RU2651212C1 - Method of reparation of cadmium sulfide films on a monocrystalline silicon - Google Patents
Method of reparation of cadmium sulfide films on a monocrystalline silicon Download PDFInfo
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- RU2651212C1 RU2651212C1 RU2017109759A RU2017109759A RU2651212C1 RU 2651212 C1 RU2651212 C1 RU 2651212C1 RU 2017109759 A RU2017109759 A RU 2017109759A RU 2017109759 A RU2017109759 A RU 2017109759A RU 2651212 C1 RU2651212 C1 RU 2651212C1
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- cadmium
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- monocrystalline silicon
- pyrolysis
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 18
- 229910021421 monocrystalline silicon Inorganic materials 0.000 title claims abstract description 12
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 11
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 18
- 239000000443 aerosol Substances 0.000 claims abstract description 15
- 238000000197 pyrolysis Methods 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000004767 nitrides Chemical class 0.000 claims abstract description 3
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 abstract description 11
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 8
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 5
- 230000008021 deposition Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000007921 spray Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 150000001661 cadmium Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000009718 spray deposition Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- WLZRMCYVCSSEQC-UHFFFAOYSA-N cadmium(2+) Chemical compound [Cd+2] WLZRMCYVCSSEQC-UHFFFAOYSA-N 0.000 description 1
- NCDKOFHLJFJLTB-UHFFFAOYSA-N cadmium(2+);dioxido(oxo)silane Chemical compound [Cd+2].[O-][Si]([O-])=O NCDKOFHLJFJLTB-UHFFFAOYSA-N 0.000 description 1
- GYKJCZLJNKYSRK-UHFFFAOYSA-N cadmium;thiourea Chemical class [Cd].NC(N)=S GYKJCZLJNKYSRK-UHFFFAOYSA-N 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000224 chemical solution deposition Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- -1 space group ) Chemical compound 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
Description
Изобретение относится к получению поликристаллических пленок сульфида и оксида кадмия на монокристаллическом кремнии с помощью техники пиролиза аэрозоля раствора на нагретой подложке.The invention relates to the production of polycrystalline films of sulfide and cadmium oxide on monocrystalline silicon using the technique of pyrolysis of aerosol solution on a heated substrate.
Сульфид кадмия является одним из перспективных материалов для создания тонкопленочных фотопреобразователей, сенсоров, датчиков и других устройств (Фотопроводящие пленки (типа CdS) / Под ред. З.И. Киръяшкиной, А.Г. Рокаха. Саратов: Изд-во Сарат.ун-та, 1979. - 195 с.). Актуальной задачей для создания фотоэлектронных устройств является синтез пленок сульфида кадмия с контролируемыми свойствами на поверхности монокристаллических полупроводников, в частности кремния. Варьирование оптических, электрических и фотоэлектрических свойств, а также кристаллической структуры сульфида кадмия возможно с помощью метода пиролиза аэрозоля на нагретой подложке.Cadmium sulfide is one of the promising materials for the creation of thin-film photoconverters, sensors, sensors and other devices (Photoconductive films (CdS type) / Edited by ZI Kiryashkina , AG Rokakha . Saratov: Publishing house Sarat.un- that, 1979. - 195 p.). An urgent task for the creation of photoelectronic devices is the synthesis of cadmium sulfide films with controlled properties on the surface of single-crystal semiconductors, in particular silicon. Varying the optical, electrical, and photoelectric properties, as well as the crystal structure of cadmium sulfide, is possible using the aerosol pyrolysis method on a heated substrate.
