Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy
Magnesium fluoride and tellurium oxide were used for fabrication of the protective and antireflective coatings on the DKDP crystals. The variation of the technology of coating deposition leads to changes of surface composition of coatings which was studied by using the X-ray photoelectron spectros...
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| Cite this: | Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy / V.Yu. Loya, A.V. Lada, P.P. Puga, V.T. Gritsyna // Физическая инженерия поверхности. — 2004. — Т. 2, № 4. — С. 220–223. — Бібліогр.: 4 назв. — англ. |
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nasplib_isofts_kiev_ua-123456789-984942025-02-09T22:18:25Z Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy Дослідження оптичних покриттів на DKDP монокристалів методом рентгенівської фотоелектронної спектроскопії Исследование оптических покрытий на DKDP монокристаллов методом рентгеновской фотоэлектронной спектроскопии Loya, V.Yu. Lada, A.V. Puga, P.P. Gritsyna, V.T. Magnesium fluoride and tellurium oxide were used for fabrication of the protective and antireflective coatings on the DKDP crystals. The variation of the technology of coating deposition leads to changes of surface composition of coatings which was studied by using the X-ray photoelectron spectroscopy (XPS). The XPS data allow us to conclude that carbon and its compounds, as well as oxygen resulting in the oxide formation, are the main impurities introduced at the different stages of coating deposition. The results of paper testify the fact that the ion beam processing of the DKDP single crystals with film coatings deposited onto their working surfaces facilitates the recovery of the initial composition of the film under deposition, the removal of impurities from the film surfaces that, in turn, contributes to the improvement of mechanical properties of the coating and its consolidation. Для одержання захисних і просвітляючих покриттів кристалів ДКДР використовувалися фторид магнію та оксид телуру. Модифікація технології нанесення покриттів призвела до зміни складу поверхні покрить, що досліджувалися методом рентгенівської фотоелектронної спектроскопії (РФС). Дані РФС дозволяють зробити висновок, що вуглець та його сполуки, а такожкисень, що призводить до утворення оксидів, є основними домішками, які вводяться на різних етапах нанесення покриттів. Результати роботи свідчать на користь того, що обробка монокристалів ДКДР з плівками, осадженими на їх робочі поверхні, за допомогою іонного пучка сприяє відновленню вихідного складу осаджуваної плівки, вилученню домішок з її поверхні, що, в свою чергу, покращує механічні властивості покриття і його експлуатаційні характеристики. Для получения защитных и просветляющих покрытий кристаллов ДКДР использовались фторид магния и оксид теллура. Модификация технологии нанесения покрытий привела к изменению состава поверхности покрытий, исследуемых методом рентгеновской фотоэлектронной спектроскопии (РФС). Данные РФС позволяют заключить, что углерод и его соединения, а также кислород, приводящий к образованию оксидов, являются основными примесями, вводимыми на различных этапах нанесения покрытий. Результаты работы свидетельствуют в пользу того, что обработка монокристаллов ДКДР с пленками, осажденными на их рабочие поверхности, с помощью ионного пучка способствует восстановлению исходного состава осаждаемой пленки, удалению примесей с ее поверхности, что, в свою очередь, улучшает механические свойства покрытия и его эксплуатационные характеристики. 2004 Article Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy / V.Yu. Loya, A.V. Lada, P.P. Puga, V.T. Gritsyna // Физическая инженерия поверхности. — 2004. — Т. 2, № 4. — С. 220–223. — Бібліогр.: 4 назв. — англ. 1999-8074 https://nasplib.isofts.kiev.ua/handle/123456789/98494 621.793 en Физическая инженерия поверхности application/pdf Науковий фізико-технологічний центр МОН та НАН України |
| institution |
Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| collection |
DSpace DC |
| language |
English |
| description |
Magnesium fluoride and tellurium oxide were used for fabrication of the protective and antireflective
coatings on the DKDP crystals. The variation of the technology of coating deposition leads to changes
of surface composition of coatings which was studied by using the X-ray photoelectron spectroscopy
(XPS). The XPS data allow us to conclude that carbon and its compounds, as well as oxygen resulting
in the oxide formation, are the main impurities introduced at the different stages of coating deposition.
