Classifications

• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
  • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
  • G03F7/0002—Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
  • H01L21/0271—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B81—MICROSTRUCTURAL TECHNOLOGY
  • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
  • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
  • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
  • B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
  • B81C1/00031—Regular or irregular arrays of nanoscale structures, e.g. etch mask layer
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
  • C08F212/02—Monomers containing only one unsaturated aliphatic radical
  • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
  • C08F212/06—Hydrocarbons
  • C08F212/08—Styrene
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
  • C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
  • C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
  • C08F299/022—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polycondensates with side or terminal unsaturations
  • C08F299/024—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates from polycondensates with side or terminal unsaturations the unsaturation being in acrylic or methacrylic groups
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
• • G—PHYSICS
  • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
  • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
  • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
  • G03F7/0035—Multiple processes, e.g. applying a further resist layer on an already in a previously step, processed pattern or textured surface
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/02104—Forming layers
  • H01L21/02107—Forming insulating materials on a substrate
  • H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
  • H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
  • H01L21/02118—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer carbon based polymeric organic or inorganic material, e.g. polyimides, poly cyclobutene or PVC
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/02104—Forming layers
  • H01L21/02107—Forming insulating materials on a substrate
  • H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
  • H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
  • H01L21/02293—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process formation of epitaxial layers by a deposition process
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
  • H01L21/0271—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers
  • H01L21/0273—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising organic layers characterised by the treatment of photoresist layers
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/027—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34
  • H01L21/033—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising inorganic layers
  • H01L21/0334—Making masks on semiconductor bodies for further photolithographic processing not provided for in group H01L21/18 or H01L21/34 comprising inorganic layers characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane
  • H01L21/0338—Process specially adapted to improve the resolution of the mask
• • 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
  • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
  • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
  • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
  • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
  • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
  • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
  • H01L21/308—Chemical or electrical treatment, e.g. electrolytic etching using masks
  • H01L21/3083—Chemical or electrical treatment, e.g. electrolytic etching using masks characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane
  • H01L21/3086—Chemical or electrical treatment, e.g. electrolytic etching using masks characterised by their size, orientation, disposition, behaviour, shape, in horizontal or vertical plane characterised by the process involved to create the mask, e.g. lift-off masks, sidewalls, or to modify the mask, e.g. pre-treatment, post-treatment
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B81—MICROSTRUCTURAL TECHNOLOGY
  • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
  • B81C2201/00—Manufacture or treatment of microstructural devices or systems
  • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
  • B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
  • B81C2201/0147—Film patterning
  • B81C2201/0149—Forming nanoscale microstructures using auto-arranging or self-assembling material
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B81—MICROSTRUCTURAL TECHNOLOGY
  • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
  • B81C2201/00—Manufacture or treatment of microstructural devices or systems
  • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
  • B81C2201/0198—Manufacture or treatment of microstructural devices or systems in or on a substrate for making a masking layer
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L25/00—Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
  • C08L25/02—Homopolymers or copolymers of hydrocarbons
  • C08L25/04—Homopolymers or copolymers of styrene
  • C08L25/06—Polystyrene
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
  • C08L33/04—Homopolymers or copolymers of esters
  • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
  • C08L33/10—Homopolymers or copolymers of methacrylic acid esters
  • C08L33/12—Homopolymers or copolymers of methyl methacrylate

Definitions

• the present invention relates to a method of forming a chemical guiding structure for the self-assembly of a block copolymer by chemo-epitaxy.
• the present invention also relates to a method of chemo-epitaxy from a chemical guiding structure.
• Directed self-assembly is an emerging lithography technique for forming critical dimension patterns smaller than 30 nm. This technique is a cheaper alternative to extreme ultraviolet lithography (EUV) and electron beam lithography (e-beam).
• EUV extreme ultraviolet lithography
• e-beam electron beam lithography
• the known processes for self-assembly of block copolymers can be grouped into two categories: grapho-epitaxy and chemo-epitaxy.
• Grapho-epitaxy consists in forming primary topographic patterns called guides on the surface of a substrate, these patterns delimiting zones within which a layer of block copolymer is deposited.
• the guide patterns control the organization of the copolymer blocks to form higher resolution secondary patterns within these areas.
• Chemo-epitaxy consists in modifying the chemical properties of certain regions of the surface of the substrate, to guide the organization of the block copolymer subsequently deposited on this surface.
• the chemical modification of the substrate can in particular be obtained by grafting a polymer neutralization layer. Then, this neutralization layer is structured to create a chemical contrast on the surface of the substrate.
• the regions of the substrate not covered by the neutralization layer have a preferential chemical affinity for one of the blocks of the copolymer, while the regions of the substrate covered by the neutralization layer have an equivalent chemical affinity for all the blocks of the copolymer.
• the structuring of the neutralization layer is conventionally obtained by an optical or electron beam lithography step.
