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WO2025093450A1 - Diamant monocristallin cvd - Google Patents

Diamant monocristallin cvd Download PDF

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Publication number
WO2025093450A1
WO2025093450A1 PCT/EP2024/080313 EP2024080313W WO2025093450A1 WO 2025093450 A1 WO2025093450 A1 WO 2025093450A1 EP 2024080313 W EP2024080313 W EP 2024080313W WO 2025093450 A1 WO2025093450 A1 WO 2025093450A1
Authority
WO
WIPO (PCT)
Prior art keywords
diamond
single crystal
crystal diamond
cvd single
less
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/EP2024/080313
Other languages
English (en)
Inventor
David William HARDEMAN
Gruffudd Trefor WILLIAMS
Daniel Edward FIELD
Adam RATHMILL
Michael Ian PEARSON
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Element Six Technologies Ltd
Original Assignee
Element Six Technologies Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from GB2316754.7A external-priority patent/GB2638116A/en
Application filed by Element Six Technologies Ltd filed Critical Element Six Technologies Ltd
Publication of WO2025093450A1 publication Critical patent/WO2025093450A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02—Elements
    • C30B29/04—Diamond
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B7/00—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor
    • B24B7/20—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground
    • B24B7/22—Machines or devices designed for grinding plane surfaces on work, including polishing plane glass surfaces; Accessories therefor characterised by a special design with respect to properties of the material of non-metallic articles to be ground for grinding inorganic material, e.g. stone, ceramics, porcelain
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • C30B25/20—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer
    • C30B25/205—Epitaxial-layer growth characterised by the substrate the substrate being of the same materials as the epitaxial layer the substrate being of insulating material
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure

