CN106744931B - A kind of method that plasma etching graphite prepares diamond particles - Google Patents
A kind of method that plasma etching graphite prepares diamond particles Download PDFInfo
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- CN106744931B CN106744931B CN201611130191.9A CN201611130191A CN106744931B CN 106744931 B CN106744931 B CN 106744931B CN 201611130191 A CN201611130191 A CN 201611130191A CN 106744931 B CN106744931 B CN 106744931B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 239000010432 diamond Substances 0.000 title claims abstract description 138
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 137
- 239000010439 graphite Substances 0.000 title claims abstract description 125
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 125
- 239000002245 particle Substances 0.000 title claims abstract description 62
- 238000001020 plasma etching Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000004381 surface treatment Methods 0.000 claims abstract description 17
- 239000001257 hydrogen Substances 0.000 claims description 22
- 229910052739 hydrogen Inorganic materials 0.000 claims description 22
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
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- 238000001291 vacuum drying Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 7
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- 229910000831 Steel Inorganic materials 0.000 claims 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
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- 238000002604 ultrasonography Methods 0.000 claims 1
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- 238000005516 engineering process Methods 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 description 14
- 239000013078 crystal Substances 0.000 description 11
- 239000007789 gas Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 8
- 238000001069 Raman spectroscopy Methods 0.000 description 7
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- 239000004575 stone Substances 0.000 description 4
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 2
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Crystals, And After-Treatments Of Crystals (AREA)
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Abstract
A kind of method that plasma etching graphite prepares diamond particles, the present invention relates to diadust growing technology fields.The problem that diamond cost is higher, quality is relatively low, is not easy to disperse, technique is uncontrollable, substrate selection is limited is prepared the invention solves existing.Method：One, the surface treatment of graphite flake；Two, diamond is prepared on graphite using plasma etching method；Three, disperse diamond particles, that is, complete the method that plasma etching graphite prepares diamond particles.The present invention is used for a kind of method that plasma etching graphite prepares diamond particles.
Description
Technical field
The present invention relates to diadust growing technology fields.
Background technology
Diamond possesses excellent physics, chemical property, such as hardness highest, chemical stability, thermal conductivity and thermal stability
It is good etc. so that it is widely paid close attention to and applied in many fields.However, the natural diamond reserves in nature are limited,
And difficulty is exploited, causes natural diamond expensive, it is difficult to be used for industrialized production.
It manually prepares diamond at present and mostly uses high temperature and pressure (HPHT) method and make catalyst with catalyst using graphite as raw material
Prepare diamond.Diamond prepared by this method contains more impurity (such as catalyst) and fault of construction, of low quality, it is difficult to
Satisfaction is widely applied, especially in high-end fields such as semiconductors.And high temperature and high pressure method equipment is complicated, expensive, danger coefficient
Greatly.
Using Microwave Irradiation Assisted Chemical vapor deposition (MPCVD) method, with microwave-excitation reaction gas, without electrode fouling, work
Make to stablize, be easy to accurately control, it can be compared with preparing high quality diamond under low pressure.CVD method prepares carbon used in diamond
Mainly there is CH in source4、C2H2、CH3OH、C2H5OH、CH3COCH3、CH3COOH, graphite.Currently used carbon source is mainly gaseous carbon source
CH4, after being mixed with hydrogen under microwave action, in matrix surface depositing diamond.The diamond particles that this method generates hold
Easily film forming, and should not detach.And need to increase hydrocarbon gas gas circuit, in experimental implementation diamond is prepared compared with by carbon source of graphite
Method it is cumbersome.And it when using hydrocarbon gas diamond synthesis, needs to control hydrocarbon gas proportion well.If hydrocarbon
Gas concentration is higher, and the diamond quality of synthesis can be caused to decline, and the content of graphite and amorphous carbon increases；If hydrocarbon gas concentration
It is relatively low, it can cause to generate the reduction of diamond rate, the diamond content of synthesis reduces.And graphite does carbon source diamond synthesis purity
Higher, reaction speed is very fast, it is only necessary to single hydrogen source gas, easy to operate, cost reduction.
