CN104630899B - The separation method of diamond layer - Google Patents
The separation method of diamond layer Download PDFInfo
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- CN104630899B CN104630899B CN201510023495.4A CN201510023495A CN104630899B CN 104630899 B CN104630899 B CN 104630899B CN 201510023495 A CN201510023495 A CN 201510023495A CN 104630899 B CN104630899 B CN 104630899B
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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
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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
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/04—After-treatment of single crystals or homogeneous polycrystalline material with defined structure using electric or magnetic fields or particle radiation
Abstract
The invention discloses a kind of separation method of diamond layer, this method comprises the following steps：Using laser to carrying out two-dimensional scan inside pending diamond, in pending diamond surface certain depth below formation non-diamond layer；Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond.Diamond substrate surface will not be destroyed using this method, compared with laser cutting technique, the loss in diamond cut is reduced；Compared with ion implanting isolation technics, cost saved, shortened process time.
Description
Technical field
The invention belongs to technical field of semiconductors, and in particular to the separation method of diamond layer.
Background technology
Diamond is as sintered carbide tools, and the substrate of electronic device, application in the industry is quite varied.In all applications
In, it is intended to use large dimond as raw material.For polycrystalline diamond, the polycrystalline substrates more than 2 inches are
Through that can synthesize, and as optical window, the field such as sintered carbide tools.On the other hand, single-crystal diamond substrate is by natural
Or diamond synthesis is using formed by the method dicings such as laser cutting, cleavage.As needed, corresponding surface is entered
Row polishing.However, it is known that natural diamond is very rare, large scale natural diamond price is again very expensive.Enter
One step says that although HTHP diamond synthesis is widely used in each industrial circle, but this method has one again
Fixed limitation, such as synthesis rate are slow, and as size increases, yield can drastically decline.Therefore, 1 × 1cm2Monocrystalline almost
As the limit.The HTHP diamond synthesis being commercially used, common size is usually 5 × 5mm2。
It is currently reported using the method high speed synthetic single crystal diamond of chemical vapor deposition (CVD), add in growth
Enter a small amount of nitrogen, adjust growth technique, the speed of growth of diamond can be caused more than 150 μm/h [1].Using this method,
The crystal thickness of synthesis can be caused more than 1cm [2].Can be in CVD furthermore with the technology of CVD method synthetic single crystal diamond
Cavity constructions are easier to increase the area of diamond synthesis in the case of expanding.By controlling technique, it is a small amount of miscellaneous that adjustment is imported
Matter gas, can carry out epitaxial growth with large area high-speed.Microwave plasma CVD (MPCVD) is big at present
Most common technology in area single crystal diamond film, with reference to three dimensional growth and the spelling that diamond is carried out on HTHP substrate
Connection technology, the single-crystal diamond size that current large area deposition technology is obtained has had arrived at 2 inches [3].
Therefore, large area monocrystalline can further be obtained by large area deposition technology on HTHP diamond crystal
Diamond substrate.So, then using large area single-crystal diamond substrate as kind of a crystalline substance, by the method for stripping by the list of epitaxial growth
Diamond layer is separated from kind of crystalline substance, so as to obtain the commercialization substrate used in industry and research.
As described above, on the single-crystal diamond crystals synthesized by chemical vapour deposition technique, required for cutting us
Diamond substrate, commonly used approach is laser cutting, diamond saw cutting etc..When being cut using these methods, cutting area
The lesion thickness in domain arrives hundreds of microns tens of, and such thickness is suitable with semiconductive substrate thickness, substantially reduces
Plant brilliant utilization ratio.It is therefore desirable to find new cutting method, the loss caused in cutting process is reduced as far as possible.
The team such as Fairchild and Mokuno are it has been reported that use energetic carbon ions or He isotopic geochemistry to diamond
It is then rotten using electrochemistry in underlayer surface certain depth below formation non-diamond layer, then in high temperature after annealing in substrate
The method of erosion erodes non-diamond layer so that Buddha's warrior attendant stone surface separates [4,5] from original diamond substrate.But, it is required
Energy is about that 3MeV grades of high energy implanters are very expensive, and the ion implanting time is also very long, so using ion implanting
Method separation diamond is restricted in commercial Application and scientific research.