Definitions

  • the invention relates to the field of CVD single crystal diamond, and to methods of processing CVD single crystal diamond.
  • Diamond materials may be categorized into three main types: natural diamond materials; HPHT (high pressure high temperature) synthetic diamond materials, and CVD (chemical vapour deposited) synthetic diamond materials. These categories reflect the way in which the diamond materials are formed. Furthermore, these categories reflect the structural and functional characteristics of the materials. This is because while natural, HPHT synthetic, and CVD synthetic diamond materials are all based on a theoretically perfect diamond lattice the defects in these materials are not the same. For example, CVD synthetic diamond contains many defects unique to the process of CVD, and whilst some defects are found in other diamond forms, their relative concentration and contribution is very different. As such, CVD synthetic diamond materials are different to both natural and HPHT synthetic diamond materials.
  • Diamond materials may also be categorized according to their physical form.
  • diamond materials may be categorized into three main types: single crystal diamond materials; polycrystalline diamond materials; and composite diamond materials.
  • Single crystal diamond materials are in the form of individual single crystals of various sizes ranging from small “grit” particles used in abrasive applications through to large single crystals suitable for use in a variety of technical applications as well for gemstones in jewellery applications.
  • Polycrystalline diamond materials are in the form of a plurality of small diamond crystals bonded together by diamond-to-diamond bonding to form a polycrystalline body of diamond material such as a polycrystalline diamond wafer.
  • Such polycrystalline diamond materials can be useful in various applications including thermal management substrates, optical windows, and mechanical applications.
  • Composite diamond materials are generally in the form of a plurality of small diamond crystals bonded together by diamond-to-diamond or a non-diamond matrix to form a body of composite material.
  • Various diamond composites are known including diamond containing metal matrix composites, particularly cobalt metal matrix composites known as polycrystalline diamond (PCD), and skeleton cemented diamond (ScD) which is a composite comprising silicon, silicon carbide, and diamond particles.
  • PCD polycrystalline diamond
  • ScD skeleton cemented diamond
  • CVD processes for synthesis of diamond material are well known. Being in the region where diamond is metastable compared to graphite, synthesis of diamond under CVD conditions is driven by surface kinetics and not bulk thermodynamics. Diamond synthesis by CVD is normally performed using a small fraction of carbon (typically ⁇ 5%), in the form of a carbon containing gases, in an excess of molecular hydrogen. If molecular hydrogen is heated to temperatures in excess of 2000 K, there is a significant dissociation to atomic hydrogen. In the presence of a suitable substrate material, CVD synthetic diamond material can be deposited. Polycrystalline CVD diamond material may be formed on a non-diamond substrate such as a refractory metal or silicon substrate. Single crystal CVD synthetic diamond material may be formed by homoepitaxial growth on a single crystal diamond substrate.
  • Atomic hydrogen present in the process selectively etches off non-diamond carbon from the substrate such that diamond growth can occur.
  • Various methods are available for heating carbon containing gas species and molecular hydrogen in order to generate the reactive carbon containing radicals and atomic hydrogen required for CVD synthetic diamond growth including arc-jet, hot filament, DC arc, oxy-acetylene flame, and microwave plasma.
  • a problem with prior art methodologies is how to achieve large area single crystal CVD synthetic diamond material. It has been found that large area single crystal diamond can be grown by a process known as “heteroepitaxial growth”. This is where diamond nucleates and grows epitaxially on a non-diamond substrate. Iridium has been found to be a suitable substrate to allow diamond nucleation and growth, but other substrates such as silicon, silicon carbide, copper, nickel, rhenium and titanium carbide have been investigated. US 7,396,408 describes such a process. In this case, diamond is grown in a CVD process using a silicon carbide, sapphire, or silicon single crystal wafer that has a layer of iridium deposited on its surface.
  • This is used as a substrate on which to heteroepitaxially deposit and grow diamond.
  • diamond crystallites nucleate on the iridium film. These crystallites grow and merge to form a single crystal layer, which is continued until a single crystal diamond wafer of the desired thickness is formed.
  • the dislocation density reduces via dislocation interactions (fusion and annihilation) as growth proceeds, leading to a single crystal diamond wafer that has a higher dislocation density adjacent to the original nucleation face compared to the growth face.
  • diamond surfaces are prepared by scaife polishing, a technique in which the diamond surface is brought into contact with a rotating iron or iron-based disc and pressure applied. Further surface processing often includes an oxygen plasma etch.
  • a problem with scaife polishing is that it is only suitable for single crystal diamond with relatively small dimensions.
  • a problem with oxygen plasma etching is while it can reduce sub-surface damage, it can increase the roughness of the surface.
  • An object of the invention is to provide a CVD single crystal diamond with a relatively large surface area and a relatively low surface roughness.
  • a method of processing a CVD single crystal diamond comprising: providing a CVD single crystal diamond with a minimum lateral dimension of at least 20 mm, the CVD single crystal diamond further comprising a major surface; processing the major surface using a diamond-matrix wheel, the diamond-matrix wheel comprising embedded diamond particles embedded in a matrix.
  • the method further comprises applying a treatment to the major surface to reduce subsurface damage at the major surface without substantially increasing surface roughness.
  • the treatment comprises inductively couple plasma, ICP, etching.
  • the treatment comprises chemical mechanical polishing, CMP.
  • CMP chemical mechanical polishing
  • the diamond-matrix wheel optionally has a surface roughness of Ra of less than 2 pm.
  • the method optionally further comprises, prior to processing the major surface using the diamond-matrix wheel, conditioning the diamond-matrix wheel to control its surface roughness.
  • the conditioning optionally comprises using the diamond-matrix wheel to process a sacrificial part, the sacrificial part comprising a superhard material.
  • the superhard material optionally comprises any of diamond, polycrystalline diamond PCD, and polycrystalline cubic boron nitride.
  • the method optionally further comprises in a CVD reactor, homoepitaxially growing further diamond on the major surface of the CVD single crystal diamond.
  • a CVD single crystal diamond having a largest linear dimension of at least 20 mm and a major surface, the major surface having a surface roughness Sa of less than 1 nm over at least 90% of the major surface.
  • the surface roughness Sa is selected from any of less than 0.8 nm, less than 0.6 nm, less than 0.4 nm, and less than 0.2 nm.
  • the CVD single crystal diamond has a surface roughness Ra selected from any of less than 1 nm, less than 0.8 nm, less than 0.6 nm, less than 0.4 nm, and less than 0.2 nm.
  • the major surface has a surface roughness Sa of less than 1 nm an area of the major surface selected from any of least 95%, at least 98% and at least 99%.
