CN108588680A - Atomic layer deposition prepares Mo and adulterates Al2O3The method of high resistance film - Google Patents
Atomic layer deposition prepares Mo and adulterates Al2O3The method of high resistance film Download PDFInfo
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- CN108588680A CN108588680A CN201810489472.6A CN201810489472A CN108588680A CN 108588680 A CN108588680 A CN 108588680A CN 201810489472 A CN201810489472 A CN 201810489472A CN 108588680 A CN108588680 A CN 108588680A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
- C23C16/45527—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations
- C23C16/45529—Atomic layer deposition [ALD] characterized by the ALD cycle, e.g. different flows or temperatures during half-reactions, unusual pulsing sequence, use of precursor mixtures or auxiliary reactants or activations specially adapted for making a layer stack of alternating different compositions or gradient compositions
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/06—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material
- C23C16/08—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of metallic material from metal halides
- C23C16/14—Deposition of only one other metal element
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/403—Oxides of aluminium, magnesium or beryllium
Abstract
The present invention relates to a kind of atomic layer depositions to prepare Mo doping Al2O3The method of high resistance film, to solve the problem of that the prior art can not accurately control film thickness and doping ratio the existing defects especially in terms of the precision of control film thickness reaches atomic level and realizes large area homoepitaxial simultaneously.This approach includes the following steps：1) matrix is put within the deposition chamber；2) settling chamber is vacuumized and heats matrix；3) 8~11 Al are carried out2O3Deposition cycle, single Al2O3Deposition includes：3.1) sources precursor A l are passed through to settling chamber, the sources Al purge settling chamber in the time of settling chamber's exposure setting；3.2) it is passed through presoma oxygen source, obtains single layer Al2O3；3.3) settling chamber is purged；4) 1 Mo deposition is carried out；4.1) sources presoma Mo are passed through to settling chamber, purge settling chamber；4.2) it is passed through reducing agent, obtains single layer Mo metal simple-substances；4.3) settling chamber is purged；5) step 3) and step 4) are repeated in repeatedly, obtains Mo doping Al2O3High resistance film.
Description
Technical field
The present invention relates to the preparation methods of field of photovoltaic materials high resistance film, and in particular to a kind of atomic layer deposition preparation Mo
Adulterate Al2O3The method of high resistance film.
Background technology
Since the 1980s, thin film technique and thin-film material are quickly grown, academic and engineer application field all
Achieve great successes, it has also become current material science one of research field the most active.For a long time, conductive film
Research hotspot focuses on low-resistance film, especially using the AZO films of Al doping ZnO (Al-Doped ZnO) as representative, electrically conducting transparent
The characteristic research of film and preparation method have become research hotspot instantly, and the research of high resistance film is then rarely reported.Although
By adjusting Zn/Al ratios, AZO films can also be prepared into high resistance film, but this AZO films are in high-temperature work environment or high
After temperature baking or annealing, stability is poor, and change in resistance reaches several magnitudes, and practicability is extremely restricted.
Traditional method for manufacturing thin film is mainly two kinds of physical vapour deposition (PVD) (PVD) and chemical vapor deposition (CVD).PVD
With higher deposition rate, but it is poor around plating property, is usually used in the film preparation of flat sample surfaces, for groove and hole
The sample of structure, especially in the hole of the groove of high-aspect-ratio and big L/D ratio, PVD is difficult the film of depositing homogeneous；CVD
The film of preparation has certain shape-retaining ability, can in the groove of smaller depth-to-width ratio deposition film, but there are more holes for film layer
Hole and defect.In addition, two methods of PVD and CVD, can not all be accurately controlled film thickness and doping ratio, especially
It is the existing defects in terms of the precision of control film thickness reaches atomic level and realizes large area homoepitaxial simultaneously.
Invention content
Present invention aim to address the deficiencies present in existing method for manufacturing thin film, and to film thickness and can not mix
Miscellaneous ratio is accurately controlled, and especially the precision in control film thickness reaches atomic level and realizes that large area is uniform simultaneously
In terms of growth the problem of existing defects, a kind of technique for atomic layer deposition preparation Mo doping Al is provided2O3The method of high resistance film,
The adhesive force that is prepared is strong, surfacing, thickness are uniform, resistivity up to 105-1011Ω cm, and thermal stability
It is good.
