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    • 专利摘要:
    A method of depositing a dielectric film on a substrate in a process chamber of an inductively coupled plasma-enhanced chemical vapor deposition reactor. The gap between the conductive lines on the semiconductor substrate can be filled and a cap layer can be deposited. By heating the substrate support means in which the substrate is placed in the process chamber, it is possible to produce a film with reduced film stress and significantly improved physical properties.
    公开号:KR20000062317A
    申请号:KR1019997005753
    申请日:1997-12-22
    公开日:2000-10-25
    发明作者:셔플보담폴케빈；맥밀린브라이언；디모스알렉스티.；구옌후옹；베르니부치；벤-도르모니크
    申请人:리차드 에이치. 로브그렌；램 리서치 코포레이션；
    IPC主号:
    专利说明:

    Inductively coupled plasma CVD
    Chemical vapor deposition (CVD) is a technique commonly used to form various thin films in semiconductor integrated circuits. CVD can form a high purity, high quality thin film such as SiO 2 , Si 3 N 4 , Si, or the like. In the reaction step of forming a thin film, the reactor in which the semiconductor substrate is placed is heated to a high temperature of 500 to 1000 ° C. The raw material to be deposited is supplied into the reactor in gaseous form, and gaseous molecules are thermally decomposed and then combined in a gaseous state on the substrate surface to form a thin film.
    The plasma-enhanced CVD apparatus uses a plasma reaction similar to that in the CVD apparatus as described above, but forms thin films at lower temperatures. The plasma CVD apparatus includes a process chamber consisting of a plasma generating chamber, a gas introduction system and an exhaust system, which may be part of or separate from the reaction chamber. In the apparatus, the plasma may be generated from various plasma sources. Substrate support means are provided in the reaction chamber that may include an RF biasing element that applies a radio frequency (RF) bias and a cooling mechanism to prevent the temperature of the substrate from rising by plasma action.
    Vacuum processing chambers are generally used for supplying a deposition gas to a vacuum chamber to chemically deposit a material on a substrate and for applying an RF field to the gas. For example, parallel plates and electron-cyclotron resonance (ECR) reactors are commonly used. See US Pat. Nos. 4,340,463 and 5,200,232. During processing, the substrate is held in place in the vacuum chamber by the substrate support means. Conventional substrate support means include mechanical clamps and electrostatic clamps (ESC). Examples of mechanical and electrostatic substrate support means are disclosed in US Pat. No. 5,262,029 and US Patent Application No. 08 / 401,524, filed March 10, 1995.
    Plasma-enhanced chemical vapor deposition (PECVD) is used to deposit intermetallic dielectric layers used in integrated circuits at low temperatures. M. Gross et al. (“Silicon dioxide trench filling process in a radio-frequency hollow cathode reactor”, J. Vac. Sci. Technol. B 11 (2), Mar / apr 1993) have shown that low frequencies (1 MHz), a method of filling silicon trenches without voids using a hollow cathode reactor where silane gas is supplied through a normal target that releases oxygen and xenon at low pressure (˜0.2 Pa). Is disclosed. In this method, a trench with a 1 micron opening and an aspect ratio of up to 2.5: 1 is filled at a rate of 400 μs / min by causing surface adsorbates and ion induced reactions due to high ion bombardment and low gas phase reaction rates and growing an oriented oxide film. .
    P. Shufflebotham et al. ("Biased Electron Cycloyron Resonance Chemical-Vapor Deposition of Silicon Dioxide Inter-Metal Dielectric thin Films," Materials Science Forum Vol. 140-142, 1993). In Enhanced Chemical Vapor Deposition (ECR-CVD) systems, a high aspect ratio gap of less than 0.5 microns can be achieved by applying an intermetallic dielectric (IMD) onto a wafer up to 200 mm in diameter using an O 2 -Ar-SiH 4 gas mixture. Disclosed is a one-step low temperature gap filling method capable of filling with SiO 2 . The one step method replaces the sequential gap filling and flattening step of CVD SiO 2 with a plasma etch-back step, which has a gap width of 0.5 microns or less and an aspect ratio (gap height: width) of 1.5. It is not suitable for gaps larger than 1: 1.
    Prior art devices have some serious drawbacks in IMD applications. ECR and helicon sources rely on complex and expensive magnetic field arcs. Moreover, the magnetic field may damage the semiconductor element on the wafer. In addition, ECR, helicon, and helical resonator sources generate plasma at some distance from the wafer, making it difficult to simultaneously produce a uniform, high-purity film, and perform plasma cleaning to control particulates in situ without additional equipment. Is difficult.
    The present invention relates to a method and apparatus for high density plasma-enhanced chemical vapor deposition of semiconductive and dielectric films, and more particularly, to depositing the film in a large aspect ratio gap on a semiconductor substrate, such as a silicon wafer having a metallization layer. It is about technology to do.
    The invention will be explained in more detail with reference to the accompanying drawings, in which like elements are denoted by like reference numerals.
    1 is a schematic diagram of a high density inductively coupled plasma reactor that may be used to practice the method according to the present invention.
    2 shows the FTIR spectra of films deposited at various oxygen to silane feed flow rates (total flow rate constant).
    3A, 3B, 3C and 3D are scanning electron micrographs (SEM) images of decorated samples to exaggerate defects in the film; The structure consisted of polysilicon on oxide and all samples were deposited for 3 minutes except for the 3a sample deposited for 1 minute.
    4 shows a plasma reactor with a gas supply system.
    5 shows an injector of the gas supply system.
    The present invention relates to a process using inductively coupled plasma-enhanced chemical vapor deposition (IC PECVD) high density plasma systems. The system is compact, washable in place, and provides high quality semiconductor and dielectric films.
    According to one aspect of the invention, there is provided a method of filling a gap between conductive lines on a semiconductor substrate, the method comprising providing a substrate to a process chamber of an inductively coupled plasma-enhanced chemical vapor deposition reactor that may comprise a substantially planar induction coil. step; Supplying a process gas to the process chamber, which may include an amount of inert gas sufficient to aid gap filling; And growing a dielectric film on the substrate such that the dielectric film is deposited in a gap between conductive lines on the substrate.
