CN102345111A - Film forming method and apparatus - Google Patents
Film forming method and apparatus Download PDFInfo
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- CN102345111A CN102345111A CN2011102170380A CN201110217038A CN102345111A CN 102345111 A CN102345111 A CN 102345111A CN 2011102170380 A CN2011102170380 A CN 2011102170380A CN 201110217038 A CN201110217038 A CN 201110217038A CN 102345111 A CN102345111 A CN 102345111A
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Abstract
The invention provides a method which utilizes a film forming apparatus to form a film made of silicon oxide film upon a to-be-processed object. Further provided is a film forming apparatus. The film forming apparatus comprises a processing container, a raw material gas feeding system having a first open-and-close valve capable of feeding raw material gas inside the processing container, a reactive gas feeding system having a second open-and-close valve capable of feeding the reactive gas inside the processing container, and a vacuum venting system having a third open-and-close valve capable of venting the atmosphere gas out the processing container to form vacuum. The adsorption process and the reaction process have multiple alternations amid intervals. The adsorption process comprises the steps of: closing the third open-and-close valve, opening the first open-and-close valve in specified period to feed raw material gas to the processing container, and closing the first open-and-close valve to keep the state regulation period, thus to make the raw material gas be attached to the surface of the to-be-processed object. The reaction process comprises the steps of opening the second open-and-close valve, and feeding reactive gas to the processing container, thus to make the reactive gas and the raw material gas react to form the film.
Description
Technical field
The present invention relates to film and film deposition system that silicon oxide film is piled up on handled object surfaces such as semiconductor crystal wafer.
Background technology
Generally speaking, in order to make semiconductor integrated circuit, the semiconductor crystal wafer that formed by silicon substrate etc. (below be called wafer) is carried out various processing such as film forming processing, etch processes, oxide treatment, DIFFUSION TREATMENT, upgrading processing.For example film forming is handled in the film deposition system of film deposition system at patent documentation 1 disclosed one chip, patent documentation 2 disclosed batch types and is carried out.As shown in Figure 1, the film deposition system of batch type comprises: the processing vessel 2 of longitudinal type; Be housed in the processing vessel 2, be used for the multilayer twelve Earthly Branches and make brilliant boat 4 into a plurality of wafer W of handled object; In processing vessel 2, extend along the short transverse of processing vessel 2, and be used for dispersing nozzle 8,10 towards brilliant boat 4 base feed gases; Be formed on the venting port 12 of the bottom of processing vessel 2; 12 that be connected via pressure-regulating valve 14B and venting port, as to comprise vacuum pump 16 vacuum evacuating system 14; And the heating part 6 that centers on processing vessel 2.
And, in the film deposition system of Fig. 1, for example forming under the situation of silicon oxide film, the brilliant boat 4 that is used to support a plurality of wafer W is accommodated in the processing vessel 2, and the temperature that wafer W is heated to regulation by heating part 6 is for example about 600 ℃.From the for example silicon unstripped gas that gas supply part 7 is supplied with as unstripped gas to dispersing nozzle 8, a plurality of gas jetting hole 8A that are provided with from the length direction along dispersing nozzle 8 supply with silicon unstripped gas towards wafer W.In addition, supply with the for example ozone gas as reactant gases from gas supply part 7 to dispersing nozzle 10, a plurality of gas jetting hole 10A that are provided with from the length direction along dispersing nozzle 10 are towards wafer W ozone supply gas.On the other hand, exhaust is carried out by vacuum evacuating system 14 in the inside of processing vessel 2, is maintained at the pressure of regulation.Silicon unstripped gas and ozone gas react, and on wafer W, piling up has silicon oxide film.
In addition; Sometimes adopt following film; Promptly; Through open and close valve 8B and the open and close valve 10B that alternately opens and closes gas supply part 7; Come alternately to supply with repeatedly the unstripped gas that contains Si and as the ozone gas of oxidizing gas; The unstripped gas that contains Si and the ozone gas that are adsorbed on the wafer are reacted, form silicon oxide film.This film has formed membranous better, even and also can the such advantage of film forming under cold condition.
Patent documentation 1: japanese kokai publication hei 09-077593 communique
Patent documentation 2: TOHKEMY 2009-246318 communique
Patent documentation 3: TOHKEMY 2006-054432 communique
In addition, in the manufacturing process of semiconducter device, carry out in order to construct Wiring structure etc. sometimes as the film laminated that contains metal of wiring as the such operation of the above-mentioned silicon oxide film of insulating film.When carrying out above-mentioned operation; In preceding operation, on wafers such as silicon substrate, form as the for example tungsten film of the film that contains metal etc.; This wafer is exposed in the normal atmosphere atmosphere in the dust free chamber (clean room) ground and carries, or is incorporated in the conveying container of the non-active gas atmosphere that is closed with cleaning ground and carries.
At this moment; React as the surface of the tungsten film of the above-mentioned film that contains metal and oxygen, the moisture in the cleaning atmosphere gas in the dust free chamber; Or react, thereby can be on this tungsten film surface form metal oxide film naturally with as thin as a wafer thickness with oxygen, moisture that trace in conveying container exists.
Because this metal oxide film that forms naturally becomes the reason of the electrical specification variation that makes semiconducter device; So suppress this metal oxide film thickness increase or remove this metal oxide film; Though it is good to remove this metal oxide film; But it is not correspondingly can increase process number, so preferred with the operation of removing this metal oxide film.Therefore, in the past, generally speaking, do not remove metal oxide film and directly on this metal oxide film, formed silicon oxide film with the CVD method of above-mentioned that kind.
On the other hand; Merely using under the situation of the range upon range of silicon oxide film of CVD method of usefulness in the past; Because oxidizing gas as a side film forming gas; Produce the phenomenon of the thickness increase of metal oxide film on the contrary; Its result can produce the electrical specification that makes semiconducter device and reduce such problem (for example patent documentation 3) significantly.Particularly during this metal oxide film thickening, electrical specification is further reduced, also exist because of formed needle crystal to produce the such problem of shape defect.
