WO2014087655A1 - 複合プレートおよびその製造方法 - Google Patents
複合プレートおよびその製造方法 Download PDFInfo
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- WO2014087655A1 WO2014087655A1 PCT/JP2013/007159 JP2013007159W WO2014087655A1 WO 2014087655 A1 WO2014087655 A1 WO 2014087655A1 JP 2013007159 W JP2013007159 W JP 2013007159W WO 2014087655 A1 WO2014087655 A1 WO 2014087655A1
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- WIPO (PCT)
- Prior art keywords
- composite plate
- sintered body
- zirconia
- thickness
- zirconia sintered
- Prior art date
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Definitions
- the present invention relates to a composite plate of a zirconia sintered body and fiber-reinforced plastics having scratch resistance and impact resistance, and a method for producing the same.
- an exterior member of a portable electronic device has a thin plate shape with a thickness of 2 mm or less and must withstand a collision such as dropping, so that a material having particularly high impact resistance is required.
- the materials used for the exterior member include metals, resins, and glass, but glass materials are widely used because of scratch resistance and high design.
- the glass material currently used is tempered glass tempered by ion exchange. In this tempered glass, a tempered layer of about several tens of ⁇ m is generated on the glass surface by ion exchange, and compressive stress is generated on the surface to prevent the progress of scratches.
- the strengthening mechanism of tempered glass is derived from the tempered layer, there are the following problems and further improvements are required. (1) If there is a scratch exceeding the reinforcing layer, there is a risk of immediate destruction.
- the glass itself has a Vickers hardness of about 600, and is easily scratched by contact with metal, concrete, etc., and the strength may be significantly reduced by scratches associated with use.
- zirconia ceramics are widely used in industrial materials because they are excellent in heat resistance, wear resistance, and corrosion resistance.
- zirconia ceramics have high strength, high toughness, high hardness, and scratch resistance, and further, it is easy to improve the design by coloring, and therefore, the use of zirconia ceramics is increasing.
- Patent Document 1 reports that 8 mm thick alumina and silicon carbide are bonded to fiber reinforced plastics.
- ⁇ External members such as portable electronic devices need to be resistant to free fall of impacts of about the product's own weight (about 100 g).
- thick ceramics must be used, so that the weight of the member increases and cannot be used as a portable exterior member.
- it is essential to improve the crack resistance with a thin plate, but hitherto, an impact resistant member that has improved the crack resistance against impacts such as dropping and collision in a zirconia plate with a thickness of 2 mm or less. And there was no manufacturing method.
- Patent Document 3 describes a watch cover glass in which sapphire and inorganic glass are bonded. This is intended to improve the scratch resistance by arranging a high-hardness sapphire on the surface of the watch cover glass. This method is intended, and this method does not provide the high impact resistance required for portable electronic device applications.
- the present invention relates to a composite plate of a zirconia sintered body and a fiber reinforced plastic having improved impact resistance, particularly resistance to impact by impact, and a method for producing the same. Furthermore, the present invention provides a composite plate having a particularly excellent white color tone among the composite plates of a zirconia sintered body and fiber reinforced plastics in order to improve impact resistance, particularly crack resistance due to impact. It relates to the manufacturing method.
- the present inventors have examined in detail the destruction phenomenon of a zirconia thin plate when a steel ball is dropped. As a result, it was found that the ceramic plate was bent and a bending moment was generated by the drop impact of the steel ball, and tensile fracture occurred near the impact point on the back side of the impact surface. It was also found that the smaller the elastic modulus of the material, the greater the deformation due to the impact, and the longer the time taken to absorb the impact, the smaller the absolute value of the maximum tensile stress applied to the back surface of the impact surface.
- the inventors of the present invention have made extensive studies based on the above-described knowledge, so that the fiber-reinforced plastics is disposed on the back surface of the zirconia thin plate (elastic modulus 200 GPa), and the two are closely fixed to each other.
- the back surface where tensile stress occurs is made of fiber-reinforced plastics, and the impact surface where compressive stress is generated is made into a zirconia sheet, realizing the impact resistance of the zirconia sheet As a result, the present invention has been completed.
- the translucency caused the interior to be transparent and the design properties were lowered. Therefore, a white composite plate excellent in design was completed by using a white adhesive for tightly fixing the zirconia thin plate and the fiber reinforced plastics.
- the present invention is a composite plate having a thickness of 2 mm or less in which a zirconia sintered body and fiber reinforced plastics are laminated and fixed in close contact with each other, and the thickness ratio between the zirconia sintered body and the fiber reinforced plastics Composite plate, (zirconia sintered body thickness / fiber reinforced plastics thickness) of 0.01 to 1 and apparent density of composite plate of 4.3 g / cm 3 or less, zirconia sintered body, fiber A composite plate having a thickness of 2 mm or less in which reinforced plastics are laminated and fixed in close contact with each other, and the maximum difference in surface irregularities of the zirconia sintered body is 50 ⁇ m or less per 1 cm 2 and zirconia It is a composite plate of 2 mm or less in which a sintered body and fiber reinforced plastics are laminated and fixed to each other with a white adhesive.
- the composite plate of the present invention is a composite plate having a thickness of 2 mm or less formed by laminating a zirconia sintered body and fiber reinforced plastics and closely fixing them.
- the thickness is preferably 0.1 to 1.5 mm for light weight, more preferably 0.15 to 1.0 mm, and particularly preferably 0.15 to 0.60 mm.
- the maximum value of the difference between the surface roughness of the zirconia sintered body, the maximum value of the difference of the irregularities per 1 cm 2 is at 50 ⁇ m or less, preferably 30 ⁇ m or less, more preferably at 20 ⁇ m or less is there.
- This is a ceramic composite plate that is a thin plate-shaped composite plate with excellent impact resistance, but has an excellent white color tone as an exterior member, and can prevent the loss of decorative value due to the inside being transparent. I can do it.
- the color tone becomes dark and the decorative value is impaired.
- the absolute value of the a * value and the b * value increases, the white color with a reddish, bluedish, yellowish or greenish color is obtained, and the decorative value is impaired.
- the zirconia sintered body and the fiber reinforced plastics are firmly fixed by a white adhesive.
- white adhesives include epoxy thermosetting adhesives, acrylic adhesives that cure at room temperature, cyanoacrylate adhesives, UV curable resins, etc., in order to suppress white color degradation due to light transmission of the zirconia sintered body.
- an epoxy thermosetting adhesive is preferable.
- a white adhesive containing a white filler is particularly preferable for improving the rigidity of the adhesive layer and imparting a white color tone.
- the white filler include alumina and silica.