    According to another aspect of the present invention, there is provided a method of filling a gap between conductive lines on a semiconductor substrate, the method comprising providing a substrate to a process chamber of an inductively coupled plasma-enhanced chemical vapor deposition reactor that may comprise a substantially planar induction coil. step;
    (i) supplying a first process gas that may comprise an amount of inert gas sufficient to aid gap filling; And (ii) filling the gap between conductive lines on the substrate by growing a first dielectric film in the gap at a first deposition rate; And
    Supplying a second process gas to the process chamber to deposit a capping layer comprising a second dielectric film on the first dielectric film at a second deposition rate greater than the first deposition rate. Provide a method.
    According to another aspect of the present invention, there is provided a method comprising: providing a substrate in a process chamber of an inductively coupled plasma-enhanced chemical vapor deposition reactor and placing the substrate on substrate support means; Supplying a process gas to the process chamber, which may include an amount of inert gas sufficient to aid gap filling; Adjusting a surface temperature of the substrate support means; And applying dielectrically inductively coupled RF energy to the process chamber to energize the process gas into a plasma state to grow a dielectric film on the substrate. .
    According to another aspect of the present invention, there is provided a plasma processing chamber, substrate supporting means for supporting a substrate in the processing chamber and maintaining a temperature of about 80 to 200 ° C, a conductive coil disposed outside the processing chamber, and the processing chamber. Means for supplying a process gas to the process chamber, and an RF energy source for inductively coupling RF energy into the processing chamber to energize the process gas into a plasma state.
    Depending on the film to be deposited. The process gas may comprise a silicon containing reactive gas selected from the group consisting of SiH 4 , SiF 4 , Si 2 H 6 , TEOS, TMCTS, and mixtures thereof. The process gas may comprise a reactive gas selected from the group consisting of H 2 , O 2 , N 2 , NH 3 , NF 3 , N 2 O, NO 3, and mixtures thereof. In other cases, the process gas may comprise a reactive gas selected from the group consisting of boron containing gas, phosphorus containing gas and mixtures thereof. More preferably, the process gas may further comprise an inert gas such as argon.
    One feature of the invention is that the inductively coupled plasma is generated by a flat coil shaped RF antenna. That is, the IC PECVD reactor is easy to scale up, for example, to scale up to accommodate 300 mm wafers and 600 mm x 720 mm flat panel displays. Inductively coupled plasma (ICP) sources generate a uniform high density plasma over a large area regardless of the bias power used to control ion sputter energy. Unlike ECR or helicon sources, no magnet is required.
    1 shows an ICP reactor 20 capable of treating a substrate with a high density plasma, and a suitable reactor includes a LAM Research Corp. TCP (trademark) system based in Fremont, California. See US Patent No. 4,948,458 to Ogle, incorporated herein by this reference. The reactor includes a process chamber 21 for generating a plasma adjacent to the substrate 23. The substrate is supported on a water-cooled substrate support means 24 and the temperature of the substrate is adjusted by supplying helium gas through the conduit 25 to the space between the substrate and the substrate support means. The substrate support means may comprise a heat-treated anodized aluminum electrode, or a ceramic material having a buried electrode, which electrode is powered by an RF source 26 and an associated circuit 27 to provide RF matching and the like. Is supplied. The temperature of the substrate during processing is monitored by a temperature measuring device 28 attached to a temperature probe.
    A turbo pump is connected to the outlet port 30 to apply vacuum to the chamber 21, and a pressure regulating valve can be used to maintain the desired vacuum pressure. Process gas may be supplied to the chamber through conduits 31 and 32 that supply the reactive gas to a gas distribution ring extending around the lower dielectric window, or through a dielectric window showerhead. The external ICP coil 34 located outside the chamber in close proximity to the window is supplied with RF power by an associated circuit 36 for impedance matching with the RF source 35. As shown, the outer induction coil is substantially flat and generally includes a single conductive element made of a flat spiral or a series of concentric ring shapes. The plate-shaped structure can be used to accommodate a larger substrate by increasing the length of the conductive element to increase the diameter of the coil, or to install a plurality of coils to generate a uniform plasma over a wide area. Easy to scale up When the substrate is processed in the chamber, the RF source 35 supplies the coil 34 with an RF current of about 100 kHz-27 MHz, more preferably 13.56 MHz, and the RF source 26 provides about the bottom electrode. The RF current is supplied at 100 kHz-27 MHz, more preferably 400 MHz, 4 MHz or 13.56 MHz. By supplying RF power to the electrode a large DC sheath voltage can be provided over the substrate surface.
    When an RF bias is applied to the substrate in the gap filling step, ion bombardment of the growth film is caused. The RF frequency can be any value beyond what is needed to sustain a steady state sheath that is hundreds of kHz. Substrate bias provides numerous advantages in the properties of the film and can also be used to sputter the growth film in the gap filling step simultaneously. In this case, a narrow, high aspect ratio gap can be quickly filled with a high density dielectric. RF bias can also be used for cap layer deposition.
    Reactor 20 is a gap filling method according to the present invention, which increases the etch-to-deposition rate (EDR) using a heavy inert gas to fill gaps with a large aspect ratio of 0.5 microns or less without voids. It can be used to practice. The gap filling method is pending in the applicant's application on March 29, 1996, and is described in more detail in US Application No. 08 / 623,825, "Advanced Method for High Density Plasma CVD Gap Filling," incorporated herein. . Heavy inert gases are effective for sputtering corners of the gap side walls, ie corners cut at an angle of 45 degrees. The inert gas reduces the power required to fill a given gap structure because the inert gas forms heavy ions that have a low ionization potential and increase the sputtering rate relative to the deposition rate at a given RF power. In addition, the low ionization potential of the inert gas assists in plasma evolution, allowing more uniform ion bombardment across the substrate. Xenon is most preferred as the inert gas because xenon is the heaviest of the non-reactive inert gases. Krypton is lighter than xenon and has a higher ionization potential but can be used. Argon can also be used as the inert gas. The amount of inert gas supplied is preferably effective to provide a sputter etching component of similar size to the deposition rate such that the etch deposition rate is preferably 5 to 70%, more preferably 10 to 40%.
    In carrying out the deposition process in an ICP-CVD reactor, the chamber may be maintained at a vacuum pressure of less than 100 mTorr, preferably up to 30 mTorr, more preferably about 1 to 5 mTorr. The flow rate of the individual components of the process is generally 10 to 200 sccm for 200 mm substrates and can be greater for larger substrates. A turbomolecular pump throttled by the gate valve is used to regulate the process pressure. The relative amounts of the individual components depend in part on the stoichiometry of the component (s) being deposited. The ICP power is preferably 200 to 3000 watts and the RF bias power is about 0-8 watts / cm 2 , preferably at least 2 watts / cm 2 . For example, a heat transfer gas comprising helium and / or argon is supplied at a pressure of 1 to 10 Torr to bring the temperature of the substrate to preferably about 20 to 500 ° C., more preferably about 100 to 400 ° C., most preferably Maintain at about 150 to 375 ° C.
