WO1999036589A1 - Method of cleaning a cvd cold-wall chamber and exhaust lines - Google Patents
Method of cleaning a cvd cold-wall chamber and exhaust lines Download PDFInfo
- Publication number
- WO1999036589A1 WO1999036589A1 PCT/US1998/024124 US9824124W WO9936589A1 WO 1999036589 A1 WO1999036589 A1 WO 1999036589A1 US 9824124 W US9824124 W US 9824124W WO 9936589 A1 WO9936589 A1 WO 9936589A1
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- WO
- WIPO (PCT)
- Prior art keywords
- chamber
- gas
- deposits
- radicals
- chlorine
- Prior art date
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Classifications
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- 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
- C23C16/4405—Cleaning of reactor or parts inside the reactor by using reactive gases
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- 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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
Definitions
- the present invention relates to the field of methods of cleaning a deposition chamber, and more specifically, to a method of removing silicon deposition by-products from internal chamber components and chamber exhaust lines while minimizing the effect on quartz chamber components.
- FIG. 1 A cross-sectional view of a typical single wafer, cold- wall CVD apparatus is shown in Figure 1.
- the Figure shows a thermal reactor 100 for processing semiconductor substrates comprising, a double-dome reactor vessel 114 principally made of quartz that defines a reactor chamber 102, upper 118 and lower 104 quartz chamber liners, gas inlet manifold 106, a gas exhaust manifold 108, exhaust line 109, a radiant heating system 128, a drive assembly 126, a susceptor 124, a wafer 125, and a preheat ring 130.
- Susceptor 124 is larger than wafers processed.
- a 200 mm wafer would be processed on a 240 mm susceptor.
- the gas inlet 106 is coupled to a gas supply of silicon, for example, dichlorosilane (DCS) or monosilane (S-H4), or silane tetrachloride (SiC-4), or trichlorosilane (TCS) and chlorine.
- DCS dichlorosilane
- S-H4 monosilane
- SiC-4 silane tetrachloride
- TCS trichlorosilane
- the pumping means coupled to exhaust line 109 for exhausting chamber.
- chamber processes could be practiced at atmosphere pressure which would not require pumping means to provide chamber exhaust.
- chamber processes could be performed at reduced pressures by utilizing a pumping means to lower chamber pressure.
- the illustrated reactor 100 does not use a plasma for either deposition or cleaning.
- the double dome rector vessel 114 includes a top dome 120 and a bottom dome 116, of quartz which are cooled by circulating cooling air around the outer surface of the quartz. Additionally, cooling water is circulated through the walls of the reactor such that a cold-wall, i.e., T all ⁇ Tprocess/ is maintained. Typical dome temperatures range from about 100°C-600°C.
- the drive assembly 126 is coupled to a motor (not shown) to rotate the susceptor 124 during the deposition process to enhance coating uniformity of the wafer 125 supported on top of the susceptor 124. Temperature measured at the susceptor is commonly used and referred to as process temperature, chamber temperature, deposition temperature or susceptor temperature.
- the cold-wall is an important feature of the single wafer system since it reduces the deposition of semiconductor materials on the interior surface of the upper 120 and lower 116 quartz domes.
- the susceptor 124 is usually constructed of a thin plate for low thermal mass and a surrounding rim for rigidity.
- the diameter of a susceptor in a typical reaction vessel is approximately 1.5 inches larger than the diameter of the wafers being processed.
- a typical susceptor diameter for 200 mm wafers, for example, would be about 240 mm. Even though other wafer diameters are processed such as 150 mm or 300 mm, the susceptor diameter is always larger than the wafer diameter. Thus, a circumferential area is therefore exposed to the depositing semiconductor material.
- the susceptor 124 is typically made of graphite and coated with a silicon carbide coating such that it can be heated up to the deposition temperature without significant contamination.
- the preheat ring 130 substantially seals the gap between the susceptor 124 and the quartz liner 104 and 118 of the reactor vessel 102 to control the heat lost from the edge of the susceptor.
- the preheat ring 130 is made of graphite material coated with silicon carbide for absorbing energy from radiant heating system 128. A quartz preheat ring can also be used.
