RU2606690C2 - Method of amorphous silicon coating producing on metal substrate internal surface - Google Patents
Method of amorphous silicon coating producing on metal substrate internal surface Download PDFInfo
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- RU2606690C2 RU2606690C2 RU2015128392A RU2015128392A RU2606690C2 RU 2606690 C2 RU2606690 C2 RU 2606690C2 RU 2015128392 A RU2015128392 A RU 2015128392A RU 2015128392 A RU2015128392 A RU 2015128392A RU 2606690 C2 RU2606690 C2 RU 2606690C2
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- gas
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- silicon
- internal surface
- coating
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- 239000000758 substrate Substances 0.000 title claims abstract description 23
- 238000000576 coating method Methods 0.000 title claims abstract description 18
- 239000011248 coating agent Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000002184 metal Substances 0.000 title claims abstract description 6
- 229910021417 amorphous silicon Inorganic materials 0.000 title claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 30
- 239000011261 inert gas Substances 0.000 claims abstract description 12
- 239000012686 silicon precursor Substances 0.000 claims abstract description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 10
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 229910052990 silicon hydride Inorganic materials 0.000 claims abstract description 9
- 229910052786 argon Inorganic materials 0.000 claims abstract description 5
- 239000001307 helium Substances 0.000 claims abstract description 5
- 229910052734 helium Inorganic materials 0.000 claims abstract description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000012159 carrier gas Substances 0.000 claims abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 4
- 239000011707 mineral Substances 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 238000007664 blowing Methods 0.000 claims abstract description 3
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003345 natural gas Substances 0.000 abstract description 4
- 239000003921 oil Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000003908 quality control method Methods 0.000 abstract description 3
- 238000005259 measurement Methods 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 230000004913 activation Effects 0.000 abstract 1
- -1 for example Substances 0.000 abstract 1
- 239000003915 liquefied petroleum gas Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000010410 layer Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 101100160821 Bacillus subtilis (strain 168) yxdJ gene Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
Настоящее изобретение относится к способу защиты поверхности металлических изделий от коррозии путем нанесения слоя аморфного кремния и может быть использовано в газоносных системах отбора и хранения проб природного газа для подготовки субстрата (сосуда для хранения газа и подводящего трубопровода) в системах контроля качества продукции в нефтяной и газовой промышленности, в коммерческих узлах учета, в системах измерений количества и показателей качества газа и сжиженных углеводородных газов на магистральных газопроводах.The present invention relates to a method for protecting the surface of metal products from corrosion by applying a layer of amorphous silicon and can be used in gas-bearing systems for sampling and storing natural gas samples for preparing a substrate (gas storage vessel and supply pipe) in product quality control systems in oil and gas industry, in commercial metering stations, in systems for measuring the quantity and quality indicators of gas and liquefied hydrocarbon gases in main gas pipelines.
Известен способ пассивации внутренней поверхности газосборного сосуда для защиты поверхности от коррозии, при котором внутреннюю поверхность сосуда сначала обезвоживают, затем сосуд вакуумируют, вводят газ, содержащий гидрид кремния, сосуд с газом нагревают под давлением, при этом газ разлагается на составные части и слой кремния осаждается на внутренней поверхности сосуда. Продолжительность осаждения кремния контролируют, чтобы предотвратить образование пыли кремния в сосуде. Сосуд затем продувают инертным газом для удаления газа, содержащего гидрид кремния. Операцию совершают в несколько циклов, пока вся поверхность сосуда не покроется кремнием. Сосуд опорожняют и охлаждают до комнатной температуры. (Патент US на изобретение №6,511,760, МПК7B65D 85/00, опубл. 28.01.2003 г.) [1].A known method of passivation of the inner surface of the gas collection vessel to protect the surface from corrosion, in which the inner surface of the vessel is first dehydrated, then the vessel is evacuated, gas containing silicon hydride is introduced, the vessel with gas is heated under pressure, and the gas decomposes into its constituent parts and the silicon layer is deposited on the inner surface of the vessel. The duration of silicon deposition is controlled to prevent the formation of silicon dust in the vessel. The vessel is then purged with an inert gas to remove a gas containing silicon hydride. The operation is performed in several cycles until the entire surface of the vessel is covered with silicon. The vessel is emptied and cooled to room temperature. (US patent for the invention No. 6,511,760, IPC 7 B65D 85/00, published on January 28, 2003) [1].
Недостатком этого способа является отсутствие стадии первичной подготовки сосуда, что негативно сказывается на качестве и воспроизводимости полученного покрытия, заполнение сосуда чистым гидридом кремния повышает стоимость операции, а его использование на продувку линий вызывает выброс непрореагировавшего токсичного сырья, что ухудшает экологическую обстановку.The disadvantage of this method is the lack of a stage of primary preparation of the vessel, which negatively affects the quality and reproducibility of the resulting coating, filling the vessel with pure silicon hydride increases the cost of the operation, and its use for purging the lines causes the release of unreacted toxic raw materials, which worsens the environmental situation.