Technical proposal that the invention solves the above-mentioned problems is,
A kind of atomic layer deposition preparation Mo doping Al2O3The method of high resistance film, includes the following steps：
1) matrix is put within the deposition chamber；
2) settling chamber is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 120~350 DEG C；
3) 8~11 Al are carried out2O3Deposition cycle；
Single Al2O3Deposition includes step 3.1) to step 3.3),
3.1) sources precursor A l are passed through to settling chamber, the sources Al purge settling chamber in the time of settling chamber's exposure setting, will be more
Remaining presoma purging is clean；
3.2) it is passed through presoma oxygen source, oxygen source obtains list in the time of settling chamber's exposure setting by Chemisorption
Layer Al2O3；
3.3) settling chamber is purged, extra presoma and by-product are purged clean；
4) 1 Mo deposition is carried out；
4.1) sources presoma Mo are passed through to settling chamber, the sources Mo purge settling chamber in the time of settling chamber's exposure setting, will be more
Remaining presoma purging is clean；
4.2) it is passed through reducing agent, single layer Mo metal simple-substances are obtained by Chemisorption；
4.3) settling chamber is purged, extra presoma and by-product are purged clean；
5) it is repeated in step 3) and step 4) repeatedly, after cooling obtains Mo doping Al2O3High resistance film.
Further, in step 5), step 3) and step 4) 500~650 times are repeated.
Further, the purge gas in step 3) and step 4) is nitrogen or argon gas.
Further, in step 3), exposure duration and purge time of the presoma in settling chamber are：The sources Al, purge gass
Body, oxygen source, purge gas=0.1s, 3s, 0.1s, 3s.
Further, in step 4), exposure duration and purge time of the presoma in settling chamber are：The sources Mo, purge gass
Body, reducing agent, purge gas=0.5s, 5s, 0.5s, 5s.
Further, the matrix in step 1) is glass, silicon chip, ceramics, plastics or has superelevation aspect ratio trench, greatly enhances
Material of the diameter than microwell array.
Further, the sources Al in step 3) are trimethyl aluminium, dimethyl aluminium or aluminium chloride.
Further, the oxygen source in step 3) is gaseous state deionized water, ozone or hydrogen peroxide.
Further, the sources Mo in step 4) are molybdenum hexafluoride.
Further, the reducing agent in step 4) is disilane or silane.
Beneficial effects of the present invention are：
1. the present invention adulterates Al using Mo prepared by technique for atomic layer deposition2O3Film, surface roughness are less than 1nm, and thin
Film thickness uniformly, surfacing, compact structure, strong adhesive force.This have the advantage that partial circulating can be accurately controlled
Doping ratio, systemic circulation can be accurately controlled film thickness, partial circulating and systemic circulation combination, so that it may to accurately control film
Resistivity.And tradition PCD and CVD method can not so be accurately controlled film thickness and doping ratio, accordingly
Also the resistivity of film can not just be accurately controlled.
2. the method for the present invention preparation process is simple, deposition process is controllable, by controlling Mo doping ratios and systemic circulation number,
It can be 105~1011Accuracy controlling film resiativity within the scope of Ω cm.
3. the present invention adulterates Al using Mo prepared by technique for atomic layer deposition2O3Film, under high-temperature work environment or high temperature
After annealing, resistivity is held essentially constant, and film thermostabilization is very excellent.Such high resistance film is in Memister, photoconduction
Type detector, microchannel plate, photoelectric display device, solar cell, antistatic, anti-microwave radiation, electrochromism function element
Equal fields have a wide range of applications.
Description of the drawings
Fig. 1 is that atomic layer deposition of the present invention prepares Mo doping Al2O3Film flow chart；
Fig. 2 is that atomic layer deposition of the present invention prepares Mo doping Al2O3Thin film precursor pulse sequence figure；
Fig. 3 is that atomic layer deposition of the present invention prepares Mo doping Al2O3Membrane structure schematic diagram；
Fig. 4 is Mo doping ratios of the present invention and its corresponding film resiativity schematic diagram.
Specific implementation mode
Present disclosure is described in further detail below in conjunction with specific embodiment：
Mo, which is prepared, the present invention provides a kind of atomic layer deposition of field of photovoltaic materials adulterates Al2O3The method of high resistance film.
Atomic layer deposition is a kind of special chemical vapor deposition method, is by the way that vaporous precursors pulse is alternately passed through reative cell
And chemisorption and react and formed a kind of method of film on depositing base.Film prepared by atomic layer deposition has conformal
Property it is good, large-area uniformity is high, step coverage is high, thickness can be controlled in atomic level the advantages that, both can be flat in large area
Face matrix surface, can also be in complicated nanoscale matrix surface (the porous material of such as superelevation aspect ratio trench or complicated bend
Material) on carry out film growth, most potential film growth techniques are increasingly becoming, in microelectronics, optical thin film, nanometer material
The fields such as material, the energy, catalysis have a wide range of applications potentiality.
