CN101671813A - Film forming method of ti-series film - Google Patents
Film forming method of ti-series film Download PDFInfo
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- CN101671813A CN101671813A CN200910173311A CN200910173311A CN101671813A CN 101671813 A CN101671813 A CN 101671813A CN 200910173311 A CN200910173311 A CN 200910173311A CN 200910173311 A CN200910173311 A CN 200910173311A CN 101671813 A CN101671813 A CN 101671813A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/28—Manufacture of electrodes on semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/268
- H01L21/283—Deposition of conductive or insulating materials for electrodes conducting electric current
- H01L21/285—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation
- H01L21/28506—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers
- H01L21/28512—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System
- H01L21/28556—Deposition of conductive or insulating materials for electrodes conducting electric current from a gas or vapour, e.g. condensation of conductive layers on semiconductor bodies comprising elements of Group IV of the Periodic System by chemical means, e.g. CVD, LPCVD, PECVD, laser CVD
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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
- C23C16/45563—Gas nozzles
- C23C16/45565—Shower nozzles
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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
- C23C16/52—Controlling or regulating the coating process
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02046—Dry cleaning only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/324—Thermal treatment for modifying the properties of semiconductor bodies, e.g. annealing, sintering
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Abstract
The present invention provides a film forming method of Ti-series film, which does not generate the adverse states such as the reaction among pre-coated film, spraying head and the base and can suppress the inter-surface deviation of the thickness of processed film. The following processes are performed repeatedly: a process of heating a base (2) and forming the pre-coated film on the surface of the spraying head (10) with the processing gas which contains Ti at a state that a wafer (W) does not exist on a base (2); a process for setting the wafer (W) on the base which is heated to a preset temperature, supplying processing gas into a chamber (1) and forming a Ti film on the wafer (W); and a process of introducing cleaning gas into the chamber (1) for washing the chamber (1) at the state that a wafer (W) does not exist on a base (2). In the forming process of pre-coated film, after a low-temperature pre-coated film (71) is formed when the temperature of the base (2) is lower than the temperature in the Ti film forming process, a high-temperature pre-coated film (72) is formed in the temperature when the Ti film is formed.
Description
Technical field
The present invention relates to the storage media that the film of Ti class film and storage are used to implement the program of its method, it is in chamber, spray the processing gas that contains Ti from spray header, film forming contains the film (Ti class film) of Ti element on the surface of the processed substrate on the mounting table in being disposed at chamber.
Background technology
In the manufacturing of semiconducter device, corresponding to nearest densification and highly integrated requirement, the trend of circuit structure being made Miltilayer wiring structure is arranged, therefore, as the contact hole of the semiconductor substrate of lower floor and the connection section of the wiring layer on upper strata, as the interlayers such as through hole of wiring layer connection section each other up and down be electrically connected usefulness to imbed technology more and more important.
In order to form the middle metal or alloy and the Si substrate of lower floor and contacting of poly-Si layer that uses of imbedding of this contact hole and through hole, before imbedding them, elder generation is at the inboard film forming Ti film of contact hole or through hole.
All the time, with this Ti film of physical vapor deposition (PVD) film forming, but along with the miniaturization of device and highly integrated requirement, the chemical vapor deposition (CVD) that selectable rank spreadability (step coverage) is more good.
About the CVD film forming of Ti film, proposing has following technology: use TiCl
4Gas, H
2Gas, Ar gas are as film forming gas, they are indoor via the spray header introduction chamber, with handled object be semiconductor wafer (below, be called wafer simply) under the state of the interior pedestal that well heater is housed, be heated to specified temperature in mounting, and the above-mentioned gas plasma is made TiCl by apply High frequency power to parallel plate electrode
4Gas and H
2The plasma CVD film forming Ti film (for example, patent documentation 1) of gas reaction.
When utilizing plasma CVD film forming Ti film like this, utilize ClF
3In the chamber after the above-mentioned Ti film of purge of gas film forming finishes, then and film forming handle equally, same temperature when making pedestal become with Ti film film forming is used TiCl
4Gas and H
2Gas carries out forming the precoating processing of Ti film on chamber inner wall, pedestal and spray header, thereafter, as mentioned above, film forming Ti film on wafer.
But same temperature is carried out under the situation of precoating processing when making pedestal become with Ti film film forming, and when cleaning, the AlN and the purge gas that constitute pedestal are ClF
3The AlF class material that generated of reaction distils when precoating, and attached to the spray header surface, the film that pre-coating film might take place when film-forming process is peeled off and become the reason of generation particulate as the film a little less than the connecting airtight property.In addition, might be when precoating to be handled, Ni that Ti that contains in the film forming gas and chamber or spray header contain reaction forms NiTi, and NiTi is ingested in the pre-coating film, thereafter, stripping in film-forming process and pollute wafer surface.
Therefore, having proposed to make base-plate temp in the patent documentation 2 is temperature when being lower than film-forming process, preferred below 500 ℃ for example 450 ℃ carry out the technology that precoating is handled.
