CN110527981A - A kind of atomic layer deposition apparatus and method - Google Patents
A kind of atomic layer deposition apparatus and method Download PDFInfo
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- CN110527981A CN110527981A CN201810873257.6A CN201810873257A CN110527981A CN 110527981 A CN110527981 A CN 110527981A CN 201810873257 A CN201810873257 A CN 201810873257A CN 110527981 A CN110527981 A CN 110527981A
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- presoma
- solvent
- operated valve
- transfer conduit
- reaction chamber
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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
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4408—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber by purging residual gases from the reaction chamber or gas lines
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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
- C23C16/448—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 generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
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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
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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]
- C23C16/45544—Atomic layer deposition [ALD] characterized by the apparatus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Chemical Kinetics & Catalysis (AREA)
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- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a kind of atomic layer deposition apparatus and methods.The equipment includes reaction chamber, solvent flush system and multiple precursor delivery systems, wherein, each precursor delivery system includes presoma transfer conduit and the precursor source bottle that connect with presoma transfer conduit on-off, and a plurality of presoma transfer conduit imports reaction chamber jointly；Solvent flush system includes solvent delivery pipeline and the solvent source bottle that connect with solvent delivery pipeline on-off, solvent delivery pipeline is selectively connected to at least one presoma transfer conduit, is purged with being passed through purging solvent to presoma transfer conduit and/or reaction chamber.The present invention can reduce the indoor unexpected reactant deposition of chamber, improve film purity, improve the quality of deposition film；Film gauge uniformity can be improved, improve the repeatability of film performance between piece；And the particulate matter attachment that can reduce chamber inner wall, to improve the purity of deposition film.
Description
Technical field
The present invention relates to semiconductor integrated circuit manufacturing fields, and in particular, to a kind of atomic layer deposition apparatus and method.
Background technique
Zirconium oxide (ZrO2) is good oxygen ion conductor, can be used for the solid electrode on such as fuel cell.And
And ZrO2 can be used in high-k (high dielectric constant) dielectric layer on integrated circuit due to high dielectric constant.
The ZrO2 of atomic layer deposition (Atomic layer deposition, ALD) method deposition is with ZAZ (ZrO2-
Al2O3-ZrO2) multilayered structure form has been used to dynamic random access memory (Dynamic Random Access
Memory, DRAM) capacitor on.Film deposition in, especially ALD deposition when, the crystalline size of ZrO2 can pass through ZrO2
It is laminated with other unformed layers such as aluminium oxide (Al2O3) and blocks grain growth, to control its physical size.
ALD reaction for the presoma of low-steam pressure, the repeatability for improving film performance between uniformity of film and piece are
One larger challenge of process optimization, the reason is that, for the deposition of ZrO2, no matter using the halide of zirconium or the alkoxide of zirconium
Equal organometallic precursors, common feature is all that steam forces down under room temperature, and source bottle heating temperature and vapour pressure are difficult to control, and
And it is easy to produce particle.
In the prior art, as shown in Figure 1 as the process steps of the ALD deposition ZrO2 of presoma using TEMAZ.The
One step, carrier gas such as inert gas N2 carry presoma TEMAZ steam and enter in chamber and adsorb on substrate；Second step uses
Inert gas purge presoma TEMAZ pipeline and chamber, i.e. inert gas reach chamber；Third step, carrier gas carry oxide H2O
Steam reacted to chamber and with saturation absorption presoma TEMAZ on substrate；4th step, is aoxidized using inert gas purge
Object H2O pipeline.Above four steps are repeated until reaching expected thickness.
Existing ALD reaction system has the disadvantage in that
1, gas circuit and blind short, the measurement branch of block etc. are all the position that source steam flow rate is even stagnated slowly, source steam residual
It can condense to form particle, common purging is difficult to thoroughly remove, and agglomeration is easily corroded after accumulation；
2, during ALD reacts to form ZrO2, it is shorter that presoma TEMAZ enters the purge time after chamber, more
The serious is TEMAZ intrinsic viscosity is larger, common purging is difficult that remaining presoma is fully erased.Remain in transfer conduit,
Presoma residual in the spaces such as gas distributing device, chamber inner wall is adsorbed, and unexpected ALD reaction, generation occurs
Grain object pollution chamber and film；
3, in technical process, the TEMAZ presoma of some concentrations may be desorbed and move to substrate local surfaces,
Parasitic growth occurs with H2O, therefore thicker in these regions generation film, film quality is poor, and influences entire film thickness
Uniformity；
4, the uncontrollable parasitic growth of chamber interior not only impacts the thickness uniformity, but also is degrading chamber
Process environments, directly affecting is exactly the degradations such as film gauge uniformity that same ALD technique is formed with time change,
Repeatability decline between piece.
Fig. 2 a is the ZrO2 film thickness profile shape formed at chamber deposition initial stage, and Fig. 2 b is chamber through after a period of time
The ZrO2 film thickness profile shape that (ZrO2 that period about deposited 50nm) is formed afterwards.Table 1 is the detailed of two kinds of film thicknesses
Details condition.On the whole, chamber deposition initial film the thickness uniformity is good, same on piece maximum thickness and minimum value gap compared with
It is small.But with the increase of sedimentation time, after depositing a period of time, film gauge uniformity is reduced, and on piece thickness disparity is obvious
Increase.On thickness distribution figure, fringe region thinner thickness.The reason for causing edge thickness relatively thin is more, for example, presoma
TEMAZ lacks when deposition in the concentration of chamber inner wall in edge presoma, absorption unsaturation etc..Also there is gas in thickness distribution
The planform of body distributor, this causes presoma absorption related to gas distributing device structure.
