CN102054687B - Removal method of surface oxide - Google Patents
Removal method of surface oxide Download PDFInfo
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- CN102054687B CN102054687B CN2009101985974A CN200910198597A CN102054687B CN 102054687 B CN102054687 B CN 102054687B CN 2009101985974 A CN2009101985974 A CN 2009101985974A CN 200910198597 A CN200910198597 A CN 200910198597A CN 102054687 B CN102054687 B CN 102054687B
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Abstract
The invention discloses a removal method of surface oxide. The method comprises: providing a semiconductor substrate the surface of which is at least provided with a silicon region; carrying out remote electric slurry etching on the semiconductor substrate, wherein the etching gas comprises fluorate nitrogen and ammonia gas, the flow capacity of the fluorate nitric is 2sccm to 10sccm, the flow capacity of ammonia gas is 80sccm to 150sccm, and the air pressure is 4mTorr to 6mTorr; and carrying out in-place heating on the semiconductor substrate. Compared with the prior art, in the invention, the etching effect of the surface oxide is improved, and the surface characteristic of the semiconductor substrate of the surface oxide after the removal process is improved.
Description
Technical field
The present invention relates to technical field of semiconductors, particularly a kind of removal method of oxide on surface.
Background technology
Along with development of semiconductor; Get into after the 65nm technology; The nisiloy material is brought into use in the self-aligned silicide contact of semiconductor device, and before the nickel deposition substrate surface is cleaned, and removing natural oxidizing layer (native oxide) becomes very crucial processing step.Traditional argon electricity slurry bombardment technology and hydrofluoric acid immerse technology and have run into a lot of technological problemses.Argon electricity slurry bombardment technology can cause damage to base material owing to be in the environment of electricity slurry and particle bombardment, to carry out, and particularly gets into after the 65nm technology, and this damage is particularly serious.It is relatively poor to the selectivity of silica and silicon that hydrofluoric acid immerses technology, can cause the loss and the profile varying of silicon base, also can cause " spike defect " in addition.Therefore, need a kind of new, oxide on surface removal method low intensive, that have better choice property to substitute traditional method.
Disclosed application number is the removal method that 200710170621.4 one Chinese patent application discloses a kind of oxide on surface; Mainly comprise two steps: at first carry out long-range electricity slurry etching; Etching gas comprises nitrogen fluoride, ammonia; Lower powered electricity slurry is converted into fluoride with nitrogen fluoride, ammonia, and fluoride and oxide on surface reaction generate silicate; Carrying out original position heating afterwards, is to take out behind the gaseous state with said silicate heating sublimation.
Fig. 1 to Fig. 3 has provided the corresponding cross-sectional view of removal method of above-mentioned oxide on surface.
As shown in Figure 1, the semiconductor-based end 100, be provided, have natural oxidizing layer 101 at said the semiconductor-based end 100.
The material of said natural oxidizing layer 101 is a silica, and thickness is 25 dust to 45 dusts.
As shown in Figure 2, to carrying out long-range electricity slurry etching in the said semiconductor-based end 100, etching gas comprises nitrogen fluoride (NF
3), ammonia (NH
3), can also comprise hydrogen (H in the said etching gas
2), argon gas (Ar), helium (He).In etching process, nitrogen fluoride and ammonia are converted into fluoride under the effect of electricity slurry, and the surperficial oxide of the surface condensation and the preferential and semiconductor-based ends 100 reacts said fluoride at the said semiconductor-based ends 100, and oxide layer 101 is converted into silicate layer 102.
As shown in Figure 3; To carrying out the original position heating in the said semiconductor-based end 100; Said silicate layer 102 is heated distillation in the heating process in position for gaseous state and taken out, thereby has removed said oxide layer 101, makes the surface at the said semiconductor-based end 100 become clean Surface.
Above-mentioned patent application provides a kind of low intensive chemical etching method to come oxide on surface is removed, owing to do not have electricity slurry and particle bombardment, has reduced the damage to the semiconductor base material; Immerse technology with traditional hydrofluoric acid on the other hand and compare, above-mentioned disclosed scheme has better choice property, has reduced the loss and the profile varying of silicon base.
