WO2001075189A2 - Cleaning of a plasma processing system silicon roof - Google Patents
Cleaning of a plasma processing system silicon roof Download PDFInfo
- Publication number
- WO2001075189A2 WO2001075189A2 PCT/US2001/010791 US0110791W WO0175189A2 WO 2001075189 A2 WO2001075189 A2 WO 2001075189A2 US 0110791 W US0110791 W US 0110791W WO 0175189 A2 WO0175189 A2 WO 0175189A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- roof
- cleaning
- etching
- silicon
- particulate matter
- Prior art date
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/32—Gas-filled discharge tubes
- H01J37/32431—Constructional details of the reactor
- H01J37/32798—Further details of plasma apparatus not provided for in groups H01J37/3244 - H01J37/32788; special provisions for cleaning or maintenance of the apparatus
- H01J37/32853—Hygiene
- H01J37/32862—In situ cleaning of vessels and/or internal parts
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4407—Cleaning of reactor or reactor parts by using wet or mechanical methods
Definitions
- Plasma processing systems and especially inductively coupled plasma systems are important in semiconductor processing. Very thin, well controlled layers may be formed and shaped. However, the energies induced in the plasma tend to cause significant erosion and contamination of the chamber, especially the roof of the chamber.
- silicon carbide SiC
- polycrystalline silicon silicon carbide
- IPS inductively coupled plasma sources
- Coatings such as polymer films
- Coatings are often used to further stabilize the surface, and much of the contamination can be removed by ablating or etching the polymer films.
- contaminants also penetrate into the base material, and must be removed or contained.
- HF hydrofluoric acid
- DI water deionized water
- RIE reactive ion etching
- the use of a relatively gentle acid or base such as a trinary system of acetic, nitric, and HF acids, in which the HF is heavily Abuffered ⁇ by milder acids, reduces damage to the grain boundaries of the silicon-based material used for the chamber surfaces.
- the cleaning material can be an acid, in what is often called an acid chemical polishing (ACP), or a base in a base cleaning process (BCP).
- ACP acid chemical polishing
- BCP base cleaning process
- base etching is slower, more selective as a function of the material composition, and very sensitive to the specific polycrystalline structure.
- BCP is also more susceptible to faceting the material being etched, and may shorten the life of the roof being cleaned. Consequently, ACP is preferred.
- Relatively soft materials in a form often call Abeads ⁇ , may be used in the present invention for ablating, sometimes called Abead blastingg (BB), but a purely chemical approach using a relatively mild trinary acidic mixture is preferred. Since the chamber roof material is removed with much less violence, the crystalline structure is believed to be less damaged, resulting in particle counts being reduced.
- the initial ablating is followed, or replaced by, a relatively mild etch, such as with a trinary acid mixture of C 2 H 3 00H (acetic), HNO 3 (nitric) and HF (hydrofluoric), as shown in the figures. The mixture is chosen and adjusted to reduce or even eliminate damage to grain boundaries so that the material grain structure is less prone to fracturing.
- a desirable etch rate is substantially 1 micron per minute, but the achieved rate depends on the characteristics of the silicon roof and may be in a range of about 0.1 to 10 microns per minute.
- the surface roughness or morphology (R A ) is desirably substantially 150, but may be in a range of about 100 to 200.
- the gentle etch of the invention results in less particulate matter being dispersed from the roof in subsequent processing operations. The result is less particulate matter being present on, for example, silicon wafers in semiconductor processing, and has been demonstrated to be below a 100,000 (100K) particles per cubic centimeter baseline for the present invention.
- Another advantage of the present invention is that the particulate matter has been isolated and reduced to the point that it can be quantized, such as by a particulate matter count (PMC) in the deionized (DI) water used for final rinsing of the chamber surfaces.
- PMC particulate matter count
- DI deionized
- Quantity determinations of particulate matter in DI are well known. Relating these measurements, other than in a quantitative way, to particulate matter on wafers has not been known or even suspected.
- the present invention by reducing the PMC well below previous levels, also allows qualitative, rather than the prior art quantitative, measurements, where wafer rejections due to particulate matter can be predicted with considerable accuracy based on the resulting PMC in the water. This results in a reliable qualitative method for determining how many particles can be expected to be deposited on the semiconductor wafers .