Table 1
The information for being disclosed in background of invention part is merely intended to deepen the reason to general background technique of the invention
Solution, and it is known to those skilled in the art existing to be not construed as recognizing or imply that the information is constituted in any form
Technology.
Summary of the invention
In order to overcome problem above existing in the prior art, the invention proposes a kind of atomic layer deposition apparatus and sides
Method, by the improvement to atomic layer deposition apparatus and technique, reduce to the maximum extent the presoma of low-steam pressure in pipeline and
The indoor residual of chamber, thus reduce transfer conduit chamber inner wall occur absorption and desorption and other unexpected reactions can
Energy；By increasing the formation of passivation layer, the depositional environment of deposition later period chamber is improved, so as to improve the thickness of deposition film
Uniformity and process repeatability.
According to an aspect of the invention, it is proposed that a kind of atomic layer deposition apparatus.The equipment includes reaction chamber, solvent punching
Brush system and multiple precursor delivery systems, wherein
Each precursor delivery system includes presoma transfer conduit and can lead to the presoma transfer conduit
The precursor source bottle of disconnected property connection, a plurality of presoma transfer conduit import the reaction chamber jointly；
The solvent flush system includes solvent delivery pipeline and connect with the solvent delivery pipeline on-off molten
Agent source bottle, the solvent delivery pipeline at least one presoma transfer conduit is selective is connected to, with to the presoma
Transfer conduit and/or the reaction chamber are passed through purging solvent and are purged.
Preferably, the solvent flush system further includes the solvent recovery unit being connected and solvent purification device, wherein
The solvent recovery unit includes the first solvent recovery unit and the second solvent recovery unit, a plurality of presoma
Transfer conduit is connect by importing pipeline with the first solvent recovery unit on-off, the reaction chamber and described second
The connection of solvent recovery unit on-off.
Preferably, the equipment further includes vacuum pump, and the vacuum pump is via wherein the one of butterfly valve and the reaction chamber
A outlet end connection, the spool of the butterfly valve are in permanent angle mode.
Preferably, in each precursor delivery system, the precursor source bottle pass through the first valve module realize with
The on-off of the presoma transfer conduit connects, wherein
First valve module includes three pneumatic operated valves and three hand-operated valves, and the setting of the first pneumatic operated valve is passed in the presoma
On defeated pipeline；
The arrival end and the presoma of first pneumatic operated valve are set after the second pneumatic operated valve and the series connection of the second hand-operated valve
Between the arrival end of source bottle；
Third pneumatic operated valve and third hand-operated valve series connection after be arranged in first pneumatic operated valve outlet end and the presoma
Between the outlet end of source bottle；
One end of first manual valve is connected between second pneumatic operated valve and second hand-operated valve, and the other end is connected to
Between the third pneumatic operated valve and the third hand-operated valve.
Preferably, the solvent source bottle is realized by the second valve module and is connected with the on-off of the solvent delivery pipeline
It connects, wherein
Second valve module includes three pneumatic operated valves and two hand-operated valves, after the 4th pneumatic operated valve and the 4th hand-operated valve are connected
It is connected to the arrival end of the solvent source bottle, is connected to going out for the solvent source bottle after the 5th pneumatic operated valve and the series connection of the 5th hand-operated valve
Mouth end；
One end of 6th pneumatic operated valve is connected between the 4th pneumatic operated valve and the 4th hand-operated valve, and the other end is connected to
Between 5th pneumatic operated valve and the 5th hand-operated valve.
Preferably, the atomic layer deposition apparatus further includes additional gas transfer conduit, the reaction chamber another
Outlet end is provided with control valve, the outlet of the control valve and the additional transmitted piping connection, in the additional transmitted pipeline
Inlet be provided with mass flow controller.
Preferably, heating device is provided in the solvent delivery pipeline and the presoma transfer conduit.
According to another aspect of the invention, it is proposed that a kind of Atomic layer deposition method.It the described method comprises the following steps:
Step 1, inert gas carry after the first presoma enters the reaction chamber of atomic layer deposition apparatus and are adsorbed on substrate
Surface；
Step 2, inert gas purge the first forerunner transfer conduit；
Step 3, inert gas carry before the second presoma enters after the reaction chamber with the first of the substrate surface
Precursor reactant is driven, to form default film over the substrate；
Second presoma transfer conduit described in step 4, inert gas purge；
Step 5 judges whether the film performance of any a piece of substrate and the default film on adjacent a piece of substrate is deteriorated, such as
It is no, then the step 1 is repeated to the step 4 more times；If so, then executing following step 6；
Step 6, inert gas carry solvent vapo(u)r and purge the first presoma transfer conduit and/or second forerunner
Body transfer conduit and/or the reaction chamber.