• the article of C-C. Liu et al. entitled ["Integration of block copolymer directed assembly with 193 immersion lithography", J. Vac. Self. Technol., B 28, C6B30-C6B34, 2010] discloses a chemopitaxis method comprising forming a chemical guiding structure on the surface of a substrate.
• the chemical guiding structure is composed of guiding units of a polymer having a preferential affinity for one of the blocks of the copolymer and a random copolymer film grafted onto the substrate outside the patterns, in a so-called back region. -plan.
• the random copolymer is neutral with respect to the block copolymer, so that the domains of the copolymer are (after assembly) oriented perpendicularly to the substrate.
• the chemical guiding structure is intended to direct the self-assembly of the PS-b-PMMA (polystyrene-b / oc-polymethylmethacrylate) block copolymer.
• the guide patterns in the form of lines, consist of cross-linked polystyrene (X-PS).
• the random copolymer, grafted between the lines, is PS-r-PMMA.
• this chemo-epitaxy process firstly comprises forming a cross-linked polystyrene film 11 on a silicon substrate 10.
• a mask consisting of resin patterns 12 is then formed on the film of crosslinked polystyrene 1 1, by optical lithography (typically 193 nm immersion). Then, the dimensions of the resin patterns 12 are reduced by an oxygen-based plasma step in order to obtain a width W of the order of the half-period of the block copolymer.
• the cross-linked polystyrene film 11 is also etched through the mask 12 by the plasma. This etching step is commonly called "trim etch".
• Cross-linked polystyrene units in the form of parallel lines, are thus formed on the substrate 10.
• the polystyrene lines 11 ' have a width W equal to 15 nm and are spaced two by two by a distance Ls equal to 90 nm.
• the substrate 10 is covered with a solution comprising the graftable random copolymer, then the random copolymer is grafted between the lines 11 'to form a neutralization layer 13.
• a layer of PS- b-PMMA 14 is deposited and then assembled on the guide structure composed of the polystyrene lines 1 'and the neutralization layer 13.
• the crosslinkable polymer layer must be very thin (typically less than or equal to 10 nm) and uniform in thickness to ensure, after assembly of the block copolymer, a good quality transfer of the patterns in the underlying layers. But when the polymer is deposited by centrifugation ("spin coating" in English), it is difficult with such a method to obtain a thin layer and constant thickness. In particular, problems of dewetting of the polymer are observed. Moreover, crosslinking has a planarizing effect. Thus, when the starting surface is not flat but has a topology, it is even more difficult to obtain a uniform layer thickness.
• the aim of the invention is to make the formation of a chemical guiding structure on a substrate simpler and of better quality, with a view to its use in a chemo-epitaxy process, and to ensure better control of the thickness of this structure.
• the use of a graftable polymer - rather than a crosslinkable polymer material - to form the initial pattern greatly simplifies the formation of the chemical guiding structure.
• the chemical guiding structure is also of better quality, because the grafting makes it possible to obtain a very fine initial pattern (typically of thickness less than or equal to 10 nm) and uniform in thickness.
• the deposition is carried out in the same way, by centrifugation of a polymer solution, but on greater thicknesses, which avoids the problems of dewetting.
• the final thickness of the graft polymer is furthermore controlled by the grafting step, and not by the deposition step proper.
• This thickness is easily controllable, by varying the molar mass of the graftable polymer material and the grafting kinetics.
• the grafting temperature is advantageously lower than the degradation temperature of the polymer, in order to preserve the properties of the latter.
• the grafting makes it possible to obtain uniform thicknesses even on surfaces having a topology, since it does not have a planarizing effect (unlike crosslinking).
• the second polymer By choosing a second polymer of molar mass greater than that of the first polymer, it is avoided that the second polymer, deposited on the pattern (s) of the first polymer, covers the first graft polymer.
• the second polymer can thus be grafted only in the regions of the surface of the substrate that are not occupied by the first graft polymer.
• the second molar mass is preferably greater than or equal to 150% of the first molar mass, and more preferably greater than 200% of the first molar mass.
• the second molar mass is furthermore less than or equal to 500% of the first molar mass.
• the step of forming the initial pattern of the first polymer material comprises the following operations:
• the step of forming the initial pattern comprises the following operations:
• the first polymer material has a preferential affinity for one of the blocks of the copolymer and the second polymeric material is neutral with respect to the block copolymer.
• the step of forming the initial pattern comprises the following operations: - forming a mask on the substrate;
• the first polymer material is neutral with respect to the block copolymer and the second polymeric material has a preferential affinity for one of the blocks of the copolymer.
• the mask of the second and third embodiments advantageously comprises at least one spacer-shaped pattern of critical dimension less than 20 nm.
• the mask comprises at least two spacers of critical dimension substantially equal to half the natural period of the block copolymer and the spacers are further spaced two by two and center to center by a distance substantially equal to an integer multiple of the natural period of the block copolymer.
