CN101381861B - Film formation method - Google Patents
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- CN101381861B CN101381861B CN2008101093741A CN200810109374A CN101381861B CN 101381861 B CN101381861 B CN 101381861B CN 2008101093741 A CN2008101093741 A CN 2008101093741A CN 200810109374 A CN200810109374 A CN 200810109374A CN 101381861 B CN101381861 B CN 101381861B
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Abstract
A film formation method for a semiconductor process is arranged to form a thin film on a target substrate by CVD, while supplying a first process gas for film formation and a second process gas for reacting with the first process gas to a process field accommodating the target substrate. The method alternately includes first to fourth steps. The first step performs supply of the first and second process gases to the process field. The second step stops supply of the first and second process gases to the process field. The third step performs supply of the second process gas to the process field while stopping supply of the first process gas to the process field. The fourth step stops supply of the first and second process gases to the process field.
Description
The application's dividing an application that be the denomination of invention submitted on June 28th, 2005 for the application 2005100802412 of " film and film deposition system "
Technical field
The present invention relates on processed substrates such as semiconductor wafer to form film deposition system and method that semiconductor processes that film uses is used.At this, so-called semiconductor processes is meant: in order to pass through at wafer or LCD (liquid-crystal display, Liquid Crystal Display) forms semiconductor layer, insulation layer, conductive layer etc. with the pattern of regulation or on the processed substrates such as glass substrate of FPD (flat-panel monitor, Flat Panel Display) usefulness and be manufactured on the various processing that the structure that contains semiconducter device or the wiring that is connected with semiconducter device, electrode etc. on this processed substrate is implemented.
Background technology
When making the semiconducter device that constitutes semiconductor integrated circuit,, for example on the semiconductor wafer, various processing such as film forming, oxidation, diffusion, upgrading, annealing, etching have been implemented at processed substrate.The spy opens in the 2004-6801 communique, discloses the method for carrying out these semiconductor processes in vertical (so-called intermittent type) thermal treatment unit.In this method, at first semiconductor wafer is transferred on the vertical chip support from wafer case, and be supported with multistage formation.In wafer case, example goes into to hold 25 wafer, and can load 30～150 wafer on chip support.Then, change chip support over to its inside from the below of processing vessel, simultaneously processing vessel is carried out the resistance to air loss locking.Then, under the state of various treatment condition such as the flow of controlling processing gas, processing pressure, treatment temp, the thermal treatment of stipulating.
In recent years, be accompanied by, wish in the manufacturing process of semiconducter device, to alleviate its thermal hysteresis, improve Devices Characteristics semiconductor integrated circuit Highgrade integration and the highly requirement of miniaturization more.In vertical treatment unit, wish to require the method for improvement semiconductor processes according to some.For example in the middle of CVD (the Chemical Vapor Deposition chemical vapor deposition) method that a kind of film forming is handled, a kind of one side base feed gas etc. is off and on arranged, carry out one or more layers film forming repeatedly method (for example, the spy opens flat 6-45256 communique, the spy opens flat 11-87341 communique) of atom or molecular level thick layer on one side.Such film is commonly referred to as ALD (Atomic layer Deposition atomic layer deposition) method, thus, even wafer is not exposed under the high temperature like this, also can carries out purpose and handle.
Figure 13 is using as the dichlorosilane (DCS) of silane-based gas with as the NH of nitriding gas
3Form under the situation of silicon nitride film (SiN), in film in the past, expression supply gas and the timing diagram that applies the RF form.As shown in Figure 13, in processing vessel, sandwich is cleaned the phase, intermittently mutual DCS and the NH of supplying with
3Gas.Supplying with NH
3Apply RF (high frequency) during gas, promote in processing vessel, to generate the nitrogenizing reaction of plasma body.That is, at first in processing vessel, supply with DCS, thus, on wafer surface, adsorb one or more layers DCS with molecular level.Remaining DCS is discharged during cleaning.Then, by supplying with NH
3Generate plasma body, form silicon nitride film by nitrogenize at low temperatures.Carry out a succession of such operation repeatedly, just finished the film of specific thickness.
In above-mentioned film, not only obtain reasonable stepped covering, and compare with the film that carries out high temperature CVD, owing to implemented low temperatureization, can reduce the Si-H key in the film, promote membranous characteristic.But in this kind film in the past, although promoted reaction to carry out by plasma body, film forming speed is still quite low, and productivity is also low.
Summary of the invention
The purpose of this invention is to provide a kind of film and film deposition system, can keep the high-quality while of film, can improve film forming speed significantly.
A first aspect of the present invention is the film that a kind of semiconductor processes is used, this film be supply with in holding the treatment zone of processed substrate that film forming uses first handle gas and with above-mentioned first handle second of gas reaction and handle gas, by CVD film forming method on above-mentioned processed substrate, it is characterized in that, comprise following intersection operation:
To above-mentioned treatment zone supply with above-mentioned first and second first operations of handling gases,
Stop to above-mentioned treatment zone supply with above-mentioned first and second second operations of handling gases,
Supply with above-mentioned second when handling gas to above-mentioned treatment zone, stop to above-mentioned treatment zone supply with above-mentioned first the 3rd operation of handling gas,
Stop to supply with the 4th operation of the above-mentioned first and second processing gases to above-mentioned treatment zone.
A second aspect of the present invention is the film that a kind of semiconductor processes is used, this film be supply with in the treatment zone that holds processed substrate that film forming uses first handle gas, with above-mentioned first handle second of gas reaction handle gas and with first and second the 3rd any all different processing gases of handling in the gases, by CVD film forming method on above-mentioned processed substrate, it is characterized in that, comprise following intersection operation:
Supplying with the above-mentioned first and the 3rd processing gas to above-mentioned treatment zone when, stop to supply with first operation of the above-mentioned second processing gas to above-mentioned treatment zone, above-mentioned first operation has by excitation mechanism, make the above-mentioned the 3rd handle body with excited state supply to above-mentioned treatment zone during,
Stop to above-mentioned treatment zone supply with above-mentioned first to the 3rd second operation of handling gas,
Supply with to above-mentioned treatment zone above-mentioned second handle gas in, stop to above-mentioned treatment zone supply with the above-mentioned first and the 3rd the 3rd operation of handling gas,
Stop to supply with the 4th operation of first to the 3rd processing gas to above-mentioned treatment zone.
