CN100567566C - A kind of vacuum plasma reactor that is used for large area film growth - Google Patents

A kind of vacuum plasma reactor that is used for large area film growth Download PDF

Info

Publication number
CN100567566C
CN100567566C CNB2007101349541A CN200710134954A CN100567566C CN 100567566 C CN100567566 C CN 100567566C CN B2007101349541 A CNB2007101349541 A CN B2007101349541A CN 200710134954 A CN200710134954 A CN 200710134954A CN 100567566 C CN100567566 C CN 100567566C
Authority
CN
China
Prior art keywords
battery lead
lead plate
radio
power supply
plasma reactor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB2007101349541A
Other languages
Chinese (zh)
Other versions
CN101148756A (en
Inventor
辛煜
施毅
左则文
宁兆元
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing University
Suzhou University
Original Assignee
Nanjing University
Suzhou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing University, Suzhou University filed Critical Nanjing University
Priority to CNB2007101349541A priority Critical patent/CN100567566C/en
Publication of CN101148756A publication Critical patent/CN101148756A/en
Application granted granted Critical
Publication of CN100567566C publication Critical patent/CN100567566C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Plasma Technology (AREA)

Abstract

The invention discloses a kind of vacuum plasma reactor that is used for large area film growth, comprise reaction cavity, radio-frequency power supply, described reaction cavity top is provided with air inlet port, the bottom is provided with vacuum pumping opening, be provided with the battery lead plate that is connected by matching network with radio-frequency power supply, the substrate frame electrode that is used for carrying substrates in the described reaction cavity, it is characterized in that: the pole plate array of described battery lead plate for constituting by square-shaped electrode; Described air inlet port is communicated to the gas flow guiding hole that is positioned at each square battery lead plate central authorities through the branched inlet pipe road; Also be provided with the ground connection uniform flow ring that is in the isoplanar with electric pole plate and substrate frame battery lead plate and is arranged in co-axial alignment, be distributed with through hole on the described ground connection uniform flow ring.The present invention has improved the coupling efficiency of radio frequency power, can obtain uniform radio-frequency field in than the big area scope.