  • the largest linear dimension is selected from any of at least 50 mm, at least 75 mm, at least 100 mm and at least 120 mm.
  • the CVD single crystal diamond optionally further has a thickness selected from any of at least 100 pm, at least 500 pm, at least 1 mm, at least 2 mm and at least 4 mm.
  • the major surface has an average surface dislocation density over at least 90% of the major surface selected from any of no more than 10 5 cm -2 , no more than 5 x 10 4 cm -2 , no more than 10 4 cm -2 , no more than 5 x 10 3 cm -2 and no more than 10 3 cm -2 .
  • the CVD single crystal diamond optionally further comprises a single substitutional nitrogen concentration as measured by electron paramagnetic resonance (EPR) of at least 1x10 13 atoms cm -3 and no more than 5x10 18 cnv 3 .
  • the single substitutional nitrogen concentration as measured by electron paramagnetic resonance (EPR) is at least 3x10 15 atoms cm -3 and no more than 5x10 17 cnv 3 .
  • the major surface of the CVD single crystal diamond is oriented within 10° of a ⁇ 100 ⁇ crystallographic plane.
  • the major surface of the CVD single crystal diamond is oriented within 10° of a ⁇ 111 ⁇ crystallographic plane.
  • the CVD single crystal diamond optionally displays SiV' luminescence, quantified by a ratio of a total peak area of the SiV' zero-phonon lines to a peak area of the first-order diamond Raman signal in a photoluminescence measurement performed at a temperature of 77 K using an excitation wavelength of 660 nm, selected from any of less than 1.0, less than 0.5; less than 0.1 ; less than 0.05; and less than 0.01.
  • the CVD single crystal diamond optionally comprises at least two discrete layers.
  • a device comprising the CVD single crystal diamond described above in the second aspect.
  • Figure 1 is a flow diagram illustrating exemplary steps in processing a CVD single crystal diamond
  • Figure 2 illustrates schematically a side elevation of a diamond-matrix wheel before and after wheel conditioning
  • Figures 3a and 3b are scanning electron micrographs showing a surface of a diamondmatrix wheel before and after wheel conditioning
  • Figures 4a and 4b are atomic force microscope, AFM, images of single crystal diamond with a processed surface
  • Figure 5 is an optical micrograph of a surface of a grown diamond showing surface defects.
  • Figure 1 is a flow diagram setting out exemplary steps. The following numbering corresponds to that of Figure 1 :
  • a CVD single crystal diamond is provided that has at least one lateral dimension of least 25 mm.
  • One way to achieve this is to heteroepitaxially grow diamond in a CVD process as described in US 7,396,408.
  • the largest linear dimension may be at least 50 mm, at least 75 mm, at least 100 mm and at least 120 mm. Such large areas can be achieved using heteroepitaxial growth, as described above, or any other techniques such as tiling a plurality of substrates together before growth.
  • Ra is an average surface roughness value, the mean deviation.
  • Rz is a measure of the maximum peak to valley height.
  • Rsk is a skewness parameter where positive values indicate a surface dominated by peaks and asperities, whilst a negative value is valley dominated.
  • Diamond grit particles are typically measured using the well-known mesh system by passing diamond grits through a series of screens with increasingly finer mesh sizes. Particles stopped by a screen of a particular mesh were measured by that mesh number. The mesh number can be easily converted to pm.
  • the 33 pm wheel was used to process a major surface of a CVD single crystal diamond having lateral dimensions of 30 x 30 mm and a thickness of 500 pm.
  • the processing was at a diamond-matrix wheel speed of between 1000 and 2000 rpm, and a load of between 10 kPa and 28 kPa for 48 hours.
  • Figures 4a and 4b show AFM, images of the CVD single crystal diamond with a processed surface.
  • Figure 4a shows the surface of a CVD single crystal diamond processed using a standard 76 pm diamond-matrix wheel. The roughness Sa of the major surface of the CVD single crystal diamond was found to be under 1 nm.
  • Figure 4b shows the surface of a CVD single crystal diamond processed using a conditioned 33 pm diamond-matrix wheel. The roughness Sa of the major surface of the CVD single crystal diamond was found to be less than 0.2 nm over substantially the whole surface area.
  • the CVD single crystal diamond processed using the conditioned 33 pm diamond-matrix wheel was then subjected to an ICP etch to reduce subsurface damage.
  • the ICP etch was applied to the surface of the diamond using ICP/RF power of 500 W 1200 W for 50 minutes using a platen temperature of 5 °C and in an atmosphere of Ar (10 seem) and Ch (20 seem).
  • a portion of the surface of the diamond is shown in Figure 5, which had a dislocation density measured at the surface of around 10 5 cm -2 .
  • the CVD single crystal diamond was then placed into a CVD reactor for use as a substrate on which to homoepitaxially grow further CVD single crystal diamond.
  • process gases are fed into the CVD reactor.
  • Such process gases typically include a carbon-containing gas such as methane, and hydrogen.
  • a plasma is formed from the gases and the further CVD single crystal diamond grows on the buffer layer.
  • CVD synthesis conditions are typically controlled such that the CVD single crystal diamond substrate is held at a desired temperature (typically between 800°C and 1200°C). If the temperature is too low, then growth rates are low.
  • An upper limit to the growth temperature of 1200°C is generally required to avoid detrimental defect formation in the homoepitaxially grown diamond material such as twins.
  • the temperature in combination with other parameters such as carbon containing gas concentration, affects the morphology of the homoepitaxially grown diamond material and thus can be selected and controlled to achieve a desired morphology.
  • CVD synthesis conditions are also typically controlled such that a CVD synthesis atmosphere comprises a carbon containing gas (e.g. methane) at a concentration by volume in a range 3 to 8%, more preferably in a range 4 to 6%. If the carbon containing gas concentration is too low, then growth rates are too low. If the carbon containing gas concentration is too high, then cracking may occur and/or the material may have a poor optical quality. Furthermore, as previously stated, carbon containing gas concentration, in combination with other parameters such as the CVD single crystal diamond substrate temperature, affects the morphology of homoepitaxially grown diamond material and thus is selected and controlled to achieve the desired morphology close to net shape of the final processed product.
  • a carbon containing gas e.g. methane
  • CVD synthesis conditions are further controlled to provide a high power density across the substrate of at least 150 W/cm 2 , 180 W/cm 2 , 200 W/cm 2 , 230 W/cm 2 , 250 W/cm 2 , 270 W/cm 2 , 290 W/cm 2 , 310 W/cm 2 , or 330 W/cm 2 .
  • the power density will generally be less than 600 W/cm 2 , 500 W/cm 2 , or 400 W/cm 2 .
  • power density is defined as the total microwave input power divided by the area of the substrate, or the substrate holder, whichever has the greater area.
  • CVD synthesis conditions are further controlled to achieve a further CVD single crystal diamond growth rate selected from any of at least 4 pm per hour, at least 5 pm per hour, at least 10 pm per hour and at least 15 pm per hour until it reaches a descried thickness.
  • a surface processing operation is performed on the further CVD single crystal diamond to reduce surface damage.
  • processing techniques include one or more of cutting, cleaving, lapping, polishing, scaife polishing and/or etching. This may reduce any surface roughness that arises during the growth process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