- the ratio of the thickness of the zirconia sintered body to the thickness of the fiber reinforced plastics is 0.01 to 1.
- the ratio of the thickness of the zirconia sintered body to the thickness of the fiber-reinforced plastics is 0.01 to 1, it is possible to obtain an impact-resistant composite plate that is lightweight and has excellent scratch resistance. If it is less than 0.01, sufficient wear resistance cannot be obtained, and if it exceeds 1, the apparent density of the composite increases.
- the apparent density ( ⁇ (composite plate)) of the composite plate of the present invention is calculated from the true density of the zirconia sintered body ( ⁇ (zirconia)) and the true density of the fiber reinforced plastics ( ⁇ (fiber reinforced plastics)). It is given by (1).
- the density of the fiber-reinforced plastics varies depending on the type of plastics and the amount of fibers added, but a typical density is 0.9 to 2.45 g / cm 3 .
- the apparent density of the composite plate of the present invention is 4.3 g / cm 3 or less, preferably 0.9 ⁇ 4.3g / cm 3, more preferably 2.0 ⁇ 4.0g / cm 3, particularly preferably 2. If it is 2 to 3.2 g / cm 3, it is possible to obtain a lightweight feeling sufficient for use as an exterior member. Moreover, since glass is not used, it is excellent also about safety.
- the zirconia sintered body and the fiber reinforced plastics are closely fixed.
- the method for tightly fixing both of them include a fixing method using an adhesive, and a method of fixing plastics by dissolving them in heat, a solvent or the like and bringing them into close contact with a zirconia sintered body.
- the thickness of the adhesive layer is preferably 200 ⁇ m or less, more preferably 100 ⁇ m or less, and particularly preferably 50 ⁇ m or less.
- yttria-stabilized zirconia having both high strength, wear resistance and high toughness is preferable.
- Yttria-stabilized zirconia having high strength, wear resistance and high toughness can be obtained.
- a more preferable yttria content is 2 to 4 mol%.
- a stabilizer other than yttria can be used. Examples of other stabilizers include calcia, magnesia, and ceria.
- the zirconia sintered body in the composite plate of the present invention may further contain a colorant or the like to improve the design.
- a colorant for example, a white pigment such as alumina and a color pigment such as a transition metal oxide are preferably contained.
- the white pigment oxides such as alumina, silica, mullite, zinc oxide, and spinel can be used.
- it can be used as long as it is a general inorganic pigment, such as spinel complex oxides containing transition metals such as Fe, Co, Ni, Mn, erbium, neodymium, praseodymium, etc. Rare earth oxides can be used.
- the zircon etc. which added the transition metal can also be used. Transition metal oxides such as nickel and iron can also be used as pigments.
- the relative density of the zirconia sintered body in the composite plate of the present invention is preferably 97% or more, and in order to further improve the scratch resistance, it is also caused by irregularities on the surface of the sintered body based on residual pores. In order to suppress a decrease in design properties during mirror finishing, 98% or more is more preferable, and 99% or more is even more preferable.
- the zirconia sintered body in the composite plate of the present invention has a Vickers hardness of preferably 1000 or more, more preferably 1100 or more, more preferably 1200 or more, in order to exhibit sufficient scratch resistance. Highly preferred.
- fiber reinforced plastics used in the composite plate of the present invention include glass fiber reinforced plastics, carbon fiber reinforced plastics, aromatic polyamide fiber reinforced plastics, and cellulose fiber reinforced plastics. Carbon fiber reinforced plastics or glass fiber reinforced plastics that are easy to use industrially are preferred. Further, glass fiber reinforced plastics are preferable for members that require radio wave transmission.
- plastics used for fiber reinforced plastics include unsaturated polyester thermosetting resins, epoxy resins, polyamide resins, phenol resins, acrylic resins, silicones, polysulfone, polyethersulfone, and PET.
- examples of fibers that reinforce plastics include glass fibers, carbon fibers, cellulose fibers, aramid fibers, boron fibers, and polyethylene fibers.
- Examples of the method include finely cutting these fibers and uniformly coating the resin, or infiltrating the plastic with the fibers having directionality.
- the impact resistance (crack resistance) of the composite plate of the present invention is as follows.
- the composite plate is bonded onto an aluminum alloy with a double-sided tape having a thickness of 0.1 mm, and a 130 g steel ball can be freely dropped from any height.
- the height at which cracks occur in the zirconia sintered body is 10 cm or more, preferably 15 cm or more, and more preferably 20 cm or more.
- the composite plate of the present invention can be manufactured, for example, by joining a thin plate made of a zirconia sintered body and fiber reinforced plastics at a temperature of 300 ° C. or lower using an adhesive.
- the adhesive used for bonding include an epoxy thermosetting adhesive, an acrylic adhesive that cures at room temperature, a cyanoacrylate adhesive, and an adhesive such as an ultraviolet curable resin. It is preferable to use an epoxy-based thermosetting adhesive in that the bonding strength between the zirconia sintered body and the fiber-reinforced plastics is high, and the heat resistance and impact resistance are also high. It is also possible to add a filler such as inorganic particles to the adhesive to improve the rigidity of the adhesive layer. In order to realize a higher adhesive force, it is preferable to clean the bonded surface by ultraviolet / ozone treatment or plasma treatment. Also, the bonded surface of zirconia can be cleaned by heating.
- fiber reinforced plastics can be melted with heat or a solvent and welded to a zirconia sheet. It is also possible to place a zirconia thin plate in the mold and pour the fiber-reinforced plastics imparted with fluidity into the mold for welding to obtain a joined body.
- a prepreg impregnated with fibers can be adhered to zirconia, and then cured by ultraviolet rays or heat to be polymerized to obtain a composite.
- the thin plate of the zirconia sintered body according to the composite plate of the present invention can be prepared using a general ceramic molding method.
- a press method, an extrusion method, a slurry casting method, an injection molding method, and a sheet molding method can be exemplified, and among these, a sheet molding method using a doctor blade is preferable.
- a slurry in which zirconia powder and an organic binder are mixed is formed on a green sheet having a thickness of 1 mm or less by a doctor blade, and sintered at 1300 to 1500 ° C. to obtain a zirconia sintered body.
- the composite plate can be manufactured by grinding and polishing the surface of the zirconia sintered body.
- vacuum sintering, hot pressing, hot isostatic pressing (HIP) and the like can be used in addition to normal atmospheric sintering.
- the zirconia sintered body used for the composite plate of the present invention is preferably one whose surface side is mirror-polished.
- Ra arithmetic mean height
- the arithmetic average height is a value obtained by extracting a reference length from the roughness curve in the direction of the average line, and summing and averaging the absolute values of deviations from the average line of the extracted portion to the measurement curve.