    Heated mechanical or preferably electrostatic chucks (ESCs) are used to hold the substrate to prevent damage to metallization or existing films and structures on the substrate and for accurate and precise process control. It is preferable that ESC is bipolar or unipolar. Preferably, to maintain the temperature of the wafer at 325 to 375 ° C., the electrode is maintained at a temperature of about 50 to 350 ° C. The temperature of the preferred electrode depends in particular on the RF bias level and the specific deposition step. For example, in the gap filling step, it is desirable to maintain the temperature of the electrode at about 80 ° C. (full bias) to 200 ° C. (no bias). Similarly, the capping step is preferably maintained at about 125 ° C. (full bias) to 350 ° C. (no bias). Gap filling and capping steps are described herein. Suitable chucks for temperature control are pending, filed on September 30, 1996 by Brian McMillin, and are disclosed in the patent application "Various High Temperature Chuck for High Density Plasma Chemical Vapor Deposition" incorporated herein.
    During deposition, the substrate (eg, wafer) generally maintains a higher temperature than the ESC due to plasma heating. Thus, even if the ESC is heated, its temperature is lower than that of the substrate. The electrode preferably provides helium back cooling for temperature control of the substrate. The temperature of the substrate can be controlled by adjusting the RF bias and ESC temperature or other variables mentioned herein. As will be described in more detail in the Examples herein, the temperature of the electrode can have a significant impact on the physical properties of the film being deposited.
    ICP-CVD reactors are particularly suitable for SiO2 deposition for IMD applications, in which the quality of the films produced is substantially indistinguishable from SiO2 grown by thermal oxidation (thermal oxide) of crystalline Si. In addition, the method can fill a narrow width of 0.25 microns with a 3: 1 aspect ratio gap or a wider gap with a high quality material. In addition, the deposition temperature can be 450 ° C. or less for compatibility with aluminum metallization, and the thickness uniformity is 2% i− on 8 in (20.32 cm) wafers without substantially changing other film properties. Better. Finally, in process productivity, ICP-CVD has a deposition rate of 5,000 mW / min or more in the gap filling step. For the cap layer up to about 1.5 μm / min provides a deposition rate while maintaining good uniformity. The conductive lines can of course be made of other suitable materials, including, for example, copper, tungsten and mixtures thereof.
    By the method according to the invention, the method of depositing SiO 2 in a gap with a high aspect ratio of 0.5 microns or less comprises a simultaneous SiO 2 deposition and sputtering step. As a result, anisotropic deposition fills the gap from the base, and the angle dependence of the sputtering yield prevents the top of the gap from pinching off during deposition. One of the key features of most high density plasma systems is that bias power determines the sheath voltage on the wafer, essentially independent of plasma generation. High bias power generates a large sheath voltage, thus causing a strong ion bombardment on the wafer surface. In the absence of an RF bias, the jagged appearance of the sidewall film results in poor film quality and gapfill performance. That is, a very porous and heavy deposit is deposited on the metal interconnects, which prevents the deposition on the deeply dug base and eventually breaks out of the gap and leaves voids.
    ICP can generate a high density plasma (eg, greater than about 1 × 10 11 ions / cm 3 ) while maintaining a very low pressure (eg, less than about 10 mTorr). Advantages of high density PECVD include increased throughput, uniform ion and radical density over a large area, and ease of manufacture of subsequently scaled up reactors. If separately provided with RF biasing of the substrate electrode, the ICP-CVD system can independently control the ion impact energy and more freely control the plasma deposition step.
    In an ICP system, the growth of SiO 2 film proceeds by an ionic activity between oxygen species impinging on the wiper from the plasma source and silane fragments adsorbed on the wafer. The use of ICP-CVD allows filling gaps with high aspect ratios of less than 0.5 microns on 8 inch (20.32 cm) diameter wafers with high quality SiO 2 dielectrics. In essence, it provides an easy to fabricate ICP-CVD intermetallic dielectric CVD process using high density plasma.
    Process gas distribution system
    For high density plasma PECVD, it has already been described that the use of a gas distribution system capable of supplying a uniform but high amount of reactive gas to the substrate surface can increase the deposition rate and at the same time minimize the need for chamber cleaning. Preferred gas distribution systems are described in U.S. Application Serial No. 08 / 672,315, filed June 28, 1996 by Brighter McMillin et al. "Intensive, temperature-controlled plasma processing system and high density plasma chemical vapor deposition of dielectric films."
    4 shows a plasma processing system including such a gas distribution system. The system includes a substrate support 130 and a processing chamber 140. The support means may comprise, for example, an RF biased electrode. The support means can be supported by the lower end wall of the chamber or cantilevers extending from the side wall of the chamber. The substrate 12 may be mechanically or electrostatically clamped to the electrode.
    The system further includes an antenna 150 or other shaped antenna, such as a flat multi-rotational coil as shown in FIG. 4, which antenna inductively couples RF energy into the chamber to provide a high density plasma. Powered by the source and a suitable RF impedance matching circuit. The chamber may comprise a vacuum pumping device suitable for maintaining the interior of the chamber at a desired pressure. As shown in FIG. 4, a dielectric window or a non-planar dielectric window, such as a flat dielectric window 155 of uniform thickness, is provided between the antenna 150 and the interior of the processing chamber 140 at the top of the processing chamber. A vacuum wall can be formed.
    The first gas ring 170 is provided below the dielectric window 155. Gas ring 170 may be mechanically attached to the chamber housing above the substrate. Gas ring 170 may be made of, for example, aluminum or anodized aluminum. The second gas ring 160 may also be provided below the dielectric window 155. One or more gases, such as argon and oxygen, are supplied through the outlet of the second gas ring 160. Any suitable gas ring can be used for the second gas ring 16. As shown in FIG. 4, the second gas ring 160 may be separated by an optional spacer 165 made of aluminum or anodized aluminum and positioned on the gas ring 170. Alternatively, although not shown, the second gas ring 160 may be positioned between the gas ring 170 and the substrate 120, beneath the gas ring 170, or the gas may be injected vertically from the chamber floor. It may be positioned below the substrate 120 in a direction that can be. Alternatively, argon and oxygen may be supplied through an outlet connected to the chamber floor having a spacer 165 separating the dielectric window 155 and the first gas ring 170.
