CN1644754A - Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof - Google Patents
Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof Download PDFInfo
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- CN1644754A CN1644754A CN 200410011164 CN200410011164A CN1644754A CN 1644754 A CN1644754 A CN 1644754A CN 200410011164 CN200410011164 CN 200410011164 CN 200410011164 A CN200410011164 A CN 200410011164A CN 1644754 A CN1644754 A CN 1644754A
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Abstract
The invention was about low voltage metal organic chemistry vapour deposition equipment and the preparation. The system was made up of gas transport system, reaction chamber, sample pretreatment chamber, control system, tail gas treatment system. The sample pretreatment chamber was made up of ectotheca, sample pallet shelf, sample desk, gas bleed spore, plasma generator, flange, plate valve of switch between the sample pretreatment chamber and reaction chamber, flange of plate valve, magnetic transmit bar, magnetic cannula, flange of transmit bar. Its advantages include increased the growing of ZnO film and uniformity, benefit for the P type and intermingle of high impedance.
Description
Technical field
The present invention relates to the equipment and the growth technique thereof of wide band gap semiconducter ZnO film material growth, particularly relate to organometallics gas deposition (MOCVD) equipment of a kind of low pressure condition work and utilize the processing method of this equipment growing ZnO thin-film material.
Background technology
Zinc oxide (ZnO) material is another important wide bandgap semiconductor materials of world's photoelectric field hot research after gan (GaN), and its band gap and lattice parameter and GaN are very approaching, and crystal formation is identical, and close photoelectric characteristic is arranged.And ZnO also has higher fusing point and exciton bind energy, and exciton gain is higher, epitaxy temperature required low, cost is low, etching and make the more convenient grade of follow-up complete processing be better than the multifrequency nature of GaN easily demonstrates than GaN and has bigger development potentiality.The growth of ZnO film material has several different methods, and evaporation, magnetron sputtering, ion beam sputtering, pulsed laser deposition (PLD), organometallics vapour deposition (MOCVD), molecular beam epitaxy (MBE) etc. are arranged.Sputter is the most frequently used method, but can only grow second-rate polycrystal film, can not satisfy many preparation of devices needs.The MOCVD method can growing large-area evenly, optics and all higher ZnO film of crystalline quality, be fit to suitability for industrialized production.Therefore being fit to the MOCVD equipment of preparation ZnO film material and exploring new processing method is the problem that present scientific and technological circle and industrial community need to be resolved hurrily.Present and the immediate existing MOCVD equipment of the present invention is the MOCVD equipment with vertical response chamber that U.S. Emcore company makes.This MOCVD equipment is made of gas transport system, reaction chamber, Controlling System, exhaust treatment system etc.Wherein most crucial part is a reaction chamber, see accompanying drawing 1, the reaction chamber of this MOCVD equipment is by the base flange plate that has aspirating hole (8) (1), reaction chamber sidewall (2), turning axle (3), magnetic fluid bearing (4), motor (5), upper flange plate (6), Stainless Steel Cloth (7), heating piece (9), substrate slice pallet (10), main source gas circuit (11), secondary gas circuit (12), (13), mixing chamber (14) waits parts to constitute.
With the mocvd method growing ZnO thin-film normally with the alkylate zinc ethyl [Zn (C of Zn
2H
5)
2] or zinc methide [Zn (CH
3)
2] be the Zn source, with the high purity oxygen O source, on sapphire (other substrates such as Si, GaAs or ZnO) substrate, grow.MOCVD equipment with U.S. Emcore company makes runs into following insoluble problem when growing ZnO thin-film:
1. because Zn (C
2H
5)
2[Zn (CH
3)
2] all with O
2Gas-phase reaction very easily takes place, if this two provenance feeds reaction chamber by main source gas circuit (11) or secondary gas circuit (12), (13) simultaneously, will meet in the reaction chamber space before arriving substrate, react, thereby grow into the ZnO particle, be deposited on the substrate, make the growth quality variation of ZnO film;
2. usually the ZnO film of growth thereby realizes that ZnO material p type or high resistant doping are very difficult because nonstoichiometry than having oxygen room and gap zinc atom, makes material be the n type;
3. for uniformly growing film material on substrate, the source must be evenly distributed on the substrate surface.
