CN1256462C - Hot wire auxiliary microwave electron rotating resonance chamical gas phase settling method and device - Google Patents
Hot wire auxiliary microwave electron rotating resonance chamical gas phase settling method and device Download PDFInfo
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- CN1256462C CN1256462C CN 200310110350 CN200310110350A CN1256462C CN 1256462 C CN1256462 C CN 1256462C CN 200310110350 CN200310110350 CN 200310110350 CN 200310110350 A CN200310110350 A CN 200310110350A CN 1256462 C CN1256462 C CN 1256462C
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Abstract
The present invention relates to a hot wire auxiliary microwave electron rotating resonance chemical gas phase settling method and a device, which belongs to the field of microwave low temperature plasma. The method comprises a microwave source and plasma, wherein the microwave source is used in an electron rotating resonance system, and a magnetic field coil of the plasma generates electron rotating resonance in a resonant cavity. The method is characterized in that a hot wire unit generating thermal radiation to the plasma is added between a resonant cavity outlet and a sample wafer station of a settling chamber, and gases in the plasma are prompted to be more sufficiently decomposed; a ring is arranged out of the plasma and can not block thin film deposition. The device is characterized in that the hot wire unit prompting the sufficient decomposition of the gases is arranged between the outlet of the resonant cavity 10 and the sample wafer station 12 of the settling chamber 11; the hot wire unit is composed of a hot wire ring 15 arranged in the settling chamber 11, a holding electrode 16 for fixing the hot wire ring 15, an electrode 17 of evacuated package and a hot wire power supply 18 arranged out of the settling chamber 11; the plasma 23 in the settling chamber 11 penetrates through the hot wire ring 15. The present invention solves the problem of insufficient decomposition of gases and groups in plasma.
Description
Technical field
Auxiliary microwave electron cyclotron resonance chemical gaseous phase depositing process of heated filament and device belong to the microwave low temperature plasma technical field.
Background technology
Gas molecule is decomposed more fully, for the nonthermal plasma chemistry vapour deposition, is very important and crucial technology.Microwave electron cyclotron resonance chemical vapour deposition (ECR-CVD) is the novel thin film technology of preparing that grows up the nearly more than ten years.Because its degree of ionization height, group activity are greatly, particle energy is easy to characteristics such as control, is subject to people's attention day by day.But, when application the type conventional apparatus is carried out the high speed deposition of film, still find to exist gas molecule to decompose inadequately problem fully.
For example, at silane (SiH
4) during plasma body high speed deposition of amorphous silicon (a-Si:H) film, the problem that ubiquity film hydrogen content is higher, at the film hydrogen content of 250 ℃ of deposit up to 20~30atom% (M S Kang, J Y Kim, et al, Characteristic of a-Si:H films preparedby ECR-CVD as a function of theH
2/ SiH
4, Mater.Chem.Phys.1997,51:152-156).Like this high hydrogen content is unfavorable for the light durability of film.Generally speaking, silane (SiH
4) there is SiH in the plasma body of gas
3, SiH
2, SiH, Si and H and ionic group thereof, and SiH wherein
3The group proportion is maximum, the SiH in the plasma body
3Content is high more, and the film hydrogen content is high more.To when guaranteeing the film high speed deposition, reduce the hydrogen content of film, must make silane (SiH
4) gas molecule decomposes more fully.
Up to the present, for applied microwave electron cyclotron resonance chemical vapor deposition device carries out the film high speed deposition, still do not have a kind of comparatively simple method, can solve gas and the sufficient inadequately problem of group decomposition in the plasma body preferably.
Summary of the invention
The objective of the invention is to, be at the still sufficient inadequately problem of decomposing gas in the existing plasma body of Ecr plasma applied technical field, proposed a kind of new method and solved this problem.And be the technical scheme of Method Of Accomplishment, designed the auxiliary microwave electron cyclotron resonance chemical vapor deposition unit of heated filament.
The auxiliary microwave electron cyclotron resonance chemical gaseous phase depositing process of heated filament in the technical scheme of the present invention: include the microwave source that utilizes in the electron cyclotron resonace system, magneticfield coil produces electron cyclotron resonace in resonator cavity plasma body, this plasma body enters the sediment chamber through the resonator cavity outlet, be used for exemplar is carried out thin film deposition, it is characterized in that, between the print platform of resonator cavity outlet and sediment chamber, produce strong thermal-radiating heated filament unit but increase an article on plasma body, impel the gas in the plasma body to decompose more fully; And the heated filament ring is positioned at outside the plasma body, can not hinder depositing of thin film.
