US20100252067A1 - Cleaning device and cleaning process for a plasma reactor - Google Patents

Cleaning device and cleaning process for a plasma reactor Download PDF

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Publication number
US20100252067A1
US20100252067A1 US12/308,296 US30829607A US2010252067A1 US 20100252067 A1 US20100252067 A1 US 20100252067A1 US 30829607 A US30829607 A US 30829607A US 2010252067 A1 US2010252067 A1 US 2010252067A1
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Prior art keywords
biasable
walls
reactor
sequence
biasing
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Abandoned
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US12/308,296
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English (en)
Inventor
Jacques Henri Pelletier
Ana Lacoste
Alexandre Bes
Stéphane Jean Louis Bechu
Jérôme Sirou
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Centre National de la Recherche Scientifique CNRS
Universite Joseph Fourier Grenoble 1
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Individual
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Assigned to CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS), UNIVERSITE JOSEPH FOURIER - GRENOBLE 1 reassignment CENTRE NATIONAL DE LA RECHERCHE SCIENTIFIQUE (CNRS) ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BECHU, STEPHANE JEAN LOUIS, BES, ALEXANDRE, LACOSTE, ANA, PELLETIER, JACQUES HENRI, SIROU, JEROME
Publication of US20100252067A1 publication Critical patent/US20100252067A1/en
Abandoned legal-status Critical Current

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    • 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
    • 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
    • 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
    • H01J37/32871—Means for trapping or directing unwanted particles
    • 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
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67017—Apparatus for fluid treatment
    • H01L21/67063—Apparatus for fluid treatment for etching
    • H01L21/67069—Apparatus for fluid treatment for etching for drying etching

