CN114232089B - Periodic modulation method for nucleation density of diamond on silicon carbide substrate - Google Patents

Periodic modulation method for nucleation density of diamond on silicon carbide substrate Download PDF

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CN114232089B
CN114232089B CN202111326033.1A CN202111326033A CN114232089B CN 114232089 B CN114232089 B CN 114232089B CN 202111326033 A CN202111326033 A CN 202111326033A CN 114232089 B CN114232089 B CN 114232089B
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growth
diamond particles
silicon carbide
flow rate
carbide substrate
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CN114232089A (en
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彭燕
胡秀飞
王希玮
徐现刚
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Shandong University
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    • 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
    • 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
    • C30B28/00—Production of homogeneous polycrystalline material with defined structure
    • C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
    • C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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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)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The application provides a periodic modulation method of nucleation density of diamond on a silicon carbide substrate, which is used for preparing grooves on a carbon surface or a silicon surface of the silicon carbide substrate. And placing the silicon carbide substrate with the grooves in a growth cavity of a CVD device, introducing reaction gas and auxiliary gas to grow diamond particles, and finally, after growing for a preset time, taking the silicon carbide substrate out of the growth cavity, and observing the morphology and nucleation density of the diamond particles at the bottom, the side wall and the outside of the grooves. Based on the difference of the nucleation densities of the diamond particles at different positions of the groove when the diamond particles are contacted with plasmas in the growth process, the periodic modulation of the nucleation densities of the diamond particles on the silicon carbide substrate is realized.

Description

Periodic modulation method for nucleation density of diamond on silicon carbide substrate
Technical Field
The application relates to the technical field of chemical vapor deposition of diamond films, in particular to a periodic modulation method of nucleation density of diamond on a silicon carbide substrate.
Background
Diamond has excellent optical, electrical, mechanical and thermal properties and thus has great potential for use. Particularly, the diamond film has the characteristics of wide band gap, optical transparency and abnormally high thermal conductivity, and is an ideal semiconductor material. Has good application prospect in high-tech fields such as high-density integrated circuit packaging materials, protective coatings, electrochemical electrodes and the like. In recent years, research into growing diamond thin films using a Microwave Plasma Chemical Vapor Deposition (MPCVD) method has received increasing attention because even polycrystalline diamond has a greater advantage than most existing crystals. In particular, the highest acoustic velocity and thermal conductivity driven by high carrier mobility and unique optical properties make diamond films ideal materials for many emerging device applications, such as ultra-high frequency acoustic filters, power electronics, integrated optical circuits, and quantum transducers.
The substrate for diamond film growth is silicon (Si), molybdenum (Mo), silicon carbide (SiC), or the like. Since the lattice parameter and structure of the substrate material associated with diamond are important considerations in determining good film growth, all substrate materials do not react the same in achieving good film adhesion. The lattice match of diamond to beta-SiC is good, with a lattice mismatch of about 18.2% (diamond to Si lattice mismatch of 52%). Therefore, when SiC is used as a substrate, nucleation is more likely. In addition, the SiC material has small thermal expansion coefficient and high heat conduction coefficient, and the characteristics are very similar to those of diamond, so that the adhesion of the diamond film on the SiC substrate is better. The combination of the properties of the two materials has great application potential. Since nucleation of diamond polycrystal has many problems at present, many researches show that there is a close relationship between the thermal conductivity and the grain size, and in order to modulate the thermal conductivity of diamond polycrystal, it is necessary to modulate the particles of diamond polycrystal.
Disclosure of Invention
In order to solve the problems, the embodiment of the application provides a method for periodically modulating nucleation density of diamond on a silicon carbide substrate.
The method for periodically modulating the nucleation density of the diamond on the silicon carbide substrate mainly comprises the following steps:
preparing a groove on a carbon surface or a silicon surface of a silicon carbide substrate;
placing the silicon carbide substrate in a growth chamber of a CVD apparatus;
and introducing reaction gas and auxiliary gas to grow diamond particles, and taking out the silicon carbide substrate from the growth cavity after the diamond particles grow to a preset time.
According to the method for periodically modulating the nucleation density of the diamond on the silicon carbide substrate, grooves are formed in the carbon surface or the silicon surface of the silicon carbide substrate, then the silicon carbide substrate with the grooves is placed in a growth cavity of a CVD device, reaction gas and auxiliary gas are introduced to grow diamond particles, finally, after the growth is carried out for a preset time, the silicon carbide substrate is taken out from the growth cavity, and the shape and the nucleation density of the diamond particles at the bottom, the side wall and the outside of the grooves are observed. Based on the difference of the nucleation densities of the diamond particles at different positions of the groove when the diamond particles are contacted with plasmas in the growth process, the periodic modulation of the nucleation densities of the diamond particles on the silicon carbide substrate is realized.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, and it will be obvious to a person skilled in the art that other drawings can be obtained from these drawings without inventive effort.
