Synthesis of zn se nanocrystals (1)

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Synthesis Of ZnSe Nanocrystals, Study of its properties and applications. By : JITESH KUMAR(BE/15007/12) ATISH SINHA(BE/15009/12) GAURAV RAJ ANAND(BE/15067/12) Under the guidance of Prof. S.K CHAUBEY 1 [email protected]

Transcript of Synthesis of zn se nanocrystals (1)

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Synthesis Of ZnSe Nanocrystals, Study of its properties and applications.

By :JITESH KUMAR(BE/15007/12)ATISH SINHA(BE/15009/12)

GAURAV RAJ ANAND(BE/15067/12)Under the guidance of Prof. S.K CHAUBEY

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CONTENTS

• Abstract• Introduction• Objective• Methodology• Work Done• Results• Applications• References

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ABSTRACT

Highly crystalline, well-dispersed ZnSe nanocrystal with a relatively narrow particle size distribution was successfully synthesized by using solvo-thermal mechanism using ZnCl2, Se powder , hydrazine hydrate and ethylene glycol. The samples were characterized by means of X-ray diffraction (XRD), and Fourier transform infrared (FT-IR). All the desired properties of nanocrystals prepared here imply the possibility of high quality ZnSe nanocrystals developed under the appropriate reaction conditions. These properties were further applied in various applications like Cancer Detection and improving existing solar cells.

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Introduction

Nanocrystals• A nanocrystal is a crystalline particle with at least one

dimension measuring less than 1000 nanometers (nm), where 1 nm is defined as 1 thousand-millionth of a meter (10-9 m).

• The size of nanocrystals distinguishes them from larger crystals. For example, silicon nanocrystals can provide efficient light emission while bulk silicon does not and may be used for memory components.

• Semiconductor nanocrystals having dimensions smaller than 10nm are also described as quantum dots.

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Application of Nanocrystals:

• Illumination • Flat panel display • Refining of Crude Oil into Diesel • Optical and Infrared Lasers • Removal of pollutants and toxins • Solar panels • Drug Manufacture • Protein Analysis • Bio-tags for gene identification• Cancer Detection

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Zinc Selenide:• Zinc selenide (ZnSe) is a light-yellow, solid compound comprising zinc (Zn)

and selenium(Se).• It is an intrinsic semiconductor with a band gap of about 2.70 eV at 25 °C

(77 °F). • ZnSe rarely occurs in nature, and is found in the mineral that was named

after Hans Stille called "stilleite“.

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Properties of ZnSe:• ZnSe can be made in both hexagonal (wurtzite) and cubic (zincblende)

crystal structure.• It is a wide-bandgap semiconductor of the II-IV semiconductor

group (since zinc and selenium belong to the 12th and 16th groups of the periodic table, respectively).

• The material can be doped n-type doping with, for instance, halogen elements. P-type doping is more difficult, but can be achieved by introducing gallium .

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Applications of Zinc Selenide:• ZnSe is used to form II-VI light-emitting

diodes and diode lasers. It emits blue light.• ZnSe doped with magnesium (ZnSe:Mg) has been used

as an infrared laser gain medium emitting at about 2.4 µm.

• In daily life, it can be found as the entrance optic in the new range of "in-ear" clinical thermometers, seen as a small yellow window

• ZnSe activated with tellurium is a scintillator with emission peak at 640 nm, suitable for matching with photodiodes. It is used in x-ray and gamma ray detectors.

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OBJECTIVE

• Synthesis of Zinc Selenide Nanocrystals • Study of its optical and electrical properties • Preparation of Doped ZnSe • Application in Cancer Detection • Application in Photovoltaic Cells

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Methodology

• The methodology used in preparation of ZnSe nanocrystals by us is called solvo thermal synthesis method.

• In this case, we use water as a solvent, because of which it is called hydrothermal synthesis.

• Solvothermal synthesis is a method for preparing a variety of materials such as metals, semiconductors, ceramics, and polymers.

• The process can be used to prepare many geometries including thin films, bulk powders, single crystals, and nanocrystals.

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• The method can be used to prepare thermodynamically stable and metastable states including novel materials that cannot be easily formed from other synthetic routes.

• Over the last decade, a majority (~80%) of the literature concerning solvothermal synthesis has focused on nanocrystals.

• A magnetic stirrer was used for this process, which was set at different RPMs for a good number of hours for mixing and drying.

• A microwave was used for further drying.

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WORK DONE

Chemicals Required:• 1. Selenium Powder - 2gms • 2. Zinc Chloride - 4gms • 3. Ethylene Glycol - 54mL • 4. Hydrazine Hydrate – 18.5mL • 5. Distilled Water – 126mL • 6. Mg – 0.4gms

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• In the typical synthesis of ZnSe, highly pure ZnCl2 powder (99.9%) and elemental Selenium (99.999%) was used without further purification. Ethylene glycol and Hydrazine hydrate were also used.