Definitions

  • the invention concerns a device for cleaning a reactor.
  • the invention concerns more precisely a device for plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit.
  • the invention concerns the method of cleaning a reactor implemented with the device according to the invention.
  • the invention applies to reactors using dry methods and the walls of which are covered with undesirable deposits.
  • the invention applies to the cleaning of deposition and surface treatment reactors.
  • the invention can also apply to CVD (silicon, tungsten), laser deposition or MBE (molecular beam epitaxy) reactors, the walls of which it is necessary to clean periodically to prevent redeposition or dust on the surfaces.
  • CVD silicon, tungsten
  • MBE molecular beam epitaxy
  • auxiliary gas plasmas that are as reactive as possible vis- ⁇ dot over (a) ⁇ -vis the deposits to be removed by reactive chemical method, and at relatively high pressure in order to produce the greatest possible concentrations of reactive species (for example atomic fluorine F for chemical etching of Si, SiO 2 , Si 3 N 4 or W, atomic oxygen O for the etching of carbon or polymers) and heating the walls in order to thermally activate the chemical etching reactions.
  • reactive species for example atomic fluorine F for chemical etching of Si, SiO 2 , Si 3 N 4 or W, atomic oxygen O for the etching of carbon or polymers
  • One objective of the invention is therefore to propose a cleaning device requiring only minor modifications to the reactor.
  • An objective of the invention is to propose a simplified cleaning method relying on plasma-assisted dry chemical etching methods, in particular using ion bombardment.
  • a method for the plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit on its walls and on at least one other biasable surface characterised in that at least one sequence, referred to as a positive sequence, of cleaning the walls of the reactor was implemented by positive biasing of the or each biasable surface, with respect to the walls of the reactor, the walls being at a referenced potential.
  • a device for the plasma-assisted dry chemical cleaning of a reactor having an undesirable deposit on its walls and on at least one other biasable surface characterised in that it comprises means for positively biasing, with respect to the walls of the reactor maintained at a referenced potential, the or each biasable surface.
  • FIG. 1 depicts by way of example DC voltages applied to at least one biasable surface of a reactor, according to the two types of sequence, with respect to the referenced wall potential V w ;
  • FIG. 2 depicts, by way of example, a periodic voltage signal V(t) supplied to at least one biasable surface, during a sequence referred to as sequence 1 or negative sequence, in which the biasable surface auto-biases negatively with respect to the referenced potential of the walls V w ;
  • FIGS. 3 a and 3 b depict, by way of examples, periodic voltage signals supplied and applied to at least one biasable surface, during a sequence referred to as sequence 2 or positive sequence, in which the biasable surface periodically has a positive potential with respect to the referenced potential of the walls V w ;
  • FIG. 4 depicts, by way of example, a period voltage signal supplied and applied to at least one biasable surface, in which the biasable surface periodically has a positive and negative potential with respect to the referenced potential of the walls V w ;
  • FIGS. 5 , 6 , 7 and 8 depict schematically different variant embodiments of a device according to the invention.
  • the method according to the invention is a plasma-assisted chemical etching cleaning method.
  • the cleaning method according to the invention can be implemented, it is necessary for the plasma to be produced in a reactor with walls at referenced potentials (for example earthed).
  • the cleaning operation comprises at least one cleaning sequence (by plasma etching) in which the walls of the reactor are cleaned by positive biasing, with respect to the walls of the reactor, of the or each biasable surface (for example substrate carrier or electrode).
  • This sequence or sequences are called sequence 2 or positive sequence in the remainder of the description.
  • the operation comprises, according to the application, at least one other sequence of cleaning the or each biasable surface (for example substrate carrier and/or electrode) by negative biasing of the biasable surface with respect to the walls of the reactor.
  • This sequence or sequences are called sequence 1 or negative sequence in the remainder of the description.
  • a sequence 2 may suffice: there is then complete cleaning of the walls of the reactor (chamber) by application to the biasable surface (substrate carrier or electrode) of a positive DC voltage with respect to the walls.
  • a sequence 1 and a sequence 2 there is then complete cleaning of the biasable surface by application to this surface (substrate carrier or electrode) of a negative DC voltage with respect to the walls (for example earthed) and the complete cleaning of the walls of the chamber by application to the surface (substrate carrier or electrode) of a positive DC voltage with respect to the walls.
  • V(t) supplied to the biasable surface and to which it is raised changes from a sequence 1 , referenced 1 , to a sequence 2 , referenced 2 , and where V w is the potential of the walls of the reactor.
  • sequence 1 it is of little importance whether sequence 1 is carried out followed by sequence 2 or vice versa. However, in practice, it is more suitable to commence with sequence 1 , that is to say to carry out the cleaning of the biasable surface.
  • the biasable surface (substrate carrier or electrode) can be small compared with the surface of the walls to be cleaned but must have a sufficiently large size to disturb the plasma, so that the potential of the plasma V p is positioned, at each moment t, at a value that is always more positive than the most positive surface (wall or electrode).
  • the condition to be fulfilled for constituting a substrate carrier or a large-size electrode is that the ratio of the surface S s of the substrate carrier or large-size electrode to the surface S w of the walls is at least greater than approximately 1.5 times the square root of the ratio of the mass m e of the electrons to of the ions m i , that is to say:
  • the ratio is therefore necessary for the ratio to be greater than 1/180 ( 1/30 for hydrogen and 1/500 for xenon), which is generally the case with substrate carriers or electrodes used in microelectronics or in surface treatments by furnace.
  • the surface S s does not disturb the plasma, which corresponds to the case of electrostatic probes or Langmuir probes.
  • the plasma potential V p remains practically unchanged compared with the potential of the walls (generally earthed) if the biasable surface of the surface S s is positively biased with respect to the potential V w of the walls.
  • the ion bombardment energy W w of the walls of the reactor is then close to:
  • V f the potential of the biasable surface which in floating, then equal as a first approximation to the potential of the walls (V f ⁇ V w ).
  • the biasable surface S s profoundly disturbs the equilibrium of the plasma if it is raised to a positive potential V 0 with respect to the potential of the walls V w (sequence 2 ).
  • the plasma potential V p is offset by the value V 0 ⁇ V w and the ion bombardment energy V w of the walls is, as a first approximation, for a DC voltage V 0 , equal to:
  • the biasable surface S s to the DC potential V 0 with respect to the potential of the walls V w (sequence 2 )
  • the ion bombardment energy W s of the electrode is equal to:
  • the ion bombardment energy W s of the surface S s is equal to:
  • a sequence 2 or a succession of a sequence 1 and a sequence 2 may suffice according to circumstances. However, if the cleaning of the walls contaminates the large-sized biasable surface, or vice versa, it is preferable to provide a certain number of alternating sequences until there is complete cleaning of the reactor (walls and large-sized biasable surface).
  • the substrate carrier is used as a large-sized electrode, some parts concealed by the substrate may prove to be free of deposit. In fact the deposit may affect solely the edges of the substrate carrier but in this case it is preferable to clean the whole of the substrate carrier (sequence 1 ).
  • sequence 1 is carried out followed by sequence 2 or vice versa.
  • sequence 2 it is more suitable to commence with sequence 1 , that is to say to carry out the cleaning of the biasable surface.
  • the periodic voltage of frequency f 0 supplied for example by a periodic voltage generator, is referenced with respect to the potential of the walls of the reactor (generally earthed), which is not in principle the case with the biasable surface (auto-biasing mode is thought of).
  • a first sequence sequence 1 or negative sequence
  • it is usual to carry out negative auto-biasing of the biasable surface by applying a periodic voltage to the biasable surface through a low-impedance capacitor (the current case of RF auto-biasing) and therefore to clean the large-sized biasable surface by chemical etching assisted by ion bombardment (plasma).
  • a low-impedance capacitor the current case of RF auto-biasing
  • an adapted means therefore supplies a periodic voltage signal V(t) (such as the one illustrated in FIG. 2 ) to the biasable surface which, for its part, biases itself (auto-biasing) so that it receives, during a period, as many positive charges (ions) as negative charges (electrons) having regard to the voltage values taken by this signal and that of the plasma potential.
  • V(t) such as the one illustrated in FIG. 2
  • This auto-biasing results from the non-linearity of the current/voltage characteristic of the plasma.
  • the invention consists of applying to it, during a second sequence (sequence 2 or positive sequence), a periodic voltage referenced (for example to the potential of the walls, generally earthed) so that the voltage applied to the biasable surface during the positive half wave takes a positive value +V 0 with respect to the potential of the walls.
  • a periodic voltage referenced for example to the potential of the walls, generally earthed
  • FIG. 3 a and FIG. 3 b Examples of periodic voltage signals supplied by a means adapted to the biasable surface are illustrated on FIG. 3 a and FIG. 3 b .
  • the signal supplied by the adapted means is that carried by the biasable surface.
  • the signal supplied by the adapted means is carried to the biasable surface solely when V>V w , (sequence 2 ), the biasable surface therefore “sees” the same signal as at FIG. 3 a.
  • a periodic voltage referenced (for example to the potential of the walls, generally earthed) is applied to the biasable surface so that the voltage applied to the biasable surface during the negative half waves (sequences 1 ) takes a negative value V 0 with respect to the potential of the walls, and so that the voltage applied during the positive half waves (sequences 2 ) takes a positive value +V 0 with respect to the potential of the walls ( FIG. 4 ).
  • the low-impedance capacitor is short-circuited ( FIG. 6 ) so that the voltage supplied by adapted means corresponds to the voltage carried to the biasable surface.
  • the angular velocity ⁇ 0 of the cleaning sequences is not a limitative given of the method.
  • this angular velocity may be smaller or greater than the ion plasma angular velocity ⁇ pi defined by ⁇ pi 2 ⁇ n e 2 / ⁇ 0 m i where n is the density of the plasma, ⁇ e the charge on the electron, m i the mass of the ions of the plasma and ⁇ 0 the permittivity of the vacuum.
  • the shape of the periodic signal (the succession of periodic alternating sequences) may be sinusoidal, rectangular or other.
  • equations (2) to (6) are in practice valid in the case of the application of rectangular signals or periodic angular velocity voltages ⁇ 0 ⁇ pi and highly asymmetric surfaces S s and S w .
  • the cleaning by the succession of periodic alternating sequences presented above when the deposit to be cleaned is insulating may also be applied to the cleaning of conductive deposits.
  • the cleaning of conductive deposits in two or more sequences under DC voltage procures the advantage of not requiring a periodic voltage generator, much more expensive that a DC supply.
  • the voltages applied must be adjusted so that the ion bombardment energy of the electrode or walls of the reactor remains below or close to the sputtering threshold of the materials that make them up (negligible sputtering of the electrode and walls of the reactor) that is to say typically below 100 eV.
  • the cleaning devices according to the invention comprise, and this in a manner known in the plasma assisted dry chemical cleaning devices, means of producing, in a reactor, a reactive plasma capable of forming volatile reaction products with the deposits to be removed.