- Fig. 1A illustrates an IPS system having an IPS chamber in accordance with the present invention.
- Fig. IB illustrates the energies involved in binding particulate matter to a chamber roof as a function of the chemical structure of the particle.
- Fig. 2 illustrates the dispersion of copper (Cu) in a contaminated chamber roof.
- Fig. 4 is a picture of a surface prepared by bead blasting with SiC and cleaning with a strong HF etch in the prior art at substantially 1000X magnification.
- Fig. 5 illustrates the etch rates of a trinary system of acids when applied to a chamber roof.
- Fig. 6 illustrates particulate matter in water after ultrasonic agitation, both with and without HF clean steps.
- Fig. 7 is a picture at substantially 200X magnification of faceting of a silicon surface after a base cleaning process (BCP).
- Fig. 8 is a picture at substantially 2000X magnification of faceting of a silicon surface after a base cleaning process (BCP).
- Fig. 9 is a picture at 200X magnification of faceting of a silicon surface after an acid chemical polishing (ACP).
- Fig. 10 is a picture at 2000X magnification of faceting of a silicon surface after an acid chemical polishing (ACP).
- Fig. 11 illustrates laser particle counts (LPC) from a silicon roof after BCP operations, and a BKM#2 cleaning.
- LPC laser particle counts
- Fig. 12 illustrates laser particle counts (LPC) from a silicon roof after ACP operations, and a BKM#2 cleaning.
- Fig. 13 illustrates the effectiveness of the present invention in removing metal contamination and particle reduction from a chamber roof for both Base clean and Acid chemical polishing processes.
- Fig. 14 illustrates the effectiveness of the present invention in reducing silicon (Si) particulate count with BCP.
- Fig. 15 illustrates the effectiveness of the present invention in reducing silicon (Si) particulate count with ACP.
- Fig 16 provides an example of a particulate material count (PMC) for a 200 mm silicon wafer in accordance with the present invention.
- the graph at the bottom of the figure gives the PMC in terms of particle size.
- Fig 17 provides an example of a particulate material count (PMC) for a 200 mm silicon wafer in accordance with the prior art.
- the graph at the bottom of the figure gives the PMC in terms of particle size.
- the present invention relates to cleaning of plasma type processing chambers in terms of a complete solution, as opposed to merely improving on a single parameter or problem. It is therefore necessary to consider both reducing contamination levels, especially copper (Cu) contamination, and reducing particulate matter counts, primarily silicon based particles. Cleaning the surfaces, and especially removing Cu from the surfaces, is also crucial in controlling the operation of the chamber.
- the roof, or window, of an IPS when contaminated, changes the coupling of the RF power from the coil to the plasma and results in process drift, which affects controllability. Most sputtered particles are volatile, and are easily removed. Copper, however, is non volatile and is hard to remove from fhe chamber.
- VLSI or ULSI very high level integrated circuits
- Fig. IB shows XPS/ESCA Analysis of Si Roof Particles, which is X-ray Spectroscopy and electron spectroscopy with chemical analysis (XPS/ESCA), which are being used to determine the binding energies and chemical composition of particles in a Si roof for a processing chamber.
- C/S overall particle count
- the first large peak 105 is SiO2 (glass).
- the second large peak 107 is silicon (Si).
- Silicates, SiX, where X may be, for example, a nitride or similar materials, are shown by peak 109. This type of particle is likely not large enough, either in particle size or particle numbers to be of great concern.
- the next peak 111 is likely to be pieces of the silicon carbide (SiC) often used for bead blasting (BB).
- BB is similar to micro scale Asand blasting ⁇ such as for removing paint on buildings.
- the peak 111 is also likely not of any great concern. Additionally, the present invention does not use SiC, and preferably does not use BB.
- Cu forms a heavy surface concentration, and is dispersed to relatively large depths below the surface.
- Cu is shown to be at an unacceptably high concentration 203, such as 1X10 ⁇ 16 atoms/cubic centimeter (cc), at more than substantially 1.5 microns in depth, and in one instance of Fig. 2, nearly 10 microns in depth. It has been determined by the present invention that for some applications, the concentration of Cu contamination is problematic out to about 20 microns in depth, and as a precaution, cleaning of a roof should go out to 50 microns
- Fig. 4 illustrates how the surface of a roof of the prior art as shown in Fig. 3 appears at a much higher magnification.
