US20060207890A1 - Electrochemical etching - Google Patents

Electrochemical etching Download PDF

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Publication number
US20060207890A1
US20060207890A1 US11/081,762 US8176205A US2006207890A1 US 20060207890 A1 US20060207890 A1 US 20060207890A1 US 8176205 A US8176205 A US 8176205A US 2006207890 A1 US2006207890 A1 US 2006207890A1
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workpiece
etchant
acid
etch
layer
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Norbert Staud
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WD Media LLC
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Assigned to KOMAG, INC. reassignment KOMAG, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: STAUD, NORBERT
Priority to JP2006070731A priority patent/JP2006257553A/ja
Publication of US20060207890A1 publication Critical patent/US20060207890A1/en
Assigned to WD MEDIA, INC. reassignment WD MEDIA, INC. MERGER (SEE DOCUMENT FOR DETAILS). Assignors: KOMAG, INC.
Priority to US12/966,859 priority patent/US9068274B1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
    • C25F3/00—Electrolytic etching or polishing
    • C25F3/02—Etching
    • C25F3/14—Etching locally

Definitions

  • Embodiments of this invention relate to the field of etching and, more specifically in one embodiment, to the anisotropic, electrochemical etching of metallic materials.
  • the etchant contains an electrolyte, which may not be capable of etching a material to be etched through a chemical reaction (i.e., the etchant does not etch merely through contact with the material).
  • an electrolytical process By applying an electric voltage to the etchant between the material and an electrode immersed in the etchant, an electrolytical process, however, is initiated, in which the material is one pole, (e.g., the anode), and the electrode the opposite pole.
  • electric current flows in the etchant, and ions in the etchant react in an etching manner with the material.
  • Etch Width may be expressed as: X - Y - 2 AR * Z
  • An AR of 1 adds twice the etch depth Z to the width of the originally exposed gap area of the disk surface.
  • An AR of 1.5 translates to an added etch width that is 1.33 times the depth Z during the etch process. For example, for a target depth Z of 40 nanometers (nm), an AR of 1 results in 80 nm being added to the starting width, whereas an AR of 1.5 adds 53 nm and an AR of 2 adds 40 nm.
  • FIG. 1 illustrates a difference between an AR of 1 and an AR of 2 for a typical electrochemical, wet-etch process.
  • An embossable layer deposited over a nickel-phosphorous (NiP) layer of a disk substrate forms a width Y prior to a wet-etch process.
  • NiP nickel-phosphorous
  • the recessed area formed in the NiP layer after the etching process has a width X and a depth Z.
  • the acidic etchant typically produces an isotropic effect that undercuts the embossable layer to react with the NiP layer in all directions.
  • an AR of 1 produces a post-etch width of about 200 nm
  • an AR of 2 produces a post-etch width of about 150 nm. Because the width of the recessed area is significantly greater than the depth in typical wet-etch processes (i.e., AR values around 1), achieving high area densities is virtually impossible.
  • Olsson U.S. Pat. No. 6,245,213 to Olsson et al. (hereinafter “Olsson”) describes a low concentration etchant, which etches isotropically in the absence of an electric field, etches anisotropically and at a higher rate, in the presence of the electric field. Olsson discloses that it is possible to etch lines and grooves having greater depth than width, with experiments showing a depth-to-width ratio of 3.5:1 when etching thin copper foil. However, there appears to be limits to how high the depth-to-width may be because the anisotropic nature of the etching process is based mainly on the relatively low concentration of the etchant.
  • FIG. 2 illustrates a graph showing a theoretical, calculated widening of the initial gap width as a function of the AR for an etch process for a targeted etch depth of 40 nm.
  • an AR value of 1 adds 80 nm to the initial gap width, and decreases (not linearly) as the AR value increases.
  • An AR value of 3 only adds about 25 nm to the initial gap width.
  • An AR value greater than 1 may be desirable in certain manufacturing processes such as in the manufacture of a discrete track recording disk in order to maximizing its recording density.
  • FIG. 1 illustrates the difference between different AR values for an etch process.
  • FIG. 2 illustrates a graph showing a theoretical, calculated widening of the initial gap width as a function of the AR for an etch process.
  • FIG. 3 illustrates a block diagram that provides an overview of an electrochemical, wet-etch process for forming a DTR pattern on the surface of a disk substrate.
  • FIG. 4B illustrates the disk substrate of FIG. 4A with an embossable layer deposited over the NiP layer.
  • FIG. 4C illustrates the disk substrate of FIG. 4A after it has been imprinted with a pattern of raised and recessed areas.
  • FIG. 5A shows an enlarged cross sectional view of the disk substrate of FIG. 4A with an electrochemical etchant dispensed over the embossable layer.
