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US20070029519A1 - Surface treating solution for fine processing of glass base plate having a plurality of components - Google Patents

Surface treating solution for fine processing of glass base plate having a plurality of components Download PDF

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Publication number
US20070029519A1
US20070029519A1 US10/487,770 US48777002A US2007029519A1 US 20070029519 A1 US20070029519 A1 US 20070029519A1 US 48777002 A US48777002 A US 48777002A US 2007029519 A1 US2007029519 A1 US 2007029519A1
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solution
acid
glass substrate
etching
concentration
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US10/487,770
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English (en)
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Hirohisa Kikuyama
Tatsuhiro Yabune
Masayuki Miyashita
Tadahiro Ohmi
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Priority to US12/237,981 priority Critical patent/US8066898B2/en
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    • 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
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
    • C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching

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  • the present invention relates to a surface treatment solution for finely processing the surface of a glass substrate containing multiple ingredients. More specifically, the present invention relates to a surface treatment solution, useful for the fine surface processing of glass substrates, containing cation-yielding elements and their cation-yielding oxides, which is very profitably used for wet-etching/cleaning the surface of such glass substrates or etching/cleaning the surface of such glass substrates carrying finely fabricated semiconductor elements thereon during the fabrication of semiconductor devices.
  • Glass substrates to be used for the construction of liquid crystal (LC)-based or organic electroluminescence (EL)-based flat panel display devices have come to have an increasingly reduced thickness to meet the demand for more compact and power-saving display devices.
  • the so-called mother glass plate has an increasingly larger size to improve the production efficiency and reduce the production cost.
  • a glass substrate is obtained by thinning a mother glass plate.
  • the mechanical thinning of a mother glass plate has a limitation, because a mother glass plate must have strength sufficiently high enough to withstand stresses imposed during the thinning process. Therefore, if further thinning is required for a mechanically thinned glass plate (coarse glass substrate), the coarse glass substrate must be subjected to another kind of fine processing, e.g., chemical fine processing.
  • the problem 2) was ascribed to that crystals developed on the surface of a glass substrate and adhered thereto interfere with etching and/or that cation-yielding elements and their oxides contained in a glass substrate are differently susceptible to etching, which causes the local variation in etching rate and etching amount.
  • the present inventors succeeded in obtaining this knowledge for the first time.
  • the most important point of the technique for finely processing glass substrates is to uniformly process or treat glass substrates while preventing the occurrence of surface roughness.
  • the present invention provides a surface treatment solution for uniformly processing the surface of glass substrates containing multiple ingredients such as glass substrates to be used for the construction of LC-based or organic EL-based flat panel display devices, with which it is possible to etch such glass substrates without invoking crystal precipitation and surface roughness.
  • the present inventors had studied hard to solve the above problems, and found that it is possible to solve the above problems by providing a surface treatment solution which is specifically adapted for the fine processing of glass substrates containing multiple ingredients, the treatment solution containing, in addition to HF and NH 4 F, at least one acid whose dissociation constant is larger than that of HF. This finding led the inventors to the present invention.
  • a first aspect of the present invention is to provide a surface treatment solution for finely processing a glass substrate containing multiple ingredients which contains as a uniform mixture, in addition to HF and NH 4 F, at least one acid whose dissociation constant is larger than that of HF.
  • a fourth aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients, which contains as a uniform mixture, in addition to HF and NH 4 F, at least one inorganic acid either monovalent or multivalent, whose dissociation constant is larger than that of HF.
  • a fifth aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients wherein the acid whose dissociation constant is larger than that of HF is one or more chosen from the group comprising HCl, HBr, HNO 3 , and H 2 SO 4 .
  • a sixth aspect of the present invention is provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients which further contains a surfactant at 0.0001 to 1 wt %.
  • a seventh aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients, particularly a glass substrate containing, in addition to silicates or its main ingredient, one or more elements chosen from the group comprising Al, Ba, Ca, Mg, Sb, Sr and Zr.