But, in the film-forming process that after precoating, carries out, except that being on the wafer the film forming Ti film at processed substrate, along with to semiconductor wafer film forming repeatedly, also film forming Ti film on spray header that is formed with pre-coating film and pedestal.But, in the technology of patent documentation 2, pre-coating film during than film-forming process temperature low, pre-coating film is membranous different with the Ti film that forms when the film-forming process, therefore when film-forming process, on the pre-coating film of spray header and pedestal, generate, adhere to membranous different Ti film, occur in film forming before the film that adheres to membranous stable in the thickness of the Ti of wafer film inhomogeneous and so on phenomenon between wafer surface.
Patent documentation 1:(Japan) spy opens the 2003-313666 communique
Patent documentation 2: the international brochure that discloses No. 2008/047838
Summary of the invention
The present invention develops in view of such situation, and its purpose is, a kind of film of Ti class film is provided, and it does not produce pre-coating film and spray header or pedestal in film forming unfavorable conditions such as reaction can suppress to handle deviation between the face of thickness.In addition, its purpose is, a kind of storage media that stores the embodied on computer readable of the sequence of control that is used to carry out aforesaid method is provided.
In order to solve above-mentioned problem, first aspect present invention provides a kind of film of Ti class film, use comprises the chamber of accommodating handled object, ejection comprises the gas ejection parts of the processing gas that contains Ti gas and purge gas in described chamber, the mounting table of mounting handled object in described chamber, with the device of heating unit of the described mounting table of heating at the surface filming Ti of handled object class film, it is characterized in that, comprise: do not exist on the described mounting table under the state of handled object, utilize described heating unit to heat described mounting table, and in described chamber, spray described processing gas from described gas ejection parts, form the operation of pre-coating film at least on the surface of described gas ejection parts; Thereafter, mounting handled object on the described mounting table of the state after being heated by described heating unit is supplied with described processing gas, the operation of a plurality of handled objects being carried out the processing of film forming Ti class film on handled object in described chamber; With do not exist on the described mounting table under the state of handled object, in described chamber, import purge gas, to the operation of cleaning in the described chamber, carry out above-mentioned these operations successively repeatedly, wherein, in forming the operation of described pre-coating film, the low temperature of temperature when making the temperature of described mounting table become and forming after the low temperature pre-coating film than described film formation process, under the temperature when described film formation process, form the high temperature pre-coating film.
In the above-mentioned first aspect, described mounting table can be used the mounting table that is made of AlN, and in addition, described gas ejection parts can use the surperficial at least parts that are made of the material that contains Ni.
In addition, the temperature of the described mounting table when forming described low temperature pre-coating film is preferably more than 350 ℃ and 550 ℃ of less thaies, when forming described high temperature pre-coating film and the temperature of the described mounting table during the described Ti class of film forming film is preferably more than 550 ℃ and below 680 ℃.When forming described pre-coating film and the temperature of the described gas ejection parts during the described Ti class of film forming film is preferably more than 350 ℃ and below 500 ℃.
In addition, preferred described pre-coating film and the utilization of described Ti class film contain Ti gas and reducing gas forms.The film forming of described pre-coating film preferably contains Ti gas and reducing gas carries out by alternately supplying with.In addition, the film forming of described pre-coating film also can comprise the nitriding treatment of pre-coating film.As described Ti class film, can use the Ti film, in this case,, can use TiCl as described processing gas
4Gas and H
2Gas.In addition, after also can finishing, the Ti film is implemented nitriding treatment in the operation of the described Ti class of film forming film.
In addition, as described gas ejection parts, typically, can use with described mounting table mutually opposed to each other to setting and be formed with the spray header of a plurality of gas squit holes.
Second aspect present invention provides a kind of storage media, and it is worked on computers, stores the program that is used to be controlled to film device, it is characterized in that, described sequence of control is controlled described film deposition system, on computers so that it carries out aforesaid method when carrying out.
In addition, among the present invention, the unit of gas flow uses mL/min, but the volume of gas can Yin Wendu and air pressure and bigger variation takes place, so uses the value that is scaled standard state among the present invention.In addition, the flow that is scaled standard state is used sccm (Standerd CubicCentimeter per Minutes) expression usually, therefore is designated as sccm.The standard state here is the state (STP) of temperature 0 ℃ (273.15K), air pressure 1atm (101325Pa).
According to the present invention, in the operation that forms pre-coating film, after under the low temperature of the temperature of the temperature that makes mounting table during, forming the low temperature pre-coating film than film formation process, form the high temperature pre-coating film under the temperature when film formation process, therefore, can utilize the low temperature pre-coating film to suppress the unfavorable conditions such as reaction of pre-coating film and spray header or pedestal, and utilize film membranous of the stable first-class coating of spray in Ti film film forming of high temperature pre-coating film, suppress deviation between the face of processing thickness.
Description of drawings
Fig. 1 is the schematic sectional view of one of the Ti film film deposition system that uses in the enforcement of Ti film film of expression one embodiment of the present invention example;
Fig. 2 is the schema of the Ti film film of expression one embodiment of the present invention;
Fig. 3 be illustrated in only be formed with on pedestal and the spray header state of low temperature pre-coating film and thereafter film forming the figure of the state of Ti film is arranged;
Fig. 4 be illustrated in the state that is formed with low temperature pre-coating film and high temperature pre-coating film on pedestal and the spray header and thereafter film forming the figure of the state of Ti film is arranged;
Fig. 5 is with the typical temperature curve example of the pedestal of Ti film of the present invention and the figure of existing temperature curve example contrast expression;
Fig. 6 is the figure of the typical temperature curve of expression the present invention and existing spray header.