Summary of the invention
The present invention provides a kind of according to above-mentioned situation can suppress the film and the film deposition system of this thickness through the thickness of control metal oxide film, and this metal oxide film is present in the interface between the film that contains metal of substrate of the film that is made up of silicon oxide film and this film.
The inventor concentrates on studies to the formation of silicon oxide film; Its result; The increase of thickness of having found metal oxide film is relevant with the diffusion as the ozone of reactant gases; And the opinion below having obtained; Thereby accomplished the present invention, this opinion does, through in the absorption process of absorption unstripped gas, unstripped gas being enclosed in the processing vessel; Can make a large amount of unstripped gas be adsorbed on crystal column surface, can suppress the influence that ozone brings thus.
According to the 1st technical scheme of the present invention; A kind of film that uses film deposition system on handled object, to form the film that is made up of silicon oxide film is provided; The surface of this handled object is formed with the film that contains metal; This film deposition system comprises: the unstripped gas plenum system; It has the 1st open and close valve, can be in above-mentioned processing vessel base feed gas; The reactant gases plenum system, it has the 2nd open and close valve, can be in above-mentioned processing vessel supply response gas; Vacuum evacuating system, it has the 3rd open and close valve, the atmosphere in the above-mentioned processing vessel can be lined up vacuum.In this film; Between absorption process and reaction process, there are off period ground alternate repetition repeatedly this absorption process and reaction process; This absorption process does; Close above-mentioned the 3rd open and close valve of above-mentioned vacuum evacuating system; Open the 1st specified time limit of above-mentioned the 1st open and close valve of above-mentioned raw materials gas supply system; After above-mentioned processing vessel is supplied with above-mentioned raw materials gas; Close the 1st open and close valve; Keeping above-mentioned the 1st open and close valve to close under the state of the 2nd specified time limit, making the interior above-mentioned raw materials gas adsorption of above-mentioned processing vessel in the surface of above-mentioned handled object; This reaction process does, opens above-mentioned the 2nd open and close valve of above-mentioned reactant gases plenum system, in above-mentioned processing vessel, supplies with above-mentioned reactant gases, above-mentioned reactant gases and above-mentioned raw materials gas are reacted and forms film.
According to the 2nd technical scheme of the present invention, a kind of film deposition system is provided, it comprises: processing vessel, it can accommodate handled object; Maintaining part, it is used to keep above-mentioned handled object; The heating part, it is used to heat above-mentioned handled object; The unstripped gas plenum system, it has open and close valve, can be in above-mentioned processing vessel base feed gas; The reactant gases plenum system, it has open and close valve, can be in above-mentioned processing vessel supply response gas; Vacuum evacuating system, it has open and close valve, the atmosphere in the above-mentioned processing vessel can be lined up vacuum; Apparatus control portion, its control device integral body make the whole film of carrying out the 1st technical scheme of this device.
Description of drawings
Enroll in this specification sheets and to constitute its a part of accompanying drawing and represent embodiment of the present invention, together play the effect that principle of the present invention is described with the detailed description of above-mentioned bright and following in general embodiment.
Fig. 1 is the synoptic chart of film deposition system of the batch type of expression corresponding technology.
Fig. 2 is the pie graph of the film deposition system of expression embodiment of the present invention.
Fig. 3 is the graphic representation of the action of each valve of expression when carrying out the film of embodiment of the present invention.
Fig. 4 is the amplification view of expression with the cross section of the formed multilayer film of film of embodiment of the present invention.
Fig. 5 be during the maintenance of expression unstripped gas with the graphic representation of the relation of per 1 round-robin rate of film build.
Fig. 6 is the graphic representation of relation of thickness of the metal oxide film of expression per 1 round-robin rate of film build and tungsten.
Fig. 7 is used to illustrate that the film that contains metal contains the figure of the oxidized reason of film and the near interface between the silicon oxide film of metal at this.
Fig. 8 is the graphic representation of relation of thickness of the metal oxide film of expression per 1 round-robin rate of film build and titanium nitride film.
Embodiment
Film according to the embodiment of the present invention and film deposition system; Can suppress this thickness through the thickness of control metal oxide film, this metal oxide film is present in the interface between the film that contains metal of substrate of the film that is made up of silicon oxide film and this film.Its result can prevent the reduction of electrical specification through the thickness that suppresses above-mentioned metal oxide film, and can also prevent the generation of shape defect.
Below, based on the film and the film deposition system of detailed description of the drawings embodiment of the present invention.Fig. 2 is the pie graph of an example of the film deposition system of expression embodiment of the present invention, and Fig. 3 is the graphic representation of the action of each open and close valve of expression when carrying out the film of embodiment of the present invention.
Here, be that example describes with following situation, that is: as unstripped gas, use as 3DMAS (Tris (dimethylamino) silane:SiH (N (CH that contains the organic raw material of Si
3)
2)
3), use ozone as reactant gases as oxidizing gas, form silicon oxide (SiO as film
2) film.
As shown in Figure 2, this film deposition system 20 has and can accommodate many processing vessels 22 as the semiconductor crystal wafer W of handled object.This processing vessel 22 has the dual pipe structure that the urceolus 26 by inner core of lengthwise 24 and lengthwise constitutes, and this inner core 24 is the cylindrical shape that the top is arranged; This urceolus 26 is the cylindrical shape that the top is arranged.Urceolus 26 with the mode at the interval that between the interior week of the periphery of inner core 24 and urceolus 26, is separated with regulation around inner core 24.
Above-mentioned inner core 24 forms underpart opening with urceolus 26 by quartz.For example accommodating under the situation of wafer W that diameter is 300mm, the diameter of processing vessel 22 is about 400～500mm.The internal capacity of processing vessel 22 depends on the number of accommodating of wafer W, and under the situation of for example accommodating maximum about 150 wafer W, is about 200 liters.