- the maximum value of the surface unevenness difference of the zirconia sintered body joined to the fiber reinforced plastic is 50 ⁇ m or less per 1 cm 2 .
- the maximum height (Ry) represents the height from the lowest valley bottom to the highest mountain peak for each reference length, and Ry is preferably 10 ⁇ m or less.
- the ten-point average roughness (Rz) is selected from 5 points from the highest peak of each reference length and 5 points from the lowest peak, and represents the average height, and Rz is preferably 5 ⁇ m or less.
- the composite plate of the present invention is thin and has high impact resistance and scratch resistance, it can be used as a housing member for portable electronic devices such as smartphones, tablet terminals, notebook PCs, and small music players. Can do. It can also be used as an input device member such as a touch pad. Moreover, since the thing using glass fiber reinforced plastics has high radio wave permeability, it can be used also for members, such as a protection member of an antenna. Furthermore, by using colored zirconia, it is possible to use it as a watch member because it is easy to improve the design.
- FIG. It is a figure which shows the external appearance of the zirconia composite plate obtained in Example 4.
- FIG. It is a microscope picture which shows the surface after performing a damage process to the zirconia composite plate obtained in Example 37. It is a figure which shows the state after performing a nail penetration test to the zirconia composite plate obtained in Example 39.
- 6 is a photomicrograph showing the surface after scratching the aluminosilicate tempered glass used in Comparative Example 5.
- FIG. It is a figure which shows the state after performing the nail penetration test with respect to the base material (white zirconia sintered compact) of the comparative example 6.
- the three-dimensional surface shape of the zirconia composite plate of Example 42 The surface profile of the composite plate of Reference Example 1.
- the surface shape of the zirconia sintered body of Reference Example 2. The figure which shows the tablet type terminal of 1st Embodiment.
- each sintered body obtained by sintering the powder used in the following examples and comparative examples is a sintered body using white zirconia powder (3YS20A): 5.51 g / cm 3 , black Sintered body using zirconia powder (product name “TZ-Black” manufactured by Tosoh Corporation): 6.06 g / cm 3 , Sintered body using zirconia powder (product name “3YSE” manufactured by Tosoh Corporation): 6.09 g / Cm 3 .
- 3YS20A is a system in which 20 wt% alumina is added to zirconia containing 3 mol% yttria, and TZ-Black is a spinel compound black pigment added to zirconia containing 3 mol% yttria.
- 3YSE is a system in which 0.25 wt% of alumina is added as an auxiliary to zirconia containing 3 mol% of yttria. (Impact strength measurement) The impact strength of the composite plate was evaluated using a steel ball drop test. For the steel ball drop test, a method similar to ISO14368-3 in the “Watch Glass Dimensions, Test Method” standard was applied.
- a steel ball of 130 g was freely dropped from an arbitrary height to the center position of the composite plate, and the height at which the composite plate was broken was measured.
- the bending strength of the composite plate was measured according to biaxial bending strength measurement (ISO / DIS6872).
- the support radius was 6 mm, the center of the composite plate was placed on the support, the zirconia surface was face up, the fiber reinforced plastic surface was the back surface, and the indenter was measured so that a load was applied to the center of the zirconia surface.
- the bending strength was calculated using a converted radius using a flat plate area.
- the three-dimensional shape measurement of the surface unevenness of the composite plate was evaluated using ZygoNewView7100.
- the surface unevenness per cm 2 was measured around the center of the test piece.
- the surface shape was measured by measuring the focal length using an optical microscope.
- the apparent density was calculated by setting the density of zirconia (3YS20A) to 5.47 g / cm 3 (relative density 99.3%), the density of glass fiber reinforced plastics to 2.0 g / cm 3, and zirconia and glass fiber reinforced resin. And the ratio was calculated.
- Example 1-3 White zirconia powder (trade name “3YS20A” manufactured by Tosoh Corporation) was molded at a pressure of 50 MPa by a mold press. The molded body was further molded by a cold isostatic press (CIP) with a pressure of 200 MPa.
- CIP cold isostatic press
- the obtained molded body was heated to 1500 ° C. at a temperature rising rate of 100 ° C./h in the atmosphere, and held at 1500 ° C. for 2 hours for sintering.
- the characteristics of the obtained sintered body are shown in Table 3 as reference examples.
- the obtained sintered body was subjected to double-side grinding and double-side polishing to a predetermined thickness to obtain a zirconia thin plate.
- Hv10 indicates Vickers hardness measured using an indenter load of 10 kgf.
- the evaluation results of the obtained composite plate are shown in Table 1.
- the apparent density of each composite plate was 4.3 g / cm 3 or less, and the Vickers hardness of each composite plate was 1000 or more.
- As a result of performing a steel ball drop test in increments of 5 cm it was found that all became 10 cm or more and exhibited high impact resistance.
- a steel ball drop test was performed in which a healthy part of the tested test piece was aimed at and dropped once from a drop height of 30 cm and 50 cm. The impact resistance was higher than that evaluated in 5 cm increments. It is considered that a high value was exhibited because the interface of the adhesive layer was not peeled off due to repeated impact tests.
- Example 4-10 A white zirconia sintered body (3YS20A) was obtained in the same manner as in Example 1. The adhesive was not peeled off due to processing, and zirconia chipping was not observed. Moreover, the photograph of the obtained composite_body
- the mirror-polished surface of the zirconia sintered body and the glass fiber reinforced plastics are uniformly applied to the upper and lower surfaces of the composite plate using an epoxy thermosetting resin (manufactured by Nagase ChemteX, product number “XN1245SR”). It was put in a suspended state and bonded under the conditions of 120 ° C. and 30 minutes.
- the obtained composite plate was cut into a shape of 32 mm ⁇ 25 mm, and the ceramic side was ground and mirror-polished so that the total thickness of the zirconia sintered body, the adhesive, and the fiber reinforced plastic was about 0.8 mm.
- Table 1 The evaluation results of the obtained composite plate are shown in Table 1.
- the apparent density of each composite plate was 4.3 g / cm 3 or less, and the Vickers hardness of each composite plate was 1000 or more.
- Table 1 shows the results of a steel ball drop test performed under the same conditions as in Example 1. The results of the impact resistance test were all 10 cm or more, and it was found that high impact resistance was exhibited.
- Examples 11-12 A room temperature curable acrylic adhesive (G55-03, NS-700M-20, manufactured by Denki Kagaku Kogyo Co., Ltd.) is used as the adhesive, and it is uniformly applied to the adhesive surface, and the load is evenly applied to the upper and lower surfaces of the composite plate.