• the invention also relates to a method of chemopitaxis comprising forming a chemical guiding structure on a substrate using the forming method described above, depositing a block copolymer on the guiding structure. chemical and assembly of the block copolymer.
• FIG. 1, previously described, represents steps of a chemo-epitaxy process according to the prior art
• FIGS. 2A to 2G show steps of a method for forming a chemical guiding structure, according to a first embodiment of the invention
• FIGS. 3A to 3G represent steps of a method for forming a chemical guiding structure, according to a second embodiment of the invention
• FIGS. 4A to 4D show steps of a method for forming a chemical guiding structure, according to a third embodiment of the invention.
• FIGS. 5A to 5D show steps of a method for forming a chemical guiding structure, according to a fourth embodiment of the invention.
• FIGS. 6A to 6E show steps of a method for forming a chemical guiding structure, according to a fifth embodiment of the invention.
• FIGS. 7B and 7C represent an alternative embodiment of the steps represented by FIGS. 6B and 6C.
• Figure 8 shows schematically the assembly of a block copolymer deposited on the chemical guiding structure of Figure 2G, 3G, 4D, 5D or 6E.
• a chemical guiding structure here designates a set of at least two polymer units, arranged side by side on the substrate and having different chemical affinities, this set being repeated periodically on the surface of the substrate. A chemical contrast is thus created on the surface of the substrate.
• the substrate 100 is for example made of silicon.
• This chemical guiding (or contrast) structure is intended to be coated with a block copolymer, as part of a chemo-epitaxial directed block copolymer self-assembly process.
• the chemical contrast makes it possible to direct (or "Guide") the organization of the monomer blocks that make up the copolymer.
• the chemical affinities of the polymer units are relative to the blocks of the copolymer. These affinities can be chosen from the following possibilities:
• the guide structure 200 preferably has a plurality of guide patterns 210 and a neutralization layer 220.
• the neutralization layer 220 occupies a region of the surface of the substrate 100 adjacent to the guide patterns 210, and preferably the entire surface of the substrate 100 outside the guiding patterns 210.
• the guiding patterns 210 and the neutralization layer 220 function to chemically (and differently) functionalize the substrate 100. also be described as patterns and functionalization layer.
• the guiding units 210 are formed of a polymer having a preferential affinity for one of the blocks of the copolymer, while the neutralization layer 220 consists of a polymer whose affinity is neutral.
• grafting of a polymer on a substrate means the formation of covalent bonds between the substrate and the chains of the polymer.
• crosslinking of a polymer involves the formation of several bonds between the polymer chains without necessarily the formation of covalent bonds with the substrate.
• FIGS. 2A to 2G are sectional views illustrating steps S1 1 to S17 of the chemical guide structure forming method, according to a first embodiment of the invention.
• the first step S1 1 of the method comprises depositing a first layer 1 10 of sacrificial material on the substrate 100 and forming at least one cavity 1 1 1 in the first layer 1 10.
• a first layer 1 10 of sacrificial material is depositing on the substrate 100 and forming at least one cavity 1 1 1 in the first layer 1 10.
• several cavities 11 are formed in the first layer 1 10 of sacrificial material. For the sake of clarity, only two of these cavities 11 1 have been shown in Figure 2A.
• Each cavity 1 1 1 has a bottom January 12 and side walls 1 13 extending in a secant direction on the surface of the substrate 100.
• the side walls 1 13 extend in a direction perpendicular to the surface of the substrate 100.
• each cavity January 1 opens onto the surface of the substrate 100.
• the bottom 1 12 of the cavity 1 1 1 is constituted by the substrate 100, the surface is preferably flat.
• Each cavity 1 1 1 preferably has a depth H of between 30 nm and 150 nm and a width W 'of between 30 nm and 60 nm.
• the depth H of a cavity is measured perpendicularly to the surface of the substrate 100 (it is therefore equal to the thickness of the first layer 1 10 sacrificial material), while the width W 'of the cavity is measured parallel to the substrate surface 100 in the sectional plane of FIG. 2A.
• the cavities January 1 may in particular take the form of a trench, a cylindrical well or a well of rectangular section.
• the cavities 1 1 1 are straight trenches of identical dimensions and oriented parallel to each other. They also form a periodic structure, that is to say that they are spaced regularly.
• the period P of this structure is preferably between 60 nm and 140 nm.
• the sacrificial material of the first layer 1 is preferably chosen from materials that can easily be removed by wet etching and / or by dry etching, selectively with respect to the substrate 1 00.
• materials that can easily be removed by wet etching and / or by dry etching, selectively with respect to the substrate 1 00.
• the first layer 10 of sacrificial material can be formed of an antireflection coating containing silicon (also called "SiARC" for "Silicon-containing Anti-Reflective Coating").
• the cavities 11 1 can be formed by photolithography or other structuring techniques, such as electron beam lithography ("e-beam").
