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CN109371463A - A kind of substrate selection method of cvd diamond crystal seed - Google Patents

A kind of substrate selection method of cvd diamond crystal seed Download PDF

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Publication number
CN109371463A
CN109371463A CN201811428583.2A CN201811428583A CN109371463A CN 109371463 A CN109371463 A CN 109371463A CN 201811428583 A CN201811428583 A CN 201811428583A CN 109371463 A CN109371463 A CN 109371463A
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Prior art keywords
substrate
hpht
growth chamber
diamond
crystal seed
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CN201811428583.2A
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Chinese (zh)
Inventor
刘宏明
左浩
李升�
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Xi'an Carbon Star Semiconductor Technology Co Ltd
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Xi'an Carbon Star Semiconductor Technology Co Ltd
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Priority to CN201811428583.2A priority Critical patent/CN109371463A/en
Publication of CN109371463A publication Critical patent/CN109371463A/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B25/00Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02Epitaxial-layer growth
    • C30B25/18Epitaxial-layer growth characterised by the substrate
    • C30B25/186Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/02Elements
    • C30B29/04Diamond

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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 present invention relates to the technical field of diamond, it more particularly to a kind of substrate selection method of cvd diamond crystal seed, can choose that quality is high, defect is few, provide good substrate for the epitaxial growth of single-crystal diamond;The following steps are included: (1) selects substrate;(2) acetone cleans;(3) ultrasonic cleaning;(4) it is dried;(5) reaction condition adjusts;(6) positive etching processing;(7) reversed etching processing;(8) it observes for the first time;(9) it observes for second.

