CN105923653A - Preparation method for nano Cu3SbS4 ternary semiconductor material - Google Patents

Preparation method for nano Cu3SbS4 ternary semiconductor material Download PDF

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CN105923653A
CN105923653A CN201610454705.XA CN201610454705A CN105923653A CN 105923653 A CN105923653 A CN 105923653A CN 201610454705 A CN201610454705 A CN 201610454705A CN 105923653 A CN105923653 A CN 105923653A
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sbs
preparation
semiconductor material
ball milling
powder
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谭国龙
盛号号
徐期树
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Wuhan University of Technology WUT
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G30/00—Compounds of antimony
    • C01G30/002—Compounds containing, besides antimony, two or more other elements, with the exception of oxygen or hydrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
    • 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
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a preparation method for a nano Cu3SbS4 ternary semiconductor material. The preparation method comprises the following steps: taking a mixture of high-purity Cu, Sb and S powder as a raw material and sealing the raw material into a ball milling pot; after sealing the ball milling pot, putting the ball milling pot into a glove box; fully filling wtih inert gas to remove oxygen gas in the raw material; mounting the ball milling pot on a ball mill and carrying out ball milling; adjusting the running speed of a motor of the ball mill to be higher than 1200r/min; milling powder for 5h to generate the nano Cu3SbS4 ternary semiconductor material. A prepared nano Cu3SbS4 crystal has uniform components and a single structure; covering matters including impurities and the like do not exist on the surface and the intrinsic physical performances of the material are displayed very well. The material has very good photoelectric properties so that the material can become a practical photoelectric device material and can be used in fields including infrared detection, infrared remote sensing, night vision devices and the like. Furthermore, the preparation method has the advantages that the preparation process is simple, the raw materials are easy to obtain and low in price and belong to an environment-friendly type and large-batch production can be realized and the like.