  • FIG. 5B shows the disk substrate of FIG. 4A with a recessed area formed within the NiP layer.
  • FIG. 6 illustrates the effect on the electric field by the embossable layer during the electrochemical, wet-etch process.
  • FIG. 7 is a block diagram of one method for forming a DTR pattern on a disk substrate using an anisotropic, wet-etch process.
  • FIG. 8 is a block diagram of another method for forming a DTR pattern on a disk substrate using an anisotropic, wet-etch process.
  • FIG. 9 is a block diagram of another method for forming a DTR pattern on a disk substrate using an anisotropic, wet-etch process.
  • FIG. 10 is a schematic view of an electrochemical bath.
  • FIG. 11 is a table showing examples of adsorbates.
  • first element disposed above or below another element may be directly in contact with the first element or may have one or more intervening elements.
  • a workpiece is disposed within an etchant solution having a composition comprising a dilute acid and a non-ionic surfactant.
  • An electric field is generated within the etchant solution to cause an anisotropic etch pattern to form on a surface of the workpiece.
  • the workpiece may be composed of any material that is capable of being etched or patterned electrochemically.
  • the workpiece may be a disk substrate having one or more layers disposed thereon.
  • the NiP layer may be formed by electroplating, electroless plating, or by other methods known in the art.
  • One benefit of plating the disk substrate with a rigid or metallic material such as NiP is providing mechanical support to the disk substrate for subsequent texturing, polishing, and/or patterning processes that may be used in the disk manufacturing process.
  • the NiP layer may then be coated with a resist, an imprintable, or other embossable layer material that in one embodiment, serve as a mask for the desired pattern during the etching process, block 303 .
  • Spin coating, dip coating, and spray coating are just some methods of depositing the embossable layer on the NiP layer.
  • the embossable layer is then imprinted with the desired pattern, block 304 .
  • a stamper having a negative, or inverse template of the desired pattern may be pressed against the embossable layer to form an initial pattern of raised areas and recessed areas. The recessed areas may then undergo an initial etching process (e.g., plasma ashing) to remove the embossable material and expose the NiP layer.
  • an initial etching process e.g., plasma ashing
  • reactive gas etching may be used to expose the NiP layer.
  • the exposed NiP areas may then undergo another etching process—an electrochemical, wet-etch—that includes an etchant made of a dilute acid combined with a non-ionic surfactant and/or surface adsorbate, block 305 .
  • the etchant may be dilute acid such as citric acid and a non-ionic surfactant (e.g., alkyl ethoxylates).
  • the etchant may be a dilute acid having a metal adsorbate (e.g., nickel adsorbate).
  • the etchant may be made of a dilute citric acid, a non-ionic surfactant, and a nickel adsorbate.
  • the electrochemical etch process discussed herein may be used to form a discrete track recording (DTR) pattern in a disk.
  • DTR pattern may be formed by nano-imprint lithography (NIL) techniques, in which a rigid, pre-embossed forming tool (a.k.a., stamper, embosser, etc.), having an inverse pattern to be imprinted, is pressed into an embossable film (i.e., polymer or embossable material) disposed above a disk substrate to form an initial pattern of compressed areas. This initial pattern ultimately forms a pattern of raised and recessed areas.
  • NIL nano-imprint lithography
  • an etching process is used to transfer the pattern through the embossable film by removing the residual film in the compressed areas.
  • another etching process may be used to form the pattern in a layer (e.g., substrate, nickel-phosphorous, soft magnetic layer, etc.) residing underneath the embossable film.
  • the resulting DTR track structure contains a pattern of concentric raised areas and recessed areas under a magnetic recording layer.
  • the raised areas also known as hills, lands, elevations, etc.
  • the recessed areas also known as troughs, valleys, grooves, etc.
  • etching process in the manufacture of a DTR disk is an important process to define the width and depth of grooves that separate the raised areas from each other. For a given target depth, it is desirable to keep the final width of the groove as narrow as possible in order to achieve high storage or magnetic area densities.
  • FIGS. 4A-4C show expanded cross sectional views illustrating one embodiment of preparatory stages of a disk substrate prior to an electrochemical, wet-etch process.
  • the etch process is used to form a DTR on a NiP layer of a longitudinal magnetic recording disk.
  • the various layers illustrated in FIGS. 4A-4C are exemplary and may not be scaled to representative sizes.
  • the DTR process begins with a NiP layer 402 plated over disk-shaped substrate 401 .
  • Disk substrate 401 may be made of a number of materials including metals (e.g., aluminum), glass, ceramic, or other conventional disk substrate materials known in the art.
