CN205893385U - Chemical vapor deposition device - Google Patents
Chemical vapor deposition device Download PDFInfo
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- CN205893385U CN205893385U CN201620827266.8U CN201620827266U CN205893385U CN 205893385 U CN205893385 U CN 205893385U CN 201620827266 U CN201620827266 U CN 201620827266U CN 205893385 U CN205893385 U CN 205893385U
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- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 68
- 239000007789 gas Substances 0.000 claims abstract description 153
- 230000006698 induction Effects 0.000 claims abstract description 46
- 239000012495 reaction gas Substances 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000003708 ampul Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
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- 230000007797 corrosion Effects 0.000 claims description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052802 copper Inorganic materials 0.000 claims description 7
- 239000010949 copper Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
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- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004804 winding Methods 0.000 claims description 5
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 64
- 229910052710 silicon Inorganic materials 0.000 abstract description 52
- 239000010703 silicon Substances 0.000 abstract description 52
- 229910052799 carbon Inorganic materials 0.000 abstract description 35
- 239000008187 granular material Substances 0.000 abstract description 27
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- 239000005543 nano-size silicon particle Substances 0.000 description 34
- 238000006243 chemical reaction Methods 0.000 description 32
- 239000010439 graphite Substances 0.000 description 29
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
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- 239000010406 cathode material Substances 0.000 description 7
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- 239000000843 powder Substances 0.000 description 7
- 230000008021 deposition Effects 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 5
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Carbon And Carbon Compounds (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The utility model provides a chemical vapor deposition device, include: the chemical vapor deposition room, gaseous feed system, the reaction gas guiding device communicates respectively with gaseous feed system and chemical vapor deposition room, including the air duct, the air duct includes air induction conduit and air outlet duct, air outlet duct is arranged in sample placing chamber, air outlet duct sets up the air guide hole along airflow direction's endcapped on the pipe wall, plasma generator and/or heating device, vacuum system is with chemical vapor deposition room intercommunication. Chemical vapor deposition device can be fine will react the even diffusion of gas to the sample, improve combined material's homogeneity, effective utilization ratio that promotes reaction gas is favorable to improving production efficiency, reduce cost simultaneously, utilizes the carbon granule combined material of the cladding silicon that its preparation obtained to have characteristics such as high power capacity, high initial efficiency and long -life.
Description
Technical field
The utility model belongs to the preparing technical field of nano silicon material and lithium ion battery negative material, is related to one kindization
Learn vapor phase growing apparatus, the chemical vapor deposition unit of more particularly, to a kind of carbon granule preparing coated Si.
Background technology
Lithium ion battery is the ideal source of portable electric appts, electric automobile and energy-storage system, exploitation specific energy height,
The good and with low cost new electrode materials of security are the core contents of Study on Li-ion batteries development field, new negative pole
The research of material is significant to the development of lithium ion battery of new generation.
Ripe lithium ion battery negative material is mainly graphite type material at present, and its theoretical specific capacity is only 372mah/
It is impossible to meet the following demand to high-energy-density for the lithium ion battery, the theoretical specific capacity of si is 4200mah/g to g, but the machine of si
Tool poor-performing, li+ embeds and abjection process, and the structural change of silicon phase leads to si to have larger volumetric expansion (> 300%)；sei
Film rupture, peeling, lead to the electrical contact of pole piece to be affected, and pole piece impedance increases；These reasons lead to si material capacity to decay
Greatly, cycle life is low.
Si particle nanosizing can reduce li+The mechanical stress of deintercalation process, reduces volumetric expansion, can improve li simultaneously+Pass
Defeated dynamics, improves material ions electrical conductivity, thus improving the capability retention of silicium cathode, improving the cycle performance of electrode.Newly
In type negative material, the silicon of nanosizing and the composite of graphite have larger application prospect, and the mechanical performance of c is applied to delay
Rush the volumetric expansion of si.Meanwhile, the c of high conductivity can improve the electric conductivity of high power capacity si well, and this makes nano-silicon and stone
The composite of ink has excellent chemical property.Prepare nano-silicon and graphite composite material, the size Control of nano-silicon and
Dispersing uniformity in graphite matrix for the silicon nanoparticle is key technology.
In existing equipment, using plasma enhanced chemical vapor deposition technology and swinging tube furnace Dynamic deposition technology
Combine, preferable uniformity nano-silicon/graphite composite structure can be prepared.But, because silicon source reaction gas spreads along pipeline, lead
Cause different deposition regions nano-silicon uniformity difference.Additionally, recombination region is in tube wall graphite base, this free diffusing
Mode lead to the reacting gas of pipeline mid portion with air-flow discharge system outside, cause to waste.
Cn 202543325u discloses a kind of chemical vapor deposition stove air inlet distribution apparatus.It includes body of heater base plate and sets
Air inlet pipe on described body of heater base plate, is characterized in being provided with kuppe on the top of air inlet pipe, and kuppe is in lower openings
Drum-shaped structure, the top of kuppe or side wall are provided with through hole.But described distribution device in gas-fluid is only applicable to chemical vapor deposition
Long-pending stove.
Utility model content
For existing swinging tubular type Dynamic deposition stove, because silicon source reaction gas spreads along pipeline, lead to different deposition regions
Nano-silicon uniformity difference；In tube wall graphite base, the mode of free diffusing leads to pipeline mid portion to recombination region
Reacting gas with air-flow discharge system outside, cause the problems such as waste, the purpose of this utility model is to provide a kind of chemistry gas
Phase precipitation equipment (cvd), introduces reacting gas guiding device in described chemical vapor deposition unit, can be good at reaction gas
Uniformly it is diffused on sample, improves the uniformity of composite, effectively lift the utilization rate of reaction gas simultaneously, be conducive to improving
Production efficiency, reduces cost, the carbon granule composite of the coated Si being prepared using it has high power capacity, high efficiency first
And the features such as the long-life.