In the above-mentioned disclosed technical scheme; Control to long-range electricity slurry etching is the etching effect that influences in the oxide on surface removal process; And the key factor of the surface characteristic of semiconductor substrate after the removal process; Semiconductor substrate surface characteristics variation can make the resistance consistency (Rs Uniformity) that is formed on suprabasil rete of said peninsula body such as metal silicide subsequently descend.
Summary of the invention
The problem that the present invention solves provides a kind of removal method of oxide on surface, improves the etching effect in the oxide on surface removal process, the surface characteristic of semiconductor substrate after the raising removal process.
For addressing the above problem, the invention provides a kind of removal method of oxide on surface, comprise the steps:
The semiconductor-based end is provided, and said semiconductor-based basal surface has a silicon area at least;
To carrying out long-range electricity slurry etching in the said semiconductor-based end, etching gas comprises nitrogen fluoride and ammonia;
To carrying out the original position heating in the said semiconductor-based end;
In the said long-range electricity slurry etching process flow of nitrogen fluoride be 2sccm (ml/min) to 10sccm, the flow of ammonia is 80sccm to 150sccm, reaction pressure is that (millitorr is 1mTorr=0.133Pa) to 6mTorr for 4mTorr.
Optional, electricity slurry power is 25 watts to 45 watts in the said long-range electricity slurry etching process.
Optional, the temperature at the semiconductor-based end is for being lower than 40 degrees centigrade described in the said long-range electricity slurry etching process.
Optional, the temperature of said add in-place thermal process is 140 degrees centigrade to 200 degrees centigrade.
Optional, the said time of moving back the add in-place thermal process is 40 seconds to 80 seconds.
Optional, the atmosphere of said add in-place thermal process is non-oxidizing gas atmosphere.
Optional, said non-oxidizing gas is selected from a kind of in nitrogen, helium, argon gas, the hydrogen.
Compared with prior art, above-mentioned disclosed technical scheme has following advantage:
In the removal method of above-mentioned disclosed oxide on surface, the flow and the reaction pressure of nitrogen fluoride in the etching process and ammonia are optimized, improved the etching effect in the oxide on surface removal process, improved the surface characteristic of semiconductor substrate after the removal process.
Through to the optimization of add in-place thermal process, further improved the surface characteristic of semiconductor substrate after the oxide on surface removal process.
Description of drawings
Fig. 1 to Fig. 3 is the corresponding cross-sectional view of prior art surface oxide layer removal method;
Fig. 4 to Fig. 9 is the sketch map that concerns of long-range electricity slurry etch rate and reactant flow and reaction pressure;
Figure 10 is the schematic flow sheet of embodiment of the invention oxide on surface removal method;
Figure 11 to Figure 17 is the corresponding cross-sectional view of forming process of embodiment of the invention semiconductor surface self-aligned metal silicate.
Embodiment
The invention provides a kind of removal method of oxide on surface; Flow and reaction pressure to nitrogen fluoride in the etching process and ammonia are optimized; Improve the etching effect in the oxide on surface removal process, improved the surface characteristic of semiconductor substrate after the removal process.
For make method of the present invention, feature and advantage can be more obviously understandable, does detailed explanation below in conjunction with the accompanying drawing specific embodiments of the invention.
The flow and the reaction pressure of existing oxide on surface removal method unqualified etching reaction gas nitrogen fluoride and ammonia; And the inventor finds; The flow of nitrogen fluoride and ammonia and reaction pressure are the principal elements that influences etching process and etch rate (etch rate); If the flow of nitrogen fluoride and ammonia and reaction pressure control are improper; Can make that thereby the too fast etching process that causes of etch rate is unstable, thereby influence the etching effect in the oxide on surface removal process, and the surface characteristic of substrate after the removal process.Therefore, need the flow and the reaction pressure of adjustment nitrogen fluoride and ammonia to control etch rate.