- a person of ordinary skill in the art would see a solid surface, corifirming that particulate matter dispersal has been rm ' nimized.
- a more informed look at the surface in the light of the present invention shows evidence of flaking 221 from the otherwise smooth surface such as at plateau 223. Viewed in this light, one might expect that the surface is prone to flaking off of particulate matter, which is believed to be the case.
- Fig. 5 shows a HNO3-HF-CH3COOH Trinary Etch Diagram useful for determining etch activity, such as etch rate, on a Si roof of a chamber of the present invention.
- the present invention uses HNO 3 to oxidize Si into SiO 2 to trap contaminants.
- HF is used to remove the SiO 2 formed by the HNO 3
- the C 2 H 3 00H provides wetting of the material to facilitate fhe forming and subsequent removal of the SiO 2 . This is a relatively gentle process with little damage to the silicon based structure of the roof.
- the prior art has depended on SiC BB and a highly concentrated HF cleaning to recover contaminated chamber roof material, and especially roof material contaminated with Cu, which is very difficult to remove from a chamber surface.
- Cu also affects the coupling of the plasma to the RF source, and creates problems with system stability. Intuitively, the combination of harsh ablation of the surface coupled with vigorous (also called strong) etching would appear to result in the most economic and effective way to provide the lowest contamination and the lowest particulate matter.
- the present invention shows that the SiC BB of the prior art results in a weakening of the binding of particles to the roof material. Further, the relatively concentrated HF apparently attacks the grain boundary of the material, especially where the SiC BB has weakened the material, resulting in a high particulate matter count and possible migration of contaminants into the material.
- the invention avoids the weakening of the material of the prior art BB and harsh HF clean. This advantageous result is not apparent with only the use of a softer material in the BB, or with a less vigorous HF etch after a SiC BB. Rather, the primary result of either a softer material in bead blasting or a less vigorous HF etch without the present invention is reducing throughput and co ⁇ espondingly increasing cost. Considerable improvements are seen, however, when both the BB and the HF treatments are properly modified, or if only an optimized base or preferably an optimized acid etch is used in accordance with the present invention, such as at the point 303 in the trinary diagram.
- Fig. 6 is an embodiment of the invention including LPC Particle Count Analysis Si Roof Coupon: Post Bead Blasting and illustrates the effect on particulate matter of a Post HF Clean versus No HF Clean.
- using HF versus not using HF seems to result in equivalent results, but multiple Ultrasonification steps, and in this figure, more than ten ultrasonification steps, indicates degradation due to the use of the prior art methods of using vigorous HF cleaning.
- the present invention uses HF, but with much less vigorous cleaning, in contrast to the prior art. Reduction of the use of HF in cleaning a roof is shown to result in a reduction of particulate matter from the roof in this figure.
- Fig. 8 illustrates BCP as in Fig. 7 with the invention at much higher magnification, showing as long as care is used, damage to fhe crystal boundaries is not very significant.
- faceting which is largely a consequence of the anisotropic etch, is pronounced, with reflecting surfaces in some profusion, but the integrity of the surface is seen to be quite good, with no obvious flaking as in the prior art BB and HF etch process.
- Fig. 9 is a SEM Microstructure Post ACP Treatment Si Coupon #2 and illustrates ACP in accordance with the present invention.
- a rather dull, substantially non reflecting surface is apparent. While there is little or no evidence of pitting or similar problems, the lighter surfaces suggest a relatively rugged surface on a very small scale.
- Fig. 11 is a IPS Roof Metal Concentration level Base Treatment w/o Bead Blasting + BKM2 rinse illustrating an embodiment of the base cleaning of the present invention.
- a Typical BKM (best known method) Clean is compared to a Ceiling Post Base Clean. All significant trace metals are shown reduced in this figure, and the most important contaminant, Cu, is reduced by a factor of more than 20 and is below a baseline level of about 1 X 10 A 10.
- potassium which is not shown for the prior art Typical BKM Clean, all trace metals are shown to be reduced. This reduction is especially important with respect to copper (Cu), since copper has been shown to be a cause of instability in the plasma.