A third aspect of the present invention is the film deposition system that a kind of semiconductor processes is used, and it is characterized in that, comprising:
Have the treatment zone that holds processed substrate processing vessel,
In above-mentioned treatment zone, support above-mentioned processed substrate holding components,
Heat the above-mentioned processed substrate in the above-mentioned treatment zone well heater,
Discharge gas in the above-mentioned treatment zone exhaust system,
To above-mentioned treatment zone supply with film forming with first treating-gas supply system of the first processing gas,
To above-mentioned treatment zone supply with above-mentioned first handle second of gas reaction handle second treating-gas supply system of gas,
Optionally the above-mentioned treatment zone of subtend supply with above-mentioned second handle excitation mechanism that gas excites,
The control section of control said apparatus action.
A fourth aspect of the present invention is the medium that comprises that the available computers that contains the programmed instruction that moves in treater reads, it is characterized in that,
Supply with in the treatment zone that holds processed substrate that film forming uses first handle gas and with above-mentioned first handle second of gas reaction and handle gas, in the CVD film deposition system that film forming semiconductor processes is used on above-mentioned processed substrate, the said procedure instruction is when being moved by treater, alternatively implement following operation
To above-mentioned treatment zone supply with above-mentioned first and second first operations of handling gases,
Stop to above-mentioned treatment zone supply with above-mentioned first and second second operations of handling gases,
Supply with to above-mentioned treatment zone above-mentioned second handle gas in, stop to above-mentioned treatment zone supply with above-mentioned first the 3rd operation of handling gas,
Stop to supply with the 4th operation of the above-mentioned first and second processing gases to above-mentioned treatment zone.
A fifth aspect of the present invention is the medium that comprises the embodied on computer readable of the programmed instruction that is used for moving on treater, it is characterized in that,
Supply with in the treatment zone that holds processed substrate that film forming uses first handle gas, with above-mentioned first handle second of gas reaction handle gas and with first and second any all different the 3rd processing gases of handling in the gases, in the CVD film deposition system that film forming semiconductor processes is used on above-mentioned processed substrate, the said procedure instruction is when being moved by treater, alternatively implement following operation
Supplying with the above-mentioned first and the 3rd processing gas to above-mentioned treatment zone when, stop to supply with first operation of the above-mentioned second processing gas to above-mentioned treatment zone, above-mentioned first operation has by excitation mechanism, make the above-mentioned the 3rd handle gas with excited state supply to above-mentioned treatment zone during,
Stop to above-mentioned treatment zone supply with above-mentioned first to the 3rd second operation of handling gas,
Supply with to above-mentioned treatment zone above-mentioned second handle gas in, stop to above-mentioned treatment zone supply with the first and the 3rd the 3rd operation of handling gas,
Stop to supply with the 4th operation of above-mentioned first to the 3rd processing gas to above-mentioned treatment zone.
In aspect first to the 5th, above-mentioned first handles gas comprises silane-based gas, and above-mentioned second handles gas comprises nitriding gas or nitrogen oxidizing gas, and the above-mentioned the 3rd handles gas comprises the gas that is selected from nitrogen, rare gas, nitrogen oxide gas.For example, the above-mentioned first processing gas comprises from dichlorosilane (DCS), hexachloro-silane (HCD), single silane (SiH
4), disilane (Si
2H
6), more than one the gas selected in the hexamethyldisilazane (HMDS), tetrachloro silicane (TCS), disilazane (DSA), nitrilotrisilane (TSA), dual-tert-butyl aminosilane (BTBAS).Above-mentioned second handles gas comprises, for example, is selected from ammonia [NH
3], nitrogen [N
2], nitrous oxide [N
2O], more than one gas of nitrogen protoxide [NO].
Other purposes of the present invention and advantage will be stated in the narration below, and will narrate thus or by implementing a detail knowledge of the present invention part wherein.Objects and advantages of the present invention can be implemented and obtain by means of mode that particularly points out in the back and combination thereof.
Description of drawings
Incorporate the present invention into and constitute the accompanying drawing of this specification sheets part, the preferred embodiments of the present invention are described, and, be used for illustrating principle of the present invention in the above with being described in detail of general narration that provides and preferred embodiment given below.
Fig. 1 is the sectional view of the film deposition system (vertical CVD device) of expression first embodiment of the invention.
Fig. 2 is the transverse section orthographic plan that is illustrated in the part of device shown in Fig. 1.
Fig. 3 is in the film of first embodiment, and the timing diagram of RF state is supplied with and applied to expression gas.
The figure of the thickness data of Fig. 4 silicon nitride film that to be expression obtained by the experiment 1 of first embodiment.
Fig. 5 is the figure of expression by the experiment 1 silicon nitride film film forming speed that obtains.
Fig. 6 is the figure of expression by the inner evenness of the experiment 1 silicon nitride film thickness that obtains.
Fig. 7 is the infrared rays diffraction result schematic diagram of expression by experiment 1 silicon nitride film that obtains.
Fig. 8 is in the film of the first embodiment alternate embodiment, and the timing diagram of RF form is supplied with and applied to expression gas.
Fig. 9 is the sectional view of the film deposition system (vertical CVD device) of expression second embodiment of the present invention.
Figure 10 is in the film of second embodiment, and the timing diagram of RF form is supplied with and applied to expression gas.
The figure of Figure 11 A silicon nitride film film forming speed that to be expression obtained by the experiment 3 of second embodiment.
Figure 11 B is the figure of expression by the improvement rate of the experiment 3 silicon nitride film film forming speeds that obtain.
Figure 12 is the roughly block diagram of situation of expression master control part separation structure.
Figure 13 is the timing diagram that the RF form was supplied with and applied to gas in the film that is illustrated in the past.
Embodiment
Embodiments of the present invention are described with reference to the accompanying drawings.In the following description, the textural element of said function and structure uses same symbol for having roughly, only carries out repeat specification in the case of necessary.