For reaching this purpose, the utility model employs the following technical solutions:
A kind of chemical vapor deposition unit, described chemical vapor deposition unit includes:
I () CVD chamber, including sample holding chamber；
(ii) gas supply system, is connected with CVD chamber, for CVD chamber supply response gas；
(iii) reacting gas guiding device, is respectively communicated with gas supply system and CVD chamber, for by instead
Should gas equably import in sample holding chamber；Described reacting gas guiding device includes wireway, and described wireway includes air inlet
Conduit and outtake tube；Described outtake tube be located at sample holding chamber in, described outtake tube along the endcapped of airflow direction,
Gas port is arranged on tube wall；
(iv) plasma generator and/or heater, makes to produce plasma in sample holding chamber or makes chemical gas
Gas temperature in phase settling chamber raises；
V () vacuum system, is connected with CVD chamber, for providing the vacuum of CVD chamber.
The chemical vapor deposition unit that the utility model provides passes through reacting gas guiding device by reacting gas in sample
Dispersed in holding chamber, substantially increase the utilization rate of reacting gas, be conducive to improve production efficiency, reduces cost.
The chemical vapor deposition unit that the utility model provides is particularly suited for preparing the carbon granule composite of coated Si,
Reacting gas evenly is conducive to, during the carbon granule preparing silicon cladding, improving the dispersion in graphite surface for the nano-silicon
The uniformity.
Described chemical vapor deposition unit also includes driving means, and described driving means are connected with CVD chamber,
For driving CVD chamber to rotate.
Preferably, described driving means include providing the rotation motor of power and the rotary shaft being rotated by rotation motor, institute
State rotary shaft to be fixedly connected with CVD chamber.
The chemical vapor deposition unit arranging described driving means is dynamic cvd equipment.The setting of described driving means is more
Added with beneficial in sample holding chamber reacting gas dispersed.Driving means are used for driving CVD chamber to rotate, from
And Dynamic deposition, during the carbon granule preparing silicon cladding, the carbon granule composite wood of the coated Si that can have good uniformity
Material.
Described chemical vapor deposition unit also includes exhaust collection processing system, described exhaust collection processing system and chemistry
The gas outlet of vapor deposition chamber connects, and the tail gas producing for collection is simultaneously processed to it.Exhaust collection processing system can have
Imitate avoids the pollution to environment and the corrosion to vacuum equipment.
Preferably, described exhaust collection processing system includes the cold-trap cooling down by liquid nitrogen, described cold-trap and chemical gaseous phase
The gas outlet of settling chamber connects.
Preferably, metal screen is set between described cold-trap and the gas outlet of CVD chamber；
Preferably, the mesh number of described metal screen is 200-500 mesh, such as 220 mesh, 250 mesh, 300 mesh, 320 mesh, 350 mesh,
380 mesh, 400 mesh, 420 mesh, 450 mesh or 480 mesh etc., preferably 200 mesh, 325 mesh or 500 mesh.
Described metal screen can effectively stop carbon granule, it is to avoid its impact to vacuum equipment.
A diameter of outtake tube diameter of the diameter with diameter greater than outtake tube of described air induction conduit, preferably air induction conduit
1.5-5 times, such as 1.8 times, 2 times, 2.3 times, 2.5 times, 2.8 times, 3 times, 3.5 times, 4 times, 4.5 times or 4.8 times etc..
Preferably, a diameter of 20-40mm of described air induction conduit, such as 22mm, 25mm, 28mm, 30mm, 32mm, 35mm, 38mm
Or 39mm etc..
Preferably, a diameter of 1-5mm of described gas port, such as 1.5mm, 2mm, 2.5mm, 3mm, 3.5mm, 4mm or 4.5mm
Deng gas port is spaced apart 10-35mm, such as 12mm, 15mm, 18mm, 20mm, 22mm, 25mm, 28mm, 30mm, 32mm or 34mm
Deng.
Preferably, described wireway includes corrosion-resistant pipe, preferably earthenware.
Reacting gas guiding device described in the utility model is corrosion-resistant ceramic structure, and tube wall perforate, to improve reaction
Gas is in the scattered uniformity of reaction cavity, and lifts the utilization ratio of reaction gas.Further, guiding device can improve and receive
Rice silicon grain, in the dispersing uniformity of graphite surface, improves the homogeneity of silicon nanoparticle size.
Described CVD chamber includes inlet plenum, sample holding chamber and discharge chamber along airflow direction.
Preferably, described inlet plenum, sample holding chamber and discharge chamber independently are quartz ampoule, the preferably pipe of sample holding chamber
Footpath is bigger than the caliber of inlet plenum and discharge chamber.
Preferably, the internal diameter of described inlet plenum and discharge chamber independently is 4-5cm, such as 4.2cm, 4.3cm, 4.4cm,
4.5cm, 4.6cm or 4.8cm etc..
Preferably, described inlet plenum is identical respectively with wall thickness with the external diameter of discharge chamber.
Preferably, the internal diameter of described sample holding chamber is 1.4-2 times of inlet plenum internal diameter, such as 1.5 times, 1.6 times, 1.7 times,
1.8 times or 1.9 times etc..
Preferably, the length of described sample holding chamber is 10-30cm, such as 12cm, 15cm, 18cm, 20cm, 22cm, 25cm,
28cm or 29cm etc..
Preferably, described air induction conduit is located in inlet plenum.
Described sample holding chamber places at least one piece baffle plate, such as 2 pieces, 3 pieces, 4 pieces, 5 pieces, 6 pieces, 7 pieces, 8 pieces, 9 pieces or 10
Block etc., preferably 3-6 block, described baffle plate is arranged along axis in the shape of a spiral in the inwall of sample holding chamber in sample holding chamber,
The hand of spiral is identical with the direction of rotation of CVD chamber, and the spiral starting point of described baffle plate is arranged at sample holding chamber length
1/3-1/2 at, such as 1.1/3,1.2/3,1.3/3 or 1.4/3 etc..
Preferably, the height of described baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter, such as 0.25 times, 0.3 times,
0.35 times, 0.4 times or 0.45 times etc..
Preferably, the length of described baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter, such as 0.25 times, 0.3 times,
0.35 times, 0.4 times or 0.45 times etc..
Preferably, described baffle plate is straight panel and/or wave-shape board, preferably wave-shape board.
Preferably, described baffle plate is evenly distributed in the inner section of sample holding chamber from spiral starting point, and in same circumference
On line.
The utility model the caliber of sample holding chamber is set to big compared with the caliber of inlet plenum and discharge chamber, can be effectively
Extend the time of staying in CVD chamber for the sample, prevent from flowing out with air-flow in sample.Further, the utility model
By to the structure of baffle plate and the concrete setting of arrangement, significantly more efficient sample stopping in CVD chamber can be extended
Stay the time, improve the speed of reaction, and the deposition uniformity of deposited thing.