Discover that through the inventor mutual restriction between the flow of nitrogen fluoride and ammonia and the reaction pressure influences etch rate jointly.Please refer to Fig. 4 to Fig. 9, Fig. 4 to Fig. 6 has provided under fixing ammonia flow, the relation of etch rate and nitrogen fluoride flow and reaction pressure, that is: and under identical ammonia flow, the nitrogen fluoride flow is more little, and etch rate is more little; Under identical ammonia and nitrogen fluoride flow, reaction pressure is big more, and etch rate is more little.Fig. 7 to Fig. 9 has provided under fixing nitrogen fluoride flow, the relation of etch rate and ammonia flow and reaction pressure, that is: and under identical nitrogen fluoride flow, ammonia flow is big more, and etch rate is more little; Under identical nitrogen fluoride and ammonia flow, reaction pressure is big more, and etch rate is more little.Therefore, the present invention takes all factors into consideration three's restriction relation, reduces the flow of nitrogen fluoride within the specific limits, improves the flow of ammonia and improves reaction pressure simultaneously, to obtain relatively low etch rate, improves etching effect.
Figure 10 has provided the schematic flow sheet of removal method of the oxide on surface of the embodiment of the invention.
Shown in figure 10, execution in step S1 provides the semiconductor-based end, and said semiconductor-based basal surface has a silicon area at least; Execution in step S2, to carrying out long-range electricity slurry etching in the said semiconductor-based end, etching gas comprises nitrogen fluoride and ammonia, and the flow of nitrogen fluoride is 2sccm to 10sccm, and the flow of ammonia is 80sccm to 150sccm, and reaction pressure is 4mTorr to 6mTorr.Execution in step S3 is to carrying out the original position heating in the said semiconductor-based end.
Below in conjunction with accompanying drawing; Forming process with the semiconductor device surface self-aligned metal silicate is that example is elaborated; Figure 11 to Figure 17 has provided the corresponding cross-sectional view of said forming process; Wherein, Figure 11 to Figure 15 is the cross-sectional view corresponding with the step of oxide on surface removal method shown in Figure 10.
Shown in figure 11, the semiconductor-based end 200, be provided, have a silicon area at least at said semiconductor-based basal surface.Be example with the semiconductor-based end 200 in the present embodiment with MOS memory.Said metal-oxide-semiconductor field effect t comprises source electrode 201, drain electrode 202 and grid 203; Below said grid 203, grid oxic horizon 204 is arranged, the material of said grid oxic horizon 204 is a silica; Be formed with side wall (spacer) 205 in the both sides of said grid 203, the material of said side wall can be a kind of in silica, the silicon nitride; Periphery at said metal oxide field effect is formed with isolated area 210, and the material of isolated area 210 is a kind of or their combination in dielectric such as silica, silicon nitride, the carborundum; Said grid 203 is a polycrystalline silicon material.
Because said source electrode 201, drain electrode 202 are to the silicon materials formation of mixing; Its surperficial silicon materials contact with oxygen molecule and can form natural oxidizing layer; Shown in figure 12, the surface of source electrode 201 is formed with natural oxidizing layer 201a, and the surface of drain electrode 202 is formed with natural oxidizing layer 202a; In like manner, said grid 203 is a polycrystalline silicon material, and the surface also can be formed with natural oxidizing layer 203a.The thickness of said natural oxidizing layer 201a, 202a, 203a is 25 dust to 45 dusts.Said natural oxidizing layer 201a, 202a, 203a can influence the reaction between metal material and the silicon materials in process subsequently, make the contact resistance of metal silicide increase, and reduce the performance of device.Therefore, before forming self-aligned metal silicate, need remove, remove said natural oxidizing layer 201a, 202a and 203a the oxide on 200 surfaces, the said semiconductor-based end.
Shown in figure 13, to carrying out long-range electricity slurry etching in the said semiconductor-based end 200, etching reaction gas is nitrogen fluoride (NF
3) and ammonia (NH
3).Nitrogen fluoride and ammonia react under the effect of electricity slurry; Generate the fluoride etching agent; Said fluoride etching agent is surface condensation at the semiconductor-based ends 200, and preferential reacts generation fluorine silicon silicate layer 201b, 202b and 203b with said natural oxidizing layer 201a, 202a and 203a.