＜the first embodiment 〉
Fig. 1 is the sectional view of the film deposition system (vertical CVD device) of expression first embodiment of the present invention.Fig. 2 is the transverse section orthographic plan that is illustrated in the part of device shown in Fig. 1.This film deposition system 2 contains the unstripped gas (first handle gas) of the dichlorosilane (DCS) as silane-based gas with supply and contains ammonia (NH as nitriding gas
3) support gas (second handle gas), the mode of being piled into silicon nitride film (SiN) constitutes.
The part that runs through in rotating shaft 20 is provided with, and for example magnetic fluid seal spare 22, supports rotating shaft 20 keeping the bubble-tight while to rotate.Around lid 18 and the lower end of manifold 8, for example be provided with and wait the sealing element 24 that forms, the interior stopping property of maintenance container by O shape circle.
Rotating shaft 20 is installed in the front end of supporting the joint arm 26 on the hoisting appliance 25 such as support elevator for example.Make liftings such as chip support 12 and lid 18 by hoisting appliance 25.In addition, also worktable 16 is arranged on regularly lid 18 1 sides, does not make chip support 12 rotations also can carry out the processing of wafer W.
In the side of manifold 8, connecting the gas supply part branch of the treatment zone 5 supply predetermined processing gases in processing vessel 4.The gas supply part branch comprises supports gas supply system (second treating-gas supply system) 28, unstripped gas plenum system (first treating-gas supply system) 30 and purge gas plenum system 32.Unstripped gas plenum system 30 is for example supplied with silane-based gas DCS (dichlorosilane) as film forming unstripped gas.Support gas supply system 28, supply with for example ammonia (NH
3) as optionally carrying out on one side the support gas (second handles gas) that plasma bodyization reacts with unstripped gas on one side.Purge gas plenum system 32 is supplied with rare gas element, for example nitrogen N
2As purge gas.In unstripped gas and support gas (first and second handle gas), can mix an amount of carrier gas as required, but for the purpose of simplifying the description, not mention below.
Particularly, unstripped gas plenum system 30 has two gas dispersion nozzles 36, and they are made by silica tube, and the sidewall turning that inwardly runs through manifold 8 extends upward (with reference to Fig. 2).On each gas dispersion nozzle 36, along the direction (above-below direction) of its length, the whole wafer W facing on the chip support 12 form a plurality of gas jetting hole 36A with certain interval.Each gas jetting hole 36A forms parallel gas flow with respect to the multi-disc wafer W on chip support 12, in the horizontal direction base feed gas equably roughly.And gas dispersion nozzle 36 is not provided with two, only is provided with one and is fine yet.
Support gas supply system 28 and also have two gas dispersion nozzles 34, they are also made by silica tube, and the sidewall turning that inwardly runs through manifold 8 extends upward.On gas dispersion nozzle 34, along the direction (above-below direction) of its length, the whole wafer W facing on the chip support 12 form a plurality of gas jetting hole 34A with certain interval.Each gas jetting hole 34A forms parallel gas flow with respect to the multi-disc wafer W on chip support 12, roughly supplies with equably in the horizontal direction and supports gas.Purge gas plenum system 32 has the gas jet 38 of the sidewall setting that runs through manifold 8.
On the sidewall of a part of processing vessel 4, along the direction configuration gas excitation portion 50 of its height.Opposite side at the processing vessel 4 relative with gas excitation portion 50 disposes elongated venting port 52, is used for discharging inner environmental gas and forms vacuum, is to form by for example the sidewall of processing vessel 4 being cut a part at above-below direction.
Particularly, gas excitation portion 50 has elongated opening 54 up and down, and it forms with the sidewall that certain width cuts processing vessel 4 along above-below direction.This opening 54 is covered by the quartzy lid of making 56, and this lid combines with the outer wall welding of processing vessel 4, and has resistance to air loss.The section of lid 56 is spills, and is outstanding to the outside of processing vessel 4, and has elongated shape up and down.
Form from the sidewall of processing vessel 4 by such structure outstanding, and the gas excitation portion 50 of one side direction processing vessel 4 inner openings.That is, the treatment zone 5 in the internal space of gas excitation portion 50 and the processing vessel 4 is communicated with.Opening 54 forms enough length on above-below direction, can cover the whole wafers that remain on the chip support 12 on the short transverse thus.
On the outer side of 56 two sidewalls of lid,, dispose a pair of elongated electrode 58 in mode respect to one another along its length direction (above-below direction).To produce the high frequency electric source 60 that plasma body uses by supply lines is connected on the electrode 58.By on electrode 58, applying for example high-frequency voltage of 13.56MHz, between pair of electrodes 58, form and be used for the high-frequency electric field of activated plasma.In addition, the frequency of high-frequency voltage is not limited to 13.56MHz, also can use other frequency, for example 400kHz etc.
In the outside of lid 56, be equipped with by for example quartzy insulation protective jacket 64 that constitutes, cover lid 56.With as the relative part of the electrode 58 of insulation protective jacket 64 inboards, dispose the cooling body (not shown) that constitutes by refrigerant pass.For example in refrigerant pass, flow through as the nitrogen that is cooled of refrigeration agent, make electrode 58 coolings.In addition, in the outside of insulation protective jacket 64, be provided with the guard shield (not shown) that covers it and prevent HF leakage.
Near opening 54 outsides of gas excitation portion 50, promptly erect two gas dispersion nozzles 36 of configuration in the both sides in opening 54 outsides (in the processing vessel 4).The unstripped gas that contains DCS gas by each the gas jet 36A that on gas dispersion nozzle 36, forms towards the center position injection of processing vessel 4.
In addition, in the venting port 52 that is provided with gas excitation portion 50 subtends, the exhaust coating member 66 that is " コ " font by the section of quartz manufacturing has been installed, has been covered venting port by welding.This exhaust coating member 66 extends upward along the sidewall of processing vessel 4, forms pneumatic outlet 68 above processing vessel 4.Connect the vacuum evacuating system GE that vacuum pump etc. is housed at pneumatic outlet 68 places.
To surround the mode of processing vessel 4, be provided with well heater 70, be used for surrounding gas and wafer W in the heat treated container 4.Near the venting port 70 in processing vessel 4, be provided with the thermopair (not shown) of control heater 70 usefulness.