As shown in Figures 1 to 4, the present invention utilizes technique for atomic layer deposition, alternately presoma is passed through to settling chamber, in settling chamber
Al is carried out on interior substrate, substrate or substrate material2O3With Mo alternating deposits, Mo doping Al is obtained2O3The adjustable high resistant of resistivity
Film.High resistance film thickness that the method for the present invention is prepared is uniform, surface is smooth, compactness is good, thermal stability is good, resistivity
It can be 105-1011It is accurately adjusted between Ω cm.
The settling chamber of the present invention refers to：The settling chamber of atomic layer deposition apparatus.
Al2O3Deposition refers to：It is passed through trimethyl aluminium to settling chamber, then settling chamber is purged with high pure nitrogen, before extra
It is clean to drive body purging, then is passed through gaseous state deionized water, single layer Al is obtained by Chemisorption2O3, finally use High Purity Nitrogen air-blowing
Settling chamber is swept, extra presoma and by-product are purged clean.Exposure duration and high pure nitrogen of the presoma in settling chamber
Purge time is：TMA/N2/H2O/N2=0.1s/3s/0.1s/3s, the present invention use this longer exposure duration, can be complete
It is sufficiently carried out adsorption reaction.
Mo is deposited：It is passed through molybdenum hexafluoride (MoF to settling chamber6), settling chamber then is purged with high pure nitrogen, it will be extra
Presoma purging it is clean, then be passed through disilane (Si2H6) or silane (Si2H4), single layer Mo gold is obtained by Chemisorption
Belong to simple substance, finally purge settling chamber with high pure nitrogen, extra presoma and by-product is purged clean.Presoma is in settling chamber
Exposure duration and the purge time of high pure nitrogen be：MoF6/N2/Si2H6(Si2H4)/N2=0.5s/5s/0.5s/5s, this hair
It is bright to use this longer exposure duration, it can cmpletely carry out adsorption reaction.
Mo adulterates Al2O3Refer to：Carrying out multiple Al2O3After deposition cycle, a Mo deposition cycle is carried out, in this, as
One systemic circulation, i.e., according to (100-X) % (TMA-H2O)-X% (Si2H6/Si2H4-MoF6) order controls the doping ratio of Mo
Example (X represents 0~100, the as ratio of Mo, this ratio is controlled by cycle-index), then systemic circulation number is controlled, it is controlled with this
Made membrane thickness.
The doping ratio of Mo is 8%~11% in the present invention, that is, carries out 8~11 Al2O3After deposition cycle, 1 Mo is carried out
Deposition, in this, as a systemic circulation, systemic circulation carries out 500~650 times, obtains the Mo doping Al of 60~120nm of thickness2O3It is high
Hinder film.
The present invention carries out 8~11 Al2O3Deposition cycle and 1 Mo deposition, it is therefore an objective to control the ratio of Mo doping；Such as 8 times
Al2O3Ratio with 1 Mo, Mo is 11%；Similarly, 9 Al2O3Ratio with 1 Mo, Mo is 10%；10 Al2O3With 1 time
The ratio of Mo, Mo are 9%；11 Al2O3Ratio with 1 Mo, Mo is 8%；Coordinate 500~650 systemic circulations control film thick
Degree can obtain Mo doping Al in 60~120nm2O3The resistivity of film mutually should be 109、108、107、106Ω cm magnitudes, i.e.,
High resistance film can be obtained, this have the advantage that partial circulating can be accurately controlled doping ratio, systemic circulation can be accurate
Control film thickness, partial circulating and systemic circulation combination, so that it may to accurately control the resistivity of film.
The present invention uses high pure nitrogen N2Or argon Ar, as carrier gas and purge gas, nitrogen and argon gas are inert gases,
It will not react with deposited film, different presoma pulses can not only be isolated with inert gas purge, prevent presoma
Gas phase reaction occurs in settling chamber, while having the function of purifying settling chamber, excessive precursor species, anti-can also be taken out of
Answer by-product.
The vacuum step of the method for the present invention is to improve film to be discharged the foreign gas in cavity, prevent from polluting
Purity requirement.Matrix is heated, is in order to which presoma is more preferably adsorbed onto matrix surface.
As shown in Figure 1, the atomic layer deposition of the present invention, which prepares Mo, adulterates Al2O3The method of high resistance film specifically includes following
Step：
1) matrix is put within the deposition chamber；Matrix is for the plane of material or to have with glass, silicon chip, ceramics, plastics etc.