It is 200 DEG C~1200 DEG C that CVD method, which prepares diamond required temperature, needs to select substrate, Ying Xuan according to temperature requirement
The small material of high temperature resistant, coefficient of thermal expansion is selected, prevents matrix in reaction and cooling procedure from melting or bursting apart, this makes substrate select
Receive many limitations.
Invention content
The invention solves it is existing prepare diamond cost is higher, quality is relatively low, be not easy to disperse, technique is uncontrollable,
The limited problem of substrate selection, and a kind of method that plasma etching graphite prepares diamond particles is provided.
A kind of method that plasma etching graphite prepares diamond particles, specifically follows the steps below：
One, the surface treatment of graphite flake：
Graphite flake adhesive tape is glued and goes to surface layer, is then surpassed respectively using absolute ethyl alcohol, acetone and deionized water successively
Sound cleans 10min~20min, and the graphite flake after cleaning is placed in drying in vacuum drying chamber, done by the graphite flake after being cleaned
Dry temperature is 60 DEG C~80 DEG C, and the time is 15min~30min, and the graphite flake after drying is cooled to room temperature, is surface-treated
Graphite flake afterwards；
Two, diamond is prepared on graphite using plasma etching method：
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, is in hydrogen flow rate
50sccm~1000sccm, temperature are 200 DEG C~1200 DEG C, pressure is 100mbar~500mbar and microwave power is 1800W
Under conditions of~5000W, deposition 30min~for 24 hours, obtain the diamond of plasma etching graphite preparation；
Three, disperse diamond particles：
Diamond prepared by plasma etching graphite is scraped from graphite flake surface, the diamond particles reunited,
With stainless steel mortar grinder and beat diamond particles 25min~35min of reunion, the diamond particles after being ground,
Water bath heating temperature be 50 DEG C~80 DEG C under conditions of, by the diamond particles after grinding be placed in mass percent be 20%~
30min~1h in 70% sulfuric acid, then diamond particles are cleaned with deionized water, until the pH of cleaning solution is 7, it is then sharp successively
It is cleaned by ultrasonic 25min~35min respectively with acetone and alcohol, the diamond particles after being cleaned, finally by the gold after cleaning
Hard rock particle, which is placed in vacuum drying chamber, to be dried, that is, completes the method that plasma etching graphite prepares diamond particles.
The beneficial effects of the invention are as follows：Using solid graphite as carbon source and substrate, etched in the bombardment of hydrogen plasma
Under, diamond particles can be directly grown on graphite.Compared to using gaseous carbon source to grow diamond, graphite had not only made carbon source but also can
Make matrix, saves the trouble of selection substrate material, easy to operate, raising prepares the quality and quantity of diamond, with natural Buddha's warrior attendant
Stone ingredient is almost the same, and size can reach micron order.And the reunion diamond prepared only need to be i.e. dispersible by simple processing.
Compared with other prepare the processing method of diamond, with diamond prepared by hydrogen plasma etching solid graphite method, processing side
Method is simpler, quick, economical, environmental-friendly.
The present invention is used for a kind of method that plasma etching graphite prepares diamond particles.
Description of the drawings
Fig. 1 is that the amplification 10000 of diamond prepared by plasma etching graphite prepared by one step 2 of embodiment is swept again
Retouch electron microscope picture；
Fig. 2 is 1300 times of scannings of amplification of diamond prepared by plasma etching graphite prepared by one step 2 of embodiment
Electron microscope picture；
Fig. 3 is the X-ray diffractogram of diamond prepared by plasma etching graphite prepared by one step 2 of embodiment；1
It is (220) crystal face of diamond for (111) crystal face of diamond, 2,3 be (311) crystal face of diamond, and 4 be diamond
(400) crystal face, 5 be (331) crystal face of diamond；
Fig. 4 is laser Raman spectroscopy figure, and 1 is natural diamond, 2 plasma etchings prepared for one step 2 of embodiment
Diamond prepared by graphite, 3 be the polycrystalline graphite piece described in one step 1 of embodiment；
Fig. 5 is that the diamond particles of high degree of dispersion prepared by embodiment one amplify 1500 times of scanning electron microscope diagram；
Fig. 6 is that the diamond particles of high degree of dispersion prepared by embodiment one amplify 10000 times of scanning electron microscope diagram.