Bibliography
[1]“High optical quality multicarat single crystal diamond produced
by chemical vapor deposition”Yu-fei Meng*,Chih-shiue Yan,Szczesny Krasnicki
Phys.Status Solidi A 209,No.1,101–104(2012)
[2]“Synthesizing single-crystal diamond by repetition of high rate
Homoepitaxial growth by microwave plasma CVD”Y.Mokuno*,A.Chayahara,Y.Soda,
Y.Horino,N.Fujimori.Diamond&Related Materials 14(2005)1743–1746
[3]“A 2-in.mosaic wafer made of a single-crystal diamond”H.Yamada,
A.Chayahara,Y.Mokuno,Y.Kato,and S.Shikata.Applied Physics Letters 104,102110
(2014)
[4]“Fabrication of Ultrathin Single-Crystal Diamond Membranes**”
Barbara A.Fairchild,*Paolo Olivero,Sergey Rubanov.Adv.Mater.2008,20,4793–
4798.
[5]"Synthesis of large single crystal diamond plate by high rate
homoepitaxial growth using microwave plasma CVD and lift-off process"
Y.Mokuno,A.Chayahara,H.Yamada.Diamond&Related Materials 17(2008)415–418.
The content of the invention
The technical problems to be solved by the invention are that there is provided a kind of diamond layer for above-mentioned the deficiencies in the prior art
Separation method, diamond surface will not be destroyed using this method, compared with laser cutting technique, reduced in diamond cut
Loss；Compared with ion implanting isolation technics, cost saved, shortened process time.
In order to solve the above technical problems, the technical solution adopted by the present invention is, the separation method of diamond layer, this method bag
Include following steps：
Using laser to carrying out the diamond lattic structure at two-dimensional scan, destruction scanning inside pending diamond, treating
The diamond surface certain depth below formation non-diamond layer of processing；Non-diamond layer is removed, to realize to above-mentioned Buddha's warrior attendant
The separation up and down of stone.
Further, using the method erosion removal of electrochemical corrosion non-diamond layer.
Further, before non-diamond layer is removed, pending diamond is annealed in >=800 DEG C of vacuum, made
Obtain non-diamond layer graphitization.
Further, be using the energy density of laser：Breakdown threshold-the 1.2J/cm of pending diamond2。
Further, the depth of the non-diamond layer of the formation is lower 1 μm -10 μm of top layer, and thickness is 100nm-10 μm.
Further, the surface area of the non-diamond layer is less than or equal to the surface area of diamond.
Further, the diamond is polycrystalline structure or mono-crystalline structures, while can be the natural diamond of insulation
Or the diamond of insulation.
Further, the laser is femtosecond laser or wide laser pulse.
Present invention also offers the application of the separation method of diamond layer, for peeling off diamond substrate top layer.
It is outer in diamond substrate for peeling off present invention also offers another application of the separation method of diamond layer
Epitaxial growth diamond layer, be specifically：Using laser to being carried out inside pending diamond substrate at two-dimensional scan, destruction scanning
Diamond lattic structure, in pending diamond substrate surface certain depth below formation non-diamond layer；In diamond substrate
The certain thickness diamond layer of surface epitaxial growth；Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond,
Obtain the Buddha's warrior attendant stone lining below diamond substrate and Epitaxial Growth of Diamond layer and non-diamond layer more than non-diamond layer
Bottom.
A kind of method for peeling off diamond of the invention, has the following advantages that：1. in the short time can more than 3mm ×
The epitaxial growth gold in thin layer of diamond (i.e. diamond substrate top layer) or diamond substrate is peeled off on more than 3mm diamond
Hard rock layer, and then form the ability of large area single-crystal diamond batch production.2. do not influenceed by diamond crystal structures.3. with
Existing laser cutting technique is compared, and substantially reduces the loss in diamond cut.Compared with ion implanting isolation technics, save
Cost, shortens process time.4. due to can easily peel off diamond layer, industrially realizing to repeatedly use
Diamond or epitaxial layer, do not result in waste.5. what preferred femtosecond laser was utilized is avalanche ionization or multiphoton ionization
Etc. nonlinear effect, its process is not in fusion process, can carry out micron even nanoscale retrofit.
Brief description of the drawings
Fig. 1 is the schematic diagram that the laser system selected by non-diamond is formed in diamond in the present invention；
Fig. 2 is electrochemical corrosion system in the present invention；
Fig. 3 is the metallograph of the non-diamond layer inside the diamond obtained by the embodiment of the present invention.
Wherein：1. attenuator；2. spectroscope；3. power meter；4. condenser lens；5. displacement platform；6. motor driver；7.