L'invention concerne un procédé de transformation d'un diamant monocristallin CVD, le procédé comprenant l'obtention d'un diamant monocristallin CVD présentant une dimension latérale minimale d'au moins 20 mm, le diamant monocristallin CVD comprenant en outre une surface principale. La surface principale est transformée à l'aide d'une meule en diamant-matrice, la meule en diamant-matrice comprenant des particules de diamant incorporées qui sont incorporées dans une matrice. L'invention concerne également un diamant monocristallin CVD ayant une dimension linéaire la plus grande d'au moins 20 mm et une surface principale, la surface principale ayant une rugosité de surface Sa inférieure à 1 nm sur au moins 90 % de la surface principale.
PCT/EP2024/080313 2023-11-01 2024-10-25 Diamant monocristallin cvd Pending WO2025093450A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
GB2316754.7A GB2638116A (en) 2023-11-01 2023-11-01 CVD single crystal diamond material
GB2316754.7 2023-11-01
GB2403847.3A GB2635248A (en) 2023-11-01 2024-03-18 CVD single crystal diamond
GB2403847.3 2024-03-18

Publications (1)

Publication Number Publication Date
WO2025093450A1 true WO2025093450A1 (fr) 2025-05-08

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08133893A (ja) * 1994-11-07 1996-05-28 Sumitomo Electric Ind Ltd 自立したダイヤモンドウェハーおよびその製造方法
WO2004046427A1 (fr) * 2002-11-21 2004-06-03 Element Six Limited Diamant de qualite optique
US7396408B2 (en) 2003-05-06 2008-07-08 Universität Augsburg Monocrystalline diamond layer and method for the production thereof
US20220241927A1 (en) * 2019-10-23 2022-08-04 Huaqiao University Method for polishing single-crystal diamond

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH08133893A (ja) * 1994-11-07 1996-05-28 Sumitomo Electric Ind Ltd 自立したダイヤモンドウェハーおよびその製造方法
WO2004046427A1 (fr) * 2002-11-21 2004-06-03 Element Six Limited Diamant de qualite optique
US7396408B2 (en) 2003-05-06 2008-07-08 Universität Augsburg Monocrystalline diamond layer and method for the production thereof
US20220241927A1 (en) * 2019-10-23 2022-08-04 Huaqiao University Method for polishing single-crystal diamond

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
AIDA HIDEO ET AL: "Mirror-grinding of single-crystal diamond substrates with a rotary grinder", DIAMOND AND RELATED MATERIALS, ELSEVIER SCIENCE PUBLISHERS , AMSTERDAM, NL, vol. 121, 27 November 2021 (2021-11-27), XP086925021, ISSN: 0925-9635, [retrieved on 20211127], DOI: 10.1016/J.DIAMOND.2021.108733 *
LIU NIAN ET AL: "Damage-free highly efficient plasma-assisted polishing of a 20-mm square large mosaic single crystal diamond substrate", SCIENTIFIC REPORTS, vol. 10, no. 1, 10 November 2020 (2020-11-10), US, XP093251566, ISSN: 2045-2322, Retrieved from the Internet <URL:https://www.nature.com/articles/s41598-020-76430-6> DOI: 10.1038/s41598-020-76430-6 *
MILDRENRABEAU: "Optical Engineering of Diamond", 2013, WILEY-VCH, pages: 130

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