Nomenclature
1 chamber
2 pedestals
5 well heaters
10 spray headers
20 gas supply mechanisms
21 ClF
3The gas supply source
22 TiCl
4The gas supply source
23 Ar gas supply sources
24 H
2The gas supply source
25 NH
3The gas supply source
26 N
2The gas supply source
34 high frequency electric sources
50 control parts
71 low temperature pre-coating films
72 high temperature pre-coating films
81 Ti films
The W semiconductor wafer
Embodiment
Below, with reference to accompanying drawing embodiments of the present invention are specifically described.
Fig. 1 is the schematic sectional view of one of the Ti film film deposition system of use during the film of the Ti film of expression one embodiment of the present invention is implemented example.This Ti film film deposition system 100 promptly, forms plasma body and carries out the film forming plasma CVD film deposition system of CVD by form high-frequency electric field on parallel plate electrode as constituting as lower device.
This Ti film film deposition system 100 has chamber 1 roughly cylindraceous.In the inside of chamber 1, be used for flatly supporting processed substrate and be the pedestal 2 that constitutes by AlN of wafer W, with state configuration by cylindric support unit 3 supportings of bottom, centre located therein.Be provided with the guide ring 4 that is used to guide wafer W in the outer edge of pedestal 2.In addition, imbed the well heater 5 that is made of refractory metals such as molybdenums on pedestal 2, this well heater 5 is by being the temperature that wafer W is heated to regulation from heater power source 6 power supply and with processed substrate.Be embedded with electrode 8 as the lower electrode performance function of parallel plate electrode, these electrode 8 ground connection at the near surface of pedestal 2.
On the roof 1a of chamber 1, be provided with also spray header 10 as the upper electrode performance function of parallel plate electrode via insulating element 9.This spray header 10 is made of epimere block 10a, stage casing block 10b, hypomere block 10c, is roughly discoid.Epimere block 10a have with stage casing block 10b and hypomere block 10c together constitutes the horizontal part 10d of spray header main part and above the periphery of this horizontal part 10d ring-shaped continuous support 10e, form concavity.And, by the 10e of this annular support portion supporting spray header 10 integral body.And, on hypomere block 10c, alternately form the squit hole 17 and 18 that sprays gas.Upper surface at epimere block 10a is formed with first gas introduction port 11 and second gas introduction port 12.Among epimere block 10a, there are a plurality of gas passages 13 in 11 branches from first gas introduction port.Be formed with gas passage 15 on the block 10b of stage casing, above-mentioned gas path 13 is communicated with these gas passages 15 via horizontally extending access 13a.In addition, this gas passage 15 is communicated with the squit hole 17 of hypomere block 10c.In addition, among the epimere block 10a, there are a plurality of gas passages 14 in 12 branches from second gas introduction port.Be formed with gas passage 16 on the block 10b of stage casing, above-mentioned gas path 14 is communicated with these gas passages 16.In addition, this gas passage 16 is connected with horizontally extending access 16a in the block 10b of stage casing, and this access 16a is communicated with a plurality of squit holes 18 of hypomere block 10c.And above-mentioned first and second gas introduction port 11,12 is connected with the gas piping of gas supply mechanism 20.
It is ClF that gas supply mechanism 20 has the purge gas of supply
3The ClF of gas
3 Gas supply source 21, supply Ti chemical compound gas are TiCl
4The TiCl of gas
4 Gas supply source 22, the Ar gas supply source 23 of supplying with Ar gas, supply reducing gas are H
2The H of gas
2 Gas supply source 24, supply nitriding gas are NH
3The NH of gas
3 Gas supply source 25, supply N
2The N of gas
2Gas supply source 26.And, at ClF
3 Gas supply source 21 is connected with ClF
3Gas supply pipe road 27 and 30b are at TiCl
4Be connected with TiCl on the gas supply source 22
4Gas supply pipe road 28 is connected with Ar gas supply pipe road 29, at H on Ar gas supply source 23
2Be connected with H on the gas supply source 24
2Gas supply pipe road 30 is at NH
3Be connected with NH on the gas supply source 25
3Gas supply pipe road 30a is at N
2Be connected with N on the gas supply source 26
2Gas supply pipe road 30c.And, on each gas piping, be provided with mass flow controller 32 and clip two valves 31 that mass flow controller 32 is provided with.
