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  • 1.
    Huang, Jing-Jia
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Militzer, Christian
    SGL Carbon GmbH, Germany.
    Wijayawardhana, Charles
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Forsberg, Urban
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Pedersen, Henrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Superconformal silicon carbide coatings via precursor pulsed chemical vapor deposition2023Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 41, nr 3, artikel-id 030403Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    In this work, silicon carbide (SiC) coatings were successfully grown by pulsed chemical vapor deposition (CVD). The precursors silicon tetrachloride (SiCl4) and ethylene (C2H4) were not supplied in a continuous flow but were pulsed alternately into the growth chamber with H-2 as a carrier and a purge gas. A typical pulsed CVD cycle was SiCl4 pulse-H-2 purge-C2H4 pulse-H-2 purge. This led to growth of superconformal SiC coatings, which could not be obtained under similar process conditions using a constant flow CVD process. We propose a two-step framework for SiC growth via pulsed CVD. During the SiCl4 pulse, a layer of Si is deposited. In the following C2H4 pulse, this Si layer is carburized, and SiC is formed. The high chlorine surface coverage after the SiCl4 pulse is believed to enable superconformal growth via a growth inhibition effect.

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  • 2.
    Huang, Jing-Jia
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Militzer, Christian
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Halvledarmaterial. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Wijayawardhana, Charles
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Forsberg, Urban
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Pedersen, Henrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Conformal and superconformal chemical vapor deposition of silicon carbide coatings2022Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 40, nr 5, artikel-id 053402Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    The approaches to conformal and superconformal deposition developed by Abelson and Girolami for a low-temperature, low-pressure chemical vapor deposition (CVD) setting relevant for electronic materials in micrometer or submicrometer scale vias and trenches, are tested here in a high-temperature, moderate pressure CVD setting relevant for hard coatings in millimeter-scale trenches. Conformal and superconformal deposition of polycrystalline silicon carbide (SiC) can be accomplished at deposition temperatures between 950 and 1000 degrees C with precursor partial pressure higher than 20 Pa and an optional minor addition of HCl as a growth inhibitor. The conformal deposition at low temperatures is ascribed to slower kinetics of the precursor consumption along the trench depth, whereas the impact of high precursor partial pressure and addition of inhibitor is attributable to surface site blocking. With the slower kinetics and the site blocking from precursor saturation leading the growth to nearly conformal and the possibly preferential inhibition effect near the opening than at the depth, a superconformal SiC coating with 2.6 times higher thickness at the bottom compared to the top of a 1 mm trench was achieved. Published under an exclusive license by the AVS.

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  • 3.
    Huang, Jing-Jia
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Militzer, Christian
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Halvledarmaterial. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Germany.
    Wijayawardhana, Charles
    SGL Carbon GmbH, Germany.
    Forsberg, Urban
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Ojamäe, Lars
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Pedersen, Henrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Controlled CVD Growth of Highly ⟨111⟩-Oriented 3C-SiC2022Ingår i: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 126, nr 23, s. 9918-9925Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    Highly ⟨111⟩-oriented 3C-SiC coatings with a distinct surface morphology consisting of hexagonally shaped pyramidal crystals were prepared by chemical vapor deposition (CVD) using silicon tetrachloride (SiCl4) and toluene (C7H8) at T ≤ 1250 °C and ptot = 10 kPa. In contrast, similar deposition conditions, with methane (CH4) as the carbon precursor, resulted in randomly oriented 3C-SiC coatings with a cauliflower-like surface of SiC crystallites. No excess carbon was detected in the highly ⟨111⟩-oriented 3C-SiC samples despite the use of aromatic hydrocarbons. The difference in the preferred growth orientation of the 3C-SiC coatings deposited by using C7H8 and CH4 as the carbon precursors was explained via quantum chemical calculations of binding energies on various crystal planes. The adsorption energy of C6H6 on the SiC (111) plane was 6 times higher than that on the (110) plane. On the other hand, CH3 exhibited equally strong adsorption on both planes. This suggested that the highly ⟨111⟩-oriented 3C-SiC growth with C7H8 as the carbon precursor, where both C6H6 and CH3 were considered the main active carbon-containing film forming species, was due to the highly preferred adsorption on the (111) plane, while the lower surface energy of the (110) plane controlled the growth orientation in the CH4 process, in which only CH3 contributed to the film deposition. 

