be heated to 100 DEG C until its be dissolved as colorless and transparent solution,
This solution is as the propiodal precursor solution in synthesis, for use.
(4) the caesium source precursor solution that step (2) obtains is heated to 180 DEG C by, propiodal prepared by later step (3)
Precursor solution is rapidly injected in the caesium source precursor solution for being heated to 180 DEG C, and isothermal reaction 10min is quenched with water-bath immediately
It is nanocrystalline to obtain cube blocky cesium iodide for cold three-neck flask.
(5) reaction solution that obtains cold bath quenching is collected in 50mL centrifuge tube, centrifugal speed 8000r/min, from
Heart 8min, it is nanocrystalline in centrifugation bottom of the tube and wall to have obtained cesium iodide, takes cesium iodide nanocrystalline, and receive to the cesium iodide of acquisition
5mL n-hexane is added in meter Jing Zhong, with ultrasonic machine ultrasound, makes cesium iodide is nanocrystalline to be uniformly dispersed in wherein, centrifuge separation, again
Ultrasound, dispersion, centrifugation are carried out using n-hexane, is dispersed in n-hexane for the cesium iodide finally obtained is nanocrystalline.
It is respectively that spherical cesium iodide is nanocrystalline, hexagonal plate cesium iodide to verify the final product of Examples 1 to 3 acquisition
It is nanocrystalline, cube blocky cesium iodide is nanocrystalline, corresponding performance detection is carried out to it respectively, specifically includes X-ray powder diffraction
(XRD), transmission electron microscopy (TEM) and high resolution TEM scanning (HRTEM) test.
(1) XRD is tested
The final product of acquisition is tested according to the standard that conventional XRD is tested, test results are shown in figure 1.
By XRD diagram it is found that three diffraction spots can be mapped well with standard card, standard card is PDF#
06-0311, corresponding is simple cubic phase (Pm3m), without the appearance of other miscellaneous peaks, it was demonstrated that the iodate that embodiment 1,2,3 obtains
Caesium it is nanocrystalline be mutually it is purer, without the generation of by-product or other phases, wherein 2 θ=27.59,39.42,48.79,
56.97,64.43,71.46 and 78.23 ° of corresponding peaks be { 110 }, { 200 }, { 211 }, { 220 }, { 310 }, { 222 } and
{ 321 } crystal face.
(2) TEM and HRTEM test
According to the mode of operation that conventional TEM, HRTEM are scanned, specific test result is as shown in Figure 2-5.
Wherein, Fig. 2,3 are that the spherical cesium iodide that embodiment 1 obtains is nanocrystalline, and Fig. 2 is under the transmission electron microscope of low power
The cesium iodide nanosphere observed, from the figure, it can be seen that the cesium iodide of our synthesis is nanocrystalline to have good monodispersity,
Size is very uniform, and the average grain diameter of particle is 15nm.Fig. 3 is receiving of observing under powerful transmission electron microscope
The finer pattern of rice ball, is clear that the lattice on its surface, is carried out with DigitalMicrograph software to it
Measurement, spacing of lattice areCorresponding is the lattice of (110) crystal face.
Fig. 4 is that the hexagonal plate cesium iodide that embodiment 2 obtains is nanocrystalline, and Fig. 4 is hexagonal plate under low power transmission electron microscope
Cesium iodide is nanocrystalline.Equally, by measurement, average side length 40nm, illustration is high power transmission electron microscope picture, is sent out by measurement
Existing, spacing of lattice matches with (110) crystal face in standard card, while clearly lattice fringe also illustrates to obtain nanometer
Brilliant crystallinity is fine；
Fig. 5 is that cube blocky cesium iodide that embodiment 3 obtains is nanocrystalline, as the average side length of Fig. 5, cubic block are about
40nm, illustration also illustrate that (110) crystal face of its lattice and cesium iodide crystal matches.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc. within mind and principle should all include within protection scope of the present invention.
Claims (10)
1. a kind of preparation method that cesium iodide is nanocrystalline, which is characterized in that at least include the following steps:
Caesium source precursor solution is reacted into 5~12min with propiodal precursor solution at 165~195 DEG C, reaction terminates to quench immediately
It is nanocrystalline to obtain cesium iodide for cold treatment；
Caesium source precursor solution, propiodal precursor solution are insoluble oxygen molecule, hydrone.
2. the nanocrystalline preparation method of cesium iodide as described in claim 1, which is characterized in that according to molar ratio, the caesium source
The ratio of iodine is (4.0~5.0): (3.0~9.5) in cesium element and the propiodal precursor in precursor solution.
3. the nanocrystalline preparation method of cesium iodide as described in claim 1, which is characterized in that caesium source precursor solution is
Cesium carbonate solution, the solvent of the cesium carbonate solution are the mixture of octadecene and oleic acid.
4. the nanocrystalline preparation method of cesium iodide as claimed in claim 3, which is characterized in that the octadecene and oleic acid are mixed
The volume ratio of conjunction is (28~35): 1.
5. the nanocrystalline preparation method of cesium iodide as described in claim 1, which is characterized in that the propiodal precursor solution is
Diiodinating germanium solution or IodineSodium Solution or liquor kalii iodide or any one of iodate calcium solution or tin tetraiodide solution, it is described
The solvent of propiodal precursor solution is the mixture of oleic acid, oleyl amine, octadecene.
6. the nanocrystalline preparation method of cesium iodide as claimed in claim 5, which is characterized in that according to volume ratio, the oleic acid:
Oleyl amine: octadecene=1:1:(18~22).
7. the nanocrystalline preparation method of cesium iodide as claimed in claim 5, which is characterized in that the propiodal precursor solution
Solvent further includes tri octyl phosphine, and the volume ratio of the tri octyl phosphine and the octadecene is (1.8~2.5): 1.
8. the nanocrystalline preparation method of cesium iodide as described in claim 1, which is characterized in that caesium source precursor solution,
Propiodal precursor solution is prepared in starvation and in an inert atmosphere.
9. a kind of cesium iodide is nanocrystalline, which is characterized in that the cesium iodide is nanocrystalline using such as any one of claim 1~8 institute
The nanocrystalline preparation method of the cesium iodide stated is prepared, and the cesium iodide is nanocrystalline for ball shaped nano crystalline substance, hexagonal plate nanometer
Brilliant, cube bulk is any one of nanocrystalline.
10. as the cesium iodide of the nanocrystalline preparation method preparation of any one of claim 1~8 cesium iodide it is nanocrystalline medical treatment at
Application in picture, electron emitter imaging field.
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