The results of paper testify the fact that the ion beam processing of the DKDP single crystals with
film coatings deposited onto their working surfaces facilitates the recovery of the initial composition of
the film under deposition, the removal of impurities from the film surfaces that, in turn, contributes to
the improvement of mechanical properties of the coating and its consolidation. |
| format |
Article |
| author |
Loya, V.Yu. Lada, A.V. Puga, P.P. Gritsyna, V.T. |
| spellingShingle |
Loya, V.Yu. Lada, A.V. Puga, P.P. Gritsyna, V.T. Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy Физическая инженерия поверхности |
| author_facet |
Loya, V.Yu. Lada, A.V. Puga, P.P. Gritsyna, V.T. |
| author_sort |
Loya, V.Yu. |
| title |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| title_short |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| title_full |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| title_fullStr |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| title_full_unstemmed |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| title_sort |
investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy |
| publisher |
Науковий фізико-технологічний центр МОН та НАН України |
| publishDate |
2004 |
| url |
https://nasplib.isofts.kiev.ua/handle/123456789/98494 |
| citation_txt |
Investigation of the optical coatings on the dkdp single ctystals by x-ray photoelectron spectroscopy / V.Yu. Loya, A.V. Lada, P.P. Puga, V.T. Gritsyna // Физическая инженерия поверхности. — 2004. — Т. 2, № 4. — С. 220–223. — Бібліогр.: 4 назв. — англ. |
| series |
Физическая инженерия поверхности |
| work_keys_str_mv |
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| first_indexed |
2025-12-01T09:18:46Z |
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2025-12-01T09:18:46Z |
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1850297003617026048 |
| fulltext |
ФІП ФИП PSE т. 3, № 1, vol. 3, No. 1220
INTRODUCTION
Di-deuterium potassium phosphate (DKDP) single
crystals have found wide practical application in the
different-purpose optical and laser device pro-
duction. This is due to high optical homogeneity of
the above crystals which provides laser harmonics
generation, parametric frequency tuning and laser
emission amplification [1]. The disadvantage of the
above crystals includes their relatively high
hygroscopicity leading to the thickening of polished
crystalline element surfaces under the influence of
atmospheric humidity. This deterioration of crystal
surface could be eliminated only partially using
special polymer coatings [2] which, unfortunately,
do not demonstrate enough strength to the action of
laser emission. More promising are the multi-layer
inorganic coatings. However the choice of material
and technology of deposition onto crystal surface is
a complicated tech-nical task caused mainly by such
DKDP properties as high fragility in combination with
low melting tem-perature. This eliminates the
possibility of application of thermal heating of sample
under surface cleaning and improvement of adhesion
of the deposited film.
Here we report the results of investigation of the
deposition conditions of double-layer protective and
antireflective TeO2 and MgF2-based coatings onto
the DKDP elements. In Tab. 1 we present the
characteristics of obtained coatings which allow
achieving the value of reflectance of the working
crystal surfaces of 0,1% at the emission wavelength
of Nd laser.
EXPERIMENTAL TECHNIQUES
We have studied three series of samples (A, B, C)
differing by the method of coating deposition by using
the thermal evaporation at 10–6 Torr pressure using
the ВУ-2M vacuum setup. There were investigated
three types of coatings deposited on the surface of
DKDP single crystals. The A series samples were
produced by serial deposition of the TeO2 and MgF2
layers of preset thickness onto the crystal with no
vacuum chamber depressurizing. To produce the
samples of series B, after the deposition of the TeO2
layer the chamber was depressurized with further
pumping out and deposition of the MgF2 layer. The
UDC 621.793
INVESTIGATION OF THE OPTICAL COATINGS ON THE DKDP SINGLE
CRYSTALS BY X-RAY PHOTOELECTRON SPECTROSCOPY
V.Yu. Loya, A.V. Lada , P.P. Puga, V.T. Gritsyna*
Institute of Electron Physics, Ukrainian National Academy of Sciences (Uzhgorod)
*V.N. Karazin Kharkiv National University
Ukraine
Received 09.12.2004
Magnesium fluoride and tellurium oxide were used for fabrication of the protective and antireflective
coatings on the DKDP crystals. The variation of the technology of coating deposition leads to changes
of surface composition of coatings which was studied by using the X-ray photoelectron spectroscopy
(XPS). The XPS data allow us to conclude that carbon and its compounds, as well as oxygen resulting
in the oxide formation, are the main impurities introduced at the different stages of coating deposition.
The results of paper testify the fact that the ion beam processing of the DKDP single crystals with
film coatings deposited onto their working surfaces facilitates the recovery of the initial composition of
the film under deposition, the removal of impurities from the film surfaces that, in turn, contributes to
the improvement of mechanical properties of the coating and its consolidation.
Table 1
Calculated values of coating layer thickness for the
emission at the wavelength of Nd laser
Material of
coating
Coating thickness,
µm
Refractive index
λ = 1,06 λ = 0,53 λ = 1,06µm λ = 0,53µm
TeO2
0,0199
0,220
0,012
0,103
2,208 2,295
MgF2
0,254
0,149
0,125
0,067
1,313 1,380
ФІП ФИП PSE т. 3, № 1, vol. 3, No. 1 221
C series samples were produced by simultaneous
deposition of both layers onto the crystal with preset
deposition cycle period.