Have, film deposition system 2 comprises the main control part 48 that is made of computer of the action of control device integral body etc. again.Main control part 48, according to the processing parameter that the film forming that pre-deposits at its incidental storage part is handled, for example the thickness of the film of Xing Chenging or composition carry out film forming processing as described below.In this storing section stores handle the thickness of the flow of gas and film and relation conduct between the forming control data that prestores.Thereby main control part 48 just can be controlled hoisting appliance 25, gas supply system 28,30,32, exhaust system GE, gas excitation portion 50 and well heater 70 etc. based on the processing parameter or the control data of these storages.
The following describes use and carry out film forming method (so-called ALD film forming) at the device shown in Fig. 1.Briefly, in this film, base feed gas in the treatment zone 5 that holds wafer W (film forming is handled gas with first) and support gas (handling gas with second of the first processing gas reaction) form film by CVD on wafer W.
At first, will keep multi-disc at normal temperatures, for example 50～100 chip sizes are that the chip support 12 of the wafer W of 300mm is packed in the processing vessel 4 that is set in specified temperature.Vacuumize in processing vessel 8 then, and maintain under the predetermined process pressure, simultaneously, the temperature of rising wafer is up to being stabilized in the treatment temp that film forming is used.
Then, by gas dispersion nozzle 36 and 34, supplying with the unstripped gas that contains DCS gas off and on and containing NH in the dominant discharge respectively
3The support gas of gas.Particularly, from the gas jetting hole 36A base feed gas of gas dispersion nozzle 36, make to form parallel gas stream with respect to the multi-disc wafer W on the chip support 12.In addition, support gas, make to form parallel gas stream with respect to the multi-disc wafer W on the chip support 12 from the gas jetting hole 36A supply of gas dispersion nozzle 34.Two kinds of gases react on wafer W, form silicon nitride film thus on wafer W.
The support gas of being supplied with by the gas jetting hole 36A of gas dispersion nozzle 34, by the plasma generation area PS between the pair of electrodes 58 time, a part is by plasma bodyization optionally.At this moment, generate for example N
*, NH
*, NH
2 *, NH
3 *Deng free radical (active seed) (symbol * represents it is free radical).These free radicals flow to the center of processing vessel 4 from the opening 54 of gas excitation portion 50, supply between the wafer W with streamlined state.
Above-mentioned free radical be adsorbed on the reaction of the lip-deep DCS gas molecule of wafer W, on wafer W, form silicon nitride film thus.And in contrast, on the surface of wafer W, adsorbed the position of free radical, and under the situation that flows through DCS gas, same reaction also can take place, on wafer W, form silicon nitride film.
Fig. 3 is in the film of first embodiment, and the timing diagram of RF state is supplied with and applied to expression gas.As shown in FIG. 3, in the film of this embodiment, alternatively repeat first to fourth during (first to fourth operation) T1～T4.That is, repeatedly repeat the circulation that is made of T1～T4 during first to fourth, the silicon nitride film that forms in each circulation obtains having the silicon nitride film of final thickness by the lamination of film.
Particularly, between the first phase, among (first operation) T1, (in Fig. 3, be expressed as NH to treatment zone 5 base feed gases (in Fig. 3, being expressed as DCS) and support gas
3).In the second phase (second operation) T2, stop to treatment zone 5 base feed gases and support gas.Between the third phase, among (the 3rd operation) T3,, stop to treatment zone 5 base feed gases when treatment zone 5 is supplied with support gas.In addition, between the third phase among the T3,, make support gaseous plasmaization in gas excitation portion 50, the support gas of supplying with under the state that is exciting to treatment zone 5 thus by opening RF power supply 60.Between the fourth phase, among (the 4th operation) T4, stop to treatment zone 5 base feed gases and support gas.
Second and the fourth phase between T2, T4 use during the cleaning of the entrap bubble in getting rid of processing vessel 4.This so-called cleaning, be meant and flowing through N
2In the time of rare gas elementes such as gas, with vacuum exhausts in the processing vessel 4, or stop the supply of all gas, with vacuum exhausts in the processing vessel 4, to remove the entrap bubble in the processing vessel 4.Moreover, first and the third phase between among T1, the T3, when base feed gas with when supporting gas, can stop the vacuum exhaust in the processing vessel 4.But, on one side at one side base feed gas with support gas when carrying out vacuum exhaust in the processing vessel 4, during whole first to fourth, can carry out the vacuum exhaust in the processing vessel 4 in the full time of T1～T4 constantly.
In Fig. 3, T1 is set at about 1～20 second between the first phase, and for example about 10 seconds, second phase T2 was set at about 1～20 second, and for example about 10 seconds, T3 was set at about 1～30 second between the third phase, and for example about 10 seconds, T4 was set at about 1～20 second, for example about 10 seconds during the 4th.But these times only simply are examples, are not limited to this numerical value.
As mentioned above, supply contains NH together
3The support gas of gas and contain DCS unstripped gas during T1 and supply with separately and contain NH
3T3 during the support gas of gas, T2, T4 during intersect to implement cleaning.Can improve its film forming speed significantly in the high-quality while of the silicon nitride film of keeping formation thus.Think following reason is arranged.That is, as T1 between first phase base feed gas together with when supporting gas, the DCS molecule that is adsorbed in wafer surface is by the NH that supplies with simultaneously
3Gas makes part nitrogenize by halves.Therefore, between the first phase among the T1, adsorptive capacity is not having when saturated, and the absorption of DCS gas molecule is being carried out always, and the adsorptive capacity of DCS gas just is higher than the amount in previous methods (flowing through unstripped gas separately) as a result.T3 between the third phase then is by the NH by plasma exciatiaon
3Gas fully reacts the part that does not have complete reaction to make and form silicon nitride film under the state of high film forming speed.
Above-mentioned film forming is handled and is carried out according to following treatment condition.The flow of DCS gas for example is 1000sccm (1slm) in the scope of 100～3000sccm.NH
3The flow of gas for example is 1000sccm in the scope of 100～5000sccm.Treatment temp is lower than common CVD to be handled, and is specially 180～600 ℃ (not containing), for example 550 ℃.When treatment temp was lower than 180 ℃, can't react did not almost have the accumulation of film.And when treatment temp is higher than 600 ℃, can form the also poor accumulating film of mass ratio CVD.