    A plurality of removable injectors 180 are connected to the first gas ring 170 to supply associated silicon-containing gases such as SiH 4 or SiF 4 , TEOS, and the like. These gases are supplied from the injector 180 to the substrate via the injector outlet orifice 187. In addition, the reactive gas may be supplied through an outlet of the first gas ring 170. The injector may be made of ceramics such as aluminum, anodized aluminum, quartz or Al 2 O 3 . Although only two injectors are shown, any number can be installed. For example, an injector may be connected to each outlet of the first gas ring 170. Preferably, 8 to 32 injectors are used in 200-210 mm diameter rings for 200 mm substrates.
    The injector 180 is positioned above the substrate 12 such that the orifice is spaced a predetermined distance from the substrate, for example, 3 to 10 cm. According to a preferred embodiment, the injector may be spaced apart from the inside or outside of the periphery of the substrate, for example 0-5 cm from the periphery of the substrate. This is to ensure that any potential particle fragments from the inlet do not fall on the substrate and contaminate the substrate. The lengths of the injectors can all be the same or a combination of different lengths to increase deposition rate and uniformity. The injector is preferably oriented such that a portion of the injector supplies the process gas in a direction that crosses the exposed surface of the substrate.
    Unlike the design of the gas supply system, which preferentially distributes the gas over the substrate, the injector according to another embodiment of the invention is oriented to supply the gas in a direction that intersects the exposed surface of the substrate at an acute angle. The injection angle may be about 15 to 90 degrees, preferably 15 to 45 degrees from the horizontal plane of the substrate. The injection angle or axis may be parallel to the axis of the injector, or alternatively, may have an angle of 90 degrees or less relative to the axis of the injector. The outlet orifice diameter of the injector may be 0.010 to 0.060 inch, preferably about 0.020 to 0.040 inch. The hollow core of the injector 180 can be drilled to about twice the diameter of the outlet orifice 187 to allow sonic flow to occur at the outlet orifice and not within the core of the injector. The flow rate of SiH 4 is preferably 25-300 sccm for 200 mm substrates and may be greater for larger substrates.
    Another gas supply system using a plurality of injectors is shown in FIG. 5. In this embodiment, the orifice 187A is oriented to supply gas along the injection axis A (toward the dielectric window) in the direction away from the wafer 120A. The injection angle or axis may be parallel to the axis B of the injector, or alternatively at an angle of 90 degrees or less, or more, with respect to the axis of the injector. In such a structure, the implant axis may have an angle of about 5 to 90 degrees, preferably 15 to 75 degrees, most preferably 15 to 45 degrees with respect to the substrate. This structure is characterized by a process gas concentrated on the wafer to increase the deposition rate and good uniformity. It also provides the advantage that the sensitivity to orifice shielding is relaxed. The reduced likelihood of orifice shielding allows more wafers to be processed until injector cleaning is needed, ultimately increasing wafer throughput.
    Since the orifice size is small and the number of injectors is small and the flow rate of SiH 4 is large, the pressure difference between the gas ring 170 and the inside of the chamber is large. For example, if the pressure in the gas ring exceeds 1 Torr and the pressure inside the chamber is about 10 mTorr, the pressure difference is about 100: 1. This results in choked sound flow at the injector outlet. The inner orifice of the injector may be shaped to provide supersonic flow at the outlet.
    Injecting SiH 4 at sonic speed can prevent plasma from penetrating the injector. This structure prevents the SiH 4 from being plasma-induced decomposition, forming amorphous silicon residues in the gas ring and the extension tube of the injector.
    Example
    Processes for gap fill and cap layer deposition generally include an initial optional sputter clean / preheat step and a high bias power gap fill step in the plasma without any silicon containing gas. After the gap is partially filled, the final sacrificial layer or “cap” layer of the film is deposited, preferably at low RF bias power. Preferably, prior to depositing the cap layer, substantially all or at least most of the gap is filled in the gap filling step. The cap layer deposition step requires only a bias power sufficient to prevent sputtering while film growth is required so that the quality of the film is properly maintained. The cap layer is deposited at a higher rate than the gap filling step. Preferably, this cap film is removed in a subsequent chemical-mechanical polishing (CMP) flattening step.
    The IC PECVD system generates a high density, low pressure plasma in a process gas comprising a semiconductor or dielectric and a component forming a cap film. The process of the present invention is suitable for any suitable semiconductor, dielectric and / or cap film such as hydrogenated amorphous silicon Si: H, silicon oxide SiO x , where x is 1.5 to 2.5, silicon nitride SiN, silicon fluoride SiO x F y Provided that x is 1.5 to 2.5 and y is 2 to 12 and mixtures thereof. Both stoichiometric and non stoichiometric compounds can be deposited, and the x and y values are controllable by adjusting process variables such as the selection of reactive gases and their relative flow rates. Inorganic and organic polymers may also be deposited. Preferred dielectrics and cap films include SiO 2 . In the present specification, the present invention has been described using only SiO 2 as an example, but the present invention may be applied to other films.
    The composition of the process gas depends on the semiconductor and / or dielectric to be deposited. In silicon-containing films, the process gas is, for example, silane (SiH 4 ), tetraethylorthosilicate (TEOS), 1,3,5,7-tetramethylsilicate (TMCTS), disilane (Si 2 H 6 ) Or other silicon-containing organometallic gas. The process gas preferably includes an inert gas, such as argon, krypton, xenon, and mixtures thereof, in order to be able to control the nature or sputter rate of the plasma, particularly in the gap filling step prior to cap layer deposition. In order to incorporate the non-silicone component into the film, the process gas may comprise a reactive gas such as H 2 , O 2 , N 2 , NH 3 , NF 3 , N 2 O, NO and mixtures thereof. The reactive gas may also include boron and / or phosphorus to produce boro-phospho-silicate glass (BSPG), boro-silicate glass (BSG) and phospho-silicate glass (PSG) films.
    Example I (Gap Filling Process)
    SiO 2 IMD deposition was performed in an ICP system similar to FIG. 1. Mechanically clamped 150 mm wafers were used. Two gas rings located at the base edge of the window 33 were used. One ring distributes SiH 4 and the other distributes argon and oxygen. System variables are set as shown in Table 1. The temperature of the electrode was kept at 80 ° C.