Specific implementation mode
Technical solution of the present invention is not limited to the specific implementation mode of act set forth below, further include each specific implementation mode it
Between arbitrary combination.
Specific implementation mode one：A kind of plasma etching graphite described in present embodiment prepares the side of diamond particles
Method specifically follows the steps below：
One, the surface treatment of graphite flake：
Graphite flake adhesive tape is glued and goes to surface layer, is then surpassed respectively using absolute ethyl alcohol, acetone and deionized water successively
Sound cleans 10min~20min, and the graphite flake after cleaning is placed in drying in vacuum drying chamber, done by the graphite flake after being cleaned
Dry temperature is 60 DEG C~80 DEG C, and the time is 15min~30min, and the graphite flake after drying is cooled to room temperature, is surface-treated
Graphite flake afterwards；
Two, diamond is prepared on graphite using plasma etching method：
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, is in hydrogen flow rate
50sccm~1000sccm, temperature are 200 DEG C~1200 DEG C, pressure is 100mbar~500mbar and microwave power is 1800W
Under conditions of~5000W, deposition 30min~for 24 hours, obtain the diamond of plasma etching graphite preparation；
Three, disperse diamond particles：
Diamond prepared by plasma etching graphite is scraped from graphite flake surface, the diamond particles reunited,
With stainless steel mortar grinder and beat diamond particles 25min~35min of reunion, the diamond particles after being ground,
Water bath heating temperature be 50 DEG C~80 DEG C under conditions of, by the diamond particles after grinding be placed in mass percent be 20%~
30min~1h in 70% sulfuric acid, then diamond particles are cleaned with deionized water, until the pH of cleaning solution is 7, it is then sharp successively
It is cleaned by ultrasonic 25min~35min respectively with acetone and alcohol, the diamond particles after being cleaned, finally by the gold after cleaning
Hard rock particle, which is placed in vacuum drying chamber, to be dried, that is, completes the method that plasma etching graphite prepares diamond particles.
Graphite flake adhesive tape is glued in present embodiment step 1 and goes to surface layer, it is found that is left on adhesive tape
The graphite marking, and the new surface that graphite flake obtains.
It is to utilize microwave excitation in present embodiment step 2, glow discharge is generated in reative cell, makes hydrogen point
Sub- ionization forms hydrogen plasma, diamond is prepared for etching graphite flake.Using Non-contact Infrared Temperature Measurement meter measure etc. from
The temperature on the graphite flake surface under daughter effect；The parameters such as temperature and pressure are realized by certain physics law in reaction cavity
Coupling regulation and control avoid individually regulation and control and cause the difficulties such as heavy workload, inaccuracy.It therefore can be by accurately controlling single pressure
Value changes to realize the adjustment of the parameters such as temperature, plasma density in linkage.The carbon source and substrate of present embodiment
It is graphite, graphite surface that can be after being bombarded by hydrogen plasma after above-mentioned steps obtains the diamond with aggregate structure
Particle.Gas needed for present embodiment is mainly single hydrogen, and the diamond quality to change synthesis also may be used with size
The inert gas of proper content is added, such as helium, argon gas.
To improve the growth rate of diamond, increases the particle size of diamond synthesis, can be ground with diadust
Graphite flake is put into progress ultrasonic wave decentralized processing in the suspension containing diadust by graphite flake；Then this is being carried out
Specific implementation mode step 2 prepares diamond using the method for plasma etching on graphite.
For present embodiment step 3 compared with other diamonds disperse patent, this method is simple and environmentally-friendly, inexpensive.