4. heat distribution should be very even on the substrate, otherwise will influence the homogeneity of ZnO film thickness and quality;
5. sample directly enters reaction chamber, and substrate, sample and reaction chamber all are subject to topsoil.
Summary of the invention
The object of the invention provides and a kind ofly is grown in Organometallic chemical vapor deposition (MOCVD) equipment of growing zinc oxide film special use under the low pressure condition and utilizes the grow processing method of high crystalline quality and high optical quality zinc-oxide film of this equipment.
MOCVD of the present invention system also is by the gas transport system, reaction chamber (101), Controlling System, exhaust treatment systems etc. partly constitute, wherein reaction chamber (101) (seeing accompanying drawing 2 and accompanying drawing 2 explanations) is by the base flange plate that has aspirating hole (8) (1), reaction chamber sidewall (2), turning axle (3), magnetic fluid bearing (4), motor (5), upper flange plate (6), Stainless Steel Cloth (7), heating piece (9), substrate slice pallet (10), impurity source gas circuit (11), secondary gas circuit (12) (13), mixing chamber (14), zinc source spray gun (15), oxygen source spray gun (16), even air-casing (17), radio-frequency (RF) plasma reactor (18) parts constitute; Feature of the present invention is the impurity source gas circuit (11) that former main gas circuit (11) is changed into logical impurity source, a radio-frequency (RF) plasma reactor of interpolation (18) below the impurity source gas circuit (11) in mixing chamber (14), impurity source gas enters reaction chamber after entering radio-frequency (RF) plasma reactor (18) ionization again; Insert zinc source spray gun (15) and oxygen source spray gun (16) respectively in the sidewall both sides of reaction chamber; All add on zinc source spray gun (15) and the oxygen source spray gun (16) and be with even air-casing (17).In order to suppress Zn (C
2H
5)
2(or [Zn (CH
3)
2]) and O
2Gas-phase reaction takes place in the space generate the ZnO particle deposition on substrate, the Zn (C that feature of the present invention also has Ar to carry
2H
5)
2(or [Zn (CH
3)
2]) pass through zinc source spray gun (15) and O
2Feed reaction chamber respectively by oxygen source spray gun (16), spray gun is very near from substrate, can not surpass 2 centimetres farthest, and several millimeters distances are best, the open slots (19) of even air-casing (17) (referring to accompanying drawing 3 and accompanying drawing 3 explanations) towards the below towards substrate, like this from the Zn (C of two even air-casings ejections
2H
5)
2(or [Zn (CH
3)
2]) and O
2Do not meet, only on the moving substrate of high speed rotating, meet and react in the reaction chamber space.Thereby suppressed Zn (C
2H
5)
2(or [Zn (CH
3)
2]) and O
2In the space gas-phase reaction taking place generates the problem of ZnO particle deposition on substrate.For zinc source and oxygen source are evenly distributed on substrate surface, feature of the present invention all adds on zinc source spray gun (15) and oxygen source spray gun (16) in addition and is with even air-casing (17), shut on the spray gun top, spray gun evenly has 1～2 millimeter aperture (seeing accompanying drawing 3 and accompanying drawing 3 explanations) every 3～5 millimeters vertically upward, the open slots (19) of even air-casing (17) towards the below towards substrate, enter reaction chamber from open slots (19) again after zinc source and oxygen source air-flow are turned back by even air-casing (17) from the aperture ejection back of spray gun like this and spray to substrate, if so just can overcome the source air-flow from the aperture of spray gun during directly towards substrate, the source air-flow of ejection is difficult to uniform problem, thereby obtains the high source air-flow of homogeneity.In order to make the substrate homogeneous heating, feature of the present invention also is the oxidation resistant resistance-type heating piece (9) of particular design, this heating piece is radial (seeing Fig. 4 and Fig. 4 explanation), thermal field is even during heating, when being heated evenly to around expand, can prevent influences heats because of cold cycling makes heater texturing, and the material of heating piece (9) is oxidation resistant molybdenum sheet.