Известны способы получения пленок сульфидов ряда металлов (Zn, Cd, Ga, In, Pb, Bi, Cr, Mn и др.) с использованием тиокарбамидных координационных соединений как прекурсоров (Наумов А.В., Семенов В.К., Авербах Е.М. Тиомочевинные координационные соединения в процессах синтеза сульфидов металлов // Химическая промышленность. 2003. Т. 80, №2. С. 17-26). К ним относятся метод пиролиза аэрозоля (англ. Spray Pyrolysis Deposition, Chemical Spray Deposition) (Chamberlin R.R., Skarman J.S. Chemical spray deposition process for inorganic films // J. Electrochem. Soc. 1966. V. 113, N 1. P. 86-89), методы химического осаждения из растворов (метод «химической ванны» (англ. Chemical Bath Deposition), «метод погружения» (англ. Dip Method)). Одним из недостатков этих методов является невозможность получения пленок с хорошей адгезией на полупроводниковых подложках, в том числе подложках mono-Si. Эпитаксиальные пленки сульфидов на Si и АIIIВV можно получать методом вакуумного распыления (Fuke S., Araki H., Kuwahara K. et al. Indium doping effects on vapor-phase growth of ZnS on GaP // J. Appl. Phys. V. 59. 1986. P. 1761-1763). К числу недостатков в этом случае относятся сложность технологического процесса, высокая стоимость оборудования, а также трудности в управлении отклонениями от стехиометрии фаз переменного состава.Known methods for producing sulfide films of a number of metals (Zn, Cd, Ga, In, Pb, Bi, Cr, Mn, etc.) using thiocarbamide coordination compounds as precursors ( Naumov A.V., Semenov V.K., Averbakh E. M. Thiourea coordination compounds in the synthesis of metal sulfides // Chemical Industry. 2003. V. 80, No. 2, P. 17-26). These include aerosol pyrolysis (Spray Pyrolysis Deposition, Chemical Spray Deposition) ( Chamberlin RR, Skarman JS . Chemical spray deposition process for inorganic films // J. Electrochem. Soc. 1966. V. 113,
Наиболее близким к предлагаемому способу является способ получения пленок CdS на стеклообразных подложках распылением растворов тиокарбамидных комплексов кадмия (Наумов А.В., Семенов В.Н, Гончаров Е.Г. Свойства пленок CdS, полученных из координационных соединений кадмия с тиомочевиной // Неорган. материалы. 2001. Т. 37, №6. С. 647-652). Способ предполагает синтез исходного координационного соединения кадмия (II) с тиокарбамидом, а затем пиролиз аэрозоля водного раствора этого соединения на нагретой подложке, в результате чего образуются слои сульфида кадмия. Недостатком способа является избирательная адгезия к стеклообразным подложкам (кварцевое и силикатное стекло, ситалл) и невозможность осаждения качественных слоев на монокристаллах кремния.Closest to the proposed method is a method for producing CdS films on glassy substrates by spraying solutions of cadmium thiourea complexes ( Naumov A.V., Semenov V.N., Goncharov E.G. Properties of CdS films obtained from cadmium coordination compounds with thiourea // Neorgan. materials. 2001. V. 37, No. 6. S. 647-652). The method involves the synthesis of the initial coordination compound of cadmium (II) with thiocarbamide, and then the pyrolysis of the aerosol of an aqueous solution of this compound on a heated substrate, resulting in the formation of layers of cadmium sulfide. The disadvantage of this method is the selective adhesion to glassy substrates (quartz and silicate glass, glass) and the impossibility of deposition of high-quality layers on silicon single crystals.
Задачей изобретения является разработка процесса осаждения пленок сульфида кадмия на поверхности mono-Si без предварительной обработки подложки.The objective of the invention is to develop a process for the deposition of films of cadmium sulfide on the surface of mono- Si without preliminary processing of the substrate.
Технический результат изобретения заключается в осаждении зеркально гладких поликристаллических пленок гексагональной модификации сульфида кадмия толщиной до 250 нм на монокристаллическом кремнии, обладающих хорошей адгезией к подложке.The technical result of the invention consists in the deposition of mirror-smooth polycrystalline films of hexagonal modification of cadmium sulfide with a thickness of up to 250 nm on monocrystalline silicon, which have good adhesion to the substrate.
