Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09G—POLISHING COMPOSITIONS; SKI WAXES
  • C09G1/00—Polishing compositions
  • C09G1/02—Polishing compositions containing abrasives or grinding agents
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B24—GRINDING; POLISHING
  • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
  • B24B37/00—Lapping machines or devices; Accessories
  • B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
  • B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
  • B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K3/00—Materials not provided for elsewhere
  • C09K3/14—Anti-slip materials; Abrasives
  • C09K3/1409—Abrasive particles per se
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K3/00—Materials not provided for elsewhere
  • C09K3/14—Anti-slip materials; Abrasives
  • C09K3/1454—Abrasive powders, suspensions and pastes for polishing
• • 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
  • C23F3/00—Brightening metals by chemical means
  • C23F3/02—Light metals
  • C23F3/03—Light metals with acidic solutions
• • 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
  • H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
  • H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
  • H01L21/321—After treatment
  • H01L21/32115—Planarisation
  • H01L21/3212—Planarisation by chemical mechanical polishing [CMP]

Definitions

• Polishing liquid for polishing aluminum film and method for polishing aluminum film using the same
• the present invention relates to a polishing liquid for polishing an aluminum film and a method for polishing an aluminum film using the same, and is particularly used for forming damascene wiring in a semiconductor integrated circuit (hereinafter referred to as LSI).
• the present invention relates to an aluminum film polishing polishing liquid and an aluminum film polishing method using the same.
• CMP Chemical mechanical polishing
• Damascene wiring technology can simplify the wiring process, improve yield and reliability, and is expected to be applied in the future.
• copper which is a low resistance, is mainly used for high-speed logic devices as a wiring metal for damascene wiring, and it is low-cost for memory devices represented by DRAM.
• Aluminum or tandasten is used.
• a general method of metal CMP for polishing a metal film is to apply a polishing pad on a circular polishing platen (platen), immerse the surface of the polishing pad with a polishing solution, and form a metal film on the substrate. , And rotate the polishing platen with a predetermined pressure (hereinafter referred to as polishing pressure) applied from the back side, and the convex metal film is formed by mechanical friction between the polishing liquid and the convex part of the metal film. To be removed.
• polishing pressure a predetermined pressure
• the polishing liquid used in CMP is generally composed of an oxidizing agent and abrasive grains, and can be used as necessary. Further, a metal oxide solubilizer is added. It is thought that the basic mechanism of CMP by this CMP polishing liquid is that the surface of the metal film is first oxidized with an oxidizing agent and the oxidized layer is scraped off with abrasive grains.
• CMP requires high-speed polishing of a metal film, flatness of the polished surface, and low defect density on the polished surface.
• the aluminum film is softer than other metal films for damascene wiring such as a copper film and a tungsten film, it can be polished at a high speed, but is not like an alumina particle.
• CMP is performed using a polishing solution containing relatively hard polishing abrasive grains, among the defects on the polishing surface, the surface roughness increases, the smoothness is impaired, and the wiring yield is significantly reduced. is there.
• the present invention provides an aluminum film polishing polishing liquid capable of smoothly and rapidly polishing the surface of an aluminum film used in LSI and the like, and an aluminum film polishing method using the same. .
• the present invention is (1) for polishing an aluminum film having a pH of 2 to 4, comprising a polycarboxylic acid having a first-stage acid dissociation index of 3 or less at 25 ° C, colloidal silica, and water. Concerning polishing liquid.
• the present invention relates to (2) the polishing slurry for polishing an aluminum film according to (1), wherein the polyvalent carboxylic acid is at least one selected from oxalic acid, malonic acid, and tartaric acid.
• the present invention also relates to (3) the polishing slurry for polishing an aluminum film according to (1), wherein the secondary particle of the colloidal silica has an average particle size of 5 to 100 nm.
• the present invention relates to (4) the polishing liquid for polishing an aluminum film according to any one of (1) to (3), further comprising an oxidizing agent.
• the present invention provides: (5) The oxidant according to (4), wherein the oxidizing agent is at least one selected from hydrogen peroxide, nitric acid, potassium periodate, hypochlorous acid, and ozone water.
• the present invention relates to a polishing liquid for polishing an aluminum film.