  • An eighth aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients, particularly a glass substrate used for the construction of a flat panel display device.
  • a ninth aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients, which contains HF at 25 mol/kg or lower.
  • a tenth aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients, which contains NH 4 F at 0.001 to 11 mol/kg.
  • An eleventh aspect of the present invention is to provide a surface treatment solution as described in any one of the foregoing aspects of the invention for finely processing a glass substrate containing multiple ingredients wherein, if etching is performed at an appropriate temperature using an acid-added etching solution with the concentration x of acid being varied, and it is found that crystal precipitation remains inhibited as long as x is below X 3 or the maximum effective concentration, the concentration x of acid in the solution is adjusted to be x ⁇ x 3 [mol/kg].
  • FIG. 1 shows a graph relating the etching rate f(x) with the concentration of x of the acid in the solution, when etching solutions containing an acid whose dissociation constant is larger than that of HF at different concentrations are applied to a heated silicon oxide film the change of etching rate being traced;
  • FIG. 2 shows a graph illustrating when acid-added etching solutions with the concentration of acid in the solution being varied are applied to a glass substrate containing Al compounds, with dots relating the concentration of Al ions in the solution with the etched amount;
  • FIG. 3 shows a plot illustrating when acid-added etching solutions with the concentration of acid in the solution being varied are applied to a glass substrate containing Ba compounds, with dots relating the concentration of Ba ions in the solution with the etched amount;
  • FIG. 4 shows a graph illustrating when acid-added etching solutions with the concentration of acid in the solution being varied are applied to a glass substrate containing Ca compounds, with dots relating the concentration of Ca ions in the solution with the etched amount;
  • FIG. 5 shows a plot illustrating when acid-added etching solutions with the concentration of acid in the solution being varied are applied to a glass substrate containing Sr compounds, with dots relating the concentration of Sr ions in the solution with the etched amount.
  • the present invention will be detailed below. First, the present inventors inquired about the causes responsible for the formation of crystals and surface roughness.
  • metal elements contained in a glass substrate dissolve in an etching solution to turn into cations there.
  • Those cations derived from the etched glass substrate react with anions derived from anion-yielding species in the etching solution.
  • the cations react with fluorine ions (F ⁇ ions) to produce metal salts (e.g., fluoride salts).
  • F ⁇ ions fluorine ions
  • metal salts e.g., fluoride salts
  • etching proceeds at widely different speeds according to localities because of the ingredients having greatly different susceptibilities to etching, which may cause the etched surface to be roughened and irregular in profile.
  • An effective measure for inhibiting the development of fluorides which are hardly soluble to an etching solution is to modify the reaction system in such a manner as to lower the concentration of F ⁇ ion in the etching solution.
  • the etching solution in order to etch a glass substrate having such a composition, the etching solution must include substances such as HF or BHF that can dissolve silicon oxide.
  • HF 2 ⁇ ions act as dominant ions in the etching of silicon oxide.
  • an etching solution according to the invention must include, in addition to HF and NH 4 F, at least one acid (high-ionizing acid) which has a larger dissociation constant than HF.
  • the etching solution of the invention for glass substrates containing multiple ingredients preferably contains an acid (high-ionizing acid) whose dissociation constant is larger than that of HF at a concentration of x [mol/kg].
  • the x should be x ⁇ x 3 where x 3 represents the maximum concentration at which deposition of crystals on a glass substrate can be prohibited at a temperature appropriate for etching. At such a concentration, the composition of the etching solution becomes uniform, and roughening of the etched glass surface is inhibited.
  • crystal precipitates developed in the etching solution may adhere to the surface of a glass substrate to cause the etched glass surface to be roughened, or crystal precipitates may be brought into contact with a surface of the container to be broken into fine particles which may adhere to the surface of a glass substrate to cause it to be roughened.