- a zirconia composite plate was obtained in the same manner as in Example 4 except that the state was fixed and cured at room temperature for a whole day and night. The evaluation results of the obtained composite plate are shown in Table 1. All composite plates obtained a high impact resistance of 10 cm or more.
- Example 13-18 In bonding, the bonded surface of the zirconia plate and the glass fiber reinforced plastics was washed with acetone, further irradiated with ultraviolet ozone, and the washed surface was bonded using an epoxy adhesive.
- Example 4 A zirconia composite plate was obtained in the same manner as described above. The evaluation results of the obtained composite plate are shown in Table 1. It was found that those irradiated with ultraviolet ozone showed high impact resistance.
- the temperature was increased to 1450 ° C. in the atmosphere at a temperature increase rate of 100 ° C./h, and held at 1450 ° C. for 2 hours for sintering.
- 1400 at the same temperature increase rate.
- the mixture was heated to 1 ° C. and held at 1400 ° C. for 1 hour for sintering.
- the characteristics of the obtained sintered body are shown in Table 3 as reference examples.
- the obtained sintered body was subjected to double-side grinding and double-side polishing to a predetermined thickness to obtain a zirconia thin plate.
- the obtained zirconia thin plate was bonded to glass fiber reinforced plastics in the same manner as in Example 4 to obtain a composite plate.
- each composite plate was 4.3 g / cm 3 or less, and the Vickers hardness of each composite plate was 1000 or more.
- Table 1 shows the results of a steel ball drop test performed under the same conditions as in Example 1. The results of the impact resistance test were all 10 cm or more, and it was found that high impact resistance was exhibited.
- Examples 26-31 A composite plate was produced from a zirconia thin plate obtained by subjecting a zirconia sintered body obtained from each powder of 3YS20A, 3YSE, and TZ-Black to a hot isostatic pressing (HIP) treatment.
- HIP hot isostatic pressing
- 3YS20A, 3YSE, and TZ-Black sintered bodies were produced according to Example 4, Example 19, and Example 22, respectively, and then subjected to HIP treatment under an argon gas atmosphere and 150 MPa conditions.
- the HIP treatment temperature was 1450 ° C. for 1 hour for 3YS20A and 3YSE, and 1350 ° C. for 1 hour for TZ-Black.
- the HIP-treated body was tempered at 1000 ° C. for 1 hour, and a composite plate was prepared in the same manner as in Example 4. The relative density of all the sintered bodies reached 100% by the HIP treatment.
- Table 1 shows the results of the impact test of the obtained composite plate. It was found that the one using HIP-treated zirconia exhibits higher impact resistance.
- Examples 32-35 A zirconia composite plate was produced in the same manner as in Example 1 except that carbon fiber reinforced plastic (manufactured by CF Design Co., Ltd.) was used. The characteristics of the carbon fiber reinforced plastics used are shown in Table 4 as reference examples. Here, the density of the carbon fiber reinforced plastics was 1.5 g / cm 3 . Table 1 shows the results of a steel ball drop test performed in increments of 5 cm on the obtained composite plate. The results of the impact resistance test were all 10 cm or more, and it was found that high impact resistance was exhibited.
- carbon fiber reinforced plastic manufactured by CF Design Co., Ltd.
- Example 36 A composite plate was produced under the same conditions as in Example 4.
- the thickness of the sintered body was 0.239 mm
- the thickness of the glass fiber reinforced resin was 0.501 mm
- the thickness of the adhesive layer was 31 ⁇ m.
- the thickness of the zirconia sintered body / the thickness of the fiber reinforced plastic was 0.48.
- the apparent density of the composite plate was 3.00 g / cm 3 and the Vickers hardness was 1430.
- Example 37 A composite plate was produced in the same manner as in Example 4.
- the thickness of the sintered body was 0.210 mm
- the thickness of the glass fiber reinforced resin was 0.510 mm
- the thickness of the adhesive layer was 35 ⁇ m.
- the thickness of the zirconia sintered body / the thickness of the fiber-reinforced plastics was 0.41.
- the apparent density of the composite plate was 2.87 g / cm 3 and the Vickers hardness was 1430.
- the # 100 paper file was placed on the zirconia side surface of this composite plate, and further a load of 3 kg of iron weight was applied, and the iron weight was scratched by reciprocating a distance of 30 cm on the paper file five times.
- the steel ball breaking height did not change to 20 cm before and after the scratch treatment, and no reduction in impact strength due to the scratch treatment was observed.
- a micrograph of the surface of the zirconia after the injury is shown in FIG.
- Example 38 A 3YS20A 32 mm ⁇ 25 mm composite plate was produced in the same manner as in Example 4, and the bending strength was measured.
- the thickness of the sintered body was 0.257 mm
- the thickness of the glass fiber reinforced resin was 0.525 mm
- the thickness of the adhesive layer was 19 ⁇ m.
- the thickness of the zirconia sintered body / the thickness of the fiber reinforced plastic was 0.49.
- the apparent density of the composite plate was 3.07 g / cm 3 and the Vickers hardness was 1430.
- the bending strength was 800 MPa, showing a high value.
- the bending elastic modulus estimated from the load-displacement curve in the test was about 40 GPa, which was significantly lower than that of zirconia (250 GPa).
- Example 39 A nail penetration test was carried out on 3YS20A (32 mm ⁇ 25 mm) bonded to glass fiber reinforced plastics in the same manner as in Example 4.
- the thickness of the sintered body was 0.198 mm
- the thickness of the glass fiber reinforced resin was 0.504 mm
- the thickness of the adhesive layer was 45 ⁇ m.
- the thickness of the zirconia sintered body / the thickness of the fiber reinforced plastic was 0.39.
- the apparent density of the composite plate was 2.80 g / cm 3 and the Vickers hardness was 1430. The crack did not progress even when the nail was stabbed, and a through hole was formed only in the periphery of the nail.
- the state of the composite plate after the nail penetration test is shown in FIG.
- Example 40 700 g of TZ-3YS powder, 14 g of a commercially available polycarboxylic acid ester type polymer dispersant as a dispersant, 3.5 g of commercially available polyethylene glycol mono-para-iso-octylphenyl ether as an antifoaming agent, 245 g of ethyl acetate as a solvent, and 245 g of n-butyl acetate, 49 g of butyral resin (polymerization degree: about 1000) powder as a binder, and 42 g of industrial dioctyl phthalate as a plasticizer were added and mixed in a ball mill for 48 hours. Using a doctor blade apparatus and a blade, PET was used as a carrier film, and a green sheet was formed on the carrier film.