The groove of superelevation depth-to-width ratio, microwell array of big L/D ratio etc.；
2) settling chamber is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 120~350 DEG C, preferable temperature is
200℃；
3) 8~11 Al are carried out2O3Deposition cycle；
Single Al2O3Deposition includes step 3.1) to step 3.3),
3.1) sources precursor A l are passed through to settling chamber, the sources Al utilize High Purity Nitrogen air-blowing in the time of settling chamber's exposure setting
Settling chamber is swept, extra presoma is purged clean；The sources Al can be trimethyl aluminium (TMA), dimethyl aluminium Al (CH3)2Cl or chlorination
Aluminium (AlCl3)；
3.2) it is passed through presoma oxygen source, oxygen source obtains list in the time of settling chamber's exposure setting by Chemisorption
Layer Al2O3, oxygen source can be gaseous state deionized water, ozone or hydrogen peroxide；
3.3) it utilizes high pure nitrogen to purge settling chamber, extra presoma is purged clean；Presoma is in settling chamber
The purge time of exposure duration and high pure nitrogen is：The sources Al/N2/ oxygen source/N2=0.1s/3s/0.1s/3s；
4) 1 Mo deposition is carried out；
4.1) sources presoma Mo are passed through to settling chamber, the sources Mo utilize High Purity Nitrogen air-blowing in the time of settling chamber's exposure setting
Settling chamber is swept, extra presoma and by-product are purged totally, the sources Mo can be molybdenum hexafluoride (MoF6)；
4.2) it is passed through reducing agent, single layer Mo metal simple-substances are obtained by Chemisorption, reducing agent can be disilane
(Si2H6) or silane (Si2H4)；
4.3) it utilizes high pure nitrogen to purge settling chamber, extra presoma and by-product is purged clean；Presoma is heavy
Exposure duration and the purge time of high pure nitrogen in product room be：The sources Mo/N2/ reducing agent/N2=0.5s/5s/0.5s/5s；
5) step 3) and step 4) are repeated in repeatedly, concretely 500~650 times, Mo doping Al is obtained after cooling2O3
High resistance film.
Embodiment one
Matrix is packed into atomic layer deposition room, is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 200 DEG C, it opens
Begin to carry out Al2O3Deposition, i.e. TMA/N2/H2O/N2=(0.1s/3s/0.1s/3s) after recycling 11 times, carries out 1 Mo deposition, i.e.,
MoF6/N2/Si2H6(Si2H4)/N2=(0.5s/5s/0.5s/5s), 11 Al2O3Deposition cycle and 1 Mo deposition are 1 big
Cycle, systemic circulation stop deposition after carrying out 500 times, and room temperature to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Mo
Adulterate Al2O3The matrix of film.
Embodiment two
Matrix is packed into atomic layer deposition room, is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 200 DEG C, it opens
Begin to carry out Al2O3Deposition, i.e. TMA/N2/H2O/N2=(0.1s/3s/0.1s/3s) after recycling 10 times, carries out 1 Mo deposition, i.e.,
MOF6/N2/Si2H6(Si2H4)/N2=(0.5s/5s/0.5s/5s), 10 Al2O3 deposition cycles and 1 Mo deposition are 1 big
Cycle, systemic circulation stop deposition after carrying out 550 times, and room temperature to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Mo
Adulterate Al2O3The matrix of film.
Embodiment three
Matrix is packed into atomic layer deposition room, is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 200 DEG C, it opens
Begin to carry out Al2O3Deposition, i.e. TMA/N2/H2O/N2=(0.1s/3s/0.1s/3s) after recycling 9 times, carries out 1 Mo deposition, i.e.,
MOF6/N2/Si2H6(Si2H4)/N2=(0.5s/5s/0.5s/5s), 9 Al2O3Deposition cycle and 1 Mo deposition are 1 big
Cycle, systemic circulation stop deposition after carrying out 600 times, and room temperature to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Mo
Adulterate Al2O3The matrix of film.
Example IV
Matrix is packed into atomic layer deposition room, is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 200 DEG C, it opens
Begin to carry out Al2O3Deposition, i.e. TMA/N2/H2O/N2=(0.1s/3s/0.1s/3s) after recycling 8 times, carries out 1 Mo deposition, i.e.,
MOF6/N2/Si2H6(Si2H4)/N2=(0.5s/5s/0.5s/5s), 8 Al2O3Deposition cycle and 1 Mo deposition are 1 big
Cycle, systemic circulation stop deposition after carrying out 650 times, and room temperature to be deposited is cooled to room temperature, and open settling chamber, and taking-up deposited Mo
Adulterate Al2O3The matrix of film.