  • the performance of an etching solution may be evaluated by applying the solution to a heated silicon oxide film having a certain thickness, measuring the thinning of the film over time, and determining the etching rate (thinning per unit time).
  • the performance of an etching solution containing a high-ionizing acid may be evaluated by plotting the etching rate f(x) [A/min] as a function of the concentration (x) of the acid.
  • etching solution comprising HF or BHF
  • HF and NH 4 F dissociate into respective positive and negative ions, and thus F ⁇ ions are produced.
  • F ⁇ ions react with H + ions in the solution to produce HF, a bound compound including HF 2 ⁇ , or an ion. If an acid (high-ionizing acid) whose dissociation constant is larger than that of HF is added to the etching solution, H + ions (newly added) react with F ⁇ ions in the solution to produce HF or a bound compound with HF 2 ⁇ ions.
  • the reaction system may undergo following reactions to maintain the acid-base equilibrium: HF 2 ⁇ ions are decomposed into HF and F ⁇ ions, and the F ⁇ ions react with newly added H + ions to produce HF.
  • the concentration of HF 2 ⁇ ions is reduced, which leads to the reduction of the etching rate.
  • a high-ionizing acid as described above is added to an HF-based etching solution at a concentration higher than x 1 or the concentration that gives a maximum of f(x) or f(x 1 ), thereby controlling the concentration of F ⁇ ions in the solution, it is possible to inhibit the formation of the fluorides of cation-yielding elements contained in a glass substrate, i.e., fluorides hardly soluble to the solution.
  • the amount of a high-ionizing acid added to an etching solution is preferably adjusted such that the concentration x of the acid in the solution is in the following range: x 2 ⁇ ( x 2 ⁇ x 1 )/2 ⁇ x ⁇ x 2 +( x 2 ⁇ x 1 )/2. This is because then it is possible to prevent the adhesion of crystal precipitates to the etched surface, to minimize any increase in surface roughness, and to maintain the original transparency of the glass substrate throughout the etching process.
  • the concentration in question is more preferably in the following range: x 2 ⁇ ( x 2 ⁇ x 1 )/3 ⁇ x ⁇ x 2 +( x 2 ⁇ x 1 )/3, and most preferably in the following range: x 2 ⁇ ( x 2 ⁇ x 1 )/4 ⁇ x ⁇ x 2 +( x 2 ⁇ x 1 )/4.
  • the concentration x of a high-ionizing acid is preferably adjusted to be in the range: x 2 ⁇ ( x 2 ⁇ x 1 )/2 ⁇ x ⁇ x 3 .
  • the concentration x of a high-ionizing acid is preferably adjusted to be in the range: x 1 ⁇ ( x 3 ⁇ x 1 )/2 ⁇ x ⁇ x 3 .
  • the species of acid is not limited to any specific one, but may include inorganic acids such as hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, and the like, and organic acids such as oxalic acid, tartaric acid, iodoacetic acid, fumaric acid, maleic acid, and the like.
  • the acid is a hydrophilic acid, because it facilitates, when added to an etching solution, the uniform dispersal of the solutes of the solution.
  • the acid is an inorganic acid because it, when added to an etching solution, can prevent the etched surface from being contaminated by organic materials.
  • inorganic acids hydrochloric acid, nitric acid, sulfuric acid and hydrobromic acid are most preferred because they have a higher dissociation constant.
  • the acid may include multivalent acids as well as monovalent acids.
  • the use of a multivalent acid may be advantageous because it gives a larger amount of H + ions at a given concentration.
  • hydrochloric acid is particularly preferred because it has a most balanced action.
  • the preferable species of acid should be determined in accordance with the cation-yielding elements and their oxides contained in a glass substrate to be treated, together with the concentrations of those elements and oxides.
  • the acid may comprise one kind of acid or multiple kinds of acids.