Said nitrogen fluoride and ammonia react generation fluoride etching agent under the effect of electricity slurry process is following:
NF
3+NH
3→NH
4F+NH4F·HF
Said fluoride etching agent and natural oxidizing layer course of reaction are following:
NH
4F/NH
4F·HF+SiO
2→(NH
4)
2SiF
6+H
2O
The material of said fluorine silicon silicate layer 201b, 202b and 203b is exactly the (NH in the above-mentioned chemical equation
4)
2SiF
6
In said long-range electricity slurry etching process, the flow of nitrogen fluoride and ammonia and reaction pressure are the principal elements that influences fluoride etching agent and natural oxidizing layer reaction.For guarantee natural oxidizing layer can by evenly, etching is removed completely, needs strict control flow rate of reactive gas and reaction pressure, thereby obtains lower etch rate, improves etching effect.
Described in the present invention in the long-range electricity slurry etching process flow of nitrogen fluoride be 2sccm (ml/min) to 10sccm, the flow of ammonia is 80sccm to 150sccm, under this reaction condition, etch rate is less, can significantly improve etching effect.The flow of preferred nitrogen fluoride is 5sccm in the present embodiment, and the flow of ammonia is 100sccm.Reaction pressure is 4mTorr to 6mTorr in the said long-range electricity slurry etching process, and preferred reaction pressure is 5mTorr in the present embodiment.In addition, in other embodiments of the invention, the etching gas in the said long-range electricity slurry etching process can also comprise hydrogen, argon gas and helium.
Electricity slurry power is 25 watts to 45 watts in the said long-range electricity slurry etching process, and preferred power is 30 watts in the present embodiment.
The temperature at the semiconductor-based end 200 is for being lower than 40 degrees centigrade in the said long-range electricity slurry etching process.In this temperature range, fluoride etching agent NH
4F/NH
4Condensation can take place on the surface at the said semiconductor-based end 200 in FHF; Guarantee the carrying out of etching process; Condensation does not even take place in the condensing rate decline on surface, the semiconductor-based ends 200 in the too high or low excessively fluoride etching agent that all can cause of temperature, and then influences etching effect.Preferred temperature is 35 degrees centigrade in the present embodiment.
Need to prove that in order to improve etching effect, improve the surface characteristic of substrate after the etching process, etch rate of the present invention is relatively low, the duration of long-range electricity slurry etching process can be longer relatively.But; Because the thickness of natural oxidizing layer is generally less; The duration of said long-range electricity slurry etching process shared ratio in whole oxide on surface removal process is less, and main time loss is follow-up add in-place thermal process, so the present invention is to the influence of production capacity and little.
Shown in figure 14, to carrying out the original position heating in the said semiconductor-based end 200.Fluorine silicon silicate layer 201b, 202b and the 203b on said source electrode, drain and gate surface are the gaseous state product in decomposes more than 70 degrees centigrade; And detached; The removal process of oxide on surface is accomplished on the surface of exposing said source electrode 201, drain electrode 202 and grid 203.
The process of said fluorine silicon silicate layer decomposes is following:
(NH
4)
2SiF
6→SiF
4↑+NH
3↑+HF↑
Product after said fluorine silicon silicate layer decomposes all is a gaseous state, and after the said original position heating, using gases discharger such as exhaust pump detach discharge with said gaseous products.
Heating process described in the present embodiment is the original position heating, accomplishes in same semiconductor equipment with long-range electricity slurry etching process before.
The heating-up temperature of said add in-place thermal process is 140 degrees centigrade to 200 degrees centigrade, and preferred heating-up temperature is 150 degrees centigrade to 180 degrees centigrade in the present embodiment.The inventor finds that in this temperature range, the speed of said fluorine silicon silicate layer 201b, 202b and 203b decomposes is comparatively even, can further improve the surface characteristic of substrate after the oxide on surface removal process.Temperature is too high or mistake is low can make the decomposition rate of fluorine silicon silicate layer too fast or slow excessively, the surface characteristic variation that makes substrate.