• e-beam electron beam lithography
• the formation of the cavities 11 may in particular comprise the following operations:
• a layer of resin or several layers intended to form a hard mask for example a stack of three layers successively comprising a spin-on carbon layer ("Spin On Carbon", SOC), an antireflection coating containing silicon (SiARC) and a resin layer;
• SOC spin On Carbon
• SiARC antireflection coating containing silicon
• the first layer 1 is advantageously etched anisotropically, for example by means of a plasma.
• An anisotropic etching technique provides better control of cavity dimensions 1 1 1.
• the method then comprises the formation of spacers against the side walls of the cavities 11, in order to reduce the width W 'of the cavities beyond the resolution limit of the photolithography, typically up to a value of between 10 nm and 20 nm.
• These spacers can be made in two successive steps S12 and S13, respectively represented by FIGS. 2B and 2C.
• a second layer 120 made of sacrificial material is conformally deposited on the substrate 100 covered with the first layer 1 10.
• the second layer 120 is thus of constant thickness and conforms to the relief of the first layer 1 10.
• the thickness of the second layer 120 is preferably between 5 nm and 25 nm.
• the conformal deposition technique used for depositing the second layer 120 is for example the Atomic Layer Deposition (or ALD), which may be plasma enhanced (PEALD, Plasma Enhanced Atomic Layer Deposition).
• the sacrificial material of the second layer 120 can in particular be chosen from silicon dioxide (SiO 2), a silicon oxynide (SiO x Ni), alumina (Al 2 O 3) and hafnium dioxide (HfO 2). It is not necessarily identical to the sacrificial material of the first layer 1 10.
• the second layer 120 is then etched anisotropically, preferably by means of a plasma.
• the preferred direction of etching is perpendicular to the surface of the substrate 100.
• This anisotropic etching step makes it possible to eliminate only the horizontal portions of the second layer 120, disposed above the first layer 1 and at the bottom of the cavities 1 1.
• the vertical portions of the second layer 120, arranged against the side walls 1 13 of the cavities January 1, are retained and constitute spacers 130.
• the etching of the second layer 120 is selective with respect to the substrate 100 and to the first layer 110.
• the substrate is preferably insensitive to the etching of the sacrificial material.
• a specific layer may be provided to protect the substrate 100 from etching.
• a first polymer 140 having a preferential affinity for one of the blocks of the copolymer is then grafted onto the substrate 100 at the bottom of the cavities 11 to 1.
• the first polymer 140 can be dissolved in a solvent to form a first polymer solution, and then the first solution is deposited on the substrate 100 until the cavities 11 are filled, partially or completely.
• the first polymer solution is preferably deposited on the substrate 100 by centrifugation (or "spin-coating" in English).
• the deposition of the first solution is followed by a grafting operation of the first polymer, for example by annealing.
• annealing is carried out at a temperature of 250 ° C.
• This solvent is, for example, propylene glycol monomethyl ether acetate (PGMEA).
• the molar mass M1 of the first polymer 140 is preferably less than 5 kg. mol -1 , to ensure a high graft density at the substrate 100.
• Step S15 of Figure 2E then consists in removing the first layer 110 and the spacers 130 of sacrificial material selectively relative to the substrate 100 and the first polymer 140 grafted onto the substrate.
• the first polymer 140 grafted onto the surface of the spacers 130 is eliminated at the same time as the spacers 130.
• the patterns of the first polymer grafted to the bottom 1 12 of the cavities 11 1. These patterns have the shape and dimensions of the bottom 1 12 of the cavities 1 1 1 1 after the step of forming the spacers 130 (see Fig.2C, reduction of the width W 'of the cavities 1 1 1).
• the units of the first polymer constitute the guiding units 210 of the chemical guiding structure 200.
• the first polymer 140 is preferably a homopolymer, for example polystyrene (h-PS) or polymethylmethacrylate (h-PMMA).
• step S15 can be carried out wet in a single operation if the sacrificial material of the first layer 1 and the sacrificial material of the spacers 130 are identical or at least sensitive to the same etching solution.
• the etching solution is, for example, a solution of hydrofluoric acid (HF) when the first layer 1 and the spacers 130 are in S1O2.
• the elimination of the first layer 110 and the spacers 130 may also be carried out in two successive operations.
• the sacrificial materials and the etching solutions are then necessarily different (for example HF for SiO 2, H 3 PO 4 for Si 3 N 4 ).
• Step S15 removal of the first layer 1 10 and spacers 130 is preferably followed by rinsing solvent (water, PGMEA %), to remove the etching residues.
• rinsing solvent water, PGMEA
• the first polymer solution is deposited in step S14 in excess thickness on the first layer 1 10.
• the first polymer 140 is then grafted also on the first layer 110 in sacrificial material.
• the first polymer guide patterns 210 and at least one region of the substrate 100 adjacent to the guide patterns 210 are covered with a film 150 of a second polymer solution.