Diamond size prepared by plasma etching graphite reaches micron order, and growth rate is apparently higher than using Si as substrate
The diamond of preparation, and purity is high, substantially without the impurity such as graphite and amorphous carbon；And the diamond generated easily disperses, and is not necessarily to
By mechanical equipment or chemical reagent, only need simple hand grinding that can be disperseed.Experimental implementation is also relatively easy, is not necessarily to it
His hydrocarbon gas is as carbon source.
The advantageous effect of present embodiment is：Using solid graphite as carbon source and substrate, in hydrogen plasma
Under bombardment etching, diamond particles can be directly grown on graphite.Compared to using gaseous carbon source to grow diamond, graphite was both made
Carbon source can make matrix again, save the trouble of selection substrate material, and easy to operate, raising prepares the quality and quantity of diamond, with
Natural diamond ingredient is almost the same, and size can reach micron order.And the reunion diamond prepared need to only pass through simple processing
It is i.e. dispersible.Compared with other prepare the processing method of diamond, with the Buddha's warrior attendant of hydrogen plasma etching solid graphite method preparation
Stone, processing method are simpler, quick, economical, environmental-friendly.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：Graphite described in step 1
Piece is highly oriented pyrolytic graphite piece, crystalline flake graphite piece, amorphous graphite piece or polycrystalline graphite piece.It is other with one phase of specific implementation mode
Together.
Specific implementation mode three：Unlike one of present embodiment and specific implementation mode one or two：Institute in step 1
The size for the graphite flake stated is 10 × 10 × 1mm to 30 × 30 × 10mm.It is other the same as one or two specific embodiments.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate is 200sccm, temperature is
200 DEG C~1200 DEG C, pressure be 100mbar~500mbar and under conditions of microwave power is 1800W~5000W, deposition
30min~for 24 hours.It is other identical as specific implementation mode one to three.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
Under conditions of 1000sccm, temperature are 900 DEG C, pressure is 100mbar~500mbar and microwave power is 1800W~5000W,
Deposition 30min~for 24 hours.It is other identical as specific implementation mode one to four.
Specific implementation mode six：Unlike one of present embodiment and specific implementation mode one to five：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
Under conditions of 1000sccm, temperature are 200 DEG C~1200 DEG C, pressure is 200mbar and microwave power is 1800W~5000W, sink
Product 30min~for 24 hours.It is other identical as specific implementation mode one to five.
Specific implementation mode seven：Unlike one of present embodiment and specific implementation mode one to six：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
1000sccm, temperature are 200 DEG C~1200 DEG C, pressure is 100mbar~500mbar and microwave power is 1800W~5000W's
Under the conditions of, deposit 12h.It is other identical as specific implementation mode one to six.
Specific implementation mode eight：Unlike one of present embodiment and specific implementation mode one to seven：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate is 200sccm, temperature is
900 DEG C, pressure be 200mbar and under conditions of microwave power is 1800W~5000W, deposit 12h.Other and specific embodiment party
Formula one to seven is identical.
Specific implementation mode nine：Unlike one of present embodiment and specific implementation mode one to eight：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
1000sccm, temperature are 200 DEG C~900 DEG C, pressure is 100mbar~200mbar and microwave power is 1800W~5000W's
Under the conditions of, deposit 30min~12h.It is other identical as specific implementation mode one to eight.
Specific implementation mode ten：Unlike one of present embodiment and specific implementation mode one to nine：It will in step 2
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
1000sccm, temperature are 900 DEG C~1200 DEG C, pressure is 200mbar~500mbar and microwave power is 1800W~5000W's
Under the conditions of, deposition 12h~for 24 hours.It is other identical as specific implementation mode one to nine.