Description

A kind of substrate selection method of cvd diamond crystal seed
Technical field
The present invention relates to the technical fields of diamond, select more particularly to a kind of substrate of cvd diamond crystal seed Method.
Background technique
Diamond is commonly called as " spark ", that is, our diamonds for often saying, he is a kind of mineral being made of pure carbon, and Most hard substance in nature, from after confirming that diamond was made of pure carbon in 18th century, people have been begun to people The research of diamond is made, only passes through the progress of high pressure research and High-Voltage Experimentation technology in the 1950s, is just obtained real Success and rapidly development, diamond be also widely used in it is various industry, technique industries, diamond be utilize The carbon source being precipitated when being pyrolyzed and be electrolysed certain carbonaceous materials carries out outer on diamond seeds or the substance of certain substrate effects Prolong made of growth.
Chemical vapor deposition (CVD) refers to the gas phase reaction under high temperature, can enable high-melting-point substances at low temperature Synthesis, can especially synthesize high-melting-point substances such as single-crystal diamond at low temperature, be made that huge contribution in energy conservation invention.
Microwave plasma CVD (MPCVD) is a kind of important method for preparing monocrystalline diamond, MPCVD Epitaxial growth single-crystal diamond is that homoepitaxy carries out on the single-crystal diamond substrate of high temperature and high pressure method (HPHT) growth.
But HPHT diamond substrate quality is uneven, and the substrate purchased all is after cutting, polishing grinding , this masks the defect of substrate itself, it is difficult to be selected from diamond surface pattern, and above and below HPHT diamond substrate The quality in two faces is also different, easily the quality of the diamond at influence epitaxial growth.
Summary of the invention
In order to solve the above technical problems, the present invention, which provides one kind, can choose that quality is high, defect is few, it is single-crystal diamond Epitaxial growth provides the substrate selection method of the cvd diamond crystal seed of good substrate.
A kind of substrate selection method of cvd diamond crystal seed of the invention, comprising the following steps:
(1) it selects substrate: selecting that shape is good, the HPHT diamond substrate of surface no significant defect purchased on the market;
(2) acetone cleans: the HPHT diamond substrate that will be singled out is put into progress soaking and washing 30min in acetone cleaning solution;
(3) ultrasonic cleaning: the cleaning container with acetone cleaning solution and diamond substrate is put into ultrasonic cleaning equipment, Ultrasonic cleaning is carried out to HPHT diamond substrate;
(4) be dried: by the HPHT diamond substrate after ultrasonic cleaning be removed and placed in after drying unit at 65 DEG C into Row drying and processing;
(5) reaction condition adjusts: the HPHT diamond substrate after drying being put into growth chamber, and adjusts in growth chamber and is Vacuum state, and HPHT diamond substrate temperature is made to be increased to 850 DEG C;
(6) H positive etching processing: is passed through into growth chamber2And O2Mixed gas, and adjust the intracorporal pressure of growth chamber and Microwave power carries out the etching of 0.5-1h to the upper surface of HPHT diamond substrate;
(7) reversed etching processing: overturning HPHT diamond substrate makes the HPHT diamond substrate back side upward, and continue to growth H is passed through in cavity2And O2Mixed gas, and the intracorporal pressure of growth chamber and microwave power are adjusted, to HPHT diamond substrate The etching of lower surface progress 0.5-1h;
(8) it observes for the first time: the HPHT diamond substrate by positive etching processing and reversed etching processing being taken out, and is placed Under microscope, by microscope, to treated, HPHT diamond substrate carries out preliminary observation, and eliminates more than wherein defect Sample;
(9) second observe: the sample not being eliminated being placed under the microscope of more high magnification numbe, to its upper and lower two surface into Row observation, and compared two-by-two, select the higher surface of quality to carry out epitaxial growth as HPHT diamond seeds substrate.
A kind of substrate selection method of cvd diamond crystal seed of the invention, the ultrasonic cleaning temperature in the step (3) It is 45 DEG C.
A kind of substrate selection method of cvd diamond crystal seed of the invention, in the step (6) and step (7) to life The H being passed through in long cavity2Flow be 300-600sccm, O2Flow be 2-12sccm.
The substrate selection method of a kind of cvd diamond crystal seed of the invention, it is preferred that in the step (6) and step (7) The H being passed through into growth chamber2Flow be 450sccm, O2Flow be 9sccm.
A kind of substrate selection method of cvd diamond crystal seed of the invention, the growth in the step (6) and step (7) The intracorporal pressure of chamber is 120-180mbar.
The substrate selection method of a kind of cvd diamond crystal seed of the invention, it is preferred that in the step (6) and step (7) The intracorporal pressure of growth chamber be 150mbar.
A kind of substrate selection method of cvd diamond crystal seed of the invention, the growth in the step (6) and step (7) The intracorporal microwave power of chamber is 3.5kW.
Compared with prior art the invention has the benefit that a kind of substrate of cvd diamond crystal seed of the invention selects Method is performed etching respectively using upper and lower surfaces of the mixed gas of hydrogen and oxygen to HPHT diamond substrate, and carved By observing under microscope substrate after erosion, the sample more than defect is eliminated, and sample further few to defect is upper and lower Two surfaces are observed, and so as to select quality height, defect few, provide good base for the epitaxial growth of single-crystal diamond The HPHT diamond substrate at bottom, and then the quality and purity of the single-crystal diamond that CVD growth goes out can be improved, so that it is played Biggish economic benefit.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for Illustrate the present invention, but is not intended to limit the scope of the invention.
Embodiment 1