• the present invention provides (6) the aluminum film according to any one of (1) to (5), wherein the substrate on which the aluminum film is formed is pressed against a polishing cloth of a polishing platen and pressed.
• the present invention relates to an aluminum film polishing method, wherein an aluminum film is polished by moving a substrate and a polishing surface plate while supplying a polishing liquid for polishing between the film and a polishing cloth.
• the polishing slurry for aluminum film polishing of the present invention By using the polishing slurry for aluminum film polishing of the present invention, the surface of the aluminum film can be polished smoothly and at high speed. Therefore, LS using aluminum film
• I can contribute to quality improvement such as I.
• the polishing solution for polishing an aluminum film of the present invention contains a polycarboxylic acid having a first-stage acid dissociation index of 3 or less at 25 ° C, colloidal silica, and water, and has a pH of 2 to 4. It is characterized by this.
• the polyvalent carboxylic acid used in the present invention is a carboxylic acid having two or more carboxyl groups in one molecule, preferably a dicarboxylic acid.
• the polycarboxylic acid has a first-stage acid dissociation index (pKal) at 25 ° C. of 3 or less, preferably 2.95 or less, more preferably 2.90 or less.
• the polycarboxylic acid having a first-stage acid dissociation index (pKal) exceeding 3 at 25 ° C. cannot achieve the object of the present invention because the polishing rate becomes slow.
• strong polycarboxylic acids include oxalic acid, malonic acid, tartaric acid, maleic acid, citrate, and ammonium salts thereof, which may be hydrates.
• oxalic acid, malonic acid, and tartaric acid are preferable in that a practical polishing rate can be obtained, and oxalic acid is particularly preferable.
• These polycarboxylic acids can be used alone or in combination of two or more.
• the acid dissociation index (pKa) is a logarithm of the reciprocal of the acid dissociation constant. For example, “Basic Manual for Chemistry” revised 4th edition (issued on September 30, 1993), Maruzen Co., Ltd., 11 Detailed description on pages 317-321.
• the blending amount of the polyvalent carboxylic acid in the polishing slurry for aluminum film polishing of the present invention is preferably 0.0001 to 0.05 mol with respect to 100 g of the total weight of the polishing night, 0.001 to 0. More preferred to be Olmol. If this amount exceeds 0.05 mol, the smoothness of the aluminum film after polishing tends to deteriorate, and if it is less than 0. OOOlmol, there is a tendency that a sufficient aluminum film polishing rate cannot be obtained.
• a polyvalent carboxylic acid having a first-stage acid dissociation index of 3 or less at 25 ° C. has an effect of improving the polishing rate for an aluminum film. Found it expensive.
• the oxidizing agent used in the present invention is hydrogen peroxide; peracetic acid, perbenzoic acid, tert-butylhydride oral peroxide, potassium permanganate, potassium dichromate, potassium iodate, potassium periodate, Nitric acid, iron nitrate, perchloric acid, hypochlorous acid, ferricyanium potassium, ammonium persulfate, ozone water, etc., among them hydrogen peroxide, nitric acid, potassium periodate, hypochlorous acid and ozone Water is preferred and hydrogen peroxide is particularly preferred.
• These oxidizing agents can be used alone or in combination of two or more.
• the substrate is a silicon substrate including an integrated circuit element
• contamination with alkali metal, alkaline earth metal, halide, or the like is not desirable. Therefore, an oxidizing agent that does not contain a nonvolatile component is desirable.
• an oxidant that includes a nonvolatile component may be used.
• the amount of the oxidizing agent in the polishing liquid for polishing aluminum film is preferably in the range of 0.3: to 50% by weight with respect to the total weight of the polishing liquid, and is in the range of 0.3 to 40% by weight. It is more preferable. If the blending amount is less than 0.1% by weight, a sufficient polishing rate tends not to be obtained for the aluminum film, and even if it exceeds 50% by weight, the polishing rate is not improved.
• colloidal silica is used as the abrasive. Since colloidal silica is excellent in smoothing the surface of an aluminum film, a polishing liquid containing it can achieve the object of the present invention.
• the average particle size of the powerful colloidal silica secondary particles is preferably in the range of 5-100 nm, more preferably in the range of 10-90 nm.