In the bottom of urceolus 26, be connected with the manifold (manifold) 28 of for example stainless steel airtightly by containment members 30 such as O RunddichtringOs with cylindrical shape, utilize the bottom of these manifold 28 supporting urceolus 26.In addition, this manifold 28 is supported by not shown pedestal (Baseplate).And be provided with at the inwall of manifold 28 and have annular supporting station 32, utilize the bottom of these supporting station 32 supporting inner cores 24.
In the inner core 24 of processing vessel 22, contain brilliant boat 34 as the wafer maintaining part.Spacing with regulation in brilliant boat 34 keeps a plurality of wafer W as handled object.In this embodiment, utilize brilliant boat 34 with roughly equidistantly multilayer ground keep diameter be 300mm, the wafer W about 50～100 for example.Brilliant boat 34 can go up and down as described in the back, through the lower openings of manifold 28, accommodates in the inner core 24 from the below of processing vessel 22, takes out from inner core 24.Brilliant boat 34 is for example made by quartz.
In addition, when brilliant boat 34 is accommodated, as the lower openings of the manifold 28 of the lower end of processing vessel 22 by cap 36 sealings that for example constitute by quartzy, stainless steel plate.In order to keep stopping property, between the bottom of processing vessel 22 and cap 36, be folded with for example containment member 38 such as O RunddichtringO.Brilliant boat 34 is carried to put carrying across the heat-preservation cylinder 40 of quartz system to be put on the platform 42, puts platform 42 this year and is rotated a upper end of spools 44 and supports, and this turning axle 44 runs through the cap 36 of the lower ending opening that is used to open and close manifold 28.
Between hole and turning axle 44 that the confession turning axle 44 of cap 36 runs through, for example be provided with magnetic fluid seal spare 46, turning axle 44 is by sealing airtightly and can be supported rotatably thus.Turning axle 44 is installed in the front end of the arm 50 on the hoisting appliances 48 such as being supported in boat elevator for example, and brilliant boat 34 is gone up and down with cap 36 grades integratedly.In addition, also can put platform 42 and be fixedly arranged at cap 36 sides, not make brilliant boat 34 rotatably wafer W carried out film forming and handle carrying.
Sidepiece at processing vessel 22 is provided with the heating part 52 that constitutes around the well heater of for example being made by carbon filament (carbon wire) of processing vessel 22, thus, is arranged in the processing vessel 22 of these 52 inboards, heating part and the wafer W of this processing vessel 22 and is heated.And, in manifold 28, be provided with unstripped gas plenum system 54, the reactant gases plenum system 56 that is used for supply response gas that is used for base feed gas and be used to supply with sweeping gas plenum system 58 as the non-active gas of sweeping gas.
Particularly, unstripped gas plenum system 54 has gas jet 60, and this gas jet 60 is made up of quartz, has the L word shape, installs with the mode of the inboard that extends through manifold 28 airtightly.Extend in this gas jet 60 whole zone along short transverse in inner core 24, is formed with a plurality of gas jetting hole 60A with the spacing of stipulating, can be from laterally to being bearing in each the wafer W base feed gas on the brilliant boat 34.On gas jet 60, be connected with gas passage 62.
In gas passage 62, be provided with successively as mass flow controller flow director 62A be used for the beginning of gas communication and stop the open and close valve 62B of (blocking); Therefore, on one side can be as required on one side the flow of pilot-gas nozzle 60 make the unstripped gas circulation, stop.As unstripped gas, as above-mentioned, use the 3DMAS that contains Si here.3DMAS as this liquid starting material is gasified by gasifier 63, is carried by vector gas.Particularly, through temperature with gasifier 63 adjustment 3DMAS, the vapour pressure of control 3DMAS, the amount of the 3DMAS that control will be gasified.As carrier gas physical efficiency N
2The non-active gas of rare gas such as gas and Ar, He etc.In addition, also can carry the 3DMAS gas gasified without vector gas ground.
In this embodiment, as the gasifier of gasifier 63 use baking (baking) modes.This gasifier has the material container 63T and the well heater 63A that is used for heating raw container 63T that is used to store 3DMAS, makes the 3DMAS gasification through the 3DMAS in the heating raw container, directly in processing vessel 22, imports gasification 3DMAS gas.In this case, without vector gas.In gasifier 63, also be provided with pressure warning unit 63B, the temperature of control 3DMAS makes the vapour pressure of 3DMAS be higher than the pressure in the processing vessel 22.This control utilizes not shown temperature regulator to carry out.
In addition, as gasifier 63, also can use the gasifier of injection (injection) mode.In this gasifier; In processing vessel 22, supply with when gasifying 3DMAS gas in order to make stability of flow; Need about 5～10 seconds discharge unstripped gases, so have to waste the organo metallic material gas of high price with in processing vessel 22, not feeding unstripped gas.Thereby, from the preferred gasifier that uses roasting mode of the effective viewpoint of utilizing of raw material.
In addition, reactant gases plenum system 56 has gas jet 64, and this gas jet 64 is made up of quartz, has the L word shape, installs with the mode of the inboard that extends through manifold 28 airtightly.Extend in this gas jet 64 whole zone along short transverse in inner core 24, is formed with a plurality of gas jetting hole 64A with the spacing of stipulating, can be from laterally to being bearing in each the wafer W supply response gas on the brilliant boat 34.On gas jet 64, be connected with gas passage 66.In gas passage 66, be provided with successively as mass flow controller flow director 66A be used for the beginning of gas communication and stop the open and close valve 66B of (blocking); Therefore, on one side can be as required on one side the flow of pilot-gas nozzle 64 make the reactant gases circulation, stop.Here, as reactant gases, as above-mentioned with ozone (O
3).