• the second polymer solution is advantageously deposited on the entire surface of the substrate 100, preferably by centrifugation.
• the film 150 of the second solution then completely covers the substrate 100 and the guide patterns 210. Its thickness is typically between 15 nm and 100 nm (before grafting).
• the second polymer solution comprises a second polymer 160 dissolved in a solvent.
• the second polymer 160 has a molar mass M2 greater than that (M1) of the first polymer 140 and, in this first embodiment, a chemical affinity neutral with respect to the contemplated block copolymer. The attractive forces between each of the blocks of the copolymer and the second polymer 160 are then equivalent.
• the second polymer 160 is preferably a random copolymer such as PS-r-PMMA.
• the second polymer 160 is grafted onto the surface of the substrate 100, in the region or regions covered by the film 150.
• the grafting is carried out for example by annealing according to the same operating method. than that described in relation to FIG. 2D.
• the grafting is further advantageously followed by a solvent rinsing operation, in order to remove the second ungrafted polymer.
• the first polymer guide units 210 having a high graft density they are not affected by the grafting of the second polymer 160 of larger molar mass M2. Indeed, the lower the molar mass of a graftable polymer, the shorter the polymer chains, and the spaces between these chains are reduced. As a result, a higher molecular weight polymer (i.e. having longer chains) can not penetrate these spaces.
• the second graft polymer 160 thus forms the neutralization layer 220 of the guiding structure 200.
• the neutralization layer 220 advantageously covers the entire surface of the substrate 100, with the exception of the locations occupied by the guiding patterns 210.
• the molar mass M2 of the second polymer 160 is advantageously greater than or equal to 150% of the molar mass M1 of the first polymer 140 (M2> 1.5 ⁇ M1), preferably greater than or equal to 200% of the molar mass M1 of the first polymer 140 (M2> 2 * M1).
• M2> 1.5 ⁇ M1 the molar mass M1 of the first polymer 140
• M2> 2 * M1 the molar mass M2 of the second polymer 160
• a slight difference in thickness exists between the guiding patterns 210 and the neutralization layer 220.
• the greater thickness of the neutralization layer 220 can be explained by the larger molar mass M2 of the second polymer 160.
• this difference in thickness is not not detrimental to the subsequent assembly of the block copolymer because the thickness is constant within each polymer film.
• the neutralization layer 220 has a thickness of between 7 nm and 15 nm, while the thickness of the guide units 210 is between 3 nm and 7 nm
• a second polymer 160 of molecular weight M2 that is less than or equal to 500% of the molar mass M1 of the first polymer 140 is advantageously chosen.
• Molar mass M2 of the second polymer 160 is for example between 15 kg.mol 1 and 20 kg.mol -1 .
• the repetition step Ls corresponds to the distance between the edge of a guide pattern 210 and the same edge of the next guide pattern 210, for example the two edges on the left (or which separates the centers of two guide patterns 210 consecutive).
• the repetition step Ls is here equal to the period P of the cavities 1 1 1 (see Fig.2A).
• FIGS. 3A to 3G show steps S21 to S27 of the chemical guide structure forming method, according to a second embodiment of the invention.
• This second embodiment differs from the first embodiment only in the manner in which the first polymer guide patterns 210 are formed. Rather than locating the grafting of the first polymer 140 using a mask (see FIG. 2D), the first polymer can be grafted onto a large area of the substrate, and then structured using a mask comprising spacers. . Steps S21 to S24 relate to the formation of the spacers.
• mesa-shaped units 300 are formed on the substrate 100, by example by depositing a layer of sacrificial material and structuring of the layer by photolithography.
• the sacrificial material of the mandrels 300 is for example a carbonaceous material deposited by centrifugation ("Spin On Carbon", SOC).
• a layer 301 of the first polymer 140 is grafted onto the substrate 100 and the mandrels 300.
• the grafting of the first polymer 140 can be accomplished as described above in connection with the Figure 2D (deposition of a solution by centrifugation, graft annealing and rinsing).
• the layer 301 of the first polymer then covers the entire free surface of the substrate 100 and mandrels 300. It is preferably of constant thickness (2-15 nm).
• a layer 302 made of sacrificial material (eg S1O2, SiOxNy, Al2O3HfO2, etc.) is deposited conformably (eg PLD, PEALD) on the layer 301 of the first polymer 140.
• the thickness of the layer 302 of sacrificial material is constant and preferably between 10 nm and 20 nm.
• step S24 the layer 302 of sacrificial material is etched selectively with respect to the first polymer 140.
• This etching is anisotropic, in a direction perpendicular to the surface of the substrate 100, so removing the horizontal portions of the layer 302 of sacrificial material and keeping only its vertical portions, arranged against the flanks of the mandrels 300.
• a dry etching technique is employed in step S24, for example a plasma etching based fluorine (F2).
• the vertical portions of the layer 302 of sacrificial material constitute spacers 31 1.