Description

A kind of vacuum plasma reactor that is used for large area film growth
Technical field
The present invention relates to a kind ofly be used to adopt the vacuum plasma mode to carry out the device of film growth, be specifically related to a kind of vacuum plasma reactor that is used for large area film growth.
Background technology
Plasma body is that roughly suitable a kind of of the density of ion and electronics is electroneutral ionized gas.The plasma body that industry is used belongs to low-temperature plasma usually, and its plasma density is 10 8-10 11Cm -3Between, the about several electrons volt of average electron temperature is typical weakly ionized gas.These low-temperature plasmas are exciting generation under the condition at certain vacuum under the electromagnetic excitation usually, feeding air pressure in vacuum cavity is that tens milli torrs are to the differential responses gas between tens torrs, can realize substrate sample such as semiconductor wafer, isolator, metal are carried out different processing, as film growth, substrate etching, surface plasma processing etc.
Being used for exciting the hertzian wave form of the low-temperature plasma that produces the industry use can be radio frequency or microwave.But, also need the constraint in magnetic field to produce highdensity plasma body sometimes, thereby complex structure, cost height because the plasma body of microwave-excitation also needs other expensive waveguide components as annex usually; By comparison, consider that the plasma device of radio-frequency drive has simple structure, advantage such as cheap from the angle of processing and manufacturing.
Industrial normal radio frequency (RF) plasma device that uses comprises two classes, one class is that the RF field is transferred to battery lead plate in the vacuum cavity by cable via a matching network, rf electric field is perpendicular to battery lead plate, when the radio frequency power of importing is enough high, radio-frequency field just can make reactant gases ionization, thereby excite the generation radio-frequency plasma, the plasma body that forms in vacuum cavity thus is commonly referred to capacitively coupled plasma; Another kind of is that the RF field is transferred to the ruhmkorff coil that places medium window outside by cable via a matching network, rf electric field is parallel to dielectric-slab, when the radio frequency power of importing is enough high, radio-frequency field just can make reactant gases ionization, thereby excite the generation radio-frequency plasma, the plasma body that forms at vacuum cavity is commonly referred to inductive coupled plasma thus.The matching network that is connected between radio-frequency power supply and battery lead plate or the coil comprises two variable capacitys usually, can make the impedance of radio-frequency power supply and the loaded impedance of plasma body be complementary by regulating these two variable capacitys, thereby obtain maximum radio frequency power transmission efficiency.
Reactant gases normally enters cavity at the reaction cavity top in the spray mode, then by the air-bleed system that the vacuum unit is formed residual gas is extracted out in the bottom of cavity.Substrate sample is placed on the electrode of bottom, plasma exciatiaon district usually.Usually, bottom electrode can heat, and with the heat transferred substrate, improves the quality of substrate surface film growth by heat exchange pattern.When substrate was carried out etching processing, bottom electrode did not then need heating, and applied the rf bias power supply of a lower frequency usually, to strengthen the etching effect of substrate.
Although above-mentioned structure of reactor is through being usually used in processing the sample of prior art, but, handle the large size sample especially need be on glass substrate during the uniform silicon film of high-speed rapid growth big area, the plasma reactor of said structure can not satisfy service requirements.Merely amplify the diameter existing problems of bore and the electroplax plate or the dielectric-slab of reactor: on the one hand, the homogeneity of silicon film growth depends on the homogeneity of electromagnetic wave excites plasma body, and this is decided by that battery lead plate or the ruhmkorff coil above the dielectric-slab in the vacuum plasma reactor encourage the homogeneity that produces radio-frequency field, how to produce the key that uniform radio-frequency field is the large-area vacuum plasma reactor design when therefore, the vacuum reactor bore amplifies.Owing to be subjected to the influence of standing-wave condition, and in order to obtain uniform radio-frequency field, the diameter of battery lead plate or dielectric-slab is restricted, and can't make large-area reaction cavity volume.
Summary of the invention
The object of the invention provides a kind of vacuum plasma reactor that is applicable to large area film growth, and a uniform radio-frequency field is provided in than the big area scope.
For achieving the above object, the technical solution used in the present invention is: a kind of vacuum plasma reactor that is used for large area film growth, comprise reaction cavity, radio-frequency power supply, described reaction cavity top is provided with air inlet port, the bottom is provided with vacuum pumping opening, be provided with the battery lead plate that is connected by matching network with radio-frequency power supply, the substrate frame electrode that is used for carrying substrates in the described reaction cavity, the pole plate array of described battery lead plate for constituting by square-shaped electrode; Described air inlet port is communicated to the gas flow guiding hole that is positioned at each square battery lead plate central authorities through the branched inlet pipe road; Also be provided with the ground connection uniform flow ring that is in the isoplanar with electric pole plate and substrate frame battery lead plate and is arranged in co-axial alignment, be distributed with through hole on the described ground connection uniform flow ring.