• the average particle size of the secondary particles is less than 5 nm, there is a tendency that a sufficient polishing rate cannot be obtained for the aluminum film.
• the average particle size of the secondary particles exceeds lOOnm, the surface of the polished aluminum film is not cleaned. On the other hand, there is a tendency that sufficient smoothness cannot be obtained.
• the average particle size of the secondary particles is determined by centrifuging the polishing solution for 10 minutes under the condition of a rotation speed of 80 OOmin- 1 , and measuring the supernatant with a zeta potential 'particle size measuring device Zeta Sizer 3000HS manufactured by Malvern. be able to.
• Colloidal silica includes, for example, a fumed method in which silicon chloride and the like react with oxygen and hydrogen in the gas phase, a sol-gel method in which alkoxysilane force such as tetraethoxysilane is hydrolyzed and synthesized, and impurities by purification. It is possible to use colloidal silica synthesized by an inorganic colloid method or the like from which the metal has been removed. In particular, it is preferable to use colloidal silica synthesized by a sol-gel method that is synthesized by hydrolytic condensation of alkoxysilane such as tetraethoxysilane. The colloidal silica is preferably highly pure in order to avoid contamination of the aluminum surface.
• colloidal silica having a sodium content of preferably 10 ppm or less, more preferably 8 ppm or less, and particularly preferably 5 ppm or less is preferred. If the sodium content exceeds lOppm, contamination of the aluminum surface with sodium may occur when used as a CMP slurry.
• the compounding amount of colloidal silica in the polishing slurry for aluminum film polishing is preferably 0.01 to 10% by weight with respect to the total weight of the polishing solution, and is in the range of 0.05 to 5% by weight. That power is preferred. If the blending amount is less than 0.01% by weight, there is a tendency that no significant difference is observed from the polishing rate when a polishing liquid not containing colloidal silica is used. There is a tendency not to be seen.
• the polishing liquid of the present invention is a slurry in which colloidal silica is dispersed in water.
• the amount of water added is the balance with respect to the total amount of various components (polyvalent carboxylic acid, oxidizing agent, colloidal silica, and other optional additives).
• the pH of the polishing solution for polishing an aluminum film of the present invention is 2 to 4, preferably 2.:! To 3.8. Preferably it is in the range of 2.2 to 3.7. If the pH is less than 2, damage is caused to the piping system of the polishing apparatus, resulting in inferior operability. If the pH exceeds 4, the smoothness of the polished aluminum film surface decreases or the storage stability of the polishing liquid is reduced. Sexuality may be impaired.
• a method of adjusting the pH of the polishing liquid to the above range a method of adjusting by the addition amount of the polyvalent carboxylic acid, ethylenediamine, ethanolamine, ammonia, sodium hydroxide, potassium hydroxide, tetramethylammonium. Examples thereof include a method of adjusting by adding an alkali component such as muhydroxide, and the method is usually performed by a method of adjusting by adding an inorganic base such as ammonia.
• the polishing liquid of the present invention includes coloring agents such as dyes and pigments, solvents that can be mixed with water, water-soluble polymers, and other additives that are generally added to abrasives. Further, it may be added as long as the working effect of the polishing liquid is not impaired.
• the substrate on which the aluminum film is formed is pressed against a polishing cloth on a polishing platen and pressed, and the polishing liquid for polishing an aluminum film of the present invention is applied between the aluminum film and the polishing cloth.
• the aluminum film is polished by powering the substrate and the polishing surface plate while supplying them in between.
• the substrate on which the aluminum film to be polished is formed is a substrate related to semiconductor device manufacturing, for example, a semiconductor substrate at a stage where a circuit element and a wiring pattern are formed, and a stage where a circuit element is formed. And the like.
• a polishing apparatus that can be used, a holder for holding a substrate and a surface plate with a polishing cloth (pad) attached (a motor whose rotational speed can be changed, etc. are attached). It is not limited in particular.
• a polishing apparatus manufactured by Nano Factor Co., Ltd .: FACT-200 can be used.
• polishing cloth examples include a general nonwoven fabric, foamed polyurethane, porous fluororesin, and the like, and there is no particular limitation.