As to further improvement of the present invention, in order to improve the base vacuum degree of reaction chamber, make reaction chamber cleaner, the present invention has also added molecular pump (20) in the bottom of reaction chamber, and molecular pump can make the vacuum tightness of reaction chamber reach 10
-3-10
-4Pa.
Directly enter reaction chamber in order to overcome sample, make substrate sample and reaction chamber all be subject to the problem of topsoil, the present invention has also added the substrate sample pretreatment chamber (102) that links with reaction chamber, by pretreatment chamber's outer wall (21), sample tray frame (22), sample table (23), pretreatment chamber's aspirating hole (24), plasma generator (25), plasma generator device flange (26), substrate sample pretreatment chamber and reaction chamber be connected slide valve (27), slide valve flange (28), magnetic force driven rod (29), magnetosheath (30), driven rod flange parts such as (31) constitute.
Utilize equipment of the present invention and technology, in the process of zinc-oxide film growth, can fully suppress Zn (C
2H
5)
2(or [Zn (CH
3)
2]) and O
2In the space gas-phase reaction taking place grows into the ZnO particle, characteristics such as the source is evenly distributed on substrate surface, substrate homogeneous heating, reaction chamber cleanliness factor height all make the zinc-oxide film of growth have high crystalline quality and optical quality, thereby help obtaining p type or the adulterated zinc-oxide film of high resistant.
Description of drawings
Fig. 1: the MOCVD equipment reaction chamber structural representation that U.S. Emcore company makes;
Fig. 2: the MOCVD equipment reaction chamber structural representation that the present invention manufactures and designs;
Fig. 3 (a): the MOCVD reaction chamber spray gun structure synoptic diagram of the present invention's design;
Fig. 3 (b): the equal air-casing open slots of the MOCVD reaction chamber spray gun synoptic diagram of the present invention's design;
Fig. 4: the heating piece synoptic diagram of the present invention's design;
Fig. 5: the X-ray diffraction spectrogram of ZnO film;
Fig. 6: the room temperature Raman spectra of ZnO film sample;
Fig. 7: the atomic force microscope stereographic map of ZnO film;
As shown in Figure 1, parts (1) are base flange plate, and (2) are the reaction chamber sidewall, (3) be turning axle, (4) are magnetic fluid bearing, and (5) are motor, (6) be upper flange plate, (7) be Stainless Steel Cloth, (8) are aspirating hole, and (9) are heating piece, (10) be the substrate slice pallet, (11) be main source gas circuit, (12), (13) are secondary gas circuit, and (14) are mixing chamber.
As shown in Figure 2, parts (1) are base flange plate, (2) be the reaction chamber sidewall, (3) be turning axle, (4) be magnetic fluid bearing, (5) be motor, (6) are upper flange plate, and (7) are Stainless Steel Cloth, (8) be aspirating hole, (9) be heating piece, (10) are the substrate slice pallet, and (11) are the impurity source gas circuit, (12), (13) be secondary gas circuit, (14) be mixing chamber, (15) are zinc source spray gun, and (16) are the oxygen source spray gun, (17) be even air-casing, (18) be radio-frequency (RF) plasma reactor, can select the model of radio frequency power source, promptly select the maximum radio frequency output rating of radio frequency power source according to the size of reaction chamber, the SY1000W radio frequency power source and the SP II radio frequency adaptation that have adopted Chinese Academy of Sciences's Beijing microelectronics center to produce in the present invention, the size of reaction chamber can design in proportion according to the size of substrate slice pallet, and (20) are molecular pump, has constituted reaction chamber (101) with upper-part; (21) be pretreatment chamber's outer wall, (22) for sample tray frame, (23) for sample table, (24) pretreatment chamber aspirating hole, (25) for plasma generator, (26) plasma generator device flange, (27) are the driven rod flange for the be connected slide valve, (28) slide valve flange, (29) magnetic force driven rod, (30) magnetosheath, (31) of substrate sample pretreatment chamber and reaction chamber, constituted the substrate sample pretreatment chamber (102) that links with reaction chamber with upper-part.