And sweeping gas plenum system 58 has gas jet 68, and this gas jet 68 is made up of quartz, has the L word shape, installs with the mode of the inboard that extends through manifold 28 airtightly.Extend in this gas jet 68 whole zone along short transverse in inner core 24, is formed with a plurality of gas jetting hole 68A with the spacing of stipulating, can be from laterally each the wafer W that is bearing on the brilliant boat 34 being supplied with sweeping gas.On gas jet 68, be connected with gas passage 70.In gas passage 70, be provided with successively as mass flow controller flow director 70A be used for the beginning of gas communication and stop the open and close valve 70B of (blocking); Therefore, on one side can be as required on one side the flow of pilot-gas nozzle 68 make the sweeping gas circulation, stop.In this embodiment,, as above-mentioned, use nitrogen as sweeping gas.In other the embodiment,, also can use rare gas place of nitrogen such as Ar, He as sweeping gas.
And; Each gas jet 60,64,68 concentrates a side that is arranged in the inner core 24 (in illustrative example; Because spatial relation; Gas jet 68 is illustrated in a side opposite with other gas jet 60,64); On the sidewall relative of inner core 24, be formed with the bigger a plurality of gas stream through holes 72 of diameter along above-below direction with this each gas jet 60,64,68 with arranging.Therefore, quilt is supplied with the gas that comes from gas jet 60,64,68 mobile from process along continuous straight runs between the wafer, the gap 74 that process gas stream through hole 72 is directed between inner core 24 and the urceolus 26.
And, in the upper side of manifold 28, be formed with inner core 24 and urceolus 26 between the venting port 76 that is connected of gap 74, be provided with the vacuum evacuating system 78 that is used for processing vessel 22 is carried out vacuum exhaust at these venting port 76 places.Particularly; Vacuum evacuating system 78 has the exhaust channel 80 that is connected with venting port 76; Be provided with open and close valve 80B and vacuum pump 82 midway successively at exhaust channel 80; Can carry out the pressure adjustment to the atmosphere in the processing vessel 22 on one side and carry out vacuum exhaust on one side; The aperture of the spool of this open and close valve 80B can be adjusted, through the pressure in the aperture adjustment processing vessel 22 that changes this spool.The spool of being located at the open and close valve 80B of exhaust channel 80 can adjustment at random in the scope from the fully open position to the full close position.And, be under the situation of full cut-off at spool, fully blocked by open and close valve 80B from the gas of processing vessel 22.
In addition, has the apparatus control portion 84 that for example constitutes in order to be controlled to film device 20 whole actions by computer.Use device control part 84, the on-off action in beginning and the aperture of spool that stops, comprising the open and close valve 80B of vacuum evacuating system 78 of controlling the supply of each gas is adjusted at, operation pressure, film-forming temperature etc. are implemented film forming and are handled in film deposition system 20.Carry out the computer program that is used to be controlled to film device 20 molar behaviors through use device control part 84 and carry out such control.Such computer program is stored in the storage media 86, is loaded (load) in apparatus control portion 84.As storage media 86, can be with floppy disk, CD (Compact Disc), hard disk, flash memory or DVD etc.
Then, with reference to Fig. 4～Fig. 7 film deposition system 20 films that carry out, embodiment of the present invention of using formation as above are described.Fig. 4 is the amplification view of expression with the cross section of the multilayer film of this film formation; Fig. 5 be during the maintenance (hold) of expression unstripped gas with the graphic representation of the relation of per 1 round-robin rate of film build; Fig. 6 is the graphic representation of relation of the thickness of expression per 1 round-robin rate of film build and metal oxide film, and Fig. 7 is the figure that is used to illustrate the reason that the near interface of film between film that contains metal and silicon oxide film that contain metal is oxidized.As above-mentioned, below Shuo Ming action is carried out based on being stored in the program in the storage media 86.
And in following explanation, wafer W for example can be a Silicon Wafer, in its surface, in preceding operation, forms as the for example tungsten film that contains the film of metal.This wafer W is housed in the conveying container, and the film deposition system in the operation is transported to film deposition system 20 in the past.At this moment, the inner atmosphere of conveying container be maintained at dust free chamber in the identical air atmosphere of atmosphere or the non-active gas atmosphere of cleaning.And the tungsten film surface is exposed under oxygen in the air atmosphere in the dust free chamber, the moisture, or is exposed under oxygen in the non-active gas atmosphere that trace is present in cleaning, the moisture.Its result is formed with the native metal oxide film on the tungsten film surface with as thin as a wafer thickness.
In addition, at this moment, the temperature in the processing vessel 22 is maintained at the temperature lower and higher than normal temperature than film-forming temperature.
Then, the vacuum pump 82 of vacuum evacuating system 78 starts, and will line up vacuum in the processing vessel 22, and utilizes open and close valve 80B, makes processing vessel 22 interior pressure maintain the operation pressure of regulation.In the film process, vacuum pump 82 and open and close valve 80B are by continuous drive.
In addition,, wafer W is heated to film-forming temperature and is stable at this temperature through increasing to heating part 52 supply capabilities, afterwards, as such shown in following, to carry out film forming handle required predetermined process gas carry out flow control on one side carry out film forming handle on one side.
That is, supply with as the 3DMAS gas that contains Si gas, from gas jet 64 ozone supplies of reactant gases plenum system 56 from the gas jet 60 of unstripped gas plenum system 54.And the N that supplies with as sweeping gas from the gas jet of sweeping gas plenum system 58 68
2Gas.
Each gas along continuous straight runs of being supplied with multilayer be bearing between the wafer on the brilliant boat 34 and flow, through flowing into the gap 74 between inner core 24 and the urceolus 26 at the gas stream through hole 72 of opposition side.Afterwards, these gases are discharged from the venting port 76 of the lower end of being located at urceolus 26 by vacuum evacuating system 78.