  • biasable surface substrate carrier or electrode
  • S s surface area S s sufficient with respect to the surface area S w of the walls [equation (1)] to allow modification of the plasma potential.
  • the biasable surface is then said to be of large size.
  • These means also comprise means of applying to the large-size biasable surface excessive biasing sequences using DC or periodic voltages according to the method of the invention.
  • the plasma production means can consist of different types of plasma such as microwave plasmas for example distributed electron cyclotron resonance (DECR) plasmas, multi-dipole plasmas (non-limitative examples), such as continuous or radio-frequency capacitive discharges, diodes or triodes, where one of the electrodes is used as a biasable substrate carrier, or such as inductive discharges with inductor internal to the chamber.
  • the substrate holders generally comply with the criterion of surface area ratio of equation (1).
  • a conventional means For application of a periodic negative auto-biasing voltage (sequence 1 , insulating deposit), a conventional means consists of a generator capable of delivering a periodic voltage through a low-impedance capacitor.
  • obtaining a positive biasing voltage during the positive half wave requires a generator capable of delivering a periodic voltage referenced with respect to a defined potential.
  • the invention requires, in very many cases, a generator capable of successively delivering either a periodic voltage through a low-impedance capacitor (biasing of the substrate during the method preceding the cleaning and/or during sequence 1 ), or a referenced periodic voltage having during the positive half wave (sequence 2 ) a positive voltage with respect to the potential of the wall.
  • a device according to the invention will then have to require a generator capable of delivering a periodic voltage referenced with respect to the wall, that is to say having a periodically negative and then positive voltage, symmetrical for example with respect to the potential of the wall.
  • a first device comprises means of applying DC voltages that are negative and positive, with reference to the walls of the reactor, to a biasable surface (a substrate carrier for example), and this independently or not of the production of the plasma.
  • This first device is illustrated in FIG. 5 . It has a reactor 10 referenced to earth 11 , a biasable surface 12 electrically connected by a means 13 to a DC voltage generator 14 , comprising means of controlling the generator in order to successively deliver positive and negative voltages, with reference to the walls of the reactor.
  • a second device ( FIG. 6 ) comprises a periodic voltage generator 140 , electrically connected to the or each biasable surface 12 by means of a circuit 15 comprising a low-impedance capacitor 151 and means 152 for short-circuiting the capacitor.
  • the biasing of the biasable surface takes place independently or not of the production of the plasma.
  • the short-circuiting means 152 may for example, but non-limitatively, be formed by a switch, disposed in parallel to the low-impedance capacitor.
  • the switch in open during a sequence 1 ( FIG. 6 and FIG. 2 ), so that the voltage generated by the generator passes through the capacitor before arriving at the or each biasable surface.
  • the switch is closed for a sequence 2 , so that the voltage generated by the generator is the voltage of the or each biasable surface ( FIG. 3 a and FIG. 3 b ).
  • a third device comprises means of applying a periodic voltage, for example by a periodic voltage generator 141 , to the or each biasable surface 12 , by means of a direct electrical connection 13 ( FIG. 7 ).
  • This voltage is referenced to the potential of the walls of the reactor (generally earthed), and this independently or not of the production of the plasma.
  • the biasing is not independent of the production of the plasma, whereas it is generally so in inductive plasmas and microwave plasmas.
  • One of the main advantages of the invention is its simplicity in terms of the method and device compared with current techniques.
  • sequence 1 or negative sequence mentioned in the description above uses known plasma-assisted etching methods in so far as the or each biasable surface is negatively biased with respect to the plasma potential (which is slightly greater than the potential of the walls).
  • sequence 2 or positive sequence modifies the nominal functioning of the reactor in order to achieve an objective of cleaning the walls of the reactor, which are for this purpose put to a referenced potential.
  • cathode which constitutes a biasable surface
  • at least one anode intended to collect the electrons, which is, in nominal functioning, biased positively with respect to the plasma potential.
  • the biasing thereof does not cause any sputtering of the biasable surface if the biasing thereof is independent of the production of the plasma (for example plasmas produced by microwaves), and is maintained at a value less than that corresponding to the sputtering of the surfaces of the reactor;
  • a capacitive discharge is considered in a reactor 10 connected to earth 11 created between a biasable surface (a substrate carrier) to which a voltage is applied and an earthed electrode 15 ( FIG. 8 ) or also a reactor of the same dimensions in which the plasma is produced by microwaves and where the same substrate carrier can be biased by a voltage.
  • the element 16 corresponds, according to the type of voltage generated, to the generator 14 in FIG. 5 , to the assembly formed by the generator 140 and the circuit 15 in FIG. 6 , or to the generator 141 in FIG. 7 .
  • the ratios of the earthed surfaces and those biasable continuously or periodically (RF) is 700 cm 2 /7000 cm 2 , that is to say 1/10, which perfectly corresponds to the criterion defined by equation (1) and to the case of a substrate-carrier surface that is small compared with the surface of the walls.
  • a well known example is the removal of the deposits of SiO 2 on the walls of a deposition reactor.
  • this deposit can be removed by means of an SF 6 plasma by the formation of the reaction products SiF 4 and O 2 by chemical etching assisted by ion bombardment.
  • CF 4 and more generally fluorocarbon gases, may, according to the plasma parameters, lead to a CF x deposit of the Teflon type.