Processing pressure is 1Torr among (absorption process) T1 between the first phase for example in the scope of 27Pa (0.2Torr)～1330Pa (10Torr), is 0.3Torr among the T3 that (uses the pecvd nitride operation) between the third phase.During less than 27Pa, film forming speed is lower than realistic scale in processing pressure.Under the situation of processing pressure greater than 1330Pa, abundant activated plasma.
Between the first phase among (absorption process) T1, gas DCS and NH
3Throughput ratio [DCS/NH
3] be set in the scope about 1/10～10.As gas NH
3The very few situation of throughput ratio under, can not produce and supply with NH simultaneously
3The effect of gas.And work as NH
3Throughput ratio when too much, can not produce film forming body.
＜experiment 1 〉
1 estimate to use the film of first embodiment of timing diagram shown in Figure 3 and the silicon nitride film that forms according to the film in the past (ALD method) of timing diagram shown in Figure 13 by experiment.In two embodiment PE1 and PE2 of first embodiment, get NH respectively
3Feed rate be 500sccm (0.5slm) and 1000sccm (1slm).In the comparative example CE1 of in the past film, get NH
3Feed rate be 1000sccm (1slm).Film forming cycle number is got 160 times altogether.
Fig. 4 is the figure of expression by the thickness data of experiment 1 silicon nitride film that obtains.Fig. 5 is the figure of expression by the experiment 1 silicon nitride film film forming speed that obtains.Fig. 6 is that expression is by the figure of the thickness of testing 1 silicon nitride film that obtains at inner evenness.Fig. 7 is the figure of expression by the experiment 1 silicon nitride film infrared ray diffraction result who obtains." TOP " in Fig. 4～Fig. 7, " CTR " and " BTM " represent to be arranged in the position of semiconductor wafer of top, central authorities and the bottom of chip support respectively.
For at the thickness TH of the silicon nitride film shown in Fig. 4 (nm), in comparative example CE1, with the location independent of wafer, TH is about about 15nm.In two embodiment PE1 and PE2, with the location independent of wafer, TH is about 20nm.That is, can confirm that two embodiment PE1 compare with comparative example CE1 with PE2, silicon nitride film that can the accumulative facies uniform thickness.
For being equivalent to each round-robin film forming speed Rth (nm/ circulation) shown in Fig. 5, in comparative example CE1, Rth is about about 0.1nm.In two embodiment PE1 and PE2, Rth is about 0.12～0.13nm.That is, can confirm to compare with comparative example CE1, in two embodiment PE1 and PE2, film forming speed has increased.
For the homogeneity PTuni of the thickness shown in Fig. 6 in face (± %), in comparative example CE1, PTuni is about ± 3.5～4.5%, in two embodiment PE1 and PE2, PTuni is about ± 3.0～4.0%.That is, can confirm to compare with comparative example CE1, two embodiment PE1 and PE2 can improve the homogeneity of thickness in face.
For the infra-red intensity LD (a.u) that obtains at the infrared ray diffraction shown in Fig. 7, in comparative example CE11,, on LD, demonstrate the peak P1 that expression has " Si-H key " in the position of wave number about 2200 by membranous.CE11 uses with hexachloro-silane (HCD) as handle gas, the silicon nitride film that forms in LP (low pressure)-CVD as a comparative example.On the other hand, in embodiment PE1, LD roughly is smooth on the whole.That is, can confirm to compare with comparative example CE11, embodiment PE1 is film forming membranous good.
According to the timing diagram of Fig. 3, supply with together and contain NH
3The support gas of gas and contain DCS gas unstripped gas during T1, do not apply RF, and contain NH supplying with separately
3T3 during the support gas of gas applies RF.The RF state that applies shown in Fig. 8 that can be used in replaces this timing diagram.Fig. 8 is the film in the embodiment that first embodiment changes, expression supply gas and the timing diagram that applies RF.
According to the timing diagram of Fig. 8, supply with together and contain NH
3The support gas of gas and contain DCS gas unstripped gas during T1 and supply with separately and contain NH
3During the support gas of gas during these two of the T3 in, apply RF to excite support gas.In the case, T1 between the first phase excites support gas when flowing through unstripped gas, absorption DCS and NH on semiconductor wafer W
3Free radical.T3 between the third phase then is by the NH of plasma exciatiaon
3Gas makes the part complete reaction of incomplete reaction, forms silicon nitride film under the state of high film forming speed.
＜experiment 2 〉
Can use N
2Gas replaces NH
3Gas is as nitriding gas.In method, use N according to Fig. 3
2Gas replaces NH
3Gas carries out the film forming experiment 2 of silicon nitride film.Consequently, its film forming speed is the 0.1nm/ circulation.In addition, in the method for Fig. 8, use N
2Gas replaces NH
3Gas carries out the film forming of silicon nitride film, and its film forming speed is the 0.5nm/ circulation.Thereby, can confirm method by Fig. 8, using N
2Gas replaces NH
3Gas can improve film forming speed during as nitriding gas significantly.
＜the second embodiment 〉
Fig. 9 is the sectional view of the film deposition system (vertical CVD device) of expression second embodiment of the invention.The film deposition system 2X of second embodiment, except supporting gas supply system (second treating-gas supply system) 28, unstripped gas plenum system (first treating-gas supply system) 30 and purge gas plenum system 32, also comprise assist gas plenum system (the 3rd treating-gas supply system) 84.84 supplies of assist gas plenum system are with unstripped gas or support all different assist gas of gas.Particularly, assist gas contains the gas that is selected from nitrogen, rare gas, nitrogen oxide gas, in the present embodiment, and by for example N
2Or Ar gas constitutes.For with assist gas plenum system 84 relevant portions beyond part, the film deposition system 2X shown in Fig. 9 with have identical in fact structure at the film deposition system shown in Fig. 12.
Assist gas plenum system 84 has common gas dispersion nozzle 34 with support gas supply system 28, therefore just has the gas jetting hole 34A that forms on gas dispersion nozzle 34.For this reason, nozzle 34 connects N through the gas supply pipe road (gas passage) 86 of assist gas plenum system 84
2Or the gas source 85 of Ar gas.The flow director 86B of switch-valve 86A and mass flow controller and so on is housed on gas supply pipe road 86.Thus can be at control N
2Or the supply gas Ar gas flow time.As assist gas, can use nitrogen oxide gas to replace rare gas elementes such as nitrogen or rare gas as mentioned above.
