CN109911894A - The method of MPCVD method growth polycrystalline diamond flag - Google Patents
The method of MPCVD method growth polycrystalline diamond flag Download PDFInfo
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- CN109911894A CN109911894A CN201910279579.2A CN201910279579A CN109911894A CN 109911894 A CN109911894 A CN 109911894A CN 201910279579 A CN201910279579 A CN 201910279579A CN 109911894 A CN109911894 A CN 109911894A
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Abstract
The invention discloses the methods of MPCVD method growth polycrystalline diamond flag, are related to diamond field, the specific steps of which are as follows: (1) pre-processes the substrate in microwave plasma CVD equipment；(2) in the process forming core 0.4-0.6h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；Growth time is controlled according to the requirement of final growth thickness, carries out multiplicating growth after can repeatedly shutting down, grind, polishing.The polycrystalline diamond self-supporting piece thickness that the present invention is grown up to grade more than, face and can effectively inhibit the phenomenon that diamond particles with thickness increase and constantly increase, diamond particles are refined while meeting thickness requirement to reach, the purpose of diamond chip consistency, mechanical strength and surface of polished finish is promoted, to more fully play the value of CVD polycrystalline diamond abrasive compact.
Description
Technical field
The present invention relates to diamond field, specifically MPCVD method grows polycrystalline diamond
The method of flag.
Background technique
At present polycrystalline diamond abrasive compact almost hardness, thermal conductivity, optical transmittance and in terms of all
The natural diamond of high-quality has been met or exceeded, but breaking strength is unsatisfactory, lower than natural diamond about one
A order of magnitude, this results in polycrystalline diamond to be easy to appear cracking phenomena in use to its service life that terminates.It makes
At the main reason for this problem in addition to diamond sheet deposition and cooling procedure in there are other than stress, another is most important
Reason be exactly in deposition process diamond grain size it is excessive；On the other hand, the increase of diamond grain size, while also reducing
Surface compact degree and finish after diamond chip polishing, limit its application.
But polycrystalline diamond flag is grown to crystal competitive growth mode, the forming core of diamond film in such a mode
Face particle is tiny and aufwuchsplate particle is coarse, cross section show crystal grain in up big and down small like cone cell crystalline form, and the thickness of piece
This bigger phenomenon is more obvious, and breaking strength also decreases.Therefore its cause is promoted while improving the thickness of diamond chip
Density, reducing diamond particle size is to improve the effective ways of diamond chip breaking strength, so that it is more more fully to play CVD
The value of diamond material.Researcher comes up with a variety of method refinement crystal grain thus: as improved Enhancing Nucleation Density, introducing nitrogen
Or oxygen, argon gas etc., but these methods can only all reduce the phenomenon that diamond particles increase and can not fundamentally change Buddha's warrior attendant
The competitive growth mechanism of stone film.
Summary of the invention
1. to solve the problems, such as
Aiming at the problems existing in the prior art, the purpose of the present invention is to provide microwave plasma CVDs
Method grow polycrystalline diamond flag method, by this method grow polycrystalline diamond self-supporting piece thickness up to millimeter and with
On, and can effectively inhibit the phenomenon that diamond particles constantly increase as thickness increases, meeting thickness to reach
It is required that while refine diamond particles, the consistency of diamond chip and the purpose of mechanical strength are promoted, to more fully send out
The value of CVD polycrystalline diamond abrasive compact is waved, to solve the problems, such as to mention in above-mentioned background story.
2. technical solution
To achieve the above object, the invention provides the following technical scheme:
The method that MPCVD method grows polycrystalline diamond flag, the specific steps of which are as follows:
(1) substrate in microwave plasma CVD equipment is pre-processed；
(2) in the process forming core 0.4-0.6h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；
(3) long-time that polycrystalline diamond flag is carried out under conditions of fixed methane, hydrogen and other addition gases is raw
Long, at 800-1050 DEG C, growth time was controlled at 10-50 hours for growth temperature control；
(4) after growing 10-50 hours, stop other gases supply in addition to hydrogen, the plasma generated with hydrogen
0.5-1h is performed etching to the diamond chip sample in reaction cabin, microwave plasma CVD is slowly reduced later and sets
Microwave power in standby, and phased out hydrogen is supplied, and so that the temperature of diamond growth substrate is reduced to 80-160 DEG C, is finally stopped
Only all gas is supplied and is shut down, and diamond chip sample is taken out after reaction warehouse is cooled to room temperature；
(5) diamond chip sample is put into the concentrated sulfuric acid of heating and impregnates, removes the non-diamond generated in growth course
State carbon, is cleaned later, is removed the concentrated sulfuric acid, is then ground, polished, cleaned to aufwuchsplate；
(6) sample is reloaded in the reaction warehouse in microwave plasma CVD equipment, repeats above-mentioned gold
Growth step (1)-(4) of hard rock piece control growth time according to the requirement of final growth thickness, can repeatedly shut down, grind, throw
Multiplicating growth is carried out after light.