Select that shape is good, the HPHT diamond substrate of surface no significant defect purchased on the market, the HPHT gold that will be singled out Hard rock substrate is put into progress soaking and washing 30min in acetone cleaning solution, will have the cleaning of acetone cleaning solution and diamond substrate Container is put into ultrasonic cleaning equipment, ultrasonic cleaning is carried out to HPHT diamond substrate at 45 DEG C, by ultrasonic cleaning HPHT diamond substrate afterwards carries out drying and processing after being removed and placed in drying unit at 65 DEG C, by the HPHT Buddha's warrior attendant after drying Stone lining bottom is put into growth chamber, and adjusting in growth chamber is vacuum state, and is increased to HPHT diamond substrate temperature 850 DEG C, the H that flow is 600sccm is passed through into growth chamber2The O for being 12sccm with flow2Mixed gas, and adjust growth The intracorporal pressure of chamber is 150mbar, microwave power 3.5kW, and the quarter of 0.5-1h is carried out to the upper surface of HPHT diamond substrate Erosion, overturn HPHT diamond substrate, make the HPHT diamond substrate back side upward, and continue to be passed through flow into growth chamber be The H of 600sccm2The O for being 12sccm with flow2Mixed gas, and adjust the intracorporal pressure of growth chamber be 150mbar, microwave function Rate is 3.5kW, and the etching of 0.5-1h is carried out to the lower surface of HPHT diamond substrate, will be carved by positive etching processing and reversely The HPHT diamond substrate of erosion processing is taken out, and is placed under microscope, by microscope to treated HPHT Buddha's warrior attendant stone lining Bottom carries out preliminary observation, and eliminates the sample more than wherein defect, and the sample not being eliminated is placed in the microscope of more high magnification numbe Under, its upper and lower two surface is observed, and is compared two-by-two, selects the higher surface of quality brilliant as HPHT diamond Kind substrate carries out epitaxial growth.
Embodiment 2
Select that shape is good, the HPHT diamond substrate of surface no significant defect purchased on the market, the HPHT gold that will be singled out Hard rock substrate is put into progress soaking and washing 30min in acetone cleaning solution, will have the cleaning of acetone cleaning solution and diamond substrate Container is put into ultrasonic cleaning equipment, ultrasonic cleaning is carried out to HPHT diamond substrate at 45 DEG C, by ultrasonic cleaning HPHT diamond substrate afterwards carries out drying and processing after being removed and placed in drying unit at 65 DEG C, by the HPHT Buddha's warrior attendant after drying Stone lining bottom is put into growth chamber, and adjusting in growth chamber is vacuum state, and is increased to HPHT diamond substrate temperature 850 DEG C, the H that flow is 450sccm is passed through into growth chamber2The O for being 9sccm with flow2Mixed gas, and adjust growth The intracorporal pressure of chamber is 150mbar, microwave power 3.5kW, and the quarter of 0.5-1h is carried out to the upper surface of HPHT diamond substrate Erosion, overturn HPHT diamond substrate, make the HPHT diamond substrate back side upward, and continue to be passed through flow into growth chamber be The H of 450sccm2The O for being 9sccm with flow2Mixed gas, and adjust the intracorporal pressure of growth chamber be 150mbar, microwave function Rate is 3.5kW, and the etching of 0.5-1h is carried out to the lower surface of HPHT diamond substrate, will be carved by positive etching processing and reversely The HPHT diamond substrate of erosion processing is taken out, and is placed under microscope, by microscope to treated HPHT Buddha's warrior attendant stone lining Bottom carries out preliminary observation, and eliminates the sample more than wherein defect, and the sample not being eliminated is placed in the microscope of more high magnification numbe Under, its upper and lower two surface is observed, and is compared two-by-two, selects the higher surface of quality brilliant as HPHT diamond Kind substrate carries out epitaxial growth.
Embodiment 3
Select that shape is good, the HPHT diamond substrate of surface no significant defect purchased on the market, the HPHT gold that will be singled out Hard rock substrate is put into progress soaking and washing 30min in acetone cleaning solution, will have the cleaning of acetone cleaning solution and diamond substrate Container is put into ultrasonic cleaning equipment, ultrasonic cleaning is carried out to HPHT diamond substrate at 45 DEG C, by ultrasonic cleaning HPHT diamond substrate afterwards carries out drying and processing after being removed and placed in drying unit at 65 DEG C, by the HPHT Buddha's warrior attendant after drying Stone lining bottom is put into growth chamber, and adjusting in growth chamber is vacuum state, and is increased to HPHT diamond substrate temperature 850 DEG C, the H that flow is 300sccm is passed through into growth chamber2The O for being 6sccm with flow2Mixed gas, and adjust growth The intracorporal pressure of chamber is 150mbar, microwave power 3.5kW, and the quarter of 0.5-1h is carried out to the upper surface of HPHT diamond substrate Erosion, overturn HPHT diamond substrate, make the HPHT diamond substrate back side upward, and continue to be passed through flow into growth chamber be The H of 300sccm2The O for being 9sccm with flow2Mixed gas, and adjust the intracorporal pressure of growth chamber be 150mbar, microwave function Rate is 3.5kW, and the etching of 0.5-1h is carried out to the lower surface of HPHT diamond substrate, will be carved by positive etching processing and reversely The HPHT diamond substrate of erosion processing is taken out, and is placed under microscope, by microscope to treated HPHT Buddha's warrior attendant stone lining Bottom carries out preliminary observation, and eliminates the sample more than wherein defect, and the sample not being eliminated is placed in the microscope of more high magnification numbe Under, its upper and lower two surface is observed, and is compared two-by-two, selects the higher surface of quality brilliant as HPHT diamond Kind substrate carries out epitaxial growth.
Diamond growth is carried out as substrate using the cvd diamond crystal seed that embodiment 1 to embodiment 3 is picked out, and right What it grew obtains following result by comparison:
Growth thickness: 2 > embodiment of embodiment, 1 > embodiment 3.
Growth quality: 2 > embodiment of embodiment, 3 > embodiment 2.
The substrate selection method of a kind of cvd diamond crystal seed of the invention, using the mixed gas pair of hydrogen and oxygen The upper and lower surfaces of HPHT diamond substrate perform etching respectively, and after etching by observing under microscope substrate, The sample more than defect is eliminated, and two surfaces up and down of sample further few to defect are observed, so as to select matter Amount is high, defect is few, provides the HPHT diamond substrate of good substrate for the epitaxial growth of single-crystal diamond, and then can be improved The quality and purity for the single-crystal diamond that CVD growth goes out, so that it plays biggish economic benefit.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the technical principles of the invention, several improvements and modifications, these improvements and modifications can also be made Also it should be regarded as protection scope of the present invention.