From TiCl
4The TiCl that gas supply source 22 extends
4Gas supply pipe road 28 is connected with above-mentioned first gas introduction port 11, at this TiCl
4Be connected with from ClF on the gas supply pipe road 28
3The ClF that gas supply source 21 extends
3Gas supply pipe road 27 and the Ar gas supply pipe road 29 of extending from Ar gas supply source 23.In addition, from H
2The H that gas supply source 24 extends
2Gas supply pipe road 30 is connected with above-mentioned second gas introduction port 12, at this H
2Be connected with from NH on the gas supply pipe road 30
3The NH that gas supply source 25 extends
3Gas supply pipe road 30a, from N
2The N that gas supply source 26 extends
2Gas supply pipe road 30c reaches from ClF
3The ClF that gas supply source 21 extends
3Gas supply pipe road 30b.Therefore, when handling, from TiCl
4The TiCl of gas supply source 22
4Gas and from the Ar gas of Ar gas supply source 23 together via TiCl
4Gas supply pipe road 28, sprays in chamber 1 from squit hole 17 through gas passage 13,15 in spray header 10 from first gas introduction port 11 of spray header 10, on the other hand, and from H
2The H of gas supply source 24
2Gas is via H
2Gas supply pipe road 30, sprays in chamber 1 from squit hole 18 through gas passage 14,16 in spray header 10 from second gas introduction port 12 of spray header 10.That is, spray header 10 is with TiCl
4Gas and H
2Gas supplies to back hybrid (the post mix type) in the chamber 1 fully independently, and their hybrid concurrencies after ejection produce reaction.In addition, being not limited to this, also can be with TiCl
4Gas and H
2Under the mixed state of gas they are supplied to the formula that is pre-mixed in the chamber 1.
On spray header 10, be connected with high frequency electric source 34, make from this high frequency electric source 34 to spray header 10 supply high frequency electric power via matching box 33.By carrying out the film forming processing via the gas plasmaization that spray header 10 supplies in the chamber 1 from high frequency electric source 34 supply high frequency electric power.
In addition, on the horizontal part 10d of the epimere block 10a of spray header 10, be provided with the well heater 45 that is used to heat spray header 10.On this well heater 45, be connected with heater power source 46, to well heater 45 power supplies, spray header 10 can be heated to temperature desired thus from heater power source 46.In order to improve the heating efficiency of well heater 45, be provided with heat insulating member 47 at the recess of epimere block 10a.
Central part at the diapire 1b of chamber 1 is formed with circular hole 35, is provided with the outstanding exhaust chest 36 of mode to cover this hole 35 on diapire 1b downwards.Be connected with vapor pipe 37 in the side of exhaust chest 36, on this vapor pipe 37, be connected with gas barrier 38.And, by making this gas barrier 38 work, can be with the specified vacuum degree that reduces pressure in the chamber 1.
On pedestal 2, can be provided with three (only two of diagrams) wafer supporting pins 39 that are used for supporting wafer W and make its lifting with respect to the surface of pedestal 2 with haunting, these wafer supporting pins 39 are fixed on the supporting plate 40.And wafer supporting pin 39 carries out lifting by driving mechanisms such as cylinder 41 via supporting plate 40.
Sidewall at chamber 1 is provided with the import and export 42 of carrying out the wafer W turnover between the not shown wafer transport chamber that is used in chamber 1 and adjacent setting and the gate valve 43 that opens and closes these import and export 42.
The formation portion of Ti film film deposition system 100 is heater power source 6 and 46, valve 31, mass flow controller 32, matching box 33, high frequency electric source 34, driving mechanism 41 etc. for MPU being arranged the control part 50 of (computer) is connected controlled structure with possessing.In addition, the user interface 51 that is connected with the keyboard of input operation that the operator instructs in order to manage Ti film film deposition system 100 etc. or touch panel, constitutes by indicating meter of the operational situation of visual representation Ti film film deposition system 100 etc. at control part 50.In addition, control part 50 be connected with store be used for by the control of control part 50 realize the various processing that Ti film film deposition system 100 is carried out program, be used for making the portion that respectively constitutes of Ti film film deposition system 100 carry out promptly the fill a prescription storage part 52 of (recipe) of the program of handling according to treatment condition.Prescription is stored among the storage media 52a in the storage part 52.Storage media can be fixed memory medium such as hard disk, also can be mobile memory mediums such as CDROM, DVD.In addition, also can suitably transmit prescription via for example dedicated line from other devices.And as required, prescription is carried out control part 50 to be used to access arbitrarily from the indication of user's interface 51 etc. from storage part 52, under the control of control part 50, carries out desirable processing by Ti film film deposition system 100 thus.
Below, the Ti film film of the present embodiment in the above the sort of Ti film film deposition system 100 is described.
In the present embodiment, as shown in Figure 2, repeat precoating operation (operation 1), Ti film film formation process (operation 2), dry-cleaning operation (operation 3).And, after these operations repetition stipulated numbers, carry out washing in the chamber 1 termly.
The precoating operation of operation 1 is that purpose is carried out with the conditioning in the chamber 1, under the state of wafer not being imported in the chamber 1, repeatedly repeats deposit of Ti film and nitriding treatment, forms pre-coating film on the surface of spray header 10 and pedestal 2.
The Ti film film formation process of operation 2 is: in the chamber 1 after the precoating that so is through with, wafer W is carried out the deposit and the nitriding treatment of Ti film, to many pieces preferred below 3000 pieces for example 500 pieces of wafer W carry out the processing of film forming Ti film continuously.
In the dry-cleaning operation of operation 3, utilizing purge gas is C1F
3Gas is to because of cleaning in the many pieces of contaminated chambers 1 of Ti film film forming.