As a further solution of the present invention: other addition gases are argon gas in the step (3).
As a further solution of the present invention: pretreated method is to pass through mechanical lapping, diamond in the step (1)
The methods of micro-powdered polishing and cleaning are handled, grease, iron rust or other impurities element on removing substrate, so that substrate
The good nucleation rate for increasing diamond on substrate while directly contact, diamond used in this step are carried out between diamond
Grain size of micropowder is between W0.25-W0.5.
As a further solution of the present invention: grinding technics is using mechanical lapping or laser processing work in the step (5)
Skill.
As a further solution of the present invention: polishing process is polished using diadust in the step (5), diamond
Grain size of micropowder between W0.25-W0.5, thus effectively promoted regrow during diamond second nucleation efficiency, inhibit
Diamond grain size.
As a further solution of the present invention: in the step (4), cooling, shutdown process continue 1-2 hours, to have
Effect avoids diamond chip from generating since temperature change is too fast and burst phenomenon.
As a further solution of the present invention: the base metals in substrate include one of Zr, Mo, W and Ti or more
Kind, carbide is formed in conjunction with carbon by base metals, is provided more binding sites for the deposition process of diamond, is conducive to
The formation of diamond.
As a further solution of the present invention: substrate is identical or close as the thermal expansion coefficient of diamond, reduces formation
The difference of thermal expansivity between diamond chip and base material when reducing cooling, and then reduces diamond chip cracking or falls off
Probability.
Compared with prior art, the beneficial effects of the present invention are:
The polycrystalline diamond self-supporting piece thickness that the present invention is grown can effectively inhibit Buddha's warrior attendant up to millimeter or more
The phenomenon that stone particle constantly increases as thickness increases, to reach the refinement diamond while meeting thickness requirement
Grain promotes the purpose of the consistency of diamond chip, mechanical strength and surface of polished finish, to more fully play CVD
The value of polycrystalline diamond abrasive compact.
Detailed description of the invention
After Fig. 1 is disposably grown in the method for MPCVD method growth polycrystalline diamond flag
40 times of enlarged structure schematic diagrams of optical microscopy of polycrystalline diamond flag (600 μm thick).
Fig. 2 is that MPCVD method is grown in the method for polycrystalline diamond flag using after diauxic growth
Polycrystalline diamond flag (thick 760 μm) 40 times of enlarged structure schematic diagrams of optical microscopy.
Fig. 3 is that MPCVD method is grown in the method for polycrystalline diamond flag using after three secondary growths
Polycrystalline diamond flag (thick 1050 μm) 40 times of enlarged structure schematic diagrams of optical microscopy.
Fig. 4 is the diamond that MPCVD method grows that the method for polycrystalline diamond flag generates.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
In the embodiment of the present invention, the method that MPCVD method grows polycrystalline diamond flag, tool
Steps are as follows for body:
(1) substrate in microwave plasma CVD equipment is pre-processed；
(2) in the process forming core 0.5h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；
(3) long-time that polycrystalline diamond flag is carried out under conditions of fixed methane, hydrogen and other addition gases is raw
Long, at 800-1050 DEG C, growth time was controlled at 40 hours for growth temperature control；
(4) after growing 40 hours, stop other gases supply in addition to hydrogen, the plasma generated with hydrogen is to anti-
It answers the diamond chip sample in cabin to perform etching 1h, slowly reduces later micro- in microwave plasma CVD equipment
Wave power, and phased out hydrogen is supplied, and the temperature of diamond growth substrate is made to be reduced to 80-160 DEG C, finally stops whole gas
Body is supplied and is shut down, and diamond chip sample is taken out after reaction warehouse is cooled to room temperature；
(5) diamond chip sample is put into the concentrated sulfuric acid of heating and impregnates, removes the non-diamond generated in growth course
State carbon, is cleaned later, is removed the concentrated sulfuric acid, is then ground, polished, cleaned to aufwuchsplate；
Other addition gases are argon gas in the step 3.