Described plasma generator includes radio-frequency power supply and the inductance-coupled coil being electrically connected with radio-frequency power supply, described inductance
Coupling coil uniform winding is outside sample holding chamber.
Preferably, described inductance-coupled coil includes hollow copper tubing.
Preferably, it is connected with coolant inside described hollow copper tubing.
Preferably, described coolant is cooling water.
Typical but non-limiting heater includes heating furnace etc..
Described gas supply system includes at least one air inlet pipe connecting with CVD chamber, such as 2,3,4
Root, 5,6,7 or 10 etc., preferably 3-5 root air inlet pipe.The radical of described air inlet pipe can be selected according to actual conditions
Select.
Preferably, described air inlet pipe is the air inlet pipe that can control feed rate.
Preferably, described gas supply system also sets up tracing system, and described tracing system is arranged at air inlet pipe and chemistry
Between the air inlet of vapor deposition chamber, for controlling temperature during gas entrance CVD chamber at 25-100 DEG C, such as 26
DEG C, 27 DEG C, 28 DEG C, 30 DEG C, 32 DEG C, 35 DEG C, 38 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C or 90 DEG C etc..
Compared with prior art, the beneficial effects of the utility model are:
The chemical vapor deposition unit that the utility model provides passes through to introduce guiding device, and reacting gas is equal through gas port
The even utilization rate (improve more than 30%) being scattered in conversion zone, substantially increasing reacting gas, be conducive to improve production efficiency,
Reduces cost.
It is combined using the carbon granule that the chemical vapor deposition unit that the utility model provides is particularly suited for preparing silicon cladding
Material, and preparation method is simple, easy industrialized production, due to described chemical vapor deposition unit can provide uniformly anti-
Answer gas, be more beneficial for improving the dispersed homogeneous degree in graphite surface for the nano-silicon, the carbon granule of the coated Si preparing is combined
Material have high power capacity, height first efficiency, long-life the features such as.
Brief description
Fig. 1 is the structural representation of the chemical vapor deposition unit that embodiment 2 provides；
Fig. 2 is the structural representation of the reacting gas guiding device that embodiment 2 provides；
Fig. 3 is the scanning electron microscope image of the carbon granule composite that Application Example 1 obtains coated Si；
Fig. 4 is the scanning electron microscope image of the carbon granule composite of coated Si that comparative example 1 is obtained；
Fig. 5 is the x-ray diffraction collection of illustrative plates of the silicon nanoparticle illustrating that embodiment 1 is obtained；
Fig. 6 is the x-ray diffraction collection of illustrative plates of the silicon nanoparticle illustrating that embodiment 2 is obtained；
Fig. 7 be in embodiment 2 cylindrical sample holding chamber along bus expansion after structural representation；
Wherein: 100, CVD chamber；101, sample holding chamber；102, inlet plenum；103, discharge chamber；104, gear
Plate；200, plasma generator；201, inductance-coupled coil；202, radio-frequency power supply；300, gas supply system；301, air inlet
Pipe；302, tracing system；400, vacuum system；500, reacting gas guiding device；501, air induction conduit；502, outtake tube；
503, gas port；600, exhaust collection processing system, 601, metal filter screen.
Specific embodiment
For ease of understanding the utility model, it is as follows that the utility model enumerates embodiment.Those skilled in the art it will be clearly understood that
Described embodiment is only to aid in understanding the utility model, is not construed as to concrete restriction of the present utility model.
The utility model provides a kind of chemical vapor deposition unit and includes:
I () CVD chamber, including sample holding chamber；
(ii) gas supply system, is connected with CVD chamber, for CVD chamber supply response gas；
(iii) reacting gas guiding device, is respectively communicated with gas supply system and CVD chamber, for by instead
Should gas equably import in sample holding chamber；Described reacting gas guiding device includes wireway, and described wireway includes air inlet
Conduit and outtake tube；Described outtake tube be located at sample holding chamber in, described outtake tube along the endcapped of airflow direction,
Gas port is arranged on tube wall；
(iv) plasma generator and/or heater, makes to produce plasma in sample holding chamber or makes chemical gas
Gas temperature in phase settling chamber raises；
V () vacuum system, is connected with CVD chamber, for providing the vacuum of CVD chamber.
Embodiment 1
A kind of chemical vapor deposition unit includes:
I () CVD chamber 100, described CVD chamber is quartz ampoule；Described quartz ampoule downstream direction
Discharge chamber 103 including the inlet plenum 102 of 5cm length, the sample holding chamber 101 of 10-30cm length and 5cm length；Inlet plenum 102 internal diameter
Identical with discharge chamber 103 internal diameter, it is 4-5cm；The internal diameter of described sample holding chamber 101 is the 1.4-2.0 of inlet plenum 102 internal diameter
Times；
The sample holding chamber 101 of described quartz ampoule arranges 4 pieces of baffle plates 104, and described baffle plate 104 is in quartzy inside pipe wall along axis
Arrange in the shape of a spiral；The spiral starting point of described baffle plate 104 is arranged at the 1/3-1/2 of sample holding chamber 101；
Described height of baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter；
Described baffle length is 0.2-0.5 times of described sample holding chamber length；
Described baffle plate is wave-shape board；
(ii) plasma generator 200, for producing plasma；Described plasma generator includes radio-frequency power supply
202, and the inductance-coupled coil 201 being electrically connected with radio-frequency power supply, described inductance-coupled coil 201 uniform winding is in chemical vapor deposition
Outside long-pending room 101；Described inductance-coupled coil 201 is made up of hollow copper tubing；It is connected with coolant inside described hollow copper tubing；Described
Coolant is cooling water；
(iii) gas supply system 300, for CVD chamber supply response gas；Described gas supply system
Including 4 air inlet pipe 301 being connected with the inlet plenum 102 of CVD chamber 100；Described air inlet pipe 301 can control into
Gas speed；Described gas supply system also includes tracing system 302, to control gas temperature at 25-100 DEG C；
(iv) vacuum system 400, for providing the vacuum of CVD chamber；
V () reacting gas guiding device 500, for uniformly introducing reaction gas to sample holding chamber 101；Described reaction
Air flow guiding device 500 is corrosion-resistant pipe；Described reacting gas guiding device 500 includes wireway, and described wireway includes
Air induction conduit 501 and outtake tube 502, described air induction conduit 501 is placed in inlet plenum 102, and with gas supply system 300
Gas outlet is connected, described outtake tube 502 be located at sample holding chamber 101 in, be connected with sample holding chamber 101, described go out
Airway 502, along the endcapped of airflow direction, convinces pore 503 by patient analysis along tube wall；Described air induction conduit with diameter greater than going out conductance
The diameter of pipe, 1.5-5 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 20-40mm of described air induction conduit；Described
The a diameter of 1-5mm of gas port 503, gas port 503 is spaced apart 10-35mm；
(vi) exhaust collection processing system 600, including the cold-trap being cooled down by liquid nitrogen, is gone forward side by side for collecting the tail gas producing
Row is processed.