Below, the precoating operation of above-mentioned operation 1 is described in detail.
The precoating operation of operation 1 is carried out after new product state (or wash back) or above-mentioned dry-cleaning, under the state of wafer W not being imported in the chamber 1, at first, carry out precoating under the temperature of film-forming temperature being lower than, form low temperature pre-coating film (operation 1-1),, temperature risen to film-forming temperature carry out high temperature precoating, form high temperature pre-coating film (operation 1-2) thereafter.
At first be that initial, under same temperature with Ti film film forming the time was carried out situation that precoating handles, the AlN and the purge gas that constitute pedestal 2 were ClF being lower than the reason that forms the low temperature pre-coating film under the temperature of film-forming temperature
3The AlF class material that reaction generates distils when precoating, as the film a little less than the connecting airtight property attached to the spray header surface, when film-forming process, the film that might produce pre-coating film is peeled off and is become the reason of particulate, and in addition, the Ni reaction that contains in Ti that contains in the film forming gas when precoating and chamber or the spray header forms NiTi, NiTi is ingested in the pre-coating film, thereafter, stripping in film-forming process might be polluted wafer surface.
But, shown in Fig. 3 (a), carry out precoating under the temperature of film-forming temperature and only form under the situation of low temperature pre-coating film 71 being lower than on the surface of pedestal 2 and spray header 10, in Ti film film formation process thereafter, shown in Fig. 3 (b), when film forming Ti film 81 on wafer W, also film forming Ti film 81 on the low temperature pre-coating film 71 on the surface of pedestal 2 and spray header 10 simultaneously.At this moment, low temperature pre-coating film 71 and Ti film 81 are because of film-forming temperature different and membranous (crystallization phases and residual chlorine dose etc.) difference.Therefore, in the film forming starting stage of Ti film, be coated on the membranous instability of the film of pedestal 2 and spray header 10, this can involve film forming deviation (thickness drift) between the face of the thickness of the Ti of wafer W film.
Therefore, in the present embodiment, shown in Fig. 4 (a), in the precoating operation, at first, be lower than under the temperature of film-forming temperature, on pedestal 2 and spray header 10, forming low temperature pre-coating film 71, then, thereon, with the same temperature of film-forming temperature under, form high temperature pre-coating film 72.Like this, by forming high temperature pre-coating film 72 under the temperature same with Ti film film forming the time, in Ti film film formation process thereafter, film forming Ti film under the temperature identical with the high temperature precoating, therefore, stablize the membranous of film that becomes mem stage to be coated on pedestal 2 and spray header 10, can suppress film forming deviation (thickness drift) between the face of the thickness of the Ti of wafer W film significantly.
In addition, owing to the Cl in the film of low temperature pre-coating film 71 does not fully remove, therefore, Cl concentration ratio high temperature pre-coating film 72 height.Therefore, under the situation that only is formed with low temperature pre-coating film 71, peel off and to produce particulate because of Cl moves to small film that the surface of pre-coating film causes.Relative with it, by form high temperature pre-coating film 72 on low temperature pre-coating film 71, the Cl amount that moves to the pre-coating film surface reduces, and can reduce the generation of particulate.
At this, the temperature of the pedestal 2 during low temperature precoating (operation 1-1) is preferably more than 350 ℃ and 550 ℃ of less thaies.Reason is as follows: when 350 ℃ of less thaies, the Ti film forms difficulty, and more than 550 ℃ the time, the Ni reaction that contains in Ti that contains in the film forming gas and chamber or the spray header may form NiTi.Preferred temperature is more than 400 ℃ below 500 ℃.
The temperature of the pedestal 2 during high temperature precoating in addition, (operation 1-2) is identical with Ti film film formation process.Thus, after precoating finishes, can begin the film forming of Ti film immediately.At this moment, as described later, the temperature of the pedestal 2 during Ti film film forming is preferred scope below 680 ℃ more than 550 ℃, therefore, also in preferred scope below 680 ℃ more than 550 ℃, carrying out in this scope carries out under the film forming temperature of Ti film the temperature of the pedestal 2 during the high temperature precoating.More preferably more than 600 ℃ below 680 ℃.
In addition, the temperature of spray header 10 and form the low temperature pre-coating film and form the high temperature pre-coating film and all be preferably more than 350 ℃ below 500 ℃.This is following cause: in this temperature range, the reaction of the Ni by preventing Ti and spray header 10 can suppress the generation of particulate, and can form stable film.
Below, concrete precoating is described in proper order.The formation of the formation of low temperature pre-coating film and high temperature pre-coating film is all following to be carried out: at first, under the state of wafer not being imported in the chamber 1, utilize gas barrier 38 with the state that is evacuated in the chamber 1, with Ar gas and N
2Gas imports in the chamber 1, and utilizes well heater 5 that pedestal 2 is heated up, at the temperature-stable of pedestal 2 in the moment of specified temperature, with TiCl
4Gas imports with the regulation flow, and applies High frequency power from high frequency electric source 34, with Ar gas, the H that is directed in the chamber 1
2Gas, TiCl
4Gas plasmaization, thus chamber 1 inwall, exhaust chest 36 inwalls, spray header 10, and pedestal 2 on form the Ti film, and then, only stop TiCl
4Gas makes the NH as nitriding gas
3Gas communication, and apply High frequency power to spray header 10, with these gas plasmaizations, with the nitrogenize of Ti film.Repeating repeatedly, for example carry out for 33 times these Ti films forms and nitriding treatment, film forming low temperature pre-coating film or high temperature pre-coating film.In addition, also can not carry out the Ti film that nitriding treatment ground forms specific thickness.
