CN109824024A - A kind of preparation method of lanthanide doped selenizing zinc nano material - Google Patents
A kind of preparation method of lanthanide doped selenizing zinc nano material Download PDFInfo
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- CN109824024A CN109824024A CN201910204318.4A CN201910204318A CN109824024A CN 109824024 A CN109824024 A CN 109824024A CN 201910204318 A CN201910204318 A CN 201910204318A CN 109824024 A CN109824024 A CN 109824024A
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Abstract
The invention discloses a kind of preparation methods of lanthanide ion doping selenizing zinc nano material, including following steps: step 1, weighing a certain amount of zinc selenide and lanthanide ion raw materials of compound in the balance, be put into machine and be allowed to be sufficiently mixed uniformly.Step 2, the powder mixed is put into progress solid-phase sintering processing in tube furnace.Step 3, the powder of fired completion is put into machine and is ground, a certain amount of powder is taken to be put into small beaker, while a certain amount of organic solvent is added and is allowed to disperse.Step 4, ultrasonic instrument is placed above small beaker, is ultrasonically treated.Step 5, the substance that ultrasound is completed is put into centrifuge, carries out centrifugal treating.Step 6, the selenizing zinc nano material that the clear yellow solution in upper layer is lanthanide ion doping is collected.The advantages such as preparation process of the present invention is simple, yield is high, controllable preparation, and in biomedicine, solar battery, the fields such as temperature detection have broad application prospects.
Description
Technical field
The invention belongs to field of nano material preparation, in particular to a kind of selenizing zinc nano material of lanthanide ion doping
Preparation method.
Background technique
Nano material refers to that at least one dimension is the material in nano-scale to a certain material in three dimensions, this is
It is equivalent to the scale of 10~100 atom packings together.Nano material has five big effects, is respectively: bulk effect, surface
Effect, quantum size effect, quantum tunneling effect, Dielectric confinement effect.The research of nano material, especially two-dimension nano materials
Research be nowadays researcher scientific research very popular direction, because its nano-device, high-efficiency solar electricity
Pond, treatment of cancer, biomedical imaging etc. are widely used.
Zinc selenide is a kind of II-VI race's semiconductor material of direct band gap, and forbidden bandwidth is 2.7ev, refractive power system under room temperature
Number up to 2.61, is a kind of photoelectric material that purposes is very extensive.A variety of photoelectric properties that zinc selenide is shown make it in light
Detection, blue emission laser, bioprobe etc. have highly important purposes.
Lanthanide series is located at the period 6 third subgroup of the periodic table of elements, including: the elements such as cerium, praseodymium, neodymium, these
The 4f electron orbit of element in occupation of very abundant energy level, it can be achieved that from ultraviolet to infrared absorption and transmitting, thus sending out
Optical arena is using very extensive.Both advantages can be played to zinc selenide semiconductor by lanthanide-doped, are allowed in photoelectricity
Field has a good application prospect.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of lanthanide doped zinc selenides
The preparation method of nano material, the technical solution used in the present invention are as follows:
A kind of preparation method of lanthanide doped selenizing zinc nano material, specific preparation process are as follows:
(1) a certain amount of zinc selenide raw material and lanthanide ion compound are weighed in the balance, puts it into machine and carries out adequately
Mixing and grinding.
(2) substance mixed is put into tube furnace, certain temperature schedule is set and is passed through certain gas, be sintered
Processing.
(3) that the substance sintered is put into machine is sufficiently levigate, takes a certain amount of powder to be put into beaker, while being added one
Fixed organic solvent is allowed to disperse.
(4) beaker is put into ice bath device, ultrasonic instrument is placed above beaker, be ultrasonically treated.
(5) the good substance of ultrasound is put into centrifuge, centrifugal treating.
(6) the upper layer yellow solution of centrifuge tube is taken out.
The doping of lanthanide ion in the step (1) are as follows: 0.1%~10%.
The atmosphere being passed through in the step (2) are as follows: nitrogen, helium, argon gas, nitrogen and hydrogen balance air pressure；Tubular type
The heating rate of furnace are as follows: 1 DEG C/min~100 DEG C/min, the firing time are as follows: the h of 1 h~24.
The milling time of machine is put into the step (3) are as follows: the min of 10 min~60；The organic solvent of addition are as follows: second
Alcohol, acetone, hexamethylene, cyclohexanol, methyl pyrrolidone, deionized water.
Ice bath temperature in the step (4) are as follows: -10 DEG C~10 DEG C；Ultrasonic time are as follows: the h of 1 h~24.