• the spacers 31 1 are therefore projecting units grouped in pairs and arranged on either side of the mandrels 300 (only two pairs of spacers are shown in FIG. 3D).
• the section and the dimensions of the spacers 31 1, in a plane parallel to the substrate 100, correspond to those of the guide patterns 210 that are to be made.
• the set of spacers 31 1 is a mask of engraving 310.
• the first graftable polymer 140 is preferably insensitive to the plasma used, if necessary, to deposit the layer 302 of sacrificial material (PECVD, PEALD, etc.) and / or to etch the same layer 302 anisotropically.
• PECVD sacrificial material
• PEALD PEALD
• h-PS polystyrene
• h-PMMA polymethyl methacrylate
• the method then comprises a step S25 of etching the layer 301 of the first polymer through the mask 310, until reaching the substrate 100.
• the etching anisotropic, can be carried out by means of a plasma, for example based on oxygen (O2).
• O2 oxygen
• the mandrels 300 carbon material are advantageously eliminated during this same step S25.
• the substrate 100 is preferably insensitive to etching (or protected by a layer insensitive to etching).
• the width W (measured in the section plane of FIGS. 3A-3G) is the smallest dimension of the spacers 31 1, which is commonly called “critical dimension”. It sets the width of the guide patterns 210 of the chemical guiding structure 200 (see Fig.3E).
• the critical dimension W of the spacers 31 1 - and therefore of the guide patterns 210 - is preferably less than 20 nm.
• step S26 consists in removing the mask 310 made of sacrificial material selectively with respect to the substrate 100 and the first grafted polymer, so as to expose the guiding patterns 210.
• the withdrawal of the mask 310 can be performed by wet etching (for example HF in the case of spacers 31 1 in S1O2).
• the guiding patterns 210 may undergo, before removal of the spacers 31 1, an additional etching step, called “trim etch", in order to reduce their critical dimension. Thanks to the formation of spacers, and even more after the additional etch etching step, it is possible to reach critical dimensions well below the resolution limit of the photolithography.
• the width W of the spacers after the additional etching step can reach here a value between 5 nm and 20 nm, and preferably between 5 nm and 12.5 nm.
• step S27 of FIG. 3G a neutralization layer 220 made of second polymer 160 is deposited on the substrate 100 in the regions devoid of guide patterns 210.
• the neutralization layer 220 is formed of a second polymer 160 , grafted, of molar mass M2 greater than the molar mass M1 of the first polymer.
• step S27 of FIG. 3G proceeds as described in connection with FIGS. 2F-2G (steps S16-S17).
• FIGS. 4A to 4D show steps S31 to S34 of the chemical guide structure forming method, according to a third embodiment of the invention.
• the neutralization layer 220 is first formed by using a first polymer 140 of molar mass M1, then the second polymer 160 of molecular weight M2 (greater than M1) is grafted over the first polymer.
• the first polymer 140 thus has a neutral affinity (eg random copolymer) here, while the second polymer 160 has a preferential affinity for one of the blocks of the copolymer.
• the molar mass of a copolymer (random or block) varies according to its composition, and in particular according to the degree of monomer repetition (or degree of polymerization).
• the method starts with a step S31 for forming a mask 310 'on the substrate 100.
• the mask 310' of FIG. 4A is advantageously identical to the mask 310 of the figures 3D-3E and comprises patterns 31 1 spacer-shaped W-width.
• the first polymer 140 is grafted onto the substrate 100 through the mask 310 ', and advantageously over the entire surface of the substrate 100, to form the neutralization layer 220.
• the neutralization layer 220 comprises at least one neutralization unit 222, and preferably several distinct neutralization units 222. These neutralization patterns 222 may adopt different geometry in top view, for example a rectangular shape.
• Step S32 can be implemented as indicated above, by depositing a solution layer comprising the first polymer 140, annealing and rinsing.
• the layer of solution deposited on the substrate 100 has a thickness less than the height of the spacers 31 1, so that the latter are not completely covered with graft polymer to facilitate their removal.
• the mask 310 ' is removed, preferably by wet etching (eg HF) so as not to damage the neutralization layer 220. At least the upper face of the spacers 31 1 is exposed to the etching solution. In the neutralization layer 220, hollow patterns 221 are obtained whose number, dimensions and shape correspond to those of the spacers 31 1.
• the guiding units 210 are formed in the recessed patterns 221 by grafting the second polymer 160. As the molar mass M2 of the second polymer material 160 is greater than the molar mass M1 of the first polymer 140, the guide patterns 210 have in this embodiment of the method a greater thickness than the functionalization layer 220.
• Figs. 5A to 5D show steps S41 to S44 of the chemical guide structure forming method, according to a fourth embodiment of the invention.
• This fourth embodiment differs from the third mode of implementation in that a step or elevation 500 is created between the spacers 31 1 of each pair.