Embodiment 2
A kind of dynamic chemical vapor precipitation equipment (dynamic cvd equipment), its structural representation is as shown in figure 1, described dynamic
Cvd equipment includes:
I () CVD chamber 100, described CVD chamber 100 is quartz ampoule；Described quartz ampoule favorable current side
Discharge chamber 103 to the inlet plenum 102, the sample holding chamber 101 of 10-30cm length and 5cm length including 5cm length；In inlet plenum 102
Footpath is identical with discharge chamber 103 internal diameter, is 4-5cm；The internal diameter of described sample holding chamber 101 is the 1.4- of inlet plenum 102 internal diameter
2.0 again；
The sample holding chamber 101 of described quartz ampoule arranges 4 pieces of baffle plates 104, and described baffle plate 104 is in quartzy inside pipe wall along axis
Arrange in the shape of a spiral, the hand of spiral is identical with the direction of rotation of CVD chamber 100；The spiral starting point of described baffle plate 104
It is arranged at the 1/3-1/2 of sample holding chamber 101；Described baffle plate 104 is evenly distributed in sample holding chamber from spiral starting point
On section, and on same circumference, as shown in Figure 7；
Described height of baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter；
Described baffle length is 0.2-0.5 times of described sample holding chamber length；
Described baffle plate is wave-shape board；
(ii) plasma generator 200, for producing plasma；Described plasma generator includes radio-frequency power supply
202, and the inductance-coupled coil 201 with radio-frequency power supply Electricity Federation, described inductance-coupled coil 201 uniform winding is in chemical vapor deposition
Outside long-pending room 101；Described inductance-coupled coil 201 is made up of hollow copper tubing；It is connected with coolant inside described hollow clearance；Described
Coolant is cooling water；
(iii) gas supply system 300, for CVD chamber supply response gas；Described gas supply system
For 4 air inlet pipe 301 being connected with the inlet plenum 102 of CVD chamber 100；Described air inlet pipe 301 can control air inlet
Speed；Described gas supply system also includes tracing system 302, to control temperature at 25-100 DEG C；
(iv) vacuum system 400, for providing the vacuum of CVD chamber；
(v) reacting gas guiding device 500, as shown in Fig. 2 for reaction gas is uniformly introduced sample holding chamber 101；Institute
Stating reacting gas guiding device 500 is corrosion-resistant pipe；Described reacting gas guiding device 500 includes wireway, described air guide
Pipe includes air induction conduit 501 and outtake tube 502, and described air induction conduit 501 is placed in inlet plenum 102, and supplies system with gas
The gas outlet of system 300 is connected, and described outtake tube 502 is located in sample holding chamber 101, is connected with sample holding chamber 101,
Described outtake tube 502, along the endcapped of airflow direction, convinces pore 503 by patient analysis along tube wall；Described air induction conduit with diameter greater than
The diameter of outtake tube, 15-5 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 20- of described air induction conduit
40mm；The a diameter of 1-5mm of described gas port 503, gas port 503 is spaced apart 10-35mm；
(vi) driving means, for driving CVD chamber to rotate；Described driving means include providing the rotation of power
Turn motor and the rotary shaft being rotated by rotation motor, described rotary shaft is fixedly connected with CVD chamber 100；
(vii) exhaust collection processing system 600, including the cold-trap being cooled down by liquid nitrogen, is entered for collecting the tail gas producing
Row is processed.
Embodiment 3
A kind of dynamic cvd equipment, described dynamic cvd equipment includes:
I () CVD chamber 100, for depositing silicon on carbon particles；Described CVD chamber 100 is quartz
Pipe；Described quartz ampoule downstream direction includes the inlet plenum 102 of 5cm length, the sample holding chamber 101 of 10-30cm length and 5cm length
Discharge chamber 103；Inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is 4-5cm；The internal diameter of described sample holding chamber 101
For inlet plenum 102 internal diameter 1.4-2.0 times；
The sample holding chamber 101 of described quartz ampoule arranges 4 pieces of baffle plates 104, and described baffle plate 104 is in quartzy inside pipe wall along axis
Arrange in the shape of a spiral, the hand of spiral is identical with the direction of rotation of CVD chamber 100；The spiral starting point of described baffle plate 104
It is arranged at the 1/3-1/2 of sample holding chamber 101；
Described height of baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter；
Described baffle length is 0.2-0.5 times of described sample holding chamber length；
Described baffle plate is wave-shape board；
(ii) heater, including heating furnace, described CVD chamber is located in heating furnace；
(iii) gas supply system 300, for CVD chamber supply response gas；Described gas supply system
For 4 air inlet pipe 301 being connected with the inlet plenum 102 of CVD chamber 100；Described air inlet pipe can control air inlet speed
Rate；Described gas supply system also includes tracing system 302, to control temperature at 25-100 DEG C；
(iv) vacuum system 400, for providing the vacuum of CVD chamber；
V () reacting gas guiding device 500, for uniformly introducing sample holding chamber 101 by reaction gas；Described reacting gas
Guiding device 500 is corrosion-resistant pipe；Described reacting gas guiding device 500 includes wireway, and described wireway includes air inlet
Conduit 501 and outtake tube 502, described air induction conduit 501 is placed in inlet plenum 102, and with the giving vent to anger of gas supply system 300
Mouthful be connected, described outtake tube 502 is located in sample holding chamber 101, is connected with sample holding chamber 101, described go out conductance
Pipe 502, along the endcapped of airflow direction, convinces pore 503 by patient analysis along tube wall；Described air induction conduit with diameter greater than outtake tube
Diameter, 1.5-5 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 20-40mm of described air induction conduit；Described air guide
The a diameter of 1-5mm in hole 503, gas port 503 is spaced apart 10-35mm；
(vi) driving means, for driving CVD chamber to rotate；Described driving means include providing the rotation of power
Turn motor and the rotary shaft being rotated by rotation motor, described rotary shaft is fixedly connected with CVD chamber 100；
(vii) exhaust collection processing system 600, including the cold-trap being cooled down by liquid nitrogen, is entered for collecting the tail gas producing
Row is processed.