Above, constituted the vacuum plasma excitation area between battery lead plate array and the substrate frame electrode, owing to adopt the square-shaped electrode plate to constitute the pole plate array, can obtain uniform radio-frequency field in than the big area scope, simultaneously, the gas flow guiding hole lays respectively at the central authorities of each square-shaped electrode plate, can guarantee the uniform distribution of reactant gases, ground connection uniform flow ring article on plasma body region limits, and avoids plasma body to leak from the battery lead plate side, to improve the homogeneity of plasma body.During use, start radio-frequency power supply, the radio-frequency voltage of output is fed on the battery lead plate in parallel through the output port of matching network, the vertical electric field that utilizes this voltage to produce on battery lead plate comes gas breakdown, the electronics that produces obtains energy from this electric field, and excites the intravital reactant gases of vacuum chamber, makes it to produce ionization, form plasma body, be capacitance coupling plasma.This plasma body is made up of charged electronics and ion, and the reactant gases in the vacuum cavity decomposes under the continuous bump of electronics, produces a large amount of ion or active group, and active group and substrate surface form chemical reaction, are achieved growth for Thin Film.Other volatile resultant of reaction is then extracted cavity out from bleeding point.
Optimized technical scheme, described pole plate array is made of the square-shaped electrode plate parallel connection of 2~4 identical sizes, the length of side of each pole plate is between 200 millimeters to 500 millimeters, each battery lead plate is evenly arranged in same plane, isolated by ceramic insulating material each other, isolation distance is between 1 millimeter to 3 millimeters.
In the technique scheme, be provided with the metal shielding board of ground connection around the end face of described battery lead plate reaches, isolate by insulcrete between described subordinate shielding slab and the battery lead plate.
In the technique scheme, the excitation frequency of described radio-frequency power supply is higher than 27MHz, is beneficial to the raising of plasma density.
Further technical scheme, described substrate frame electrode is connected to DC pulse negative bias power supply through a resonator, filter network structure.The resonator, filter network structure is mainly used in to isolate and comes from radio frequency fundamental current and the higher harmonic current signal that is applied on the array square-shaped electrode; The DC pulse negative bias that substrate applies mainly is the ion composition in the induced plasma, bombardment substrate surface, the bonding force of enhanced film and substrate surface.
In the technique scheme, pulse-repetition, amplitude and the EDM Generator of Adjustable Duty Ratio of described DC pulse negative bias power supply, described pulse-repetition be in the scope of 6KHz~15KHz, and amplitude is between ± 500V, and dutycycle is between 0.1~0.5.
In the technique scheme, described substrate frame electrode has the freedom of motion of vertical direction, to regulate the spacing of plasma excitation region.
Described radio-frequency power supply by the syndeton between matching network and battery lead plate is, penetrates at the reaction cavity top and is provided with electrode, and the middle position that electrode is positioned at the battery lead plate array is connected with each battery lead plate through the cable of isometric symmetrical distribution; Described air inlet port is positioned at electrode tip central authorities, and each air inlet subtube is communicated with air inlet port and comparative electrode is symmetrically distributed.
Further technical scheme, the surface of described battery lead plate and each described cable all is coated with silver conductive layer, and the thickness of silver conductive layer is between 1 micron to 10 microns.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
1. the present invention adopts the mode of battery lead plate parallel connection rather than large electrode plate mode to obtain large-area vacuum plasma excitation area, has improved the coupling efficiency of radio frequency power, can obtain uniform radio-frequency field in than the big area scope;
2. among the present invention, the gas flow guiding hole lays respectively at the central authorities of each square-shaped electrode plate, can guarantee the uniform distribution of reactant gases, and utilizes ground connection uniform flow ring article on plasma body region to limit, avoided plasma body to leak, can improve the homogeneity of plasma body from the battery lead plate side.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention one;
Fig. 2 is the synoptic diagram of battery lead plate array among the figure one.
Wherein: 1, reaction cavity; 2, substrate frame electrode; 3, intake valve; 4, matching network; 5, radio-frequency power supply; 6, branched inlet pipe road; 8, battery lead plate; 10, cable; 12, shielding slab; 13, insulcrete; 14, insulating material; 16, uniform flow ring; 17, electrode; 18, air inlet port; 19, electrical insulation ring; 20, shield ring; 21, filter network; 22, pod apertures.
Embodiment
Below in conjunction with drawings and Examples the present invention is further described:
Embodiment one:
Referring to accompanying drawing 1, wherein plasma reactor comprises vacuum reaction cavity 1, its preferably distributing style be a cylindric design, to guarantee the diad symmetry of reaction cavity 1 relative entire electrode.Reaction cavity 1 has comprised metal sidewall and top cover of a columnar high conduction, and reaction cavity 1 bottom is two and is the bleeding point that symmetry is placed, by vacuum unit (not shown) vacuum suction carried out in reaction cavity 1 inside.Place, top cover axle center is provided with the metal electrode 17 and the co-axial electrical insulation ring 19 of co-axial good conductivity, and electrical insulation ring 19 is isolated electricity between metal electrode 17 and the top cover.Place, the axle center of metal electrode 17 is drilled with air inlet port 18, and the pod apertures 22 that is communicated to each battery lead plate center by branched inlet pipe road 6 evenly imports to the plasma exciatiaon district in the mode of spray.
The symmetrical respectively top that is connected to each sub-electrode plate 8 of each cable 10 that links to each other with metal electrode 17,4 square-shaped electrode plates have been arranged in parallel, isolation distance between the electrode is between 1-2mm, the electrical signal that the first half branch of each sub-electrode plate that all link to each other with cable produces all has the shielding slab 12 of ground connection to shield, be equipped with insulcrete 13 between each battery lead plate and the shielding slab, only the battery lead plate towards the plasma exciatiaon district partly is open.In addition, carry out electricity by electrically insulating material between metal electrode 17 and the shielding slab and isolate, the part of metal electrode 17 in reaction cavity 1 carried out signal shielding by shield ring 20, and electric isolated material is an electrical insulation ring 19.
Second position of substrate frame comprises the bell housing of a ground connection, and the electrically insulating material electricity has been isolated substrate frame electrode 2 and bell housing.Substrate frame electrode 2 links to each other with a pulsed bias power supply by a resonator, filter network.The resonator, filter network is made up of the oscillator circuit of two-stage inductance and electric capacity basically.The two-stage parallel connection loop that inductance and electric capacity are formed mainly be used for stoping very high frequency(VHF) excite generation from plasma body the flow through fundamental current and the second harmonic current of lower electrode plate.In a preferred embodiment, the very high frequency(VHF) excitation frequency is 60MHz, therefore, and the oscillation frequency that two-stage LC oscillator circuit need have been modulated 60MHz and 120MHz respectively.
Need to prove, although the above-mentioned position that utilizes electric pole plate and lower electrode plate can be defined in the plasma body that top crown excited the two-plate zone, but still have the ionized gas of part can escape into other parts of vacuum cavity, thereby reduced the growth homogeneity of the film sample of plasma body on substrate frame from the pole plate excitation area.Comprised in the present embodiment and be provided with the ground connection uniform flow ring 16 that is drilled with many apertures in the periphery of two battery lead plates, the effect of uniform flow ring 16 is to have stoped the diffusion of plasma body to other vacuum areas on the one hand, on the other hand, strengthened the local effect of institute's activated plasma, increase plasma electron density, helped improving the growth velocity of silicon film.
The principle of work of the vacuum plasma reactor of present embodiment is as follows, the process gas that sends with certain flow from gas flow controller flows to the pod apertures at each battery lead plate center by intake valve 3 average marks, and enters into plasma excitation region in the spray mode.In plasma excitation region, process gas is converted the plasma body that is weak ionization under the very high frequency(VHF) effect of electric field, various groups spread the surface that is transported to the substrate frame sample in effect of electric field in the plasma body, form a film sample under certain temperature condition.What electric pole plate applied is a very high frequency(VHF) voltage signal, and what lower electrode applied is a dc negative bias voltage pulse signal.In this preferred embodiment, the very high frequency(VHF) excitation frequency is 60MHz, and the recurrence interval of direct current pulse power source is 8KHz, and dutycycle is 10%.
In the present embodiment, (230mm * 230mm) parallel connection, isolated material each other are tetrafluoroethylene to four prescription shape battery lead plates, and isolation distance is 2 millimeters.Regulate the vertical position of substrate frame, make that the vertical range of substrate frame and battery lead plate is 4 centimetres.With silane (with H 2Mix, blending ratio is 5: 95) with the flow of 100sccm via main induction trunk 18 and each minute induction trunk 6 and 7 enter in the vacuum chamber 1, discharge air pressure is 4Pa, substrate is large-area glass substrate.Starting frequency is the radio-frequency power supply of 60MHz, and the excitation plasma body, and radio frequency power is set at 900W, and the thin film deposition time is 30 minutes.The total thickness of the silicon film of growing on the glass substrate is about 320 nanometers, film in the 400mm scope ununiformity less than 10%.
Embodiment two: (230mm * 230mm) parallel connection, isolated material each other are tetrafluoroethylene to basic structure, and isolation distance is 2 millimeters with embodiment one, four prescription shape battery lead plate.Regulate the vertical position of substrate frame, make that the vertical range of substrate frame and battery lead plate is 5 centimetres.With silane (with H 2Mix, blending ratio is 5: 95) with the flow of 150sccm via main induction trunk 18 and each minute induction trunk 6 and 7 enter in the vacuum chamber 1, discharge air pressure is 15Pa, substrate is large-area glass substrate.Starting frequency is the radio-frequency power supply of 60MHz, and the excitation plasma body, and radio frequency power is set at 1200W, and the thin film deposition time is 30 minutes.The total thickness of the silicon film of growing on the glass substrate is about 500 nanometers, film in the 400mm scope ununiformity less than 6%.