Then, on one side with reference to Fig. 3 the situation of the supply of each gas is described particularly on one side.As above-mentioned, here unstripped gas and reactant gases are alternately supplied with repeatedly.The on-off action of the open and close valve 62B of (A) expression unstripped gas of Fig. 3, the on-off action of the open and close valve 66B of (B) expression reactant gases of Fig. 3, the on-off action (aperture of spool) of the open and close valve 80B of (C) expression vacuum evacuating system of Fig. 3.
That is, alternately carry out repeatedly each following operation successively repeatedly, form film; This each operation comprises: absorption process, shown in Fig. 3 (A), open unstripped gas open and close valve 62B regulation during; Temporarily supply with the unstripped gas that contains Si, make unstripped gas be adsorbed in wafer W surface; Deairing step stops the supply of unstripped gas, and the atmosphere gas in the processing vessel 22 is carried out exhaust; Reaction process, shown in Fig. 3 (B), the open and close valve 66B that opens reactant gases supplies with the ozone as reactant gases, and ozone and the unstripped gas that is adsorbed on the crystal column surface are reacted, and forms the thin SiO of thickness
2Film; Deairing step, the supply of stopped reaction gas is carried out exhaust to the atmosphere gas in the processing vessel 22.
At this, be 1 circulation during from 1 absorption process to next absorption process, in 1 circulation, as above-mentioned, form extremely thin (1 molecular layer or several molecule layer degree) film.The time T 1 of the absorption process in 1 circulation and the time T 2 of reaction process are about 60sec, and the time T 3 of preceding half the deairing step in 1 circulation is respectively about 10sec with the time T 4 of later half deairing step.In addition, in each deairing step, also can supply with the N2 sweeping gas simultaneously.Its result forms film as shown in Figure 4.That is, film forming shown in Fig. 4 (A), is formed with the film that contains metal 100 that for example is made up of tungsten film on wafer W surface before handling, and contains film 100 surfaces of metal at this, as above-mentioned, in wafer is carried, forms native metal oxide film 102.In this embodiment, be tungsten film owing to contain the film 100 of metal, so metal oxide film 102 for example is WOx (x: positive integer).After film forming is handled, shown in Fig. 4 (B), on metal oxide film 102, form the film 104 that constitutes by silicon oxide film.At this moment, as described in the back, unstripped gas is remained in the processing vessel 22 hermetically ability reducing metal oxide film 102, the thickness of control metal oxide film 102.
Here; In the film of this embodiment; Be not base feed gas all in the whole process of absorption process; But shown in Fig. 3 (A); Only in absorption process initial the 1st specified time limit t1 open open and close valve 62B, make the unstripped gas circulation, afterwards; Close open and close valve 62B, place the 2nd specified time limit h.And, shown in Fig. 3 (C), in the whole process of absorption process T1, all close the open and close valve 80B of vacuum evacuating system.Unstripped gas is only in initial t1 circulation the 1st specified time limit, after processing the 2nd specified time limit h, the open and close valve 62B of unstripped gas and the open and close valve 80B of vacuum evacuating system all are closed, so unstripped gas is closed (delay) in processing vessel 22.Its result is that metal oxide film 102 surface adsorption have a large amount of unstripped gases on wafer W surface.At this moment, as described in the back,, can control the thickness of above-mentioned metal oxide film 102 through adjusting the length of (below be also referred to as " during the maintenance ") h the 2nd specified time limit.
The flow of the unstripped gas among initial the 1st specified time limit t1 is about 10～500sccm.In addition, the pressure in the processing vessel of absorption process T1 22 initial sharply rise after, when having closed the open and close valve 62B of unstripped gas, become constantly, the pressure of this moment also depends on the feed rate with unstripped gas, for example is about 667Pa.
Then, after absorption process finishes, half deairing step T3 before getting into.That is, stopping under all gas condition of supplying, the open and close valve 80B of vacuum evacuating system is being placed standard-sized sheet, utilizing vacuum pump 82 promptly to discharge and remain in the gas in the processing vessel 22.In addition, in this case, also can supply with as the N2 gas of sweeping gas and promote the discharge of entrap bubble.Thus, the concentration of the unstripped gas (3DMAS) in the processing vessel 22 sharply reduces.
Then, get into reaction process T2., shown in Fig. 3 (B), open the open and close valve 66B of reactant gases here, during reaction process T2 whole in, supply with ozone as reactant gases.The open and close valve 80B of the vacuum evacuating system of this moment can standard-sized sheet, as long as the free air delivery of gas is enough, spool also can be the aperture below 100%, and for example the aperture of spool is constant in illustrative example is 50%.
In addition, at this moment, for example supply with the O of 6.5 per minute standard liters (slm) to ozonizer
2Produce 200g/Nm
3About ozone, supply with the reactant gases of the ozone contain this amount.Through the supply of ozone, react with the unstripped gas that is adsorbed on wafer W surface, formation constitutes film 104 by silicon oxide.In this case, in film in the past, ozone spreads in being adsorbed on the unstripped gas of crystal column surface, film 104, and the surface of the film that contains metal 100 of oxidation lower floor causes the thickness of metal oxide film 102 to increase.
But; In this embodiment; H during the maintenance of setting unstripped gas as above-mentioned; Make unstripped gas suitably be adsorbed in crystal column surface; So the diffusion of ozone is suppressed; Can suppress the increase of metal oxide film 102, moreover, can also utilize on the contrary that the length of h reduces the thickness of metal oxide film 102 during the maintenance.