In the step 1 pretreated method be by mechanical lapping, the methods of diadust polishing and cleaning into
Row processing, grease, iron rust or other impurities element on removing substrate, so that being carried out between substrate and diamond good straight
Increase the nucleation rate of diamond on substrate while contact, diadust partial size used in this step is in W0.25.
Grinding technics uses mechanical lapping or laser processing technology in the step 5.
Polishing process is polished using diadust in the step 5, and diadust partial size is in W0.25, thus effectively
The second nucleation efficiency of diamond during regrowing is promoted, diamond grain size is inhibited.
In the step 4, cooling, shutdown process continue 2 hours, to effectively avoid diamond chip due to temperature change
It is too fast and generate burst phenomenon.
Base metals in substrate include one or more of Zr, Mo, W and Ti, through base metals in conjunction with carbon
Carbide is formed, more binding sites is provided for the deposition process of diamond, is conducive to the formation of diamond.
Substrate is identical or close as the thermal expansion coefficient of diamond, reduces hot between the diamond chip of formation and base material
Expansile difference, when reducing cooling, and then the probability for reducing diamond chip cracking or falling off.
Embodiment 2
In the embodiment of the present invention, the method that MPCVD method grows polycrystalline diamond flag, tool
Steps are as follows for body:
(1) substrate in microwave plasma CVD equipment is pre-processed；
(2) in the process forming core 0.5h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；
(3) long-time that polycrystalline diamond flag is carried out under conditions of fixed methane, hydrogen and other addition gases is raw
Long, at 800-1050 DEG C, growth time was controlled at 24 hours for growth temperature control；
(4) after growing 24 hours, stop other gases supply in addition to hydrogen, the plasma generated with hydrogen is to anti-
It answers the diamond chip sample in cabin to perform etching 1h, slowly reduces later micro- in microwave plasma CVD equipment
Wave power, and phased out hydrogen is supplied, and the temperature of diamond growth substrate is made to be reduced to 80-160 DEG C, finally stops whole gas
Body is supplied and is shut down, and diamond chip sample is taken out after reaction warehouse is cooled to room temperature；
(5) diamond chip sample is put into the concentrated sulfuric acid of heating and impregnates, removes the non-diamond generated in growth course
State carbon, is cleaned later, is removed the concentrated sulfuric acid, is then ground, polished, cleaned to aufwuchsplate；
(6) sample is reloaded in the reaction warehouse in microwave plasma CVD equipment, is repeated once
Growth step (1)-(4) for stating diamond chip, i.e., diamond chip is grown by secondary total 48h in the present embodiment.
Other addition gases are argon gas in the step 3.
In the step 1 pretreated method be by mechanical lapping, the methods of diadust polishing and cleaning into
Row processing, grease, iron rust or other impurities element on removing substrate, so that being carried out between substrate and diamond good straight
Increase the nucleation rate of diamond on substrate while contact, diadust partial size used in this step is in W0.25.
Grinding technics uses mechanical lapping or laser processing technology in the step 5.
Polishing process is polished using diadust in the step 5, and diadust partial size is in W0.25, thus effectively
The second nucleation efficiency of diamond during regrowing is promoted, diamond grain size is inhibited.
In the step 4, cooling, shutdown process continue 2 hours, to effectively avoid diamond chip due to temperature change
It is too fast and generate burst phenomenon.
Base metals in substrate include one or more of Zr, Mo, W and Ti, through base metals in conjunction with carbon
Carbide is formed, more binding sites is provided for the deposition process of diamond, is conducive to the formation of diamond.
Substrate is identical or close as the thermal expansion coefficient of diamond, reduces hot between the diamond chip of formation and base material
Expansile difference, when reducing cooling, and then the probability for reducing diamond chip cracking or falling off.