As mentioned above, gas dispersion nozzle 34 is made of silica tube, and the sidewall that inwardly runs through manifold 8 bends towards direction and extends.On gas dispersion nozzle 34, form a plurality of gas jetting hole 34A along its length (above-below direction) and across the interval of regulation, make whole wafer W on its subtend chip support 12.Each gas jetting hole 34A forms parallel gas stream facing to the multi-disc wafer W on the chip support 12, supplies with substantially equably in the horizontal direction and supports gas or assist gas.Assist gas plenum system 84, can be not yet with support gas supply system 28 common gas dispersing nozzles 34, with gas dispersion nozzle 34 the gas dispersion nozzle that assist gas uses is set simultaneously and gets final product.
The following describes the film (so-called ALD film forming) that use is carried out at the device shown in Fig. 9.In general, in this film, base feed gas in the treatment zone 5 that holds wafer W (film forming is handled gas with first) and support gas (handling gas with second of the first processing gas reaction) and aforesaid assist gas (the 3rd handles gas) form film by CVD on wafer W.
At first, will keep multi-disc at normal temperatures, for example 50～100 chip sizes are that the chip support 12 of 300mm wafer W is sent in the processing vessel 4 that is set in specified temperature.When vacuumizing and maintaining predetermined process pressure in the processing vessel 8, the temperature of rising wafer is up to being stabilized in the treatment temp that film forming is used then.
Then, dominant discharge and supply with the unstripped gas that contains DCS off and on, contain NH respectively by gas dispersion nozzle 36,34
3Support gas and assist gas.Particularly, from the gas jetting hole 36A of gas dispersion nozzle 36, to form the mode base feed gas of parallel gas stream facing to the multi-disc wafer W on the chip support 12.In addition, from the gas jetting hole 36A of gas dispersion nozzle 34, supply with support gas and assist gas in the mode that forms parallel gas stream facing to the multi-disc wafer W on the chip support 12.DCS gas and NH
3Gas reacts on wafer W, forms silicon nitride film thus on wafer W.
Figure 10 is in the film of second embodiment, and the timing diagram of the form of RF is supplied with and applied to expression gas.As shown in Figure 10, in the film of this embodiment, (first to fourth operation) T11～T14 during overlapping first to fourth.That is, repeatedly repeat the circulation that constitutes by T11～T14 during first to fourth,, obtain the silicon nitride film of final thickness by being layered in the film of the silicon nitride film that forms in each circulation.
Particularly, between the first phase, among (first operation) T11, (in Figure 10, be expressed as N to treatment zone 5 base feed gases (in Figure 10, being expressed as DCS) and assist gas on the one hand
2Or Ar), stop to supply with support gas simultaneously and (in Figure 10, be expressed as NH to treatment zone 5
3).Between the first phase, among the T11, connect RF power supply 60, make the assist gas plasma bodyization, to the assist gas of treatment zone 5 supplies under excited state by gas excitation portion 50.In the second phase (second operation) T12, stop to treatment zone 5 base feed gases simultaneously, support gas and assist gas.Between the third phase, among (the 3rd operation) T13,, stop to treatment zone 5 base feed gas and assist gass when treatment zone 5 is supplied with support gas.And between the third phase, among the T13, begin to connect RF power supply 60 from the centre, and will support gaseous plasmaization by gas excitation portion 50, only during inferior, in treatment zone 5, supply with the support gas under excited state thus among the T13b.Between the fourth phase, among (the 4th operation) T14, stop base feed gas, support gas and assist gas in treatment zone 5.
Second and the fourth phase between T12, T14, as using during cleaning, to give off the entrap bubble in processing vessel 4.This so-called cleaning, be meant and flowing through N
2In the time of rare gas elementes such as gas,, perhaps stop to supply with all gases fully, with vacuum exhaust in the processing vessel 4, to remove the entrap bubble in the processing vessel 4 with vacuum exhaust in the processing vessel 4.First and the third phase between among T11, the T13, at base feed gas, when supporting gas and assist gas, can stop at the vacuum exhaust in the processing vessel 4.But,, when carrying out the vacuum exhaust of processing vessel 4 simultaneously, can during whole first to fourth, continue the vacuum exhaust in the processing vessel 4 among T11～T14 at base feed gas, support gas and assist gas.
In Figure 10, T11 is set to about 1～20 second between the first phase, for example about 10 seconds, second phase T12 was set to about 1～20 second, for example about 10 seconds, T13 is set to about 1～30 second between the third phase, for example about 20 seconds, inferior during T13b be set to about 1～25 second, for example about 15 seconds, T14 is set to about 1～20 second between the fourth phase, for example about 10 seconds.But these times are only represented an example, are not limited to these numerical value.
As mentioned above, by adding and exciting assist gas, by the active seed promotion decomposition of the unstripped gas of supply meanwhile of above-mentioned assist gas.The result just can improve the film forming speed of silicon nitride film.At this moment, particularly use N
2Gas not only can promote the decomposition of unstripped gas during as assist gas, also by the direct chemical combination of active seed of the active seed of nitrogen and silicon and directly form SiN.The result can further improve the film forming speed of silicon nitride film.
In second embodiment, treatment temp and processing pressure and DCS gas, NH
3The flow of all gases such as gas is all identical with first embodiment.The flow of assist gas is set at the flow that is lower than as unstripped gas DCS gas, for example gets about about 1/10 of DCS gas flow.
Between the third phase among the T13, through after the specified time Δ t, connect RF power supply 60, make support gaseous plasmaization at gas excitation portion 50 places, thus only during inferior T13b supply with the support gas that is in excited state to treatment zone 5.This so-called preset time Δ t is promptly up to making NH
3The time that gas flow is stable is for example about 5 seconds.But, also can as at first embodiment, during whole supply support gas, all make and support gas in gas excitation portion 50 plasma bodyizations.So make the stability of flowization of supporting gas just connect the RF power supply later on and produce plasma body, can improve the homogeneity of the active seed concentration of (short transverse) between the wafer W two sides.