• In this synthesis process, ZnCl2 (4.0 g) and elemental selenium (2.0 g) was taken with deionized water, ethylene glycol and hydrazine hydrate in the volume ratio of 7:3:1 respectively in a 200ml capacity conical flask.

• The solution is then put on a magnetic stirrer for a good number of hours at 60 degree celcius and then filtered out.

• The filtered sample is then dried in microwave for apprx. 10 mins at 120 degree celcius.

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EQUATIONS: 1. ZnCl2 + Se + X ZnSe X = C2H6O6 + N2H4 + H2O 2.ZnCl2 + Se + X + Mg ZnSe:Mg

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RESULTS• XRD• FTIR• SEM

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ZnSe IV

Operations: Smooth 0.150 | Background 1.000,1.000 | ImportFile: SAIFXR160217C-04 (ZnSe-IV).raw - Step: 0.020 ° - Step time: 29.1 s - WL1: 1.5406 - kA2 Ratio: 0.5 - Generator kV: 35 kV - Generator mA: 35 mA - Type: 2Th/Th locked

Lin

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nts)

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2-Theta - Scale

3 10 20 30 40 50 60 70 80

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ZnSe IV

Operations: Smooth 0.150 | Background 1.000,1.000 | Import8)

7)6)5)4)3)2)1)File: SAIFXR160217C-04 (ZnSe-IV).raw - Step: 0.020 ° - Step time: 29.1 s - WL1: 1. Obs. Max: 47.747 ° - FWHM: 0.439 ° - Raw Area: 5.503 Cps x deg.

Obs. Max: 43.699 ° - FWHM: 0.370 ° - Raw Area: 9.752 Cps x deg. Obs. Max: 32.924 ° - FWHM: 0.209 ° - Raw Area: 10.32 Cps x deg. Obs. Max: 31.768 ° - FWHM: 0.237 ° - Raw Area: 23.03 Cps x deg. Obs. Max: 29.726 ° - FWHM: 0.316 ° - Raw Area: 28.02 Cps x deg. Obs. Max: 23.535 ° - FWHM: 0.345 ° - Raw Area: 11.14 Cps x deg. Obs. Max: 22.370 ° - FWHM: 0.251 ° - Raw Area: 13.76 Cps x deg. Obs. Max: 15.169 ° - FWHM: 0.211 ° - Raw Area: 17.13 Cps x deg.

Lin

(Cou

nts)

01002003004005006007008009001000110012001300140015001600170018001900200021002200230024002500260027002800290030003100320033003400

2-Theta - Scale

3 10 20 30 40 50 60 70 80

2th=

15.1

74 °

,d=5

.834

06

2th=

20.4

89 °

,d=4

.331

20

2th=

22.3

57 °

,d=3

.973

402t

h=23

.523

°,d

=3.7

7899

2th=

24.6

17 °

,d=3

.613

49

2th=

29.7

31 °

,d=3

.002

492t

h=30

.488

°,d

=2.9

2969

2th=

31.7

67 °

,d=2

.814

562t

h=32

.933

°,d

=2.7

1756

2th=

34.9

42 °

,d=2

.565

75

2th=

40.6

60 °

,d=2

.217

152t

h=41

.574

°,d

=2.1

7051

2th=

43.6

95 °

,d=2

.069

91

2th=

45.3

59 °

,d=1

.997

812t

h=46

.437

°,d

=1.9

5389

2th=

47.7

62 °

,d=1

.902

74

2th=

49.3

32 °

,d=1

.845

79

2th=

51.2

62 °

,d=1

.780

72

2th=

55.9

41 °

,d=1

.642

37

2th=

58.4

89 °

,d=1

.576

752t

h=59

.911

°,d

=1.5

4268

2th=

61.3

44 °

,d=1

.510

03

2th=

63.4

19 °

,d=1

.465

52

2th=

67.1

13 °

,d=1

.393

56

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Ideal Curve (Comparision)

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RESULTS FROM XRD• The general plot shows very less Intensity peak

areas for most of 2θ , though with some fluctuations.

• The area under the Intensity count is almost constant for most of the region.

• Peak areas change due to imperfect structure.• Peak values are changed due to absorption of light

by the structure of material.• The fluctuation in the graph is due to the

impurities.• This shows overall good crystalline properties.

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RESULTS FROM FTIR• Transmittance is high for a wide range of wave no.• This means that the absorbance is quite low.• This shows presence of mostly very fine

nanoparticles.• The sharp bottoms represent the impurities.• This goes along with the properties expected of the

Zinc Selenide.• It can be used solar cells, lasers etc.

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Intended Applications

• Early detection of breast cancer using total biochemical analysis of peripheral blood components: a preliminary study.

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Cancer Detection• The aim of this study was to evaluate the feasibility of

detecting breast cancer by analyzing the total biochemical composition of plasma as well as peripheral blood mononuclear cells (PBMCs) using infrared spectroscopy.

• PBMCs and plasma were isolated and dried on a zinc selenide and measured under a Fourier transform infrared (FTIR) microscope to obtain their infrared absorption spectra. Differences in the spectra of PBMCs and plasma between the groups were analyzed as well as the specific influence of the relevant pathological characteristics of the cancer patients.