Preferably, the method also includes following step；
Step 7, inert gas carry after third presoma enters the reaction chamber and are adsorbed on the reaction chamber inner wall
With the baffle surface on the substrate；
Step 8, inert gas purge third forerunner's transfer conduit；
Step 9, inert gas carry the 4th presoma enter the reaction chamber after with third forerunner's precursor reactant, with formed
Passivation layer；
Step 10, the 4th forerunner's transfer conduit of inert gas purge.
Preferably, first presoma and the third presoma are presoma not of the same race, second presoma with
4th presoma is presoma mutually of the same race.
Preferably, the default film is ZrO2 film, and the passivation layer is Al2O3 passivation layer.
The present invention has following advantageous effects:
It is forced down for precursor vapor, the feature that property is sticky, purges presoma pipeline and chamber by washing away solvent,
Residual of the presoma in transfer conduit is effectively removed, reduces presoma in the low local location of chamber inner wall especially temperature
Absorption improves film purity, improves the quality of deposition film so as to reduce the indoor unexpected reactant deposition of chamber；
It reacts to form chamber passivation layer by ALD, is covered in chamber and the forerunner removed is failed by solvent purging on a small quantity
Body absorption, is farthest restored to desired process conditions for chamber, to improve film gauge uniformity, improves film between piece
The repeatability of energy；And the particulate matter attachment that can reduce chamber inner wall, to improve the purity of deposition film.
Method of the invention has other characteristics and advantages, these characteristics and advantages from the attached drawing being incorporated herein and with
Will be apparent in specific embodiment afterwards, or by the attached drawing and subsequent specific embodiment being incorporated herein into
Row statement, these the drawings and specific embodiments in detail are used together to explain specific principle of the invention.
Detailed description of the invention
Exemplary embodiment of the present is described in more detail in conjunction with the accompanying drawings, of the invention is above-mentioned and other
Purpose, feature and advantage will be apparent, wherein in exemplary embodiments of the present invention, identical reference label is usual
Represent same parts.
Fig. 1 shows the flow chart of atom layer deposition process in the prior art；
Fig. 2 a and Fig. 2 b are the film thickness profiles after deposition initial stage and deposition a period of time；
Fig. 3 shows the structure chart of atomic layer deposition apparatus in accordance with an exemplary embodiment of the invention；
Fig. 4 shows the flow chart of Atomic layer deposition method in accordance with an exemplary embodiment of the invention.
Main appended drawing reference explanation:
1 reaction chamber, 2 gas evenly mixing devices, 3 substrates, 4 pedestals, 5 vacuum pumps, 6 butterfly valves, 7 carrier gas, 10 chamber injection ends,
20 chamber output ends, 11,12 precursor source bottles, 13 solvent source bottles, 14 solvent recovery units, 15,16,17,18 mass flow controls
Device processed, 21,22 presoma transfer conduits, 23 solvent delivery pipelines, 24 inert gas delivery tube roads, 25 first presomas transmission branch
Road, 26 second presoma transmission branches, 27 first inert gas delivery branches, 28 second inert gas delivery branches, 29 is additional
Gas transport pipeline, 101-109 control valve, 111,114 first pneumatic operated valves, 112,115 second pneumatic operated valves, 113,116 third gas
Dynamic valve, 117 the 4th pneumatic operated valves, 118 the 5th pneumatic operated valves, 119 the 6th pneumatic operated valves, 121,124 first manual valves, 122,125 second
Hand-operated valve, 123,126 third hand-operated valves, 127 the 4th hand-operated valves, the 128, the 5th hand-operated valve, 141 first solvent recovery units, 142
Second solvent recovery unit.
Specific embodiment
The present invention will be described in more detail below with reference to accompanying drawings.Although showing the preferred embodiment of the present invention in attached drawing,
However, it is to be appreciated that may be realized in various forms the present invention and should not be limited by the embodiments set forth herein.On the contrary, providing
These embodiments are and the scope of the present disclosure completely can be communicated to ability to keep the disclosure more thorough and complete
The technical staff in domain.
Fig. 3 shows the structure chart of atomic layer deposition apparatus in accordance with an exemplary embodiment of the invention.The equipment is main
It include: reaction chamber, solvent flush system and multiple precursor delivery systems.For simplicity, Fig. 3 only shows two of them
Precursor delivery system, other precursor delivery systems are not shown, and structure is similar to shown system.
As shown in figure 3, reaction chamber 1 includes that the gas evenly mixing device (showerhead) 2 that top is arranged in and setting exist
The pedestal 4 of bottom is arranged on pedestal 4, and substrate (wafer) 3, forerunner's precursor reactant is formed by film and is deposited on substrate 3.
Purpose using gas evenly mixing device 2 is that presoma is enable to be uniformly distributed on substrate 3, i.e. can if it is mixed gas
It is enough to be uniformly mixed.7 be the carrier gas for carrying presoma and entering reaction chamber and carrying out pipeline and chamber purging, and it typically is inertia
Gas, for example, argon gas, helium, nitrogen etc..