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US12/308,296 2006-06-13 2007-06-13 Cleaning device and cleaning process for a plasma reactor Abandoned US20100252067A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0605238A FR2902029B1 (fr) 2006-06-13 2006-06-13 Dispositif et procede de nettoyage d'un reacteur par plasma
PCT/EP2007/055830 WO2007144378A2 (fr) 2006-06-13 2007-06-13 Dispositif et procede de nettoyage d'un reacteur par plasma

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CN103035466A (zh) * 2011-10-08 2013-04-10 北京北方微电子基地设备工艺研究中心有限责任公司 一种预清洗方法及等离子体设备
US10290475B2 (en) * 2012-10-11 2019-05-14 Varian Semiconductor Equipment Associates, Inc. Biasing system for a plasma processing apparatus

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US6832996B2 (en) 1995-06-07 2004-12-21 Arthrocare Corporation Electrosurgical systems and methods for treating tissue
JP7209508B2 (ja) * 2018-10-16 2023-01-20 株式会社東芝 プロセス装置

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FR2902029B1 (fr) 2009-01-23
US9812298B2 (en) 2017-11-07
EP2035597B1 (de) 2012-03-07
US20140305467A1 (en) 2014-10-16
WO2007144378A3 (fr) 2008-04-24
ATE548481T1 (de) 2012-03-15
EP2035597A2 (de) 2009-03-18
FR2902029A1 (fr) 2007-12-14

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