CN108163820A - A kind of method of low temperature preparation tin diselenide nano line - Google Patents

A kind of method of low temperature preparation tin diselenide nano line Download PDF

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Publication number
CN108163820A
CN108163820A CN201810195164.2A CN201810195164A CN108163820A CN 108163820 A CN108163820 A CN 108163820A CN 201810195164 A CN201810195164 A CN 201810195164A CN 108163820 A CN108163820 A CN 108163820A
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reaction
tin diselenide
diselenide nano
nano line
low temperature
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CN108163820B (en
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张虎林
袁仲云
禚凯
曹胜利
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Taiyuan University of Technology
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Taiyuan University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention discloses a kind of methods of low temperature preparation tin diselenide nano line, belong to technical field of inorganic compound semiconductor nano material；It only need to be under 100 120 DEG C of lower temperature using cheap simple raw material using solvent structure tin diselenide nano wire material：Inorganic salts, ethyl alcohol, hydrazine hydrate, ammonium hydroxide carry out one-step synthesis；Easy to operate, controllable parameter is less in building-up process, and synthesis cost is low；Obtained tin diselenide nano wire material freely disperses development growth in the solution, has one-dimensional present situation pattern, and well-crystallized；In the synthesis process without introducing surfactant or template, process is pollution-free, and nanowire surface is clean, is suitble to carry out it Study on Physical, while also easily carry out surface modification.