＜experiment 3 〉
Use is carried out evaluation experimental 3 according to forming silicon nitride film at the film of second embodiment of timing diagram shown in Figure 10 with according to the film in the past (ALD) at timing diagram shown in Figure 13.In two embodiment PE11, PE12 of second embodiment, use N respectively
2Gas and Ar gas are as assist gas.The comparative example CE1 of film did not use assist gas in the past, according to carry out (identical in fact with the comparative example CE1 of experiment 1) at the timing diagram shown in Figure 13.Film forming cycle number 160 times altogether.
Figure 11 A is the film forming speed figure of expression by experiment 3 silicon nitride films that obtain.Figure 11 B is the figure of expression by the experiment 3 silicon nitride film film forming speed improvement rates that obtain.Moreover " TOP " in Figure 11 A, Figure 11 B, " CTR " and " BTM " represent that respectively semiconductor wafer in the chip support is positioned at the position of top, central authorities and bottom.
For being equivalent at each the round-robin film forming speed Rth (nm/ circulation) shown in Figure 11 A, in comparative example CE1, with the location independent of wafer, Rth is about 0.1nm.Using N
2Among the embodiment PE11 of gas as assist gas, Rth is about 0.45～0.55nm.In using the embodiment PE12 of Ar gas as assist gas, Rth is about 0.25～0.4nm.
For at the film forming speed improvement rate IRth (%) shown in Figure 11 B, using N
2Among the embodiment PE11 of gas as assist gas, IRth is about 150～300%.In using the embodiment PE12 of Ar gas as assist gas, IRth is about 300～500%.
That is, CE1 compares with comparative example, confirms that two embodiment PE11, PE12 can increase film forming speed.In addition, the film forming speed of embodiment PE11 also is higher than the film forming speed of embodiment PE12, can think following reason.Promptly as mentioned above, N
2The active seed of gas not only promotes unstripped gas to decompose, and can form silicon nitride with the silicon direct reaction that is excited.
＜with first and second embodiment common item and the variation instance
The method of first and second embodiments is based on as mentioned above that handling procedure implements under the control of main control part 48.Figure 12 is the schematic block diagram of expression main control part 48 structures.Main control part 48 has CPU210, is connecting storage part 212, importation 214 and output 216 etc. therewith.In storage part 212, storing handling procedure and method parameter.Importation 214 comprises the input unit of talking with usefulness with the user, for example keyboard or pointing device, and the driving mechanism of storage media etc.Output 216 outputs are used to control the control signal of each equipment of treatment unit.Figure 12 storage media 218 that also expression can off line simultaneously.
The method of above-mentioned embodiment can as the programmed instruction that is used for moving, be applicable to various semiconductor processing devices by writing with calculating machine-readable getting on the storage media on treater.Perhaps, this kind programmed instruction goes for the various semiconductor processing devices that transmit by communication media.This storage media is for example disk (floppy disk, hard disk (example is the hard disk in storage compartment 212) etc.), CD (CD, DVD etc.), magneto-optic disk (MO etc.), semiconductor memory etc.The computer of control semiconductor processing device action by reading in program stored instruction in the storage media, moves it and implements aforesaid method on treater.
In first and second embodiments, use the silane-based gas of DCS gas as unstripped gas.But be not limited to this,, can use to be selected from dichlorosilane (DCS), hexachloro-silane (HCD), single silane [SiH as unstripped gas
4], disilane [Si
2H
6], more than one gas of hexamethyldisilazane (HMDS), tetrachloro silicane (TCS), disilazane (DSA), nitrilotrisilane (TSA) and dual-tert-butyl aminosilane (BTBAS).
In addition, in first and second embodiments, can use nitrous oxide [N
2O], the nitrogen oxidizing gas of nitrogen oxide [NO] and so on replaces NH
3Gas, N
2Nitriding gas such as gas are as supporting gas.Can also use oxidizing gas to replace nitriding gas as supporting gas.
In addition, in second embodiment, use rare gas as assist gas, but be not limited to Ar gas, can use He, Ne, Kr, Xe etc.Also can use nitrous oxide [N
2O], nitrogen oxide [NO], nitrogen peroxide [NO
2] wait nitrogen oxide to use as assist gas.
In above-mentioned first and second embodiments,, have and to form the excitation portion 50 of plasma body and the unitized construction that processing vessel 4 is made one as film deposition system 2.In addition, also excitation portion 50 and processing vessel 4 can be set respectively, beyond processing vessel 4, excite NH in advance
3Gas (so-called remote plasma body) is supplied with this NH that excites in processing vessel 4
3Gas.Being not limited to semiconductor wafer as processed substrate, also can be other substrates such as LCD substrate, glass substrate.
For one of skill in the art, additional advantage and improvement all are easily.Therefore, the present invention is not limited to these concrete details and representative embodiments shown here and described at it aspect more widely.Only otherwise depart from the spirit and scope of as defined in the claims inventive concept and equivalent thereof, can carry out variation miscellaneous.
Claims (18)
1. film that semiconductor processes is used, this film be supply with in the treatment zone that holds processed substrate that film forming uses first handle gas and with described first handle second of gas reaction and handle gas, by CVD film forming method on described processed substrate, it is characterized in that: this method circulates first～the 4th following operation in order and carries out:
Supply with first operation of the described first and second processing gases to described treatment zone;
Do not supply with described first and second and handle gas, second operation of carrying out vacuum exhaust to described treatment zone;
Supplying with the described second processing gas to described treatment zone when, do not supply with described first the 3rd operation of handling gas to described treatment zone, described the 3rd operation comprise by excitation mechanism make described second handle gas with excited state supply with described treatment zone during; With
Do not supply with first and second and handle gas, the 4th operation of carrying out vacuum exhaust to described treatment zone.
2. the method described in claim 1 is characterized in that: described first operation do not comprise by described excitation mechanism excite described second handle gas during.
3. the method described in claim 1 is characterized in that: described first operation be included in by described excitation mechanism make described second handle gas with excited state supply with described treatment zone during.
4. the method described in claim 1, it is characterized in that: described excitation mechanism is included in the space that is communicated with described treatment zone, be configured in described second and handle the supplying opening of gas and the plasma generation area between the described substrate, described second handles gas is excited by described plasma generation area the time.