Embodiment 3
In the embodiment of the present invention, the method that MPCVD method grows polycrystalline diamond flag, tool
Steps are as follows for body:
(1) substrate in microwave plasma CVD equipment is pre-processed；
(2) in the process forming core 0.5h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；
(3) long-time that polycrystalline diamond flag is carried out under conditions of fixed methane, hydrogen and other addition gases is raw
Long, at 800-1050 DEG C, growth time was controlled at 24 hours for growth temperature control；
(4) after growing 24 hours, stop other gases supply in addition to hydrogen, the plasma generated with hydrogen is to anti-
It answers the diamond chip sample in cabin to perform etching 1h, slowly reduces later micro- in microwave plasma CVD equipment
Wave power, and phased out hydrogen is supplied, and the temperature of diamond growth substrate is made to be reduced to 80-160 DEG C, finally stops whole gas
Body is supplied and is shut down, and diamond chip sample is taken out after reaction warehouse is cooled to room temperature；
(5) diamond chip sample is put into the concentrated sulfuric acid of heating and impregnates, removes the non-diamond generated in growth course
State carbon, is cleaned later, is removed the concentrated sulfuric acid, is then ground, polished, cleaned to aufwuchsplate；
(6) sample is reloaded in the reaction warehouse in microwave plasma CVD equipment, is repeated twice
Growth step (1)-(4) for stating diamond chip, i.e., diamond chip is grown by amounting to 72h three times in the present embodiment.
Other addition gases are argon gas in the step 3.
In the step 1 pretreated method be by mechanical lapping, the methods of diadust polishing and cleaning into
Row processing, grease, iron rust or other impurities element on removing substrate, so that being carried out between substrate and diamond good straight
Increase the nucleation rate of diamond on substrate while contact, diadust partial size used in this step is in W0.25.
Grinding technics uses mechanical lapping or laser processing technology in the step 5.
Polishing process is polished using diadust in the step 5, and diadust partial size is in W0.25, thus effectively
The second nucleation efficiency of diamond during regrowing is promoted, diamond grain size is inhibited.
In the step 4, cooling, shutdown process continue 2 hours, to effectively avoid diamond chip due to temperature change
It is too fast and generate burst phenomenon.
Base metals in substrate include one or more of Zr, Mo, W and Ti, through base metals in conjunction with carbon
Carbide is formed, more binding sites is provided for the deposition process of diamond, is conducive to the formation of diamond.
Substrate is identical or close as the thermal expansion coefficient of diamond, reduces hot between the diamond chip of formation and base material
Expansile difference, when reducing cooling, and then the probability for reducing diamond chip cracking or falling off.
The product in embodiment 1, embodiment 2 and example 3 is detected by vernier caliper, is wherein averaged in embodiment 1
Polycrystalline diamond thick film of the thickness at 600 μm obtains polycrystalline diamond thick film of the average thickness at 760 μm in embodiment 2, implements
Polycrystalline diamond thick film of the average thickness at 1050 μm is obtained in example 3, and polycrystalline diamond thick film thin and thick is uniform, presentation quality compared with
It is good；
And the product in comparative example 1, embodiment 2 and embodiment 3, i.e. embodiment 1 are the polycrystalline after disposable growth
Diamond thick-film, the product in embodiment 2 are the polycrystalline diamond thick film after diauxic growth, for after three secondary growths in embodiment 3
Polycrystalline diamond thick film.There are apparent coarse grains phenomenon, compact structures for polycrystalline diamond thick film after disposable growth
Spend it is bad, although the polycrystalline diamond film thickness tested of diauxic growth is than the epitaxial diamond films that disposably grow
It is 160 μm or so thick, according to Figure of description it is found that the crystallite dimension in epitaxial diamond films after secondary recycling is significantly less than one
The crystallite dimension of epitaxial diamond films after secondary regeneration, diamond growth face consistency are more preferable；And growth experiment obtains three times
Epitaxial diamond films Thickness ness is but attached according to specification than disposably grow 550 μm of polycrystalline diamond film thickness or so
Figure is it is found that the crystallite dimension in epitaxial diamond films after tertiary recycling is significantly less than the epitaxial diamond films after primary recycling
Crystallite dimension, crystallite dimension is close with diauxic growth experiment, and diamond growth face consistency is more preferable.Since repeated growth method exists
Second nucleation, therefore second nucleation phenomenon can be promoted on the diamond crystals surface grown up to, this phenomenon results in new gold
The formation of hard rock crystal simultaneously competes limited growing space with the diamond particles grown up to cause showing for crystal grain refinement