In atomic layer deposition apparatus according to the present invention, each precursor delivery system includes presoma transfer conduit
The precursor source bottle connecting with the presoma transfer conduit on-off, a plurality of presoma transfer conduit import described anti-jointly
Answer chamber；
Solvent flush system includes solvent delivery pipeline and the solvent source bottle that connect with the solvent delivery pipeline on-off,
The solvent delivery pipeline is selectively connected to at least one presoma transfer conduit, with to the presoma transfer conduit and/or institute
State reaction chamber be passed through purging solvent purged.
As shown in figure 3, the gas delivery system include presoma transfer conduit 21, presoma transfer conduit 22 and respectively with
Precursor source bottle 11 that presoma transfer conduit 21 is connected with 22 on-off of presoma transfer conduit, 12 gas of precursor source bottle
Transfer conduit 21 and gas transfer conduit 22 import reaction chamber 1 jointly, and point is referred to as chamber injection end 10.Indifferent gas
Body can enter reaction chamber 1 by presoma transfer conduit 21 and/or presoma transfer conduit 22.
Precursor source bottle heating to a certain extent when can generate precursor vapor, at this point, precursor source bottle be passed through it is lazy
When property gas, precursor vapor takes precursor source bottle out of by inert gas.
When precursor transfer conduit 21 is connected to precursor source bottle 15, it is passed through the inert gas of presoma transfer conduit 21
The presoma carried out in precursor source bottle 15 transmits in pipeline；Precursor transfer conduit 21 and precursor source bottle 11 disconnect
When, the inert gas for being passed through presoma transfer conduit 21 does not carry presoma, directly transmits in pipeline.Presoma is transmitted
Pipeline 22 and precursor source bottle 12 are also same situation.
Solvent flush system includes solvent delivery pipeline 23 and the solvent source that connect with 23 on-off of solvent delivery pipeline
Bottle 13,21 selectivity of solvent delivery pipeline 13 and presoma transfer conduit are connected to, to presoma transfer conduit 21 and/or to react
Chamber 1 is passed through purging solvent and is purged.
Solvent flush system further includes the solvent recovery unit 14 being connected and solvent purification device (being not shown in Fig. 3),
Wherein, solvent recovery unit includes the first solvent recovery unit 141 and the second solvent recovery unit 142, presoma transfer conduit
21 and presoma transfer conduit 22 by import pipeline connect with 141 on-off of the first solvent recovery unit, reaction chamber 1 and
The connection of second solvent recovery unit, 142 on-off.
It is passed through the presoma transfer conduit connecting with reaction chamber 1 by the way that solvent will be washed away, it can be to presoma transfer conduit
Or solvent flush is carried out together with reaction chamber 1, to reduce in 1 inner wall of presoma transfer conduit and reaction chamber
Absorption and desorption and the possibility of unexpected reaction occurs.
By recycling to washing away solvent, recovered solvent can be purified again using solvent purification device again.Solvent
Purifying can be using physical separation such as distillation or chemical purification such as catalytic purification.Wash away solvent can according to ALD react before
It drives volume property and reaction temperature feature is selected.
Washing away solvent in solvent source bottle 13 is liquid, when solvent source bottle 13 is connected to solvent delivery pipeline 23, is entered
The inert gas of solvent delivery pipeline 23 enters solvent source bottle 13, carries out solvent vapo(u)r, continuation is transmitted in pipeline, before arrival
Drive body transfer conduit 21.First solvent recovery unit 141 is connect with presoma transfer conduit 21, to recycle rushing after washing away pipeline
Brush solvent.Solvent delivery pipeline 23 and the tie point of presoma transfer conduit 21 are referred to as solvent delivery tie point 30.
Further include vacuum pump 5 in the atomic layer deposition apparatus, transfer conduit 21 be selectively connected to reaction chamber 1 or with
The connection of 1 vacuum pump.
Specifically, it may be accomplished by the selectivity of presoma transfer conduit 21 Yu reaction chamber 1 and vacuum pump
Connection.
Presoma transfer conduit 21 is divided to for two branches, respectively the first presoma transmission branch 25 and the second presoma biography
Defeated branch 26, the first presoma transmission branch 25 are connected to chamber injection end 10, and the second presoma transmission branch 26 is connected to very
The arrival end of sky pump 5, tie point are referred to as chamber output end 20.Control is preferably provided between chamber injection end 10 and reaction chamber 1
Valve 107 processed, is preferably provided with control valve 108 between chamber output end 20 and vacuum pump 5.Chamber injection end 10 and chamber output end 20
It is connect respectively with the first solvent recovery unit 141 and the second solvent recovery unit 142, and is preferably provided with control on connecting line
Valve 105 and control valve 106 processed.
Control valve 101 and control are respectively equipped in the first presoma transmission branch 25 and in the second presoma transmission branch 26
Valve 102 processed.When control valve 101 is opened, control valve 102 is closed, and the gas in presoma transfer conduit 21 enters the first presoma
Branch 25.At this point, control valve 105 is closed when control valve 107 is opened, then gas can then enter reaction chamber 1, conversely, then entering
First solvent recovery unit 141.When control valve 101 is closed, control valve 102 is opened, the gas in presoma transfer conduit 21 into
Enter the second presoma branch 26.At this point, control valve 106 is closed, then gas is aspirated by vacuum pump 5, instead when control valve 108 is opened
It, then enter the second solvent recovery unit 142.
