Classifications

• • 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
  • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
  • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
  • C03C3/066—Glass compositions containing silica with less than 40% silica by weight containing boron containing zinc
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
  • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
  • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
  • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
• • 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
  • C03C3/00—Glass compositions
  • C03C3/04—Glass compositions containing silica
  • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
  • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
  • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
  • C03C3/093—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium containing zinc or zirconium
• • 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
  • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
  • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
  • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P14/00—Formation of materials, e.g. in the shape of layers or pillars
  • H10P14/60—Formation of materials, e.g. in the shape of layers or pillars of insulating materials
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
  • H10P52/00—Grinding, lapping or polishing of wafers, substrates or parts of devices
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
  • H10W74/00—Encapsulations, e.g. protective coatings
  • H10W74/10—Encapsulations, e.g. protective coatings characterised by their shape or disposition
• • H—ELECTRICITY
  • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
  • H10W—GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10
  • H10W74/00—Encapsulations, e.g. protective coatings
  • H10W74/40—Encapsulations, e.g. protective coatings characterised by their materials

Definitions

• the present invention relates to glass for covering semiconductor elements, materials for covering semiconductor elements, and sintered bodies for covering semiconductor elements.
• the surface of semiconductor devices such as silicon diodes and transistors, including the PN junction, is covered with glass. This makes it possible to stabilize the surface of the semiconductor element and suppress deterioration of characteristics over time.
• the characteristics required of glass for covering semiconductor devices are (1) the coefficient of thermal expansion should match that of the semiconductor device so that cracks etc. do not occur due to the difference in the coefficient of thermal expansion with the semiconductor device; (2) In order to prevent deterioration of the characteristics of the semiconductor element, it must be possible to coat at a low temperature (for example, 900° C. or lower), and (3) it must not contain impurities such as alkaline components that adversely affect the surface of the semiconductor element.
• zinc-based glasses such as ZnO-B 2 O 3 -SiO 2- based glasses, PbO-SiO 2 -Al 2 O 3 -based glasses, and PbO-SiO 2 -Al 2 O 3 -B 2 glasses have been used as glasses for covering semiconductor devices.
• Lead-based glasses such as O 3 -based glass are known, but currently, from the viewpoint of workability, PbO-SiO 2 -Al 2 O 3 -based glass, PbO-SiO 2 -Al 2 O 3 -B 2 O
• Lead-based glasses such as type 3 glasses are the mainstream (see, for example, Patent Documents 1 to 4).
• the lead component of lead-based glass is a component harmful to the environment. Furthermore, since the above-mentioned zinc-based glass contains small amounts of lead and bismuth components, it cannot be said that it is completely harmless to the environment.
• zinc-based glass tends to have a high coefficient of thermal expansion, and when coated on the surface of a semiconductor element such as Si, there is a risk that the semiconductor element may crack or warp.
• the present invention was made in view of the above circumstances, and its technical object is to provide a glass for covering semiconductor elements that has a small environmental impact, a low coefficient of thermal expansion, and a low surface charge density. .
• the present inventors have discovered that the above technical problems can be solved by using SiO 2 -ZnO-Al 2 O 3 -based glass having a specific glass composition, and have proposed the present invention. It is. That is, the glass for covering a semiconductor device of the present invention has a glass composition, in terms of mol%, of SiO 2 30 to less than 53%, ZnO 15 to 30%, Al 2 O 3 2 to 14%, and B 2 O 3 0 to 10%. %, MgO+CaO 11 to 30%, and is characterized by containing substantially no lead component.
• MgO+CaO refers to the total amount of MgO and CaO.
• substantially not containing means that the relevant component is not intentionally added as a glass component, and does not mean that impurities that are unavoidably mixed are completely eliminated. Specifically, it means that the content of the relevant component including impurities is less than 0.1% by mass.
• the glass for covering semiconductor elements of the present invention has the content range of each component regulated. As a result, the environmental load is small, the thermal expansion coefficient is low, and the surface charge density is reduced. As a result, it can be suitably used for covering semiconductor elements for low breakdown voltage.
• the glass for covering semiconductor elements of the present invention preferably contains Zn 2 SiO 4 as the main crystal after heat treatment.
• heat treatment refers to heat treatment at 800 to 1000° C. for 10 minutes or more.
• the material for covering a semiconductor element of the present invention contains a glass powder made of the above-mentioned glass for covering a semiconductor element.