- the top surface 129 of preheat ring 130 is exposed to the deposition material and therefore accumulates a film of such material due to the fact that the ring is heated to the deposition temperature.
- a reactant gas mixture including a silicon source such as silane, disilane, dichlorosilane, trichlorosilane, or silicon tetrachloride
- a carrier gas such as hydrogen
- H2 or other gas provides positive pressure to the backside of the susceptor and preheat ring to prevent backside silicon deposition.
- HC1 hydrogen chloride
- the chamber is heated from the wafer transfer temperature to a temperature of about 1200°C. Once the chamber reaches 1200°C, above the dissociation temperature of HC1 gas, HC1 is introduced into the chamber. As a result of the high temperature, the HC1 dissociates into reactive hydrogen (H) and chlorine (CI) which will react with the silicon by-products.
- the CI radicals also react with quartz process parts like the quartz dome and liner.
- the quartz dome Since deposition rate is proportional to temperature of the surface and the cooling air keeps the dome several hundred degrees cooler than the susceptor, the quartz dome accumulates deposits at a slower rate than they accumulate on the susceptor and preheat ring. Thus, the quartz components are usually coated to a much lesser degree than other chamber components and could be susceptible to damage from the chlorine radicals with energy levels beyond thermal reaction energy.
- the HC1 flow is stopped and the chamber once again cooled from clean temperature of about 1200°C to a wafer transfer temperature. Although HC1 removes silicon deposits from the chamber components, it does not remove them completely from the system. Instead, when the H/Cl/Si mixture reaches the relatively cooler exhaust line it condenses forming a chlorosilane polymer.
- a method of removing silicon deposits from a cold-wall CVD silicon deposition reactor with a process that does not utilize high temperatures and the necessary thermal transients; can remove chamber deposits without harm to internal chamber components; and can react with and remove polymer residue in the chamber exhaust line.
- the present invention discloses a method of cleaning a CVD cold- wall chamber and exhaust lines.
- a chlorine gas Cl2
- the chamber is maintained at a temperature and pressure which results in chlorine dissociation into radicals while also providing a sufficient density of chlorine radicals to clean chamber internal components without damage to quartz components.
- the chloride radicals react with and remove the by-products from internal components and exhaust lines.
- chlorine gas may be thermally decomposed into radicals of sufficient density to selectively remove byproducts of polysilicon deposition from internal components and exhaust lines.
- chlorine gas may be thermally decomposed into radicals of sufficient density to selectively remove by-products of amorphous silicon deposition from internal components and exhaust lines.
- chlorine gas may be thermally decomposed into radicals of sufficient density to selectively remove by-products of epitaxial silicon deposition from internal components and exhaust lines.
- a chlorine source gas may be thermally decomposed into chlorine radicals of sufficient density to selectively remove by-products of silicon deposition. Things well known regarding CVD equipment features, chamber lines and processing have not been described in detail but can be appreciated by those of ordinary skill in the art.
- Figure 1 is an illustration of a cross-sectional view of a conventional single wafer, cold-wall CVD apparatus.
- FIG. 2 is a block diagram which illustrates the method of the present invention.
- Figure 3 is a table showing silicon removal rates for different temperatures and dilution gases.
- FIG. 1 contains block diagram 200 which sets forth the novel deposition and clean process of the present invention.
- the cleaning process of the present invention is set forth in blocks 202-208.
- the first step of the present invention as set forth in block 201 is to deposit a silicon film in the chamber.
- the silicon film deposition occurs inside a thermal reaction chamber like the one shown in Figure 1.
- a single substrate, like silicon wafer 125, is transferred into chamber 102 and placed on susceptor 124.
- Wafer transfer temperature typically ranges from about 500°C to about 1050°C. Several factors affecting transfer temperature are wafer handler mechanics and metallurgy, anticipated wafer processing temperature, as well as overall system throughput concerns.
- a typical wafer transfer temperature is about 900°C for epitaxial silicon processes while polysilicon could use a transfer temperature of about 650°C.
- lamp sources 128 provide radiant heat which is transmitted through upper 120 and lower 116 quartz domes and are incident upon susceptor 124 and preheat ring 130.
- the susceptor 124 and preheat ring 130 are made of material opaque to the incident radiant energy which absorbs the radiant energy thereby increasing the temperature of susceptor 124 and preheat ring 130.