Claims (6)

1. vacuum plasma reactor that is used for large area film growth, comprise reaction cavity (1), radio-frequency power supply (5), described reaction cavity top is provided with air inlet port, the bottom is provided with vacuum pumping opening, be provided with the battery lead plate that is connected by matching network (4) with radio-frequency power supply, the substrate frame electrode (2) that is used for carrying substrates in the described reaction cavity, it is characterized in that: the pole plate array of described battery lead plate (8) for constituting by square-shaped electrode; Described air inlet port is communicated to the gas flow guiding hole that is positioned at each square battery lead plate central authorities through branched inlet pipe road (6); Also be provided with the ground connection uniform flow ring that is in the isoplanar with electric pole plate and substrate frame battery lead plate and is arranged in co-axial alignment, be distributed with through hole on the described ground connection uniform flow ring.
2. vacuum plasma reactor as claimed in claim 1, it is characterized in that: described pole plate array is made of the square-shaped electrode plate parallel connection of 2~4 identical sizes, the length of side of each pole plate is between 200 millimeters to 500 millimeters, each battery lead plate is evenly arranged in same plane, isolated by ceramic insulating material (14) each other, isolation distance is between 1 millimeter to 3 millimeters.
3. vacuum plasma reactor as claimed in claim 1 is characterized in that: the excitation frequency of described radio-frequency power supply is higher than 27MHz.
4. vacuum plasma reactor as claimed in claim 1 is characterized in that: described substrate frame electrode is connected to DC pulse negative bias power supply through a resonator, filter network structure.
5. vacuum plasma reactor as claimed in claim 4, it is characterized in that: pulse-repetition, amplitude and the EDM Generator of Adjustable Duty Ratio of described DC pulse negative bias power supply, described pulse-repetition is in the scope of 6KHz~15KHz, and amplitude is between ± 500V, and dutycycle is between 0.1~0.5.
6. vacuum plasma reactor as claimed in claim 1 is characterized in that: described substrate frame electrode has the freedom of motion of vertical direction, to regulate the spacing of plasma excitation region.
CNB2007101349541A 2007-10-31 2007-10-31 A kind of vacuum plasma reactor that is used for large area film growth Expired - Fee Related CN100567566C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2007101349541A CN100567566C (en) 2007-10-31 2007-10-31 A kind of vacuum plasma reactor that is used for large area film growth

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2007101349541A CN100567566C (en) 2007-10-31 2007-10-31 A kind of vacuum plasma reactor that is used for large area film growth

Publications (2)

Publication Number Publication Date
CN101148756A CN101148756A (en) 2008-03-26
CN100567566C true CN100567566C (en) 2009-12-09

Family

ID=39249451

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2007101349541A Expired - Fee Related CN100567566C (en) 2007-10-31 2007-10-31 A kind of vacuum plasma reactor that is used for large area film growth

Country Status (1)

Country Link
CN (1) CN100567566C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102694148A (en) * 2012-05-28 2012-09-26 东莞新能源科技有限公司 Dry-process deburring method for positive plate of lithium ion battery