• the semiconductor element coating material of the present invention has a thermal expansion coefficient of 20 ⁇ 10 ⁇ 7 /°C or more and 48 ⁇ 10 ⁇ 7 /°C or less in the temperature range of 30 to 300° C. after heat treatment. This makes it easier to avoid the occurrence of cracks or warpage in the semiconductor element.
• the "thermal expansion coefficient in the temperature range of 30 to 300°C” refers to a value measured by a push rod type thermal expansion coefficient measuring device.
• the sintered body for covering semiconductor elements of the present invention is characterized in that it contains Zn 2 SiO 4 as a main crystal, and the volume ratio of Zn 2 SiO 4 is 10 to 40%.
• the sintered body for covering a semiconductor element is a material obtained by heat-treating a material for covering a semiconductor element.
• the sintered body for covering semiconductor elements of the present invention is characterized in that it contains Zn 2 SiO 4 as a main crystal and has a porosity of 10% or less.
• the sintered body for covering semiconductor elements of the present invention has a glass composition, in terms of mol%, of SiO 2 30 to less than 53%, ZnO 15 to 30%, Al 2 O 3 2 to 14%, and B 2 O 3 0 to 10. %, MgO+CaO 11 to 30%, and preferably contains substantially no lead component.
• the present invention it is possible to provide a glass for covering semiconductor elements that has a small environmental load, a low coefficient of thermal expansion, and a low surface charge density.
• the glass for covering semiconductor devices of the present invention has a glass composition, in terms of mol%, of SiO 2 30 to less than 53%, ZnO 15 to 30%, Al 2 O 3 2 to 14%, B 2 O 3 0 to 10%, It is characterized by containing more than 11% to 30% of MgO+CaO and substantially no lead component.
• % means mol%.
• a numerical range indicated using " ⁇ " in this specification means a range that includes the numerical values listed before and after " ⁇ " as the minimum and maximum values, respectively.
• SiO 2 is a network forming component of glass and is a component that increases acid resistance. It is also a constituent of Zn 2 SiO 4 .
• the content of SiO 2 may be less than 30-53%, 30-52%, 30-51%, 30-50%, 30-50%, 32-48%, especially 35-45%. preferable. If the content of SiO 2 is too small, the coefficient of thermal expansion tends to increase and the acid resistance tends to decrease. Moreover, Zn 2 SiO 4 becomes difficult to precipitate, and the coefficient of thermal expansion of the coating material becomes too high, resulting in large warpage during firing coating. On the other hand, if the content of SiO 2 is too high, the firing temperature will become too high, making it impossible to form the coating layer at an appropriate temperature.
• ZnO is a component that stabilizes glass. It is also a constituent of Zn 2 SiO 4 .
• the content of ZnO is 15-30%, preferably less than 17-28%, 19-26%, 19.5-25%, particularly 20-24%. If the ZnO content is too low, devitrification during melting becomes strong, making it difficult to obtain a homogeneous glass. Moreover, Zn 2 SiO 4 becomes difficult to precipitate, and the thermal expansion coefficient of the coating material becomes too high, resulting in large warpage during firing coating. On the other hand, if the ZnO content is too high, acid resistance tends to decrease. In addition, the crystallinity becomes too strong, the viscosity increases rapidly during firing, and defects such as bubbles are likely to be included in the coating material.
• SiO 2 +ZnO total amount of SiO 2 and ZnO
• total amount of SiO 2 and ZnO is preferably 45 to less than 80%, 50 to 70%, particularly 55 to less than 65%. If the total amount of SiO 2 and ZnO is too small, Zn 2 SiO 4 will be difficult to precipitate, the thermal expansion coefficient of the coating material will become too high, and the warpage during firing and coating will become large. On the other hand, if the total amount of SiO 2 and ZnO is too large, the crystallinity becomes too strong, the viscosity increases rapidly during firing, and defects such as bubbles are likely to be included in the coating material.
• Al 2 O 3 is a component that stabilizes the glass and adjusts the surface charge density.
• the content of Al 2 O 3 is between 2 and 14%, preferably between 4 and 12%, particularly between 5 and 10%. If the content of Al 2 O 3 is too low, the glass tends to devitrify during molding. On the other hand, if the content of Al 2 O 3 is too large, the surface charge density may become too large.
• B 2 O 3 is a network forming component of glass and is a component that increases softening fluidity.
• the content of B 2 O 3 is 0 to 10%, preferably 0 to 7%, 0 to 5%, particularly 0 to 3%. If the content of B 2 O 3 is too large, it becomes difficult to crystallize the glass, and acid resistance tends to decrease.