• This step 500 facilitates the self-assembly of the subsequently deposited block copolymer on the chemical guiding structure.
• the height of the step 500 is preferably between 10% and 50% of the natural period Lo of the block copolymer, for example between 3 nm and 15 nm for a natural period block copolymer Lo equal to 30 nm.
• FIG. 4A FIG. 5A shows the step S41 of forming the mask 310 'on the substrate 100a.
• the mask 310 'advantageously comprises several pairs of spacers 31 1 (only two pairs of spacers are however represented).
• the steps 500 can be created during this step S41 by etching a portion of the substrate 100 during the delineation of the mandrels 300, before the spacers 31 1 are formed against the flanks of the mandrels 300 (see step S21 of FIG. 3A). .
• Non-selective etch chemistry relative to the substrate 100 is then used to etch the sacrificial material layer.
• an HBr / 02 plasma can be used.
• the substrate 100 may be formed (at least on the surface) of hafnium dioxide (HfO 2) or alumina (Al 2 O 3) and the sacrificial material may be a resin.
• the following steps S42 to S44 of the method according to the fourth mode of implementation are identical to the steps S32 to S34 described in relation to FIGS. 4B-4D.
• step S42 see FIG. 5B
• the first polymer 140 is grafted onto the substrate 100 through the mask 310 'to form the neutralization layer 220.
• Some neutralization units 222 are raised thanks to the steps 500 formed in the substrate 100.
• S43 see FIG.
• the spacers 31 1 of the mask 310 ' are eliminated selectively with respect to the substrate 100 and to the neutralization layer 220 to form the recessed patterns 221 in their place. spacers 31 1.
• the guiding units 210 are formed in the recessed patterns 221 by grafting thereto the second polymer 160 (of molar mass M2 greater than the molar mass M1 of the first polymer 140).
• Another way to form the steps or elevations 500 is to deposit a layer of sacrificial material (eg TiN, FI FO2, Al2O3) (different from the material of the substrate) on the substrate 100 before forming the mandrels 300. This layer is then selectively etched relative to the substrate 100 during the delimitation of the mandrels 300. This implementation variant allows better control of the thickness of the steps 500.
• a layer of sacrificial material eg TiN, FI FO2, Al2O3
• FIGS. 6A to 6E show steps S51 to S55 of the chemical guide structure forming method, according to a fifth embodiment of the invention.
• the steps 500 are formed under the spacers 31 1 of the mask 310 ', so as to raise the guide patterns 210 relative to the neutralization layer 220.
• the mask 310 ' is formed on a substrate 100 comprising a support layer 100a and a surface layer 100b disposed on the support layer 100a.
• the surface layer 100b also called hard mask layer, is formed of a material capable of being etched selectively with respect to the material of the support layer 100a.
• the support layer 100a is TiN whereas the surface layer 100b is resin, or the support layer 100a is oxide whereas the surface layer 100b is TiN.
• the thickness of the surface layer 100b is preferably between 3 nm and 30 nm.
• the step S52 of FIG. 6B consists in etching, through the spacers of the mask 310 ', the surface layer 100b selectively with respect to the support layer 100a (thus serving as a stop layer for etching). This etching is preferably performed by plasma.
• the surface layer 100b is then limited to patterns spaced from each other and located under the spacers 31 1. These patterns constitute the steps 500.
• the shape and dimensions of the steps 500 correspond to those of the spacers 31 1.
• the first polymer 140 is grafted through the mask 310 ', on the support layer 100a and between the steps 500, to form the neutralization layer 220.
• the spacers 31 1 of the mask 310 ' are eliminated selectively with respect to the surface layer 100b, the neutralization layer 220 and the support layer 100a (preferably by wet etching , for example HF).
• the steps 500 are then exposed.
• the guiding units 210 are formed by grafting the second polymer 160 on the steps 500.
• the second polymer 160 has a molar mass M2 greater than the molar mass M1 of the first polymer 140 it is not grafted on the neutralization layer 220 (it does not replace or mix with the first polymer).
• this fifth embodiment differs from the fourth mode of implementation in that the steps 500 are delimited after the formation of the spacers 31 1 (and not before as in Figure 5A).
• the surface layer 100b is etched through the mask 310 'over only a part of its thickness (by controlling the etching time) during the step S52 and the layer of Neutralization 220 is deposited on the remaining portion of the surface layer 100b between steps 500 in step S53.
• the spacers 31 1 are removed by wet etching (eg HF).
• the chemical guiding structure 200 obtained at the end of the process according to the invention and represented in FIGS. 2G, 3G, 4D, 5D and 6E can be used in a directed block copolymer self-assembly process ("Directed Self-Assembly ", DSA), and more particularly in a chemo-epitaxy process, in order to generate patterns of very high resolution and density.
• DSA directed block copolymer self-assembly process
• chemo-epitaxy process in order to generate patterns of very high resolution and density.