FIG. 1 is a schematic diagram of a basic flow of a method for periodically modulating nucleation density of diamond on a silicon carbide substrate according to an embodiment of the present application;
FIG. 2 is a schematic diagram of an implementation of the present application that provides nucleation of diamond on a SiC substrate;
FIG. 3a is an SEM image of diamond particles deposited at the bottom of a groove in a SiC substrate with a methane concentration of 1sccm and a nucleation time of 10 minutes;
FIG. 3b is an SEM image of diamond particles deposited at the bottom of a groove in a SiC substrate with a methane concentration of 3sccm and a nucleation time of 10min
FIG. 3c is an SEM image of diamond particles deposited at 6sccm methane concentration and 10min nucleation time at the bottom of a groove in a SiC substrate;
FIG. 3d is an SEM image of diamond particles deposited at 9sccm methane concentration and 10min nucleation time at the bottom of a groove in a SiC substrate;
FIG. 3e is an SEM image of diamond particles deposited at the bottom of a groove in a SiC substrate with a methane concentration of 12sccm and a nucleation time of 10 minutes;
FIG. 4a is CH 4 Under the conditions of 6sccm flow rate and 1h growth time, the groove of the SiC substrate is formedSEM images of diamond particles deposited thereat;
FIG. 4b is an SEM image of diamond particles deposited at the bottom of the grooves of FIG. 4 a;
FIG. 4c is a first SEM image of diamond particles deposited on the sidewalls of the grooves of FIG. 4 a;
FIG. 4d is a second SEM image of diamond particles deposited on the sidewalls of the grooves of FIG. 4 a;
FIG. 4e is a first SEM image of diamond particles deposited outside the grooves of FIG. 4 a;
FIG. 4f is a second SEM image of diamond particles deposited on the sidewalls of the grooves of FIG. 4 a;
fig. 5 is a raman spectrum of diamond nucleated at grooves in a SiC substrate at a CH4 flow rate of 6sccm and a growth time of 1 h.
Detailed Description
Reference will now be made in detail to exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, the same numbers in different drawings refer to the same or similar elements, unless otherwise indicated. The implementations described in the following exemplary examples do not represent all implementations consistent with the invention. Rather, they are merely examples of apparatus and methods consistent with aspects of the invention as detailed in the accompanying claims.
In this embodiment, the diamond film deposition is performed by microwave plasma chemical vapor deposition (Microwave Plasma Chemical Vapor Deposition, MPCVD) method, and the principle described by the ARDIS-300MPCVD apparatus manufactured by russian Optosystems company is adopted, and the apparatus for CVD (chemical vapor deposition ) may be used in the implementation process, and the embodiment is not limited in particular.
The method provided in this embodiment will be described in detail with reference to the accompanying drawings. Fig. 1 is a schematic flow chart of a method for periodically modulating nucleation density of diamond on a silicon carbide substrate according to the present embodiment, which mainly includes the following steps:
s101: grooves are made in the carbon or silicon side of the silicon carbide substrate.
Specifically, grooves can be formed on the C surface or the Si surface of the silicon carbide substrate by a method of laser cutting or saw blade cutting, the grooves can be uniformly distributed or non-uniformly distributed, the grooves can be alternately distributed or non-alternately distributed, the width of the grooves can be 100-500 μm in size, and the depth of the grooves can be 50-300 μm, but the grooves are not in the numerical range. In order to better observe the nucleation conditions of different positions of the groove, the cross section of the groove is preferably square, and the cross section of the groove can be rectangular or square.
S102: the silicon carbide substrate is placed in a growth chamber of a CVD apparatus.
After the trench is manufactured, the silicon carbide substrate can be subjected to surface cleaning treatment by sequentially adopting hydrofluoric acid, acetone, absolute ethyl alcohol and deionized water so as to remove scraps generated during manufacturing the trench, and the cleaning method is not limited to the cleaning method.
S103: and introducing reaction gas and auxiliary gas to grow diamond particles, and taking out the silicon carbide substrate from the growth cavity after the diamond particles grow to a preset time.
After the silicon carbide substrate is placed in the growth cavity of the MPCVD equipment, H is introduced 2 、CH 4 As a reaction gas, ar, O 2 And/or N 2 And the like as an assist gas, wherein the assist gas in this embodiment plays a role in adjusting the diamond particle size, nucleation quality, and the like.
In this example, a microwave power of 2000-8000W was used, the silicon carbide substrate temperature was measured with a double interference bolometer at 800-1100℃, the substrate temperature was measured with a double interference bolometer with emissivity of 0.1 through a 2mm slit, and the deposition process utilized H 2 And CH (CH) 4 Is carried out under a pressure of about 150Torr, H 2 The flow rate of the catalyst is about 50to 600sccm, CH 4 The flow rate of the catalyst is 1-40 sccm.
