US3369990A - Cathodic sputtering apparatus including thermionic means for increasing sputtering efficiency - Google Patents

Cathodic sputtering apparatus including thermionic means for increasing sputtering efficiency Download PDF

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US3369990A
US3369990A US422667A US42266764A US3369990A US 3369990 A US3369990 A US 3369990A US 422667 A US422667 A US 422667A US 42266764 A US42266764 A US 42266764A US 3369990 A US3369990 A US 3369990A
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cathode
sputtering
glow discharge
region
gas
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US422667A
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Robert L Hallen
Robert M Valletta
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International Business Machines Corp
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International Business Machines Corp
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Priority to US422667A priority Critical patent/US3369990A/en
Priority to FR42301A priority patent/FR1459624A/fr
Priority to DE19651515305 priority patent/DE1515305A1/de
Priority to GB54281/65A priority patent/GB1100198A/en
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3435—Applying energy to the substrate during sputtering
    • C23C14/345—Applying energy to the substrate during sputtering using substrate bias
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3471—Introduction of auxiliary energy into the plasma
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F4/00—Processes for removing metallic material from surfaces, not provided for in group C23F1/00 or C23F3/00
    • 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
    • H01J37/34—Gas-filled discharge tubes operating with cathodic sputtering

Definitions

  • cathodic sputtering Although the phenomenon of cathodic sputtering has been known in the art of deposition of thin films for many years, the employment of such techniques has not been as popular as thin film deposition by vacuum evaporation. However, in recent years, there has been an increased interest in the deposition of thin films other than conductive metal films particularly in the field of microelectronic and monolithic circuit art. Cathodic sputtering is particularly advantageous over other techniques in the deposition of films of refractory materials including oxides, carbides and the like.
  • the mechanism of cathodic sputtering is one in which a glow discharge is established between an anode and a cathode, the current therebetween being conducted by the flow of electrons to the anode and positive ions to the cathode.
  • the glow discharge is maintained by ionization of gases existing within the glow discharge region which ionization is achieved by collisions of the gas partcles with the electron flow from the cathode to the anode.
  • the positive ions are accelerated toward the cathode, they achieve sufiicient energy to dislodge atoms or molecules from the cathode material upon impact with the cathode.
  • atoms or molecules of the cathode material are sputtered and deposited upon an appropriate substrate which in most situations is the anode. It is to be noted that the sputtered atoms are not ionized and that the mechanism by which such atoms are sputtered appears to be primarily one of a momentum and energy transfer. Because of this, the sputtering rate can be controlled by controlling the current density as well as the pressure of the gas in the glow discharge region.
  • the deposition rate will increase with an increase of current density, that is to say with an increase in the rate of ionic bombardment of the cathode, and will decrease with an increase in pressure as the number of collisions encountered by the sputtered particles will be proportional to the number of particles in the plasma in the glow discharge region.
  • an increase in current can only be achieved by an increase in pressure and, at higher pressures, the percentage of sputtered atoms reaching the anode is greatly reduced.
  • Various schemes have been proposed to increase the current density in a closed system by the employment of a magnetic field to deflect the ions and electrons to achieve a greater percentage of particle collisions and thus increased ionization.
  • sputtering apparatus supply a continuous stream of an ionizable gas into the glow discharge region with the pressure being maintained at a given level by exhausting gas from the region at a given rate.
  • the relationship between the current and the pressure of the region. as Well as the sputtering rate is the same as for a closed 3,369,990 Patented Feb. 20, 1968 system and any increase in current is only achieved by an increase in pressure which ultimately reduces the deposition rate.
  • the deposition rate is achieved by supplying ionized gas or plasma to the glow discharge without relying upon the glow discharge phenomenon for the creation of such ions.
  • the pressure required for operation of the apparatus is only a minimum pressure required to sustain the glow discharge mechanism necessary to provide the appropriate electric field and current conductance.
  • the deposition rate can be increased by increasing the ion density in the glow discharge region and thus increasing the ionic bombardment of the cathode without increasing the pressure in the glow discharge region.
  • a feature, then, of the present invention resides in a cathode sputtering apparatus which is provided with one or more sources of an ionized gas or plasma and means to exhaust the apparatus to maintain a constant pressure in such apparatus. More specifically, a feature of the present invention resides in means for supplying a continuous flow of an ionizable gas to one or more positions adjacent the glow discharge region and in means to ionize the gas prior to its injection into the glow discharge region and to control the rate of such ionization.
  • FIGURE 1 is a cross-sectional view of a cathode sputtering apparatus employing features of the present inventron;
  • FIGURE 2 is a detailed illustration of a source of ionizable gas and a gas ionizer such as is employed in the present invention
  • FIGURE 20 is a cross-sectional view of the gas ionizer as shown in FIGURE 2;
  • EIGURE 3a is an illustration of the glow discharge region of a cathode sputtering apparatus not employing the present invention.
