CN109943338A - A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method - Google Patents
A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method Download PDFInfo
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Abstract
The present invention provides a kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation methods.A certain amount of indium selenide and rare earth ion fluoride are weighed, is put into agate mortar and is fully ground.It is then put into tube furnace, is passed through gas, carry out solid-phase sintering processing.It takes a certain amount of powder baked to be put into centrifuge tube again, a certain amount of NMP is added, then centrifuge tube is placed in Ultrasound Instrument and is ultrasonically treated.The good substance of ultrasound is finally put into centrifuge, carries out centrifugal treating, collection upper layer clear solution is rear-earth-doped InSe nanometer piece solution.The present invention is by adjusting the parameters such as tubular type furnace temperature system, Ultrasound Instrument ultrasound system, centrifuge centrifugation system, the rear-earth-doped InSe nanometer piece prepared, the advantages such as, yield high, controllable preparation simple with preparation process, in low-dimensional nano-device, contactless temperature probe, the fields such as biological neural imaging have a very important role.
Description
Technical field
The invention belongs to low-dimension nano material preparation field, in particular to a kind of system of rear-earth-doped InSe nanometer piece
It is standby.
Background technique
The research and development of new material have highly important effect for the production and living of people, and in its R&D process, material
The dimension of material has become a highly important parameter for adjusting material structure characteristic.Usual material is all three-dimensional structure, and is worked as
When material is changed to two dimension by three-dimensional structure, the physicochemical properties of this material can occur to change very significantly.Indium selenide is
The bandwidth (bandgap) of a kind of semiconductor material, different crystal phases is usual are as follows: 1.3ev, 1.5ev or 1.9ev, interlayer
It is stacked by Van der Waals for, after becoming two-dimensional structure from three-dimensional structure, in low-dimensional nano-device, biological neural
The aspect of imaging, solar battery thin film, many such as high efficiency photocatalyst has critically important application.
The 4f electron orbit of rare earth element has energy level abundant, and luminescence phenomenon is exactly the transition between energy level, thus
It can realize absorption and transmitting from ultra-violet (UV) band near infrared region.Also, shining for rare earth ion is produced with very high quantum
Rate, relatively narrow bandwidth, luminescent lifetime are long, stability is good, so in illumination field using very extensive.Rare earth element is mixed
It is miscellaneous that two-dimensional layer material is made again to indium selenide semiconductor material, both advantages can be integrated, are allowed in terms of photovoltaic applications
It plays a significant role.And now grinding extensively compared to two-dimensional semiconductors materials such as molybdenum disulfide, tungsten disulfide, two selenizing molybdenums
Study carefully, people also need to further strengthen for the preparation research of rare earth doped indium selenide two-dimensional semiconductor and application.
Summary of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides a kind of near-infrared luminous rare earths to mix
Miscellaneous InSe nanometer piece preparation method, the present invention adopts the following technical scheme:
A kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method, specific preparation process are as follows:
A) a certain amount of indium selenide and rare earth ion fluoride are weighed, is put into agate mortar and is fully ground；
B) powder after grinding is put into tube furnace, adjusts tubular type furnace temperature system and is passed through gas, carried out at solid-phase sintering
Reason；
C) sintered powder is put into agate mortar and is fully ground again, taken ground powder to be put into centrifuge tube, add
Enter NMP to be allowed to disperse；
D) NMP in step c) and mixture of powders are put into Ultrasound Instrument, adjust the parameters such as Ultrasound Instrument power and time, is surpassed
Sonication；
E) the NMP mixture after ultrasonic treatment is put into a centrifuge, adjusts the parameters such as centrifuge speed and time, is carried out
Centrifugal treating；
F) the upper layer clear brown solution after centrifugal treating is collected, rear-earth-doped InSe nanometer can be observed under Electronic Speculum
Piece.
The molar percentage for the amount that rare earth ion fluoride is adulterated in the step a) are as follows: 0.01%~10%.
Temperature schedule in the step b) are as follows: the heating rate of firing temperature is risen to from room temperature are as follows: 1 DEG C/min~50 DEG C/
min；Firing temperature are as follows: 500 DEG C~1000 DEG C；Firing time are as follows: the h of 1 h~10.
The quality of ground powder is weighed in the step c) are as follows: the mg of 1 mg~100；The volume of NMP is added are as follows: 1
The ml of ml~100.