  • the etching solution further contains a surfactant to enhance the uniform etching, improve the affinity of the etched surface to a resist, and inhibit the adhesion of foreign particles to the etched surface.
  • the added amount of a surfactant is preferably 0.0001 to 1 wt %.
  • etching rate f(x) is obtained for a given high-ionizing acid in combination with an etching solution through a preliminary experiment performed on a heated silicon oxide film, it is possible to readily determine the concentrations of the acid in the solution at which f(x) takes a maximum and minimum.
  • the concentration x of the acid in an etching solution is preferably chosen to be in the range of x>x 1 , more preferably x>x 2 ⁇ (x 2 ⁇ x 1 )/2, because then the compounds derived from cations obtained as a result of dissolution of ingredients contained in an etched glass substrate become highly soluble to the solution.
  • the concentration x of the acid in an etching solution is preferably chosen to be in the range: x 2 ⁇ ( x 2 ⁇ x 1 )/2 ⁇ x ⁇ x 2 +( x 2 ⁇ x 1 )/2, because then it is possible to prevent the adhesion of crystal precipitates to the etched surface, and to minimize any increase in surface roughness, and to maintain the original transparency of the glass substrate throughout the etching process.
  • the etching solution according to the invention adapted for etching a glass substrate containing multiple ingredients, contains as indispensable components, HF and NH 4 F, and a high-ionizing acid whose dissociation constant is higher than that of HF, and, as needed, a surfactant.
  • Other components may be added to the etching solution, as long as their addition does not interfere with the proper function of the etching solution.
  • the species of the metal elements are not limited to any specific ones but may include any various metals.
  • their concentration is preferably limited to 1 ppb or lower, more preferably 0.5 ppb or lower, most preferably 0.01 ppb or lower.
  • a glass substrate containing multiple ingredients may contain any metals, as long as its main ingredient is silicates.
  • the etching solution of the invention is particularly effective for a glass substrate which contains, as metal elements, one or more chosen from the group comprising Al, Ba, Ca, Mg, Sb, Sr and Zr.
  • the glass substrate to be treated by an etching solution of the invention preferably includes those used for the construction of flat panel display devices.
  • the concentration of HF in an etching solution of the invention is preferably 25 mol/kg or lower.
  • the concentration of NH 4 F in an etching solution of the invention is preferably 0.001 to 11 mol/kg.
  • the concentration x of the acid in an etching solution is preferably chosen to satisfy x ⁇ x 3 [mol/kg], where X 3 represents the maximum concentration at which deposition of crystals on a glass substrate can be prohibited at a temperature appropriate for etching.
  • the concentration of components included in an etching solution of the invention are preferably adjusted such that precipitation of crystals occurs at 20° C. or lower, because then it is possible to prohibit the precipitation of crystals during the preparation of the etching solution.
  • the glass substrate used in the experiment included glass substrates to be incorporated in LC displays.
  • the test glass substrates were submitted to EDX (energy dispersion type X-ray analysis) to determine their ingredients. The results are shown in Table 2.
  • Table 2 Contents of individual Elements Atomic weight elements (wt %) Si 28.09 30.43 O 16.00 46.65 Al 26.98 8.74 Ba 137.3 9.42
  • Ca 40.08 2.25 Ga 69.72 0.26 Mg 24.31 0.25 Sb 121.8 0.11 Sn 118.7 0.19 Sr 87.62 1.60 Zr 91.22 0.10
  • etching rate f(x) of the resulting solutions (which may be abbreviated as 1/3/x solutions) was determined by applying the solutions to a heated silicon oxide film at 23° C., and the f(x) was plotted as a function of the concentration x [mol/kg) of HCl in the solution as shown in FIG. 1 .
  • x 1 and x 2 represent the concentrations of HCl at which the etching rate f(x) determined on a heated silicon oxide film was maximal and minimal respectively, and x 3 the maximum concentration of HCl at which no crystal precipitation was present.