    Effect of Oxygen to Silane Flow Rate (total Flow Rate Constant) on Film Characteristics
    The stoichiometric ratio of the film was determined by the chemical composition of the plasma. The mass flow rate R between silane and oxygen was defined as follows. Q is a mass flow rate of gas.
    R = Q SiH4 / (Q SiH4 + Q O2 )
    It should be noted that the effective oxygen-silane ratio for the wafer also depends on other process variables. The effect of R on film properties is shown in Table 2.
    The plasma chemistry of the deposition reaction can be broadly classified into the following equation.
    R <0.5: SiH 4 -limited (2 + n) O 2 + SiH 4 → SiO 2 : (OH) 4n + (2-2n) H 2 O
    R ≥ 0.5: O 2 -restricted O 2 + SiH 4 → SiO 2 : (H) 2n + (2-n) H 2
    In the above formula, SiO 2 : (X) n means a stoichiometric oxide containing approximately n fractions of X (0 ≦ n <1). Based on the measured OH content, n is always less than 0.025 (OH <10 atomic%). Scheme 1 is dominant when film growth is in a silane-limited environment (R ≦ 0.5). In this reaction, the amount of water released into the plasma increases as R decreases, which explains the increase in OH concentration in the film as R decreases. Conversely, in an oxygen-limited environment, H2 production sites are increased by Scheme 2 (R> 0.5), which means that as R increases, the amount of H coalesced as Si-H increases (resulting in Si-rich subs such as Si 2 O 3). Explain the phenomenon of oxide).
    The data also shows that significant changes occur in the process near R = 0.40. This change was seen in all film properties as described in Table 2 and corresponds to the conversion from silane-limiting chemistry, ie reaction 1 to oxygen-limiting chemistry, ie reaction 2, as described above. The deposition rate was linearly proportional to the flow rate of silane and the silane-limiting region (R <0.40) was extrapolated to zero thickness of zero flow rate, as expected.
    In general, film stress is derived from mechanical stress and inherent stress of the film resulting from the difference in thermal expansion between the film and the substrate. The former is mainly determined by the deposition temperature. In the latter case, the microstructure and stoichiometry of the film are the dominant factors. Under SiH 4 -limiting conditions, the stress of the film depends mainly on the deposition rate. Faster film growth is expected to reduce thermal relaxation and ion / impact densification time. O 2 - film growth under the constraint is even faster deposition rate O 2 - is less compressed than films grown under a sufficient condition.
    The FTIR spectrum shown in Figure 2 illustrates the relationship between reaction 1 and reaction 2. When R was small, Si-OH and Si-HOH absorption bands were observed but Si-H was not observed. Si-OH was not observed when R was large, but Si-H and a suboxide (Si 2 O 3 ) Si-O band existed. When R was in the middle, minimal Si-OH and Si-H appeared only on the O 2 -fill side of the critical region. The intermediate region R is optimal for obtaining the desired dielectric constant. In addition, since the refractive indices of 1.465 to 1.480 correspond to films having good dielectric constants, the refractive indices can also be a measure of desirable process conditions.
    Effect of ICP Power on Film Properties
    Table 3 below shows the effect of the ICP power on the film characteristics when the bias power is 1000W.
    The effect of ICP power on film properties is similar to that of total flow rate. Both are believed to be intrinsically related to the deposition precursor supply phenomenon. The first deposition precursor is produced by silane decomposition, and what is fed to the surface of this paper wafer depends on the rate of generation of the species in the plasma and the losses due to pump losses and deposition on the reactor walls. Both the total flow rate and the ICP power can affect the effective R at the wafer through a generation or loss mechanism.
    In the case of precursor generation, calculations based on bond strengths indicate that the energy required to decompose SiH 4 is less than the energy required to decompose O 2 . In this case, increasing the silane supply (total flow rate) will increase the supply of SiH x to any relevant oxygen species. As observed, this leads to reaction chemistry with a larger R. The dependency is uncertain, but ICP power also affects the process.
    Effect of Bias Power on Film Properties
    The bias power is applied to the wafer to increase the DC sheath potential, and thus the dynamic energy of the impact ions, to the extent that the film can be sputtered and grown. The quality of the film is improved in various ways. The O 2 plasma preceding the deposition sputter cleans the wafer surface to form a clean, tacky interface. Since the silver wafer is heated due to ion bombardment during deposition, the temperature needs to be controlled by helium back cooling. Ion bombardment also preferentially sputters and “etches” weak and uneven structures on the film and then densifies through compression. This allows for higher quality film deposition at lower temperatures than other methods. The effect of the bias film on the film properties is shown in Table 4.
    It can be seen that the properties of uniform films vary significantly from 400 to 500 watts. Ion energy increases in proportion to bias power below 400 watts, but the dominant effect of bias power is thought to increase plasma generation on the wafer since the ions do not have enough energy to sputter. Above 400 watts, the average ion energy is estimated to be above the sputtering limit for SiO2, and the overall deposition rate decreases because the secondary plasma generation is more dominant than the effect of the sputtering component.
    Gap-filled deposition
    Gap filling performance is predictable from the etch / deposition rate, ER / DR, calculated from the deposition rate under the presence or absence of RF bias (the "zero-bias" condition actually used 100 W, which caused the secondary plasma generation). Can be.
    E / D = [DR (No Bias)-DR (Bias)] ÷ DR (No Bias)
    Wherein DR is the deposition rate.
    The larger the E / D, the more aggressive gaps can be filled. In general, to maximize the overall deposition rate, the lowest E / D should be used as long as the desired gap can be filled. Of course, once the gap is filled, the E / D should be reduced to the minimum value at which the film can preserve quality, i.e. allow the majority of the IMD layer to deposit at a faster rate.
    The SEM photographs of FIGS. 3A, 3B, 3C, and 3D illustrate good or bad gap fill by ICP-CVD. 3A is partially filled with a furnace bias. At the top of the line you can see the porous film form and the "bread rope" shape of the film. This is eventually overwritten as shown in FIG. 3B, leaving a void. They are also structures that preferentially sputter because the sputtering maximum is at 45 degrees. FIG. 3B shows an example of unsatisfactory charging when using a bias power but E / D is too low for the gap. It is worth noting that the breadcrumbs covered earlier during the process leave a large and deep gap. In FIG. 3C, next to another identical gap that has been successfully filled, one can see a small void formed just before the gap is filled. In this case, E / D is the lowest value. The layering operation was carefully performed by periodically depositing a thin Si-rich layer and decorating it with the appropriate stain of the sample to reveal compositional contrast. This clearly shows the filling from the base of the gap with minimal sidewall growth compared to growth in the horizontal plane. The plane cut by 45 degrees formed on the line by sputtering is also clearly visible. 3d shows the complete filling of the aggressive gap by a medium E / D process (100 sccm Ar).