- the obtained green sheet was sintered by placing a weighted alumina setter on a porous alumina setter. Sintering is performed at room temperature to 450 ° C. at a heating rate of 5 ° C./h, held at 450 ° C. for 10 hours for degreasing, and from 450 ° C. to 1000 ° C., the heating rate is 50 ° C./h, It was held at 1000 ° C. for 5 hours and then held at 1450 ° C. for 2 hours for sintering.
- the relative density of the obtained sintered body was 99% or more.
- the obtained sintered body was used in the same manner as in Example 1 by using an epoxy-based thermosetting resin (product number “XN1245SR” manufactured by Nagase ChemteX) on glass fiber reinforced plastics having a size of 32 mm ⁇ 25 mm and a thickness of 0.501 mm. Adhesive treatment.
- the composite plate was prepared by grinding and polishing the zirconia side surface of the bonded composite plate.
- the thickness of the sintered body was 0.234 mm, and the thickness of the adhesive layer was 32 ⁇ m.
- the thickness of the zirconia sintered body / the thickness of the fiber-reinforced plastics was 0.47.
- the apparent density of the composite plate was 3.15 g / cm 3 and the Vickers hardness was 1430.
- the fracture height of the composite plate was 20 cm.
- Example 1 Using 3YS20A, a zirconia sintered body thickness / glass fiber reinforced plastic thickness ratio of 2.56 was produced in the same manner as in Example 1. The results are shown in Table 2. The apparent density of the composite plate exceeded 4.3 g / cm 3 .
- Comparative Example 2 Using 3YS20A, a plate in which a zirconia sintered body and glass fiber reinforced plastics were simply laminated without using an adhesive was prepared in the same manner as in Example 1, and a steel ball drop test was performed on this plate. The results are shown in Table 2. When it was placed directly on glass fiber reinforced plastics without being bonded, it was broken at 5 cm, and it was found that the impact resistance was remarkably low.
- Comparative Example 3 A composite plate was prepared in the same manner as in Example 1 except that 3YS20A was used and ABS resin was used instead of glass fiber reinforced plastics. The results of the steel ball drop test of this composite plate are shown in Table 2. In the case of using the ABS resin, it was broken at 5 cm, and the impact resistance was found to be extremely low.
- Comparative Example 4 A 130 g steel ball was dropped at a location 1 mm away from the end face of a 0.7 mm thick aluminosilicate tempered glass (32 mm ⁇ 25 mm) toward the center of the base material. In the vicinity of the end face, fracture occurred at 5 cm.
- Comparative Example 5 The surface of an aluminosilicate tempered glass (32 mm ⁇ 25 mm, thickness 0.7 mm) was subjected to a scratch treatment in the same manner as in Example 23, and the impact resistance before and after the scratch was evaluated.
- the steel ball drop breaking strength before the damage was 30 cm, and the steel ball breaking height was 10 cm due to the scratch.
- FIG. 4 shows a photograph of the surface of the glass subjected to the scratch treatment.
- Example 6 A white zirconia sintered body was produced under the conditions described in Example 1. A nail penetration test was conducted on the sintered body having both surfaces polished to a thickness of 0.2 mm. In the zirconia thin plate, cracks developed in the entire sintered body by nail penetration, and the base material was broken into several pieces. The state of the base material after the nail penetration test is shown in FIG.
- Comparative Example 7 A composite plate using a sapphire thin plate instead of zirconia was prepared under the conditions described in Example 1.
- the thickness of the sapphire was 0.218 mm, and the thickness of the adhesive layer was 45 ⁇ m.
- the thickness of the glass fiber reinforced plastics was 0.527 mm.
- sapphire elastic modulus 400 GPa
- Example 41 700 g of TZ-3YS-E (manufactured by Tosoh) powder, 14 g of a commercially available polycarboxylic acid ester type polymer dispersant as a dispersant, 3.5 g of commercially available polyethylene glycol mono-para-iso-octylphenyl ether as an antifoaming agent, 245 g of ethyl acetate and 245 g of n-butyl acetate as a solvent, 49 g of butyral resin (polymerization degree: about 1000) powder as a binder, and 42 g of industrial dioctyl phthalate as a plasticizer were added and mixed in a ball mill for 48 hours. Using a doctor blade apparatus and a blade, polyethylene terephthalate (PET) was used as a carrier film, and a green sheet was formed on the carrier film.
- PET polyethylene terephthalate
- the obtained green sheet was sintered by placing a weighted alumina setter on a porous alumina setter. Sintering is performed at room temperature to 450 ° C. at a heating rate of 5 ° C./h, held at 450 ° C. for 10 hours for degreasing, and from 450 ° C. to 1000 ° C., the heating rate is 50 ° C./h, It was held at 1000 ° C. for 5 hours and then held at 1450 ° C. for 2 hours for sintering.
- the density of the obtained zirconia sintered body was 6.085 g / cm 3 and the relative density was 99.9% or more.
- the obtained zirconia sintered body (thickness: about 0.5 mm) was cut into a size of 32 mm ⁇ 25 mm, and processed to a thickness of 0.321 mm using surface grinding and a mirror polishing machine.
- the upper and lower surfaces were processed under equal conditions.
- Surface grinding was performed using a # 140 grindstone. When the grinding speed was high, the generation of residual stress was prominent and warping occurred, so the grinding speed was low. After grinding the upper and lower surfaces under the same conditions, mirror polishing was performed.
- the upper and lower surfaces were polished under the same polishing conditions using 9 ⁇ m, 6 ⁇ m, and 1 ⁇ m diamond abrasive grains using Tegra Force (Marumoto Strulus Co., Ltd.).
- the polishing conditions for the 9 ⁇ m and 6 ⁇ m abrasive grains were 10 minutes at a pressure of 3.5 N / cm 2, and 1 ⁇ m was 10 minutes at a pressure of 2.8 N / cm 2 .
- the thickness of the obtained sintered body was 0.250 mm, and the maximum value of the surface unevenness was a flat zirconia sintered body of 1.381 ⁇ m per cm 2 .
- the prepared composite plate had a thickness of 0.900 mm, and each layer had a sintered body of 0.321 mm, an adhesive layer of 49 ⁇ m, and fiber reinforced plastics of 0.530 mm.
- the thickness of the zirconia sintered body / the thickness of the fiber reinforced plastic was 0.61.
- the apparent density of the composite plate was 3.35 g / cm 3 and the Vickers hardness was 1240.
- the maximum value of the surface unevenness of the obtained composite plate was 14.651 ⁇ m per 1 cm 2 , and a flat composite plate having high design properties with little distortion of the reflected image was obtained.
- FIG. 6 shows the three-dimensional surface shape of the zirconia sintered body used in Example 41 by gradation processing.