The preferred condition of precoating operation is as follows.
(1) forms the Ti film
I) from the High frequency power of high frequency electric source 34
Frequency: 300kHz～27MHz
Power: 100～1500W
Ii) TiCl
4Gas flow: 1～20mL/min (sccm)
Iii) Ar gas flow: 100～2000mL/min (sccm)
Iv) H
2Gas flow: 250～5000mL/min (sccm)
V) cavity indoor pressure: 400～1333Pa (3～10Torr)
(2) nitriding treatment
I) from the High frequency power of high frequency electric source 34
Frequency: 300kHz～27MHz
Power: 400～1500W
Ii) NH
3Gas flow: 100～2000mL/min (sccm)
Iii) Ar gas flow: 100～2000mL/min (sccm)
Iv) H
2Gas flow: 250～5000mL/min (sccm)
V) cavity indoor pressure: 400～1333Pa (3～10Torr)
Below, the Ti film film formation process of operation 2 is described in detail.
In the Ti of operation 2 film film formation process, after the double-deck pre-coating film that the precoating by operation 1 as mentioned above forms low temperature pre-coating film 71 and high temperature pre-coating film 72 finishes, in chamber 1, to many pieces, preferred below 3000 pieces for example 500 pieces of wafer W carry out Ti film deposit (operation 2-1) and nitriding treatment (operation 2-2) continuously to wafer W.
The deposit of Ti film is following to be carried out, after utilizing well heater 5 that pedestal 2 is risen to specified temperature, the outside atmosphere gas that is adjusted in the chamber 1 with being connected via gate valve 43 is same, thereafter, open gate valve 43, from the not shown wafer transport chamber of vacuum state,, wafer W is imported in the chamber 1 via importing and exporting 42.The order that forms the Ti film then and in the precoating operation on spray header 10 etc. is same, with Ar gas, the H that is directed in the chamber 1
2Gas, TiCl
4Gas plasmaization also makes their reactions, thereby the Ti film of specific thickness is deposited on the wafer W.
In the nitriding treatment after the deposit of Ti film, the deposit of above-mentioned Ti film stops TiCl after finishing
4Gas becomes and makes H
2Gas and Ar gas keep the state of circulation, (chamber wall and spray header surface etc.) in the chamber 1 are heated to suitable temperature, and make NH as nitriding gas
3Gas communication, and apply High frequency power to spray header 10 from high frequency electric source 34 will be handled gas plasmaization, utilize the processing gas after the plasma, with film forming surfaces nitrided in the Ti of wafer W film.In addition, nitriding treatment is optional.
In the Ti of operation 2 film film formation process,, preferred more than 550 ℃ below 680 ℃ as the temperature range of pedestal 2.In addition, as the temperature range of spray header 10, preferred more than 350 ℃ below 500 ℃.In this Ti film film formation process, under the pedestal 2 when keeping formation high temperature pre-coating film and the state of temperature of spray header 10, wafer W is imported chamber 1 begin to handle.
Like this, when a plurality of wafer W being carried out continuously the processing of Ti film film forming, as mentioned above, in the precoating operation, as the upper strata, be formed with the high temperature pre-coating film that forms under the temperature same with Ti film film formation process the time, therefore, in Ti film film formation process, the film that is coated on pedestal 2 and spray header 10 has and equal membranous of high temperature pre-coating film, by applying membranous different film, the phenomenon of the thickness drift of Ti film can not take place, can suppress deviation between the face of thickness.
The preferred condition of Ti film film formation process is as follows.
(1) deposit of Ti film
I) from the High frequency power of high frequency electric source 34
Frequency: 300kHz～27MHz
Power: 100～1500W
Ii) TiCl
4Gas flow: 1～20mL/min (sccm)
Iii) Ar gas flow: 100～2000mL/min (sccm)
Iv) H
2Gas flow: 250～5000mL/min (sccm)
V) cavity indoor pressure: 400～1333Pa (3～10Torr)
(2) nitriding treatment
I) from the High frequency power of high frequency electric source 34
Frequency: 300kHz～27MHz
Power: 100～1500W
Ii) NH
3Gas flow: 100～2000mL/min (sccm)
Iii) Ar gas flow: 100～2000mL/min (sccm)
Iv) H
2Gas flow: 250～5000mL/min (sccm)
V) cavity indoor pressure: 400～1333Pa (3～10Torr)
Below, the dry-cleaning operation of operation 3 is described.