To better observe the diamond nucleation process, the present embodiment utilizes multiple silicon carbide substrates, each in different CH 4 Growth of diamond particles at different growth times and flow rates. Specifically, set H 2 The flow velocity of the gas is a first preset value, and different CH are respectively set 4 The growth of diamond particles is carried out at a flow rate for a first preset time, e.g., H can be set 2 The flow rate of (C) is 150-300 sccm, and CH 4 The flow rates of the diamond particles are respectively 1sccm, 3sccm, 6sccm, 9sccm and 12sccm, and the growth time is 5 to 15 minutes; set H 2 The flow rate of (2) is a first preset value, and CH is set 4 And the flow rate is a second preset value, the growth of diamond particles is carried out, and the growth time is a second preset time. Wherein the second preset time is longer than the first preset time; CH (CH) 4 When the second preset value of the flow rate is the first preset time for the growth time, the selected CH 4 Any value of flow rate. For example, set H 2 The flow rate of (C) is 150-300 sccm, and CH 4 The flow rate is any one of 1sccm, 3sccm, 6sccm, 9sccm and 12sccm, and the growth time is 0.5 to 1.5 hours.
Fig. 2 is a schematic diagram of an implementation of the present application that provides nucleation of diamond on a SiC substrate. As shown in fig. 2, the difference between the contact of the plasmas at different positions of the groove in the growth process of the diamond particles is based on that the plasmas at the bottom of the groove are least so that the nucleation density of the diamond particles is the lowest, the contact of the plasmas at the outer part of the groove is the most so that the nucleation density of the diamond particles is the largest, so that the difference of the nucleation densities of the diamond particles at different positions of the groove is further realized, and the modulation of the nucleation densities of the diamond particles at different positions of the groove is further realized, namely, the periodic modulation of the nucleation densities of the diamond particles on the silicon carbide substrate is realized.
Based on the above method, a nucleation process observation method will be further described with reference to examples. In the embodiment, grooves are prepared on the C surface of a silicon carbide substrate by adopting a saw blade machine method, the grooves are spaced by 1mm, the depth of each groove is 110 mu m, the width of each groove is 200 mu m, and after cleaning, a sample is placed in MPCVD. The deposition process was performed at a pressure of 150Torr using a microwave power of 4000W and a substrate temperature of 900℃measured with a double interference infrared bolometer, the substrate temperature being measured by a double interference infrared bolometer having an emissivity of 0.1 through a 2mm slit.H 2 The flow rate of CH is 150sccm 4 The flow rates of (1 sccm, 3sccm, 6sccm, 9sccm and 12 sccm) and the growth time was 10 minutes; another sample was grown for 1h, CH 4 The flow rate of (2) was 6sccm, and the other conditions were unchanged.
The sample was taken out and observed, and the morphology of the diamond particles was observed using a Scanning Electron Microscope (SEM) in this example. As shown in fig. 3a, 3b, 3c, 3d and 3e, which are SEM images of diamond particles deposited at the bottom of the SiC substrate groove, with methane concentrations of 1 seem, 3 seem, 6 seem, 9 seem and 12 seem, respectively, and nucleation times of 10 min. As shown in fig. 3a to 3e, spherical particles gradually increase with increasing methane concentration.
FIG. 4a is CH 4 SEM images of diamond particles deposited at the grooves of the SiC substrate under the conditions of a flow rate of 6sccm and a growth time of 1h can be compact in particle distribution in the grooves. Fig. 4b is an SEM image of diamond particles deposited at the bottom of the groove in fig. 4a, i.e. an enlarged view of region a in fig. 4a, with a median zone grain size greater than 5 μm.
Fig. 4c is a first SEM image of diamond particles deposited on the groove side wall in fig. 4a, and fig. 4d is a second SEM image of diamond particles deposited on the groove side wall in fig. 4a, i.e. an enlarged view of region B in fig. 4a, it can be seen that the crystal grains near the groove side wall are hemispherical, the crystal faces are gradually smooth, and the particles gradually form a flat square plane from the sphere, and the particle surface has many fine square planes. Fig. 4e is a first SEM image of diamond particles deposited outside the grooves in fig. 4a, i.e. an enlarged view of region C in fig. 4a, and it can be seen that the diamond grains located near the notches are significantly shaped as single crystal diamond, with the crystal planes being mostly square and triangular. A bonding layer exists between the crystal grain and the substrate; fig. 4f is a second SEM image of diamond particles deposited on the groove side walls of fig. 4a, which exhibit angular octahedral shape, flat square (100) faces and rough hexagonal (111) faces.