Description

Nanometer Cu3SbS4The preparation method of ternary semiconductor material
Technical field
The invention belongs to the preparation field of semi-conducting material, involved content is a kind of nano semiconductor material Cu3SbS4System Preparation Method.
Background technology
Owing to nano semiconductor material has exclusive characteristic, have at aspects such as thin film thermoelectric technology, transistor, light absorber devices Potential huge application, but the elements such as traditional semi-conducting material Ga, As, Se are expensive or poisonous etc., and factor is subject to The biggest restriction, is eager to find new material to replace these traditional materials.And ternary compound Cu-Sb-S due to cheap, Abundant raw material is easy to get and is easily formed the advantages such as the element extensively in-depth study by people.
Owing to tri-kinds of elements of Cu-Sb-S reserves on earth are the abundantest, they can also be as synthesis of ternary quasiconductor simultaneously Material, and by universal concern, and synthesized band gap is near infrared region, and along with Cu-Sb-S nanocrystal sets Point, the change of pattern and change, in terms of light absorbent, have huge potential application.At present, most researcher uses Be that wet chemical methods is to prepare Cu3SbS4Nano-particle, but adopt and surface can be made in this way to cover other material, make The Cu of its synthesis3SbS4There is more impurity, the performance tool of made product is had a certain impact；Or a lot of researcheres is adopted By methods such as injection, electrodeposition processes, but these methods all seem more complicated, and operation, equipment and reaction condition thereof are desirable that relatively Height, all inevitably causes pollution to sample simultaneously.Consequently found that the physical method of a kind of replacement prepare surface clean and And the single ternary semiconductor material Cu-Sb-S of chemical composition is nanocrystalline is particularly important, so it is possible not only to avoid product table Face is contaminated, and can reduce the Cost Problems in building-up process simultaneously, and mechanical alloying to be exactly such a can be mass table Face is cleaned and forms single semiconductor nanocrystal, for being compared to chemical method, has a kind of thing of above-mentioned advantage simultaneously Reason method.
Summary of the invention
Present invention aim at providing one to prepare ternary semiconductor material four sulfur antimony three bronze medal (Cu3SbS4) nanocrystalline new method, close The semiconductor nano chemical constituent become not only uniformly, structure single, and surface does not has the coverings such as impurity, well shows The intrinsic physical property of material.
For reaching above-mentioned purpose, use technical scheme as follows:
Nanometer Cu3SbS4The preparation method of ternary semiconductor material, comprises the following steps:
1) as raw material, the mixture of high-purity Cu, Sb with S powder being sealed in ball grinder, ball grinder is placed in hands after sealing In casing, it is full of noble gas and removes the oxygen in raw material；
2) ball grinder being arranged on ball milling on ball milling grinding machine, the exploitation speed adjusting ball mill motor is more than 1200r/min, powder Nanometer Cu after the 5h of end3SbS4Ternary semiconductor material generates.
By such scheme, after powder 40h, obtain nanometer Cu3SbS4Ternary semiconductor material.
By such scheme, the particle size range of described powder is 1.5nm～6.5nm.
By such scheme, Cu, Sb are above 99.9wt% with the purity of S powder.
By such scheme, Cu, Sb are (3 ± 0.1) with the mol ratio of S powder: (1 ± 0.1): (4 ± 0.1).
By such scheme, a diameter of 2-12 millimeter of ball milling in ball grinder, ball powder mass ratio is set as 2:1～30:1.
Generally, when using chemical method to prepare this kind of material, it is desirable to the external world provides hot environment, the present invention for a long time Thering is provided hot environment without by the external world when using mechanical alloying method synthesis, its main cause is employed in preparation process Initial feed be Cu, Sb and S simple substance powder body, chemical property live ripple, they reaction activation energy ratio relatively low, be susceptible to Combination reaction；It addition, from the XRD figure spectrum of different Ball-milling Times, at the starting stage of reaction, substantial amounts of Cu and S powder There occurs combination reaction, and released substantial amounts of reaction heat, these reaction heat can promote that Sb powder participates in chemical reaction, from And generate nano semiconductor material.Owing to collision can make the temperature in ball grinder raise, in the short period of time, Cu, Sb and S Powder generation alloying reaction, and release substantial amounts of reaction heat, these heats can keep hot environment in making ball grinder so that Reaction can complete in the regular hour.
The beneficial effects of the present invention is:
Four obtained sulfur antimony three copper nanocrystallite chemical compositions are uniform, structure is single, and surface does not has the coverings such as impurity, well Show the intrinsic physical property of material.
Due to the photoelectric properties that it is good so that it is a kind of material for optoelectronic devices that can be practical can be become, as can be used for infrared acquisition, The field such as infrared remote sensing, night vision device.
Additionally, the present invention has that preparation technology is simple, raw material is easy to get and low price, belongs to environmentally friendly type, and can realize The advantages such as production in enormous quantities.
Accompanying drawing explanation
Fig. 1: Cu prepared by ball milling 0h, 1h3SbS4Nanocrystalline XRD figure spectrum；
Fig. 2: Cu prepared by ball milling 5h, 10h, 20h and 40h3SbS4Nanocrystalline XRD figure spectrum；
Fig. 3: Cu prepared by ball milling 40h3SbS4Nanocrystalline TEM collection of illustrative plates；
Fig. 4: Cu prepared by ball milling 40h3SbS4Nanocrystalline HRTEM collection of illustrative plates；
Fig. 5: Cu prepared by ball milling 40h3SbS4Nanocrystalline grain size distribution；
Fig. 6: Cu prepared by ball milling 40h3SbS4Nanocrystalline infrared absorption spectroscopy.
Detailed description of the invention