- Radiant energy from lamps 128 is increased until deposition temperature is reached. The radiant energy creates a region of sufficiently high temperature localized around wafer 125 to result in silicon formation.
- silicon is deposited on the upper surface of preheat ring 129 as well as the outer circumferential portion of susceptor 124 not covered by wafer 125. Deposition temperatures vary depending on desired film deposition. Typical atmospheric epitaxial silicon film is deposited at about 1100°C.
- a silicon source gas is introduced into reactor 102.
- silicon source gases available such as silane, disilane, dichlorosilane and trichlorosilane.
- the silicon source gas is provided via gas inlet 106, which is coupled to a silicon gas supply.
- One such silicon source gas is trichlorosilane (TCS).
- TCS trichlorosilane
- the chamber is purged with an inert gas. Since hydrogen is commonly employed as a carrier gas in silicon deposition processes, the primary concern here is the removal of any residual hydrogen present in the chamber. Residual hydrogen is preferably removed to prevent the exothermic and potentially explosive formation of HCl when the chlorine cleaning gas is later introduced.
- the chamber can be purged with an inert gas such as but not limited to nitrogen, helium or argon. Purge time requirements vary depending on reactor volumes and inert gas flow rate. Representative purge time for a typical 200 mm single wafer CVD cold-wall reactor is about five seconds with helium flowed at 50 standard liters per minute (SLM).
- the next step is to adjust chamber temperature to a temperature sufficient to dissociate the chlorine source gas into chlorine radicals.
- temperature is adjusted by increasing or decreasing intensity of lamps 128 which forms localized regions of sufficiently high temperature which are generally susceptor 124 and preheat ring 130. Localized regions of sufficiently high temperature could also be formed near the surface of quartz domes 120 and 116 by reducing or eliminating cooling air flow.
- Cl2 as a chlorine source gas, any localized temperature above 250 °C will result in chlorine dissociation.
- chamber temperatures at the wafer transfer temperature or within about 75 °C of wafer transfer temperature provide adequate chloride radical density for cleaning as well as provide the added benefit of minimizing throughput impact by limiting thermal transients between wafer transfer temperature and cleaning temperature.
- CI2 chlorine gas
- advantageous chlorine radical densities can be obtained in the temperature range between 250° to 1050°C.
- chlorine gas (CI2) is provided to the chamber.
- the chlorine gas (CI2) is provided to the chamber from some bulk supply in a manner similar to a method for providing other semiconductor process gases.
- the bulk supply is coupled to the chamber via gas inlet 106.
- the chlorine gas (CI2) supplied for the cleaning process should be of sufficient purity so as not to introduce a source of contamination into the processing environment. Typical purity value when Cl2 is used as a source gas is greater than 99.998% by volume.
- the amount of chlorine gas provided to the chamber is controlled by a flow control device.
- One such device is a mass flow controller (MFC).
- a representative flow rate for chlorine gas (CI2) is 20 liters per minute although chlorine flow rates between 1 and 100 SLM have been used with advantageous results.
- the chlorine source gas may be preferably diluted by flowing an inert gas such as argon, helium or nitrogen.
- a typical dilution flow rate for 20 SLM of chlorine gas (CI2) is 2 SLM of helium.
- the next step is to adjust chamber pressure.
- a typical pressure control device is a throttle valve located between the chamber exhaust and chamber process pump. Chamber pressure is monitored and the throttle valve opens and closes to regulate chamber pressure. Advantageous results have been achieved when chamber pressure is maintained at atmospheric pressure as well as at reduced chamber pressures as low as 10 Torr.
- blocks 203, 204, and 205 have been shown and described serially only for clarity in explaining the method of the present invention. In practicing the present invention, one skilled in the art could perform the steps described in blocks 203, 204, and 205 in a different order or nearly simultaneously.
- the next step, as set forth in block 206, is to thermally decompose chlorine gas (Cl2) into chlorine radicals.
- This analysis yields a chlorine radical density at 750°C of about 7.7 x 10 12 atoms/cm 3 and at 1000°C of about 3.2 x 10 13 atoms/cm 3 in the hot zone above the susceptor.