The X-ray photoelectron spectroscopy (XPS)
technique was applied to analyze the elemental com-
position of both coating and crystal surfaces. XPS
spectra were recorded using a home-made high-
vacuum installation. AlKб (hн = 1486,6 eV) line was
used as the X-ray source and cylindrical mirror ana-
lyzer operated at constant pass energy of 100 eV
as an electron analyzer. The surface of crystals before
and after coating deposition was cleaned by the Ar+-
ion beam bombardment for 20 minutes at the beam
current density of 10 µA/cm2 and ion energy
of1 keV. The XPS spectra taken from the DKDP
single crystal surface with deposited coatings show
the lines of the main coating material elements and
an intense carbon line. Tab. 2 presents the relative
intensities of the observed lines for different samples
before and after ion beam cleaning.
EXPERIMENTAL RESULTS AND
DISCUSSION
Surface cleaning of A series samples by the Ar+ ion
beam results in almost total vanishing of the carbon
line and considerable reduction of the oxygen line
intensity. This indicates not only the high efficiency
of ion cleaning for elimination from the crystal surface
of compounds of organic origin, but also testifies
the formation of oxides on the MgF2 film surface.
This result agrees well with the data [3] on the
violation of stoichiometric composition of such films
due to the rise of anionic vacancies in the films. The
influence of atmosphere leads to neutralization of
the above indicated vacancies by the OH– ions and
the production of the complex composition
MgF2xOHx.
Analysis of the XPS spectra for the B series
samples measured immediately after the deposition
of the coatings also indicates the presence of the
magnesium, fluoride, oxygen and carbon lines of
almost the same intensity as for the A series samples.
However in this case ion cleaning of the surface leads
to essentially different results: the carbon line intensity
decreases only twice, whereas the oxygen line
undergoes almost no changes. Probably, in this case
oxygen-containing compounds are not only
adsorbed at the surface but are also involved in the
bulk of film. This is confirmed, in particular, by the
behavior of the fluoride line, the intensity of which
increases slightly after the ion cleaning.
At the simultaneous deposition of both TeO2 and
MgF2 layers onto the crystal (C series samples) the
XPS spectra demonstrate the lines of the deposited
elements: magnesium (binding energy of 54 and
95 eV), fluorine (685 eV), carbon (286 eV), oxygen
(535 eV) and tellurium (580 and 590 eV). Fig. 1
shows the XPS spectra for the C series samples
within the 500–750 eV energy range. In this energy
interval, the observed Te line has double shape and
is sensitive to the further ion beam processing, while
Table 2
XPS line intensities (relative units) of surface coatings prepared by different technological
procedures and subjected to ion beam cleaning
Sample
series
Element
Electron configuration
Binding energy, E (eV)
C O Te Mg F
1s1/2
285
1s1/2 3d5/2
3d5/2 2s1/2 2s1/2
532 573 583 91 686
After ion cleaning 7 8 – – 7 98
Before ion cleaning 35 40 – – 5 28A
After ion cleaning 12 45 – – 8 5
Before ion cleaning 23 53 – – 3 17B
After ion cleaning 12 16 25 15 7 10
Before ion cleaning 24 40 50 30 8 90
B
V.YU. LOYA, A.V. LADA, P.P. PUGA, V.T. GRITSYNA
ФІП ФИП PSE т. 3, № 1, vol. 3, No. 1222
its main maximum shifts towards the higher energies
by 10 eV with respect to the previous sample series.
After ion cleaning the intensity of these maxima is
decreased, and the maxima at 573 and 583 eV,
typical for the clean TeO4 film spectrum, are revealed
more distinctly. One may assume that at the
simultaneous deposition of both TeO2 and MgF2
layers onto the crystal the formation of TeF4-like
compounds occurs. This assumption is confirmed,
in particular, by the behavior of the fluoride lines in
the observed XPS spectrum. Ion cleaning of the
deposited film results in a slight increase (by 1,3
times) of the fluorine line intensity, while the oxygen
and carbon lines intensities decrease by 2,3 and 2,0
times, respectively. In this case the coating surface
reveals the properties similar to those of the MgF2
films.
For the oxygen lines the energy shift from 532 eV
to 535 eV is also observed allowing, thus, one to
as-sume the presence of the MgO-like oxides in
the MgF2 film or that of other combination of oxygen
compounds. In the case of C series samples, the
ccurrence of oxygen could be caused by its presence
in the residual gas of the deposition chamber.
The authors of [4] have shown that MgF2 film
processing by plasma discharge in the carbon tetra
fluoride atmosphere increases the mechanical du-
rability and enhances film resistance against the in-
fluence of climatic conditions. that could be
explained by disappearance of anionic vacancies.
This could be explained by anionic vacancies “curing”
and the recovery of the stoic-geometric composition
of pro-duced film. The results of the present paper
testify the fact that the ion beam processing of the
DKDP single crystals with film coatings deposited
onto their working surfaces facilitates the recovery
of the initial composition of the film under deposition,
the removal of impurities from the film surfaces that,
in turn, contributes to the improvement of mechanical
pro-perties of the coating and its consolidation. The
des-tructive effect of ion cleaning could be relatively
easy prevented by choosing the relevant regime in
each particular case.