The revolving speed of centrifuge in the step (5) are as follows: the r/min of 1000 r/min~10000；Centrifugation time are as follows: 1 min
~20 min.
The present invention adulterates selenizing zinc nano material by lanthanide ion prepared by solid sintering technology and liquid phase stripping method
It has the advantage that
1. prepared substance crystal phase is pure.This substance is by the way that synthesized by solid sintering technology, prepared product crystallinity is very excellent
It is different.
2. yield is high.Yield by selenizing zinc nano material prepared by liquid phase stripping method is very high.
3. luminescent properties are excellent.Prepared lanthanide doped selenizing zinc nano material, it is equal in infrared region and visible region
With good luminescent properties.
4. preparation method is simple.Material is prepared using high temperature solid phase synthesis and liquid phase stripping method, it is easy to operate and more
It is mature.
Detailed description of the invention
Fig. 1 is that erbium ion-doped selenizing zinc nano material TEM schemes.
Fig. 2 is to adulterate erbium ion selenizing zinc nano material in the photoluminescence spectra of near infrared region.
Fig. 3 is to adulterate erbium ion selenizing zinc nano material in the luminescence generated by light figure of green Region.
Fig. 4 is to adulterate erbium ion selenizing zinc nano material in the luminescence generated by light figure of red light district.
Fig. 5 is the XRD diagram of erbium ion-doped selenizing zinc nano material.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings.
Embodiment 1
Step 1 weighs the zinc selenide of 14.7682 g and the ErF_3 films raw material of 0.2318 g, is put into small grinder grinding 10
Min is allowed to be sufficiently mixed uniformly.
Ground powder is placed in tube furnace by step 2, is passed through argon gas, and temperature schedule is arranged are as follows: from room temperature with
The heating rate of 10 DEG C/min rises to 300 DEG C and keeps the temperature 1 hour, then rises to 950 DEG C again with the heating rate of 10 DEG C/min
And 4 hours are kept the temperature, finally it is naturally cooling to room temperature taking-up.
Step 3, the powder baked is placed again into small grinder and grinds 20min, then takes 100 mg's
Powder is put into small beaker, while the NMP of 50 ml is added, and is allowed to disperse.
Small beaker is put into ice bath device by step 4, guarantees that ice bath temperature is 0 DEG C or so；It is placed above beaker super
Ultrasonic time is arranged are as follows: 12h in acoustic device.
Ultrasonic good substance is put into centrifuge tube, centrifugation system is arranged by step 5 are as follows: first with 1000 r/min from
Heart rate is centrifuged 5 min for the first time, then is centrifuged 10 min again with the centrifugation rate of 3000 r/min.
Step 6 collects the upper layer clear solution in centrifuge tube, obtains kind of a lanthanide doped selenizing zinc nano material.
Embodiment 2
Step 1 weighs 19.6887 g zinc selenides and 0.3113 g fluorination thulium raw material in the balance, is placed in small grinder and grinds
20 min are ground, it is uniformly mixed.
Step 2 is put into the powder that grinding is completed in tube furnace, is passed through nitrogen, temperature schedule is then arranged are as follows: from room
Temperature rises to 300 DEG C with the heating rate of 5 DEG C/min and keeps the temperature 2 hours, then rises to 950 DEG C with the heating rate of 10 DEG C/min
And 5 hours are kept the temperature, finally it is naturally cooling to room temperature taking-up.
Step 3 is put into the powder for firing completion in small grinder and grinds 30 min, takes the powder of 50 mg to be put into small
In beaker, and the ethyl alcohol that 50 ml are added is dispersed.
Step 4 is put into small beaker in ice bath device, guarantees that ice bath temperature is 0 DEG C hereinafter, then placing ultrasound dress
It sets, and it is 9 h that ultrasonic time, which is arranged,.
The solution that ultrasound is completed is put into centrifuge tube, and centrifugation system is arranged by step 5 are as follows: first with 2000 r/min
Centrifugation rate be centrifuged 5 min for the first time, then 10 min are centrifuged again with the centrifugation rate of 4000 r/min.
Step 6 collects upper layer yellow solution, obtains kind of a lanthanide doped selenizing zinc nano material.
Embodiment 3
Step 1 weighs 14.7623 g zinc selenides and 0.2377 g fluorination ytterbium raw material, puts it into and grind 10 in small grinder
Min is allowed to uniformly mixed.