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  • 4.
    Huang, Jing-Jia
    et al.
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Bonn, Germany.
    Militzer, Christian
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Halvledarmaterial. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Bonn, Germany.
    Xu, Jinghao
    Linköpings universitet, Institutionen för ekonomisk och industriell utveckling, Konstruktionsmaterial. Linköpings universitet, Tekniska fakulteten.
    Wijayawardhana, Charles
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten. SGL Carbon GmbH, Bonn, Germany.
    Forsberg, Urban
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Halvledarmaterial. Linköpings universitet, Tekniska fakulteten.
    Pedersen, Henrik
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Kemi. Linköpings universitet, Tekniska fakulteten.
    Growth of silicon carbide multilayers with varying preferred growth orientation2022Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 447, artikel-id 128853Artikel i tidskrift (Refereegranskat)
    Abstract [en]

    SiC multilayer coatings were deposited via thermal chemical vapor deposition (CVD) using silicon tetrachloride (SiCl4) and various hydrocarbons under identical growth conditions, i.e. at 1100 °C and 10 kPa. The coatings consisted of layers whose preferred growth orientation alternated between random and highly 〈111〉-oriented. The randomly oriented layers were prepared with either methane (CH4) or ethylene (C2H4) as carbon precursor, whereas the highly 〈111〉-oriented layers were grown utilizing toluene (C7H8) as carbon precursor. In this work, we demonstrated how to fabricate multilayer coatings with different growth orientations by merely switching between hydrocarbons. Moreover, the success in depositing multilayer coatings on both flat and structured graphite substrates has strengthened the assumption proposed in our previous study that the growth of highly 〈111〉-oriented SiC coatings using C7H8 was primarily driven by chemical surface reactions.

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  • 5. Beställ onlineKöp publikationen >>
    Huang, Jing-Jia
    Linköpings universitet, Institutionen för fysik, kemi och biologi, Tunnfilmsfysik. Linköpings universitet, Tekniska fakulteten.
    Surface-Controlled Chemical Vapor Deposition of Silicon Carbide2022Doktorsavhandling, sammanläggning (Övrigt vetenskapligt)
    Abstract [en]

    Polycrystalline cubic silicon carbide, 3C-SiC, has long been investigated in the field of hard coating materials. The typical synthesis method for 3C-SiC coatings is thermal chemical vapor deposition (CVD) using either multicomponent precursors, e.g. methyltrichlorosilane, or a combination of single component precursors, e.g. silane and propane. In this thesis, the fabrication of polycrystalline SiC coatings has been explored from the new aspects on the basis of thermal CVD utilizing silicon tetrachloride (SiCl4) and various hydrocarbons, i.e. toluene (C7H8), methane (CH4) and ethylene (C2H4) as the precursors. The goal of this thesis is to control the surface chemistry in the SiCl4-based SiC CVD and has been accomplished by the following three different approaches: 

    In the first approach to control the surface chemistry of SiC CVD, the difference in the adsorption energy of aromatic and aliphatic hydrocarbons on different SiC crystal planes was utilized. Under identical deposition conditions, a highly <111>-oriented 3C-SiC coating was deposited using C7H8 as the carbon precursor, whereas using CH4 resulted in a randomly oriented 3C-SiC. The results from quantum chemical calculation showed that the active film forming carbon species, i.e. C6H6 in the C7H8 process and CH3 in both C7H8 and CH4 processes, behaved differently when they adsorbed on the 3C-SiC (111) and (110) planes. CH3 is strongly chemisorbed on both planes, while C6H6 is chemisorbed on the (111) plane, but only physiosorbed on the other. The significant difference in the adsorption energy of CH3 and C6H6 on the (111) and (110) planes therefore explains the resulting highly <111>-oriented 3C-SiC from the C7H8 process. Furthermore, the ability to deposit 3C-SiC coatings with alternating highly <111>- and randomly oriented layers by merely switching the carbon precursor between C7H8 and CH4 or C2H4 in a single CVD deposition has further proven that the effect of aromatic hydrocarbons on the preferred growth orientation of 3C-SiC was controlled primarily by the surface chemistry.  