Based on above structure, when solvent system is passed through to presoma transfer conduit and washes away solvent, the property of can choose
The presoma transfer conduit for being transmitted across presoma is only washed away, also can choose and washed away together together with reaction chamber.Two kinds of sides
After formula is washed away, solvent will all enter solvent recovery unit 14 and recycle.
In one example, vacuum pump 5 is connect via butterfly valve 6 with one of outlet end of reaction chamber 1, and butterfly valve
Spool be in permanent angle mode.
The atomic layer deposition apparatus further includes inert gas delivery tube road 24, and its inlet is provided with mass flow
Controller 17, to control the gas flow transmitted in pipeline.
Inert gas delivery tube road 24 and presoma transfer conduit 21 are equally selectively connected to reaction chamber 1 or with 1
Vacuum pump connection, can be accomplished by the following way: inert gas delivery tube road 24 is in the outlet end of mass flow controller 17
It is divided into the first inert gas delivery branch 27 and the second inert gas delivery branch 28, the first inert gas delivery branch 27 and
One presoma transmission branch 25 is connected to chamber injection end 10, the second inert gas delivery branch 28 and the second presoma after converging
Transmission branch 26 is connected to chamber output end 20 after converging.On first inert gas delivery branch 27 and the second inert gas delivery
Control valve 103 and control valve 104 are preferably respectively arranged on branch 28.
ALD reaction there are certain requirements chamber pressure, be controlled by mass flow controller 17 lazy in gas transport pipeline
Property gas transport pipeline 24 in inert gas flow and by controlling the opening angle in the butterfly valve 6 of cavity bottom
Chamber pressure is maintained in suitable interval；And by adjusting the opening angle of butterfly valve, thus it is possible to vary the pressure of chamber.
Mass flow controller is respectively arranged in the arrival end of presoma transfer conduit 21 and presoma transfer conduit 22
15 and 16, to control the gas flow transmitted in pipeline.
In one example, precursor source bottle 11 and 12 is realized and presoma transfer conduit by the first valve module respectively
21 connect with 22 on-off.
First valve module is realized preferably by three pneumatic operated valves and three hand-operated valve combinations.To control presoma transfer conduit
For first valve module of the on-off between 21 and precursor source bottle 11 comprising the first pneumatic operated valve 111, the second pneumatic operated valve 112,
Third pneumatic operated valve 113, first manual valve 121, the second hand-operated valve 122, third hand-operated valve 123.Wherein, the first pneumatic operated valve 111 is set
It sets in presoma transfer conduit 21, is arranged after the second pneumatic operated valve 112 and the series connection of the second hand-operated valve 122 in the first pneumatic operated valve 111
Arrival end and precursor source bottle 11 arrival end between, setting is the after third pneumatic operated valve 113 and third hand-operated valve 123 are connected
Between the outlet end of one pneumatic operated valve 111 and the outlet end of precursor source bottle 11, one end of first manual valve 121 is connected to the second gas
Between dynamic valve 112 and the second hand-operated valve 122, the other end is connected between third pneumatic operated valve 113 and third hand-operated valve 123.
In the case where the first pneumatic operated valve 111 opens the second pneumatic operated valve 112, third pneumatic operated valve 113 is closed, in presoma
Inert gas in transfer conduit 21 bypasses precursor source bottle 11, and transmission is without carrying presoma directly in pipeline；First
Pneumatic operated valve 111 is closed, and the second pneumatic operated valve 112, third pneumatic operated valve 113 and the second hand-operated valve 122, third hand-operated valve 123 are opened
In the case of, inert gas is by precursor source bottle 11, and the presoma carried out in precursor source bottle 11 transmits in pipeline.
It can also be configured by similar mode between other presoma transfer conduits and corresponding precursor source bottle.
Solvent delivery tie point 30 is preferably placed at the outlet end of third pneumatic operated valve 113.Due to the outlet end of precursor source 11
It is to accumulate the position of more presoma, therefore solvent delivery pipeline 23 is connected to the outlet end of third pneumatic operated valve 113, more favorably
In thoroughly washing away the presoma remained in pipeline.
In one example, solvent source bottle 13 is realized by the second valve module and is connected with the on-off of solvent delivery pipeline 23
It connects.
Second valve module is realized preferably by three pneumatic operated valves and two hand-operated valve combinations, for example including the 4th pneumatic operated valve
117, the 5th pneumatic operated valve 118, the 6th hand-operated valve 119, the 4th hand-operated valve 127, the 5th hand-operated valve 128.Wherein, the 4th pneumatic operated valve
117 and the 4th hand-operated valve 127 connect after be connected to the arrival end of solvent source bottle 13；5th pneumatic operated valve 118 and the 5th hand-operated valve 128
The outlet end of solvent source bottle 13 is connected to after series connection；One end of 6th pneumatic operated valve 119 is connected to the 4th pneumatic operated valve 117 and the 4th hand
Between dynamic valve 127, the other end is connected between the 5th pneumatic operated valve 118 and the 5th hand-operated valve 128.