Description

A kind of method of low temperature preparation tin diselenide nano line
Technical field
The invention belongs to technical field of inorganic compound semiconductor nano material, and in particular to a kind of to prepare two selenizing sijnas The method of rice noodles more particularly to a kind of method that tin diselenide nano line is prepared using low-temperature solvent heat method.
Background technology
Semiconductor photosensor is widely used in contemporary electronic systems, be in modern Intelligent Sensing System can not or Scarce basic device.For two stannic selenides as a kind of important group IV-VI semiconductor material, indirect band gap is 1 eV or so, Direct band gap is about 1.5 eV, can absorb the overwhelming majority of solar spectrum, therefore is a kind of typical excellent visible ray light Sensor material, be widely used in infrared electro instrument and remember switching switch, hologram solid-phase media etc..So far, two selenium Change the method that the synthesis of tin monocrystal nano-material mainly uses high temperature and pressure, building-up process is complicated, can generate in the synthesis process Toxic pollutant.It is seldom reported for the preparation of tin diselenide nano line, synthesizes tin diselenide nano line under cryogenic Report be even more do not have.Therefore, study and explore a kind of novel easy to operate, of low cost, easy to spread be effectively synthesized The method of tin diselenide nano line is very necessary.
Invention content
Overcome the deficiencies in the prior art of the present invention, it is therefore an objective to which solvent-thermal method need to be passed through at a lower temperature by providing a kind of The method for synthesizing tin diselenide nano wire material.
To achieve the above object, the technical solution adopted in the present invention is：A kind of low temperature preparation tin diselenide nano line Method includes the following steps.
a）The liquid ethanol that weight percent is 40-60% and liquid hydrazine hydrate that weight percent is 40-60% is uniform It is mixed to get reaction dissolvent.
b）The soluble selenous acid metal salt that butter of tin and weight ratio that weight ratio is 40-60% are 40-60% is mixed Obtain reaction raw materials.
c）Weigh reaction raw materials that weight percent is 0.5-10% and the reaction dissolvent of 90-99.5%, reaction raw materials and anti- It is 100% to answer solvent total weight percent, is placed in reaction vessel, adds in closed, the heated at constant temperature at 100-120 DEG C after ammonium hydroxide 20-40h；The pH of the ammonium hydroxide is 8-10.
d）After being cooled to room temperature washing until reaction product pH value for neutrality, obtain tin diselenide nano line.
Preferably, the selenous acid metal salt is sodium selenite or potassium selenite.
Preferably, the reaction vessel prepares container or precious metal vessel for organic polymer.
Preferably, the heated at constant temperature 20-40h at 100-120 DEG C, is that reaction vessel is placed in Muffle furnace or electricity It is carried out in resistance stove or baking oven.
Compared with prior art the invention has the advantages that：The present invention uses two selenizing sijna of solvent structure The cheap simple raw material that nanowire material need to only use under 100-120 DEG C of lower temperature：Inorganic salts, ethyl alcohol, hydrazine hydrate, ammonia Water carries out one-step synthesis, i.e. raw material and reaction dissolvent once adds in the interior heating reaction of merging constant temperature oven after reactor, operation sequence Simply, controllable parameter is less in building-up process, and synthesis cost is low.Obtained tin diselenide nano wire material is free in the solution Disperse development growth, there is one-dimensional present situation pattern, and well-crystallized.In the synthesis process without introducing surfactant or mould Plate agent, process is pollution-free, and nanowire surface is clean, is suitble to carry out it Study on Physical, while also easily carries out surface and change Property.
Description of the drawings
Fig. 1 is the x-ray diffraction pattern of tin diselenide nano wire material prepared by the method for the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of tin diselenide nano wire material prepared by the method for the present invention.
Fig. 3 is the transmission electron microscope picture of tin diselenide nano wire material prepared by the method for the present invention.
Fig. 4 is the high-resolution-ration transmission electric-lens figure of tin diselenide nano wire material prepared by the method for the present invention.
Specific embodiment
With reference to the embodiment technical solution that the present invention will be described in detail, but protection domain is not limited by this.
Embodiment 1
The specific synthetic method of tin diselenide nano wire material：The raw material for synthesizing tin diselenide nano wire material is ethyl alcohol, hydration Hydrazine, butter of tin, sodium selenite, ammonium hydroxide, the reaction of generation are as follows：
Concrete operation step is as follows：
Step 1, by weight percentage ethyl alcohol are 40% and hydrazine hydrate is that 60% weighing mixing is used as reaction dissolvent.
Step 2, by butter of tin weight percent be 40%, the weight percent of sodium selenite is 60% weighing as reaction Object.
Step 3 prepares ammonia spirit, by the way that ammonium hydroxide is dissolved in suitable quantity of water, makes final pH value in 8-10.
Step 4, heating reaction, using add in reaction vessel reaction raw materials and reaction dissolvent as total weight, with taking weight hundred Divide the reaction dissolvent for being 99.5% than the reaction raw materials for 0.5% and weight ratio, be placed in has reaction solution with inert together In reaction vessel prepared by machine polymer, while the ammonia spirit that step 3 prepares is added in, covered and enclosed, then by reaction vessel It is put into 100 DEG C of Muffle furnace, and heated at constant temperature 20 hours at such a temperature.
Step 5 is taken out reaction vessel, cooled to room temperature from Muffle furnace.
Reaction product is spent cold or thermion water and first disperses by step 6, then with centrifuge in rotating speed is 5000 ~ 30000 Rev/min speed under centrifuge or be filtered with pumping and filtering device, then will centrifuge or the product of filtering again in deionized water Dispersion, then repeat be dehydrated and cleaning 4 ~ 5 times, until reaction product pH value for neutrality to get tin diselenide nano wire material.
Embodiment 2
Synthesize tin diselenide nano wire material raw material for ethyl alcohol, hydrazine hydrate, butter of tin, potassium selenite, ammonium hydroxide, generation it is anti- It should be as follows：
Concrete operation step is as follows：
Step 1, by weight percentage ethyl alcohol are 60% and hydrazine hydrate is that 40% weighing mixing is used as reaction dissolvent.
Step 2, by butter of tin weight percent be 60%, the weight percent of potassium selenite is 40% weighing as reaction Object.
Step 3 prepares ammonia spirit, by the way that ammonium hydroxide is dissolved in suitable quantity of water, makes final pH value in 8-10.
Step 4, heating reaction, using add in reaction vessel reaction raw materials and reaction dissolvent as total weight, with taking weight hundred Divide the reaction dissolvent for being 90% than the reaction raw materials for 10% and weight ratio, be placed in has inert noble metal together to reaction solution In the reaction vessel of preparation, while the ammonia spirit that step 3 prepares is added in, then reaction vessel is put into 120 DEG C by covered and enclosed Resistance furnace in, and heated at constant temperature 30 hours at such a temperature.
Step 5 is taken out reaction vessel, cooled to room temperature from resistance furnace.
Reaction product is spent cold or thermion water and first disperses by step 6, then with centrifuge in rotating speed is 5000 ~ 30000 Rev/min speed under centrifuge or be filtered with pumping and filtering device, then will centrifuge or the product of filtering again in deionized water Dispersion, then repeat be dehydrated and cleaning 4 ~ 5 times, until reaction product pH value for neutrality to get tin diselenide nano wire material.
Embodiment 3
Synthesize tin diselenide nano wire material raw material for ethyl alcohol, hydrazine hydrate, butter of tin, potassium selenite, ammonium hydroxide, generation it is anti- It should be as follows：
Concrete operation step is as follows：
Step 1, by weight percentage ethyl alcohol are 50% and hydrazine hydrate is that 50% weighing mixing is used as reaction dissolvent.
Step 2, by butter of tin weight percent be 50%, the weight percent of potassium selenite is 50% weighing as reaction Object.
Step 3 prepares ammonia spirit, by the way that ammonium hydroxide is dissolved in suitable quantity of water, makes final pH value in 8-10.
Step 4, heating reaction, using add in reaction vessel reaction raw materials and reaction dissolvent as total weight, with taking weight hundred Divide the reaction dissolvent for being 95% than the reaction raw materials for 5% and weight ratio, be placed in has inert noble metal together to reaction solution In the reaction vessel of preparation, while the ammonia spirit that step 3 prepares is added in, then reaction vessel is put into 110 DEG C by covered and enclosed Baking oven in, and heated at constant temperature 40 hours at such a temperature.
Step 5 is taken out reaction vessel, cooled to room temperature from baking oven.
Reaction product is spent cold or thermion water and first disperses by step 6, then with centrifuge in rotating speed is 5000 ~ 30000 Rev/min speed under centrifuge or be filtered with pumping and filtering device, then will centrifuge or the product of filtering again in deionized water Dispersion, then repeat be dehydrated and cleaning 4 ~ 5 times, until reaction product pH value for neutrality to get tin diselenide nano wire material.
By 1 reaction product X-ray diffraction of embodiment（XRD）It identifies crystalline phase, it is characterized with scanning electron microscope or transmission electron microscope Pattern and size.As Fig. 1 provides X-ray diffraction（XRD）As a result, it shows to prepare two stannic selenides that product is hexagonal phase structure； The two stannic selenide crystal as made from the scanning electron microscope (SEM) photograph, Fig. 3,4 transmission electron microscope observings provided that Fig. 2 is provided show experiment are straight 50-100 nanometers of diameter, the linear structure that length is 20-40 microns.
The above content is combine specific preferred embodiment to the further description of the invention done, it is impossible to assert The specific embodiment of the present invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off Under the premise of from the present invention, several simple deduction or replace can also be made, should all be considered as belonging to the present invention by being submitted Claims determine scope of patent protection.