    The second approach to the surface-controlled SiC CVD was based on the reduction of surface reaction probability (β) for conformal film growth via low-temperature, low-pressure CVD, which was originally proposed by Abelson and Girolami. Their strategies in reducing β, including lowering the temperature and increasing the precursor partial pressure, were successfully adapted to the SiC CVD growth using SiCl4 and C2H4 as the precursors in this thesis, where an elevated temperature and a moderate pressure were used. Moreover, the addition of Cl species as a growth inhibitor to the process further reduced the β, leading to a superconformal SiC growth.  

    The third approach employed in this thesis for the SiC growth was pulsed CVD. Instead of a continuous and simultaneous SiCl4 and C2H4 flow, the precursors were pulsed alternately into the chamber with each precursor pulse being separated by a H2 purge. In this precursor delivery mode, the gas phase reactions between SiCl4 and C2H4 were avoided and hence the SiC growth was mostly controlled by the surface chemistry. Altering the pulse durations of the precursors led to a variation of growth per cycle (GPC), which was explained by a two-step mechanism. During the SiCl4 pulse, a thin layer of Si is deposited, which is carburized by carbon species produced during the C2H4 pulse. Additionally, the separation of precursor pulses should lead to a large increase in the surface coverage of Cl species, further enhancing the inhibition effect and resulting in a superconformal SiC growth. By using this approach, superconformal SiC coatings were achieved at temperatures where conventional CVD only yielded nonconformal SiC coatings. The observed decline in coating conformality with an elongated purge implied that more surface Cl species were replaced by H during the H2 purge and consequently the inhibition effect was diminished. 

    Delarbeten
    1. Controlled CVD Growth of Highly ⟨111⟩-Oriented 3C-SiC
    Öppna denna publikation i ny flik eller fönster >>Controlled CVD Growth of Highly ⟨111⟩-Oriented 3C-SiC
    Visa övriga...
    2022 (Engelska)Ingår i: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 126, nr 23, s. 9918-9925Artikel i tidskrift (Refereegranskat) Published
    Abstract [en]

    Highly ⟨111⟩-oriented 3C-SiC coatings with a distinct surface morphology consisting of hexagonally shaped pyramidal crystals were prepared by chemical vapor deposition (CVD) using silicon tetrachloride (SiCl4) and toluene (C7H8) at T ≤ 1250 °C and ptot = 10 kPa. In contrast, similar deposition conditions, with methane (CH4) as the carbon precursor, resulted in randomly oriented 3C-SiC coatings with a cauliflower-like surface of SiC crystallites. No excess carbon was detected in the highly ⟨111⟩-oriented 3C-SiC samples despite the use of aromatic hydrocarbons. The difference in the preferred growth orientation of the 3C-SiC coatings deposited by using C7H8 and CH4 as the carbon precursors was explained via quantum chemical calculations of binding energies on various crystal planes. The adsorption energy of C6H6 on the SiC (111) plane was 6 times higher than that on the (110) plane. On the other hand, CH3 exhibited equally strong adsorption on both planes. This suggested that the highly ⟨111⟩-oriented 3C-SiC growth with C7H8 as the carbon precursor, where both C6H6 and CH3 were considered the main active carbon-containing film forming species, was due to the highly preferred adsorption on the (111) plane, while the lower surface energy of the (110) plane controlled the growth orientation in the CH4 process, in which only CH3 contributed to the film deposition. 

