CN102054687A - Removal method of surface oxide - Google Patents
Removal method of surface oxide Download PDFInfo
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- CN102054687A CN102054687A CN2009101985974A CN200910198597A CN102054687A CN 102054687 A CN102054687 A CN 102054687A CN 2009101985974 A CN2009101985974 A CN 2009101985974A CN 200910198597 A CN200910198597 A CN 200910198597A CN 102054687 A CN102054687 A CN 102054687A
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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, enter 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 to carry out in the environment of electricity slurry and particle bombardment, particularly enter 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 to substitute traditional method.
Disclosed application number is the removal method that 200710170621.4 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, fluoride and oxide on surface reaction generate silicate; Carrying out original position heating afterwards, is to take out behind the gaseous state with described silicate heating sublimation.
Fig. 1 to Fig. 3 has provided the cross-sectional view of the removal method correspondence of above-mentioned oxide on surface.
As shown in Figure 1, provide the semiconductor-based end 100, have natural oxidizing layer 101 at described the semiconductor-based end 100.
The material of described 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 described semiconductor-based end 100, etching gas comprises nitrogen fluoride (NF
3), ammonia (NH
3), can also comprise hydrogen (H in the described 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 described fluoride reacts at the oxide on surface condensation of the described semiconductor-based ends 100 and preferential and surface, the 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 described semiconductor-based end 100, described silicate layer 102 is heated distillation in the heating process in position for gaseous state and taken out, thereby has removed described oxide layer 101, makes the surface at the described 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, 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 described 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 described semiconductor-based basal surface has a silicon area at least;
To carrying out long-range electricity slurry etching in the described semiconductor-based end, etching gas comprises nitrogen fluoride and ammonia;
To carrying out the original position heating in the described semiconductor-based end;
In the described 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 4mTorr (millitorr, 1mTorr=0.133Pa) main 6mTorr.
Optionally, electricity slurry power is 25 watts to 45 watts in the described long-range electricity slurry etching process.
Optionally, the temperature at the semiconductor-based end described in the described long-range electricity slurry etching process is for being lower than 40 degrees centigrade.
Optionally, the temperature of described add in-place thermal process is 140 degrees centigrade to 200 degrees centigrade.
Optionally, described time of moving back the add in-place thermal process is 40 seconds to 80 seconds.
Optionally, the atmosphere of described add in-place thermal process is non-oxidizing gas atmosphere.
Optionally, described 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 cross-sectional view of prior art surface oxide layer removal method correspondence;
Fig. 4 to Fig. 9 is the schematic diagram 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 cross-sectional view of the forming process correspondence 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 method of the present invention, feature and advantage can be become apparent more, the specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing.
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, thereby can make the too fast etching process instability that causes of etch rate, 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.
As shown in figure 10, execution in step S1 provides the semiconductor-based end, and described semiconductor-based basal surface has a silicon area at least; Execution in step S2, to carrying out long-range electricity slurry etching in the described 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 described 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 cross-sectional view of described forming process correspondence, 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.
As shown in figure 11, provide the semiconductor-based end 200, have a silicon area at least at described semiconductor-based basal surface.Be example with the semiconductor-based end 200 in the present embodiment with MOS (metal-oxide-semiconductor) memory.Described metal-oxide-semiconductor field effect t comprises source electrode 201, drain electrode 202 and grid 203; Below described grid 203 grid oxic horizon 204 is arranged, the material of described grid oxic horizon 204 is a silica; Be formed with side wall (spacer) 205 in the both sides of described grid 203, the material of described side wall can be a kind of in silica, the silicon nitride; Periphery at described 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; Described grid 203 is a polycrystalline silicon material.
Because described 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, as 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, described grid 203 is a polycrystalline silicon material, and the surface also can be formed with natural oxidizing layer 203a.The thickness of described natural oxidizing layer 201a, 202a, 203a is 25 dust to 45 dusts.Described 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 described natural oxidizing layer 201a, 202a and 203a the oxide on surface, the described semiconductor-based ends 200.
As shown in figure 13, to carrying out long-range electricity slurry etching in the described 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, described fluoride etching agent is at surface condensation of the semiconductor-based ends 200, and preferentially reacts generation fluorine silicon silicate layer 201b, 202b and 203b with described natural oxidizing layer 201a, 202a and 203a.
Described nitrogen fluoride and ammonia react generation fluoride etching agent under the effect of electricity slurry process is as follows:
NF
3+NH
3→NH
4F+NH4F·HF
Described fluoride etching agent and natural oxidizing layer course of reaction are as follows:
NH
4F/NH
4F·HF+SiO
2→(NH
4)
2SiF
6+H
2O
The material of described fluorine silicon silicate layer 201b, 202b and 203b is exactly the (NH in the above-mentioned chemical equation
4)
2SiF
6
In described 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 described 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 described 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 described 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 described 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 described 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 described 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.