- the shape is substantially flat, and in the figure, it can be seen that the shape is a slope as it goes from the left hand back to the right hand side.
- FIG. 7 shows the three-dimensional surface shape of the zirconia composite plate of Example 41 by gradation processing as in FIG. In the range of 10.52 mm ⁇ 10.43 mm, a convex shape with a low front side and a high side near the center can be seen.
- FIG. 8 shows the three-dimensional surface shape of the zirconia composite plate of Example 42 by gradation processing as in FIG. In the range of 10.52 mm ⁇ 10.43 mm, it is almost flat, but the right side is slightly lower, and the left side is higher near the center.
- Black zirconia powder (manufactured by Tosoh Corporation, trade name “TZ-Black”) was molded with a mold press at a pressure of 50 MPa. The molded body was further molded by a cold isostatic press (CIP) with a pressure of 200 MPa. The obtained molded body was sintered in the air at a temperature rising rate of 100 ° C./h and a sintering temperature of 1400 ° C. for 1 hour. The obtained zirconia sintered body was subjected to double-side grinding and double-side polishing to a thickness of about 1 mm to obtain a zirconia plate. The density of the obtained zirconia sintered body was 5.993 g / cm 3 and the relative density was 99.0%. Here, the true density of black was set to 6.053 g / cm 3 .
- the thickness of the produced composite plate was 0.817 mm, and the thickness of each layer was 0.270 mm of a zirconia sintered body, an adhesive layer of 37 ⁇ m, and fiber-reinforced plastics of 0.510 mm.
- the thickness of the zirconia sintered body / the thickness of the fiber reinforced plastic was 0.53.
- the apparent density of the composite plate was 3.23 g / cm 3 and the Vickers hardness was 1240.
- the maximum value of the difference in surface irregularities of the obtained composite plate was 11.107 ⁇ m per 1 cm 2 , which was a flat composite plate, and a high design property with little distortion of the reflected image was obtained.
- FIG. 9 shows the surface profile of the composite plate of Reference Example 1, the horizontal axis shows the distance from the end of the composite plate, and the vertical axis shows the surface height. As shown in FIG. 9, it can be seen that the surface height decreases as the distance from the end increases and becomes deeper than the reference point (0).
- Example 42 Using a method similar to that in Example 42, a zirconia composite plate with remarkably surface irregularities was prepared such that residual stress was applied to the workpiece as grinding and polishing conditions.
- the produced zirconia composite plate had a low design property in which an image reflected by zirconia was distorted.
- the maximum value of the surface unevenness per 1 cm 2 was about 72 ⁇ m.
- FIG. 4 shows the surface profile with the most unevenness as the two-dimensional data.
- FIG. 10 shows the surface shape of the zirconia sintered body of Reference Example 2 by gradation processing as in FIG. In the range of 10.52 mm ⁇ 10.43 mm, it can be seen that the shape near the center is the lowest and becomes higher toward the four corners.
- Example 43 White zirconia powder (trade name “3YS20A” manufactured by Tosoh Corporation) was molded at a pressure of 50 MPa by a mold press. The molded body was further molded by a cold isostatic press (CIP) with a pressure of 200 MPa.
- CIP cold isostatic press
- the obtained molded body was heated to 1500 ° C. at a temperature rising rate of 100 ° C./h in the atmosphere, and held at 1500 ° C. for 2 hours for sintering.
- the obtained zirconia sintered body was subjected to double-side grinding and double-side polishing to a predetermined thickness to obtain a zirconia thin plate.
- Table 5 shows the evaluation results of the obtained composite plate. As a result of performing a steel ball drop test in increments of 5 cm, it was found that the impact resistance was as high as 15 cm.
- the lightness index L *, chromaticness index a * and b * in the surface color tone (L *, a *, b *) were measured with a color difference meter.
- a lightness index L * is higher than that of Reference Example 3, and a composite plate having a more excellent white color tone is obtained.
- the total light transmittance was measured using a haze meter.
- the total light transmittance was lower than that of Reference Example 1, indicating that the light transmission was hindered and the white color tone was improved.
- Reference example 3 A white zirconia sintered body (3YS20A) was obtained in the same manner as in Example 43.
- the adhesive was not peeled off due to processing, and zirconia chipping was not observed.
- the mirror-polished surface of the zirconia sintered body and the glass fiber reinforced plastics are uniformly applied to the upper and lower surfaces of the composite plate using a black epoxy-based thermosetting resin (manufactured by Nagase ChemteX, product number “XN1245SR”). It was put in a suspended state and bonded under the conditions of 120 ° C. and 30 minutes.
- the obtained composite plate was subjected to mirror polishing by grinding the ceramic surface so that the total thickness of zirconia, adhesive, and fiber reinforced plastic was 0.8 mm.
- the brightness index L *, chromaticness index a * and b * in the surface color tone (L *, a *, b *) were measured in the same manner as in Example 43. Compared to Example 43, the lightness index is low, the color of the black adhesive is transmitted, and the white color tone is lowered.
- Comparative Example 8 A white zirconia sintered body (3YS20A) was obtained in the same manner as in Example 43. A 1 mm flat zirconia sintered body was obtained by grinding and polishing.
- the impact resistance is as low as 5 cm.
- Example 43 has a higher white color tone than that of Reference Example 3, and a color tone close to that of bulk zirconia (only a zirconia sintered body having a thickness of 1 mm or more, not a composite plate). .
- FIG. 11 is a diagram illustrating a tablet terminal according to a first embodiment.
- a casing 2 that is an exterior member of a tablet terminal 1 as a portable electronic device is formed by the composite plate shown in the above-described embodiment.
- the portable electronic device is not limited to a tablet terminal, and may be a mobile phone, a smartphone, or the like.
- FIG. 12 is a view showing a wristwatch according to a second embodiment.
- a watch side 4 which is a watch member (exterior member) of a wristwatch 3 as a watch is formed by the composite plate shown in the above-described embodiment.
- the watch is not limited to a wristwatch, and may be a pocket watch, a stopwatch, or the like.
- the composite plate of the zirconia sintered body and fiber-reinforced plastics of the present invention is lightweight and has impact resistance and scratch resistance, so that it is suitably used for small and thin members such as portable electronic devices and watch members. be able to.