Like this, reaction process T2 gets into later half deairing step T4 after finishing.That is, stop the supply of all gas and the open and close valve 80B of vacuum evacuating system is changed to standard-sized sheet, utilize vacuum pump 82 promptly to discharge and remain in the gas in the processing vessel 22.In addition, in this case, also can supply with N as sweeping gas
2Gas and promote the discharge of entrap bubble.Thus, 1 round-robin film formation process finishes, and repeated multiple times is carried out 1 each operation of round-robin as required, can access the film with required thickness, the film 104 that promptly is made up of silicon oxide.In addition, during film forming was handled, operation pressure is maintained at from the basis pressed (base pressure) (for example about 13.3Pa) in the scope of 133.3Pa.
As above-mentioned; According to this embodiment; In the absorption process T1 of base feed gas; Setting is together closed the open and close valve 80B of the open and close valve 62B of unstripped gas and vacuum evacuating system 78, unstripped gas is enclosed in the processing vessel 22 and h during the effusive maintenance in outside not; Make unstripped gas suitably be adsorbed in wafer W surface, so the thickness of the metal oxide film 102 that can suppress to be formed naturally.The length of h during particularly this keeps through adjustment can reducing metal oxide film 102, controls the thickness of this metal oxide film 102.Its result can suppress the thickness of metal oxide film 102, prevents the reduction of electrical specification, and can also prevent to produce shape defect.
Evaluation experimental and result thereof
Then, illustrate above-mentioned explanation, utilize the result of embodiment of the present invention to the evaluation experimental that film carried out.Fig. 5 be during expression keeps with the graphic representation of the relation of per 1 round-robin rate of film build, Fig. 6 is the graphic representation of relation of the thickness of expression per 1 round-robin rate of film build, the film surface of containing metal and metal oxide film.Here, between the time T 2 stuck-at-s～30sec of reaction process, between the 1st specified time limit t1 stuck-at-～30sec that the open and close valve 62B of unstripped gas opens.And the time T 1 through making absorption process changes, pent time of open and close valve 62B of unstripped gas in absorption process is promptly kept during h (=T1-t1) change.
In Fig. 5, during will keeping as transverse axis, with per 1 round-robin rate of film build as the longitudinal axis.And as unstripped gas, circulation contains the 3DMAS as the raw material of Si, as reactant gases and the ozone that circulates (oxygen that contains 10Vol% ozone).In addition, use tungsten film, with the Silicon Wafer of the metal oxide film 102 that has the tungsten that is formed naturally on this tungsten film surface as the film 100 that contains metal.Here, the total supply with 3DMAS is set at 1/4 of comparative example (condition in the past).Wafer temperature during film forming is 550 ℃, and operation pressure (maximum value) is 1.2kPa.And, do not set during the maintenance ground alternately base feed gas and reactant gases as comparative example, form silicon oxide film.Processing condition beyond the action of each open and close valve are the identical condition of situation with the film of this above-mentioned embodiment.That is, in this comparative example, the time of absorption process is 30sec, and the total supply of 3DMAS is 4 times of total supply of the film of this embodiment as above-mentioned.
Can know clearly that from Fig. 5 as this embodiment, make during the maintenance longly more in the scope of h about from 10sec to 115sec, per 1 round-robin rate of film build is straight more and becomes big linearly in the scope that is recycled to from 0.1nm/ about the 0.21nm/ circulation.This former because, h is long more during the maintenance, the unstripped gas that is adsorbed on wafer W surface increases more, its result, rate of film build is also high more.
In addition; As accessory effect; Can know under the condition in the past of supplying with X gram 3DMAS; Rate of film build is about the 0.13nm/ circulation; Yet, under the situation of the condition of this embodiment, though the amount of the raw material of being supplied with reduces to 1/4; But through during prolong keeping, rate of film build is roughly that straight line rises on the ground.And during the maintenance during for 40sec roughly, rate of film build is roughly the same with the situation of in the past condition.That is, here can know,,, still can access and the roughly equal or higher rate of film build of situation of in the past condition although then the total supply of raw material reduces to 1/4 if be set at more than the 40sec during will keeping.In other words, can know, cut down the total supply of raw material when can keep significantly with the equal rate of film build of in the past condition through as this embodiment, carrying out the operation of each open and close valve.
Then, measured metal oxide film (W0 with the corresponding tungsten of rate of film build
x) thickness.Its result is shown in Fig. 6.The thickness of metal oxide film is measured through XPS (x-ray photoelectron power spectrum).This metal oxide film is as above-mentioned, to be present in the film that contains metal 100 that is made up of tungsten and by silicon oxide (SiO
2) the metal oxide film (WO at interface between the film 104 that constitutes
x) 102.
Thickness initial value at the tungsten metal oxide film 102 that carries out being formed naturally before the film forming processing is 1.1nm.In addition, in Fig. 6, put down in writing keep during the representational value of h.Curve A among Fig. 6 is represented the characteristic of unstripped gas use 3DMAS when film-forming temperature is 550 ℃ of film forming.Clearly can know from Fig. 6; Under the little situation of rate of film build; The thickness of metal oxide film 102 becomes bigger than initial value; And; Along with rate of film build becomes big; The thickness of metal oxide film 102 sharply reduces, and rate of film build becomes the value roughly the same with initial value for the thickness of about 0.115nm/ circulation time metal oxide film 102.And when rate of film build further increased, the thickness of metal oxide film 102 reduced degree and slows down thereupon.
Like this, can know through h during the maintenance of adjustment unstripped gas rate of film build is changed, can control and be present in film 100 and the film (SiO that contains metal
2) the metal oxide film (W0 for example at interface between 104
x) 102 thickness.Can know particularly and circulate, can suppress the thickness of metal oxide film 102 and make the thickness of this metal oxide film 102 be reduced to this below initial value through rate of film build being set at more than or equal to 0.115nm/.In other words, can know for the thickness that makes metal oxide film 102 for this below initial film thickness, here, as long as the length of h is set at 23sec above (rate of film build: circulate more than or equal to 0.115nm/) during will keeping.