The auxiliary mechanism of impelling the gas in the plasma body fully to decompose of heated filament is: on the basis of traditional microwave Ecr plasma, it is auxiliary to increase heated filament, mean that extra article on plasma body carries out strong and the successive thermal radiation, this intensive thermal radiation, to the kinetic energy of gas molecule and group significantly be increased the thermal radiation transmission ofenergy to gas molecule and group in the plasma body.(electron cyclotron resonace constantly is coupled microwave energy and gives electronics being subjected to the high-energy electron of same energy, make it become high-energy electron) do the time spent, easier decomposition of the gas molecule of kinetic energy and group and ionization, thus impel the reactant gases in the plasma body to decompose more fully.
The auxiliary microwave electron cyclotron resonance chemical vapor deposition unit of heated filament in the technical scheme of the present invention, include microwave source, vacuum-sealing, thin film deposition, vacuum pump system, produce electron cyclotron resonace and deposit required axial magnetic field part, gas circuit and gas control section, each several part downward more backward annexation in the past is followed successively by, microwave generator 1 connects waveguide 2, waveguide 2 connects three end circulators 3, the reflection end of three end circulators 3 is connected with high power load 4, the exit end of three end circulators 3 is connected with three pin tuners 5, three pin tuners 5 are connected with the transition rectangular waveguide 6 of band level and vertical section, transition rectangular waveguide 6 is connected with vertical waveguide 7 downwards, window flange 9 upper surfaces that central authorities open rectangular opening are connected with waveguide 7, the lower surface of window flange 9 is pressed in ceramic microwave window 8 on the upper surface of resonator cavity 10, the upper surface of the sediment chamber 11 that the lower surface of resonator cavity 10 and diameter are bigger is connected, print platform 12 links to each other with permanent magnet unit 13, permanent magnet unit 13 is fixed on the exit end place of sediment chamber's 11 lower bottom parts by its support bar, side, 11 below, sediment chamber tapping is connected with the vacuum pump system of being made up of rotor pump 19 and turbomolecular pump 20, sediment chamber's outer wall is fixed on the worktable 14, single and magneticfield coil 21 is positioned at outside cylindrical cavity 10 walls, and be coaxial arrangement with cylindrical cavity 10, coil 21 is supported by three uniform on 11 upper surfaces, sediment chamber pillars, the gas circuit 22 that is divided into two-way, one the tunnel links to each other with resonator cavity, another road links to each other with the sediment chamber, after wherein reactant gases feeds resonator cavity 10 and sediment chamber 11, in resonator cavity 10, form Ecr plasma 23 and enter sediment chamber 11 through resonator cavity 10 outlets, the present invention is characterised in that: be provided with the heated filament unit that the reactant gases that impels in the plasma body 23 decomposes more fully between the print platform 12 in resonator cavity 10 outlet and sediment chamber 11, this heated filament unit is by the heated filament ring 15 that places in the sediment chamber 11, the fixing holding electrode 16 of heated filament ring 15, Vacuum Package electrode 17 and place the outer heater supplies in sediment chamber 11 18 to form passes in the heated filament ring 15 of plasma body 23 from this heated filament unit in the sediment chamber 11.The diameter of heated filament ring is positioned at outside the plasma body greater than the cross-sectional diameter of position plasma body, and can the article on plasma body transport to form stops.Therefore, said apparatus has been finished technical scheme of the present invention preferably.
Adopt the auxiliary obtained actual effect of microwave electron cyclotron resonance chemical vapor deposition unit of heated filament of the present invention to be:
1, the reactant gases in the Ecr plasma is fully decomposed.The reactant gases that has solved in the existing Ecr plasma decomposes inadequately problem fully
2, on the basis of traditional microwave electron cyclotron resonance chemical vapor deposition device, increase the heated filament unit, to make, install very easy, cost is lower.
Auxiliary microwave electron cyclotron resonance chemical gaseous phase depositing process of heated filament of the present invention and device, owing to solved the sufficient inadequately problem of molecular breakdown in the traditional microwave Ecr plasma preferably, created favourable condition for further using and developing the microwave electron cyclotron resonance plasma chemical vapour deposition technique.