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• Several bands in the FTIR spectra of both blood components significantly distinguished patients with and without cancer.

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Conclusion In summary, ZnSe nanocrystals were successfully

synthesised by using solvo thermal route using Zinc Chloride, Ethylene Glycol, Hydrazine Hydrate ,which was further dried. Through this method, highly crystalline, well-dispersed ZnSe nanocrystal with an average diameter of 0.23 nm and a relatively narrow particle size distribution can be obtained. It is also expected that solvothermal method could be extended to synthesize the other semiconductor nanocrystals.

Further the results show its applicability in Cancer Detection and fabrication of Solar cells.

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REFERENCES1. Chung Sua, Yi-Ting Hsieha, Chi Paib and I-Wen Suna - “Voltammetric Study of Selenium and Two-Stage

Electrodeposition of Photoelectrochemically Active Zinc Selenide Semiconductor Films in Ionic Liquid Zinc Chloride-1-Ethyl-3-Methylimidazolium Chloride” - Journal of Electrochemical Society 2015 volume 162, issue 7

2. Sandeep Arya, Saleem Khan, Parveen Lehana , Ishan Gupta, Suresh K - “Electrical properties of electrodeposited zinc selenide (ZnSe) nanowires”- Journal of Materials Science: Materials in Electronics -September 2014, Volume 25, Issue 9, pp 4150-4155

3. Biljana Pejova -” Optical phonons in nanostructured thin films composed by zincblende zinc selenide quantum dots in strong size-quantization regime: Competition between phonon confinement and strain-related effects” - Journal of Solid State Chemistry Volume 213, May 2014, Pages 22–31

4. Aparna C. Deshpandea, Shashi B. Singha, Majid Kazemian Abyaneha, Renu Pasrichab, 5. S.K. Kulkarni - Low temperature synthesis of ZnSe nanoparticles – 20086. Lin Yang, Lingyun Liu, Dingquan Xiao, Jianguo Zhu - Preparation and characterization of ZnSe nanocrystals by a

microemulsion-mediated method – 20117. Kyle H. Montgomery, Jong-Hyeok Jeon, Qiang Zhang, Maria C. Tamargo, Jerry M. Woodall- ZnSe: A Material to Improve

Efficiencies for Current Solar Cell Multi-junction Stacks - Materials Research Society Spring Meeting, April 13 – 17, 20098. Junli Xu a, , Wei Wanga, Xia Zhang a, Xinjuan Chang a, Zhongning Shi b, Geir Martin Haarberg c - Electrodeposition of ⇑

ZnSe thin film and its photocatalytic properties - Journal of Alloys and Compounds , January 20159. Udi Zelig, Eyal Barlev, Omri Bar, Itai Gross, Felix Flomen, Shaul Mordechai, Joseph Kapelushnik, Ilana Nathan,Hanoch

Kashtan, Nir Wasserberg,# and Osnat Madhala-Givon# - Early detection of breast cancer using total biochemical analysis of peripheral blood components: a preliminary study – BMC Cancer- May 2015

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10. Shyam Ranjan Kumar,a Mohan Nuthalapatia and Joydeep Maity- Development of nanocrystalline ZnSe thin film through electrodeposition from a non aqeous solution, Scripta Materilia – May 2012

11. I.T. Zedan a, , A.A. Azabb, E.M. El-Menyawy b - Structural, morphological and optical ⁎properties of ZnSe quantum dot thin films, Spectrochimica Acta – October 2015

12. A.A. Khurram a, , Faisal Jabar b, M. Mumtaz b, Nawazish A. Khan c, M. Nasir ⇑Mehmood - Effect of light, medium and heavy ion irradiations on the structural and electrical properties of ZnSe thin films, Nuclear Instruments and Methods in Physics Research- August 2013

13. A.P. Pardo Gonzalez, H.G. Castro-Lora, L.D. López-Carreño, H.M. Martínez, N.J. Torres Salcedo - PhysicalpropertiesofZnSethin films depositedonglass and siliconsubstrates, Journal of Physics and Chemistry of Solids – January 2014

14. Steven C. Erwin, Lijun Zu, Michael I. Haftel, Alexander L. Efros, Thomas A. Kennedy & David J. Norris - Doping semiconductor nanocrystals, Nature – May 2005

15. Narayan Pradhan ,† David Goorskey ,‡ Jason Thessing ,† and Xiaogang Peng *† - An Alternative of CdSe Nanocrystal Emitters:  Pure and Tunable Impurity Emissions in ZnSe Nanocrystals, J. Am. Chem. Soc., 2005, 127 (50), pp 17586–17587

16. Shinjita Acharya†, D. D. Sarma§, Nikhil R. Jana† and Narayan Pradhan*†‡ - An Alternate Route to High-Quality ZnSe and Mn-Doped ZnSe Nanocrystals, J. Phys. Chem. Lett., 2010, 1 (2), pp 485–488

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Thank You