As, therefore the method for repeated growth has remarkable result on inhibition diamond thick-film particle is coarse.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.Any reference signs in the claims should not be construed as limiting the involved claims.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (8)
1. the method for MPCVD method growth polycrystalline diamond flag, which is characterized in that its specific steps
It is as follows:
(1) substrate in microwave plasma CVD equipment is pre-processed；
(2) in the process forming core 0.4-0.6h by being grown on pretreated substrate according to conventional polycrystalline diamond chip；
(3) the long-time growth of polycrystalline diamond flag is carried out under conditions of fixed methane, hydrogen and other addition gases, it is raw
At 800-1050 DEG C, growth time was controlled at 10-50 hours for long temperature control；
(4) after growing 10-50 hours, stop other gases supply in addition to hydrogen, the plasma generated with hydrogen is to anti-
It answers the diamond chip sample in cabin to perform etching 0.5-1h, slowly reduces in microwave plasma CVD equipment later
Microwave power, and phased out hydrogen is supplied, and the temperature of diamond growth substrate is made to be reduced to 80-160 DEG C, is finally stopped complete
Portion's gas is supplied and is shut down, and diamond chip sample is taken out after reaction warehouse is cooled to room temperature；
(5) diamond chip sample is put into the concentrated sulfuric acid of heating and impregnates, removes the non-diamond state carbon generated in growth course,
It is cleaned later, removes the concentrated sulfuric acid, then aufwuchsplate is ground, polish, is cleaned；
(6) sample is reloaded in the reaction warehouse in microwave plasma CVD equipment, repeats above-mentioned diamond
Growth step (1)-(4) of piece control growth time according to the requirement of final growth thickness, after can repeatedly shutting down, grind, polishing
Carry out multiplicating growth.
2. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, other addition gases are argon gas in the step (3).
3. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, pretreated method is by mechanical lapping, the methods of diadust polishing and cleaning in the step (1)
It is handled, grease, iron rust or other impurities element on removing substrate, so that being carried out between substrate and diamond good
Increase the nucleation rate of diamond on substrate while directly contact, diadust partial size used in this step W0.25-W0.5 it
Between.
4. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, grinding technics uses mechanical lapping or laser processing technology in the step (5).
5. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
Be characterized in that, in the step (5) polishing process using diadust polish, diadust partial size W0.25-W0.5 it
Between, thus effectively promoted regrow during diamond second nucleation efficiency, inhibit diamond grain size.
6. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, cooling, shutdown process continue 1-2 hours in the step (4), to effectively avoid diamond chip due to temperature
Change too fast and generates and burst phenomenon.
7. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, the base metals in substrate include one or more of Zr, Mo, W and Ti, through base metals in conjunction with carbon
Carbide is formed, more binding sites is provided for the deposition process of diamond, is conducive to the formation of diamond.
8. the method for MPCVD method growth polycrystalline diamond flag according to claim 1,
It is characterized in that, substrate is identical or close as the thermal expansion coefficient of diamond, reduces between the diamond chip of formation and base material
The difference of thermal expansivity, when reducing cooling, and then the probability for reducing diamond chip cracking or falling off.
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| CN111118471A (en) * | 2020-01-15 | 2020-05-08 | 吉林大学 | Preparation method of high-quality polycrystalline diamond film |
| CN112030133A (en) * | 2020-11-06 | 2020-12-04 | 苏州香榭轩表面工程技术咨询有限公司 | Diamond and preparation method and application thereof |
| CN112760612A (en) * | 2020-12-28 | 2021-05-07 | 吉林工程技术师范学院 | Preparation method of self-supporting nano-needle porous diamond |
| CN113430498A (en) * | 2021-06-23 | 2021-09-24 | 太原理工大学 | Preparation method of high-precision diamond polishing sheet |
| CN113699588A (en) * | 2021-10-21 | 2021-11-26 | 天津本钻科技有限公司 | Growth method for controlling polycrystalline diamond grain size by microwave CVD method |
| CN114684818A (en) * | 2022-04-01 | 2022-07-01 | 佛山曜世新材料科技有限公司 | Diamond plasma device and diamond preparation method |
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| CN113699588A (en) * | 2021-10-21 | 2021-11-26 | 天津本钻科技有限公司 | Growth method for controlling polycrystalline diamond grain size by microwave CVD method |
| CN114684818A (en) * | 2022-04-01 | 2022-07-01 | 佛山曜世新材料科技有限公司 | Diamond plasma device and diamond preparation method |
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Application publication date: 20190621 |