Embodiment 4
A kind of dynamic cvd equipment, described dynamic cvd equipment includes:
I () CVD chamber 100, for depositing silicon on carbon particles；Described CVD chamber 100 is quartz
Pipe；Described quartz ampoule downstream direction includes the inlet plenum 102 of 5cm length, the sample holding chamber 101 of 10-30cm length and 5cm length
Discharge chamber 103；Inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is 4-5cm；The internal diameter of described sample holding chamber 101
For inlet plenum 102 internal diameter 1.4-2.0 times；
The sample holding chamber 101 of described quartz ampoule arranges 4 pieces of baffle plates 104, and described baffle plate 104 is in quartzy inside pipe wall along axis
Arrange in the shape of a spiral, the hand of spiral is identical with the direction of rotation of CVD chamber 100；The spiral starting point of described baffle plate 104
It is arranged at the 1/3-1/2 of sample holding chamber 101；
Described height of baffle plate is 0.2-0.5 times of described sample holding chamber internal diameter；
Described baffle length is 0.2-0.5 times of described sample holding chamber length；
Described baffle plate is wave-shape board；
(ii) plasma generator 200 and heater；
Plasma generator 200, for producing plasma；Described plasma generator includes radio-frequency power supply 202,
And the inductance-coupled coil 201 with radio-frequency power supply Electricity Federation, described inductance-coupled coil 201 uniform winding is in CVD chamber
Outside 101；Described inductance-coupled coil 201 is made up of hollow copper tubing；It is connected with coolant inside described hollow clearance；Described cooling
Liquid is cooling water；
Described heater includes heating furnace, and described CVD chamber is located in heating furnace；
(iii) gas supply system 300, for CVD chamber supply response gas；Described gas supply system
For 4 air inlet pipe 301 being connected with the inlet plenum 102 of CVD chamber 100；Described air inlet pipe can control air inlet speed
Rate；Described gas supply system also includes tracing system 302, to control temperature at 25-100 DEG C；
(iv) vacuum system 400, for providing the vacuum of CVD chamber；
V () reacting gas guiding device 500, for uniformly introducing sample holding chamber 101 by reaction gas；Described reacting gas
Guiding device 500 is corrosion-resistant pipe；Described reacting gas guiding device 500 includes wireway, and described wireway includes air inlet
Conduit 501 and outtake tube 502, described air induction conduit 501 is placed in inlet plenum 102, and with the giving vent to anger of gas supply system 300
Mouthful be connected, described outtake tube 502 is located in sample holding chamber 101, is connected with sample holding chamber 101, described go out conductance
Pipe 502, along the endcapped of airflow direction, convinces pore 503 by patient analysis along tube wall；Described air induction conduit with diameter greater than outtake tube
Diameter, 1.5-5 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 20-40mm of described air induction conduit；Described air guide
The a diameter of 1-5mm in hole 503, gas port 503 is spaced apart 10-35mm；
(vi) driving means, for driving CVD chamber to rotate；Described driving means include providing the rotation of power
Turn motor and the rotary shaft being rotated by rotation motor, described rotary shaft is fixedly connected with CVD chamber 100；
(vii) exhaust collection processing system 600, including the cold-trap being cooled down by liquid nitrogen, is entered for collecting the tail gas producing
Row is processed.
Application Example 1
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the equipment that embodiment 1 provides, wherein,
In described chemical vapor deposition unit, the length of sample holding chamber 101 is 10cm, inlet plenum 102 internal diameter and discharge chamber 103 internal diameter
Identical, it is 4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral shell of described baffle plate 104
Spin up point to be arranged at the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described
Baffle length is 0.4 times of described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described enter
The a diameter of 30mm of airway；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
50g average grain diameter 16-19 μm phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C；It is passed through 20sccm h2As load
Gas, is evacuated to 20pa；After 30min, it is passed through 20sccm sihcl3For react silicon source, plasma reaction power 200w,
2h is reacted under room temperature；Close sihcl after completion of the reaction3Silicon source is supplied, and is continuing with 200w plasma reaction 10min；Take out
Material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite.
Application Example 1 obtains the carbon granule composite of coated Si, and the silicon layer of described material is non crystalline structure, silicone content
About 4wt%；Fig. 3 is the scanning electron microscope image of the carbon granule composite that Application Example 1 obtains coated Si, can from figure
To silicon nanoparticle Size Distribution all with and distribution is little, silicon nanoparticle form is homogeneous, is dispersed in graphite granule table
Face.
Application Example 2
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the equipment that embodiment 2 provides, wherein,
In described dynamic cvd equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter,
It is 4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point of described baffle plate 104
It is arranged at the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle plate is long
Spend 0.4 times for described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit
A diameter of 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
30g average grain diameter 16-19 μm, phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C, is passed through 35sccm h2As load
Gas, is evacuated to 25pa, is passed through h2After 30min, speed of gyration 5r/min is set, is passed through 20sccm sihcl3For reacting silicon source,
Plasma reaction power 200w, reacts 2h at room temperature, stops silicon source supply after completion of the reaction, be continuing with 200w plasma
Precursor reactant 10min；Take out material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite.
Application Example 2 obtains the carbon granule composite of coated Si, and the silicon layer of described material is non crystalline structure, silicone content
About 13wt%.