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Abstract
Description
(1)強化層を超える傷が入ると直ちに破壊してしまうおそれがある。
(2)ガラス自体のビッカース硬度は600程度であり、金属、コンクリート等との接触により容易に傷が付き、使用に伴う加傷により強度が著しく低下することがある。
(3)強化ガラスにおいては、強化処理後に加工することが出来ない。
(4)化学強化処理したものであっても、端面の加工傷の存在により端面強度が低下することがある。
(5)強化ガラスの破壊により細かな鋭利な破片を生ずる。
=ρ(ジルコニア)×ジルコニア厚み分率+ρ(繊維強化プラスチックス)×繊維強化プラスチックス厚み分率 (1)
繊維強化プラスチックスの密度は、プラスチックスの種類および繊維の添加量によって異なるが、一般的な密度としては0.9~2.45g/cm3の密度が例示できる。
最大高さ(Ry)は、基準長さ毎の最低谷底から最大山頂までの高さを表し、Ryは10μm以下が好ましい。また、十点平均粗さ(Rz)は、基準長さ毎の山頂の高い方から5点、谷底かの低い方から5点を選び、その平均高さを表し、Rzは5μm以下が好ましい。
(相対密度)
5枚のジルコニア質焼結体を集めてアルキメデス法を用いて試料の密度を測定した。得られた密度を真密度に対する相対密度として求めた。以下の実施例・比較例で使用した粉末を焼結して得られる、それぞれの焼結体の真密度は、白色ジルコニア粉末(3YS20A)を用いた焼結体:5.51g/cm3、黒色ジルコニア粉末(東ソー製、商品名「TZ-Black」)を用いた焼結体:6.06g/cm3、ジルコニア粉末(東ソー製、商品名「3YSE」)を用いた焼結体:6.09g/cm3とした。
(衝撃強度測定)
複合プレートの衝撃強度評価は鋼球落下試験を用いて行った。鋼球落下試験は、「ウオッチ用ガラスの寸法、試験方法」規格のISO14368-3に類似した方法を適用した。すなわち、厚さ5mmの平坦なアルミ合金上(50mm×52mm)に厚さ0.1mmの両面テープ(3M製、商品番号「4511-100」)で、実施例又は比較例で得られた複合プレートを固定し、当該複合プレートの中心位置に130gの鋼球を任意の高さから自由落下させ、複合プレートが破壊する高さを測定した。なおインパクト面については表面粗さRa=0.02μm以下に鏡面研磨したものを用いた。
(曲げ強度測定)
二軸曲げ強度測定(ISO/DIS6872)に準じて複合プレートの曲げ強度を測定した。サポート半径を6mmとし、複合プレートの中央をサポートに設置し、ジルコニア面を表向き、繊維強化プラスチックス面を裏面として、圧子がジルコニア面の中央に荷重が懸かるようにして測定を行なった。曲げ強度の算出は、平板面積を用いた換算半径を用いた。ジルコニアは表面粗さRa=0.02μm以下に両面鏡面研磨したものを用いた。(表面形状測定)
複合プレートの表面凹凸の3次元形状測定は、ZygoNewView7100を用いて評価した。テストピース中央を中心として、1cm2当たりにおける表面凹凸を測定した。起伏の激しい比較例1については、光学顕微鏡を用いて焦点距離を計測することにより表面形状を測定した。
(見かけ密度)
見かけ密度の算出は、ジルコニア(3YS20A)の密度を5.47g/cm3(相対密度99.3%)、ガラス繊維強化プラスチックスの密度を2.0g/cm3とし、ジルコニアとガラス繊維強化樹脂との比率から計算を行った。
白色ジルコニア粉末(東ソー製、商品名「3YS20A」)を金型プレスによって圧力50MPaで成形した。成形体を更に圧力200MPaの冷間静水圧プレス(CIP)で成形した。
実施例1と同様な方法で白色ジルコニア質焼結体(3YS20A)を得た。加工による接着剤の剥がれ、ジルコニアのチッピングなど見られず高い加工性であった。また得られた複合体の写真を図1に示す。得られた白色ジルコニア質焼結体を片面研削し、研削した側を鏡面研磨加工した。
接着剤として、室温硬化型のアクリル系接着剤(電気化学工業社製 G55-03、NS-700M-20)を用い、接着面に均一に塗布し、複合プレートの上下面に均等に荷重が懸かる状態とし、室温で一昼夜硬化させて接着した他は実施例4と同様の手法によってジルコニア複合プレートを得た。得られた複合プレートの評価結果を表1に示す。いずれの複合プレートについても10cm以上の高い耐衝撃性を得た。
接着に際しては、ジルコニア板とガラス繊維強化プラスチックスの接着面をアセトンにて洗浄し、更に紫外線オゾンにて照射し、洗浄処理をしたものについてエポキシ接着剤を用いて接着した他は、実施例4と同様の手法によってジルコニア複合プレートを得た。得られた複合プレートの評価結果を表1に示す。紫外線オゾンを照射したものは高い耐衝撃性を示すことがわかった。
ジルコニア粉末(東ソー製、商品名「3YSE」)黒色ジルコニア粉末(東ソー製,商品名「TZ-Black」)のそれぞれを金型プレスによって圧力50MPaで成形した。各成形体を更に圧力200MPaの冷間静水圧プレス(CIP)で成形した。
3YS20A、3YSE、TZ-Blackの各粉末から得られたジルコニア質焼結体について熱間静水圧プレス(HIP)処理を行って得られたジルコニア薄板から複合プレートを作製した。
炭素繊維強化プラスチックス(株式会社CFデザイン社製)を用いた以外は実施例1と同様な方法でジルコニア複合プレートを作製した。使用した炭素繊維強化プラスチックスの特性を参考例として表4に示す。ここで炭素繊維強化プラスチックスの密度は1.5g/cm3とした。得られた複合プレートに対して、5cm刻みで鋼球落下試験を行った結果を表1に示す。また耐衝撃試験の結果も、いずれも10cm以上となり高い耐衝撃性を示すことが分かった。
実施例4と同様な条件で複合プレートを作製した。焼結体の厚みは、0.239mmであり、ガラス繊維強化樹脂の厚みは0.501mm、接着層の厚みは31μmであった。ジルコニア質焼結体の厚み/繊維強化プラスチックスの厚みは0.48であった。複合プレートの見かけ密度は、3.00g/cm3、ビッカース硬度は1430であった。
実施例4と同様な方法にて、複合プレートを製造した。焼結体の厚みは、0.210mmであり、ガラス繊維強化樹脂の厚みは0.510mm、接着層の厚みは35μmであった。ジルコニア質焼結体の厚み/繊維強化プラスチックスの厚みは0.41であった。複合プレートの見かけ密度は、2.87g/cm3、ビッカース硬度は1430であった。