Thus, our investigations allow us to conclude
that carbon and its compounds, as well as oxygen
resulting in the oxide formation, are the main
impurities introduced at the different stages of coating
deposition. One may not exclude the possibility of
oxygen production at the thermal decomposition of
tellurium dioxide used as one of the coatings. This
indicates the necessity of further search for the
coatings of optimal composition. At the same time,
the results obtained in this work allow to produce
optical elements of DKDP with protective and
antireflective coatings that possess high enough
technical characteristics and to develop the most
optimal regimes of the coating deposition.
REFERENCES
1. Van’kov A.B., Volynkin V.M., Serebyiakov V.A.,
Cher-tkov A.V. Cooled electro-optical deflector
by using DKDP crystal // Quantum electronics.–
1989.– Vol. 16, – № 11. – P. 2329-2335.
2. Shirokshina E.V., Sadovnikova T.V. The increase
of chemical resistance of parts made of DKDP
crystals //OMP. – 1981. – № 3.– P. 38-40.
3. Levina M.D., Furman Sh.A., Korolev N.V.
Investi-gations of influence of the thin film
stoichiometric composition on the change of
optical characteristics of interference coactions
Fig. 1. XPS spectra of the C series of samples: (a) – prior
to the ion-beam cleaning, (b) – after the ion-beam cleaning.
INVESTIGATION OF THE OPTICAL COATINGS ON THE DKDP SINGLE CRYSTALS BY X-RAY PHOTOELECTRON ...
ФІП ФИП PSE т. 3, № 1, vol. 3, No. 1 223
in time//Optika i Spectro-scopiya. – 1978. –Vol.
45, № 6. – P. 1173-1177.
4. Vvedensky V.D., Levina M.D. The increase the
co-atings strength of magnesium fluoride//OMP.
– 1983. – № 5. – P. 35-36.
ДОСЛІДЖЕННЯ ОПТИЧНИХ
ПОКРИТТІВ НА DKDP
МОНОКРИСТАЛАХ МЕТОДОМ
РЕНТГЕНІВСЬКОЇ
ФОТОЕЛЕКТРОННОЇ СПЕКТРОСКОПІЇ
В.Ю. Лоя, А.В. Лада ,
П.П. Пуга, В.Т. Грицина
Для одержання захисних і просвітляючих по-
криттів кристалів ДКДР використовувалися
фторид магнію та оксид телуру. Модифікація тех-
нології нанесення покриттів призвела до зміни
складу поверхні покрить, що досліджувалися ме-
тодом рентгенівської фотоелектронної спектро-
скопії (РФС). Дані РФС дозволяють зробити вис-
новок, що вуглець та його сполуки, а також кисень,
що призводить до утворення оксидів, є основними
домішками, які вводяться на різних етапах нане-
сення покриттів. Результати роботи свідчать на
користь того, що обробка монокристалів ДКДР з
плівками, осадженими на їх робочі поверхні, за
допомогою іонного пучка сприяє відновленню ви-
хідного складу осаджуваної плівки, вилученню до-
мішок з її поверхні, що, в свою чергу, покращує
механічні властивості покриття і його експлу-
атаційні характеристики.
ИССЛЕДОВАНИЕ ОПТИЧЕСКИХ
ПОКРЫТИЙ НА DKDP
МОНОКРИСТАЛЛАХ МЕТОДОМ
РЕНТГЕНОВСКОЙ
ФОТОЭЛЕКТРОННОЙ
СПЕКТРОСКОПИИ
В.Ю. Лоя, А.В. Лада ,
П.П. Пуга, В.Т. Грицына
Для получения защитных и просветляющих по-
крытий кристаллов ДКДР использовались фто-
рид магния и оксид теллура. Модификация техно-
логии нанесения покрытий привела к изменению
состава поверхности покрытий, исследуемых ме-
тодом рентгеновской фотоэлектронной спектро-
скопии (РФС). Данные РФС позволяют заклю-
чить, что углерод и его соединения, а также кис-
лород, приводящий к образованию оксидов,
являются основными примесями, вводимыми на
различных этапах нанесения покрытий. Резуль-
таты работы свидетельствуют в пользу того, что
обработка монокристаллов ДКДР с пленками,
осажденными на их рабочие поверхности, с по-
мощью ионного пучка способствует восстановле-
нию исходного состава осаждаемой пленки, уда-
лению примесей с ее поверхности, что, в свою
очередь, улучшает механические свойства по-
крытия и его эксплуатационные характеристики.
V.YU. LOYA, A.V. LADA, P.P. PUGA, V.T. GRITSYNA
|