• MgO and CaO are components that lower the viscosity of glass.
• the total amount of MgO and CaO is more than 11 to 30%, preferably 12 to 28%, 15 to 25%, particularly 16 to 24%. If the total amount of MgO and CaO is too small, the firing temperature of the glass tends to rise. On the other hand, if the total amount of MgO and CaO is too large, there is a risk that the coefficient of thermal expansion will become too high, the chemical resistance will decrease, and the insulation property will decrease.
• the material contains substantially no lead components (for example, PbO, etc.), and substantially no Bi 2 O 3 , F, or Cl. Further, it is preferable that it does not substantially contain alkaline components (Li 2 O, Na 2 O, and K 2 O) that adversely affect the surface of the semiconductor element.
• the above components contains up to 7% (preferably up to 3%) of other components (for example, SrO, BaO, MnO 2 , Nb 2 O 5 , Ta 2 O 5 , CeO 2 , Sb 2 O 3 , etc.) You may.
• other components for example, SrO, BaO, MnO 2 , Nb 2 O 5 , Ta 2 O 5 , CeO 2 , Sb 2 O 3 , etc.
• the glass for covering semiconductor elements of the present invention preferably contains Zn 2 SiO 4 as the main crystal after heat treatment.
• Zn 2 SiO 4 has a coefficient of thermal expansion very close to that of silicon, which is the coating target of the glass of the present invention, and has the role of greatly suppressing the occurrence of warpage during firing after coating.
• crystals such as ZnAl 2 O 4 may also be contained at the same time.
• the volume ratio of Zn 2 SiO 4 is preferably 10 to 40%, 12 to 35%, particularly 15 to 30%. If the volume ratio of Zn 2 SiO 4 is too small, the coefficient of thermal expansion of the coating material will become too high, resulting in large warpage during firing after coating. On the other hand, if the volume ratio of Zn 2 SiO 4 is too large, the viscosity of the glass increases rapidly above its softening point, making it more likely to contain defects such as bubbles.
• Volume ratio of Zn 2 SiO 4 refers to the background removed from the peak of Zn 2 SiO 4 obtained by X-ray diffraction method, and the integrated intensity of the sharp peak of the crystalline phase is calculated by ) is divided by the integrated intensity of the broad peak and multiplied by 100.
• the material for covering a semiconductor element of the present invention preferably contains a powder obtained by processing the glass for covering a semiconductor element, that is, a glass powder. If processed into glass powder, the surface of a semiconductor element can be easily coated using, for example, a paste method, an electrophoretic coating method, or the like. Thereafter, by heat-treating the material for covering the semiconductor element, it is possible to cover the surface of the semiconductor element with the sintered body for covering the semiconductor element.
• the average particle diameter D 50 of the glass powder is preferably 25 ⁇ m or less, particularly 15 ⁇ m or less. If the average particle diameter D 50 of the glass powder is too large, it becomes difficult to form it into a paste. Furthermore, powder adhesion by electrophoresis becomes difficult. Note that the lower limit of the average particle diameter D 50 of the glass powder is not particularly limited, but realistically it is 0.1 ⁇ m or more.
• average particle diameter D50 is a value measured on a volume basis, and refers to a value measured by a laser diffraction method.
• Glass powder can be produced, for example, by mixing the raw material powders of each oxide component into a batch, melting it at about 1500°C for about 1 hour to vitrify it, and then molding it (and then crushing and classifying it as necessary). Obtainable.
• the thermal expansion coefficient in the temperature range of 30 to 300°C is 20 ⁇ 10 -7 /°C or more and 48 ⁇ 10 -7 /°C or less, particularly 30 ⁇ 10 -7 /°C or more and 45 ⁇ 10 ⁇ 7 /°C or less is preferable.
• the coefficient of thermal expansion is outside the above range, cracks, warpage, etc. are likely to occur due to the difference in coefficient of thermal expansion with the semiconductor element.
• the surface charge density is, for example, 10 ⁇ 10 11 /cm 2 or less, especially 8 ⁇ 10 11 /cm 2 or less when coating the surface of a semiconductor device with a voltage of 1500 V or less. It is preferable. If the surface charge density is too high, the voltage resistance improves, but at the same time leakage current also tends to increase. Note that the "surface charge density" refers to a value measured by the method described in the Examples section below.
• the sintered body for covering a semiconductor element of the present invention contains Zn 2 SiO 4 as a main crystal.