    Example 2 (gap filling and capping process)
    SiO 2 IMD and capping deposition were performed on an ICP system similar to FIG. 4. In this example, a 200 mm wafer was processed. The wafer was electrostatically clamped to a temperature controlled chuck. The bottom electrode was powered from a 13.56 MHz generator. A 2000 L / sec pump was installed in the ICP / CVD system to improve pumping speed at high flow rates. ICP power was used between 1000 and 2500 watts. High bias power of 500 to 2500 watts was used for gap filling.
    The properties of the films corresponding to the general process parameters for the gap fill, cap and sacrificial cap layers are shown in Table 5. The following table also includes the preferred range of process parameters.
    In the deposition experiment (0.5 μm gap), argon was included in the process gas. However, as indicated in the preferred range, argon addition is not always necessary. In the deposition of the cap layer, high electrode RF bias power can be used for initial deposition to produce a good quality film. Thereafter, lower bias power can be applied to produce a lower quality sacrificial cap layer (preferably keeping the temperature of the residual electrode the same). Generally this sacrificial cap layer is substantially removed in a subsequent flattening process.
    In general, when the temperature of the substrate is higher, the properties of the deposited pillars are improved. Usually, the temperature of the substrate is related to two main factors: (1) heating from the substrate support means (ESC) and (2) electrode RF bias power, and at least source (ICP, ECR, etc.) power. From the plasma heating.
    In the prior art, increasing source and bias power has been used to raise the temperature of the substrate to improve the quality of the film. However, this method sometimes allows some choices of desired film properties, as demonstrated in the effects of helium backpressure, power and chamber height.
    Influence of helium backpressure, power and chamber height
    The temperature of the substrate was controlled by changing the spacer height, helium cooling pressure and power level of the ICP-CVD apparatus, and a series of depositions were performed while maintaining the temperature of the electrode at 80 ° C. Table 6 shows the results.
    Substrate temperatures around 400 ° C. have been found to produce high quality oxides. Especially, since a high temperature board | substrate drives out a volatile species, film density improves. Helium was not used for the third deposition and the temperature of the substrate is estimated to have exceeded 450 ° C.
    The first set of three wafers was when the helium pressure was reduced from 2 Torr to 0 Torr (ie, not cooled), and the temperature of the substrate rose to 275 to 400 ° C or higher. The film properties show that the higher the temperature of the wafer, the higher quality the film is produced. The OH content in the film is low and all other film properties are good. An advantage of the high temperature of the wafer is that it does not adversely affect film stress, OH% and wet etch rate.
    The second set of three-wafers (deposition 4, 5 and 6) is the case of using helium and argon cooling gases for temperature control of the substrate. The first set of three wafers used Hellum and the second set of three wafers was cooled using Argon. The results show that helium and argon produce similar treatment results.
    The first and third sets of three wafers are for comparing the plasma heating effects of the wafers. Wafer heating is possible by reducing the distance (spacer height) between the ICP coil and the substrate surface. The results show that the quality of the film changes from high to low gap spacing when the power levels are the same. For 2 or 1 Torr helium cooling the OH% is the same, but the wet etch rate is improved at lower spacing.
    Comparing the last two wafers with the third set of 3-wafers in Table 6, the ICP power was reduced from 2500 to 2000 watts. From the data it can be seen that reducing the power is less compressive. In view of the reduced wet etch rate, the weaker the plasma heating, the more porous the film structure. Therefore, the wet etch rate is better at higher power levels.
    Effect of heated electrodes on film properties
    Instead of increasing the source and bias power to increase the temperature of the substrate, the use of high temperature electrodes can further improve the properties of the film without the need to select some of the film stress, OH% and wet etch rate, I found that the width can be wider.
    This can be seen from the results shown in Table 7 below, which summarizes the results of cap layer deposition using electrodes at 70 and 120 ° C. and with or without RF bias. Preferably, in producing the cap layer film, the wet etch rate is less than 2: 1, the OH% is about 1% or less, and the magnitude of the film stress is less than 200 MPa. Increasing the plasma heating of the wafer simply by increasing the bias from 0 to 2000 W results in undesirable consequences of reduced wet etch rate but increased film stress. Conversely, increasing the temperature of the electrode reduces both film stress and wet etch rate, with or without RF bias power applied. Therefore, the preferred process uses electrodes adjusted to a temperature selected at about 60-200 ° C.
    Another advantage of using a high temperature electrode is that a wider range of process conditions, such as pressure, reactive gas flow rate and TCP power, can be used, allowing the use of a broader set of operating conditions. Is there.
    The foregoing has described the principles, preferred embodiments, and operating modes of the present invention. However, the present invention should not be construed as limited to the specific embodiments discussed above. Accordingly, the above embodiments are to be construed as illustrative and not restrictive, and those skilled in the art will be able to contemplate various modifications without departing from the scope of the invention as defined by the appended claims.
    权利要求:
    Claims (55)
    [1" claim-type="Currently amended] In the method for filling gaps between conductive lines on semiconductor substrates (23, 120),
    Providing a substrate (23, 120) in a process chamber (21, 140) of an inductively coupled plasma-enhanced chemical vapor deposition reactor (20);
    Supplying a process gas into the process chamber, the process gas comprising an inert gas in an amount sufficient to assist gap filling;
    Growing a dielectric film on the substrate such that the dielectric film is deposited in a gap between conductive lines on the substrate.
    [2" claim-type="Currently amended] The process of claim 1 wherein the process gas further comprises a silicon containing reactive gas selected from the group consisting of SiH 4 , SiF 4 , Si 2 H 6 , TEOS, TMCTS, and mixtures thereof. Decomposing the silicon-containing gas to form a silicon-containing gas and plasma phase-reacting the silicon-containing gas on a substrate surface.
    [3" claim-type="Currently amended] The process of claim 1 or 2, wherein the process gas comprises a reactive gas selected from the group consisting of H 2 , O 2 , N 2 , NH 3 , NF 3 , N 2 O, NO 3 and mixtures thereof. How to feature.
