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15ряд ключевых идей, без которых эта работа вряд ли состоялась бы.
Литература
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СТРУКТУРНО-ФАЗОВЫЙ СОСТАВ И СВОЙСТВА МНОГОФАЗНЫХ ПОКРЫТИЙ
Юров В.М.
Карагандинский университет имени Е.А. Букетова,
Караганда, Казахстан Бердибеков А.Т.
Национальный университет обороны имени Первого Президента РК - Елбасы,
Нур-Султан, Казахстан Бельгибеков Н.А.
ТОО «Research & development центр «Казахстан инжиниринг»,
Нур-Султан, Казахстан
STRUCTURAL-PHASE COMPOSITION AND PROPERTIES MULTI-PHASE COATINGS
Yurov V.
Karaganda University named after E.A. Buketov, Kazakhstan, Karaganda Berdibekov A.
National Defense University named after the First President of the republic of Kazakhstan - Elbasy,
Kazakhstan, Nur-Sultan Belgibekov N.
LLP "Research & Development center "Kazakhstan engineering",
Kazakhstan, Nur-Sultan
АННОТАЦИЯ
Одна из ключевых проблем, которые следует решить при создании нанокомпозиционных ионно-плазменных покрытий, это генерация многокомпонентных потоков, осаждаемых на подложку. В работе исследован структурно -фазовый состав многофазных покрытий. Обнаружено образование сверхтвердых покрытий, полученных при одновременном распылении титанового катода и мишени 12Х18Н10Т в среде азота, когда происходит образование нитридных фаз. Этот результат имеет важное практическое значение для упрочнения деталей механизмов и машин различных отраслей промышленности, в том числе и для деталей агрегатов тепловых электростанций.
ABSTRACT
One of the key problems that should be solved when creating nanocomposite ion-plasma coatings is the generation of multicomponent flows deposited on the substrate. The paper investigates the structural-phase composition of multiphase coatings. The formation of superhard coatings obtained by the simultaneous sputtering of a titanium cathode and a 12Kh18N10T target in a nitrogen atmosphere, when the formation of nitride phases occurs, is found. This result is of great practical importance for the strengthening of parts of mechanisms and machines of various industries, including for parts of units of thermal power plants.
Ключевые слова: ионно-плазменные покрытия, многофазные катоды, многокомпонентные потоки, микротвердость, элементный состав.
Keywords: ion-plasma coatings, multiphase cathodes, multicomponent flows, microhardness, elemental composition.
Introduction
Modern materials must combine high properties and qualities to ensure the necessary resource and reliability of the products of aerospace technology, shipbuilding, mechanical engineering, nuclear energy, radio engineering and computer technology and construction. Therefore, the development of methods for obtaining functional coatings that meet the modern requirements of industrial production will remain a priority area of practical materials science for a long time to
come [1-4]. This work presents the results of studies of multiphase coatings obtained by the ion-plasma method with ion-assisted. Previous research results are reflected in [5-10].
Structural-phase composition and properties of multiphase coatings
For the deposition of coatings, we used titanium targets VT-1-00 according to GOST 1908, targets made of steel grade 12X18H10T and a multiphase target Cr-Mn-
Si-Cu-Fe-Al. Using these targets, coatings were deposited on a steel substrate in an argon and nitrogen gas atmosphere for 40 min. The thickness of the coatings and their elemental composition were measured using a Quanta 200 3D electron microscope, which is a system with electron and focused ion beams.
The phase composition and structural parameters of the samples were studied on an XRD-6000 diffractome-ter using CuKa radiation. Analysis of the phase composition, sizes of coherent scattering regions, internal elastic stresses (Ad / d) was carried out using the PCPDFWIN and PDF4 + databases, as well as the POWDER CELL 2.4 full-profile analysis program. For the samples, the nanohardness of the coatings was determined using a nano-identification system according to
the Oliver and Fahr method using a Berkovich indenter at a load of 1 g and a holding time of 15 s. A Cr-Mn-Si-Cu-Fe-Al coating was applied to a stainless steel substrate in a nitrogen gas atmosphere for 40 min. Figure 1 shows an electron microscopic image of this coating. To measure the thickness of the Cr-Mn-Si-Cu-Fe-Al coating, an area was cut out on its surface with a focused ion beam. The layer thickness is 1 ^m. Figure 2 shows the thickness of the Cr-Mn-Si-Cu-Fe-Al coating of the model sample No. 1. To study the elemental composition, three samples were made in different areas of the selected area of the Cr-Mn-Si-Cu-Fe-Al coating. Figure 3 shows the elemental composition of the coverage at one point of the selected site.