Control device；8. laser；9. regenerative amplifier；10. speculum, 11. containers, 12. electrodes；Diamond sample after 13 scannings；
14 power supplys；15. non-diamond layer, 16 diamonds.
Embodiment
The separation method of diamond layer of the present invention, this method comprises the following steps：Using laser to pending diamond
Inside carries out the diamond lattic structure at two-dimensional scan, destruction scanning, is formed in pending diamond surface certain depth below
Non-diamond layer；Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond.Wherein it is possible to using electrochemistry
The method erosion removal of corrosion non-diamond layer.Before non-diamond layer is removed, to pending diamond at >=800 DEG C
Annealed in vacuum so that non-diamond layer graphitization.
Present invention also offers the application of the separation method of diamond layer, for peeling off diamond substrate top layer.Also it can use
In peeling off the layer of the Epitaxial Growth of Diamond in diamond substrate, it is specifically：Using laser to pending diamond substrate inside
The diamond lattic structure at two-dimensional scan, destruction scanning is carried out, is formed in pending diamond substrate surface certain depth below
Non-diamond layer；Using methods such as chemical vapour deposition techniques in the certain thickness diamond of diamond substrate surface epitaxial growth
Layer；Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond, Buddha's warrior attendant stone lining more than non-diamond layer is obtained
Diamond substrate below bottom and Epitaxial Growth of Diamond layer and non-diamond layer.Above two application only increases outer
The step of prolonging production diamond layer, remaining step all same, meanwhile, need to peel off Buddha's warrior attendant in other equally applicable industry of the present invention
Application during rock layers.
In the separation method of the bright diamond layer of we：
1. the selection of diamond
Diamond can be the natural diamond of insulation or the diamond of insulation, can be single crystal diamond
Stone can also be polycrystalline diamond.In single-crystal diamond, there are different crystal faces (100) (111), can also exist at crystal face
Inclination angle, the present invention can be applicable.
2. the formation of non-diamond layer
Using laser two-dimension scanning diamond, a large amount of free electrons are formed by Multiphoton Absorbtion process, in strong laser field
Under the conditions of, occur light and puncture so that sp in diamond3Key is to sp2Key changes.
It is as shown in Figure 1 a kind of laser system formed in diamond selected by non-diamond, including laser 8, again
Raw amplifier 9, attenuator 1 and condenser lens 4, the laser 8 are used to launch to be disposed with laser, the laser optical path
Regenerative amplifier 9, speculum 10 and attenuator 1, the emergent light side of the attenuator 1 are provided with spectroscope 2, and the emergent light shines
Penetrate and be divided into two-way on spectroscope 2, wherein laser is transmitted into power meter 3 all the way, another road laser reflection enters condenser lens
4, the light emission side of condenser lens 4 is provided with the displacement platform 5 for placing pending diamond, the road laser line focus lens 4
Focus on inside pending diamond, displacement platform 5 is also connected with motor driver 6；Laser 8 also with the phase of control device 7
Connection.It should be noted that being not limited to a certain laser system in the present invention, swashing for condition can also be met from other
Photosystem.
It is specific as follows：Titanium-doped sapphire (Ti:Sapphire, hereinafter referred to as Ti∶Sapphire laser) laser produce laser regeneration
Under amplifier amplification, single pulse energy reaches 3.7mJ, pulse width 50fs, by selecting attenuator, reaches laser energy
Breakdown threshold or the above (the natural diamond light breakdown threshold of diamond：0.4J/cm2, cvd diamond light breakdown threshold：
0.3J/cm2), then will be certain below Laser Focusing to diamond surface by condenser lens 4 and high-precision three-dimensional displacement platform 5
In depth, and carry out two-dimensional scan.
In the process, it is crucial to select suitable pulsed laser energy scanning diamond, and energy is less than threshold value, and laser is not
It is enough to cause light to puncture, energy is too high, then can damages diamond surface.Laser energy density is typically chosen from threshold value to 1.2J/
cm2In the range of.
Laser Focusing depth is determined by condenser lens 4 and displacement platform 5, in order to realize the repetition of diamond repeatedly in industry
Use, the depth of focus is chosen at 1 μm of -10 μ m below Buddha's warrior attendant stone surface.The thickness of non-diamond layer is by energy density and sweeps
Retouch speed to together decide on, the thickness of non-diamond layer is directly proportional in the timing of sweep speed one to energy density；In energy density one
Timing is inversely proportional with sweep speed.Sweep speed can be selected in 10 μm/s-100 μm/s according to experiment needs.Non-diamond layer
Thickness it is thinner, the loss to pending diamond is smaller, but is due to the limitation of process conditions, the thickness of non-diamond layer
It can control in 100nm-10 μ ms.