  • etching solution of the invention having a sufficiently large volume with respect to glass substrates to be etched was applied to glass substrates which contain a given cation-yielding element at different concentrations, and etching was allowed to proceed for a certain period and then the etching solution was stirred to ensure the uniform dispersion of the cation in the solution.
  • the effect of the etched amount on the concentration of the cation in the solution was studied.
  • the concentration of the cation in an etching solution was determined by ICP-MS (induction-coupled high frequency plasma mass spectroscopy, HP-4500, Yokokawa-Hewlett-Packard).
  • the concentration of Al ions in an etching solution derived from an etched glass substrate was plotted as a function of the etched amount, and the resulting graph is shown in FIG. 2 .
  • a BHF-based etching solution comprising HF at 1.0 mol/kg and NH 4 F at 3.0 mol/kg was prepared, and different amounts of HCl was added to the solution to prepare BHF-based etching solutions with the concentration x of HCl being varied.
  • the test etching solutions were applied to a glass substrate containing cation-yielding elements. For each cation derived from the glass substrate, the relationship of its concentration in the solution with the etched amount of the substrate was plotted as for in Al shown above.
  • FIGS. 3, 4 and 5 show the relationships thus obtained for Ba, Ca and Sr, respectively.
  • FIGS. 2, 3 , 4 and 5 shows that, when the BHF-based solutions comprising HF at 1.0 mol/kg and NH 4 F at 3.0 mol/kg, where the concentration x of HCl was varied, were applied to the glass substrate containing Al, Ba, Ca, and Sr as main cation-yielding elements, the solubility of the salts of those elements to the etching solution increases when x is equal to x 1 .
  • the BHF-based solutions comprising HF at 1.0 mol/kg and NH 4 F at 3.0 mol/kg, where the concentration x of HCl was varied, were applied to a heated silicon oxide film at 23° C., and the etching rate f(x) was plotted as a function of the concentration x [mol/kg] of HCl in the solution.
  • the concentration x of HCl is preferably in the range: x ⁇ x 2 ⁇ ( x 2 ⁇ x 1 )/2
  • the graphs show that, if the concentration x of HCl is chosen to satisfy x ⁇ 3, solubility of the salts of the main cations derived from the glass substrate to the etching solution is enhanced.
  • H + ions and Cl ⁇ ions will be added to existent ions in the solution.
  • Addition of H + ions to the reaction system disturbs the existent acid-base equilibrium such that the concentration of F ⁇ ions in the solution is lowered.
  • addition of Cl ⁇ ions produces, instead of fluorides of cation-yielding elements contained in a glass substrate, the chlorides of those cation-yielding elements which are more soluble to the etching solution, which accounts for the reduction of crystal precipitation in an HCl-added etching solution.
  • the present inventors prepared HCl-added etching solutions with the concentration x of HCl being varied whose composition was as shown in Table 1.
  • the etching solutions were applied to a heated silicon oxide film at 23° C., and the etching rate f(x) was plotted as a function of the concentration x [mol/kg] of HCl.
  • an etching solution in which the concentration x of HCl is in the range of: x ⁇ x 2 ⁇ ( x 2 ⁇ x 1 )/2 gives an environment where the solubility of the salts of cation-yielding elements contained in a glass substrate to the solution is enhanced with an increase of the concentration x of HCl.
  • a BHF-based etching solution comprising HF at 1.0 mol/kg and NH 4 F at 3.0 mol/kg was prepared, to which different amounts of HCl were added to vary its concentration x.
  • the resulting acidified BHF-based etching solution was applied to a glass substrate until the surface of the glass substrate was etched away by 25, 50 or 100 ⁇ m.
  • the micro-roughness of the etched surface was evaluated by determining the Ra value of the surface. The results are shown in Table 3.
  • the micro-roughness (Ra value) of an etched surface was determined with an instrument adapted for the purpose ( ⁇ -step 250, Tencor).