  • NiP layer 402 may be formed by electroplating, electroless plating, or by other methods known in the art.
  • Plating disk substrate 401 with a rigid or metallic material such as NiP provides mechanical support to disk substrate 402 for subsequent texturing, polishing, and/or patterning processes.
  • the surface of NiP layer 402 may be textured and polished as illustrated by FIG. 4A .
  • NiP layer 402 may be polished, for example, by a uniform etch. In alternative embodiments, other polishing techniques may be used. Polishing techniques are well known in the art; accordingly, a detailed discussion is not provided.
  • embossable layer 403 is shown after it has been imprinted with a pattern of raised areas 404 , 405 and recessed areas 406 , 407 , followed by an etching (i.e., ashing) process to remove embossable material in the recessed areas.
  • the imprinting of embossable layer 403 may utilize, for example, nano-imprint lithography techniques that are well known in the art.
  • a stamper (not shown in FIG. 4C ) bearing a discrete track recording pattern, may be used to imprint embossable layer 403 to form raised areas 404 , 405 and recessed areas 406 , 407 .
  • embossable layer 403 Because of the thickness of the embossable layer 403 , the imprint of raised and recessed areas is not likely to press into NiP layer 402 . Alternatively, if embossable layer 403 is relatively thin, it may be stamped to leave very little embossable material in the recessed areas 406 , 407 . Subsequently, embossable material in the recessed areas 406 , 407 may be removed to expose NiP layer 402 as shown. In one embodiment for example, plasma ashing may be used to remove embossable material in recessed areas 406 , 407 to expose NiP layer 402 .
  • Chemical etching removes embossable layer 403 in both the raised areas 404 , 405 and recessed areas 406 , 407 until NiP layer 402 is exposed in the recessed areas 406 , 407 .
  • Disk substrate 425 and first electrode may be spaced between about 1 mm to about 10 mm. Alternatively, another spacing may be used.
  • FIGS. 5A-5B illustrate enlarged views of raised areas 404 , 405 that define recessed area 406 that exposes a surface of NiP layer 402 .
  • FIG. 5A illustrates etchant 410 dispensed over embossable layer 403 and the exposed area (i.e., recessed area 406 ) of NiP layer 402 .
  • Raised areas 404 , 405 of NiP layer 404 define recessed area 406 which also forms the initial gap width (Y) 420 of the surface of NiP layer 402 to be etched.
  • Y initial gap width
  • FIG. 5B illustrates a recessed area 425 formed within NiP layer 402 substantially below recessed area 406 .
  • Recessed area 425 may be defined by a final etch width (X) 421 and an etch depth (Z) 422 .
  • the use of the various etchants described herein produces recessed area 425 with an AR value that is significantly greater than 1.
  • etchant 410 may be made of an acid such as oxalic acid (also known as ethanedioic acid, HO 2 CCO 2 H), and citric acid (also known as 2-hydroxy-1,2,3-propanetricarboxylic acid, HO 2 CCH 2 C(OH)(CO 2 H)CH 2 CO 2 H), each having a pH greater than or equal to 2, with the addition of a non-ionic surfactant such as an alkyl ethoxylate blend (C7-C10 alkyl chain, molecular weight about 550).
  • the addition of the non-ionic surfactant increases the AR significantly and reproducibly to an AR above 1.3, relative to an AR value measured using only hydrochloric acid, by producing an anisotropic etch effect.
  • recessed areas may be anisotropically etched by a combination of a dilute acid with a NiP adsorbate.
  • the adsorbate component of etchant 410 may act as a corrosion inhibitor to prevent the acid from reacting with the NiP near the sidewalls of the recessed areas, thereby creating a greater reaction bias near a center portion the recessed areas. Examples of adsorbates are shown in the table of FIG.
  • BTA benzotriazole
  • BPA 2-benzimidazole proprionic acid
  • BSA 1H-benzimidazole-2-sulfonic acid
  • SBA 2-sulfobenzoic acid hydrate
  • MBI 2-mercapto benzimidazole
  • A300 corrosion inhibitor A300
  • C10-C16 alkyl benzene sulfonic acid ABSA
  • an anisotropic etch effect may also be achieved by the addition of a NiP adsorbate to the dilute acid/non-ionic surfactant etchant.
  • the addition of an adsorbate to the etchant increases the AR significantly and reproducibly to an AR above 1.4, relative to an AR value measured using only hydrochloric acid.
  • the etchant with the non-ionic surfactant/adsorbate mixture may be, in one embodiment, a citric acid/alkyl ethoxylate/benzene sulfonic acid mixture ranging from a 3.5% solution to a 0.025% solution.
  • the 3.5% solution includes citric acid of about 8.75 g/l (45.0 mM), benzene sulfonic acid of about 1.75 g/l (5.4 mM), and a pH of about 2.3.