It is opened in the 4th pneumatic operated valve 117, the 5th pneumatic operated valve 118, the 6th pneumatic operated valve 119, the 4th hand-operated valve 127, the 5th hand
In the case that dynamic valve 128 is closed, the inert gas in solvent delivery pipeline 23 bypasses solvent source bottle 13, directly passes in pipeline
It is defeated without carry solvent；It is closed in the 6th pneumatic operated valve 119, the 4th pneumatic operated valve 117, the 5th pneumatic operated valve 118 and the 4th hand-operated valve
127, in the case that the 5th hand-operated valve 128 is opened, inert gas is carried out molten in solvent source bottle 13 by solvent source bottle 13
Agent is transmitted in pipeline.
One of outlet end of reaction chamber 1 is provided with control valve 108, additional gas transfer conduit 29 is connected to control
The outlet end of valve 108 processed, and mass flow controller 18 is provided in additional gas transfer conduit 29.
The purpose that additional gas transfer conduit 29 is arranged is the particle in order to reduce the generation of chamber valve switch.It passes through increasing
Add inert gas to the purging of valve position, gate valve switch motion bring particle contamination can be reduced.
In one example, it rushes in solvent delivery pipeline 23 and presoma transfer conduit 21 and is provided with heating device.
It is usually solvent vapo(u)r from the solvent that washes away carried in solvent source bottle 13 is washed away, solvent vapo(u)r is again cold in order to prevent
It is solidifying, it requires to increase heating control apparatus, such as heating tape on solvent delivery pipeline 23 and presoma transfer conduit 21, to carry out
Heated for controlling temperature appropriate.
Fig. 4 shows the flow chart of Atomic layer deposition method in accordance with an exemplary embodiment of the invention.As shown in figure 4,
This method includes S101~S107.
In step s101, inert gas is carried after the first presoma enters the reaction chamber of atomic layer deposition apparatus and is adsorbed
On the surface of substrate.
Carrier gas of the inert gas as presoma, can be argon gas, helium, nitrogen etc..
In step s 102, the first presoma of inert gas purge transfer conduit.
By the purging of inert gas, and cooperate and vacuumize, removes remaining in presoma transfer conduit and reaction chamber
Presoma.
In step s 103, the second presoma of inert gas carrying enters the first forerunner after reaction chamber with substrate surface
Precursor reactant, to form default film.
The type of first presoma and the second presoma determined based on the type of default film, for example, ZrO2Film.
In step S104, inert gas purge the second presoma transfer conduit.
Similar to step S102, by the purging of inert gas, cooperation is vacuumized, and removes presoma transfer conduit and reaction
Remaining presoma in chamber.
In step s105, whether the film performance of any a piece of substrate of judgement and the default film on adjacent a piece of substrate
It is deteriorated, if not, repeating step S101 to step S104 more times；If so, thening follow the steps S106.
Mainly judge the uniformity of film whether as the thick increase of film accumulation is deteriorated instead.
In step s 106, inert gas carries solvent vapo(u)r and purges the first presoma transfer conduit and/or the second forerunner
Body transfer conduit and/or the reaction chamber.
Carry inert gas purge the first presoma transfer conduit and/or the second presoma transfer conduit of solvent vapo(u)r
And/or reaction chamber reduces presoma in chamber inner wall effectively to remove residual of the presoma in presoma transfer conduit
The especially absorption of the low local location of temperature, so as to reduce in the indoor unexpected reactant deposition of chamber, to improve
Film purity improves the quality of deposition film.
In one example, this method further includes step S107~S110.
In step s 107, inert gas carry third presoma enter after reaction chamber be adsorbed on reaction chamber inner wall and
Baffle surface on substrate.
In step S108, inert gas purge third forerunner's transfer conduit.
In step S109, inert gas carry the 4th presoma enter the reaction chamber after it is anti-with third presoma
It answers, to form passivation layer, such as Al2O3Passivation layer.
In step s 110, the 4th forerunner's transfer conduit of inert gas purge.
It reacts to form chamber passivation layer by ALD, can not only be covered in chamber and be failed clearly by solvent purging on a small quantity
The presoma absorption removed, farthest can also be restored to desired process conditions for chamber, equal so as to improve film thickness
Even property, especially improves the repeatability of film performance between piece.The particulate matter that chamber inner wall can also be reduced by passivation layer is attached
, to improve the purity of deposition film.
First presoma and third presoma are presoma not of the same race, before the second presoma is mutually of the same race with the 4th presoma
Drive body.
Before step S107, the pipeline of the first presoma and the second presoma is transmitted preferably by inert gas purge,
And gas transport pipeline presoma transfer conduit and the indoor particle residue of chamber after solvent purges are removed by vacuumizing.
Before step S101, preferably by inert gas purge all gas transfer conduit presoma transfer conduit, with
It is provided with the good substrate surface for being conducive to ALD reaction.
Type based on the presoma that above-described Atomic layer deposition method utilizes, determines atomic layer according to the present invention
The gas transport pipeline presoma transfer conduit and corresponding precursor source bottle number that the gas delivery system of depositing device is included
Amount can know equipment using above-described atomic layer deposition and implement this method.
Using example
Below by taking deposited oxide zirconium film as an example, illustrate the process that atomic layer deposition apparatus shown in Fig. 3 is deposited into film.
(1) inert nitrogen gas carries after presoma TEMAZ steam enters reaction chamber 1 from presoma transfer conduit 21,
It is adsorbed on the surface of substrate 3.