As shown in Figure 3, parts (15) are zinc source spray gun, (16) be the oxygen source spray gun, spray gun (15), (16) shut on the top, spray gun evenly has 1～2 millimeter aperture every 3～5 millimeters vertically upward, spray gun is made by the stainless steel tube of 4～6 millimeters of diameters, (17) be even air-casing, even air-casing (17) has open slots (19), even air-casing (17) is to be made by the stainless steel tube of 6～10 millimeters of diameters, one end is an opening, be inserted in spray gun (15) by opening end, (16), also shut on the other end top (two tops that even air-casing is relative), and the width of open slots (19) is 1～2 millimeter, to spare air-casing (17) during installation and be enclosed within spray gun (15), (16) on, and make open slots (19) towards the below towards the substrate slice pallet.Fig. 4 is the shape figure of heating piece (9), and heating piece (9) is radial, and material is for being oxidation resistant molybdenum sheet, and the size of heating piece (9) can design in proportion according to the size of substrate slice pallet.
Embodiment
Further specify technical characterictic of the present invention below in conjunction with the ZnO film growth technique.
The growth technique process of ZnO film is as follows substantially:
1. be placed on the sample tray frame (22) of pretreatment chamber (102) after substrate slice (sapphire, Si, GaAs or ZnO etc.) etching being handled, the sample tray frame (22) that sample will be housed again is placed on the sample table (23), the vacuum system of opening sample pretreatment chamber (102) vacuumizes sample pretreatment chamber (102) by pretreatment chamber's aspirating hole (24), when vacuum tightness reaches 10
-1～10
-3During Pa, open plasma generator (25), sample is carried out plasma cleaned 5～10 minutes;
Substrate cleaned with the etching processing step be: toluene ultrasonic cleaning 3 minutes, acetone ultrasonic cleaning 3 minutes, the H of 160 ℃ of constant temperature is put in ethanol ultrasonic cleaning 3 minutes, and then circulation primary at last after 3 minutes with the deionized water ultrasonic cleaning
2SO
4: H
3PO
4Corrosion is 10 minutes in=3: 1 the mixed solution, rinses well with deionized water then, through high-purity N
2After doing, air-blowing sends into the pretreatment chamber of growing ZnO thin-film.
2. meanwhile, reaction chamber (101) vacuumizes with mechanical pump and molecular pump (20), and the base vacuum degree will be evacuated to higher vacuum 10
-3About Pa, improve the base vacuum degree of system, can improve the homogeneity of the growth quality and the film of sample; Then, that opens substrate sample pretreatment chamber (102) and reaction chamber is connected slide valve (27), under vacuum state, imports into substrate sample on the substrate slice pallet (10) of reaction chamber (101) from sample pretreatment chamber (102) with magnetic force driven rod (29); Draw back magnetic force driven rod (29), close connection slide valve (27);
3. heating piece (9) is switched on heated substrate tablet tray (10) and substrate, rotation substrate slice pallet (10), rotating speed can be regulated within 1000 rev/mins; High-purity N
2As the mixing chamber (14) of pilot-gas by secondary gas circuit (12), (13) feeding reactor top, evenly press down by high-density Stainless Steel Cloth (7) again, influence the air-flow upper reaches effect of film growth quality to eliminate substrate to heat the air-flow upper reaches that causes; Zn (the C that carries with Ar gas
2H
5)
2Be Zn source and O
2Spray to substrate, Zn (C by zinc source spray gun (15) and oxygen source spray gun (16) respectively
2H
5)
2And O
2On the substrate of high speed rotating and homogeneous heating, can merge reaction, on substrate, grow into ZnO film;
4. during the growing P-type ZnO film, carry out p type doping impurity, mainly be to carry out N to mix, and doped source has gas N
2, NH
3, N
2O etc., because these impurity gas resolutions are all very low, in order effectively N to be mixed among the ZnO, the present invention has added radio-frequency (RF) plasma reactor (18) in the mixing chamber of reactor top, doped source gas (N
2, NH
3, N
2O etc.) import by doped source gas circuit (11), by entering reaction chamber again after radio-frequency (RF) plasma reactor (18) ionization, mix after the ionization like this and can improve the ionization level of N, help the p type doping impurity of ZnO film, thereby a kind of approach of the p of growing type ZnO film is provided;
5. in order to improve the ZnO film quality, can anneal behind growth ending or stage by stage, annealing is to close behind the Zn source at logical O
2Situation under increase heating piece (9) electric current, improve that underlayer temperature carries out.