Application Example 3
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the equipment that embodiment 2 provides, wherein,
In described dynamic cvd equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter,
It is 4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point of described baffle plate 104
It is arranged at the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle plate is long
Spend 0.4 times for described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit
A diameter of 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
25g average grain diameter 16-19 μm, phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C, is passed through 35sccm h2As load
Gas, is evacuated to 25pa, is passed through h2After 30min, speed of gyration 5r/min is set, is passed through 25sccm sihcl3For reacting silicon source,
Plasma reaction power 200w, reacts 4h at room temperature；Stop silicon source supply after completion of the reaction, be continuing with 200w plasma
Precursor reactant 10min；Take out material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite.
Application Example 3 obtains the carbon granule composite of coated Si, and the silicon layer of described material is non crystalline structure, silicone content
About 32wt%.
Application Example 2 and Application Example 3 illustrate, the silicone content in the carbon granule composite of coated Si is with reaction gas
Volume flow, plasma reaction power and reaction time are relevant.
Application Example 4
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the equipment that embodiment 3 provides, wherein,
In described dynamic cvd equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter,
It is 4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point of described baffle plate 104
It is arranged at the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle plate is long
Spend 0.4 times for described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit
A diameter of 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
25g average grain diameter 16-19 μm, phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C, is passed through 35sccm h2As load
Gas, is evacuated to 25pa, is passed through h2After 30min, adjust sample holding chamber 101 using heating furnace and be warming up to 700 DEG C, arrange back
Rotary speed 5r/min, is passed through 25sccm sihcl3For reacting silicon source, react 4h at 700 DEG C；Stop silicon source after completion of the reaction to supply
Should, continue reaction 10min；Take out material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite.
The silicon layer of the carbon granule composite of the coated Si preparing is crystalline silicon, and silicone content is 28wt%.
Application Example 3 and Application Example 4 illustrate, plasma generator is than heating furnace to the decomposition efficiency of silicon more
High.And conversion zone temperature can produce impact to the crystalline structure of silicon, reaction under room temperature condition can obtain non-crystalline silicon, under high temperature
Crystalline silicon can be obtained.
Comparative example 1:
A kind of chemical vapor deposition unit, in addition to being not provided with reacting gas guiding device, described in remaining structure and embodiment 1
Chemical vapor deposition unit structure identical.
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the said equipment, wherein, described chemistry gas
In phase precipitation equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is
4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point setting of described baffle plate 104
At the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle length is
0.4 times of described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit diameter
For 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
50g average grain diameter 16-19 μm phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C；It is passed through 20sccm h2As load
Gas, is evacuated to 20pa；After 30min, it is passed through 20sccm sihcl3For react silicon source, plasma reaction power 200w,
2h is reacted under room temperature；Close sihcl after completion of the reaction3Silicon source is supplied, and is continuing with 200w plasma reaction 10min；Take out
Material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite, silicone content about 3wt%, Fig. 4 be sample scanning electricity
Mirror image.
Contrast Application Example 1 can be seen with comparative example 1, in gained nano-silicon/graphite composite sample under equal conditions,
Silicone content using reacting gas guiding device is 4wt%, compares the sample about 3wt% silicone content not increasing guiding device, carries
The amplitude of liter is up to 33%, shows that the utilization rate of silicon source gas improves 33%.Contrast Fig. 3 and Fig. 4 can see, without wireway
In the sample of water conservancy diversion, due to conversion zone homogeneity not, there is a small amount of agglomeration in nano-silicon；And through wireway water conservancy diversion
Sample, nano-silicon disperse evenly, particle size is more homogeneous.
Comparative example 2
A kind of dynamic cvd equipment, in addition to being not provided with reacting gas guiding device, dynamic described in remaining structure and embodiment 2
The structure of state cvd equipment is identical.
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the said equipment, wherein, described dynamic
In cvd equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is
4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point setting of described baffle plate 104
At the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle length is
0.4 times of described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit diameter
For 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
30g average grain diameter 16-19 μm, phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C, is passed through 35sccm h2As load
Gas, is evacuated to 25pa, is passed through h2After 30min, speed of gyration 5r/min is set, is passed through 20sccm sihcl3For reacting silicon source,
Plasma reaction power 200w, reacts 2h at room temperature, stops silicon source supply after completion of the reaction, be continuing with 200w plasma
Precursor reactant 10min；Take out material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite, silicone content about 10wt%.
Contrast Application Example 2 can be seen with comparative example 2, in gained nano-silicon/graphite composite sample under equal conditions,
The silicone content improving reacting gas guiding device is 13wt%, compares the former sample about 10wt% silicon not increasing guiding device and contains
Amount, lifting amplitude is up to 30%, shows that the utilization rate of silicon source gas improves 30%.
Comparative example 3
A kind of dynamic cvd equipment, in addition to being not provided with reacting gas guiding device, dynamic described in remaining structure and embodiment 3
The structure of state cvd equipment is identical.
A kind of preparation method of the carbon granule composite of coated Si, is carried out using the said equipment, wherein, described dynamic
In cvd equipment, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is
4.5cm, the internal diameter of described sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point setting of described baffle plate 104
At the 1/2 of sample holding chamber 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle length is
0.4 times of described sample holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, described air induction conduit diameter
For 30mm；The a diameter of 3mm of described gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
25g average grain diameter 16-19 μm, phosphorus content is placed in the sample holding chamber 101 of CVD chamber 100
99.95% natural spherical plumbago powder, arranges gas supply system 300 heat tracing temperature 50 C, is passed through 35sccm h2As load
Gas, is evacuated to 25pa, is passed through h2After 30min, speed of gyration 5r/min is set, is passed through 25sccm sihcl3For reacting silicon source,
Adjust sample holding chamber 101 using heating furnace and react 4h at 700 DEG C；Stop silicon source supply after completion of the reaction, continue reaction
10min；Take out material, ground, screening after obtain nano-silicon/composite cathode material of silicon/carbon/graphite.
The silicon layer of the carbon granule composite of the coated Si preparing is crystalline silicon, and silicone content is 21wt%.
Contrast Application Example 4 can be seen with comparative example 3, in gained nano-silicon/graphite composite sample under equal conditions,
The silicone content improving reacting gas guiding device is 28wt%, compares the former sample about 21wt% silicon not increasing guiding device and contains
Amount, lifting amplitude is up to 33%, shows that the utilization rate of silicon source gas improves 33%.
Can be seen by comparative example 1-3, the introducing of guiding device, can significantly lift the utilization rate of reacting gas, carry
The amplitude of liter is more than 30%.Meanwhile, it is introduced in the sample of guiding device, silicon grain is more evenly distributed in graphite surface.