  • EIGURE 3b is an illustration of the glow discharge region of a sputtering apparatus employing the present invention.
  • the mechanism by which the discharge is sustained is referred to as the abnormal glow discharge phenomenon where the current through the gas is a function of the applied voltage.
  • two particular zones of the glow d scharge are most important in the maintenance of the discharge.
  • One such zone is referred to as the Crookes dark space or the cathode dark space and consists primanly of positive ions, the more mobile electrons having been more quickly accelerated toward the anode. Because of this positive region, the established field or voltage drop is primarily across this zone and extending to the cathode.
  • the second zone of importance is adjacent the Crookes dark space on the anode side and is one in which the major portion of the ionization takes place due to collision between gas molecules and the secondary electrons emitted from the cathode and accelerated through the above referred to field.
  • This second region is referred to as the negative glow zone and is more thoroughly described in any standard text on glow discharges and gaseous conductors as is the entire glow discharge phenomenon.
  • the secondary electron emission and the negative glow zone are essential to the sustaining of the glow discharge phenomenon.
  • atoms of the cathode surface material are ejected as are the secondary electrons required to maintain the sustained glow discharge phenomenon.
  • the traverse of the glow discharge region by the ejected atoms is the result of the kinetic energy and momentum transferred to the ejected atoms at the time of the ejectment and it is to be noted that the majority of the ejected or sputtered atoms are not ionized nor can it be said that their motion is in any way due to the electric field.
  • FIGURE 1 wherein the sputtering apparatus is contained within a conventional bell jar vacuum system such as might be employed for laboratory experiments or in the manufacture of discrete layers of sputtered films.
  • a conventional bell jar vacuum system such as might be employed for laboratory experiments or in the manufacture of discrete layers of sputtered films.
  • FIGURE 1 is intended to be illustrative and that the dimensions and spacings between the respective components do not necessarily correspond to the actual dimensions that would be employed.
  • an ionizable gas is supplied by conduit 16 to regions adjacent the glow discharge maintained between sputtering cathode 12 and sputtering anode 13, conduit 16 extending through base plate 11 which completes the vacuum seal of bell jar 10.
  • the pressure is controlled by 9 regulation of valve 18 in the gas supply conduit 16 and by valve 20 in exhaust conduit 19 that also extends through base plate 11 into the interior of bell jar 10 and is connected to an appropriate vacuum pump.
  • the ionizable gas is injected into the glow discharge region, it is passed through plasma or ion generators 17, the number of such generators and conduits 16 preferably being so chosen and arranged as to be symmetrically disposed about the glow discharge region.
  • Cathode shield 21 is so arranged about sputtering cathode 12 so as to prevent bombardment of the cathode except on the surface of cathodic material 14 which is the material chosen to be sputtered onto substrate of anode 12.
  • Ion or plasma generator 17 is illustrated in more detail in FIGURES 2 and 212, FIGURE 2a representing a crosssection of the plan view illustrated in FIGURE 2.
  • Each of generators 17 include a metal cylinder 27 which serves as an electron collector or anode and contains two ports 28 through which is inserted a thermionic wire 26 to act as a cathode.
  • This cathode is coupled across an alternating voltage source 23 by conductors 24 and 25 with one side of voltage source 23 being grounded.
  • the frequency of voltage source 23 may be a standard 60 cycle frequency and voltage magnitude may be of just suflicient voltage to heat thermionic wire 26, preferably 4 to 6 volts.
  • Anode 27 is coupled to an appropriate positive voltage supply preferably approximately 50-100 volts.
  • the thermionic cathode 26 becomes sufiiciently heated, electrons are emitted therefrom and accelerated toward the cylindrical walls of anode 27.
  • the ionizable gas such as air or its constituents nitrogen and oxygen and the like is passed through the electron field, the resulting collisions between the gas molecules and the electrons result in ionization of the gas in the form of both positive ions and electrons which plasma is then introduced into the glow discharge region between sputtering cathode 12 and sputtering anode 13.
  • conduit 16 that ejects the ionizable gas through generator 17, generator 17 and the glow discharge region between sputtering cathode 12 and anode 13 are not particularly critical although the orifice of conduit 16 should be positioned as close as practical to plasma generator 17 which in turn should be positioned as close as practical to the glow discharge region without actually extending into that region.
  • the sputtering anode is grounded and the sputtering cathode is maintained at a negative potential of 5,000 volts with the spacing between the cathode and anode being approximately one and one-half inches although the values of these dimensions may be varied.
  • the plasma enters the glow discharge region it is similar in character to that portion of the region that is closer to the anode (the positive column that will be more thoroughly described below) and the plasma has a marked effect upon the structure of the glow discharge region although the gas pressure is not varied.
  • the gas pressure in the sputtering apparatus is controlled by controlling the amount of gas that enters the apparatus as well as the amount of gas exhausted therefrom. For the purposes of the following description of this effect and operation of the apparatus of the present invention, it is assumed that pressure is maintained constant and is preferably between 20 and microns of mercury.
  • FIGURE 3a illustrates a glow discharge for a situation in which there is no external source of ions and the characteristics of this region will now be briefly described in order to distinguish from the characteristics of the glow discharge of apparatus employing the present invention.