  • the 0.025% solution includes citric acid of about 0.063 g/l (0.32 mM), benzene sulfonic acid of about 0.0125 g/l (0.039 mM), and a pH of about 3.7.
  • the conductivity of the etchants may be between about 0.43-0.12 mS.
  • the electric field gradients 533 , 534 cause the adsorbates and non-ionic surfactants to accumulate near the edges of the sidewalls (i.e., gap width ends) of raised areas 504 , 505 , and preferentially adsorb on the NiP layer 502 near the side walls, thereby promoting anisotropic etching of the NiP layer.
  • a constant 0.5 amp current (about 9.2V) was applied to the etchant for 9 seconds.
  • the current density was greater than about 50 mA/cm 2 during the etch.
  • HCL control etch Normalized to the first etch process (HCL control etch), an AR value of about 1.4 was produced. Compared to the HCL control that produced an AR of 1, the AR produced by this etchant proved to be statistically significant.
  • FIGS. 7-9 are block diagrams of various methods for forming etch patterns on a disk substrate using an anisotropic, wet-etch process.
  • the wet etch process maximizes AR values to produce disk having high storage density.
  • a disk substrate may be patterned for production as a magnetic recording disk, or other types of digital recording disks such as CD's or DVD's, or alternatively, for semiconductor wafers or display panels.
  • a disk substrate e.g., disk 401
  • NiP layer e.g., NiP layer 402
  • the disk substrate may be a metal or metal alloy such as AlMg.
  • the NiP layer may be formed by electroplating, electroless plating, or by other methods known in the art.
  • an etchant having a dilute acid with a non-ionic surfactant may be applied to the exposed surface of the NiP layer to form a recessed area (i.e., the grooves of the etch pattern), block 705 .
  • a bath similar to that described above with respect to FIG. 10 may be used apply the etchant.
  • the dilute acid may be citric acid or oxalic acid.
  • the non-ionic surfactant may be an alkyl ethoxylate or alkyl ethoxylate blend, with C7-C10 alkyl chain, and a molecular weight of about 550.
  • the etchant may be about a 4.5 mM citric acid or oxalic acid solution with alkyl ethoxylate. In another embodiment, the etchant may be about a 1.5 mM oxalic acid solution with alkyl ethoxylate.
  • An electric field may then be generated within the etchant, block 706 . In one embodiment, the electric field is generated by applying a current to the etchant. In one embodiment, a current between about 0.05 amp to 2.0 amp may be applied to the dilute acid and non-ionic surfactant.
  • the conductivity of the etchant solution may be between about 0.43-0.12 mS.
  • the etch rate may be constant or variable, with etch rates between about 5 nm/sec to about 20 nm/sec.
  • an etchant having a dilute acid with a NiP adsorbate may be applied to the exposed surface of the NiP layer to form a recessed area (i.e., the grooves of the etch pattern), block 707 .
  • Adsorbates refer to chemicals that affect the surface properties of NiP.
  • adsorbates may be responsible for increased AR by preferential, strong adsorption to sidewalls of recessed areas because of small electric field gradients between sidewalls and the center of recessed area. This results in faster electro-migration and diffusion from bulk electrolyte to the sidewalls.
  • the adsorbates may be preferentially distributed near the sidewalls of the recessed areas to localize reaction of the acid with the NiP near the center of the recessed area.
  • adsorbates include MBI, SBA, ABSA, A300, BTA, BPA, and BSA.
  • an etchant having a dilute acid, a non-ionic surfactant, and a NiP adsorbate may be applied to the exposed surface of the NiP layer to form a recessed area (i.e., the grooves of the etch pattern), block 708 .
  • the etchant may be citric acid with a non-ionic alkyl ethoxylate blend and alkylbenzenesulfonic acid.
  • the apparatus and methods discussed herein may be used with various types of workpieces. As discussed above, the apparatus and methods discussed herein may be used for the etching of disk surfaces for the production of magnetic recording disks.
  • the magnetic recording disk may be, for example, a DTR longitudinal magnetic recording disk having, for example, a nickel-phosphorous (NiP) plated substrate as a base structure.
  • the magnetic recording disk may be a DTR perpendicular magnetic recording disk having a soft magnetic film disposed above a substrate for the base structure.
  • the apparatus and methods discussed herein may be used for the manufacture of other types of digital recording disks, for example, optical recording disks such as a compact disc (CD) and a digital-versatile-disk (DVD).
  • the apparatus and methods discussed herein may be used in the manufacture of other types of workpieces, for example, the semiconductor wafers, and display panels (e.g., liquid crystal display panels).

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