Weigh element Cu, Sb and S powder body each 6.4893g, 4.1447g and 4.3661g respectively, keep the error weighed at ± 0.0002g In the range of, load weighted sample it is placed in the ball grinder of different-diameter sizes of balls mill and seals, being placed in glove box and open wide 60 Minute to remove air, take out after sealing, be loaded on ball mill (SPEX 8000) and carry out ball milling, respectively ball milling 1 hour, 5 hours, 10 hours, 20 hours, 40 hours, the sample for different Ball-milling Times to be sampled in glove box, with Avoid oxidation.
Respectively the sample of different time sections being carried out XRD test, its XRD figure is composed as shown in Figure 1 and Figure 2.
Fig. 1, Fig. 2 are the Cu that mechanical alloying is prepared3SbS4The XRD figure spectrum of nanocrystalline powder.This figure demonstrates whole In mechanical milling process, element powder body is through the structural evolution of chemical machinery alloying, and Fig. 1 b shows the ball milling sample of 1 hour, now with Fig. 1 a compares, and the diffraction maximum of element powders Cu substantially disappears, but does not has peak to show to have synthesized Cu3SbS4Nanocrystalline, this display Cu may be added in bigger lattice, and is not detected.After ball milling 5 hours, the diffraction maximum of single-element powder body Intensity continues to reduce, and Ball-milling Time is the most long, and the diffraction peak intensity of element powders is the lowest more low, simultaneously Cu3SbS4Feature diffraction { 110}, { 112}, { 204}, { 312}, { 224} can detect in XRD diffracting spectrum, shows Cu at peak3SbS4Sample Synthesize.After ball milling 10 hours, the diffraction maximum of element powder body is wholly absent, and the product of generation is entirely pure Cu3SbS4 Crystal, only sample { 112}, { 204}, { the crystal face intensity enhancing at 312}, and { 211}, { the crystal face intensity at 224} has subtracted Weak, this shows that there are certain relation the size of particle and the time of ball milling.Meanwhile, within the time of 10 hours to 40 hours, Do not have new diffraction maximum to produce, show to generate stable Cu3SbS4Nanocrystalline, and do not have impurity to produce.
Fig. 3 is the ball milling Cu of 40 hours3SbS4The nanocrystalline TEM collection of illustrative plates being diffused in TOP/TOPO and pyridine solution thereof. It will be seen that most nanoparticle is to be evenly dispersed in organic solvent from figure, there is no the phenomenon of polymerization.This be by Generate netted polymer in TOP and TOPO reaction, and be dispersed in whole pyridine solution so that Cu3SbS4Receive Meter Jing, is relatively easy to distinguish single nanoparticle above than more uniform absorption.Therefore, do not see in the collection of illustrative plates of TEM To substantial amounts of Cu3SbS4Nanocrystalline particle aggregation phenomenon together.
Fig. 4 is the Cu of ball milling preparation in 40 hours3SbS4Nanocrystalline HRTEM collection of illustrative plates.Fig. 4 (a) is ball milling 40 hours Cu3SbS4The HRTEM collection of illustrative plates of nanocrystal, it can be clearly seen that lattice fringe from figure, this shows to use mechanical alloying Cu synthesized by method3SbS4Nanocrystal has good crystallinity, and this is consistent with the result measured by XRD figure spectrum.Meanwhile, In HRTEM, both it can be seen that the Cu of zincblende lattce structure3SbS4Nanocrystalline, again it can be seen that the Cu of wurtzite structure3SbS4 Nanocrystalline, show the Cu having two kinds of structures3SbS4Nanocrystalline coexist.In Fig. 4 (a), the interplanar distance of part A is, this Consistent with the PDF (35-0581) in XRD software, corresponding lattice paprmeter is (211), and this has very with the result measured by xrd Good concordance.Fig. 4 (b) shows four little Cu3SbS4Nano-particle, its magnitude range is 1.5nm to 6.5nm, from figure In it can be seen that show lattice fringe be one-dimentional structure, it is more difficult to from these images, identify Cu3SbS4The knot of nanocrystal Structure and orientation.
Fig. 5 is ball milling Cu after 40 hours3SbS4Nanocrystalline grain size distribution, is fitted it with Gaussian function, it is seen that Its coincidence statistics rule.It can be seen that Cu3SbS4Nanocrystalline particle size distribution range is in 1.5nm～6.5nm, Gauss Distributed model concentrates on 3.4nm, it is believed that Cu3SbS4Nanocrystalline average-size is exactly this numerical value.
Fig. 6 is 40 hours Cu of preparation3SbS4Nanocrystal mid-infrared and far collection of illustrative plates, it is clear that Cu3SbS4Be directly between A kind of optical type of gap semiconductor.For Cu3SbS4Spectrum, at wavelength the absorbance of band-gap energy have one notable under Sliding and a slip, this is the typical characteristic of indirect gap semiconductor optical spectra.Its energy gap can be by using in ultrared (aE)1/2Straight line than E determines, indirect band gap energy is by (aE) at linear extrapolation slip1/2Edge determines to zero absorption. Fig. 5 shows that absorbance is the least, because these photons are not enough to excite the electronics in valence band to jump when photon energy is less than band-gap energy Adjourn to conduction band.When photon energy is more than band-gap energy, then absorbance the most slowly growth can show unexpected increase, slowly increases Absorbance be derived from indirect band gap, absorbance increases sharply suddenly, is derived from the transition of direct band gap.Meanwhile, from infrared spectrum It can be seen that for Cu3SbS4After ball milling 40 hours, can significantly see two peaks, respectively at 28807nm and At 40510nm, this is the diffraction maximum that the first exciton and the second exciton are the most corresponding, thus corresponding to the first exciton and the second exciton Energy be respectively 0.042eV and 0.031eV, after Producing reason is one photon of Electron absorption, transit to corresponding track Up, unnecessary energy discharges with the form of exciton, and this is the character of typical semiconductor material.It should be noted that machinery The Cu that alloyage prepares3SbS4Energy gap is 0.046eV, and this shows that its energy gap is the lowest, to the absorption region of light very Extensively, even to far infrared region from UV, visible light to mid-infrared, this militarily has huge application prospect.