Here, per 1 round-robin rate of film build less than 0.115nm/ round-robin situation under, reason such as the following stated that the thickness of metal oxide film becomes thicker than initial value.Promptly; Shown in Fig. 7 (A); Under the few situation of the quantity of the molecule 1 10 of the unstripped gas of the silicon on the surface that is adsorbed in the metal oxide film 102 that is formed naturally film 100 surface of containing metal; The gap that molecule 1 is 10 is big, and the ozone 112 of Dao Ruing passes the gap easily and spreads shown in arrow labeled afterwards.Its result, easily the ozone of diffusion arrives metal oxide film 102 and the film 100 that contains metal in the gap, further oxidized metal oxide film 102 and the film 100 that contains metal, the thickness thickening of metal oxide film 102 itself.
Shown in Fig. 7 (B), when per 1 round-robin rate of film build increased, the quantity of molecule 1 10 that is adsorbed on the unstripped gas of the silicon on the metal oxide film 102 became many, the gap smaller that molecule 1 is 10.Its result, ozone 112 is difficult to pass the gap, thus inhibition contains the oxidation of the film 100 of metal.
In addition, rate of film build is more than or equal to the 0.115nm/ circulation time, reason such as the following stated that the Film Thickness Ratio initial value of metal oxide film 102 is little.That is, produce reductive action down because contain unstripped gas about 550 ℃ the film-forming temperature here of silicon itself, under reductive action so the metal oxide film 102 that is formed naturally is reduced.Its result, shown in Fig. 4 (A) thickness of the initial value of this such metal oxide film 102 after the film forming of film 104, shown in Fig. 4 (B), metal oxide film 102 attenuation.
According to The above results, be under the situation of 3DMAS in unstripped gas, preferably the film-forming temperature in each operation is more than 550 ℃, particularly for the thickness that makes metal oxide film 102 is below the initial value, h is set at least more than the 23sec during preferably will keeping.But the higher limit of this temperature is about 600 ℃, is higher than about 600 ℃ from the not preferred temperature of the viewpoint of ALD (or MLD).
In addition, as the experiment of appending, as unstripped gas, film-forming temperature the experiment under 450 ℃ the situation to have carried out using 3DMAS with above-mentioned same condition.H only adopts this a kind of setting of 23sec during keeping this moment.Its result, shown in the some B among Fig. 6, rate of film build is the 0.088nm/ circulation, the thickness of the metal oxide film of tungsten is 1.77nm, and is thicker than initial value 1.1nm.Its result shows that compare with 450 ℃, film-forming temperature is preferably 550 ℃.
In addition, it is the DIPAS (diisopropylaminoethyl silane) in organic source that unstripped gas is changed to as identical aminosilane from 3DMAS, under condition same as described above, tests.Its result is represented by some C, the D among Fig. 6.The point C processing condition do, h is 23sec during the maintenance, film-forming temperature is 450 ℃.And, the some D processing condition do, h is 23sec during the maintenance, film-forming temperature is 300 ℃.
As shown in Figure 6, the rate of film build of some C is the 0.15nm/ circulation, and the thickness of tungsten metal oxide film is identical with initial value, is 1.1nm.And the rate of film build of some D is the 0.185nm/ circulation, and the thickness of tungsten metal oxide film is identical with initial value, is 1.1nm.
Like this; Shown in a C, D; Using DIPAS replacement 3DMAS to be used as under the situation of raw material; Even film-forming temperature is below 450 ℃, the lower temperature in 300～450 ℃ the scope for example; Rate of film build is also bigger; And the adsorptive capacity of silicon is many, so can suppress the growth of tungsten metal oxide film.
In above each experiment, used tungsten film as the film 100 that contains metal, also test for having used titanium nitride film (TiN) to substitute the situation that tungsten film is used as containing the film 100 of metal.Fig. 8 is the graph of relation of thickness of the metal oxide film of expression per 1 round-robin rate of film build and titanium nitride film.The initial film thickness of this metal oxide film is 2.7nm.With above-mentioned situation shown in Figure 6 likewise, make maintenance during h ground from 5sec to 113sec change.
As shown in Figure 8,, during the prolongation maintenance, be accompanied by the increase of rate of film build here, the thickness of titanium metal oxide film linearly shape reduces.And under the little situation of rate of film build, it is also thicker than initial value that the thickness of metal oxide film becomes, and it is roughly the same that rate of film build is about the thickness and the initial film thickness of metal oxide film of 0.11nm/ circulation time.And when rate of film build further increased, the thickness of metal oxide film further increased along with rate of film build and further reduces.Can make the thickness of metal oxide film be reduced to 1.7nm here.
In addition; In above embodiment; To have used the situation of tungsten film and titanium nitride film to be illustrated as example as the film that contains metal; Yet; This film that contains metal comprises the film of the nitride of metallic membrane and metal; Particularly, as the above-mentioned film that contains metal, can use selected a kind of film from the group that constitutes by tungsten film, tungsten nitride film, titanium film, titanium nitride film, tantalum film, nitrogenize tantalum film.
And, in the above-described embodiments, made 3DMAS, but be not limited to this as the unstripped gas that contains Si, can be organic source (BTBAS, 4DMAS, DIPAS) etc. with aminosilane.
And, use the ozone of oxidizing gas in the above-described embodiments as reactant gases, but be not limited to this, can use from by O
3, O
2, O
2Plasma body, N
2Selected gas more than a kind in the group that O, NO constitute in addition, also can use the oxygen activity kind and the hydroxyl activity kind that under the low pressure below the 133Pa, are produced as TOHKEMY 2005-175441 communique is disclosed.And the shape of processing vessel 22 only is to have represented an example, is not limited to the dual pipe structure of explanation here, can certainly be the processing vessel of single tube structure.
And; For example understand semiconductor crystal wafer here as handled object; But this semiconductor die fenestra comprises compound semiconductor substrates such as silicon substrate, GaAs, SiC, GaN; And being not limited to aforesaid substrate, the present invention also can be applicable to glass substrate that liquid crystal indicator uses, ceramic substrate etc.