The atmosphere of said add in-place thermal process is non-oxidizing gas atmosphere, is selected from a kind of in nitrogen, helium, argon gas, the hydrogen, and preferred heating atmosphere is a hydrogen in this enforcement.
The time of said add in-place thermal process is 40 seconds to 80 seconds, and be 60 seconds preferred heating time in the present embodiment.Through said add in-place thermal process, make fluorine silicon silicate layer 201b, 202b and the whole decomposes of 203b on source electrode, drain and gate surface, expose the surface of said source electrode 201, drain electrode 202 and grid 203.
Shown in figure 15, form metal level 206 and cap layer 207 at said semiconductor-based basal surface.
The material of said metal level 206 is selected from nickel or nickel alloy; Alloying element in the nickel alloy is selected from any one in tantalum (Ta), zirconium (Zr), titanium (Ti), hafnium (Hf), tungsten (W), cobalt (Co), platinum (Pt), molybdenum (Mo), palladium (Pd), vanadium (V) and the niobium (Nb); The material of metal level 206 is the nickel platinum alloy in the present embodiment, and the formation method is a sputtering method.
The material of said cap layer 207 is titanium nitride (TiN), and said cap layer 207 can prevent that metal level 206 ingresss of air are oxidized, and the formation of said cap layer 207 is optional, and this step can be saved.
Shown in figure 16, to carrying out first step annealing in the said semiconductor-based end 200, generate metal silicide 201c, 202c and 203c.
The temperature of said first step annealing process is 260 degrees centigrade to 350 degrees centigrade; The annealing duration is 30 seconds to 60 seconds, and annealing atmosphere is selected from helium, nitrogen, argon gas, and preferred annealing temperature is 300 degrees centigrade in the present embodiment; Annealing time is 40 seconds, and annealing atmosphere is a nitrogen.
In the said first step annealing process, the metal material in the said metal level 206 spreads in source electrode 201, drain electrode 202 and the silicon of grid 203 upper surfaces or polycrystalline silicon material, and reacts with silicon materials, generates metal silicide 201c, 202c and 203c.Because carried out the oxide on surface removal before, natural oxidizing layer is removed, therefore can not influence the diffusion and the reaction of metal material.
Shown in figure 17; Selective etch (selectiveetch) is carried out on the surface at the said semiconductor-based end 200; The metal etch that does not have in said cap layer 207 and the metal level 206 to react with silicon materials is removed, exposed said metal silicide 201c, 202c and 203c.The etching solution of selecting in the present embodiment is sulfuric acid (SPM, H
2SO
4: H
2O), comprise the sulfuric acid of about 70% to 80% volume, the water of about 20% to 30% volume; Re-use hydrochloric acid (HPM, HCl:H afterwards
2O
2) the removal metal remained.After etching finishes, rinsing and dry to remove the residual etching solution of trace is carried out at the said semiconductor-based end 200.
After selective etch,, accomplish the forming process of metal silicide to carrying out second step annealing in the said semiconductor-based end 200.The temperature of the second step annealing process is higher than first step annealing process, is 370 degrees centigrade to 420 degrees centigrade, through the second step annealing process, further reduces the contact resistance of said metal silicide 201c, 202c and 203c.
In order to verify the effect of oxide on surface removal method of the present invention; The inventor has carried out the contrast experiment; Disclosed technical scheme is carried out the forming process of metal silicide respectively in employing the foregoing description to semiconductor substrate A and B; Difference is that in oxide on surface removal process the nitrogen fluoride that semiconductor-based end A selects for use and the flow of ammonia and reaction pressure are with reference to preferred value given in the foregoing description; And the nitrogen fluoride flow that semiconductor-based end B selects for use is 14sccm, and the flow of ammonia is 70sccm, and reaction pressure is 3mTorr.Through measuring; The resistance consistency of the metal silicide of semiconductor-based end A is 0.881%; And the resistance consistency of the metal silicide of semiconductor-based end B is 1.471%, and visible, the metal silicide resistance consistency of semiconductor-based end A has obtained effective improvement; Improved 40.125% (the resistance parameter of consistency is more little, shows that the distribution of resistance consistency is good more).