After being focused on to diamond and carrying out two-dimensional scan, focal plane diamond lattic structure in diamond is punctured due to light
And be destroyed, non-diamond structure is formed, the non-diamond in diamond can be so removed using methods such as electrochemical corrosion
Layer.
After Laser Processing diamond formation non-diamond layer, pending diamond is integrally moved back in >=800 DEG C of vacuum
After fire so that non-diamond layer graphitization, so as to accelerate Electrochemical corrosion rate.
3. epitaxial growth
After diamond is by laser scanning manufacturing, microwave plasma CVD technology is used on the diamond
(MPCVD) epitaxial growth single-crystal diamond film.Although mentioning microwave plasma growth technology here, here not
The technology is confined to, such as utilizes HF CVD, direct current CVD etc..As special case, given birth to using microwave plasma CVD come extension
It is long, can be with the high-quality high-purity single crystal diamond diaphragm of epitaxial growth under specific growth conditions., can as growth gasses
To use the mixed gas of such as hydrogen and methane.For further, appropriate nitrogen is added, growth can be increased substantially
Speed, and can also draw up abnormal nucleation and misgrowth, can be in the short time particularly in the case of single-crystal diamond
It is interior to cause crystal growth to reach required thickness.The ratio of gas is generally：CH4/H2For 1%-20%；N2/CH4For 0-3%.
Here particular growth condition above-mentioned is illustrated, the frequency of the microwave plasma CVD used, generally
For 2.45GHz or 915MHz etc., for power, do not make special restriction here, be generally 0.5KW-30KW.Herein
In the case of, according to CVD structural adjustment power so that temperature reaches 900 DEG C -1250 DEG C.Maintain diamond at this temperature, can
To promote the non-diamond layer graphitization of Laser Processing.
4. electrochemical corrosion non-diamond layer
According to the method described above, diamond substrate will form non-Buddha's warrior attendant after laser action under the certain depth below of surface
Rock layers.The substrate is put into the container for fill electrolyte and carries out electrochemical corrosion.Detailed process is as follows：
As shown in Fig. 2 electrochemical corrosion system includes AC or DC power 14, graphite or platinum electrode 12, appearance
Diamond sample 13 is vertically placed in the middle of electrode after device 11 and electrolyte, scanning, and the electrolyte of addition is high resistance (~18
Ω cm) solution, addition will flood diamond-like 13.Institute's making alive is controlled by power supply 14 on electrode 12, typically to cause two
Interelectrode electric field reaches certain value.Electric field is bigger, and corrosion rate is faster.But voltage is too high, it may result in and put between electrode
Electricity, easily causes damage to diamond surface.During electrochemical corrosion, over time, electrolyte absorbs empty
CO in gas2So that bath resistance declines, and is risen by the electric current of electrolyte, increased air bubble in solution, bubble can wrap up sample
Product, so as to be unable to reach the effect of corrosion.At the same time the electric current increased can produce very big heat so that electrolyte is heated to
Boiling.So to change electrolyte in time in corrosion process so that electric current is maintained in the range of 0~1A.
EXPERIMENTAL EXEMPLIFICATIONThe：
In the present embodiment, specific is 3 × 3 × 0.3mm from a size3Single-sided polishing single-crystal diamond substrate is commercialized,
Acid treatment is carried out first, clears up burnishing surface.Then diamond substrate alcohol, acetone, deionized water are cleaned by ultrasonic.
Then, using femtosecond laser system of processing by Laser Focusing under diamond surface in certain depth, and carry out two-dimensional scan.It is burnt
About 8 μm of laser spot diameter at point, focus is under the surface at 10 μm, average laser power about 9mW at sample surfaces, sweep speed
40 μm/s, sweep span is 7 μm.The color of diamond becomes black by pale yellow after scanning, with electronic scanner microscope to its section
Face is observed, and obvious boundary layer, such as Fig. 3 are found that in focal plane, and this illustrates to there occurs that light is hit in diamond 16
Wear, form non-diamond layer 15.