As shown in figure 14, the original position heating is carried out at the described semiconductor-based end 200.Fluorine silicon silicate layer 201b, 202b and the 203b on described source electrode, drain and gate surface are the gaseous state product in decomposes more than 70 degrees centigrade, and detached, expose described source electrode 201, drain electrode 202 and the surface of grid 203, finish the removal process of oxide on surface.
The process of described fluorine silicon silicate layer decomposes is as follows:
(NH
4)
2SiF
6→SiF
4↑+NH
3↑+HF↑
Product after described fluorine silicon silicate layer decomposes all be a gaseous state, after described original position heats, the using gases discharger as exhaust pump with as described in gaseous products detach discharge.
Heating process described in the present embodiment is the original position heating, finishes in same semiconductor equipment with long-range electricity slurry etching process before.
The heating-up temperature of described 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 described 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 described 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 described add in-place thermal process is 40 seconds to 80 seconds, and be 60 seconds preferred heating time in the present embodiment.Through described 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, the surface of exposing described source electrode 201, drain electrode 202 and grid 203.
As shown in figure 15, form metal level 206 and cap layer 207 at described semiconductor-based basal surface.
The material of described 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 described cap layer 207 is titanium nitride (TiN), and described cap layer 207 can prevent that metal level 206 ingresss of air are oxidized, and the formation of described cap layer 207 is that optionally this step can be saved.
As shown in figure 16, to carrying out first step annealing in the described semiconductor-based end 200, generate metal silicide 201c, 202c and 203c.
The temperature of described 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 described first step annealing process, the metal material in the described 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.
As shown in figure 17, selective etch (selective etch) is carried out on the surface at the described semiconductor-based end 200, the metal etch that does not have in described cap layer 207 and the metal level 206 and silicon materials react is removed, exposed described 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 described semiconductor-based end 200.
After selective etch,, finish the forming process of metal silicide to carrying out second step annealing in the described 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 described 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%, as seen, 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 fill to form before the tungsten plug cleaning to crystal column surface in contact hole.
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, 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 without departing 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 described semiconductor-based basal surface has a silicon area at least;
To carrying out long-range electricity slurry etching in the described semiconductor-based end, etching gas comprises nitrogen fluoride and ammonia;
To carrying out the original position heating in the described semiconductor-based end;
It is characterized in that the flow of nitrogen fluoride is 2sccm to 10sccm in the described 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 described oxide on surface of claim 1, it is characterized in that: electricity slurry power is 25 watts to 45 watts in the described long-range electricity slurry etching process.
3. according to the removal method of the described 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 described long-range electricity slurry etching process.
4. according to the removal method of the described oxide on surface of claim 1, it is characterized in that: the temperature of described add in-place thermal process is 140 degrees centigrade to 200 degrees centigrade.
5. according to the removal method of the described oxide on surface of claim 1, it is characterized in that: the time of described add in-place thermal process is 40 seconds to 80 seconds.
6. according to the removal method of the described oxide on surface of claim 1, it is characterized in that: the atmosphere of described add in-place thermal process is non-oxidizing gas.
7. according to the removal method of the described oxide on surface of claim 6, it is characterized in that: described non-oxidizing gas is selected from a kind of in nitrogen, helium, argon gas, the hydrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347393A (en) * | 2013-07-30 | 2015-02-11 | 中芯国际集成电路制造(上海)有限公司 | Method for removing natural oxidation layer at bottom of contact window |
| CN106206285A (en) * | 2015-05-29 | 2016-12-07 | 英飞凌科技股份有限公司 | For processing the method for semiconductor layer, for processing the method for silicon substrate and for the method processing silicon layer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050230350A1 (en) * | 2004-02-26 | 2005-10-20 | Applied Materials, Inc. | In-situ dry clean chamber for front end of line fabrication |
| JP4738178B2 (en) * | 2005-06-17 | 2011-08-03 | 富士通セミコンダクター株式会社 | Manufacturing method of semiconductor device |
| 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104347393A (en) * | 2013-07-30 | 2015-02-11 | 中芯国际集成电路制造(上海)有限公司 | Method for removing natural oxidation layer at bottom of contact window |
| CN106206285A (en) * | 2015-05-29 | 2016-12-07 | 英飞凌科技股份有限公司 | For processing the method for semiconductor layer, for processing the method for silicon substrate and for the method processing silicon layer |
| CN106206285B (en) * | 2015-05-29 | 2019-05-28 | 英飞凌科技股份有限公司 | For handling the method, the method for handling silicon substrate and the method for handling silicon layer of semiconductor layer |
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