Claims (7)

1. a kind of substrate selection method of cvd diamond crystal seed, which comprises the following steps:
(1) it selects substrate: selecting that shape is good, the HPHT diamond substrate of surface no significant defect purchased on the market;
(2) acetone cleans: the HPHT diamond substrate that will be singled out is put into progress soaking and washing 30min in acetone cleaning solution;
(3) ultrasonic cleaning: the cleaning container with acetone cleaning solution and diamond substrate is put into ultrasonic cleaning equipment, Ultrasonic cleaning is carried out to HPHT diamond substrate;
(4) be dried: by the HPHT diamond substrate after ultrasonic cleaning be removed and placed in after drying unit at 65 DEG C into Row drying and processing;
(5) reaction condition adjusts: the HPHT diamond substrate after drying being put into growth chamber, and adjusts in growth chamber and is Vacuum state, and HPHT diamond substrate temperature is made to be increased to 850 DEG C;
(6) H positive etching processing: is passed through into growth chamber2And O2Mixed gas, and adjust the intracorporal pressure of growth chamber and Microwave power carries out the etching of 0.5-1h to the upper surface of HPHT diamond substrate;
(7) reversed etching processing: overturning HPHT diamond substrate makes the HPHT diamond substrate back side upward, and continue to growth H is passed through in cavity2And O2Mixed gas, and the intracorporal pressure of growth chamber and microwave power are adjusted, to HPHT diamond substrate The etching of lower surface progress 0.5-1h;
(8) it observes for the first time: the HPHT diamond substrate by positive etching processing and reversed etching processing being taken out, and is placed Under microscope, by microscope, to treated, HPHT diamond substrate carries out preliminary observation, and eliminates more than wherein defect Sample;
(9) second observe: the sample not being eliminated being placed under the microscope of more high magnification numbe, to its upper and lower two surface into Row observation, and compared two-by-two, select the higher surface of quality to carry out epitaxial growth as HPHT diamond seeds substrate.
2. a kind of substrate selection method of cvd diamond crystal seed as described in claim 1, which is characterized in that the step (3) In ultrasonic cleaning temperature be 45 DEG C.
3. a kind of substrate selection method of cvd diamond crystal seed as described in claim 1, which is characterized in that the step (6) With the H being passed through into growth chamber in step (7)2Flow be 300-600sccm, O2Flow be 2-12sccm.
4. a kind of substrate selection method of cvd diamond crystal seed as claimed in claim 3, which is characterized in that it is preferred, it is described The H being passed through in step (6) and step (7) into growth chamber2Flow be 450sccm, O2Flow be 9sccm.
5. a kind of substrate selection method of cvd diamond crystal seed as described in claim 1, which is characterized in that the step (6) It is 120-180mbar with the intracorporal pressure of growth chamber in step (7).
6. a kind of substrate selection method of cvd diamond crystal seed as claimed in claim 5, which is characterized in that it is preferred, it is described The intracorporal pressure of growth chamber in step (6) and step (7) is 150mbar.
7. a kind of substrate selection method of cvd diamond crystal seed as described in claim 1, which is characterized in that the step (6) It is 3.5kW with the intracorporal microwave power of growth chamber in step (7).
CN201811428583.2A 2018-11-27 2018-11-27 A kind of substrate selection method of cvd diamond crystal seed Pending CN109371463A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112899774A (en) * 2021-01-18 2021-06-04 武汉普迪真空科技有限公司 Method for homoepitaxial growth of monocrystal diamond from natural diamond