Diamond after femtosecond laser is processed, which is put into microwave plasma CVD chamber, carries out epitaxial growth.Before growth,
In hydrogen plasma atmosphere, substrate surface temperature is adjusted to 1000 DEG C and anneal within five minutes, one side cleaning diamond
Substrate surface, on the other hand promotes the graphitization of non-diamond layer, then carries out epitaxial growth.Microwave power is in 5kW or so, chamber
Body pressure set is 150torr, and hydrogen flowing quantity is 500sccm, and methane is 50sccm, in order to accelerate the speed of growth, in growth
A certain amount of nitrogen of artificial addition, addition is 1.0sccm here, and growth temperature is controlled at 1200 DEG C or so.Grow 12h
Afterwards, epitaxial growth thickness reaches 0.58mm.
Then, the diamond sample after epitaxial growth is put into electrochemical corrosion system.Using platinum as electrode, sample
Product are vertical with platinum electrode, and the spacing of electrode is in 1cm or so.With deionized water as electrolyte, the amount of addition will flood Buddha's warrior attendant
Stone sample.1000V AC power is connected on electrode, is corroded.Deionized water is regularly changed in corrosion.In corrosion
After 5h, black is decorporated in sample, and epitaxial diamond layer is separated with diamond substrate.
Claims (8)
1. the separation method of diamond layer, it is characterised in that this method comprises the following steps：
Using laser to carrying out the diamond lattic structure at two-dimensional scan, destruction scanning inside pending diamond, pending
Diamond surface certain depth below formation non-diamond layer；
Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond；
Using the method erosion removal of electrochemical corrosion non-diamond layer；
Before non-diamond layer is removed, pending diamond is annealed in >=800 DEG C of vacuum so that non-diamond layer stone
Mo Hua.
2. according to the separation method of the diamond layer described in claim 1, it is characterised in that use the energy density of laser
For：Breakdown threshold~1.2J/cm of pending diamond2。
3. according to the separation method of the diamond layer described in claim 1, it is characterised in that the non-diamond layer of the formation
Depth is lower 1 μm -10 μm of top layer, and thickness is 100nm-10 μm.
4. according to the separation method of the diamond layer described in claim 1, it is characterised in that the surface area of the non-diamond layer
Less than or equal to the surface area of diamond.
5. according to the separation method of the diamond layer described in claim 1, it is characterised in that the diamond be polycrystalline structure or
Person's mono-crystalline structures, while can be the natural diamond of insulation or the diamond of insulation.
6. according to the separation method of the diamond layer described in claim 1, it is characterised in that the laser be femtosecond laser or
Wide laser pulse.
7. the application of the separation method of the diamond layer as described in claim 1 to 6 is any, it is characterised in that for peeling off gold
Hard rock underlayer surface.
8. the application of the separation method of the diamond layer as described in claim 1 to 6 is any, it is characterised in that for peeling off gold
Epitaxial Growth of Diamond layer on hard rock substrate, be specifically：
Using laser to carrying out the diamond lattic structure at two-dimensional scan, destruction scanning inside pending diamond substrate, treating
The diamond substrate surface certain depth below formation non-diamond layer of processing；
In the certain thickness diamond layer of diamond substrate surface epitaxial growth；
Non-diamond layer is removed, to realize the separation up and down to above-mentioned diamond, diamond more than non-diamond layer is obtained
Diamond substrate below substrate and Epitaxial Growth of Diamond layer and non-diamond layer.
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| CN201510023495.4A CN104630899B (en) | 2015-01-17 | 2015-01-17 | The separation method of diamond layer |
| PCT/CN2015/077120 WO2016112596A1 (en) | 2015-01-17 | 2015-04-21 | Separation method for diamond layer |
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| WO2019038754A1 (en) | 2017-08-22 | 2019-02-28 | Diamtech Ltd. | System and method for creation of a predetermined structure from a diamond bulk |
| CN111996581B (en) * | 2020-07-08 | 2021-10-26 | 西安电子科技大学 | Loss-free rapid separation method for single crystal diamond and substrate |
| CN112430803B (en) * | 2020-11-16 | 2022-04-01 | 北京科技大学 | Preparation method of self-supporting ultrathin diamond film |
| CN115491764B (en) * | 2022-09-29 | 2024-01-30 | 中国电子科技集团公司第十三研究所 | Method for stripping epitaxial diamond and GaN material |
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| CN104630899A (en) | 2015-05-20 |
| WO2016112596A1 (en) | 2016-07-21 |
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