    [4" claim-type="Currently amended] 4. A process according to any one of the preceding claims wherein the process gas comprises a reactive gas selected from the group consisting of boron containing gas, phosphorus containing gas and mixtures thereof.
    [5" claim-type="Currently amended] The method of claim 1, wherein the process chamber is maintained at a pressure of about 1 mTorr to about 30 mTorr.
    [6" claim-type="Currently amended] The method of claim 1, wherein the film is deposited on a silicon wafer, and the gap is located between conductive lines comprising aluminum, copper, tungsten, and mixtures thereof.
    [7" claim-type="Currently amended] The method of any one of claims 1 to 6, further comprising applying a radio frequency bias to the substrate.
    [8" claim-type="Currently amended] 8. The method of claim 7, wherein applying a radio frequency bias to the substrate comprises supporting the substrate on substrate support means (24, 130) having electrodes for supplying a radio frequency bias, Bias is generated by supplying at least 2 watts / cm 2 of power to the electrode.
    [9" claim-type="Currently amended] 8. The method of claim 7, wherein the frequency range of the radio frequency bias applied to the substrate is between about 100 KHz and 27 MHz.
    [10" claim-type="Currently amended] 10. A method according to any one of the preceding claims, wherein the substrate is located on substrate support means (24, 130) at which the temperature is maintained at about 80 to 200 ° C.
    [11" claim-type="Currently amended] The method according to any one of claims 1 to 10, further comprising the step of supplying a heat transfer gas between the surface of the substrate and the surface of the substrate supporting means (24, 130) for supporting the substrate in the film growth step. How to.
    [12" claim-type="Currently amended] 12. The method of any one of the preceding claims, further comprising clamping the substrate onto an electrostatic or mechanical chuck in the film growth step.
    [13" claim-type="Currently amended] 13. The method of claim 12, wherein a heat transfer gas comprising helium and / or argon is supplied between the surface of the substrate and the surface of the chuck.
    [14" claim-type="Currently amended] 14. The method of any one of claims 1 to 13, further comprising plasma phase reacting an oxygen containing gas in the gap and removing polymer residues in the gap prior to the film growth step.
    [15" claim-type="Currently amended] The method according to claim 1, wherein the dielectric film comprises silicon oxide.
    [16" claim-type="Currently amended] The method of claim 1, wherein the dielectric film comprises SiO 2 .
    [17" claim-type="Currently amended] The method of claim 1, wherein the process gas comprises silicon and a fluorine containing reactant and the dielectric film comprises silicon oxyfluoride.
    [18" claim-type="Currently amended] 18. The method of any one of claims 1 to 17, wherein the gas mixture comprises a nitrogen containing gas and the dielectric film comprises silicon oxynitride.
    [19" claim-type="Currently amended] Method according to any of the preceding claims, characterized in that the inductively coupled plasma is produced by a substantially planar induction coil (34).
    [20" claim-type="Currently amended] 20. The process of any one of claims 1 to 19, wherein the process gas is supplied through gas supply means (160, 170) including an orifice (187), at least a portion of which is orthogonally intersects the exposed surface of the substrate. And oriented to supply process gas along the axis.
    [21" claim-type="Currently amended] 21. The process of claim 20, wherein the process gas supplying step comprises supplying the gas or gas mixture from the first gas ring 170 with at least a portion of the gas or gas mixture oriented towards the substrate. How to.
    [22" claim-type="Currently amended] 22. The method of claim 21 wherein the gas supply step further comprises supplying additional gas or gas mixture from the second gas ring (160).
    [23" claim-type="Currently amended] 22. The method of claim 21, wherein an injector (180) is connected to the first gas ring for injecting at least a portion of the gas or gas mixture into the chamber to face the substrate.
    [24" claim-type="Currently amended] In a method of filling gaps between conductive lines on semiconductor substrates (23, 120) and depositing a capping layer over the filled gaps,
    Providing a substrate (23, 120) in a process chamber (21, 140) of an inductively coupled plasma-enhanced chemical vapor deposition reactor (20);
    Introducing a first process gas and filling the gap between conductive lines on the substrate by growing a first dielectric film at a first deposition rate; And
    Introducing a second process gas into the process chamber and depositing a capping layer comprising a second dielectric film on the surface of the first dielectric film at a second deposition rate greater than the first deposition rate; Characterized in that the method.
    [25" claim-type="Currently amended] 25. The method of claim 24, wherein the dielectric film comprises silicon oxide, the first and second process gases comprise a silicon reactant and an oxygen reactant, the second process gas comprising a greater amount of silicon and than the first process gas. Characterized in that it contains an oxygen reactant.
    [26" claim-type="Currently amended] 25. The method of claim 24, wherein the dielectric film comprises silicon oxide, the first and second process gases comprise an inert gas, and the first process gas contains a greater amount of inert gas than the second process gas. Characterized in that the method.
    [27" claim-type="Currently amended] 27. The method of any one of claims 24 to 26, wherein an RF bias is applied during the gap filling and capping step, wherein the RF bias applied to the gap filling step is greater than the capping step.
    [28" claim-type="Currently amended] 28. The method according to any one of claims 24 to 27, wherein the substrate is located on substrate support means (24, 130) whose temperature is maintained at about 80 to 200 ° C.
    [29" claim-type="Currently amended] 20. The process of any one of claims 1 to 19, wherein the process gas is introduced through gas supply means (160, 170) comprising an orifice (187), at least a portion of the orifice crossing at an acute angle with the exposed surface of the substrate. And oriented to supply process gas along the axis.
    [30" claim-type="Currently amended] Providing substrates (23, 120) on substrate support means (24, 130) in process chambers (21, 140) of inductively coupled plasma-enhanced chemical vapor deposition reactor (20);
    Supplying a process gas into the process chamber, the process gas comprising an inert gas in an amount sufficient to cause a sputter etching;
    Adjusting the surface temperature of the substrate support means; And
    Growing a dielectric film on the substrate by applying inductively coupled RF energy into a process chamber to energize the process gas into a plasma state.
    [31" claim-type="Currently amended] 31. The process of claim 30, wherein the process gas further comprises a silicon containing reactive gas selected from the group consisting of SiH 4 , SiF 4 , Si 2 H 6 , TEOS, TMCTS, and mixtures thereof. Decomposing the silicon-containing gas to form a silicon-containing gas and plasma phase-reacting the silicon-containing gas on a substrate surface.