The ultrasonic time in the step d) are as follows: the h. of 1 h~48
The centrifugation rate of centrifuge in the step e) are as follows: the r/min of 1000 r/min~20000.
The present invention by rear-earth-doped InSe nanometer piece prepared by solid sintering technology and liquid phase stripping method have with
Lower advantage:
1. preparation process is simple.This method is prepared by solid sintering technology and liquid phase stripping method, and both methods is easy to operate
And it is more mature.
2. better crystallinity degree.This method is that rear-earth-doped indium selenide is prepared by solid sintering technology, prepared doping
Indium selenide powder crystallinity afterwards is very excellent.
3. nanometer sheet yield is high.This method is that rear-earth-doped InSe nanometer piece is prepared by liquid phase stripping method, is led to
The parameters such as ultrasonic time and power are overregulated, a large amount of nanometer sheet can be prepared.
4. the InSe nanometer piece being prepared has good luminescent properties and water soluble characteristic.
Detailed description of the invention
Fig. 1 is the TEM figure of neodymium ion doped InSe nanometer piece.
Fig. 2 is the XRD diagram for adulterating the indium selenide of neodymium ion.
Fig. 3 is the luminescence generated by light figure for adulterating the indium selenide of neodymium ion.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings.
Embodiment 1
Step 1,14.935g indium selenide and 0.065g neodymium fluoride raw material are weighed, is put into agate mortar and is fully ground, is allowed to mix
Uniformly.
Step 2, the powder after grinding is put into tube furnace, is passed through atmosphere, temperature schedule is set are as follows: from room temperature with 10
DEG C/heating rate of min rises to 300 DEG C and keeps the temperature 1 hour, then again with the heating rate of 10 DEG C/min rise to 650 DEG C it is same
4 hours of Shi Baowen are finally naturally cooling to room temperature taking-up.
Step 3, the powder baked is put into agate mortar finely ground again, takes 20 mg powder to be put into centrifuge tube, together
When be added 10ml NMP be allowed to disperse.
Step 4, centrifuge tube is put into Ultrasound Instrument, adjusting Ultrasound Instrument power is 100, and ultrasonic time is 12 hours, and is protected
Water holding bath temperature is 10 DEG C or less.
Step 5, the mixture of NMP and powder after ultrasonic treatment are put into a centrifuge, be arranged centrifugation system are as follows: first with
The centrifugation rate of 3000 r/min is centrifuged 4 min for the first time, is then centrifuged 10 min again again with the centrifugation rate of 4000 r/min.
Step 6, the clear brown solution in upper layer is collected, rear-earth-doped InSe nanometer piece can be observed under Electronic Speculum.
Embodiment 2
Step 1, the indium selenide of 14.9270g and the fluorination thulium raw material of 0.0730g are weighed, puts it into agate mortar and sufficiently grinds
Mill, is allowed to uniformly mixed.
Step 2, the powder being fully ground is put into tube furnace, is passed through atmosphere, its temperature schedule is then set are as follows: from room temperature with
The heating rate of 5 DEG C/min rises to 300 DEG C and keeps the temperature 1 hour, then rises to 550 DEG C again with the heating rate of 10 DEG C/min
And 6 hours are kept the temperature, finally it is naturally cooling to room temperature taking-up.
Step 3, the powder baked is put and is regrind in the agate mortar, be allowed to finely ground, take the powder of 10 mg
It is put into centrifuge tube, while 10 ml NMP are added and are allowed to disperse.
Step 4, centrifuge tube is put into Ultrasound Instrument, adjusting Ultrasound Instrument power is 100, and ultrasonic time is 12 hours, and is protected
Water holding bath temperature is 10 DEG C hereinafter, being ultrasonically treated.
Step 5, the mixture of the NMP being ultrasonically treated and powder are put into centrifuge, centrifugation system is then set are as follows: first
It is centrifuged 5 min for the first time with the centrifugation rate of 2000 r/min, then 10 min are centrifuged again with the centrifugation rate of 4000 r/min.
Step 6, the clear brown solution in upper layer is collected, rear-earth-doped InSe nanometer piece can be observed under Electronic Speculum.
Embodiment 3
Step 1, the indium selenide of 14.9639g and the ErF_3 films raw material of 0.0361g are weighed, then it is put into mortar and sufficiently grinds
Mill, is allowed to uniformly mixed.
