Electrical conductivity of CuI-Cu2Se-As2Se3 chalcogenide films prepared by chemical deposition

2009 ◽  
Vol 35 (6) ◽  
pp. 592-595 ◽  
Author(s):  
D. L. Baidakov ◽  
E. V. Shkol’nikov
Author(s):  
Д.Л. Байдаков ◽  
Ю.Т. Виграненко

Методом химического нанесения из растворов халькогенидных стекол в н-бутиламине получены халькогенидные пленки PbS-AgI-As2S3, PbS-Ag2S-As2S3 и PbI2-Ag2S-As2S3, изучена электропроводность и электродные свойства стекол и пленок аналогичного состава. Синтез стекол проводили согласно методике, описанной в [Легин, 1985]. Пленки наносили по следующей методике. Навеску стекла помещали в кипящий н-бутиламин, затем перемешивали в течение 3–4 ч до полного растворения стекла в амине. Для предотвращения окисления кислородом воздуха пленки наносили в закрытом боксе в атмосфере азота. Подложку помещали на устройство для вращения, наносили на нее раствор, а затем вращали подложку со скоростью 3000–4000 об/мин в течение 1 мин. Отжиг пленок проводили в боксе при температуре 90–100 С в течение 30–60 мин. Исследована электропроводность халькогенидных пленок PbS-AgI-As2S3, PbS-Ag2S-As2S3 и PbI2-Ag2S-As2S3. Величина электропроводности составляет 10–14–10–4 Ом.см–1. Установлено, что значения электропроводности стекол и пленок аналогичного состава практически не отличаются. Электроды с пленочными мембранами PbS- Ag2S-As2S3 и PbI2-Ag2S-As2S3 показали высокую чувствительность к катионам Pb2+. Нернстовская область электродного отклика лежит в пределах 10–2–10–6 моль/л нитрата свинца, предел обнаружения достигает 10–7 моль/л. Тонкопленочные электроды с мембранами PbS-AgI-As2S3 продемонстрировали достаточно высокую чувствительность к катионам Ag+. Нернстовская область электродного отклика составляет 10–1–10–6 моль/л AgNO3, предел обнаружения катионов серебра достигает 10–7 моль/л. Электродные свойства халькогенидных стекол и пленок аналогичного состава практически не отличаются. Chalcogenide films PbS-AgI-As2S3, PbS-Ag2S-As2S3 and PbI2-Ag2S-As2S3, were synthesized from the solutions of chalcogenide glasses in n-butylamine. The electrical conductivity and electrode properties of glasses and films of the same compositions were studied. The synthesis of glasses was carried out according to the procedure described in [Legin, 1985]. The films were prepared as follows. The sample of the glass was placed in boiling n-butylamine, then stirred for 3–4 hours until the glass was completely dissolved in the amine. To prevent oxidation by air oxygen, the films were applied in a closed box under a nitrogen atmosphere. The substrate was placed on a rotating device, a solution was applied thereto, and then the substrate was rotated at a speed of 3000–4000 rpm for 1 minute. Annealing of the films was carried out in the box at a temperature of 90–100 C for 30–60 min. Electrodes with membranes PbS-Ag2S-As2S3 and PbI2-Ag2S-As2S3 showed high sensitivity to cations Pb2+. The Nernst region of the electrode response lies in the range 10–2–10–6 mol/l lead nitrate, and the detection limit reaches 10–7 mol/l. Thin film electrodes with PbS-AgI-As2S3 membranes showed a fairly high sensitivity to the Ag+ cations. The Nernst region of the electrode response is 10–1–10–6 mol/l silver nitrate, the detection limit of Ag+ cations reaches 10–7 mol/l. It has been established that the electrode properties of chalcogenide glasses and films of similar composition are practically the same.