• the polishing cloth is subjected to a groove treatment so that a polishing liquid for polishing an aluminum film is accumulated. Is preferred.
• the rotation speed of the platen is preferably a low rotation of 2 OOmin- 1 or less so that the substrate does not pop out.
• the pressure applied to the substrate is aluminum after the polishing. It is preferable to set the pressure to 1 kg / cm 2 (98 kPa) or less so as not to damage the film surface.
• the method for supplying the polishing liquid for polishing an aluminum film of the present invention to a polishing apparatus is not particularly limited as long as the polishing liquid can be continuously supplied to the polishing cloth with a pump or the like during polishing.
• the supply amount of the polishing liquid is not particularly limited, but it is preferable that the surface of the polishing cloth is always covered with the polishing liquid. Specifically, it is preferable to supply 0.001 to: milliliter per lcm 2 of the polishing pad area.
• the holder may be rotated or rocked for polishing.
• a polishing method for rotating the polishing platen on a planetary surface a polishing method for moving a belt-like polishing cloth linearly in one direction in the longitudinal direction, and the like can be mentioned.
• the holder can be fixed, rotated, or rocked.
• the substrate after polishing is thoroughly washed in running water, and then water droplets adhering to the substrate are removed using a spin dryer or the like and then dried.
• polishing with the polishing solution for polishing an aluminum film of the present invention enables polishing at a polishing rate of 25 nm / min or more and an average surface roughness (Ra) of 1 nm or less.
• the index of smoothness in the present invention is the average surface roughness (Ra) of the surface of the aluminum film after completion of polishing, and the surface of the aluminum film is scanned with a scanning probe microscope (Seiko I / f Nsturmend Co., Ltd. ) Was measured by using a 5 micron mouth.
• the polishing rate was calculated from the polishing time obtained by converting the film thickness difference of the aluminum film on the substrate before and after polishing into the sheet resistance value.
• the polishing solution for polishing an aluminum film of the present invention is particularly suitable for polishing an aluminum film for LSI, but can also be used for polishing an aluminum film for other uses.
• Example 1 Oxidic acid dihydrate 0.47% by weight (0.00033 monole with respect to 100g of the total amount of polishing liquid) was dissolved in water, and then the secondary particles had an average particle size of 50nm, 20% by weight colloidal silica, 5% by weight. % are dispersed (1 wt% as solid content), 30% after a 10 wt% aqueous hydrogen peroxide concentration was pressurized example, it was adjusted to 2.5 with P H by concentration of 25 wt% aqueous ammonia for the aluminum film polishing A polishing liquid (A) was prepared.
• Colloidal silica was prepared by hydrolysis of tetraethoxysilane in an ammonia solution according to a conventional method.
• Polishing equipment FACT—200, manufactured by Nano Factor Co., Ltd.
• Polishing pad Foam polyurethane resin with closed cells
• Polishing pressure 30kPa (300gf / cm 2 )
• Polishing fluid flow rate l lcc / min
• Polishing rate for aluminum film by CMP The difference in film thickness before and after polishing the substrate was calculated from the change in sheet resistance value and calculated from the polishing time.
• Average surface roughness The average surface roughness of the aluminum film after polishing was measured using a scanning probe microscope (SPI3800N / SPA500, manufactured by Seiko Instruments Inc.), with a measurement area of 5 microns. Obtained by measuring.
• a polishing liquid (B) for polishing an aluminum film was prepared in the same manner as in Example 1 except that no hydrogen peroxide solution was added.
• the aluminum film polishing slurry (B) obtained above was used for polishing in the same manner as in Example 1 for evaluation.
• the polishing rate for the aluminum film was 6
• the average surface roughness (Ra) was 3 nm / min and 0.4 nm. Polishing was possible at high speed and good smoothness was exhibited.
• a polishing liquid (C) for polishing an aluminum film was produced in the same manner as in Example 1 except that 3% by weight of 30% hydrogen peroxide was used.
• polishing was performed in the same manner as in Example 1, and evaluation was performed. As a result of the evaluation, the polishing rate for the aluminum film was 6
• the average surface roughness (Ra) was 3 nm / min and 0.4 nm. Polishing was possible at high speed and good smoothness was exhibited.
• a polishing liquid (D) was prepared.