Description of drawings
Fig. 1 heated filament is assisted microwave electron cyclotron resonance chemical vapor deposition unit synoptic diagram 1-microwave generator, 2-horizontal rectangular waveguide, 3-three end circulators, the 4-high power load, 5-three pin tuners, the transition rectangular waveguide of 6-band level and vertical section, the waveguide 8-ceramic microwave window of 7-ditrigon, 9-window flange, 10-cylindrical cavity, 11-sediment chamber, 12-print platform, the 13-permanent magnet, 14-worktable, 15-ring-type heated filament, the 16-holding electrode, 17-Vacuum Package electrode, 18-heater supply, 19-rotor pump, the 20-turbomolecular pump, the 21-magneticfield coil, 22-gas circuit and gas control unit, 23-plasma body
Fig. 2 heated filament and holding electrode interface chart
24-holding electrode bar, 25-clamping sheath, 26-connection piece, 27-nut, 34-heated filament termination, 35-silk rolling hole
Fig. 3 holding electrode and Vacuum Package electrode interface chart
The 28-standing screw, 29-Vacuum Package battery lead rod, 30-connects ring plate, 31-insulating ceramic, 32-stainless steel sleeve, 33-vacuum blind plate
Embodiment
By the heated filament unit that ring-type heated filament 15, holding electrode 16, Vacuum Package electrode 17 and heater supply 18 are formed, be features component of the present invention, its structure is referring to Fig. 2 and Fig. 3.Ring-type heated filament ring 15 can be selected resistant to elevated temperatures thermal-radiating material for use in the described heated filament unit; Holding electrode 16 is to be enclosed within on the holding electrode bar 24 by clamping sheath 25, and being locked with nut 27 forms again; Vacuum Package electrode 17 is by standing screw 28, Vacuum Package battery lead rod 29, connecting ring plate 30, insulating ceramic 31, stainless steel sleeve 32 and vacuum blind plate 33 forms, Vacuum Package battery lead rod 29 adopts Vacuum Soldering Technology to connect with being connected ring plate 30, insulating ceramic 31, stainless steel sleeve 32 each other, adopts the argon arc welding technology to connect between the vacuum blind plate 33 stainless steel sleeves 32; Holding electrode 16 is connected with standing screw 28 by nut 27 with Vacuum Package electrode 17; Heater supply 18 is selected for use and is output as the low-voltage and high-current power supply.
The unitary installation order of heated filament is followed successively by: the silk rolling hole 35 of heated filament termination 34 holding electrode bars 24 is put clamping sheath 25, regulate circle diameter, set nut 27 makes heated filament be state shown in Figure 2.Next, Vacuum Package electrode and deposition chamber wall are fixed, because encapsulated electrode adopted the vacuum blind plate, the two can connect fast and fix by standard clip spare.At last, holding electrode 16 is connected set nut 27 by web plate 26 with the Vacuum Package electrode.So far install to reach to fix and all finish.
The auxiliary microwave electron cyclotron resonance chemical vapor deposition unit of heated filament of the present invention is seen Fig. 1, mainly comprises seven parts.First part is a microwave source.This part is used for providing microwave to the electron cyclotron resonace resonator cavity of vertical placement.Microwave source is made up of microwave generator 1, transmission system and Controlling System, and wherein transmission system is made up of three end circulators 3, three pin tuners 5 and waveguide again.Microwave generator 1 and transmission system are in the extreme higher position of apparatus of the present invention in the space, each several part downward more backward annexation in the past is, the following outlet of microwave generator 1 is connected by bolt with horizontal rectangular waveguide 2 upper inlets, rectangular waveguide 2 carries out flange with three end circulators, 3 inlet ends again and is connected, the reflection end of three end circulators 3 carries out flange with high power load 4 and is connected, the exit end of three end circulators 3 carries out flange with three pin tuners 5 and is connected, three pin tuners 5 carry out flange with the transition rectangular waveguide 6 of band level and vertical section again and are connected, and transition rectangular waveguide 6 carries out flange with the waveguide 7 of vertical ditrigon downwards and is connected.Second section is the window flange 9 that ceramic microwave window 8 and central authorities open rectangular opening, and this part is used for microwave is coupled into resonator cavity and vacuum-sealing is provided.The waveguide 7 of vertical placement carries out flange and is connected in window flange 9 upper surfaces and the first part, and the lower surface is adopted bolt to connect the ceramic microwave window is pressed on the upper surface of the cylindrical cavity 10 in the third part.Third part is made up of cylindrical cavity 10, sediment chamber 11, print platform 12, permanent magnet unit 13 and the worktable 14 etc. of vertical placement.This part is mainly used in and forms plasma body and carry out thin film deposition.The upper surface of the sediment chamber 11 that the lower surface of cylindrical cavity 10 and diameter are bigger is connected with bolting by flat seal, and print platform 12 is connected by bolt with the exit end of sediment chamber's 11 lower bottom parts by support bar with permanent magnet unit 13 and rubber seal is fixed.The 4th part is made up of heated filament ring 15, holding electrode 16, Vacuum Package electrode 17 and heater supply 18, is mainly used in to plasma body thermal radiation is provided.Ring-type heated filament 15 is fixed by holding electrode 16 and conductive channel is provided, and holding electrode 16 is connected with Vacuum Package electrode 17, and Vacuum Package electrode 17 is connected with heater supply 18, and fixes with deposition chamber wall.The 5th part is made up of rotor pump 19 and turbomolecular pump 20, is used for bleeding from the below, sediment chamber and keeping vacuum tightness.Sediment chamber's outer wall and worktable 14 are fixed together.The 6th part is single and magneticfield coil 21 and coil power, and this part is used to produce electron cyclotron resonace and deposits required axial magnetic field (permanent magnet unit 13 also is the important component part of deposition with axial magnetic field).The 7th part is gas circuit 22 and gas control unit, is used to provide plasma gas and deposition and purge gas.