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03505861A (en) * 1988-06-03 1991-12-19 マサチューセッツ・インステチュート・オブ・テクノロジー silicon dioxide film on diamond
CN102021649A (en) * 2010-12-24 2011-04-20 吉林大学 Chemical vapor deposition method for preparing diamond single crystal by adding N2O gas
CN104975343A (en) * 2015-06-04 2015-10-14 哈尔滨工业大学 Method for improving quality of diamond seed crystal with hydrogen plasma multiple etching/annealing cyclic process
CN107059120A (en) * 2017-05-09 2017-08-18 中国电子科技集团公司第四十六研究所 A kind of method that utilization square groove inserting collet suppresses polycrystalline diamond growth
CN107146756A (en) * 2017-06-27 2017-09-08 中国科学院微电子研究所 Method for preparing field effect transistor with diamond substrate
CN107275192A (en) * 2017-07-10 2017-10-20 北京科技大学 High-performance diamond method for semiconductor is prepared based on inexpensive single-crystal diamond
CN107675249A (en) * 2017-09-08 2018-02-09 西安电子科技大学 The expanding growing method of single-crystal diamond

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03505861A (en) * 1988-06-03 1991-12-19 マサチューセッツ・インステチュート・オブ・テクノロジー silicon dioxide film on diamond
CN102021649A (en) * 2010-12-24 2011-04-20 吉林大学 Chemical vapor deposition method for preparing diamond single crystal by adding N2O gas
CN104975343A (en) * 2015-06-04 2015-10-14 哈尔滨工业大学 Method for improving quality of diamond seed crystal with hydrogen plasma multiple etching/annealing cyclic process
CN107059120A (en) * 2017-05-09 2017-08-18 中国电子科技集团公司第四十六研究所 A kind of method that utilization square groove inserting collet suppresses polycrystalline diamond growth
CN107146756A (en) * 2017-06-27 2017-09-08 中国科学院微电子研究所 Method for preparing field effect transistor with diamond substrate
CN107275192A (en) * 2017-07-10 2017-10-20 北京科技大学 High-performance diamond method for semiconductor is prepared based on inexpensive single-crystal diamond
CN107675249A (en) * 2017-09-08 2018-02-09 西安电子科技大学 The expanding growing method of single-crystal diamond

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112899774A (en) * 2021-01-18 2021-06-04 武汉普迪真空科技有限公司 Method for homoepitaxial growth of monocrystal diamond from natural diamond
CN112899774B (en) * 2021-01-18 2023-10-17 武汉普迪真空科技有限公司 Method for homoepitaxial growth of monocrystalline diamond by natural diamond

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