5. the method described in claim 4 is characterized in that: described first handles gas supplies with described treatment zone between described plasma generation area and described substrate.
6. the method described in claim 1 is characterized in that: the described second and the 4th operation comprise respectively to described treatment zone supply with purge gas during.
7. the method described in claim 1 is characterized in that: in the operation that forms described film, continue the exhaust in the described treatment zone.
8. the method described in claim 1 is characterized in that: described first handles gas contains silane-based gas, and described second handles gas contains nitriding gas or nitrogen oxidizing gas.
9. the method described in claim 8, it is characterized in that: described first handles gas contains more than one the gas that is selected from dichlorosilane, hexachloro-silane, single silane, disilane, hexamethyldisilazane, tetrachloro silicane, disilazane, nitrilotrisilane, dual-tert-butyl aminosilane, and described second handles gas contains and be selected from ammonia, nitrogen, nitrous oxide, nitric oxide production more than one gas.
10. semiconductor processes film, this film be supply with in the treatment zone that holds processed substrate that film forming uses first handle gas, with described first handle second of gas reaction handle gas and with first and second the 3rd any all different processing gases of handling in the gases, by CVD film forming method on described processed substrate, it is characterized in that: this method circulates first～the 4th following operation in order and carries out:
Supplying with the described first and the 3rd processing gas to described treatment zone when, do not supply with first operation of the described second processing gas to described treatment zone, described first operation has by excitation mechanism, make the described the 3rd handle gas with excited state supply with described treatment zone during;
Do not supply with described first to the 3rd and handle gas, second operation of carrying out vacuum exhaust to described treatment zone;
Supplying with the described second processing gas to described treatment zone when, do not supply with the 3rd operation of the described first and the 3rd processing gas to described treatment zone, described the 3rd operation has under the state that is excited the described second processing gas by described excitation mechanism supplies with the duration of exciting of described treatment zone with it; With
Do not supply with first to the 3rd and handle gas, the 4th operation of carrying out vacuum exhaust to described treatment zone.
11. the method described in claim 10, it is characterized in that: described excitation mechanism have with space that described treatment zone is communicated with in, be configured in the described the 3rd and handle the supplying opening of gas and the plasma generation area between the described substrate, the described the 3rd handles gas is excited by described plasma generation area the time.
12. the method described in claim 11 is characterized in that: described first handles gas supplies with described treatment zone between described plasma generation area and described substrate.
13. the method described in claim 10 is characterized in that: described the 3rd operation had and does not make described second to handle gas under the state that described excitation mechanism is excited before described duration of exciting, with its supply with described treatment zone during.
14. the method described in claim 10 is characterized in that: described second handles gas and the described the 3rd handles the total supplying opening of gas.
15. the method described in claim 10 is characterized in that: the described second and the 4th operation has respectively during described treatment zone supply purge gas.
16. the method described in claim 10 is characterized in that; In the operation that forms described film, continue the exhaust in the described treatment zone.
17. the method described in claim 10, it is characterized in that: described first handles gas contains silane-based gas, described second handles gas contains nitriding gas or nitrogen oxidizing gas, and the described the 3rd handles gas contains the gas that is selected from nitrogen, rare gas, the nitrogen oxide.
18. the method described in claim 17, it is characterized in that: described first handles gas contains more than one the gas that is selected from dichlorosilane, hexachloro-silane, single silane, disilane, hexamethyldisilazane, tetrachloro silicane, disilazane, nitrilotrisilane, dual-tert-butyl aminosilane, and described second handles gas contains and be selected from ammonia, nitrogen, nitrous oxide, nitric oxide production more than one gas.
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| JP2005048059A JP4396547B2 (en) | 2004-06-28 | 2005-02-23 | Film forming method, film forming apparatus, and storage medium |
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| US20070240644A1 (en) | 2006-03-24 | 2007-10-18 | Hiroyuki Matsuura | Vertical plasma processing apparatus for semiconductor process |
| JP4857849B2 (en) * | 2006-03-24 | 2012-01-18 | 東京エレクトロン株式会社 | Plasma processing apparatus and plasma processing method |
| US20070259111A1 (en) * | 2006-05-05 | 2007-11-08 | Singh Kaushal K | Method and apparatus for photo-excitation of chemicals for atomic layer deposition of dielectric film |
| JP6105967B2 (en) * | 2012-03-21 | 2017-03-29 | 株式会社日立国際電気 | Semiconductor device manufacturing method, substrate processing method, substrate processing apparatus, and program |
| DE102015004419A1 (en) * | 2015-04-02 | 2016-10-06 | Centrotherm Photovoltaics Ag | Wafer boat and plasma treatment device for wafers |
| CN112420731B (en) * | 2020-11-17 | 2021-12-17 | 长江存储科技有限责任公司 | Method for forming thin film layer in deep hole and method for manufacturing semiconductor device |
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| JP2002009009A (en) * | 2000-06-20 | 2002-01-11 | Tokyo Electron Ltd | Vertical thermal treatment equipment |
| CN1423834A (en) * | 2000-04-17 | 2003-06-11 | 马特森技术公司 | UV prtreatment process for ultra-thin oxynitride for formation of silicon nitridefilms |
| CN1448997A (en) * | 1995-09-08 | 2003-10-15 | 株式会社半导体能源研究所 | Method and apparatus for manufacturing semiconductor device |
| JP2004006801A (en) * | 2002-04-11 | 2004-01-08 | Hitachi Kokusai Electric Inc | Vertical semiconductor manufacturing apparatus |
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| JP4411215B2 (en) * | 2002-11-11 | 2010-02-10 | 株式会社日立国際電気 | Substrate processing apparatus and semiconductor device manufacturing method |
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| CN1448997A (en) * | 1995-09-08 | 2003-10-15 | 株式会社半导体能源研究所 | Method and apparatus for manufacturing semiconductor device |
| CN1423834A (en) * | 2000-04-17 | 2003-06-11 | 马特森技术公司 | UV prtreatment process for ultra-thin oxynitride for formation of silicon nitridefilms |
| JP2002009009A (en) * | 2000-06-20 | 2002-01-11 | Tokyo Electron Ltd | Vertical thermal treatment equipment |
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