Beneficial effects of the present invention are verified using following embodiment：
Embodiment one：
A kind of method that plasma etching graphite prepares diamond particles follows the steps below：
One, the surface treatment of graphite flake：
Graphite flake adhesive tape is glued and goes to surface layer, is then surpassed respectively using absolute ethyl alcohol, acetone and deionized water successively
Sound cleans 10min, and the graphite flake after cleaning is placed in vacuum drying chamber dry, drying temperature by the graphite flake after being cleaned
It it is 80 DEG C, the graphite flake after drying is cooled to room temperature by time 30min, the graphite flake after being surface-treated；
The graphite flake is polycrystalline graphite piece；
Two, diamond is prepared on graphite using plasma etching method：
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, is in hydrogen flow rate
Under conditions of 200sccm, temperature are 900 DEG C, pressure is 200mbar and microwave power is 3000W, 12h is deposited, plasma is obtained
Body etches diamond prepared by graphite；
Three, disperse diamond particles：
Diamond prepared by plasma etching graphite is scraped from graphite flake surface, the diamond particles reunited,
With stainless steel mortar grinder and beat the diamond particles 30min of reunion, the diamond particles after being ground, in heating water bath
Under conditions of temperature is 80 DEG C, the diamond particles after grinding are placed in 30min in the sulfuric acid that mass percent is 50%, then use
Deionized water cleans diamond particles, until the pH of cleaning solution is 7, then utilizes acetone and alcohol to be cleaned by ultrasonic respectively successively
Diamond particles after cleaning are finally placed in vacuum drying chamber and do by 30min, the diamond particles after being cleaned
It is dry, the diamond particles of high degree of dispersion are obtained, that is, complete the method that plasma etching graphite prepares diamond particles.
Buddha's warrior attendant prepared by the plasma etching graphite of the present embodiment step 2 preparation is characterized using scanning electron microscope
The surface topography of stone, Fig. 1 are the amplification 10000 of diamond prepared by plasma etching graphite prepared by one step 2 of embodiment
Times scanning electron microscope diagram；Fig. 2 is putting for diamond prepared by plasma etching graphite prepared by one step 2 of embodiment
Big 1300 times of scanning electron microscope diagrams；The substance of generation has apparent Buddha's warrior attendant it can be seen from Fig. 1 and Fig. 2 test results
Stone pattern, size reach tens microns, hence it is evident that are more than the size (several microns) of the diamond particles prepared with gaseous carbon source.
The plasma prepared using X-ray diffraction (X-Ray Diffraction, XRD) detection the present embodiment step 2
The crystalline component of diamond prepared by graphite is etched, crystal orientation and film crystallize integrity degree；Fig. 3 is one step 2 system of embodiment
The X-ray diffractogram of diamond prepared by standby plasma etching graphite；1 is (111) crystal face of diamond, and 2 be diamond
(220) crystal face, 3 be diamond (311) crystal face, 4 be diamond (400) crystal face, 5 be diamond (331) crystal face；By
Fig. 3 test results see, (111) of the diamond, characteristic peak of (220), (311), (400), (331), almost without non-diamond
The peaks XRD of phase.
The present embodiment step 2 system is characterized using laser Raman spectroscopy (Laser Raman Spectroscopy, Raman)
The problem of composition content and integrality of diamond prepared by standby plasma etching graphite, material structure will not be destroyed；Fig. 4
It is natural diamond for laser Raman spectroscopy figure, 1,2 be prepared by plasma etching graphite prepared by one step 2 of embodiment
Diamond, 3 be the polycrystalline graphite piece described in one step 1 of embodiment；Seen by Fig. 4 test results, 1332cm-1Place is typical
Diamond peak, in 1323cm-1And 1567cm-1Place is the peaks D and the peaks G of graphite respectively, and the peaks diamond Raman of generation are
1331cm-1, the 1332cm with natural diamond-1The peaks Raman are almost the same.
As known from the above, diamond quality prepared by the plasma etching graphite that prepared by the present embodiment step 2 is higher,
Almost the same with natural diamond ingredient, size can reach micron order.
The diamond particle surfaces pattern of high degree of dispersion manufactured in the present embodiment, Fig. 5 are characterized using scanning electron microscope
Amplify 1500 times of scanning electron microscope diagram for the diamond particles of the high degree of dispersion of the preparation of embodiment one, Fig. 6 is embodiment
The diamond particles of one high degree of dispersion prepared amplify 10000 times of scanning electron microscope diagram；As seen from the figure, the present embodiment system
Standby diamond particles are easy dispersion, and dispersion effect is good.