- the equilibrium gas phase assumption is more accurate in the localized regions of high temperature where the temperature is closest to the susceptor temperature and the temperature used in the above calculation.
- the radical density decreases dramatically.
- the highest radical density expected would be about 7.7 x lO ⁇ 2 atoms/cm 3 near the susceptor and preheat ring while the density near cooled quartz walls would be several orders of magnitude less. If cooling air were reduced or eliminated from the quartz walls such that the temperature of the quartz is allowed to increase to the temperature of the susceptor and preheat ring, then radical densities of the same magnitude found at the susceptor and preheat ring could be formed near the quartz dome surface.
- the chlorine radicals are only thermally activated and not ionized by RF energy, or any other ionizing sources. As such, there are only negligible ionized species present in the chamber. These ionized species, if present at all, contribute only marginally, if at all, to the cleaning process of the present invention. Also, since thermally activated radicals lack the high energy and directional component of ionized species generated by RF energy and only thermally activated radicals are used in the present invention, the sputtering effect caused by ionized species impinging on internal chamber components leading to damage and premature wear is not present. Minimization of the sputtering effect could also be illustrated by comparing thermally generated to plasma generated radical densities.
- radicals formed by thermal decomposition of chlorine at 750 °C have a density in the localized region of high temperature of about 7.7 x lO ⁇ 2 atoms/cm 3 while it is generally held that plasma generated radicals have a density of about 1 x 10 ⁇ atoms/cm 3 .
- the density of the thermally formed chlorine radicals is over one order of magnitude less than the density of the plasma generated chlorine radicals.
- the thermally activated radical density could be many orders of magnitude less than the plasma generated radical density.
- thermally activated radicals are of lower density than plasma generated radicals and are therefore less likely to damage internal components or result in increased component wear.
- chlorine (Cl2) will thermally decompose at 250°C into chlorine radicals, other temperatures may be advantageous. Chamber temperatures within about 75°C of wafer transfer temperature, typically ranging from about 500-1050°C, yield adequate radical densities to selectively clean the quartz domes and liners while minimizing the time needed to thermally transition the chamber temperature from the transfer temperature to the cleaning temperature. Other combinations of chamber temperature, pressure and chlorine gas flow rate will produce advantageous chlorine radical densities.
- the chlorine radicals will react with and remove the silicon and silicon polymers.
- Some of the chlorine radicals will react with the silicon deposits on the susceptor 124, the preheat ring 130 and other internal components by attaching to the silicon to form SiCl and SiCl2- Some of the SiCl will react with a chlorine radical and form SiCl2 which will condense and polymerize when it reaches the relatively cooler temperature of the exhaust line. In much the same way, some of the chlorine radicals react with silicon deposits on the quartz domes 120 and 116 and quartz chamber liners 104 and 118. However, since the chlorine radicals were only thermally activated and not ionized, the silicon removal /SiCl formation process on the quartz components is much less likely to result in damage to the quartz.
- thermally activated chlorine radicals have enough energy to dislodge the silicon deposit from the quartz and form SiCl. However, it is unlikely enough energy would remain to sputter the quartz. Thus, because of their lower energy and lack of ionized species, thermally activated chlorine radicals are sufficiently reactive to selectively remove silicon from quartz without damage to the quartz. Just like the silicon removal from other portions of the chamber, the silicon deposits removed by the chlorine radicals from the quartz components will also form SiCl and SiCl2 and polymerize in the exhaust line.
- Sample silicon removal times using chlorine gas are set forth in Table 3.
- Some representative silicon removal rates at 1 atmosphere, 20 SLM chlorine (CI2) diluted with 2 SLM He are: 11 ⁇ m/min. at 600°C and 14 ⁇ m/min. at 800°C.
- 20 SLM chlorine (CI2) diluted with 2 SLM 2 silicon was removed at: 4 ⁇ m/min. at 600°C and 18 ⁇ /min. at 800 °C.
- a representative clean time for about 2.0 ⁇ m of silicon deposition on a wafer is about 20 seconds at a chamber temperature of 740°C, atmospheric pressure and chlorine flow rate of 20 SLM diluted with 2 SLM of He.