The powder ground is first put into tube furnace by step 2, is then passed through argon gas, and the temperature system of tube furnace is finally arranged
Degree are as follows: rise to 300 DEG C from room temperature with the heating rate of 10 DEG C/min and keep the temperature 1 hour, then with the heating rate of 10 DEG C/min
It rises to 950 DEG C and keeps the temperature 4 hours, be finally naturally cooling to room temperature taking-up.
The powder baked, is first put into small grinder and grinds 10 min by step 3, then takes the powder of 100 mg
End is put into small beaker, while the hexamethylene that 50 ml are added is dispersed.
Small beaker is placed in ice bath device by step 4, guarantees that ice bath temperature is 0 DEG C hereinafter, finally by Vltrasonic device
It is placed on small beaker, and ultrasonic time is set are as follows: 10 h.
The liquid that ultrasound is completed is put into centrifuge tube, while centrifugation rate is arranged by step 5 are as follows: first with 2000
The centrifugation rate of r/min is centrifuged 5 min for the first time, then is centrifuged 10 min again with the centrifugation rate of 4000 r/min.
Step 6 collects centrifuge tube clear solution at the middle and upper levels, obtains kind of a lanthanide doped selenizing zinc nano material.
Claims (6)
1. a kind of preparation method of lanthanide doped selenizing zinc nano material, which comprises the steps of:
(1) a certain amount of zinc selenide raw material and lanthanide ion compound are weighed in the balance, puts it into machine and carries out adequately
Mixing and grinding；
(2) substance mixed is put into tube furnace, certain temperature schedule is set and is passed through certain gas, be sintered place
Reason；
(3) that the substance sintered is put into machine is sufficiently levigate, and a certain amount of powder is taken to be put into beaker, while being added certain
Organic solvent is allowed to disperse；
(4) beaker is put into ice bath device, ultrasonic instrument is placed above beaker, be ultrasonically treated；
(5) the good substance of ultrasound is put into centrifuge, centrifugal treating；
(6) the upper layer yellow solution for taking out centrifuge tube obtains kind of a lanthanide doped selenizing zinc nano material.
2. the preparation method of lanthanide doped selenizing zinc nano material according to claim 1, it is characterised in that: the step
(1) doping of lanthanide ion in are as follows: 0.1%~10%.
3. the preparation method of lanthanide doped selenizing zinc nano material according to claim 1, it is characterised in that: the step
(2) atmosphere being passed through in are as follows: nitrogen, helium, argon gas, nitrogen and hydrogen balance air pressure；The heating rate of tube furnace are as follows: 1
DEG C/min~100 DEG C/min, the firing time are as follows: the h of 1 h~24.
4. the preparation method of lanthanide doped selenizing zinc nano material according to claim 1, it is characterised in that: the step
(3) milling time of machine is put into are as follows: the min of 10 min~60；The organic solvent of addition are as follows: ethyl alcohol, acetone, hexamethylene, ring
Hexanol, methyl pyrrolidone, deionized water.
5. the preparation method of lanthanide doped selenizing zinc nano material according to claim 1, it is characterised in that: the step
(4) ice bath temperature in are as follows: -10 DEG C~10 DEG C；Ultrasonic time are as follows: the h of 1 h~24.
6. the preparation method of lanthanide doped selenizing zinc nano material according to claim 1, it is characterised in that: the step
(5) revolving speed of centrifuge in are as follows: the r/min of 1000 r/min~10000；Centrifugation time are as follows: the min of 1 min~20.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110482596A (en) * | 2019-07-23 | 2019-11-22 | 中国计量大学 | A kind of bismuth titanates nanometer piece preparation method of double lanthanide ion codopes |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59120679A (en) * | 1982-12-27 | 1984-07-12 | Sumitomo Electric Ind Ltd | High-luminace illuminant for ion beam monitor and its preparation |
| CN104342158A (en) * | 2013-08-05 | 2015-02-11 | 海洋王照明科技股份有限公司 | Europium-erbium double-doped zinc selenide luminescent material, and preparation method and application thereof |
-
2019
- 2019-03-18 CN CN201910204318.4A patent/CN109824024B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59120679A (en) * | 1982-12-27 | 1984-07-12 | Sumitomo Electric Ind Ltd | High-luminace illuminant for ion beam monitor and its preparation |
| CN104342158A (en) * | 2013-08-05 | 2015-02-11 | 海洋王照明科技股份有限公司 | Europium-erbium double-doped zinc selenide luminescent material, and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110482596A (en) * | 2019-07-23 | 2019-11-22 | 中国计量大学 | A kind of bismuth titanates nanometer piece preparation method of double lanthanide ion codopes |
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