Claims (4)

  1. A kind of 1. method of low temperature preparation tin diselenide nano line, which is characterized in that include the following steps：
    a）The liquid ethanol that weight percent is 40-60% is uniformly mixed with the liquid hydrazine hydrate that weight percent is 40-60% Obtain reaction dissolvent；
    b）The soluble selenous acid metal salt that butter of tin and weight ratio that weight ratio is 40-60% are 40-60% is mixed to get Reaction raw materials；
    c）Weight percent is weighed as the reaction raw materials of 0.5-10% and the reaction dissolvent of 90-99.5%, reaction raw materials and reaction are molten Agent total weight percent is 100%, is placed in reaction vessel, adds in closed, the heated at constant temperature 20- at 100-120 DEG C after ammonium hydroxide 40h, the pH of the ammonium hydroxide is 8-10；
    d）After being cooled to room temperature washing until reaction product pH value for neutrality, obtain tin diselenide nano line.
  2. A kind of 2. method of low temperature preparation tin diselenide nano line according to claim 1, which is characterized in that the Asia Selenic acid metal salt is sodium selenite or potassium selenite.
  3. 3. the method for a kind of low temperature preparation tin diselenide nano line according to claim 1, which is characterized in that described is anti- Container is answered to prepare container or precious metal vessel for organic polymer.
  4. 4. a kind of method of low temperature preparation tin diselenide nano line according to claim 1, which is characterized in that it is described Heated at constant temperature 20-40h at 100-120 DEG C is that reaction vessel is placed in Muffle furnace or resistance furnace or baking oven to carry out.
CN201810195164.2A 2018-03-09 2018-03-09 Method for preparing tin diselenide nanowire at low temperature Active CN108163820B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240126A (en) * 2019-06-14 2019-09-17 西安交通大学 A kind of two stannic selenides of nanometer flower structure and preparation method thereof
CN113788461A (en) * 2021-09-17 2021-12-14 中国海洋大学 Application of biomineralization micro-reactor regulation solid-state synthesis nano material and potassium storage device thereof

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CN1554574A (en) * 2003-12-21 2004-12-15 浙江大学 Bi2Te3 base compound nano line and its preparing method
CN103060889A (en) * 2011-10-19 2013-04-24 中国科学院大连化学物理研究所 Solution phase method for synthesizing tin selenide monocrystal nanowire
CN104831362A (en) * 2015-06-08 2015-08-12 广东工业大学 Method for preparing tin selenide single-crystal nano-belt
CN106784678A (en) * 2016-12-19 2017-05-31 陕西科技大学 A kind of solvent-thermal method prepares flower-shaped SnSe2The method of graphene oxide compound

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1554574A (en) * 2003-12-21 2004-12-15 浙江大学 Bi2Te3 base compound nano line and its preparing method
CN103060889A (en) * 2011-10-19 2013-04-24 中国科学院大连化学物理研究所 Solution phase method for synthesizing tin selenide monocrystal nanowire
CN104831362A (en) * 2015-06-08 2015-08-12 广东工业大学 Method for preparing tin selenide single-crystal nano-belt
CN106784678A (en) * 2016-12-19 2017-05-31 陕西科技大学 A kind of solvent-thermal method prepares flower-shaped SnSe2The method of graphene oxide compound

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240126A (en) * 2019-06-14 2019-09-17 西安交通大学 A kind of two stannic selenides of nanometer flower structure and preparation method thereof
CN110240126B (en) * 2019-06-14 2021-01-19 西安交通大学 Tin diselenide with nanoflower structure and preparation method thereof
CN113788461A (en) * 2021-09-17 2021-12-14 中国海洋大学 Application of biomineralization micro-reactor regulation solid-state synthesis nano material and potassium storage device thereof
CN113788461B (en) * 2021-09-17 2023-03-10 中国海洋大学 Application of biomineralization micro-reactor regulation and control solid-state synthesis nano material and potassium storage device thereof

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