• the glass composition contains, in mol%, SiO 2 30 to less than 53%, ZnO 15 to 30%, Al 2 O 3 2 to 14%, B 2 O 3 0 to 10%, and MgO + CaO more than 11 to 30%.
• the lead component is substantially not contained.
• the suitable range of the content of each component of the sintered compact for covering a semiconductor element and the suitable range of the amount of precipitation of Zn 2 SiO 4 are the same as those of the glass for covering a semiconductor element.
• the sintered body for covering semiconductor elements of the present invention preferably has a porosity of 10% or less, 8% or less, particularly 5% or less. If the porosity is too high, the coating may become insufficient and pressure resistance may be adversely affected. Note that, realistically, the lower limit of the porosity is 0.1% or more.
• a sintered body for covering semiconductor elements containing Zn 2 SiO 4 as the main crystal is produced by mixing a nucleating agent such as ZnO powder with amorphous glass powder and then heat-treating the mixed powder. I don't mind.
• Table 1 shows Examples (Samples No. 1 to 5) of the present invention and Comparative Examples (Samples No. 6 to 9).
• Each sample was produced as follows. First, raw material powders were prepared into a batch so as to have the glass composition shown in the table, and the batch was melted at 1500° C. for 1 hour to vitrify it. Subsequently, the molten glass was formed into a film, pulverized in a ball mill, and classified using a 350 mesh sieve to obtain a glass powder having an average particle diameter D50 of 12 ⁇ m.
• the volume ratio of Zn 2 SiO 4 was measured as follows.
• the glass powder was molded into a button shape, heat-treated at 800-950°C for 10 minutes, then crushed in a mortar, and an X-ray diffraction device was used to obtain a diffraction peak. After removing the background, it was assigned to Zn 2 SiO 4 .
• the integrated intensity of the crystal-derived peak was divided by the integrated intensity of the glass-derived peak and multiplied by 100.
• the thermal expansion coefficient is a value measured in a temperature range of 30 to 300°C using a push rod type thermal expansion coefficient measuring device using a measurement sample that has been heat treated at 800 to 950°C for 10 minutes.
• the surface charge density was measured as follows. First, each sample was dispersed in an organic solvent, adhered to the surface of a silicon substrate to a constant thickness by electrophoresis, and then baked at a temperature that promotes crystallization to form a coating layer. Next, after forming an aluminum electrode on the surface of the coating layer, the change in capacitance in the coating layer was measured using a CV meter, and the surface charge density was calculated.
• the defect inclusion status was measured as follows. The glass on the silicon substrate fired as described above was observed with a stereomicroscope, and if bubbles with a diameter of 10 ⁇ m or more were not observed, it was marked as “ ⁇ ”, and if confirmed, it was marked as “x”.
• the amount of warpage was measured as follows. First, the above silicon substrate was placed on a surface plate so as to be convex downward, and an arbitrary point on the circumference of the silicon substrate was tightly fixed to the surface plate with double-sided tape. Next, the height displacement on a straight line passing through the fixed point of the silicon substrate and the center of the circle was measured using a laser displacement meter. The difference in height between the highest and lowest points of the obtained displacement was calculated, and the difference was evaluated as the amount of warpage. Note that if the amount of warpage is 300 ⁇ m or less, it can be said that the amount of warpage is small.
• the porosity was measured as follows. First, glass powder and photoresist liquid were mixed and uniformly applied onto a smooth silicon substrate of known weight. Next, after firing at 500° C. for 1 hour and 950° C. for 20 minutes, the thickness of the sintered glass film was measured with a micrometer, and the bulk density of the sintered glass film was determined by measuring the weight. Next, "(density of glass - bulk density of sintered film)/density of glass" was calculated and determined as the porosity.
• sample No. Samples Nos. 1 to 5 showed desired values in thermal expansion coefficient, surface charge density, and amount of warpage. In addition, the defect inclusion status was also good. Therefore, sample no. Nos. 1 to 5 are considered to be suitable as semiconductor element coating materials used for coating low voltage semiconductor elements.
• sample No. 6 no crystals were precipitated, the coefficient of thermal expansion was high, and the evaluation of the amount of warpage was poor.
• Sample No. Samples No. 7 and No. 8 had strong crystallinity and contained defects due to the rapid increase in viscosity during firing.
• Sample No. Sample No. 9 had too strong devitrification and could not be formed into glass.

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• 2023
  • 2023-06-16 CN CN202380050977.1A patent/CN119451920A/zh active Pending
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