Embodiment 1 is described
A kind of preparation method of silicon nanoparticle, is carried out using the equipment that embodiment 2 provides, wherein, described dynamic cvd sets
In standby, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is 4.5cm, institute
The internal diameter stating sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point of described baffle plate 104 is arranged at sample and puts
Put at the 1/2 of room 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle length is described sample
0.4 times of holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 30mm of described air induction conduit；Institute
State a diameter of 3mm of gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
Do not place any substrate in the sample holding chamber 101 of CVD chamber 100, gas supply system is set
300 heat tracing temperature 50 Cs, are passed through 20sccm ar as carrier gas, are evacuated to 15pa；After 30min, it is passed through 10sccm
sihcl3For reacting silicon source, plasma reaction power 200w is set, reacts 2h at room temperature, deposit one layer in quartzy tube wall and receive
Rice silicon；Close sihcl after completion of the reaction3Silicon source is supplied, and is continuing with 200w plasma reaction 10min；Take out material, through grinding
Pure silicon nanoparticle material is obtained after mill, screening.
Fig. 5 is the x-ray diffraction collection of illustrative plates that embodiment 1 gained silicon nanoparticle is described, be centrally located at 28.4 °, 47.3 °,
56.1 ° of diffraction maximum corresponds to crystalline silicon (111), (220), the crystal plane of (311) respectively, but peak intensity is very low, and peak
Shape broadening is clearly；This explanation explanation embodiment 1 gained silicon nanoparticle is amorphous state.
Embodiment 2 is described
A kind of preparation method of silicon nanoparticle, is carried out using the equipment that embodiment 4 provides, wherein, described dynamic cvd sets
In standby, the length of sample holding chamber 101 is 10cm, and inlet plenum 102 internal diameter is identical with discharge chamber 103 internal diameter, is 4.5cm, institute
The internal diameter stating sample holding chamber 101 is 1.5 times of inlet plenum 102 internal diameter；The spiral starting point of described baffle plate 104 is arranged at sample and puts
Put at the 1/2 of room 101；Described height of baffle plate is 0.4 times of described sample holding chamber internal diameter；Described baffle length is described sample
0.4 times of holding chamber length；3 times of a diameter of outtake tube diameter of air induction conduit, a diameter of 30mm of described air induction conduit；Institute
State a diameter of 3mm of gas port 503, gas port 503 is spaced apart 15mm.
Described preparation method comprises the steps:
Do not place any substrate in the sample holding chamber 101 of CVD chamber 100, gas supply system is set
300 heat tracing temperature 50 Cs；It is passed through 20sccm ar as carrier gas, be evacuated to 15pa；After 30min, it is passed through 10sccm
sihcl3For reacting silicon source, plasma reaction power 200w is set, reacts 2h at room temperature, deposit one layer in quartzy tube wall and receive
Rice silicon；Close sihcl after completion of the reaction3Silicon source is supplied, and continues reaction 10min；Adjust sample holding chamber using heating furnace afterwards
101 react 4h at 700 DEG C；Take out material, ground, screening after obtain pure nano-silicon powder body material.
Fig. 6 be illustrate example 2 gained silicon nanoparticle X-ray diffraction pattern it may be observed that obvious crystalline silicon (111),
(220), (311) peak, shows in sample with the presence of silicon metal.
Conversion zone temperature be can be seen that by explanation embodiment 1-2 and can produce impact, room temperature condition to the crystalline structure of silicon
Lower reaction can obtain can obtaining crystalline silicon under non-crystalline silicon, high temperature.
Applicant states, the foregoing is only specific embodiment of the present utility model, but protection model of the present utility model
Enclose and be not limited thereto, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and exist
In the technical scope that the utility model discloses, the change or replacement that can readily occur in, all fall within protection domain of the present utility model
Within the scope of disclosure.
Claims (35)
1. a kind of chemical vapor deposition unit is it is characterised in that described chemical vapor deposition unit includes:
I () CVD chamber, including sample holding chamber；
(ii) gas supply system, is connected with CVD chamber, for CVD chamber supply response gas；
(iii) reacting gas guiding device, is respectively communicated with gas supply system and CVD chamber, for by reaction gas
Equably import in sample holding chamber；Described reacting gas guiding device includes wireway, and described wireway includes air induction conduit
And outtake tube；Described outtake tube is located in sample holding chamber, and described outtake tube is along the endcapped of airflow direction, tube wall
Upper setting gas port；
(iv) plasma generator and/or heater, makes to produce plasma in sample holding chamber or makes chemical vapor deposition
Gas temperature in long-pending room raises；
V () vacuum system, is connected with CVD chamber, for providing the vacuum of CVD chamber.
2. chemical vapor deposition unit according to claim 1 is it is characterised in that described chemical vapor deposition unit also wraps
Include driving means, described driving means are connected with CVD chamber, for driving CVD chamber to rotate.
3. chemical vapor deposition unit according to claim 2 is it is characterised in that described driving means include providing power
Rotation motor and the rotary shaft being rotated by rotation motor, described rotary shaft is fixedly connected with CVD chamber.
4. chemical vapor deposition unit according to claim 1 and 2 is it is characterised in that described chemical vapor deposition unit
Also include exhaust collection processing system, described exhaust collection processing system is connected with the gas outlet of CVD chamber, is used for
Collect the tail gas producing and it is processed.
5. chemical vapor deposition unit according to claim 4 is it is characterised in that described exhaust collection processing system includes
The cold-trap being cooled down by liquid nitrogen, described cold-trap is connected with the gas outlet of CVD chamber.
6. chemical vapor deposition unit according to claim 5 is it is characterised in that described cold-trap and CVD chamber
Gas outlet between arrange metal screen.
7. chemical vapor deposition unit according to claim 6 is it is characterised in that the mesh number of described metal screen is 200-
500 mesh.
8. chemical vapor deposition unit according to claim 6 is it is characterised in that the mesh number of described metal screen is 200
Mesh, 325 mesh or 500 mesh.
9. chemical vapor deposition unit according to claim 1 and 2 is it is characterised in that the diameter of described air induction conduit is big
Diameter in outtake tube.