On HALL8800 Hall effect testers to room temperature under and by 300~450 DEG C annealing after Mo adulterate Al2O3
Film carries out electric property evaluation.The Mo that table 1 is embodiment 1-4 adulterates Al2O3Film at normal temperatures with 400 DEG C annealing after electricity
Resistance rate.
The Mo of 1 embodiment 1-4 of table adulterates Al2O3Film at normal temperatures with 400 DEG C annealing after resistivity.
It can be obtained from above-described embodiment：Al is adulterated using Mo prepared by technique for atomic layer deposition2O3Film is adulterated in Mo
Ratio is in 8%~11% range, and when film thickness is 60~120nm, film resiativity can be controlled in 105-1011Ω cm models
In enclosing, and after 300~450 DEG C of high annealings, film resiativity variation is less than an order of magnitude, and film heat stability is excellent
It is different.
Claims (10)
1. a kind of atomic layer deposition prepares Mo and adulterates Al2O3The method of high resistance film, which is characterized in that include the following steps：
1) matrix is put within the deposition chamber；
2) settling chamber is evacuated to 10-2Pa~10-5Pa, and matrix is heated to 120~350 DEG C；
3) 8~11 Al are carried out2O3Deposition cycle；
Single Al2O3Deposition includes step 3.1) to step 3.3),
3.1) sources precursor A l are passed through to settling chamber, the sources Al purge settling chamber in the time of settling chamber's exposure setting, will be extra
Presoma purging is clean；
3.2) it is passed through presoma oxygen source, oxygen source obtains single layer in the time of settling chamber's exposure setting by Chemisorption
Al2O3；
3.3) settling chamber is purged, extra presoma and by-product are purged clean；
4) 1 Mo deposition is carried out；
4.1) sources presoma Mo are passed through to settling chamber, the sources Mo purge settling chamber in the time of settling chamber's exposure setting, will be extra
Presoma purging is clean；
4.2) it is passed through reducing agent, single layer Mo metal simple-substances are obtained by Chemisorption；
4.3) settling chamber is purged, extra presoma and by-product are purged clean；
5) it is repeated in step 3) and step 4) repeatedly, after cooling obtains Mo doping Al2O3High resistance film.
2. atomic layer deposition according to claim 1 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 5) in, repeat step 3) and step 4) 500~650 times.
3. atomic layer deposition according to claim 2 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
Rapid purge gas 3) and in step 4) is nitrogen or argon gas.
4. atomic layer deposition according to claim 3 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 3) in, exposure duration and purge time of the presoma in settling chamber be：The sources Al, purge gas, oxygen source, purge gas=
0.1s、3s、0.1s、3s。
5. atomic layer deposition according to claim 4 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 4) in, exposure duration and purge time of the presoma in settling chamber be：The sources Mo, purge gas, reducing agent, purge gas=
0.5s、5s、0.5s、5s。
6. atomic layer deposition according to any one of claims 1 to 5 prepares Mo and adulterates Al2O3The method of high resistance film, feature
It is：Matrix in step 1) is glass, silicon chip, ceramics, plastics or has superelevation aspect ratio trench, big L/D ratio microwell array
Material.
7. atomic layer deposition according to claim 6 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 3) in the sources Al be trimethyl aluminium, dimethyl aluminium or aluminium chloride.
8. atomic layer deposition according to claim 7 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 3) in oxygen source be gaseous state deionized water, ozone or hydrogen peroxide.
9. atomic layer deposition according to claim 8 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：Step
It is rapid 4) in the sources Mo be molybdenum hexafluoride.
10. atomic layer deposition according to claim 9 prepares Mo and adulterates Al2O3The method of high resistance film, it is characterised in that：
Reducing agent in step 4) is disilane or silane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109680261A (en) * | 2019-01-24 | 2019-04-26 | 中国科学院西安光学精密机械研究所 | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film |
| CN111172511A (en) * | 2020-01-17 | 2020-05-19 | 胜科纳米（苏州）有限公司 | Method for preparing metal film layer on surface of organic material |
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| CN109680261A (en) * | 2019-01-24 | 2019-04-26 | 中国科学院西安光学精密机械研究所 | Microchannel plate and microchannel plate inner wall preparation Cu adulterate Al2O3The method of high resistance film |
| CN111172511A (en) * | 2020-01-17 | 2020-05-19 | 胜科纳米（苏州）有限公司 | Method for preparing metal film layer on surface of organic material |
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