Example 1: do not adopt heated filament situation deposit amorphous silicon membrane
Experiment condition is that system is evacuated to 1 * 10
-3Pa, to the silane of resonator cavity feeding diluted in hydrogen, flow is 30sccm, and air pressure is transferred to 2.0Pa, and magneticfield coil feeds the electric current of 116A, and the microwave source real output is got 500W.Heater strip not.The energising of print platform is heated to 250 ℃.
Print platform surface temperature in the film deposition process maintains 250~267 ℃.Deposition finishes the back film is detected, and the result who obtains is: thin film deposition speed is 2.5nm/s, and hydrogen richness is 25atom% in the film.
Example 2: adopt heated filament situation deposit amorphous silicon membrane
Experiment condition is that system is evacuated to 1 * 10
-3Pa, to the silane of resonator cavity feeding diluted in hydrogen, flow is 30sccm, and air pressure is transferred to 2.0Pa, and magneticfield coil feeds the electric current of 116A, and the microwave source real output is got 500W.Heater strip, the heater material is tungsten filament (tungstenic reaches more than 99.9%), and diameter 0.5mm, the diameter of heated filament ring are 120mm (heated filament planar plasma body of living in diameter is 80mm), heated filament is fixed by holding electrode and Vacuum Package electrode, and heated filament to the distance of print platform is 80mm.Heater supply is selected 10KW single-phase voltage regulating transformer for use.Heat-obtaining silk temperature is 1450 ℃ (detecting with infrared thermometer), the heating of print platform no power.
Print platform surface temperature in the film deposition process is 167~207 ℃.Deposition finishes the back film is detected, and the result who obtains is: thin film deposition speed is 2.2nm/s, and hydrogen richness is 7atom% in the film.
Comparative example 1 and example 2, as can be seen, example 2 adopts under the auxiliary situation of heated filament, the print platform is because not energising heating, though there is heated filament that it is carried out thermal radiation, its temperature is 167~207 ℃ only in deposition process, is lower than example 1 and does not adopt print platform temperature (250~267 ℃) under the auxiliary situation of heated filament.But experiment finds that but the hydrogen richness of film is 7atom% only in the example 2, and in the example 1 hydrogen richness of film up to 25atom%.General rule is, the low more film hydrogen richness of print platform temperature is high more, and this experimental result is contradiction with it obviously.Unique explanation is exactly that the adding of heated filament makes SiH
4Plasma body has obtained decomposing more fully, has increased the content of low hydrogen group, thereby has reduced the hydrogen richness of film effectively.
Need to prove that in addition at present, the high speed deposition of amorphous silicon membrane is meant that sedimentation velocity is greater than 0.3mn/s.After heated filament added, when reducing the film hydrogen content significantly, thin film deposition speed was reduced to 2.2nm/s by 2.5nm/s, slightly reduce, but thin film deposition speed still was in very high level.
Claims (3)
1, the auxiliary microwave electron cyclotron resonance chemical gaseous phase depositing process of heated filament: include the microwave source that utilizes in the electron cyclotron resonace system, magneticfield coil produces electron cyclotron resonace in resonator cavity plasma body, this plasma body enters the sediment chamber through the resonator cavity outlet, be used for exemplar is carried out thin film deposition, it is characterized in that, between the print platform of resonator cavity outlet and sediment chamber, produce strong thermal-radiating heated filament unit but increase an article on plasma body, impel the gas in the plasma body to decompose more fully; And the heated filament ring is positioned at outside the plasma body, can not hinder depositing of thin film.
