CN104831253B - Single granule layer nanometer diamond film with strong Si-V luminescence, and production method thereof - Google Patents
Single granule layer nanometer diamond film with strong Si-V luminescence, and production method thereof Download PDFInfo
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Abstract
The invention provides a single granule layer nanometer diamond film with strong Si-V luminescence, and a production method thereof. The method comprises the following steps: producing a single granule layer nanometer diamond film with the thickness of 500-700nm on a monocrystalline silicon substrate by adopting a hot filament chemical vapor deposition technology; and carrying out heat insulation on the film in 600DEG C air for 10-50min to produce the single granule layer nanometer diamond film with strong Si-V luminescence. The nanometer diamond film obtained in the invention has single granule layer characteristics and has a thickness of 500-700nm, the speak shape of the Si-V luminescence peak of the film is sharp, the Si-V luminescence intensity is greatly improved, and the preparation is of great scientific and engineering significance to realize application of the film in fields of single photon sources, quantum information processing, photoelectron devices, biological markers, semiconductor devices and field emission displays.
Description
(1) technical field
The present invention relates to a kind of individual particle with strong Si-V luminous (luminous peak position in photoluminescence spectrum is in 738nm)
Layer nano-diamond film and preparation method thereof.
(2) background technology
Silicon-room (Si-V) center in diamond, the luminous peak position in photoluminescence spectrum (PL spectrums) is in 738nm, line
Wide narrower (～5nm), luminescent lifetime very short (1.2ns) so that the Si-V centres of luminescence become the single-photon source of great potential, in amount
The fields such as sub-information process, opto-electronic device, biomarker, semiconductor device and field-emitter display have wide application
Prospect.
Optically active defect is built in Nano diamond crystal grain, it is possible to obtain with higher narrower luminous single light
The thin film of activity is learned, is that the micro-nano and miniaturization for realizing opto-electronic device lays the foundation.It is prepared by chemical vapor deposition (CVD)
In nano-diamond film, the Si-V centres of luminescence are typically in thin film growth process, by the silicon in substrate or quartz ampoule with non-
The form of doping enters thin film and is formed intentionally；This uncontrollable unintentionally doping way causes some thin film to have Si-V
It is luminous, and the Si-V luminescent properties that some thin film do not have Si-V luminescent properties, i.e. thin film are difficult to control to.In early-stage Study,
The nano-diamond film not lighted with Si-V to preparing carries out the oxidation processes of uniform temperature, obtains Si-V and sends out
Light；Result of study also shows that the surface termination state of thin film lights to its Si-V and has more important impact；That is hydrogen end of film surface
It is only luminous to Si-V to have inhibitory action, and oxygen terminates then being conducive to Si-V to light.In early-stage Study be to thickness be 3-10 μm
Nano-diamond film carries out oxidation processes；The thickness of these thin film is larger, and micro structure and composition are complex, aoxidizes rear film
Si-V luminous intensities it is high not enough, it is difficult to meet the demand of photovoltaic applications, need further to improve Si-V in thin film luminous
Intensity.Therefore, the present invention intends the thickness for reducing thin film, and in thin film growth process, control surface terminates state, explores with strong
The preparation method of the nano-diamond film of Si-V luminescent properties, for realizing nano-diamond film in single-photon source, quantum
The application in the fields such as information processing, opto-electronic device and field-emitter display has highly important scientific meaning and engineering valency
Value.
In the granted patent of applicant " a kind of N-type nano-diamond film and preparation method " (ZL200910155306.3)
In, propose donor impurity ion is injected in nano-diamond film, and vacuum annealing is carried out to thin film (thickness is 4～10 μm)
Process, obtain that resistivity is relatively low, the higher N-type nano-diamond film of mobility.The patent is related to vacuum annealing and thin film
Electric property, be not directed to the Si-V luminescent properties of thin film.The application adopts hot-wire chemical gas-phase deposition method, preparation to obtain
Obtained the thin film (thickness is 500-700nm) of a granular layer thickness, i.e. individual particle layer nano-diamond film；And thin film is entered
Oxidation processes in row air, effectively increase the Si-V luminescent properties of thin film.Receive without reference to individual particle layer in document at present
The preparation of rice diamond thin.
(3) content of the invention
It is an object of the invention to provide one kind lights with strong Si-V, and (Si-V is luminous to be referred in photoluminescence spectrum (PL spectrums)
Characteristic peak is located at 738nm, live width narrower (～5nm), luminescent lifetime very short (1.2ns) so that Si-V becomes great potential
Single-photon source) individual particle layer nano-diamond film and preparation method.