  • the region between the cathode and anode is divided into five zones labeled A, B, C, D and E.
  • the respective zones are denoted by various degrees of stippling to indicate differences in magnitude of light intensity of each zone in such a manner that the more heavy stippling represents darker zones and the lesser degrees of stippling represent brighter zones.
  • Region B represents the Crookes dark space which was briefly described above and which consists primarily of positive ions with the heaviest positive density being at the anode side of the zone.
  • zone C which has the brightest glow of any of the zones in the glow discharge and which is characterized by a slight excess of negative charges due to the electrons having been accelerated from the cathode across the voltage drop through zones A and B.
  • Zone A is generally referred to in the literature as the cathode glow zone and contains an excess of negative charges due to the secondary electron emission resulting from the ionic bombardment of the cathode surface.
  • Zone D has less intensity than the negative glow zone and is referred to in the literature as the Faraday dark space while zone E is referred to as the positive column, the Faraday dark space and the positive column being essentially neutral although ionized. Any ion motion in zone D and zone E is primarily by diffusion as there is little or no field in these zones.
  • the boundaries between zones C and D and between zones D and E are indicated by broken lines since at the reduced pressures employed in apparatus of the present invention the existence of these zones is difiicult to detect. It is also because of the reduced pressures employed in the present invention that the zones of the glow discharge as represented by FIGURE 3a will appear to be distorted compared to illustrations found in standard textbooks which are generally for glow discharges at higher pressures.
  • the thickness of the Crokes dark space is inversely proportional to the pressure and some authors attribute this to the fact that the mean free path of electrons traversing the Crookes dark space make a fixed number of collisions before passing out of the dark space into the nega tive glow zone where they play a part in the establishing of additional ionization.
  • FIGURE 3b is an illustration of the glow discharge region for apparatus employing the present invention.
  • the increase of ions in the glow discharge region has the effect of increasing the conductivity and the current density without any increase in pressure being required.
  • the change observed in the glow discharge region is that the Crookes dark space B of FIGURE 3b is decreased with the negative glow zone C being moved upwardly with an apparent expansion of the positive column E.
  • the resultant increased sputtering rate with such an increase in current density without a pressure increase is illustrated by the data listed below for the deposition of silicon dioxide (SiO where the cathode material is silicon and the gas supplied through the respective plasma generators consists of approximately 99 percent Argon (A) and 1 percent of oxygen (0 The cathode voltage was held at a negative potential of 5,000 volts and the pressure was approximately 60 microns of mercury. Under these conditions the current established in the glow discharge region was approximately 100 milliamperes and the rate of silicon dioxide deposited upon the anode substrate was measured at approximately 500 Angstroms per minute. Under similar conditions without the ion generator, a current of only 65 milliamperes was established and the deposition rate was only approximately 100 Angstroms per minute.
  • oxygen is employed to react with the silicon to form silicon dioxide, a small percentage of oxygen is employed in the above described atmosphere since an increase in the amount of oxygen results in'an excessively thick layer of oxide being formed on the cathode to the detriment of the sputtering rate.
  • the thermionic cathode constructed of a tungsten wire is supplied with an alternating current of 60 cycles and approximately 4.5 volts and anode 27 is maintained at approximately volts to establish an anode current of approximately 500 milliamperes.
  • the abnormal cathode drop is expressed by the relation I where E and F are constants, j is the current density and p is the gas pressure.
  • the pressure in the sputtering apparatus should be greater than 20 microns of mercury in order to achieve sufiicient current density, it has been observed that the sputtering rate decreases markedly when the pressure is increased above microns as the sputtered molecules encounter too many collisions on their was to the anode.
  • the present invention is particularly adaptable for the sputtering of refractory materials and various glasses by reactive sputtering wherein a constituent of the ionized gas is employed to react with the material sputtered from the cathode to form the deposited layer as is the situation in the above described example
  • the present invention is also readily adaptable to other applications of ionic bombardment of a cathode such as might be employed in cleaning a substrate positioned on the face of the cathode andother similar applications.
  • an ionizing means positioned adjacent said region and including a thermionic cathode, an electron collector positioned adjacent said thermionic cathode, and positively biased with respect thereto to establish an electron stream between said thermionic cathode and said collector, a gas supply conduit in said space having an orifice directed toward said region to continuously supply an ionizable gas generally transversely through said stream, said ionizing means positioned with the electron stream outside said region and traversing the flow of gas from said orifice of said gas supply conduit thereby causing the ionization of said gas.
  • Apparatus according to claim 1 that includes at least two of said supply conduits and ionizing means which are positioned symmetrically about said region and in a plane residing between said anode and said cathode.
  • Apparatus according to claim 1 including at least two of each of said ionizing means and conduits symmetrical- 1y positioned about said region and in a plane residing between said layer and said substrate.
  • said electron collector is comprised of a generally cylindrical element 5 which receives the gas from said gas supply conduit.