Author(s):  
Д.Л. Байдаков

Методом химического нанесения из растворов халькогенидных стекол в н-бутиламине получены многокомпонентные халькогенидные пленки CuI-As2Se3, CuI-PbI2-As2Se3, CuI-SbI3-As2Se3, CuI-SbI3-PbI2-As2Se3. Синтез многокомпонентных медьсодержащих халькогенидных стекол, использовавшихся для нанесения пленок, проводили методом вакуумной плавки в кварцевых ампулах при температуре 400…950 °С и остаточном давлении не более 0,13 Па. Закалку стекол производили от 600 °С в воду со льдом с разливом расплава в ампуле. Навеску стекла размельчали в порошок и кипятили в н-бутиламине до полного растворения. Для предотвращения процессов окисления, нанесение и отжиг пленок проводили в атмосфере химически инертного азота. Подложку помещали на устройство для вращения, наносили на нее раствор и вращали подложку со скоростью несколько тысяч оборотов в минуту. Отжиг пленок проводили при температуре 100 °С в течение 1 ч. Измерение электропроводности полученных пленок проводили на постоянном и переменном токе в зависимости от значений электропроводности в температурном интервале 20…100 °С. Измерение коэффициентов диффузии проводили абсорбционным методом. Из диффузионных экспериментов определены значения коэффициентов диффузии катионов изотопа 110mAg в медьсодержащих халькогенидных пленках. Установлено, что значения коэффициентов диффузии ионов Ag+ в химически нанесенных пленках и исходных стеклах практически не различаются. Аналогию значений коэффициентов диффузии изотопа 110mAg в халькогенидных стеклах и пленках на их основе можно объяснить сохранением полимерной сетки связей халькогенидных стекол при их растворении в органических основаниях (аминах). В процессе нанесения и формирования пленок полимерная (макромолекулярная) структура раствора халькогенидных стекол сохраняется. The method of chemical deposition from solutions of chalcogenide glasses in n-butyl amine obtained multicomponent chalcogenide films CuI-As2Se3, CuI-PbI2-As2Se3, CuI-SbI3-As2Se3, CuI-SbI3-PbI2-As2Se3. Synthesis of copper multicomponent chalcogenide glasses, used for film deposition was carried out by vacuum melting in quartz ampoule at a temperature of 400…950 °C and a residual pressure of not more than 0.13 Pa. The temperature of glass produced from the 600 °C to the ice water spill of the melt in the ampoule. Weigh glass comminuted to a powder and heated in n-butylamine until complete dissolution. To prevent oxidation, deposition and annealing of the films was carried out in an atmosphere of nitrogen chemically inert. The substrate is placed on a device for rotating, it was applied to the solution and the substrate was rotated at a speed of several thousand revolutions per minute. Annealing of the films was carried out at 100 °C for 1 hour. Measurement of the electrical conductivity of the obtained films was conducted at a constant current and variable depending on the conductivity values ​​in the temperature range from 20 to 100 °C. Measurement of diffusion coefficients was performed according to the absorption method. From diffusion experiments, the values ​​of the diffusion coefficients 110mAg isotope cations in copper chalcogenide films. It was found that the values ​​of the diffusion coefficients of the ions Ag+ in a chemically deposited films and the original glasses are indistinguishable. The analogy of the diffusion coefficient values ​​110mAg isotope in chalcogenide glasses and films based on them can be attributed to the preservation of the polymer network connections chalcogenide glasses when dissolved in organic bases (amines). During application and film formation the polymer (macromolecular) structure of chalcogenide glasses of the solution is maintained.


ChemInform ◽  
2010 ◽  
Vol 25 (6) ◽  
pp. no-no
Author(s):  
M. T. S. NAIR ◽  
P. K. NAIR ◽  
H. M. K. K. PATHIRANA ◽  
R. A. ZINGARO ◽  
E. A. MEYERS

1993 ◽  
Vol 140 (10) ◽  
pp. 2987-2994 ◽  
Author(s):  
M. T. S. Nair ◽  
P. K. Nair ◽  
H. M. K. K. Pathirana ◽  
Ralph A. Zingaro ◽  
Edward A. Meyers

2021 ◽  
Vol 24 (1) ◽  
pp. 26-33
Author(s):  
I.P. Studenyak ◽  
◽  
A.I. Pogodin ◽  
M.J. Filep ◽  
O.P. Kokhan ◽  
...  

The single crystals of quaternary halogen Ag6PS5I were grown from the solution–melt by means of a vertical zone crystallization method. The crystal structure has been ascertained using the Rietveld method. Investigation of electrical conductivity was carried out using the impedance spectroscopy technique within the frequency range 1·101 – 3·105 Hz and temperature interval 293–383 K on gold contacts applied by chemical deposition from solution. Ionic (1.79·10-3 S/cm) and electronic (1.64·10-6 S/cm) components of electrical conductivity have been determined using the Nyquist plots. The mechanism of ionic conductivity for Ag6PS5I single crystal has been proposed which can be considered as ion diffusion through “channels” Ag2–Ag2.


Author(s):  
John C. Russ ◽  
Nicholas C. Barbi

The rapid growth of interest in attaching energy-dispersive x-ray analysis systems to transmission electron microscopes has centered largely on microanalysis of biological specimens. These are frequently either embedded in plastic or supported by an organic film, which is of great importance as regards stability under the beam since it provides thermal and electrical conductivity from the specimen to the grid.Unfortunately, the supporting medium also produces continuum x-radiation or Bremsstrahlung, which is added to the x-ray spectrum from the sample. It is not difficult to separate the characteristic peaks from the elements in the specimen from the total continuum background, but sometimes it is also necessary to separate the continuum due to the sample from that due to the support. For instance, it is possible to compute relative elemental concentrations in the sample, without standards, based on the relative net characteristic elemental intensities without regard to background; but to calculate absolute concentration, it is necessary to use the background signal itself as a measure of the total excited specimen mass.


Author(s):  
Klaus-Ruediger Peters ◽  
Samuel A. Green

High magnification imaging of macromolecules on metal coated biological specimens is limited only by wet preparation procedures since recently obtained instrumental resolution allows visualization of topographic structures as smal l as 1-2 nm. Details of such dimensions may be visualized if continuous metal films with a thickness of 2 nm or less are applied. Such thin films give sufficient contrast in TEM as well as in SEM (SE-I image mode). The requisite increase in electrical conductivity for SEM of biological specimens is achieved through the use of ligand mediated wet osmiuum impregnation of the specimen before critical point (CP) drying. A commonly used ligand is thiocarbohvdrazide (TCH), first introduced to TEM for en block staining of lipids and glvcomacromolecules with osmium black. Now TCH is also used for SEM. However, after ligand mediated osinification nonspecific osmium black precipitates were often found obscuring surface details with large diffuse aggregates or with dense particular deposits, 2-20 nm in size. Thus, only low magnification work was considered possible after TCH appl ication.


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