The technical solution used in the present invention is：
A kind of preparation method of the individual particle layer nano-diamond film lighted with strong Si-V, methods described includes following
Step：(1) using hot-wire chemical gas-phase deposition method, the individual particle layer that thickness is 500-700nm is prepared on a monocrystaline silicon substrate
Nano-diamond film；(2) the individual particle layer nano-diamond film for obtaining step (1) is in the air at a temperature of 600 DEG C
Insulation 10～50 minutes, that is, be obtained the individual particle layer nano-diamond film lighted with strong Si-V.
The present invention adopts hot-wire chemical gas-phase deposition method, prepares the individual particle layer nanometer Buddha's warrior attendant that thickness is 500-700nm
Stone thin film, and carry out thermal oxidation to thin film in atmosphere, the Si-V luminous intensities of the thin film for preparing are micro- compared with thickness
The Si-V luminous intensities of the nano-diamond film of meter level are greatly enhanced.The program effectively increases nano-diamond film
Si-V luminous intensities.
The present invention also provides a kind of individual particle layer nano-diamond film lighted with strong Si-V, and the thin film is by following
Method is obtained：(1) using hot-wire chemical gas-phase deposition method, it is single of 500-700nm to prepare thickness on a monocrystaline silicon substrate
Granulosa nano-diamond film；(2) sky of the individual particle layer nano-diamond film that step (1) is obtained at a temperature of 600 DEG C
10～50 minutes are incubated in gas, that is, the individual particle layer nano-diamond film lighted with strong Si-V is obtained.
In the step (1), individual particle layer nano-diamond film is using hot-wire chemical gas-phase deposition (HFCVD) method in list
Prepare in crystalline silicon substrate, can be carried out using conventional chemical vapor equipment, it is desirable to the individual particle layer nanometer Buddha's warrior attendant for preparing
Stone film thickness is 500-700nm.
The concrete grammar that general step (1) is adopted is as follows：Monocrystalline silicon piece is polished half an hour using diamond paste, is beaten
Monocrystalline silicon piece after mill successively deionized water and acetone ultrasound wave cleaning, be dried after as nano-diamond film growth lining
Monocrystalline substrate is put into hot-filament chemical vapor deposition equipment by bottom, with acetone as carbon source, using hydrogen bubbling mode by acetone band
Enter in reative cell, wherein hydrogen, the flow-rate ratio of acetone are 200：90, heated filament is 7mm with the distance of monocrystalline substrate, reacts work(
Rate is 2200W, and operating air pressure is 1.63Kpa；Thin film growth time is 15～20 minutes；Not biasing during the course of the reaction；It is raw
After length terminates, the cooling down under conditions of obstructed hydrogen prepares the individual particle layer nanometer Buddha's warrior attendant that thickness is 500-700nm
Stone thin film.
The hot-filament chemical vapor deposition equipment is purchased from Shanghai Jiaoyou Diamond Coating Co., Ltd., model JUHF CVD
001。
The step (2) is preferably one of following operational approach：
I individual particle layer nano-diamond film that step (1) is obtained by () is incubated 20 points in the air at a temperature of 600 DEG C
Clock, that is, be obtained the individual particle layer nano-diamond film lighted with strong Si-V；
(ii) the individual particle layer nano-diamond film that step (1) is obtained is incubated into 30 in the air at a temperature of 600 DEG C
Minute, that is, the individual particle layer nano-diamond film lighted with strong Si-V is obtained；
(iii) the individual particle layer nano-diamond film that step (1) is obtained is incubated into 50 in the air at a temperature of 600 DEG C
Minute, that is, the individual particle layer nano-diamond film lighted with strong Si-V is obtained.
The beneficial effects are mainly as follows：(1) using hot-wire chemical gas-phase deposition method, thickness is prepared for 500-
The individual particle layer nano-diamond film of 700nm, thin film have Si-V glow peaks at 738nm, and more non-luminous thickness is 3-
10 μm of nano-diamond film has substantial advance.(2) by individual particle layer nano-diamond film uniform temperature air
Middle held for some time so that nano-diamond film is luminous with very strong Si-V, the Si-V of more non-oxide film are luminous strong
Degree improves 10-20 times；Its Si-V luminous intensity is improve compared with the nano-diamond film of the micron order thickness after oxidation
About 20 times.(3) the individual particle layer nano-diamond film lighted with strong Si-V that the present invention is prepared, obtains a kind of new
Film type, provide new approaches for application of the nano-diamond film in fields such as photoelectrons.