Figure 1 - SEM coating Cr-Mn-Si-Cu-Fe-Al
Figure 2 - Coating thickness Cr-Mn-Si-Cu-Fe-Al
Figure 3 - XPS coating Cr-Mn-Si-Cu-Fe-Al
Table 1 shows the percentage ratios of the chemical elements of the coating. The results of studying the phase composition and structural parameters of the sample are shown in Table 2.
Table 1
Elemental composition of the coating Cr-Mn-Si-Cu-Fe-Al
Element Wt % At % K- Ratio Z A F
N 2,89 8,88 0,0151 1,1767 0,4433 1,0024
O 5,72 15,38 0,0387 1,1656 0,5765 1,0057
Al 0,17 0,27 0,0010 1,0846 0,5532 1,0010
Si 0,29 0,45 0,0022 1,1226 0,6748 1,0020
Cr 89,08 73,67 0,8754 0,9802 1,0010 1,0015
Mn 0,00 0,00 0,0000 0,9619 1,0029 1,0004
Fe 1,26 0,97 0,0115 0,9794 0,9295 1,0003
Cu 0,58 0,39 0,0053 0,9445 0,9680 1,000
Total 100,00 100,00 - - - -
Table 2
Phase composition of Cr-Mn-Si-Cu-Fe-Al in a nitrogen gas atmosphere__
Sample Detected phases Phase content, vol.% Lattice parameters, Á CSR dimensions, nm Ad/d*10- 3
Sample Cr-Mn-Si-Cu-Fe-Al in a nitrogen gas atmosphere, 40 min FeN0.0324 60,6 a = 3,598 103,4 3,460
TiN0.31O0.31 39,4 a = 4,211 25,6 5,143
For sample No. 1, the nanohardness of the Cr-Mn-Si-Cu-Fe-Al coating in a nitrogen gas atmosphere was determined, which is equal to 7.413 GPa, which corresponds to 686.57 units of hardness by the Vickers method (Figure 4). It was determined: the yield modulus of this coating, which is 169.51 GPa, the yield is 0.68%, and the relaxation of the coating is 0.05%. To determine all of the above parameters, the Poisson number for the Cr-Mn-Si-Cu-Fe-Al coating in a nitro-
gen gas atmosphere was determined to be approximately 0.30. Sample No. 2 of stainless steel was coated with 12X18H10T + Ti in a nitrogen gas atmosphere for 40 min. As a result of the study, we measured the thickness of the applied layer and made an elemental analysis of this coating. Figure 5 shows an electron microscopic image of a 12X18H10T + Ti coating in a nitrogen gas atmosphere of a model sample before the start of the study.
Figure 4 - Nano-hardness of the Cr-Mn-Si-Cu-Fe-Al coating in a gas atmosphere of nitrogen
To measure the thickness of the deposited layer of coating 12X18H10T + Ti in a nitrogen gas atmosphere of model sample No. 2, an area was cut out on its surface with a focused ion beam. The layer thickness is 1.5 microns. Figure 6 shows the thickness of the
Figure 5 - SEM of coating 12X18H10T + Ti in a gas atmosphere of nitrogen
12X18H10T + Ti coating in a nitrogen gas atmosphere of the model sample No. 2. Figure 7 shows the elemental composition at one point of the 12X18H10T + Ti coating in a nitrogen atmosphere.
Figure 6 - Thickness of 12X18H10T + Ti coating in nitrogen environment
Figure 7 - Elemental composition of 12X18H10T+Ti coating in nitrogen atmosphere
Table 3 shows the percentage ratios of the chemical elements of the coating.