  • salts of cation-yielding elements derived from a glass substrate have such a low solubility to the etching solution that they easily crystallize and deposit on the surface of the substrate, which causes the surface roughness to be increased with the increase of etching amount.
  • the present inventors applied the various etching solutions, whose composition is as shown in Table 1, to glass substrates and examined the micro-roughness (Ra value) of etched surfaces in the same manner as described above.
  • the etching solutions were applied to a heated silicon oxide film at 23° C., and the etching rate f(x) as a function of the concentration x [mol/kg] of HCl was plotted, and x 1 or the concentration of HCl at which the etching rate f(x) takes a maximum and x 2 or the concentration of HCl at which the etching rate f(x) takes a minimum were determined.
  • the etching solution can etch glass substrates so smoothly and uniformly that the increase of micro-roughness with the increase of etching amount is inhibited.
  • a BHF-based etching solution to which HCl is added such that the concentration x of HCl in the solution satisfies the above inequality, is applied to a glass substrate containing multiple ingredients as those used for the construction of flat panel display devices, the solubility of salts of cations derived from the glass substrate to the solution is enhanced, and an increase of micro-roughness with the increase of etching amount is inhibited.
  • etching solution it is possible to uniformly etch a glass substrate containing multiple ingredients without evoking crystal precipitation and increased surface roughness.
  • a BHF-based etching solution is prepared, different amounts of HCl are added to the solution, the resulting etching solutions with the concentration x of HCl varied are applied to a heated silicon oxide film at 23° C., the etching rate f(x) is plotted as a function of the concentration x [mol/kg] of HCl, and x 1 or the concentration of HCl at which the etching rate f(x) takes a maximum and x 2 or the concentration of HCl at which the etching rate f(x) takes a minimum are determined, then the same BHF-based solution to which HCl is added such that the concentration x of HCl in the solution satisfies the following inequality: x 2 ⁇ ( x 2 ⁇ x 1 )/2 ⁇ x ⁇ x 2 +( x 2 ⁇ x 1 )/2 will ensure the uniform processing of glass substrates.
  • the present invention it is possible to process glass substrates containing multiple ingredients as those used for the construction of flat display devices without inducing crystal precipitation and/or an increase in surface roughness.
  • An etching solution according to the present invention can also be used for cleaning filters. If a conventional etching solution is used for etching glass substrates, the solution will contain fluorides of cations, derived from the glass substrates, as precipitates. The etching solution is then passed through a filter to remove fluorides. However, after repeated use, the filter will be clogged. If such a filter is rinsed with an etching solution of the invention, fluorides depositing on the fiber network of the filter will dissolve in the solution and the filter will be cleaned sufficiently to be reused.
  • an acid-added etching solution in which the concentration of the acid is adjusted according to the present invention is applied to a glass substrate containing multiple ingredients, uniform etching of the surface of the substrate is achieved without causing an increase in the surface roughness. Therefore, if the surface of a glass substrate which has been etched by means of an etching solution prepared according to the invention is inspected, and it is found to exhibit considerable roughness, it is possible to conclude that the glass substrate has a certain inherent flaw such as entrapped air bubbles. Accordingly, it is possible to identify glass substrates having an inherent flaw, by checking the surface roughness of the substrates after subjecting them to the etching by means of an etching solution prepared according to the invention.

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US10/487,770 2001-08-24 2002-08-26 Surface treating solution for fine processing of glass base plate having a plurality of components Abandoned US20070029519A1 (en)

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JP2001255387A JP5132859B2 (ja) 2001-08-24 2001-08-24 多成分を有するガラス基板用の微細加工表面処理液
PCT/JP2002/008564 WO2003018500A1 (fr) 2001-08-24 2002-08-26 Solution de traitement de surface a composants multiples destinee au traitement de precision dune plaque de base en verre

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WO2003018500A1 (fr) 2003-03-06

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