Fig. 5 is a raman spectrum of diamond nucleated at grooves in a SiC substrate at a CH4 flow rate of 6sccm and a growth time of 1 h. In this example, three positions of the groove bottom, groove side wall and outside the groove were measured, respectively, (1), (2) and (3) show raman shift positions of zero stress diamond, graphite and trans-polyacetylene. According to the raman results of fig. 5, the spherical particles in the grooves are graphite, the side walls of the grooves are diamond particles, and the diamond phase of the particles outside the grooves is more obvious.
In this specification, each embodiment is described in a progressive manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments. Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the disclosure herein. This application is intended to cover any variations, uses, or adaptations of the application following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the application pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the application being indicated by the following claims.
It is to be understood that the present application is not limited to the precise arrangements and instrumentalities shown in the drawings, which have been described above, and that various modifications and changes may be effected without departing from the scope thereof. The scope of the application is limited only by the appended claims.

Claims (8)

1. A method for periodically modulating nucleation density of diamond on a silicon carbide substrate, the method comprising:
preparing a groove on a carbon surface or a silicon surface of a silicon carbide substrate;
placing the silicon carbide substrate in a growth chamber of a CVD apparatus;
and introducing reaction gas and auxiliary gas to grow diamond particles, and taking out the silicon carbide substrate from the growth cavity after the diamond particles grow to a preset time.
2. The method of claim 1, wherein the method of preparing the grooves on the carbon or silicon side of the silicon carbide substrate comprises:
and preparing grooves on the carbon surface or the silicon surface of the silicon carbide substrate by adopting a laser cutting or saw blade machine cutting method.
3. The method of claim 1, wherein the grooves are square in cross-section.
4. A method according to claim 3, wherein the grooves have a width of 100 to 500 μm and a depth of 50to 300 μm.
5. The method of claim 1, wherein the growing of diamond particles is performed by introducing a reaction gas and an auxiliary gas, and the silicon carbide substrate is taken out of the growth chamber after growing for a preset time, comprising:
set H 2 The flow velocity of the gas is a first preset value, and different CH are respectively set 4 Growing diamond particles at the flow rate for a first preset time;
set H 2 The flow rate of (2) is a first preset value, and CH is set 4 The flow rate is a second preset value for growing diamond particles, and the growth time is a second preset time;
wherein the second preset time is longer than the first preset time; the CH is 4 When the second preset value of the flow rate is the first preset time for the growth time, the selected CH 4 Any value of flow rate.
6. The method of claim 5, wherein H is set 2 The flow velocity of the gas is a first preset value, and different CH are respectively set 4 The growth of diamond particles is carried out at the flow rate, and the growth time is a first preset time and comprises the following steps:
set H 2 The flow rate of (C) is 150-300 sccm, and CH 4 The growth of diamond particles was performed at flow rates of 1sccm, 3sccm, 6sccm, 9sccm and 12sccm, respectively, for a growth time of 5 to 15 minutes.
7. The method according to claim 5 or 6, characterized in thatCharacterized in that, set H 2 The flow rate of (2) is a first preset value, and CH is set 4 The growth of diamond particles is carried out with the flow rate being a second preset value, and the growth time is a second preset time, and the method comprises the following steps:
set H 2 The flow rate of CH is 150-300 sccm 4 The growth of diamond particles is carried out at any flow rate of 4-8 sccm, and the growth time is 0.5-1.5 h.
8. The method of claim 1, wherein the introducing of the reactant gas and the assist gas to effect growth of the diamond particles comprises:
the microwave power used is 3500-4000W, the temperature of the silicon carbide substrate is 850-950 ℃ measured by a double-interference infrared radiation pyrometer, wherein the substrate temperature is measured by the double-interference infrared radiation pyrometer with emissivity of 0.1 through a slit of 2 mm;
the reaction gas includes H 2 And CH (CH) 4， H 2 The flow rate of the catalyst is 100-400 sccm, CH 4 The flow rate of the catalyst is 1-20 sccm.
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Publication number Priority date Publication date Assignee Title
CN107287654A (en) * 2017-07-14 2017-10-24 中国电子科技集团公司第四十六研究所 A kind of method that CVD synthetic single crystal diamond reduces dislocation density
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Publication number Priority date Publication date Assignee Title
CN107287654A (en) * 2017-07-14 2017-10-24 中国电子科技集团公司第四十六研究所 A kind of method that CVD synthetic single crystal diamond reduces dislocation density
EP3890000A1 (en) * 2018-11-30 2021-10-06 Korea Polytechnic University Industry Academic Cooperation Foundation Method for manufacturing diamond substrate
CN113621938A (en) * 2020-05-06 2021-11-09 宁波材料所杭州湾研究院 Diamond film growth method, silicon wafer with diamond film and application
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