Технический результат изобретения достигается тем, что в способе получения пленок сульфида кадмия на монокристаллическом кремнии используется техника пиролиза аэрозоля раствора на нагретой подложке при постоянной температуре в интервале 450-500°С, согласно изобретению пиролиз аэрозоля проводится в два этапа, на первом в качестве распыляемого раствора используется 0.03 моль/л водный раствор хлорида или нитрида кадмия, а на втором - 0.15 моль/л водный раствор тиомочевины.The technical result of the invention is achieved by the fact that in the method for producing cadmium sulfide films on monocrystalline silicon, the technique of pyrolysis of an aerosol of a solution on a heated substrate at a constant temperature in the range of 450-500 ° C is used, according to the invention, aerosol pyrolysis is carried out in two stages, the first as a spray solution a 0.03 mol / L aqueous solution of cadmium chloride or nitride is used, and in the second, 0.15 mol / L an aqueous solution of thiourea.
На фиг. 1 приведен спектр отражения сульфидизированного слоя, осажденного при пиролизе аэрозоля раствора Сd(NO3)2 на монокристаллическом кремнии.In FIG. Figure 1 shows the reflection spectrum of a sulfidized layer deposited during pyrolysis of the aerosol of a solution of Cd (NO 3 ) 2 on single-crystal silicon.
На фиг. 2 приведены дифрактограммы слоев: 1 - осажденного при распылении раствора CdCl2 на нагретую подложку Si (100); 2 - сформированного при последующей сульфидизации.In FIG. Figure 2 shows the diffraction patterns of the layers: 1 — a solution of CdCl 2 deposited upon spraying onto a heated Si (100) substrate; 2 - formed during subsequent sulfidization.
Способ позволяет сформировать пленки CdS на поверхности mono-Si путем проведения процесса в два разделенных этапа с помощью пиролиза аэрозоля раствора, при этом не требует специальной подготовки подложек, в качестве подложек используются готовые пластины монокристаллического кремния. На первом этапе осаждается слой оксида кадмия за счет высокотемпературного гидролиза соли кадмия. На втором этапе этот слой превращается в сульфид под действием тиокарбамида как сульфидизирующего агента. Такой двухстадийный процесс отличается от обычного метода пиролиза аэрозоля тем, что обходится без образования тиокарбамидных комплексов в растворе, а слой сульфида формируется на подложке в результате взаимодействия с тиокарбамидом заранее осажденного твердофазного продукта. Осаждение ведется на воздухе. Растворы распыляются с помощью пневматической форсунки, газ-распылитель - воздух.The method allows the formation of CdS films on a mono- Si surface by carrying out the process in two separated stages using solution aerosol pyrolysis, without requiring special preparation of substrates, ready-made single-crystal silicon wafers are used as substrates. At the first stage, a cadmium oxide layer is deposited due to the high-temperature hydrolysis of the cadmium salt. In the second stage, this layer is converted to sulfide by the action of thiocarbamide as a sulfidizing agent. Such a two-stage process differs from the usual method of aerosol pyrolysis in that it dispenses with the formation of thiocarbamide complexes in solution, and a sulfide layer is formed on the substrate as a result of interaction with a thiocarbamide of a pre-deposited solid-phase product. Precipitation is carried out in air. The solutions are sprayed using a pneumatic nozzle, the gas spray is air.
С использованием этого метода были сформированы зеркально гладкие слои (CdS, CdO)/Si(100) толщиной до 250 нм с коэффициентом отражения в видимой области до 25%, имеющие интерференционную окраску (спектр отражения приведен на фиг. 1). Оптическая ширина запрещенной зоны варьируется в пределах 2.45-2.48 эВ в зависимости от исходной соли кадмия. Пленки дают четкую рентгенодифракционную картину (фиг. 2), позволяющую говорить о хорошо сформированной кристаллической структуре твердых фаз. Оксид кадмия имеет кубическую структуру (структурный тип NaCl, пространственная группа ), сульфид кадмия имеет гексагональную структуру (структурный тип вюрцита, Р6 3 mc).Using this method, specularly smooth (CdS, CdO) / Si (100) layers with a thickness of up to 250 nm with a reflectance in the visible region of up to 25% having interference color were formed (the reflection spectrum is shown in Fig. 1). The optical band gap varies between 2.45–2.48 eV, depending on the initial cadmium salt. The films give a clear x-ray diffraction pattern (Fig. 2), which allows us to speak of a well-formed crystalline structure of solid phases. Cadmium oxide has a cubic structure (structural type NaCl, space group ), cadmium sulfide has a hexagonal structure (structural type of wurtzite, P6 3 mc ).