• polishing was performed in the same manner as in Example 1 using the aluminum film polishing slurry (D) obtained above, and evaluation was performed.
• the polishing rate for the aluminum film was 32 nm / min
• the average surface roughness (Ra) was 0.6 nm, and it was possible to polish at high speed and showed good smoothness.
• Aluminum film polishing was carried out in the same manner as in Example 1 except that 0.39 wt% malonic acid (0.0035 mol per 100 g of the total amount of polishing liquid) was used instead of 0.47 wt% of oxalic acid dihydrate.
• a polishing slurry (E) was prepared.
• polishing was performed in the same manner as in Example 1 using the aluminum film polishing slurry (E) obtained above, and evaluation was performed.
• the polishing rate for the aluminum film was 4 lnm / min, average surface roughness (Ra) was 0.6 nm, high-speed polishing was possible, and good smoothness was exhibited.
• polishing was performed in the same manner as in Example 1 for evaluation.
• the polishing rate for the aluminum film was 67 nm / min
• the average surface roughness (Ra) was 0.8 nm, and it was possible to polish at high speed and showed good smoothness.
• a polishing liquid (G) for polishing an aluminum film was prepared in the same manner as in Example 6 except that no hydrogen peroxide solution was added.
• polishing was performed in the same manner as in Example 1 for evaluation.
• the polishing rate for the aluminum film was 70 nm / min
• the average surface roughness (Ra) was 0.8 nm, and it was possible to polish at high speed and showed good smoothness.
• Example 2 Using the same components as in Example 1, the amount of ammonia water was controlled to adjust the pH to 3.0 to prepare an aluminum film polishing polishing solution (H).
• the aluminum film polishing slurry (H) obtained above was used for polishing in the same manner as in Example 1 and evaluated.
• the polishing rate for the aluminum film was 6
• the average surface roughness (Ra) was 4 nm / min and 0.8 nm, and it was possible to polish at high speed and showed good smoothness.
• An aluminum film was prepared in the same manner as in Example 1 except that 0.5% by weight of malic acid (0.003 mol per 100 g of the total amount of polishing liquid) was used instead of 0.4% by weight of oxalic acid dihydrate. Polishing A polishing liquid (I) was prepared.
• polishing was performed in the same manner as in Example 1 using the aluminum film polishing slurry (I) obtained above, and evaluation was performed.
• the polishing rate for aluminum film is 1
• the average surface roughness (Ra) was 5 nm / min and the average surface roughness (Ra) was 0.6 nm.
• the smoothness was good, but the polishing rate was greatly reduced as compared with Examples 1-8.
• Example 2 Using the same components as in Example 1, the amount of aqueous ammonia was controlled to adjust the pH to 5.0 to prepare an aluminum film polishing polishing solution ⁇ ).
• polishing was performed in the same manner as in Example 1 using the aluminum film polishing slurry obtained above, and evaluation was performed. As a result of the evaluation, the polishing rate for the aluminum film was 6
• the aluminum film polishing slurry (K) obtained above was used for polishing in the same manner as in Example 1 for evaluation.
• the polishing rate for the aluminum film was 89 nm / min
• the average surface roughness Ra was 1.6 nm
• the smoothness of the force film surface that could be polished at high speed was higher than that of Examples 1-8. It got worse.
• An aluminum film was prepared in the same manner as in Example 1 except that 0.52% by weight of bromoacetic acid (0.003mol per 100 g of polishing liquid) was used instead of 0.4% by weight of oxalic acid dihydrate.
• a polishing liquid (L) for polishing was prepared.
• the aluminum film polishing slurry (L) obtained above was used for polishing in the same manner as in Example 1 and evaluated.
• the polishing rate for aluminum film is 1
• the average surface roughness (Ra) was 8 nm / min and the average surface roughness (Ra) was 0.8 nm.
• the smoothness was good, but the polishing rate was greatly reduced as compared with Example 18.
• Tables 1 and 2 show the composition of the polishing liquid and the polishing evaluation for Examples 18 and Comparative Example 14 described above, respectively.
• the concentrations of abrasive grains, organic acids, and oxidizers (% by weight) indicate the concentration of each component relative to the total weight of the polishing liquid.

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