The advantage of appending is to understand easily with distortion for a person skilled in the art.Thereby, the concrete embodiment of record, concrete detailed construction shown in the present invention with more embodiment is not limited to here.Thereby, can under the prerequisite of the scope of the general inventive concept that does not break away from claims and identity file defined thereof or spirit, carry out various changes.
The application is based on propose to the Japanese Patent Room respectively on July 29th, 2010 and on May 10th, 2011 Japanese patent application 2010-170758 number and advocates right of priority with 2011-105146 number, quotes its full content at this.
Claims (15)
1. a film uses film deposition system on handled object, to form the film that is made up of silicon oxide film, and the surface of this handled object is formed with the film that contains metal, and this film deposition system comprises:
Processing vessel, it can accommodate above-mentioned handled object;
The unstripped gas plenum system, it has the 1st open and close valve, can be in above-mentioned processing vessel base feed gas;
The reactant gases plenum system, it has the 2nd open and close valve, can be in above-mentioned processing vessel supply response gas;
Vacuum evacuating system, it has the 3rd open and close valve, the atmosphere in the above-mentioned processing vessel can be lined up vacuum,
It is characterized in that,
Between absorption process and reaction process, there are off period ground alternate repetition repeatedly this absorption process and reaction process,
This absorption process does; Close above-mentioned the 3rd open and close valve of above-mentioned vacuum evacuating system; Open the 1st specified time limit of above-mentioned the 1st open and close valve of above-mentioned raw materials gas supply system; After above-mentioned processing vessel is supplied with above-mentioned raw materials gas; Close the 1st open and close valve; Keeping above-mentioned the 1st open and close valve to close under the state of the 2nd specified time limit, making the interior above-mentioned raw materials gas adsorption of above-mentioned processing vessel in the surface of above-mentioned handled object;
This reaction process does, opens above-mentioned the 2nd open and close valve of above-mentioned reactant gases plenum system, in above-mentioned processing vessel, supplies with above-mentioned reactant gases, above-mentioned reactant gases and above-mentioned raw materials gas are reacted and forms film.
2. film according to claim 1 is characterized in that,
Open above-mentioned the 3rd open and close valve of above-mentioned vacuum evacuating system and carry out the deflated deairing step in to above-mentioned processing vessel at above-mentioned off period.
3. film according to claim 2 is characterized in that,
In above-mentioned deairing step, in above-mentioned processing vessel, supply with non-active gas.
4. film according to claim 2 is characterized in that,
In above-mentioned deairing step, stop in above-mentioned processing vessel, supplying with all gas, above-mentioned processing vessel is carried out exhaust.
5. film according to claim 1 is characterized in that,
The length of above-mentioned the 2nd specified time limit of closing through above-mentioned the 1st open and close valve of adjusting the above-mentioned raw materials gas supply system in the above-mentioned absorption process is controlled the thickness of metal oxide film that be formed at above-mentioned film that contains metal and the interface between the above-mentioned film above-mentioned contains the film of metal.
6. film according to claim 5 is characterized in that,
The length of above-mentioned the 2nd specified time limit is that the thickness that make to form the above-mentioned metal oxide film behind the above-mentioned film is such length below the initial film thickness of the above-mentioned metal oxide film that forms of nature.
7. film according to claim 1 is characterized in that,
Rate of film build in 1 circulation when above-mentioned absorption process of repeated multiple times and above-mentioned reaction process circulates more than or equal to 0.11nm/.
8. film according to claim 1 is characterized in that,
Above-mentioned raw materials gas is that organic source constitutes by aminosilane.
9. film according to claim 8 is characterized in that,
Above-mentioned aminosilane is that organic source is 3DMAS, and the temperature of the above-mentioned handled object in above-mentioned absorption process and above-mentioned reaction process is more than 550 ℃.
10. film according to claim 8 is characterized in that,
Above-mentioned aminosilane is that organic source is DIPAS, and the temperature of the above-mentioned handled object in above-mentioned absorption process and above-mentioned reaction process is below 450 ℃.
11. film according to claim 1 is characterized in that,
The above-mentioned film that contains metal is selected a kind of film from the group that is made up of tungsten film, tungsten nitride film, titanium film, titanium nitride film, tantalum film and nitrogenize tantalum film.
12. film according to claim 1 is characterized in that,
Above-mentioned raw materials gas is through utilizing gasifier that the material gasification of liquid is formed.
13. film according to claim 12 is characterized in that,
Above-mentioned gasifier comprises material container, and this material container is used to adjust the vapour pressure by the temperature decision of aforesaid liquid raw material, the amount of the raw material that control will be gasified.
14. film according to claim 1 is characterized in that,
Above-mentioned reactant gases is by from by O
3, O
2, N
2Selected gas more than a kind constitutes in the group that O, NO constitute.
15. a film deposition system is characterized in that,
This film deposition system comprises:
Processing vessel, it can accommodate handled object;
Maintaining part, it is used to keep above-mentioned handled object;
The heating part, it is used to heat above-mentioned handled object;
The unstripped gas plenum system, it has the 1st open and close valve, can be in above-mentioned processing vessel base feed gas;
The reactant gases plenum system, it has the 2nd open and close valve, can be in above-mentioned processing vessel supply response gas;
Vacuum evacuating system, it has the 3rd open and close valve, the atmosphere in the above-mentioned processing vessel can be lined up vacuum;
Apparatus control portion, it is used for control device integral body makes this install whole enforcement of rights to require 1 described film.
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| JP2010170758 | 2010-07-29 | ||
| JP2010-170758 | 2010-07-29 | ||
| JP2011-105146 | 2011-05-10 | ||
| JP2011105146A JP5541223B2 (en) | 2010-07-29 | 2011-05-10 | Film forming method and film forming apparatus |
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