Elemental composition of 12X18H10T+Ti coating in nitrogen atmosphere
Table 3
Element Wt % At % K- Ratio Z A F
N K 4,47 14,18 0,0259 1,1843 0,4877 1,0027
Ti K 73,00 67,66 0,7304 0,9902 0,9969 1,0137
Cr K 5,96 5,09 0,0547 0,9860 0,9196 1,0130
Fe K 14,17 11,26 0,1327 0,9850 0,9486 1,0024
Ni K 2,40 1,81 0,0230 0,9983 0,9620 1,0000
Total 100,00 100,00 - - - -
The results of studying the phase composition and structural parameters are shown in Table 4.
Table 4
Phase composition of 12X18H10T + Ti coating in nitrogen atmosphere _
Sample Detected phases Phase content, vol.% Lattice parameters, Á CSR dimensions, nm Ad/d*10-3
12X18H10T + Ti in a nitrogen gas atmosphere FeNi.0324 9,8 a = 3.592 10,35 2,18
TiN 85,5 a = 4,240 14,71 5,87
Fe-a 4,6 a = 2.864 7,29 4,84
For sample No. 2, the nanohardness of the 12X18H10T coating with Ti in a nitrogen gas atmosphere was determined, which is 35.808 GPa, which corresponds to 3316.2 units of hardness by the Vickers method (Figure 8). Were determined: the modulus of yield of the coating 12X18H10T with Ti in a nitrogen
gas atmosphere, which is equal to 378.56 GPa, its fluidity is 0.15%, and the relaxation of the coating is 0.05%. To determine all of the above parameters, the Poisson number was determined for coating 12X18H10T with Ti in a nitrogen gas atmosphere equal to approximately 0.27. Sample No. 3 of stainless steel
was also coated with 12X18H10T+Ti in an argon gas atmosphere for 40 minutes. Figure 9 shows the SEM of the 12X18H10T+Ti coating in an argon gas atmosphere
of the sample before the start of the study. The layer
1 1 ■
thickness is 989.98 nm. Figure 10 shows the thickness of the 12X18H10T+Ti coating in an argon gas atmosphere of sample No. 3.
Figure 8 - Nanohardness of the coating 12X18H10T+Ti in nitrogen environment
Figure 9 - SEM coating
12X18H10T+Ti in argon environment
Figure 10 - Coating thickness 12X18H10T+Ti in argon
Figure 11 shows the elemental composition of the coating at one point of the selected area of the 12X18H10T + Ti coating in an argon atmosphere. Table 5 shows the percentage ratios of the chemical elements of the coating. For sample No. 3, the nanohardness of the 12X18H10T + Ti coating in an argon gas
atmosphere (Figure 12) was determined, which is 3.339 GPa, which corresponds to 309.27 units of hardness by the Vickers method. As for the first two samples, the yield modulus was determined, which is 111.03 GPa, the fluidity is 1.07%, and the relaxation of the coating is 0.08%. Poisson's number - 0.27.
Figure 11 - Elemental composition of 12X18H10T+Ti coating in argon environment
Figure 12 - Nanohardness of Cr-Mn-Si-Cu-Fe-Al coating in nitrogen atmosphere
Elemental composition of 12X18H10T+Ti coating in argon
Table 5
Element Wt % At % K- Ratio Z A F
N K 10,26 11,68 0,1089 1,0015 0,9839 1,0765
Cr K 16,05 16,83 0,1750 0,9981 0,9836 1,1103
Fe K 64,96 63,40 0,6408 0,9980 0,9798 1,0089
Ni K 8,73 8,10 0,0840 1,0127 0,9502 1,0000
Total 100,00 100,00 - - - -
Features of the formation of multiphase coatings
From the above experimental data, it follows that when the coatings are applied for 40 minutes, coatings with a thickness of (1-1.5) microns are formed. Elemental analysis showed a high Cr content in the Cr-Mn-Si-Cu-Fe-Al coating in a nitrogen gas atmosphere -89.09%. The 12X18H10T + Ti coating in a nitrogen gas atmosphere contains 73% Ti, and the 12X18H10T + Ti coating in an argon gas atmosphere has a high Fe content of 64.96%.