Известен способ пассивации внутренней поверхности реактора, подвергаемого закоксовыванию, и реактор, при котором покрытие поверхности получают посредством термического разложения металлоорганического соединения кремния, не содержащего кислород и воду, в инертной среде, выбранной из группы, состоящей из аргона, гелия, их смесей, азота, водорода. (Патент RU на изобретение №2079569, МПК С23С 8/28, опубл. 20.05.1997 г.), [2], (прототип способа).A known method of passivation of the inner surface of the reactor subjected to coking, and a reactor in which a surface coating is obtained by thermal decomposition of an organometallic compound of silicon, which does not contain oxygen and water, in an inert medium selected from the group consisting of argon, helium, mixtures thereof, nitrogen, hydrogen. (RU patent for the invention No. 2079569, IPC С23С 8/28, publ. 05/20/1997), [2], (prototype method).
Недостатком этого способа является отсутствие стадии первичной обработки внутренней поверхности реактора, что ведет к слабой адгезии и отслаиванию покрытия. Покрытие, полученное данным способом, имеет черный цвет и липкое, что затрудняет очистку реактора.The disadvantage of this method is the lack of a stage of primary processing of the inner surface of the reactor, which leads to poor adhesion and peeling of the coating. The coating obtained by this method is black and sticky, which makes it difficult to clean the reactor.
Техническим результатом данного изобретения является повышение качества покрытия при снижении затрат.The technical result of this invention is to improve the quality of the coating while reducing costs.
Технический результат достигается способом получения покрытия из аморфного кремния на внутренней поверхности металлического субстрата, включающим очистку внутренней поверхности субстрата органическим растворителем и активирование ее раствором минеральной кислоты или щелочи, подачу в субстрат прекурсора кремния в виде гидрида кремния в количестве от 5 об. % до 30 об. % при смешивании с инертным газом в виде аргона, гелия, их смесей или азота и разложение гидрида кремния при температуре от 600°С до 1000°С в течение от 3 до 240 минут, при этом подачу прекурсора кремния в субстрат повторяют до достижения требуемой толщины покрытия с промежуточной продувкой субстрата инертным газом, а смесь газов, получаемую после проведения реакции разложения, используют повторно в качестве газа-носителя.The technical result is achieved by a method of obtaining a coating of amorphous silicon on the inner surface of a metal substrate, including cleaning the inner surface of the substrate with an organic solvent and activating it with a solution of mineral acid or alkali, feeding the silicon precursor in the form of silicon hydride in an amount of 5 vol. % up to 30 vol. % when mixed with an inert gas in the form of argon, helium, mixtures thereof or nitrogen and the decomposition of silicon hydride at a temperature of from 600 ° C to 1000 ° C for 3 to 240 minutes, while feeding the silicon precursor to the substrate is repeated until the desired thickness is reached coatings with intermediate blowing of the substrate with an inert gas, and the gas mixture obtained after the decomposition reaction is reused as a carrier gas.
Сущность изобретения заключается в том, что, в отличие от прототипа, внутреннюю поверхность субстрата очищают органическим растворителем и активируют раствором минеральной кислоты или щелочи, что повышает адгезию кремния, смешанного с инертным газом в виде аргона, гелия, их смесей или азота, выпадающего в процессе термического разложения прекурсора кремния на внутреннюю поверхность субстрата, при этом полученное покрытие обладает высоким значением краевого угла смачивания, прочно и устойчиво к механическому воздействию, что в свою очередь повышает достоверность измерения содержания воды в системах измерения влажности газа. Повторная подача прекурсора кремния в субстрат обеспечивает нанесение покрытия требуемой толщины. Повторное использование смеси газов, получаемой после проведения реакции разложения прекурсора кремния, в качестве газа-носителя снижает затраты на операцию покрытия внутренней поверхности субстрата.The essence of the invention lies in the fact that, unlike the prototype, the inner surface of the substrate is cleaned with an organic solvent and activated with a solution of mineral acid or alkali, which increases the adhesion of silicon mixed with an inert gas in the form of argon, helium, their mixtures or nitrogen falling out during the process thermal decomposition of the silicon precursor on the inner surface of the substrate, while the resulting coating has a high value of the wetting angle, is strong and resistant to mechanical stress, which in turn Reduces the reliability of measuring water content in gas moisture measuring systems. Re-feeding the silicon precursor to the substrate provides coating of the desired thickness. Reuse of the gas mixture obtained after the decomposition reaction of the silicon precursor as a carrier gas reduces the cost of the operation of coating the inner surface of the substrate.
Пример.Example.