The typical growth condition of growing ZnO thin-film is on Sapphire Substrate:
The substrate kind: sapphire, 6H-SiC, Si, GaAs and GaN are several;
Substrate dimension: 1～4 inch;
Base vacuum degree: 10
-3Pa;
Temperature of reaction: 450～650 ℃;
Rotating speed: 400～600 rev/mins;
Chamber pressure during growth: 10～10
2Pa;
Reaction gas flow: Ar (Zn (C
2H
5)
2) 4～50sccm, O
2: 50～1000sccm, N
2: 600～3000sccm, impurity gas: 10～2000sccm;
(Zn (C
2H
5)
2) source bottle temperature :-5 ℃～10 ℃;
The speed of growth: 0.1～3 μ m/h;
Radio frequency power: 300～1000W;
Annealing temperature: 650～750 ℃;
Annealing time: 5～20 minutes
Technology with MOCVD equipment of the present invention and growing ZnO thin-film thereof, we grow the second best in quality ZnO film on sapphire, Si, GaAs and InP substrate, ZnO film thickness evenly and between hundreds of nanometer and several microns can accurately be controlled, prepared high quality high resistant ZnO film by annealing process, resistivity is own up to 10
5Ω cm uses NH
3Mix N and tentatively prepare p type ZnO film.
Be our some experimental datas below, only be used to effect of the present invention is described, rather than limitation of the invention.
We are 580 ℃ in the substrate temperature of reaction, pressure is that 480pa, substrate speed of rotation are 400rpm, reaction times to be that 20min, DEZn flow are 1.25 * 10 during the reaction chamber film growth
-4Mol/min, oxygen flow 6.0 * 10
-3On sapphire C face, carried out the increment study of ZnO film under the condition of mol/min.Utilize SIMENS D0005 X-ray diffractometer (Cu target, K α radiation, wavelength are 0.154nm) to analyze the ZnO film structures of samples and the crystallization situation of being grown.The Raman scattering test macro adopts RENISHAW-Ramanscope Raman spectrometer, Ar+ ion laser 514.5nm line is as light source, and light beam focuses on the vertical sample surfaces incident in back, collects back of the body astigmatism, ccd detector by water-cooled receives, and test pattern is a room temperature back scattering geometric configuration pattern.Sample photoluminescence spectrum (PL) records in room temperature, excitation light source is He-Cd laser apparatus (325nm, 20mw), the spot diameter that converges is about 1mm, the light fluorescence that the sample transition of electron produces arrives the grating window through plus lens, emission light is received through photomultiplier, by computer data acquisition by the grating monochromator beam split.
As shown in Figure 5, the ZnO film of growth is single c-axle oriented, has only (0002) diffraction peak, and peak position is in 2 θ=34.48 °, and its halfwidth (FWHM) is 0.184 °.According to the Scherr equation: D=k λ/β cos θ, wherein: D is an average grain size, and k is a constant, and β is the diffraction peak halfwidth, and θ is the diffraction peak peak position, can calculate: average grain size D=47.21nm.