Claims (2)
1. a kind of method that plasma etching graphite prepares diamond particles, it is characterised in that a kind of plasma etching graphite
The method for preparing diamond particles follows the steps below：
One, the surface treatment of graphite flake：
Graphite flake adhesive tape is glued and goes to surface layer, then utilizing absolute ethyl alcohol, acetone and deionized water successively, ultrasound is clear respectively
10min~20min is washed, the graphite flake after cleaning is placed in vacuum drying chamber dry, dry temperature by the graphite flake after being cleaned
Degree is 60 DEG C~80 DEG C, and the time is 15min~30min, the graphite flake after drying is cooled to room temperature, after being surface-treated
Graphite flake；
Graphite flake described in step 1 is highly oriented pyrolytic graphite piece, crystalline flake graphite piece, amorphous graphite piece or polycrystalline graphite piece；
The size of graphite flake described in step 1 is 10 × 10 × 1mm to 30 × 30 × 10mm；
Two, diamond is prepared on graphite using plasma etching method：
Graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus, hydrogen flow rate be 50sccm~
Under conditions of 1000sccm, temperature are 900 DEG C, pressure is 200mbar and microwave power is 1800W~5000W, deposition 12h~
For 24 hours, the diamond of plasma etching graphite preparation is obtained；
Three, disperse diamond particles：
Diamond prepared by plasma etching graphite is scraped from graphite flake surface, the diamond particles reunited, with not
Rust steel mortar grinds and beats diamond particles 25min~35min of reunion, the diamond particles after being ground, in water-bath
Under conditions of heating temperature is 50 DEG C~80 DEG C, it is 20%~70% that the diamond particles after grinding, which are placed in mass percent,
30min~1h in sulfuric acid, then diamond particles are cleaned with deionized water, until the pH of cleaning solution is 7, acetone is then utilized successively
And alcohol is cleaned by ultrasonic 25min~35min respectively, the diamond particles after being cleaned, finally by the diamond after cleaning
Grain, which is placed in vacuum drying chamber, to be dried, that is, completes the method that plasma etching graphite prepares diamond particles.
2. the method that a kind of plasma etching graphite according to claim 1 prepares diamond particles, it is characterised in that
The graphite flake after surface treatment is placed in microwave plasma chemical vapor phase growing apparatus in step 2, is in hydrogen flow rate
Under conditions of 200sccm, temperature are 900 DEG C, pressure is 200mbar and microwave power is 1800W~5000W, 12h is deposited.
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| CN1084489A (en) * | 1993-08-23 | 1994-03-30 | 复旦大学 | A kind ofly prepare adamantine method from graphite or carbonaceous solid matter |
| US5527559A (en) * | 1994-07-18 | 1996-06-18 | Saint Gobain/Norton Industrial Ceramics Corp. | Method of depositing a diamond film on a graphite substrate |
| CN1559892A (en) * | 2004-03-12 | 2005-01-05 | 中国科学院上海应用物理研究所 | Process of carbon nano-structure body transforming into nano-diamond |
| CN103482623A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing nano diamonds by using direct-current arc process |
| CN105624642A (en) * | 2016-03-16 | 2016-06-01 | 大连理工大学 | Method for directly depositing diamond film on graphite substrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1084489A (en) * | 1993-08-23 | 1994-03-30 | 复旦大学 | A kind ofly prepare adamantine method from graphite or carbonaceous solid matter |
| US5527559A (en) * | 1994-07-18 | 1996-06-18 | Saint Gobain/Norton Industrial Ceramics Corp. | Method of depositing a diamond film on a graphite substrate |
| CN1559892A (en) * | 2004-03-12 | 2005-01-05 | 中国科学院上海应用物理研究所 | Process of carbon nano-structure body transforming into nano-diamond |
| CN103482623A (en) * | 2013-09-05 | 2014-01-01 | 大连理工大学 | Method for preparing nano diamonds by using direct-current arc process |
| CN105624642A (en) * | 2016-03-16 | 2016-06-01 | 大连理工大学 | Method for directly depositing diamond film on graphite substrate |
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