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101675106B1 (en) * 2010-05-26 2016-11-11 주식회사 탑 엔지니어링 Device and method of chemical vapor deposition
CN102651424A (en) * 2011-02-25 2012-08-29 苏州大学 Texturing device and method for silicon solar cells
CN103184433A (en) * 2012-05-24 2013-07-03 北京普纳森电子科技有限公司 Gas diffusion homogenization device and plasma process equipment using same
CN102978589B (en) * 2012-12-04 2014-10-15 中国科学院电工研究所 PECVD (plasma enhanced chemical vapor deposition) spray electrode
CN102943251B (en) * 2012-12-05 2015-03-25 山东力诺太阳能电力股份有限公司 Device for enhancing uniformity of PECVD (plasma enhanced chemical vapour deposition) coating film
CN103014660B (en) * 2012-12-14 2015-06-10 广东志成冠军集团有限公司 PECVD (plasma enhanced chemical vapor deposition) coating device and connecting device of radio-frequency power supply and vacuum chamber thereof
CN103458599B (en) * 2013-09-24 2017-02-01 南方科技大学 Low-temperature plasma processing device and method
CN103792842B (en) * 2014-01-22 2016-08-17 清华大学 A kind of base station that can be used for power field spatial distribution precise controlling and control method
CN108257840B (en) * 2016-12-29 2021-03-30 中微半导体设备(上海)股份有限公司 Plasma processing device
CN110446324A (en) * 2019-08-23 2019-11-12 常州汉劼生物科技有限公司 Electrode assembly and the plasma producing apparatus for using the electrode assembly
CN113913790A (en) * 2020-07-08 2022-01-11 湖南红太阳光电科技有限公司 Multi-section type electrode plate glow discharge device for flat plate type PECVD equipment
CN113471051B (en) * 2021-07-20 2023-08-08 电子科技大学长三角研究院(湖州) Coreactor for Joule heat and plasma
CN113966655A (en) * 2021-10-14 2022-01-25 常州大学 Cold plasma biological treatment device
CN114171364B (en) * 2021-12-03 2024-05-17 北京北方华创微电子装备有限公司 Semiconductor processing equipment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102694148A (en) * 2012-05-28 2012-09-26 东莞新能源科技有限公司 Dry-process deburring method for positive plate of lithium ion battery

Also Published As

Publication number Publication date
CN101148756A (en) 2008-03-26

Similar Documents

Publication Publication Date Title
CN100567566C (en) A kind of vacuum plasma reactor that is used for large area film growth
KR100338057B1 (en) Antenna device for generating inductively coupled plasma
CN101136279B (en) Jigger coupling coil and jigger coupling plasma device
KR101591404B1 (en) Plasma generating apparatus and plasma processing apparatus
US6899054B1 (en) Device for hybrid plasma processing
US7575987B2 (en) Method of plasma doping
CN201465987U (en) Plasma treatment device
TWI448215B (en) Apparatus for plasma processing
US20120258606A1 (en) E-Beam Enhanced Decoupled Source for Semiconductor Processing
US20100074807A1 (en) Apparatus for generating a plasma
CN109935511B (en) Plasma processing apparatus
CN103695868A (en) Linear plasma-enhanced chemical vapor deposition system with remote magnetic-mirror field constraint
KR101626039B1 (en) Consecutive substrate processing system using large-area plasma
CN101131893B (en) Inductance coupling coil and inductance coupling plasma body device
CN101042991B (en) Plasma processing apparatus
JP2760845B2 (en) Plasma processing apparatus and method
KR20080028848A (en) Inductively coupled plasma reactor for wide area plasma processing
JP4598253B2 (en) Plasma device
CN102534524B (en) Reaction chamber for PVD (Physical Vapor Deposition) process and PVD system
JP3485013B2 (en) Plasma processing method and apparatus
WO2012142038A1 (en) E-beam enhanced decoupled source for semiconductor processing
KR20020035249A (en) Device and Method for Generating Capacitively Coupled Plasma Enhanced Inductively Coupled Plasma
CN110415948B (en) Three-dimensional four-spiral inductance coupling coil
JPH05182785A (en) Microwave discharge reaction device and electrode device
KR101013357B1 (en) High power plasma generation apparatus

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20091209

Termination date: 20121031