As shown in Figure 6, because ZnO belongs to hexagonal system wurtzite structure crystal, the space point group is C
6V(p6
3Mc), comprise the atom of two chemical formulas in its primitive unit cell, so 12 vibrationals degrees of freedom are arranged.In that " symmetry of point lattice vibration is categorized as 2A
1+ 2B+2E
1+ 2E
2, one of them A
1+ E
1Be acoustic mode, the active optical mode of 2B right and wrong Raman, 2E
2Be the active nonpolar optical mode of Raman, another A
1+ E
1It is the active polarity optical mode of Raman.A
1The polarity optical mode is a nondegenerate, corresponding to the vibration of parallel Z axle; E
1The polarity optical mode is dual degeneracy, corresponding to the vibration of vertical Z axle.Under the back scattering geometric configuration, has only E
2(high) pattern and A
1(LO) pattern is that Raman is active, and they lay respectively at 437cm
-1And 579cm
-1The place.Can clearly observe in the drawings and be positioned at 435.32cm
-1E
2(high) pattern and be positioned at 575.32cm
-1A
1(LO) vibration modes illustrates that the ZnO film of growth has good wurtzite structure, especially E
2(high) appearance of pattern, it is corresponding to the wurtzite feature of ZnO crystal.Simultaneously, E
2(high) peak and A
1(LO) peak has 2cm approximately
-1Frequency displacement, this be since film in exist cause along the axial tension stress of a.In addition, A
1(LO) moving of peak position is also with the lattice imperfection V in the film
o, Z
NiFormation relevant, the same A of free carrier
1(LO) the strong coupling of pattern also can make A
1(LO) mode producing frequency displacement.Among Fig. 6, be positioned at 377.97cm
-1, 418.45cm
-1, 749.06cm
-1Raman peak be substrate Al
2O
3Scattering peak.Because the ZnO film of growth is thinner, about 420nm is less than the depth of penetration of Ar+ ion laser 514.5nm line, so the scattering peak of substrate is also high-visible.As shown in Figure 7, film surface is smooth, and uniform particles is fine and closely woven, shows that the film quality of growth is better.
We use HL5500PC Hall Effect Measurement System system, and to have tested growth temperature by the Hall method be 610 ℃, NH
3Airshed is respectively 50,80 and 110sccm, the electrical parameter of growth sample on sapphire R face substrate, and its test result is as shown in table 1.Known that by test result S50 presents weak p type conduction, hole has only 10
16Cm
-3, S80 is a high resistant n type conduction, resistivity is up to 10
8Ω cm.
Table 1: different N H
3The electrical parameter of airshed sample
Claims (8)
1, a kind of MOCVD equipment reaction chamber, by the base flange plate that has aspirating hole (8) (1), reaction chamber sidewall (2), turning axle (3), magnetic fluid bearing (4), motor (5), upper flange plate (6), Stainless Steel Cloth (7), heating piece (9), substrate slice pallet (10), gas circuit (11), secondary gas circuit (12) (13), mixing chamber (14) parts constitute, be characterised in that: gas circuit (11) is as the impurity source gas circuit of logical impurity source, a radio-frequency (RF) plasma reactor of interpolation (18) below the impurity source gas circuit (11) in mixing chamber (14) is inserted zinc source spray gun (15) and oxygen source spray gun (16) respectively in the sidewall both sides of reaction chamber.
2, MOCVD equipment reaction chamber as claimed in claim 1 is characterized in that: reaction chamber has added molecular pump (20).
3, MOCVD equipment reaction chamber as claimed in claim 1 or 2 is characterized in that: the distance of zinc source spray gun (15) and oxygen source spray gun (16) and substrate pallet is in 2 centimetres.