10. chemical vapor deposition unit according to claim 1 and 2 is it is characterised in that a diameter of of air induction conduit gives vent to anger
1.5-5 times of conduit diameter.
11. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that described air induction conduit is a diameter of
20-40mm.
12. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that a diameter of 1- of described gas port
5mm, gas port is spaced apart 10-35mm.
13. chemical vapor deposition units according to claim 1 and 2 it is characterised in that described wireway include corrosion-resistant
Pipe.
14. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that described wireway includes pottery
Pipe.
15. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that described CVD chamber edge
Airflow direction includes inlet plenum, sample holding chamber and discharge chamber.
16. chemical vapor deposition units according to claim 15 are it is characterised in that described inlet plenum, sample holding chamber
It independently is quartz ampoule with discharge chamber.
17. chemical vapor deposition units according to claim 15 are it is characterised in that the caliber ratio of sample holding chamber enters
The caliber of air chamber and discharge chamber is big.
18. chemical vapor deposition units according to claim 15 it is characterised in that described inlet plenum and discharge chamber interior
Footpath independently is 4-5cm.
19. chemical vapor deposition units according to claim 15 it is characterised in that described inlet plenum and discharge chamber outer
Footpath is identical respectively with wall thickness.
20. chemical vapor deposition units according to claim 15 are it is characterised in that the internal diameter of described sample holding chamber is
1.4-2 times of inlet plenum internal diameter.
21. chemical vapor deposition units according to claim 15 are it is characterised in that the length of described sample holding chamber is
10-30cm.
22. chemical vapor deposition units according to claim 15 are it is characterised in that described air induction conduit is located at inlet plenum
In.
23. chemical vapor deposition units according to claim 15 are it is characterised in that described sample holding chamber is placed at least
One piece of baffle plate, described baffle plate is arranged along axis in the shape of a spiral in the inwall of sample holding chamber in sample holding chamber, the hand of spiral
Identical with the direction of rotation of CVD chamber, the spiral starting point of described baffle plate is arranged at the 1/3-1/ of sample holding chamber length
At 2.
24. chemical vapor deposition units according to claim 23 are it is characterised in that described sample holding chamber places 3-6
Block baffle plate.
25. chemical vapor deposition units according to claim 23 are it is characterised in that the height of described baffle plate is described sample
0.2-0.5 times of product holding chamber internal diameter.
26. chemical vapor deposition units according to claim 23 are it is characterised in that the length of described baffle plate is described sample
0.2-0.5 times of product holding chamber internal diameter.
27. chemical vapor deposition units according to claim 23 are it is characterised in that described baffle plate is straight panel and/or ripple
Wave plate.
28. chemical vapor deposition units according to claim 23 are it is characterised in that described baffle plate is wave-shape board.
29. chemical vapor deposition units according to claim 23 are it is characterised in that described baffle plate is uniform from spiral starting point
It is distributed in the inner section of sample holding chamber, and on same circumference.
30. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that described plasma generator bag
Include radio-frequency power supply and the inductance-coupled coil being electrically connected with radio-frequency power supply, described inductance-coupled coil uniform winding is in sample holding chamber
Outside.
31. chemical vapor deposition units according to claim 30 are it is characterised in that described inductance-coupled coil includes sky
Heart copper pipe.
32. chemical vapor deposition units according to claim 1 and 2 are it is characterised in that described gas supply system includes
At least one air inlet pipe connecting with CVD chamber.
33. chemical vapor deposition units according to claim 32 are it is characterised in that described gas supply system includes 3-
5 air inlet pipe.
34. chemical vapor deposition units according to claim 32 it is characterised in that described air inlet pipe be can control into
The air inlet pipe of gas speed.
35. chemical vapor deposition units according to claim 32 are it is characterised in that described gas supply system also includes
Tracing system, described tracing system is arranged between air inlet pipe and the air inlet of CVD chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620827266.8U CN205893385U (en) | 2016-08-02 | 2016-08-02 | Chemical vapor deposition device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620827266.8U CN205893385U (en) | 2016-08-02 | 2016-08-02 | Chemical vapor deposition device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488837A (en) * | 2017-09-20 | 2017-12-19 | 大连理工大学 | Material microcosmic surface syntype coating system |
| CN110137446A (en) * | 2019-04-03 | 2019-08-16 | 兰溪致德新能源材料有限公司 | Nano-silicone wire/carbon negative electrode material process units and production technology |
| CN113373422A (en) * | 2021-04-30 | 2021-09-10 | 麦斯克电子材料股份有限公司 | Device for improving POLY-SI chemical vapor deposition and using method thereof |
| CN115259900A (en) * | 2022-03-23 | 2022-11-01 | 西北工业大学 | Very long (Ta)xHf1-x) C ultra-high temperature ceramic solid solution nanowire and preparation method thereof |
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2016
- 2016-08-02 CN CN201620827266.8U patent/CN205893385U/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107488837A (en) * | 2017-09-20 | 2017-12-19 | 大连理工大学 | Material microcosmic surface syntype coating system |
| CN107488837B (en) * | 2017-09-20 | 2019-04-16 | 大连理工大学 | Material microcosmic surface syntype coating system |
| CN110137446A (en) * | 2019-04-03 | 2019-08-16 | 兰溪致德新能源材料有限公司 | Nano-silicone wire/carbon negative electrode material process units and production technology |
| CN113373422A (en) * | 2021-04-30 | 2021-09-10 | 麦斯克电子材料股份有限公司 | Device for improving POLY-SI chemical vapor deposition and using method thereof |
| CN115259900A (en) * | 2022-03-23 | 2022-11-01 | 西北工业大学 | Very long (Ta)xHf1-x) C ultra-high temperature ceramic solid solution nanowire and preparation method thereof |
| CN115259900B (en) * | 2022-03-23 | 2024-01-30 | 西北工业大学 | Extremely long (Ta x Hf 1-x ) C superhigh temperature ceramic solid solution nanowire and preparation method thereof |
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Address after: 518106 Gongming City, Guangdong province Guangming New District Office of the West community high and New Technology Industrial Park, building eighth, Patentee after: Beitrei New Materials Group Co., Ltd Address before: 518106 Gongming City, Guangdong province Guangming New District Office of the West community high and New Technology Industrial Park, building eighth, Patentee before: Shenzhen BTR New Energy Materials Inc. |