    Ort, förlag, år, upplaga, sidor
    American Chemical Society (ACS), 2022
    Nationell ämneskategori
    Fysikalisk kemi
    Identifikatorer
    urn:nbn:se:liu:diva-186829 (URN)10.1021/acs.jpcc.2c01171 (DOI)000813434000001 ()
    Anmärkning

    Funding Agencies|SGL CARBON GmbH; Swedish Research Council (VR)

    Tillgänglig från: 2022-07-05 Skapad: 2022-07-05 Senast uppdaterad: 2022-10-27
    2. Growth of silicon carbide multilayers with varying preferred growth orientation
    Öppna denna publikation i ny flik eller fönster >>Growth of silicon carbide multilayers with varying preferred growth orientation
    Visa övriga...
    2022 (Engelska)Ingår i: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347, Vol. 447, artikel-id 128853Artikel i tidskrift (Refereegranskat) Published
    Abstract [en]

    SiC multilayer coatings were deposited via thermal chemical vapor deposition (CVD) using silicon tetrachloride (SiCl4) and various hydrocarbons under identical growth conditions, i.e. at 1100 °C and 10 kPa. The coatings consisted of layers whose preferred growth orientation alternated between random and highly 〈111〉-oriented. The randomly oriented layers were prepared with either methane (CH4) or ethylene (C2H4) as carbon precursor, whereas the highly 〈111〉-oriented layers were grown utilizing toluene (C7H8) as carbon precursor. In this work, we demonstrated how to fabricate multilayer coatings with different growth orientations by merely switching between hydrocarbons. Moreover, the success in depositing multilayer coatings on both flat and structured graphite substrates has strengthened the assumption proposed in our previous study that the growth of highly 〈111〉-oriented SiC coatings using C7H8 was primarily driven by chemical surface reactions.

    Ort, förlag, år, upplaga, sidor
    Elsevier, 2022
    Nyckelord
    Silicon carbide, Preferred growth orientation, Chemical vapor deposition, Multilayer, Toluene
    Nationell ämneskategori
    Materialkemi
    Identifikatorer
    urn:nbn:se:liu:diva-189572 (URN)10.1016/j.surfcoat.2022.128853 (DOI)000863260100006 ()
    Anmärkning

    Funding: SGL Carbon GmbH

    Tillgänglig från: 2022-10-27 Skapad: 2022-10-27 Senast uppdaterad: 2022-11-08Bibliografiskt granskad
    3. Conformal and superconformal chemical vapor deposition of silicon carbide coatings
    Öppna denna publikation i ny flik eller fönster >>Conformal and superconformal chemical vapor deposition of silicon carbide coatings
    Visa övriga...
    2022 (Engelska)Ingår i: Journal of Vacuum Science & Technology. A. Vacuum, Surfaces, and Films, ISSN 0734-2101, E-ISSN 1520-8559, Vol. 40, nr 5, artikel-id 053402Artikel i tidskrift (Refereegranskat) Published
    Abstract [en]

    The approaches to conformal and superconformal deposition developed by Abelson and Girolami for a low-temperature, low-pressure chemical vapor deposition (CVD) setting relevant for electronic materials in micrometer or submicrometer scale vias and trenches, are tested here in a high-temperature, moderate pressure CVD setting relevant for hard coatings in millimeter-scale trenches. Conformal and superconformal deposition of polycrystalline silicon carbide (SiC) can be accomplished at deposition temperatures between 950 and 1000 degrees C with precursor partial pressure higher than 20 Pa and an optional minor addition of HCl as a growth inhibitor. The conformal deposition at low temperatures is ascribed to slower kinetics of the precursor consumption along the trench depth, whereas the impact of high precursor partial pressure and addition of inhibitor is attributable to surface site blocking. With the slower kinetics and the site blocking from precursor saturation leading the growth to nearly conformal and the possibly preferential inhibition effect near the opening than at the depth, a superconformal SiC coating with 2.6 times higher thickness at the bottom compared to the top of a 1 mm trench was achieved. Published under an exclusive license by the AVS.

    Ort, förlag, år, upplaga, sidor
    A V S AMER INST PHYSICS, 2022
    Nationell ämneskategori
    Tribologi (ytteknik omfattande friktion, nötning och smörjning)
    Identifikatorer
    urn:nbn:se:liu:diva-187711 (URN)10.1116/6.0001909 (DOI)000838416200001 ()
    Anmärkning

    Funding Agencies|SGL CARBON GmbH

    Tillgänglig från: 2022-08-29 Skapad: 2022-08-29 Senast uppdaterad: 2022-10-27
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