Пример 1. Пленки оксида кадмия получали пневматическим распылением раствора CdCl2 на нагретые подложки, представляющие собой полированные пластины кремния ЭКЭФ-20 ориентации (100). Температура подложки составляла 500.0±0.1°С и контролировалась с помощью терморегулятора ТРМ-101, управляющего плоской печью резистивного нагрева. Концентрация соли кадмия составляла 0.030 моль/л, расход раствора (плотность потока аэрозоля) - в интервале от 0.1⋅10-8 до 0.5⋅10-8 л/(мм2⋅с), время напыления - от 10 до 30 мин.Example 1. Films of cadmium oxide were obtained by pneumatic spraying of a solution of CdCl 2 on heated substrates, which are polished silicon wafers of EKEF-20 orientation (100). The substrate temperature was 500.0 ± 0.1 ° С and was controlled using a ТРМ-101 thermostat controlling a flat resistive heating furnace. The concentration of cadmium salt was 0.030 mol / L, solution flow rate (spray flux density) - ranging from 0.1⋅10 -8 to 0.5⋅10 -8 l / (mm 2 ⋅s), sputtering time - from 10 to 30 minutes.
Осажденные слои подвергали дальнейшей сульфидизации, обрабатывая их аэрозолем раствора 0.150 моль/л тиокарбамида при температуре 500°С, в результате чего оксид кадмия превращался в сульфид гексагональной вюрцитной модификации. Таким образом были получены зеркально гладкие поликристаллические слои 250 нм, обладающие хорошей адгезией к подложке. Параметры решеток кубического CdO () а=0.4685 нм, гексагонального CdS (Р63mc) а=0.4130 нм, с=0.6707 нм, оптическая ширина запрещенной зоны 2.45 эВ.The deposited layers were subjected to further sulfidization, treating them with an aerosol of a solution of 0.150 mol / L thiocarbamide at a temperature of 500 ° С, as a result of which cadmium oxide turned into hexagonal wurtzite sulfide. Thus, mirror-smooth polycrystalline layers of 250 nm were obtained, which have good adhesion to the substrate. Lattice parameters of cubic CdO ( ) а = 0.4685 nm, hexagonal CdS (Р6 3 mc) а = 0.4130 nm, с = 0.6707 nm, optical band gap 2.45 eV.
Пример 2. Пневматическим распылением раствора 0.030 моль/л Cd(NO3)2 на нагретые до 500°С полированные пластины кремния ЭКЭФ-20 ориентации (100) осаждали слои, представляющие собой смесь оксида кадмия и стеклообразной фазы предположительно на основе силиката кадмия CdSiO3. Сульфидизация в аэрозоле раствора 0.150 моль/л тиокарбамида при 500°С на втором этапе привела к полному исчезновению стеклообразной фазы и превращению оксида кадмия в сульфид гексагональной модификации. Таким образом были сформированы поликристаллические слои толщиной 250 нм с хорошей адгезией к подложке, со структурными параметрами CdO 0.4684 нм, CdS 0.4130 нм (а), 0.6707 нм (с), оптической шириной запрещенной зоны 2.48 эВ.Example 2. Pneumatic spraying of a solution of 0.030 mol / L Cd (NO 3 ) 2 onto heated (500) orientation polished silicon wafers of EEC-20 orientation (100) to 500 ° C precipitated layers consisting of a mixture of cadmium oxide and a glassy phase, presumably based on cadmium silicate CdSiO 3 . The aerosol sulfidization of a solution of 0.150 mol / L thiocarbamide at 500 ° С in the second stage led to the complete disappearance of the glassy phase and the conversion of cadmium oxide to hexagonal sulfide. Thus, polycrystalline layers 250 nm thick were formed with good adhesion to the substrate, with the structural parameters CdO 0.4684 nm, CdS 0.4130 nm ( a ), 0.6707 nm ( s ), and an optical band gap of 2.48 eV.
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