• this chemo-epitaxy process comprises (besides the formation of the guiding structure 200) a step of depositing a block copolymer 800 on the chemical guiding structure 200 and a step of assembling the block copolymer 800, for example by thermal annealing.
• the block copolymer 800 can be a di-block copolymer (two monomers) or multi-block copolymer (more than two monomers), a polymer mixture, a copolymer mixture or the mixture of a copolymer and a homopolymer.
• the blocks of the copolymer are after assembly oriented perpendicularly to the substrate 1 00, thanks to the presence of the neutralization layer 220.
• the block copolymer 800 may be of any morphology, for example lamellar, cylindrical, spherical, or gyroid, depending on the proportion between the monomer blocks.
• the block copolymer 800 is of lamellar morphology (see FIG. 5), since the spacers 31 1 and the guide patterns 210 have a section (in a plane parallel to the substrate 100) in the form of a line.
• the block copolymer 800 may therefore be a standard block copolymer (Lo 3 25 nm) or a "high-X" block copolymer (Lo ⁇ 25 nm). It can in particular be chosen from the following:
• PS-b-PMMA polystyrene-block-polymethyl methacrylate
• At least one of the two blocks is chemically modified to reduce the natural period of the copolymer
• PS-b-PDMS polystyrene-block-polydimethylsiloxane
• PS-b-PLA polystyrene-block-polylactic acid
• PS-b-PEO polystyrene-block-polyethylene oxide
• PS-b-PMMA-b-PEO polystyrene-block-polymethylmethacrylate-block-polyethylene oxide
• PS-b-P2VP polystyrene-block-poly (2-vinylpyridine);
• PS-b-P4VP polystyrene-block-poly (4-vinylpyridine);
• PS-b-PFS poly (styrene) -block-poly (ferrocenyldimethylsilane);
• PS-b-PI-b-PFS poly (styrene) -block-poly (isoprene) -block-poly (ferrocenyldimethylsilane);
• PS-b-P polystyrene-block-poly (dimethylsiloxane-r-vinylmethylsiloxane);
• PS-b-PMAPOSS polystyrene-block-poly (methyl acrylate) POSS
• PDMSB-b-PS poly (1,1-dimethylsilacyclobutane) -block-polystyrene
• PDMSB-b-PMMA poly (1,1-dimethylsilacyclobutane) -block-poly (methyl)
• PMMA-b-PMAPOSS poly (methyl methacrylate) -block-poly (methyl)
• P2VP-b-PDMS poly (2-vinylpyridine) -block-poly (dimethyl siloxane);
• PTMSS-b-PLA poly (trimethylsilylstyrene) -block-poly (D, L-lactide);
• PTMSS-b-PDLA poly (trimethylsilylstyrene) -block-poly (D-lactic acid);
• PTMSS-b-PMOST poly (trimethylsilylstyrene) -block-poly (4-methoxystyrene);
• PLA-b-PDMS poly (D, L-lactide) -block-poly (dimethylsiloxane);
• PAcOSt-b-PSi2St poly (4-acetoxystyrene) -block-poly (4- (Bis (trimethylsilyl) methyl) styrene);
• PtBS-b-PMMA poly (4-tert-butylstyrene) -block-poly (methyl methacrylate);
• PCHE-b-PMMA polycyclohexane-block-poly (methyl methacrylate);
• steps 500 (FIG. 5A, 6B, 7B) on the surface of the substrate 100 promotes the alignment of the block copolymer 800.
• a physical alignment is obtained in addition to the chemical alignment (hybrid chemo-graphoepitaxy approach ).
• the steps 500 as well as the difference in thickness between the guide patterns 210 and the neutralization layer 220 have not been shown in FIG. 8.
• the training method according to the invention is not limited to the embodiments described with reference to FIGS. 2 to 7 and many variations and modifications will be apparent to those skilled in the art.
• the first polymer 140 and the second polymer 160 could have other compositions than those described above.
• other block copolymers could be used.
• the chemical guiding structures achievable by the forming method according to the invention are not limited to the juxtaposition of homopolymer guide patterns and a neutralization layer.
• Other types of units, having different chemical affinities than those described above, can be used.
• the chemical guiding structure 200 may be composed of a first unit (or set of units) having a preferential affinity for a block of the copolymer and a second unit (or set of units) having a preferred affinity for a unit. other block of the copolymer.
• the first and second polymers could then both be homopolymers.
• the block copolymer is deposited on the substrate 100 covered only with the units (210 or 222) of the first polymer 140, at the stage of FIG. 2E, 3F, 4C, 5C or 6D.
• the substrate 100 then has a chemical affinity conducive to the assembly of the block copolymer (neutral in the case of Figures 2E and 3F, preferred in the case of Figures 4C, 5C and 6D).
• the process for forming the chemical guiding structure then does not include a step of grafting the second polymer 160 (FIGS. 2F-2G, 3G, 4D, 5D, 6E).

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