In presoma transfer conduit 21, a certain amount of inert gas controlled through mass flow controller 15, by
The source bottle 11 that the presoma TEMAZ of heated for controlling temperature is passed through after two pneumatic operated valves 112 and the second hand-operated valve 122 (such as is heated to 80
DEG C), TEMAZ steam passes through third hand-operated valve 123 and third pneumatic operated valve 113 after being carried by carrier gas, returns to presoma transfer conduit
After 21, enter reaction chamber 1 using control valve 101,107.Presoma TEMAZ pulse distributes dress by the gas on chamber top
3 surface of substrate is equably adsorbed on after setting 2.
(2) inert gas purge presoma transfer conduit 21.
In the case where the first pneumatic operated valve 111 opens the second pneumatic operated valve 112, third pneumatic operated valve 113 is closed, inert gas
Not by precursor source bottle 11, i.e., presoma is not carried and is transmitted in pipeline.
By opening controlling valve 101,107, can be used in the inert gas purge presoma transfer conduit 21 of purging with
And reaction chamber, purge gas can also be made only to purge presoma transfer conduit 21 by opening controlling valve 102,108, without
Into reaction chamber 1.Meanwhile cooperating the swabbing action of vacuum pump 5, TEMAZ gas remaining in pipeline and chamber can be gone
It removes.
(3) inert gas carries presoma H2O enters the reaction chamber 1.
H2O pulse enters reaction chamber 1 by presoma transfer conduit unshowned in Fig. 3, and is adsorbed on substrate surface
Presoma TEMAZ reaction, ZrO is formed on the substrate2Film.
(4) inert gas purge transmits presoma H2The pipeline of O.
(5) judge ZrO2Whether the front and rear panel film performance of film is deteriorated, if not, it is multiple to repeat (1) to (4)；
If so, then executing (6)；
(6) the inert gas purge TEMAZ transfer conduit and/or H for washing away solvent are carried2O transfer conduit and/or reaction chamber
Room 1.
Since presoma TEMAZ steam forces down, Nature comparison is sticky, certain thickness ZrO is being deposited2After need through
Cross solvent purging chamber and pipeline.Washing away solvent can be using suitable organic solvent, because these solvents have suitable steam
Vapour pressure.
After inert gas is passed through the solvent source bottle 13 of heated for controlling temperature after the 4th pneumatic operated valve 117, the 4th hand-operated valve 127,
It carries out and washes away the 5th hand-operated valve 128 and the 5th pneumatic operated valve 118 that solvent vapo(u)r passes through 13 exit of solvent source bottle, by solvent
Transfer conduit 23 enters solvent delivery pipeline 21 in solvent delivery tie point 30.
It can be made before washing away solvent vapo(u)r purging presoma transfer conduit 21 and first by opening controlling valve 101,107
Enter solvent recovery unit 14 after driving body transfer conduit 25；It can also make to wash away solvent vapo(u)r by opening controlling valve 102,108
Enter solvent recovery unit 14 after purging presoma transfer conduit 21 and the second presoma transfer conduit 26.
(7) inert gas for carrying TMA enters after reaction chamber 1 the baffle table being adsorbed on reaction chamber inner wall and substrate
Face.
(8) inert gas purge TMA transfer conduit.
(9) H is carried2The inert gas of O reacts after entering reaction chamber 1 with TMA, to form Al2O3Passivation layer.
(10) inert gas purge H2O transfer conduit.
Form Al2O3H2O and ZrO2The H of reaction2O can share a source bottle.
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and
It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill
Many modifications and changes are obvious for the those of ordinary skill in art field.The selection of term used herein, purport
In the principle, practical application or improvement to the technology in market for best explaining each embodiment, or make the art
Other those of ordinary skill can understand each embodiment disclosed herein.
Claims (11)
1. a kind of atomic layer deposition apparatus, which is characterized in that passed including reaction chamber, solvent flush system and multiple presomas
Defeated system, wherein
Each precursor delivery system include presoma transfer conduit and with the presoma transfer conduit on-off
The precursor source bottle of connection, a plurality of presoma transfer conduit import the reaction chamber jointly；
The solvent flush system includes solvent delivery pipeline and the solvent source that connect with the solvent delivery pipeline on-off
Bottle, the solvent delivery pipeline are selectively connected to at least one presoma transfer conduit, to transmit to the presoma
Pipeline and/or the reaction chamber are passed through purging solvent and are purged.
2. atomic layer deposition apparatus according to claim 1, which is characterized in that the solvent flush system further includes being connected
The solvent recovery unit and solvent purification device connect, wherein
The solvent recovery unit includes the first solvent recovery unit and the second solvent recovery unit, a plurality of presoma transmission
Pipeline is connect by importing pipeline with the first solvent recovery unit on-off, the reaction chamber and second solvent
The connection of recyclable device on-off.
3. atomic layer deposition apparatus according to claim 2, which is characterized in that the atomic layer deposition apparatus further includes true
Sky pump, the vacuum pump are connect via butterfly valve with one of outlet end of the reaction chamber, and the spool of the butterfly valve is in
Permanent angle mode.