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US422667A 1964-12-31 1964-12-31 Cathodic sputtering apparatus including thermionic means for increasing sputtering efficiency Expired - Lifetime US3369990A (en)

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Application Number Priority Date Filing Date Title
US422667A US3369990A (en) 1964-12-31 1964-12-31 Cathodic sputtering apparatus including thermionic means for increasing sputtering efficiency
FR42301A FR1459624A (fr) 1964-12-31 1965-12-15 Appareil de pulvérisation cathodique
DE19651515305 DE1515305A1 (de) 1964-12-31 1965-12-15 Verfahren und Vorrichtung zur Kathodenzerstaeubung
GB54281/65A GB1100198A (en) 1964-12-31 1965-12-22 Improvements in or relating to cathodic sputtering

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3515663A (en) * 1968-02-01 1970-06-02 Hewlett Packard Co Triode sputtering apparatus using an electron emitter
US3516919A (en) * 1965-12-17 1970-06-23 Bendix Corp Apparatus for the sputtering of materials
US4175029A (en) * 1978-03-16 1979-11-20 Dmitriev Jury A Apparatus for ion plasma coating of articles
US5482611A (en) * 1991-09-30 1996-01-09 Helmer; John C. Physical vapor deposition employing ion extraction from a plasma
US20130327634A1 (en) * 2012-06-08 2013-12-12 Chang-Beom Eom Misaligned sputtering systems for the deposition of complex oxide thin films

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54110988A (en) * 1978-01-31 1979-08-30 Nii Chiefunorogii Afutomobirin Coating vacuum evaporation apparatus

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3021271A (en) * 1959-04-27 1962-02-13 Gen Mills Inc Growth of solid layers on substrates which are kept under ion bombardment before and during deposition
US3133874A (en) * 1960-12-05 1964-05-19 Robert W Morris Production of thin film metallic patterns
US3233137A (en) * 1961-08-28 1966-02-01 Litton Systems Inc Method and apparatus for cleansing by ionic bombardment
US3296114A (en) * 1963-07-17 1967-01-03 Lloyd Metal Mfg Company Ltd Anodizing apparatus
US3324019A (en) * 1962-12-11 1967-06-06 Schjeldahl Co G T Method of sputtering sequentially from a plurality of cathodes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3021271A (en) * 1959-04-27 1962-02-13 Gen Mills Inc Growth of solid layers on substrates which are kept under ion bombardment before and during deposition
US3133874A (en) * 1960-12-05 1964-05-19 Robert W Morris Production of thin film metallic patterns
US3233137A (en) * 1961-08-28 1966-02-01 Litton Systems Inc Method and apparatus for cleansing by ionic bombardment
US3324019A (en) * 1962-12-11 1967-06-06 Schjeldahl Co G T Method of sputtering sequentially from a plurality of cathodes
US3296114A (en) * 1963-07-17 1967-01-03 Lloyd Metal Mfg Company Ltd Anodizing apparatus

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3516919A (en) * 1965-12-17 1970-06-23 Bendix Corp Apparatus for the sputtering of materials
US3515663A (en) * 1968-02-01 1970-06-02 Hewlett Packard Co Triode sputtering apparatus using an electron emitter
US4175029A (en) * 1978-03-16 1979-11-20 Dmitriev Jury A Apparatus for ion plasma coating of articles
US5482611A (en) * 1991-09-30 1996-01-09 Helmer; John C. Physical vapor deposition employing ion extraction from a plasma
US20130327634A1 (en) * 2012-06-08 2013-12-12 Chang-Beom Eom Misaligned sputtering systems for the deposition of complex oxide thin films

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DE1515305A1 (de) 1969-08-14
GB1100198A (en) 1968-01-24
FR1459624A (fr) 1966-11-18

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