In this operation, after the above-mentioned Ti film film forming, in chamber, do not exist under the state of wafer, ClF
3Gas imports in the chamber 1, dry-cleans.The limit is by 2 heating of 5 pairs of pedestals of well heater, and dry-clean on the limit, and the temperature of the pedestal 2 of this moment is preferably set to 170～250 ℃.Like this, by under lower temperature, cleaning, can suppress ClF
3The reaction of the AlN of gas and formation pedestal 2 can reduce the AlF class substance A lF that is formed at pedestal 2
xAmount.Preferred 150～250 ℃ of the temperature of spray header 10.In addition, in matting, remove ClF
3In addition, can also use NF
3, F
2Deng outside fluorine type gas.
Below, the typical temperature curve example of pedestal in the Ti film of present embodiment and spray header and existing temperature curve example compared to be described.Fig. 5 is the figure of the temperature curve of expression pedestal, and Fig. 6 is the figure of the temperature curve of expression spray header.In addition, among these two figure, for simplicity, represent from the dry-cleaning operation.
As shown in Figure 5, the temperature curve example of existing pedestal 2 is: after dry-cleaning operation under 200 ℃, be warmed up to 450 ℃, under this temperature, carry out the precoating operation and form pre-coating film, thereafter, the temperature of pedestal 2 is warmed up to 640 ℃, wafer W is imported in the chamber 1, carry out Ti film film formation process to regulation piece number, thereafter, with pedestal 2 coolings.
Relative with it, the temperature curve example of the pedestal 2 of present embodiment is: after dry-cleaning operation under 200 ℃, form the precoating operation of following two-layer pre-coating film: be warmed up to 450 ℃, under this temperature, form the low temperature pre-coating film, temperature with pedestal 2 is warmed up to 640 ℃ again, form the high temperature pre-coating film, after this precoating operation, with the temperature maintenance of pedestal 2 under 640 ℃ state, wafer W is imported in the chamber 1, carry out Ti film film formation process to the wafer W of regulation piece number, thereafter, with pedestal 2 coolings.
In addition, no matter the temperature of spray header 10 is prior art or present embodiment as shown in Figure 6, all in the dry-cleaning operation, be set at 250 ℃, thereafter, be warmed up to the arbitrary temp (among Fig. 6 being 400 ℃) in 400～500 ℃, precoating operation and Ti film film formation process are all implemented under same temperature.
Below, the experiment of having confirmed effect of the present invention is described.
At this, with the temperature curve the sort of existing and of the present invention shown in Fig. 5,6 dry-clean, precoating, 500 pieces of wafers are repeated Ti film film forming.The surface is formed with the silicon wafer of oxide film and the silicon wafer of exposed (bare) state carries out this processing.The oxide film wafer is measured the resistance value and the thickness of the 1st piece, the 8th piece, the 16th piece Ti film, nude film is measured the resistance value and the thickness of the 2nd piece, the 9th piece, the 17th piece Ti film.With the table 1 that the results are shown in of oxide film wafer, with the table 2 that the results are shown in of nude film.In addition, grasped the membranous difference of the high temperature pre-coating film of 450 ℃ low temperature pre-coating film and 640 ℃.It is the results are shown in table 3.
[table 1]
[table 2]
[table 3]
| ??Ti(atm％) | ??N(atm％) | ??Cl(atm％) | |
| The low temperature pre-coating film | ??48 | ??48 | ??4 |
| The high temperature pre-coating film | ??47.8 | ??50.9 | ??1.3 |
Shown in table 1,2, carry out according to the present invention in the example of the present invention of low temperature precoating and high temperature precoating, no matter how confirmed counterdie, deviation has all had significantly improvement than existing situation of carrying out the low temperature precoating between the face of resistance value and thickness.
In addition, as shown in table 3, confirmed the Cl concentration difference of low temperature pre-coating film and high temperature pre-coating film, membranous have a difference.As shown in table 1, only carry out in the existing method of low temperature precoating, at the Ti film film forming initial stage, find to have particulate to produce, this be as shown in table 3 in the high low temperature pre-coating film of Cl concentration because of the Cl in the film move to the surface produce small film peel off cause.Relative with it, on the low temperature pre-coating film, be formed with among the present invention of the low high temperature pre-coating film of Cl concentration, confirmed that the Cl amount that moves to the surface is few, the generation of particulate is also few.
In addition, the present invention is not limited to above-mentioned embodiment, can carry out all distortion.For example, in the above-mentioned embodiment, to showing the situation that applies the present invention to film forming Ti film, but the present invention is not limited to this, also applicable to other the film forming of Ti class film such as TiN film.In addition, as processed substrate, being not limited to semiconductor wafer, for example also can be other substrates such as liquid crystal indicator (LCD) substrate, glass substrate, ceramic substrate.
Claims (12)
1. the film of a Ti class film, the gas ejection parts that use comprises the chamber of accommodating handled object, ejection comprises the processing gas that contains Ti gas and purge gas in described chamber, in described chamber the mounting table of mounting handled object and the device of heating unit that heats described mounting table at the surface filming Ti of handled object class film, it is characterized in that
Comprise:
Do not exist on the described mounting table under the state of handled object, utilize described heating unit to heat described mounting table, and in described chamber, spray described processing gas from described gas ejection parts, form the operation of pre-coating film at least on the surface of described gas ejection parts;
Thereafter, mounting handled object on the described mounting table of the state after being heated by described heating unit is supplied with described processing gas, the operation of a plurality of handled objects being carried out the processing of film forming Ti class film on handled object in described chamber; With
Not existing on the described mounting table under the state of handled object, in described chamber, import purge gas, to the operation of cleaning in the described chamber,
Carry out above-mentioned these operations successively repeatedly,
Wherein, in forming the operation of described pre-coating film, the low temperature of temperature when making the temperature of described mounting table become than described film formation process and forming after the low temperature pre-coating film under the temperature when described film formation process, forms the high temperature pre-coating film.