4. atomic layer deposition apparatus according to claim 2, which is characterized in that in each precursor delivery system,
The precursor source bottle passes through the realization of the first valve module and connect with the on-off of the presoma transfer conduit, wherein
First valve module includes three pneumatic operated valves and three hand-operated valves, and the first pneumatic operated valve is arranged in the presoma transfer tube
On the road；
The arrival end and the precursor source bottle of first pneumatic operated valve are set after the second pneumatic operated valve and the series connection of the second hand-operated valve
Arrival end between；
Third pneumatic operated valve and third hand-operated valve series connection after be arranged in first pneumatic operated valve outlet end and the precursor source bottle
Outlet end between；
One end of first manual valve is connected between second pneumatic operated valve and second hand-operated valve, and the other end is connected to described
Between third pneumatic operated valve and the third hand-operated valve.
5. atomic layer deposition apparatus according to claim 4, which is characterized in that the solvent source bottle passes through the second valve module
Realization is connect with the on-off of the solvent delivery pipeline, wherein
Second valve module includes three pneumatic operated valves and two hand-operated valves, is connected after the 4th pneumatic operated valve and the series connection of the 4th hand-operated valve
In the arrival end of the solvent source bottle, the outlet of the solvent source bottle is connected to after the 5th pneumatic operated valve and the series connection of the 5th hand-operated valve
End；
One end of 6th pneumatic operated valve is connected between the 4th pneumatic operated valve and the 4th hand-operated valve, and the other end is connected to described
Between 5th pneumatic operated valve and the 5th hand-operated valve.
6. atomic layer deposition apparatus according to claim 4, which is characterized in that the atomic layer deposition apparatus further includes attached
Aerating body transfer conduit, another outlet end of the reaction chamber are provided with control valve, the outlet of the control valve with it is described
Additional transmitted piping connection is provided with mass flow controller in the inlet of the additional transmitted pipeline.
7. atomic layer deposition apparatus according to claim 2, which is characterized in that the solvent delivery pipeline and the forerunner
Heating device is provided in body transfer conduit.
8. a kind of Atomic layer deposition method, which comprises the following steps:
Step 1, inert gas carry the first presoma and enter after the reaction chamber of atomic layer deposition apparatus the table for being adsorbed on substrate
Face；
Step 2, the first forerunner of inert gas purge pass the defeated pipeline of body；
Step 3, inert gas the second presoma of carrying enter the first presoma after the reaction chamber with the substrate surface
Reaction, to form default film over the substrate；
Second presoma transfer conduit described in step 4, inert gas purge；
Step 5 judges whether the film performance of any a piece of substrate and the default film on adjacent a piece of substrate is deteriorated, if not,
The step 1 is then repeated to the step 4 more times；If so, then executing following step 6；
Step 6, inert gas carry solvent vapo(u)r and purge the first presoma transfer conduit and/or second presoma biography
Defeated pipeline and/or the reaction chamber.
9. Atomic layer deposition method according to claim 8, which is characterized in that further include following step:
Step 7, inert gas carry after third presoma enters the reaction chamber and are adsorbed on the reaction chamber inner wall and institute
State the baffle surface on substrate；
Step 8, inert gas purge third forerunner's transfer conduit；
Step 9, inert gas carry the 4th presoma enter the reaction chamber after with third forerunner's precursor reactant, with formed passivation
Layer；
Step 10, the 4th forerunner's transfer conduit of inert gas purge.
10. Atomic layer deposition method according to claim 9, which is characterized in that first presoma and the third
Presoma is presoma not of the same race, and second presoma is presoma mutually of the same race with the 4th presoma.
11. Atomic layer deposition method according to claim 10, which is characterized in that the default film is ZrO2Film, institute
Stating passivation layer is Al2O3Passivation layer.
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| US20040023516A1 (en) * | 2001-10-02 | 2004-02-05 | Londergan Ana R. | Passivation method for improved uniformity and repeatability for atomic layer deposition and chemical vapor deposition |
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| US20160056033A1 (en) * | 2014-08-19 | 2016-02-25 | The Regents Of The University Of California | Low temperature atomic layer deposition of oxides on compound semiconductors |
| CN107815666A (en) * | 2017-10-31 | 2018-03-20 | 华中科技大学 | A kind of film doping method of modifying based on plasma enhanced atomic layer deposition |
| CN107868944A (en) * | 2017-10-31 | 2018-04-03 | 北京北方华创微电子装备有限公司 | A kind of titanium nitride apparatus for atomic layer deposition and its deposition process |
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|---|---|---|---|---|
| US20040023516A1 (en) * | 2001-10-02 | 2004-02-05 | Londergan Ana R. | Passivation method for improved uniformity and repeatability for atomic layer deposition and chemical vapor deposition |
| US20090162551A1 (en) * | 2007-12-21 | 2009-06-25 | Thomas Zilbauer | Hafnium oxide ald process |
| CN104488088A (en) * | 2012-07-19 | 2015-04-01 | 日立化成株式会社 | Solar cell element, production method therefor, and solar cell module |
| US20160056033A1 (en) * | 2014-08-19 | 2016-02-25 | The Regents Of The University Of California | Low temperature atomic layer deposition of oxides on compound semiconductors |
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