2, heated filament is assisted the microwave electron cyclotron resonance chemical vapor deposition unit, include microwave source, vacuum-sealing, thin film deposition, vacuum pump system, produce electron cyclotron resonace and deposit required axial magnetic field part, gas circuit and gas control section, each several part downward more backward annexation in the past is followed successively by, microwave generator (1) connects waveguide (2), waveguide (2) connects three end circulators (3), the reflection end of three end circulators (3) is connected with high power load (4), the exit end of three end circulators (3) is connected with three pin tuners (5), three pin tuners (5) are connected with the transition rectangular waveguide (6) of band level and vertical section, transition rectangular waveguide (6) is connected with vertical waveguide (7) downwards, window flange (9) upper surface that central authorities open rectangular opening is connected with waveguide (7), the lower surface of window flange (9) is pressed in ceramic microwave window (8) on the upper surface of resonator cavity (10), the upper surface of the sediment chamber (11) that the lower surface of resonator cavity (10) is bigger with diameter is connected, print platform (12) links to each other with permanent magnet unit (13), permanent magnet unit (13) is fixed on the exit end place of sediment chamber (11) lower bottom part by its support bar, side, below, sediment chamber (11) tapping is connected with the vacuum pump system of being made up of rotor pump (19) and turbomolecular pump (20), sediment chamber's outer wall is fixed on the worktable (14), single and magneticfield coil (21) is positioned at outside cylindrical cavity (10) wall, and be coaxial arrangement with cylindrical cavity (10), coil (21) is supported by three uniform on the upper surface, sediment chamber (11) pillars, the gas circuit (22) that is divided into two-way, one the tunnel links to each other with resonator cavity, another road links to each other with the sediment chamber, after wherein reactant gases feeds resonator cavity (10) and sediment chamber (11), in resonator cavity (10), form Ecr plasma (23) and enter sediment chamber (11) through resonator cavity (10) outlet, the present invention is characterised in that: be provided with the heated filament unit that the reactant gases that impels in the plasma body (23) decomposes more fully between the print platform (12) in resonator cavity (10) outlet and sediment chamber (11), this heated filament unit is by the heated filament ring (15) that places in the sediment chamber (11), the fixing holding electrode (16) of heated filament ring (15), Vacuum Package electrode (17) and place the outer heater supply (18) in sediment chamber (11) to form passes in the heated filament ring (15) of plasma body (23) from this heated filament unit in sediment chamber (11).
3, the auxiliary microwave electron cyclotron resonance chemical vapor deposition unit of heated filament according to claim 2, be characterised in that: ring-type heated filament ring (15) is used resistant to elevated temperatures thermal-radiating material in the described heated filament unit; Holding electrode (16) is to be enclosed within on the holding electrode bar (24) by clamping sheath (25), uses nut (27) to be locked again and forms; Vacuum Package electrode (17) is by standing screw (28), Vacuum Package battery lead rod (29), connecting ring plate (30), insulating ceramic (31), stainless steel sleeve (32) and vacuum blind plate (33) forms, Vacuum Package battery lead rod (29) adopts Vacuum Soldering Technology to connect with being connected ring plate (30), insulating ceramic (31), stainless steel sleeve (32) each other, adopts the argon arc welding technology to connect between vacuum blind plate (33) the stainless steel sleeve (32); Holding electrode (16) is connected with standing screw (28) by nut (27) with Vacuum Package electrode (17); Heater supply (18) is selected for use and is output as the low-voltage and high-current power supply.
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CN 200310110350 CN1256462C (en) | 2003-12-31 | 2003-12-31 | Hot wire auxiliary microwave electron rotating resonance chamical gas phase settling method and device |
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Families Citing this family (6)
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CN100593585C (en) * | 2007-08-21 | 2010-03-10 | 西安电子科技大学 | Microwave electron cyclotron resonance plasma chemistry gas phase sedimentation device |
CN102413627B (en) * | 2011-07-22 | 2013-03-20 | 中国科学院空间科学与应用研究中心 | Method for changing parameter of plasma |
CN108834296B (en) * | 2018-06-27 | 2020-07-10 | 安徽航天环境工程有限公司 | Microwave plasma device |
CN109640505A (en) * | 2019-02-25 | 2019-04-16 | 成都新光微波工程有限责任公司 | A kind of large power high efficiency multipurpose microwave plasma torch |
CN111850506B (en) * | 2020-07-07 | 2022-06-17 | 武汉大学深圳研究院 | Device and method for preparing n-type doped diamond by microwave plasma-hot wire composite chemical vapor deposition |
CN115613140B (en) * | 2022-12-16 | 2023-03-21 | 江苏邑文微电子科技有限公司 | Transverse plasma generating chamber and multifunctional high-temperature reaction device |
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