4, MOCVD equipment reaction chamber as claimed in claim 3, it is characterized in that: all add on zinc source spray gun (15) and the oxygen source spray gun (16) and be with even air-casing (17), shut on the spray gun top, spray gun evenly has 1～2 millimeter aperture every 3～5 millimeters vertically upward, towards substrate, the width of open slots (19) is 1～2 millimeter to the open slots (19) of even air-casing (17) towards the below.
5, MOCVD equipment reaction chamber as claimed in claim 1 or 2 is characterized in that: heating piece (9) is radial, and the material of heating piece (9) is oxidation resistant molybdenum sheet.
6, MOCVD equipment reaction chamber as claimed in claim 4 is characterized in that: heating piece (9) is radial, and the material of heating piece (9) is oxidation resistant molybdenum sheet.
7, MOCVD equipment reaction chamber as claimed in claim 1, it is characterized in that: added the substrate sample pretreatment chamber (102) that links with reaction chamber, constituted by the be connected slide valve (27), slide valve flange (28), magnetic force driven rod (29), magnetosheath (30), driven rod flange (31) parts of pretreatment chamber's outer wall (21), sample tray frame (22), sample table (23), pretreatment chamber's aspirating hole (24), plasma generator (25), plasma generator device flange (26), substrate sample pretreatment chamber and reaction chamber.
8, a kind of low pressure metal organic chemistry vapour phase deposition process growth technique of ZnO film comprises the steps:
1. be placed on the sample tray frame (22) of pretreatment chamber (102) after sapphire, Si, GaAs or ZnO substrate slice being cleaned, the sample tray frame (22) that sample will be housed again is placed on the sample table (23), the vacuum system of opening sample pretreatment chamber (102) vacuumizes sample pretreatment chamber (102) by pretreatment chamber's aspirating hole (24), when vacuum tightness reaches 10
-1～10
-3During Pa, open plasma generator (25), sample is carried out plasma cleaned 5～10 minutes;
2. meanwhile, reaction chamber (101) vacuumizes with mechanical pump and molecular pump (20), and the base vacuum degree will be evacuated to higher vacuum 10
-3Pa, then, that opens substrate sample pretreatment chamber (102) and reaction chamber is connected slide valve (27), under vacuum state, imports into substrate sample on the substrate slice pallet (10) of reaction chamber (101) from sample pretreatment chamber (102) with magnetic force driven rod (29); Draw back magnetic force driven rod (29), close connection slide valve (27);
3. heating piece (9) is switched on heated substrate tablet tray (10) and substrate, rotation substrate slice pallet (10), rotating speed can be regulated within 1000 rev/mins; High-purity N
2As the mixing chamber (14) of pilot-gas, evenly press down by high-density Stainless Steel Cloth (7) again by secondary gas circuit (12), (13) feeding reactor top; Zn (the C that carries with Ar gas
2H
5)
2Be Zn source and O
2Spray to substrate, Zn (C by zinc source spray gun (15) and oxygen source spray gun (16) respectively
2H
5)
2And O
2On the substrate of high speed rotating and homogeneous heating, can merge reaction, on substrate, grow into ZnO film;
4. during the growing P-type ZnO film, mainly be to carry out N to mix, doped source has gas N
2, NH
3Or N
2O, doped source gas enter reaction chamber after by radio-frequency (RF) plasma reactor (18) ionization again;
5. anneal stage by stage behind growth ending, annealing is to close behind the Zn source at logical O
2Situation under increase heating piece (9) electric current, improve that underlayer temperature carries out.
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|---|---|---|---|
| CNB2004100111640A CN1328410C (en) | 2004-10-19 | 2004-10-19 | Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof |
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|---|---|---|---|
| CNB2004100111640A CN1328410C (en) | 2004-10-19 | 2004-10-19 | Low-pressure metal organic chemical vapour phase depositing apparatus for zinc oxide and process thereof |
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| CN1328410C CN1328410C (en) | 2007-07-25 |
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