Способ осаждения кремния на внутреннюю поверхность субстрата заключается в следующем. Субстрат - баллон для отбора пробы газа, очищали от механического загрязнения раствором 1М HCl, затем промывали дистиллированной водой и обезжиривали этиловым спиртом, после чего снова промывали водой и сушили сжатым воздухом при комнатной температуре. Очищенный сухой баллон подключали с помощью быстроразъемных соединений к системе подачи газа-модификатора и помещали в печь. Печь нагревали до 600°С, пропуская через баллон поток инертного газа. При достижении заданной температуры автоматическим дозатором вводили в поток инертного газа прекурсор кремния с объемным соотношением: инертный газ / прекурсор кремния, как 7/2, после чего баллон отсекали от системы подачи газа-модификатора и проводили реакцию разложения прекурсора кремния - выдерживали баллон при указанной температуре и установившемся давлении газа-модификатора около пяти минут. По истечении пяти минут баллон соединяли с системой подачи инертного газа и продували. Процесс повторяли 4 раза для получения покрытия толщиной 400 нм. Полученное покрытие резко снизило способность внутренней поверхности баллона смачиваться водой и водными растворами.The method of deposition of silicon on the inner surface of the substrate is as follows. The substrate, a gas sampling bottle, was cleaned of mechanical pollution with a solution of 1 M HCl, then it was washed with distilled water and degreased with ethanol, then it was again washed with water and dried with compressed air at room temperature. The cleaned dry balloon was connected using quick disconnect connections to the modifier gas supply system and placed in an oven. The furnace was heated to 600 ° C, passing a stream of inert gas through a balloon. When the set temperature is reached, an automatic dispenser introduced a silicon precursor into the inert gas stream with a volume ratio of inert gas / silicon precursor as 7/2, after which the cylinder was cut off from the modifier gas supply system and the decomposition of the silicon precursor decomposition was carried out - the cylinder was kept at the indicated temperature and steady-state modifier gas pressure for about five minutes. After five minutes, the balloon was connected to an inert gas supply system and purged. The process was repeated 4 times to obtain a coating 400 nm thick. The resulting coating sharply reduced the ability of the inner surface of the container to be wetted by water and aqueous solutions.
Предлагаемое изобретение повышает качество защитного слоя покрытия и может найти применение в устройствах подготовки сосуда для хранения пробы природного газа и газоподводящего трубопровода при отборе пробы природного газа в системах контроля качества продукции в нефтяной и газовой промышленности в коммерческих узлах учета, в системах измерений количества и показателей качества газа и сжиженных углеводородных газов на магистральных газопроводах.The present invention improves the quality of the protective coating layer and can be used in vessel preparation devices for storing natural gas samples and gas supply pipelines for sampling natural gas in product quality control systems in the oil and gas industry in commercial metering stations, in quantity and quality measurement systems gas and liquefied hydrocarbon gases in gas pipelines.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2661320C1 (en) * | 2017-04-26 | 2018-07-13 | Закрытое акционерное общество Научно-инженерный центр "ИНКОМСИСТЕМ" | Method of substrate hydrophobisation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2650381C1 (en) * | 2016-12-12 | 2018-04-11 | федеральное государственное бюджетное образовательное учреждение высшего образования "Омский государственный университет им. Ф.М. Достоевского" | Method of forming amorphous silicon thin films |
| DE202017002044U1 (en) | 2017-04-18 | 2017-05-09 | Closed Joint Stock Company Research-Engineering Center "INCOMSYSTEM" | Device for passivating the surface of long pipes during inductive heating |
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| US4664938A (en) * | 1985-05-06 | 1987-05-12 | Phillips Petroleum Company | Method for deposition of silicon |
| RU2079569C1 (en) * | 1991-10-28 | 1997-05-20 | ЭНИКЕМ С.п.А. | Method of passivation of inner surface or reactor subjected to coking, and reactor |
| US6258173B1 (en) * | 1998-01-29 | 2001-07-10 | Nissin Electric Co. Ltd. | Film forming apparatus for forming a crystalline silicon film |
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| US20090029178A1 (en) * | 2004-12-13 | 2009-01-29 | Smith David A | Process for the modification of substrate surfaces through the deposition of amorphous silicon layers followed by surface functionalization with organic molecules and functionalized structures |
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- 2015-07-13 RU RU2015128392A patent/RU2606690C2/en active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4664938A (en) * | 1985-05-06 | 1987-05-12 | Phillips Petroleum Company | Method for deposition of silicon |
| RU2079569C1 (en) * | 1991-10-28 | 1997-05-20 | ЭНИКЕМ С.п.А. | Method of passivation of inner surface or reactor subjected to coking, and reactor |
| RU2189663C2 (en) * | 1997-06-30 | 2002-09-20 | Мацушита Электрик Индастриал Ко., Лтд. | Method and device for producing thin semiconductor film |
| US6258173B1 (en) * | 1998-01-29 | 2001-07-10 | Nissin Electric Co. Ltd. | Film forming apparatus for forming a crystalline silicon film |
| US20090029178A1 (en) * | 2004-12-13 | 2009-01-29 | Smith David A | Process for the modification of substrate surfaces through the deposition of amorphous silicon layers followed by surface functionalization with organic molecules and functionalized structures |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2661320C1 (en) * | 2017-04-26 | 2018-07-13 | Закрытое акционерное общество Научно-инженерный центр "ИНКОМСИСТЕМ" | Method of substrate hydrophobisation |
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| Publication number | Publication date |
|---|---|
| RU2015128392A (en) | 2016-01-10 |
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