Step 2, ground powder is put into tube furnace, is passed through atmosphere, then the temperature schedule of tube furnace is set
Are as follows: 300 DEG C are risen to the heating rate of 5 DEG C/min from room temperature and keeps the temperature 1 hour, then with the heating rate liter of 10 DEG C/min
To 500 DEG C and 6 hours are kept the temperature, is finally naturally cooling to room temperature taking-up.
Step 3, the powder of fired completion is put into agate mortar and is regrind, take the powder of 10 mg be put into from
10 ml NMP are added in heart pipe at the same time.
Step 4, centrifuge tube is placed in Ultrasound Instrument, adjusting its power is 100, and the time is 12 hours, while to be guaranteed
Bath temperature is 10 DEG C hereinafter, ultrasonic treatment.
Step 5, the NMP and mixture of powders that have been ultrasonically treated are put into centrifuge, adjust centrifugation system are as follows: first with
The centrifugation rate of 2000 r/min is centrifuged 5 min for the first time, then is centrifuged 10 min again with the centrifugation rate of 5000 r/min.
Step 6, the clear brown solution in upper layer is collected, rear-earth-doped InSe nanometer piece can be observed under Electronic Speculum.
Claims (6)
1. a kind of near-infrared luminous rear-earth-doped InSe nanometer piece preparation method, which comprises the steps of:
A) a certain amount of indium selenide and rare earth ion fluoride are weighed, is put into agate mortar and is fully ground；
B) powder after grinding is put into tube furnace, adjusts tubular type furnace temperature system and is passed through gas, carried out at solid-phase sintering
Reason；
C) sintered powder is put into agate mortar and is fully ground again, taken ground powder to be put into centrifuge tube, add
Enter NMP to be allowed to disperse；
D) NMP in step c) and mixture of powders are put into Ultrasound Instrument, adjust the parameters such as Ultrasound Instrument power and time, is surpassed
Sonication；
E) the NMP mixture after ultrasonic treatment is put into a centrifuge, adjusts the parameters such as centrifuge speed and time, is carried out
Centrifugal treating；
F) the upper layer clear brown solution after centrifugal treating is collected, rear-earth-doped InSe nanometer can be observed under Electronic Speculum
Piece.
2. near-infrared luminous rear-earth-doped InSe nanometer piece preparation method according to claim 1, it is characterised in that:
The molar percentage for the amount that rare earth ion fluoride is adulterated in the step a) are as follows: 0.1%~10%.
3. near-infrared luminous rear-earth-doped InSe nanometer piece preparation method according to claim 1, it is characterised in that:
Temperature schedule in the step b) are as follows: the heating rate of firing temperature is risen to from room temperature are as follows: 1 DEG C/min~50 DEG C/min；It fires
Temperature are as follows: 500 DEG C~1000 DEG C；Firing time are as follows: the h of 1 h~10.
4. near-infrared luminous rear-earth-doped InSe nanometer piece preparation method according to claim 1, it is characterised in that:
The quality of ground powder is weighed in the step c) are as follows: the mg of 1 mg~100；The volume of NMP is added are as follows: 1 ml~100
ml。
5. near-infrared luminous rear-earth-doped InSe nanometer piece preparation method according to claim 1, it is characterised in that:
The ultrasonic time in the step d) are as follows: the h of 1 h~48.
6. near-infrared luminous rear-earth-doped InSe nanometer piece preparation method according to claim 1, it is characterised in that:
The centrifugation rate of centrifuge in the step e) are as follows: the r/min of 1000 r/min~20000.
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Cited By (2)
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| CN110484253A (en) * | 2019-07-23 | 2019-11-22 | 中国计量大学 | A kind of preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric |
| CN113955724A (en) * | 2021-10-26 | 2022-01-21 | 深圳市第二人民医院(深圳市转化医学研究院) | Indium selenide nanosheet and preparation method of indium selenide nanosheet and gold nanoparticle composite structure |
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| CN110484253A (en) * | 2019-07-23 | 2019-11-22 | 中国计量大学 | A kind of preparation method of the rear-earth-doped metatitanic acid lanthanum nanometer sheet of up-conversion luminescence for optics thermometric |
| CN113955724A (en) * | 2021-10-26 | 2022-01-21 | 深圳市第二人民医院(深圳市转化医学研究院) | Indium selenide nanosheet and preparation method of indium selenide nanosheet and gold nanoparticle composite structure |
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