The present invention program is simple, easily operated, solves the Si-V photisms of the thin film that chemical vapor deposition is prepared
The low problem of the unstable and luminous intensity of energy, is to prepare Nano diamond opto-electronic device to lay a good foundation.The list for preparing
The Si-V luminous intensities of granular layer nano-diamond film are stronger, for realize its single-photon source, quantum information process, photoelectricity
The application in the fields such as sub- device, biomarker, semiconductor device and field-emitter display has highly important scientific meaning
And construction value.
(4) illustrate
Field emission scanning electron microscope (FESEM) photos of the Fig. 1 for the individual particle layer nano-diamond film of embodiment 1.
Section SEM figures of the Fig. 2 for the individual particle layer nano-diamond film of embodiment 1.
Photoluminescence spectrums of the Fig. 3 for the individual particle layer nano-diamond film of embodiment 1, the little figure in its lower-left is thin film
Raman spectrograms.
Fig. 4 is the luminescence generated by light spectrogram of the insulation individual particle layer nano-diamond film of 20 minutes in 600 DEG C of air.
Fig. 5 is the section SEM figures of the insulation individual particle layer nano-diamond film of 20 minutes in 600 DEG C of air.
Fig. 6 is the luminescence generated by light spectrogram of the insulation individual particle layer nano-diamond film of 30 minutes in 600 DEG C of air.
Fig. 7 is the section SEM figures of the insulation individual particle layer nano-diamond film of 30 minutes in 600 DEG C of air.
Fig. 8 is the luminescence generated by light spectrogram of the insulation individual particle layer nano-diamond film of 50 minutes in 600 DEG C of air.
Fig. 9 is the section SEM figures of the insulation individual particle layer nano-diamond film of 50 minutes in 600 DEG C of air.
(5) specific embodiment
With reference to specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in
This：
Embodiment 1：
With nano-diamond powder polishing monocrystalline silicon piece, about half an hour polishing time.The silicon chip polished spend successively from
After sub- water and acetone ultrasonic cleaning, drying, as the substrate of nano-diamond film growth.Using hot-wire chemical gas-phase deposition side
(chemical vapor depsotition equipment is purchased from Shanghai Jiaoyou Diamond Coating Co., Ltd. to method, and 001) model JUHF CVD, with acetone is
Carbon source, is brought into acetone in reative cell using hydrogen bubbling mode, and hydrogen is 200 with the flow-rate ratio of acetone：90, reaction power
For 2200W, heated filament is 7mm with the distance of silicon substrate, and operating air pressure is 1.63Kpa；Not biasing in course of reaction, during preparation
Between be 15 minutes；After growth terminates, to sample cooling down under conditions of obstructed hydrogen, thickness is prepared for 500-700nm
Individual particle layer nano-diamond film.Using surface topography and the section of field emission microscopy observation thin film, using photic
The luminescent properties of luminous spectrum testing film.
Additionally as contrast, the nano-diamond film that thickness is micron level is prepared for, method is as follows：Use nanometer grade gold
Emery polishing monocrystalline silicon piece, about half an hour polishing time.The silicon chip polished after ultrasonic cleaning, as Nano diamond
The substrate of thin film growth.Using hot-wire chemical gas-phase deposition method, (chemical vapor depsotition equipment is purchased from Shanghai friend-making diamond coatings
Company limited), with acetone as carbon source, acetone is brought in reative cell using hydrogen bubbling mode, reaction chamber temperature control exists
600～700 DEG C, preparation time is 5 hours, prepares the nano-diamond film that thickness is 3 μm.Thickness is 3 μm of nanometer gold
Diamond thin film does not have Si-V glow peaks at 738nm.