2. the film of Ti class film as claimed in claim 1 is characterized in that described mounting table is made of AlN.
3. the film of Ti class film as claimed in claim 2 is characterized in that, described gas ejection parts constitute by containing the Ni material on the surface at least.
4. as the film of each described Ti class film in the claim 1～3, it is characterized in that, the temperature of the described mounting table when forming described low temperature pre-coating film is more than 350 ℃ and 550 ℃ of less thaies, when forming described high temperature pre-coating film and the temperature of the described mounting table during the described Ti class of film forming film be more than 550 ℃ and below 680 ℃.
5. as the film of each described Ti class film in the claim 1～3, it is characterized in that, when forming described pre-coating film and the temperature of the described gas ejection parts during the described Ti class of film forming film be more than 350 ℃ and below 500 ℃.
6. as the film of each described Ti class film in the claim 1～3, it is characterized in that described pre-coating film and the utilization of described Ti class film contain Ti gas and reducing gas forms.
7. as the film of each described Ti class film in the claim 1～3, it is characterized in that the film forming of described pre-coating film contains Ti gas and reducing gas carries out by alternately supplying with.
8. as the film of each described Ti class film in the claim 1～3, it is characterized in that the film forming of described pre-coating film comprises the nitriding treatment of pre-coating film.
9. as the film of each described Ti class film in the claim 1～3, it is characterized in that described Ti class film is the Ti film.
10. the film of Ti class film as claimed in claim 9 is characterized in that, described processing gas comprises TiCl
4Gas and H
2Gas.
11. the film of Ti class film as claimed in claim 9 is characterized in that, after the operation of the described Ti class of film forming film finishes, the Ti film is implemented nitriding treatment.
12. the film as each described Ti class film in the claim 1～3 is characterized in that, described gas ejection parts are the spray headers that are provided with and are formed with a plurality of gas squit holes with described mounting table mutually opposed to each other.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2008235284 | 2008-09-12 | ||
| JP2008-235284 | 2008-09-12 | ||
| JP2008235284A JP2010065309A (en) | 2008-09-12 | 2008-09-12 | Film forming method of ti type film and storage medium thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101671813A true CN101671813A (en) | 2010-03-17 |
| CN101671813B CN101671813B (en) | 2012-02-08 |
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|---|---|---|---|
| CN2009101733117A Expired - Fee Related CN101671813B (en) | 2008-09-12 | 2009-09-02 | Film forming method of ti-series film |
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|---|---|
| JP (1) | JP2010065309A (en) |
| KR (1) | KR20100031460A (en) |
| CN (1) | CN101671813B (en) |
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| CN104821267A (en) * | 2014-01-31 | 2015-08-05 | 株式会社日立国际电气 | Substrate processing apparatus and method of manufacturing semiconductor device |
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| JP5698043B2 (en) | 2010-08-04 | 2015-04-08 | 株式会社ニューフレアテクノロジー | Semiconductor manufacturing equipment |
| JP5690219B2 (en) * | 2011-06-03 | 2015-03-25 | 株式会社日立国際電気 | Semiconductor device manufacturing method and substrate processing apparatus |
| JP6219179B2 (en) * | 2014-01-20 | 2017-10-25 | 東京エレクトロン株式会社 | Plasma processing equipment |
| JP6597740B2 (en) | 2017-08-30 | 2019-10-30 | 東京エレクトロン株式会社 | Film forming method and film forming apparatus |
| JP6917315B2 (en) * | 2018-01-15 | 2021-08-11 | 東京エレクトロン株式会社 | Precoating method and film forming method |
| JP2021038452A (en) | 2019-09-05 | 2021-03-11 | 東京エレクトロン株式会社 | Plasma treatment apparatus and control method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5140957B2 (en) * | 2005-12-27 | 2013-02-13 | 東京エレクトロン株式会社 | Deposition equipment |
| KR101139165B1 (en) * | 2006-10-19 | 2012-04-26 | 도쿄엘렉트론가부시키가이샤 | Ti FILM FORMING METHOD AND STORAGE MEDIUM |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104821267A (en) * | 2014-01-31 | 2015-08-05 | 株式会社日立国际电气 | Substrate processing apparatus and method of manufacturing semiconductor device |
| CN104821267B (en) * | 2014-01-31 | 2017-08-04 | 株式会社日立国际电气 | The manufacture method of lining processor and semiconductor devices |
Also Published As
| Publication number | Publication date |
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| KR20100031460A (en) | 2010-03-22 |
| JP2010065309A (en) | 2010-03-25 |
| CN101671813B (en) | 2012-02-08 |
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