- Chlorine gas (CI2) flow times may vary. It is important to note that the chlorine radicals should be created for a sufficient time to ensure the removal of all unwanted silicon by-product while limiting unnecessary exposure of chamber components to chlorine radicals.
- the next step of the present invention is to purge the chamber with inert gas to remove residual chlorine radicals prior to resuming deposition processing.
- the preferred intent is to avoid the combination of hydrogen and chlorine and the exothermic and potentially explosive formation of HCl.
- the potential combination exists since chlorine was just used as a cleaning gas and hydrogen is a commonly used carrier gas for silicon deposition processing.
- the chamber should be purged with an inert gas for sufficient time to remove any residual chlorine. Purge times will vary with inert gas flow rate and chamber volume. Typical purge cycle time for a 200 mm conventional single wafer cold-wall CVD reactor (shown in Figure 1) would be about 5 seconds with an inert gas such as helium flowed at a rate of 50 SLM.
- the final step of the present invention is the resumption of the deposition process cycle where a silicon film is deposited in the chamber.
- the chamber temperature is adjusted to the wafer transfer temperature which is typically in the range between about 500°C and about 1050°C. Once the wafer transfer temperature is attained, a wafer 125 will be placed on susceptor 124. Lamps 128 will provide radiant energy into chamber 102 until the chamber deposition temperature is reached.
- Deposition temperature varies depending on silicon film type. Typical epitaxial silicon deposition temperatures are about 1100°C. Once the deposition temperature is achieved, a silicon source gas is provided into chamber 102 via gas inlet 106.
- silicon deposition occurs. Deposition rate varies upon chamber temperatures, silicon source gas, source gas flow rate and chamber pressure. Numerous silicon source gases are available such as monosilane, disilane, dichlorosilane, trichlorosilane or silicon tetrachloride. One such source gas is trichlorosilane (TCS). When flowed at 11 SLM in a chamber at 760 Torr and 1100°C, TCS forms epitaxial silicon.
- TCS trichlorosilane
- the deposition process results in film formation on the wafer 125 but also results in silicon deposition on preheat ring 129, outer circumference of susceptor 124, and to a lesser extent, because they are cooler, quartz components such as upper 120 and lower 116 domes and chamber liners 104 and 118. Silicon formation on the chamber components could have detrimental impact on process repeatability because coating on the domes interferes with radiant energy transmission and any flaking deposits would generate particles which ruin wafers and negatively impact device yield.
- chlorine source gases are expected to demonstrate similar advantageous qualities of the present invention such as but not limited to the ability to dissociate into chlorine radicals at or near wafer transfer temperatures and to assist in the removal of chlorosilane polymers from the exhaust line.
- Chlorine source gases such as SiCl4 and CIF3 would be anticipated to provide similar benefits as described in the present invention and in much the same way as chlorine gas (G2).
- G2 chlorine gas
Abstract
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Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2000540289A JP2003526731A (en) | 1998-01-13 | 1998-11-12 | Method for cleaning CVD cold wall chamber and exhaust line |
EP98957860A EP1047808A1 (en) | 1998-01-13 | 1998-11-12 | Method of cleaning a cvd cold-wall chamber and exhaust lines |
KR1020007007741A KR20010034128A (en) | 1998-01-13 | 1998-11-12 | Method of cleaning a cvd cold-wall chamber and exhaust lines |
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US09/006,463 | 1998-01-13 | ||
US09/006,463 US6042654A (en) | 1998-01-13 | 1998-01-13 | Method of cleaning CVD cold-wall chamber and exhaust lines |
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WO1999036589A1 true WO1999036589A1 (en) | 1999-07-22 |
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PCT/US1998/024124 WO1999036589A1 (en) | 1998-01-13 | 1998-11-12 | Method of cleaning a cvd cold-wall chamber and exhaust lines |
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US (1) | US6042654A (en) |
EP (1) | EP1047808A1 (en) |
JP (1) | JP2003526731A (en) |
KR (1) | KR20010034128A (en) |
WO (1) | WO1999036589A1 (en) |
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Also Published As
Publication number | Publication date |
---|---|
KR20010034128A (en) | 2001-04-25 |
EP1047808A1 (en) | 2000-11-02 |
JP2003526731A (en) | 2003-09-09 |
US6042654A (en) | 2000-03-28 |
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