- Fig. 12 is a IPS Roof Metal Concentration level ACP Treatment w/o Bead Blasting + BKM2 rinse illustrating an embodiment of a preferred acid chemical polishing of the present invention.
- a "dirty" roof with, for example, Cu contamination of 112,000,000 X 10 ⁇ 10 atoms per square centimeter, corresponding to 2.8 X 10 ⁇ 17 atoms per square centimeter, is cleaned with ACP.
- the result of the ACP is a large reduction in trace metals over the Typical BKM Clean of the prior art. For example, the reduction of Cu, the most important trace metal contaminant, is by a factor of more than 100.
- the stability of the IPS process which is adversely affected by copper, is improved so that typically, a cleaned roof can be used for nearly 300 (294 confirmed) hours before being cleaned again.
- This advantageous result is achieved with a copper contamination level of less than about 1 X 10 A 10 atoms per square centimeter, such as 0.2 X 10 ⁇ 10 atoms per square centimeter.
- a cleaned roof could be used for only about 200 hours before cleaning was again needed.
- the concentrations achieved reduce the trace metal concentrations to substantially insignificant levels, and restore a roof to essentially the condition of an unused roof with respect to trace metal contamination.
- Fig. 14 is an embodiment of the present invention which illustrates how particulate matter counts are affected by a subsequent BKM#2, that is, the more advanced BKM clean up, after a base etch (BCP) of the present invention.
- BCP base etch
- FIG. 14 it is clear that BCP is an inherently clean process, since very little residue was subject to removal by the BKM#2 process. This is most clearly shown by the difference in particulate matter after 40 minutes of Sonification time, or time in an ultrasonic agitation environment.
- a net change of only 215,698 minus 123,529 particle counts per square centimeter results.
- a further ultrasonification to 70 minutes reduces the PMC well below a baseline of 200,000, and preferably 100,000, particulate matter counts (PMC), both with and without BKM#2 treatment.
- PMC particulate matter counts
- Fig. 15 is an embodiment which illustrates how particulate matter counts are affected by a subsequent BKM#2, that is, the more advanced BKM clean up, after an acid etch (ACP) of the present invention.
- ACP is an inherently clean process, since very little residue was subject to removal by the BKM#2 process. This is most clearly shown by the difference in particulate matter after 40 minutes of Sonification time, or time in an ultrasonic agitation environment.
- a net change of only 263,521 minus 242,936 particle counts per square centimeter, or a little more than 21,000 particle counts per square centimeter results. It will be understood that these numbers are approximate numbers, and will vary in the practice of the present invention.
- a further ultrasonification to 70 minutes reduces the PMC well below a baseline of 200,000 PMC, with or without BKM#2 treatment.
- Fig. 16 is an embodiment of the invention which illustrates a silicon wafer with particles after being processed in a chamber of the invention.
- an embodiment of the present invention achieved a particle count of less than 100K (100,000) particles per milliliter (mL) in water used to rinse the roof surface. It is believed that a particle count that low will result in relatively insignificant problems with particulate matter on the material being processed in a chamber of the present invention, such as a silicon wafer 703. This belief is verified by the almost total absence of particles 705 on the wafer shown, the wafer having a total of four particles 0.2 microns or larger.
- Fig. 17 illustrates by way of contrast the particulate count achieved with the prior art BB and HF etch.
- particulate matter 803 is randomly dispersed on a wafer 805.
- the particulate matter is capable of severely impacting the production, called Ayield ⁇ , of the circuits on this silicon wafer.
- the graph 807 at the bottom of Fig. 17 shows the PMC in terms of size for the wafer.
- the bulk of the particles were about 0.3 microns in diameter, but the diameters range up to about 1.5 microns, with four greater than 1 micron in diameter.
Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP01923089A EP1274876A2 (en) | 2000-04-03 | 2001-04-02 | Cleaning of a plasma processing system silicon roof |
JP2001573061A JP2003534451A (en) | 2000-04-03 | 2001-04-02 | Improved silicon roof cleaning for plasma processing systems |
KR1020027013313A KR20020087477A (en) | 2000-04-03 | 2001-04-02 | Improved cleaning of a plasma processing system silicon roof |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US54117900A | 2000-04-03 | 2000-04-03 | |
US09/541,179 | 2000-04-03 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO2001075189A2 true WO2001075189A2 (en) | 2001-10-11 |
WO2001075189A3 WO2001075189A3 (en) | 2002-02-07 |
Family
ID=24158498
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/US2001/010791 WO2001075189A2 (en) | 2000-04-03 | 2001-04-02 | Cleaning of a plasma processing system silicon roof |
Country Status (4)
Country | Link |
---|---|
EP (1) | EP1274876A2 (en) |
JP (1) | JP2003534451A (en) |
KR (1) | KR20020087477A (en) |
WO (1) | WO2001075189A2 (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003090263A1 (en) | 2002-04-17 | 2003-10-30 | Lam Research Corporation | Silicon parts for plasma reaction chambers |
US7993470B2 (en) | 2003-09-02 | 2011-08-09 | Applied Materials, Inc. | Fabricating and cleaning chamber components having textured surfaces |
CN108172513A (en) * | 2016-11-29 | 2018-06-15 | 台湾积体电路制造股份有限公司 | It is etched using with the room of top plate formed by not oxygen-containing material |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7899627B2 (en) | 2006-09-28 | 2011-03-01 | Lam Research Corporation | Automatic dynamic baseline creation and adjustment |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0680072A2 (en) * | 1994-04-28 | 1995-11-02 | Applied Materials, Inc. | A method of operating a high density plasma CVD reactor with combined inductive and capacitive coupling |
US5647386A (en) * | 1994-10-04 | 1997-07-15 | Entropic Systems, Inc. | Automatic precision cleaning apparatus with continuous on-line monitoring and feedback |
WO1999020812A1 (en) * | 1997-10-21 | 1999-04-29 | Applied Materials, Inc. | Method for cleaning an etching chamber |
-
2001
- 2001-04-02 WO PCT/US2001/010791 patent/WO2001075189A2/en not_active Application Discontinuation
- 2001-04-02 EP EP01923089A patent/EP1274876A2/en not_active Withdrawn
- 2001-04-02 JP JP2001573061A patent/JP2003534451A/en not_active Withdrawn
- 2001-04-02 KR KR1020027013313A patent/KR20020087477A/en not_active Application Discontinuation
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0680072A2 (en) * | 1994-04-28 | 1995-11-02 | Applied Materials, Inc. | A method of operating a high density plasma CVD reactor with combined inductive and capacitive coupling |
US5647386A (en) * | 1994-10-04 | 1997-07-15 | Entropic Systems, Inc. | Automatic precision cleaning apparatus with continuous on-line monitoring and feedback |
WO1999020812A1 (en) * | 1997-10-21 | 1999-04-29 | Applied Materials, Inc. | Method for cleaning an etching chamber |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2003090263A1 (en) | 2002-04-17 | 2003-10-30 | Lam Research Corporation | Silicon parts for plasma reaction chambers |
US6846726B2 (en) | 2002-04-17 | 2005-01-25 | Lam Research Corporation | Silicon parts having reduced metallic impurity concentration for plasma reaction chambers |
US7517803B2 (en) | 2002-04-17 | 2009-04-14 | Lam Research Corporation | Silicon parts having reduced metallic impurity concentration for plasma reaction chambers |
US7993470B2 (en) | 2003-09-02 | 2011-08-09 | Applied Materials, Inc. | Fabricating and cleaning chamber components having textured surfaces |
CN108172513A (en) * | 2016-11-29 | 2018-06-15 | 台湾积体电路制造股份有限公司 | It is etched using with the room of top plate formed by not oxygen-containing material |
US10504720B2 (en) * | 2016-11-29 | 2019-12-10 | Taiwan Semiconductor Manufacturing Company, Ltd. | Etching using chamber with top plate formed of non-oxygen containing material |
US11120986B2 (en) | 2016-11-29 | 2021-09-14 | Taiwan Semiconductor Manufacturing Company, Ltd. | Etching using chamber with top plate formed of non-oxygen containing material |
Also Published As
Publication number | Publication date |
---|---|
EP1274876A2 (en) | 2003-01-15 |
KR20020087477A (en) | 2002-11-22 |
WO2001075189A3 (en) | 2002-02-07 |
JP2003534451A (en) | 2003-11-18 |
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