Field emission scanning electron microscope (FESEM) photos of the Fig. 1 for individual particle layer nano-diamond film, it is seen that thin film is by receiving
The diamond crystalses composition of meter level；Fig. 2 is schemed for the section SEM of thin film, it is known that thin film is made up of single granule, therefore thin film is
Individual particle layer nano-diamond film.The thickness of thin film, about 540nm can be also measured from Fig. 2；Fig. 3 photic for thin film
Spectrogram, adopts wavelength and is tested for the light-emitting mode of the Raman spectrogrphs of 514nm.As can be seen that thin film is at 738nm
There is the individual particle layer nano-diamond film prepared with Si-V glow peaks, i.e. this programme Si-V to light, and thickness is 3 μm
Nano-diamond film does not possess Si-V and lights, it is seen that the individual particle layer nano-diamond film that this programme is prepared has real
Matter progress；But its glow peak is relatively low, the normalized intensity of Si-V glow peaks is (at 738nm at the intensity of glow peak and 540nm
The intensity ratio at peak) for 1.6；Illustrate individual particle layer nano-diamond film that hot-wire chemical gas-phase deposition prepares with compared with
Weak Si-V luminescent properties.The little figure in Fig. 3 lower-lefts is the Raman spectrograms of individual particle layer nano-diamond film, and collection of illustrative plates shows
1332cm-1Place occurs in that diamond characteristic peak, in 1560cm-1Unordered sp also can be observed2The graphite peaks of key, illustrate that thin film is main
By diamond phase and disordered graphite phase composition, it is typical nano-diamond film.
Above-mentioned individual particle layer nano-diamond film is incubated into 20 minutes in 600 DEG C of air, wavelength is adopted for 514nm
Raman spectrum glow peak test is carried out to thin film, as shown in Figure 4.As can be seen that occurring in that very in 738nm or so in spectrogram
Strong glow peak, the normalized intensity of Si-V glow peaks is 8, and more unoxidized individual particle layer film improves a lot.
The nano-diamond film that thickness is 3 μm is aoxidized according to similarity condition, 20 is incubated in 600 DEG C of air
Minute, adopting wavelength for the Raman spectrum of 514nm carries out glow peak test to thin film.As a result its Si-V normalization luminous intensity
Only 0.28, show that the individual particle layer film for aoxidizing 20 minutes has very strong Si-V luminescent properties, the luminous peak intensity of its Si-V
Degree is far above the micron order thin film after oxidation.
Fig. 5 is the section SEM figures of the insulation individual particle layer nano-diamond film of 20 minutes in 600 DEG C of air, it is known that thin
The thickness of film is 350nm, i.e. oxidation causes the thickness of thin film to reduce；Thin film is still made up of one layer of granule, is receiving for individual particle layer
Rice diamond thin.
Embodiment 2：
Using nano-diamond powder polishing monocrystalline silicon piece, about half an hour polishing time.The silicon chip polished is spent successively
Ionized water and acetone after ultrasonic machine is cleaned, is dried, as the substrate of nano-diamond film growth.Using hot-wire chemical gas
Phase deposition process (chemical vapor depsotition equipment be purchased from Shanghai Jiaoyou Diamond Coating Co., Ltd., model JUHF CVD 001),
With acetone as carbon source, acetone is brought in reative cell using hydrogen bubbling mode, hydrogen is 200 with the flow-rate ratio of acetone：90,
Reaction power is 2200W, and heated filament is 7mm with the distance of silicon substrate, and operating air pressure is 1.63Kpa；Not biasing in course of reaction
Pressure, film preparation time are 15 minutes.After growth terminates, to sample cooling down under conditions of obstructed hydrogen, thickness is prepared
Spend the individual particle layer nano-diamond film for 500-600nm.
Above-mentioned individual particle layer nano-diamond film is incubated into 30 minutes in 600 DEG C of air, adopt wavelength for
The Raman spectrum of 514nm carry out glow peak test to thin film, as shown in Figure 6.As can be seen that occurring in 738nm or so in spectrogram
Very strong glow peak, the normalized intensity of Si-V glow peaks is 12, and more unoxidized thin film improves a lot；Show oxidation 30
The thin film of minute has very strong Si-V luminescent properties.
Fig. 7 is the section SEM figures of the insulation individual particle layer nano-diamond film of 30 minutes in 600 DEG C of air, it is known that thin
The thickness of film is 300nm, i.e. oxidation causes the thickness of thin film to reduce；Thin film is still made up of one layer of granule, is receiving for individual particle layer
Rice diamond thin.
Embodiment 3：
Using nano-diamond powder polishing monocrystalline silicon piece, about half an hour polishing time.The silicon chip polished is spent successively
Ionized water and acetone after ultrasonic machine is cleaned, is dried, as the substrate of nano-diamond film growth.Using hot-wire chemical gas
Phase deposition process (chemical vapor depsotition equipment be purchased from Shanghai Jiaoyou Diamond Coating Co., Ltd., model JUHF CVD 001),
With acetone as carbon source, acetone is brought in reative cell using hydrogen bubbling mode, acetone, the flow-rate ratio of hydrogen are 200：90,
Power is 2200W, and heated filament is 7mm with the distance of silicon substrate, and operating air pressure is 1.63Kpa；Not biasing in course of reaction, system
The standby time is 15 minutes；After growth terminates, to sample cooling down under conditions of obstructed hydrogen, thickness is prepared for 500-
The individual particle layer nano-diamond film of 600nm.