    [32" claim-type="Currently amended] 32. The process of claim 30 or 31 wherein the process gas comprises a reactive gas selected from the group consisting of H 2 , O 2 , N 2 , NH 3 , NF 3 , N 2 O, NO 3 and mixtures thereof. How to feature.
    [33" claim-type="Currently amended] 33. The method of any one of claims 30 to 32, wherein the process gas comprises a reactive gas selected from the group consisting of boron containing gas, phosphorus containing gas and mixtures thereof.
    [34" claim-type="Currently amended] 34. The method of any of claims 30 to 33, wherein the process chamber is maintained at a pressure of about 1 mTorr to about 30 mTorr.
    [35" claim-type="Currently amended] 35. The method of any one of claims 30 to 34, further comprising applying a radio frequency bias to the substrate.
    [36" claim-type="Currently amended] 36. The method of claim 35, wherein applying a radio frequency bias to the substrate comprises supporting the substrate on substrate support means (24, 130) having electrodes for supplying a radio frequency bias, Bias is generated by supplying at least 2 watts / cm 2 of power to the electrode.
    [37" claim-type="Currently amended] 37. The method of claim 36, wherein the frequency range of the radio frequency bias applied to the substrate is between about 100 KHz and 27 MHz.
    [38" claim-type="Currently amended] 38. The method of any one of claims 30 to 37, wherein the substrate is located on substrate support means wherein the temperature is maintained at about 80 to 200 ° C.
    [39" claim-type="Currently amended] 39. The method of any one of claims 30 to 38, further comprising the step of supplying a heat transfer gas between the surface of the substrate and the surface of the substrate support means.
    [40" claim-type="Currently amended] 40. The method of any one of claims 30 to 39, further comprising clamping the substrate onto an electrostatic or mechanical chuck in the film growth step.
    [41" claim-type="Currently amended] 41. The method of claim 39 or 40, wherein a heat transfer gas comprising helium and / or argon is supplied between the surface of the substrate and the surface of the chuck.
    [42" claim-type="Currently amended] 42. The method of any of claims 30 to 41, wherein the dielectric film comprises silicon oxide.
    [43" claim-type="Currently amended] 42. The method of any of claims 30 to 41, wherein the dielectric film comprises SiO 2 .
    [44" claim-type="Currently amended] 44. The method of any of claims 30 to 43, wherein the process gas comprises silicon and a fluorine containing reactant and the dielectric film comprises silicon oxyfluoride.
    [45" claim-type="Currently amended] 44. The method of any of claims 30-43, wherein the gas mixture comprises a nitrogen containing gas and the dielectric film comprises silicon oxynitride.
    [46" claim-type="Currently amended] 46. The method according to any one of claims 30 to 45, wherein said inductively coupled plasma is generated by a substantially planar induction coil (34).
    [47" claim-type="Currently amended] 47. The process of any of claims 30 to 46, wherein the process gas is introduced through gas supply means (160, 170) comprising an orifice (187), at least a portion of the orifice crossing at an acute angle with the exposed surface of the substrate. And oriented to supply process gas along the axis.
    [48" claim-type="Currently amended] Plasma processing chambers 21 and 140;
    Substrate support means (24, 130) for supporting the substrates (23, 120) in the processing chamber and maintained at a temperature of about 80 to 200 ℃;
    A conductive coil 34 disposed outside the processing chamber;
    Means (31, 32, 160, 170, 187) for introducing a process gas into said processing chamber; And
    And an RF energy source (35) for inductively coupling the RF energy into the processing chamber to energize the process gas into a plasma state.
    [49" claim-type="Currently amended] 49. The system of claim 48, wherein the process gas comprises a silicon containing reactive gas selected from the group consisting of SiH 4 , SiF 4 , Si 2 H 6 , TEOS, TMCTS, and mixtures thereof.
    [50" claim-type="Currently amended] The process of claim 48 or 49, wherein the process gas comprises a reactive gas selected from the group consisting of H 2 , O 2 , N 2 , NH 3 , NF 3 , N 2 O, NO 3, and mixtures thereof. System characterized.
    [51" claim-type="Currently amended] 51. The system of any of claims 48-50, wherein the process gas comprises a reactive gas selected from the group consisting of boron containing gas, phosphorus containing gas and mixtures thereof.
    [52" claim-type="Currently amended] 52. The system of any of claims 48-51, wherein the process chamber is maintained at a pressure of about 1 mTorr to about 30 mTorr.
    [53" claim-type="Currently amended] 53. The system according to any one of claims 48 to 52, further comprising an RF generator (35, 36) coupled to the substrate to generate an RF bias.
    [54" claim-type="Currently amended] 54. The process of any one of claims 48 to 53, wherein said process gas introduction means comprises gas supply means (160, 170) comprising an orifice (187), wherein at least a portion of said orifice acutely intersects the exposed surface of the substrate. And oriented to supply process gas along the injection axis.
    [55" claim-type="Currently amended] 55. The system according to any one of claims 48 to 54, wherein the coil (34) is substantially flat.
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    同族专利:
    公开号 | 公开日
    DE69732918D1|2005-05-04|
    AT292200T|2005-04-15|
    WO1998028465A1|1998-07-02|
    JP2001507081A|2001-05-29|
    EP0953066B1|2005-03-30|
    TW432493B|2001-05-01|
    US20010019903A1|2001-09-06|
    US6184158B1|2001-02-06|
    KR100497778B1|2005-06-23|
    DE69732918T2|2006-04-13|
    EP0953066A1|1999-11-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    法律状态:
    1996-12-23|Priority to US8/772,374
    1996-12-23|Priority to US08/772,374
    1996-12-23|Priority to US08/772,374
    1997-12-22|Application filed by 리차드 에이치. 로브그렌, 램 리서치 코포레이션
    1997-12-22|Priority to PCT/US1997/022987
    2000-10-25|Publication of KR20000062317A
    2005-06-23|Application granted
    2005-06-23|Publication of KR100497778B1
    优先权:
    申请号 | 申请日 | 专利标题
    US8/772,374|1996-12-23|
    US08/772,374|US6184158B1|1996-12-23|1996-12-23|Inductively coupled plasma CVD|
    US08/772,374|1996-12-23|
    PCT/US1997/022987|WO1998028465A1|1996-12-23|1997-12-22|Inductively coupled plasma cvd|
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