Claims (6)

1. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that comprise the following steps:
1) as raw material, the mixture of high-purity Cu, Sb with S powder being sealed in ball grinder, ball grinder is placed in hands after sealing In casing, it is full of noble gas and removes the oxygen in raw material；
2) ball grinder being arranged on ball milling on ball milling grinding machine, the exploitation speed adjusting ball mill motor is more than 1200r/min, powder Nanometer Cu after the 5h of end3SbS4Ternary semiconductor material generates.
2. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that obtain nanometer Cu after powder 40h3SbS4 Ternary semiconductor material.
3. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that the particle size range of described powder is 1.5nm～6.5nm.
4. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that Cu, Sb are the highest with the purity of S powder In 99.9wt%.
5. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that Cu, Sb with the mol ratio of S powder are (3±0.1):(1±0.1):(4±0.1)。
6. nanometer Cu3SbS4The preparation method of ternary semiconductor material, it is characterised in that a diameter of 2-12 of ball milling in ball grinder Millimeter, ball powder mass ratio is set as 2:1～30:1.
CN201610454705.XA 2016-06-21 2016-06-21 Preparation method for nano Cu3SbS4 ternary semiconductor material Pending CN105923653A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107119321A (en) * 2017-04-14 2017-09-01 武汉理工大学 Ternary semiconductor PbSnS3It is nanocrystalline and preparation method thereof
CN107240637A (en) * 2017-05-04 2017-10-10 河南理工大学 Cubic phase Cu3SbS3Base thermoelectric material and preparation method thereof
CN107746076A (en) * 2017-10-20 2018-03-02 上海应用技术大学 A kind of method for preparing the copper nanocrystallite material of four antimony trisulfide three
CN109012903A (en) * 2018-07-20 2018-12-18 中国科学院长春光学精密机械与物理研究所 A kind of preparation method of interface disorder nano material
AT523321A1 (en) * 2019-12-30 2021-07-15 Rimmer Dipl Ing Dr Karl METHOD AND DEVICE FOR MANUFACTURING ANTIMONTRISULFIDE
CN115108732A (en) * 2022-06-22 2022-09-27 常州大学 Cu 3 SbS 4 Film and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08175016A (en) * 1994-12-21 1996-07-09 Ricoh Co Ltd Phase change type optical recording medium
CN104477991A (en) * 2014-11-25 2015-04-01 北京科技大学 Preparation method of low-thermal-conductivity CuSbS<2+x> thermoelectric material
CN105565379A (en) * 2015-12-07 2016-05-11 武汉理工大学 Controllable preparation method of Cu3SbS4 nanocrystalline material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08175016A (en) * 1994-12-21 1996-07-09 Ricoh Co Ltd Phase change type optical recording medium
CN104477991A (en) * 2014-11-25 2015-04-01 北京科技大学 Preparation method of low-thermal-conductivity CuSbS<2+x> thermoelectric material
CN105565379A (en) * 2015-12-07 2016-05-11 武汉理工大学 Controllable preparation method of Cu3SbS4 nanocrystalline material

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107119321A (en) * 2017-04-14 2017-09-01 武汉理工大学 Ternary semiconductor PbSnS3It is nanocrystalline and preparation method thereof
CN107240637A (en) * 2017-05-04 2017-10-10 河南理工大学 Cubic phase Cu3SbS3Base thermoelectric material and preparation method thereof
CN107240637B (en) * 2017-05-04 2019-07-09 河南理工大学 Cubic phase Cu3SbS3Base thermoelectric material and preparation method thereof
CN107746076A (en) * 2017-10-20 2018-03-02 上海应用技术大学 A kind of method for preparing the copper nanocrystallite material of four antimony trisulfide three
CN107746076B (en) * 2017-10-20 2019-11-29 上海应用技术大学 A method of preparing four antimony trisulfides, three copper nanocrystallite material
CN109012903A (en) * 2018-07-20 2018-12-18 中国科学院长春光学精密机械与物理研究所 A kind of preparation method of interface disorder nano material
CN109012903B (en) * 2018-07-20 2020-05-12 中国科学院长春光学精密机械与物理研究所 Preparation method of surface disordered nano material
AT523321A1 (en) * 2019-12-30 2021-07-15 Rimmer Dipl Ing Dr Karl METHOD AND DEVICE FOR MANUFACTURING ANTIMONTRISULFIDE
AT523321B1 (en) * 2019-12-30 2021-09-15 Rimmer Dipl Ing Dr Karl METHOD AND DEVICE FOR THE MANUFACTURING OF ANTIMONY TRISULFIDE
CN115108732A (en) * 2022-06-22 2022-09-27 常州大学 Cu 3 SbS 4 Film and preparation method thereof
CN115108732B (en) * 2022-06-22 2023-08-22 常州大学 Cu 3 SbS 4 Film and method for producing the same

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Application publication date: 20160907