Above-mentioned individual particle layer nano-diamond film is incubated into 50 minutes in 600 DEG C of air, adopt wavelength for
The Raman spectrum of 514nm carry out glow peak test to thin film, as shown in Figure 8.As can be seen that occurring in 738nm or so in spectrogram
Very strong glow peak, the normalized intensity of Si-V glow peaks are increased to 28, and more non-oxide film improves a lot；Show oxidation
The thin film of 50 minutes has very strong Si-V luminescent properties.
Fig. 9 is the section SEM figures of the insulation individual particle layer nano-diamond film of 50 minutes in 600 DEG C of air, it is known that thin
The thickness of film is 280nm, i.e. oxidation causes the thickness of thin film to reduce；Thin film is still made up of one layer of granule, is receiving for individual particle layer
Rice diamond thin.
Claims (4)
1. it is a kind of with strong Si-V light individual particle layer nano-diamond film preparation method, it is characterised in that methods described
Comprise the following steps：(1) using hot-wire chemical gas-phase deposition method, monocrystalline substrate is put into into hot-wire chemical gas-phase deposition and is set
It is standby, with acetone as carbon source, acetone is brought in reative cell using hydrogen bubbling mode, wherein hydrogen, the flow-rate ratio of acetone are
200：90, heated filament is 7mm with the distance of monocrystalline substrate, and reaction power is 2200W, and operating air pressure is 1.63Kpa；Thin film grows
Time is 15～20 minutes；Not biasing during the course of the reaction, after growth terminates, the cooling down under conditions of obstructed hydrogen,
Prepare the individual particle layer nano-diamond film that thickness is 500-700nm；(2) the individual particle layer that step (1) is obtained is received
Rice diamond thin is incubated 10～50 minutes in the air at a temperature of 600 DEG C, that is, the list lighted with strong Si-V is obtained
Granular layer nano-diamond film.
2. the method for claim 1, it is characterised in that the step (1) first adopts diamond paste to monocrystalline silicon piece
Polishing half an hour, the monocrystalline silicon piece after polishing successively deionized water and acetone ultrasound wave cleaning, be dried after as nanometer Buddha's warrior attendant
The monocrystalline substrate of stone thin film growth.
3. individual particle layer nano-diamond film obtained in method as claimed in claim 1 or 2.
4. individual particle layer nano-diamond film as claimed in claim 3, it is characterised in that the thin film is in photoluminescence spectrum
738nm at have very strong Si-V luminescent properties.
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| CN105154847B (en) * | 2015-09-09 | 2017-12-05 | 浙江工业大学 | A kind of nano-diamond film and its controllable method for preparing to be lighted with Si V |
| CN106567054B (en) * | 2016-09-30 | 2019-07-26 | 浙江工业大学 | Quartzy base Si-V luminous individual particle layer nano-diamond film and preparation method thereof |
| CN106637400B (en) * | 2016-09-30 | 2019-04-09 | 浙江工业大学 | A kind of Nano diamond crystal grain and preparation method thereof that Si-V is luminous |
| CN106637129B (en) * | 2016-09-30 | 2019-04-09 | 浙江工业大学 | A kind of complex method for the diamond particles and silica fibre that Si-V is luminous |
| CN108660429B (en) * | 2018-03-23 | 2020-06-23 | 浙江工业大学 | Grain-close-packed n-type nano-diamond film and preparation method thereof |
| CN109252212A (en) * | 2018-09-28 | 2019-01-22 | 浙江工业大学 | A kind of SiV with surface nano-structure shines single-crystalline diamond and preparation method thereof |
| CN117431061A (en) * | 2022-07-15 | 2024-01-23 | 港大科桥有限公司 | Physical unclonable function material based on diamond particles, and preparation method and application thereof |
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| JP2007173479A (en) * | 2005-12-21 | 2007-07-05 | National Institute Of Advanced Industrial & Technology | High quality synthetic diamond film, its manufacturing method, and its application |
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| CN102312215B (en) * | 2011-09-29 | 2016-09-28 | 南通科创晶膜新材料有限公司 | A kind of manufacture method of diamond film coating of microbit |
| CN104060237B (en) * | 2014-06-10 | 2016-09-21 | 浙江工业大学 | A kind of have nano-diamond film luminous for Si-V and preparation method |
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