This study of the elemental composition showed that all elements of working targets are present in their coatings, but the ratio between them can vary significantly.
In the first and second coatings, as a result of ionplasma treatment, nitrides were formed, which justifies the increase in their nanohardness. In the third coating, the nanohardness increased insignificantly relative to the nanohardness of the substrate. For the Cr-Mn-Si-Cu-Fe-Al coating in a nitrogen gas atmosphere, the na-
nohardness is 7.413 GPa, for a 12X18H10T + Ti coating in a nitrogen gas atmosphere, 35.808 GPa, and for a 12X18H10T + Ti coating in an argon gas atmosphere, it is 3.339 GPa. It follows from the data presented that the 12X18H10T + Ti coating obtained by simultaneous sputtering of a titanium cathode and a stainless steel cathode in a nitrogen gas atmosphere has the highest nanohardness. It is of interest to compare the results obtained with the known data on nanoindentation of other materials. Such data are presented in Table 6.
Properties of materials calculated
The result of the comparison shows that the nanohardness of the 12X18H10T + Ti coating in a nitrogen atmosphere exceeds all materials presented in Table 6, among which the last three are used as hardening and abrasive coatings. Structural-phase analysis revealed that the Cr-Mn-Si-Cu-Fe-Al coating in a nitrogen gas atmosphere has two phases FeN0.0324 - 60.6%, TiN -39.4%, a 12X18H10T + Ti coating in a nitrogen gas atmosphere has three phases FeN0.0324 - 9.8%, TiN -85.5%, Fe - a - 4.6%.
Table 6
from nanoindentation data [11]
Material H, GPa E, GPa R, %
Copper 2,1 121 14
Titanium (OT4-1) 4,1 130 19
Multilayer film Ti/a-C: H 8,0 128 34
Zr-Cu-Ti-Ni amorphous tape 11,5 117 42
Silicon (100) 11,8 174 62
Ti-Si-N Thin Film 28,4 295 62
The latter circumstance leads to a sharp increase in nanohardness. Table 7 lists the properties of nitride coatings.
Table 7
Properties of nitride coatings [12]
Nitride Temperature melting coating, 0C Microhardness coatings GPa Electrical conductivity coating, mkOhm-1^m-1 Top. coating tension, J/m2 Top. tension metal, J/m2
TiN 2945 20,0 40 0,474 1,933
ZrN 2955 16,0 18 0,518 2,125
HfN 3330 22,0 32 0,610 2,503
NbN 2320 14,0 78 0,670 2,741
TaN 3360 17,5 180 0,735 3,014
It can be seen that in this case the hardness of the 12X18H10T + Ti coatings in a nitrogen gas atmosphere (35.808 GPa) exceeds the hardness of all coatings presented in Table 6. One of the key problems that should be solved when creating nanocomposite ion-plasma coatings is the generation of multicomponent flows deposited on the substrate. The main idea used in this work was as follows: to generate multicomponent fluxes of ions of various metals deposited on the substrate, we used a multiphase composite cathode on one gun of the vacuum setup and a single-phase titanium cathode on the other gun. In the process of simultaneous sputtering of different cathodes, metal ions are mixed in the plasma and, after deposition, form a coating. However, the mechanism for the formation of coatings with high hardness remains unclear and research in this area is just beginning to be carried out.
Conclusions and further research prospects.
From the above experimental data, it follows that when the coatings are applied for 40 minutes, coatings with a thickness of (1-1.5) microns are formed. Elemental analysis showed a high Cr content in the Cr-Mn-Si-Cu-Fe-Al coating in a nitrogen gas atmosphere -89.09%. The 12X18H10T + Ti coating in a nitrogen gas atmosphere contains 73% Ti, and the 12X18H10T + Ti coating in an argon gas atmosphere has a high Fe content of 64.96%.
In the first and second coatings, as a result of ionplasma treatment, nitrides were formed, which justifies the increase in their nanohardness. In the third coating,
the nanohardness increased insignificantly relative to the nanohardness of the substrate.
Thanks
The work was carried out with the financial support of the Ministry of Education and Science of the Republic of Kazakhstan. Grants 0118RK000063 and F.0781.
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