Though the foregoing description is an example with the forming process of self-aligned metal silicate; But oxide on surface removal method provided by the invention can also be used for other silicon or contain the cleaning of silicon face, as in contact hole, filling the cleaning that forms before the tungsten plug crystal column surface.
To sum up; The invention provides a kind of removal method of surface oxide layer; Compared with prior art, the present invention optimizes the flow and the reaction pressure of nitrogen fluoride in the etching process and ammonia, has reduced etch rate relatively; Improve the etching effect of oxide on surface in the oxide on surface removal process, improved the surface characteristic of semiconductor substrate after the removal process.
In addition, through to the optimization of add in-place thermal process, further improved the surface characteristic of semiconductor substrate after the oxide on surface removal process.
Though the present invention discloses as above with preferred embodiment, the present invention is defined in this.Any those skilled in the art are not breaking away from the spirit and scope of the present invention, all can do various changes and modification, so protection scope of the present invention should be as the criterion with claim institute restricted portion.
Claims (7)
1. the removal method of an oxide on surface comprises:
The semiconductor-based end is provided, and said semiconductor-based basal surface has a silicon area at least;
To carrying out long-range electricity slurry etching in the said semiconductor-based end; Etching gas comprises nitrogen fluoride and ammonia; In said long-range electricity slurry etch step; Nitrogen fluoride and ammonia react under the effect of electricity slurry and generate the fluoride etching agent, and the natural oxidizing layer reaction of said fluoride etching agent and semiconductor-based basal surface generates the fluorine silicon silicate layer;
To carrying out the original position heating in the said semiconductor-based end;
It is characterized in that the flow of nitrogen fluoride is 2sccm to 10sccm in the said long-range electricity slurry etching process, the flow of ammonia is 80sccm to 150sccm, and reaction pressure is 4mTorr to 6mTorr.
2. according to the removal method of the said oxide on surface of claim 1, it is characterized in that: electricity slurry power is 25 watts to 45 watts in the said long-range electricity slurry etching process.
3. according to the removal method of the said oxide on surface of claim 1, it is characterized in that: the temperature at the semiconductor-based end is for being lower than 40 degrees centigrade described in the said long-range electricity slurry etching process.
4. according to the removal method of the said oxide on surface of claim 1, it is characterized in that: the temperature of said add in-place thermal process is 140 degrees centigrade to 200 degrees centigrade.
5. according to the removal method of the said oxide on surface of claim 1, it is characterized in that: the time of said add in-place thermal process is 40 seconds to 80 seconds.
6. according to the removal method of the said oxide on surface of claim 1, it is characterized in that: the atmosphere of said add in-place thermal process is non-oxidizing gas.
7. according to the removal method of the said oxide on surface of claim 6, it is characterized in that: said non-oxidizing gas is selected from a kind of in nitrogen, helium, argon gas, the hydrogen.
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| US9941111B2 (en) * | 2015-05-29 | 2018-04-10 | Infineon Technologies Ag | Method for processing a semiconductor layer, method for processing a silicon substrate, and method for processing a silicon layer |
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| CN1681079A (en) * | 2004-02-26 | 2005-10-12 | 应用材料有限公司 | In-situ dry clean chamber for front end of line fabrication |
| US7407888B2 (en) * | 2005-06-17 | 2008-08-05 | Fujitsu Limited | Semiconductor device and a fabrication process thereof |
| CN101440498A (en) * | 2007-11-19 | 2009-05-27 | 中芯国际集成电路制造(上海)有限公司 | Method for precleaning thin film surface oxide before deposition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1681079A (en) * | 2004-02-26 | 2005-10-12 | 应用材料有限公司 | In-situ dry clean chamber for front end of line fabrication |
| US7407888B2 (en) * | 2005-06-17 | 2008-08-05 | Fujitsu Limited | Semiconductor device and a fabrication process thereof |
| CN101440498A (en) * | 2007-11-19 | 2009-05-27 | 中芯国际集成电路制造(上海)有限公司 | Method for precleaning thin film surface oxide before deposition |
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