実施例4と同様の方法にて3YS20Aの32mm×25mmの複合プレートを製造し、曲げ強度を測定した。焼結体の厚みは、0.257mmであり、ガラス繊維強化樹脂の厚みは0.525mm、接着層の厚みは19μmであった。ジルコニア質焼結体の厚み/繊維強化プラスチックスの厚みは0.49であった。複合プレートの見かけ密度は、3.07g/cm3、ビッカース硬度は1430であった。
実施例4と同様の方法にて3YS20A(32mm×25mm)をガラス繊維強化プラスチックスに接着したものについて釘刺し試験を行った。焼結体の厚みは、0.198mmであり、ガラス繊維強化樹脂の厚みは0.504mm、接着層の厚みは45μmであった。ジルコニア質焼結体の厚み/繊維強化プラスチックスの厚みは0.39であった。複合プレートの見かけ密度は、2.80g/cm3、ビッカース硬度は1430であった。釘を刺してもクラックは全体に進行せず、釘周辺部のみに貫通穴が開いた。釘刺し試験後の複合プレートの様子を図3に示す。
TZ-3YS粉末を700g、分散剤として市販のポリカルボン酸エステル型高分子分散剤14g、消泡剤として市販のポリエチレングリコールモノ-パラ-イソ-オクチルフェニルエーテル3.5g、溶剤として酢酸エチル245g及び酢酸n-ブチル245g、結合剤としてブチラール樹脂(重合度約1000)粉末49g、及び可塑剤として、工業用のフタル酸ジオクチル42gを添加してボールミルにて48時間混合した。ドクターブレード装置およびブレードを使用しキャリヤーフィルムとしてPETを使用し、キャリヤーフィルム上にグリーンシートを成膜した。
3YS20Aを用い、実施例1と同様の方法で、ジルコニア質焼結体厚み/ガラス繊維強化プラスチックス厚みの比率を2.56にしたものを製造した。結果を表2に示す。複合プレートの見かけの密度は4.3g/cm3を超えた。
3YS20Aを用い、実施例1と同様の方法で、接着材を使用することなく単にジルコニア質焼結体とガラス繊維強化プラスチックスとを積層したプレートを作成し、このプレートの鋼球落下試験を行った結果を表2に示す。接着せずガラス繊維強化プラスチックスに直置きしてある場合、5cmで破壊し、耐衝撃特性は著しく低いことが分かった。
3YS20Aを用い、ガラス繊維強化プラスチックスのかわりにABS樹脂を用いた他は実施例1と同様の方法で複合プレートを作製した。この複合プレートの鋼球落下試験の結果を表2に示す。ABS樹脂を用いたものでは5cmで破壊し、耐衝撃特性は著しく低いことが分かった。
厚み0.7mmのアルミノシリケート系の強化ガラス(32mm×25mm)の端面から母材中央に向かって1mm離れた場所に130gの鋼球を落下した。端面付近では5cmで破壊が生じた。
アルミノシリケート系の強化ガラス(32mm×25mm、厚み0.7mm)の表面に対して、実施例23と同じ方法で加傷処理を行い、加傷前後の耐衝撃性を評価した。加傷前の鋼球落下破壊強度は、30cmであり、加傷によって鋼球破壊高さは、10cmとなった。加傷後の表面粗さは、Ra=0.8μm、Ry=6.72μmであった。加傷処理をしたガラスの表面写真を図4に示す。
実施例1に記載した条件で白色ジルコニア質焼結体を作製した。この焼結体の両面を研磨し厚み0.2mmとしたものについて釘刺し試験を行った。ジルコニア薄板では釘刺しにより焼結体全体にクラックが進展し、母材は数個の破片に破断した。釘刺し試験後の母材の様子を図5に示す。
実施例1に記載した条件でジルコニアの代わりにサファイヤ薄板を用いた複合プレートを作製した。サファイヤの厚みは、0.218mmであり、接着層の厚みは45μmであった。ガラス繊維強化プラスチックスの厚みは0.527mmであった。この複合プレートを実施例1記載の方法にて評価した結果、5cmで破壊した。サファイヤ(弾性率400GPa)は、ジルコニアと比較して弾性率が高いため、衝撃による変形能力が不十分であり、サファイヤ側に高い引っ張り応力が発生したものと考えられる。
TZ-3YS-E(東ソー製)粉末を700g、分散剤として市販のポリカルボン酸エステル型高分子分散剤14g、消泡剤として市販のポリエチレングリコールモノ-パラ-イソ-オクチルフェニルエーテル3.5g、溶剤として酢酸エチル245g及び酢酸n-ブチル245g、結合剤としてブチラール樹脂(重合度約1000)粉末49g、及び可塑剤として、工業用のフタル酸ジオクチル42gを添加してボールミルにて48時間混合した。ドクターブレード装置およびブレードを使用しキャリヤーフィルムとしてポリエチレンテレフタレート(PET)を使用し、キャリヤーフィルム上にグリーンシートを成膜した。
図8は実施例42のジルコニア複合プレートの3次元表面形状を図6と同様にグラデーション処理により示す。10.52mm×10.43mmの範囲において、ほぼ平坦であるが、右側が少し低く、左側が中央付近で高い形状が見て取れる。高低差は8.63670μm-(-2.47014μm)=11.10684μmで、a点、b点、c点は夫々平均高さを示す。
図9は参考例1の複合プレートの表面プロファイルを示し、横軸は複合プレートの端から距離、縦軸は表面高さを示す。図9に示すように、端からの距離が長くなるに従って表面高さが低くなり、基準点(0)を超えてさらに深くなることが見て取れる。
図10は、参考例2のジルコニア質焼結体の表面形状を図6と同様にグラデーション処理により示す。10.52mm×10.43mmの範囲において、中心付近が最も低く、四隅に向かうに従って高くなっている形状が見て取れる。高低差は4.31637μm-(-2.70643μm)=7.0228μmで、a点、b点、c点は夫々平均高さを示す。
白色ジルコニア粉末(東ソー製、商品名「3YS20A」)を金型プレスによって圧力50MPaで成形した。成形体をさらに圧力200MPaの冷間静水圧プレス(CIP)で成形した。
実施例43と同様な方法で白色ジルコニア質焼結体(3YS20A)を得た。加工による接着剤の剥がれ、ジルコニアのチッピングなど見られず高い加工性であった。ついでジルコニア質焼結体の鏡面研磨面とガラス繊維強化プラスチックスを黒色エポキシ系熱硬化性樹脂(ナガセケムテックス製、商品番号「XN1245SR」)を用いて、複合プレートの上下面に均等に荷重が懸かる状態とし、120℃、30分の条件で接着した。得られた複合プレートをジルコニア、接着剤、繊維強化プラスチックスの全厚みが0.8mmとなるようにセラミックス面を研削、鏡面研磨した。
実施例43と同様な方法で白色ジルコニア質焼結体(3YS20A)を得た。研削・研磨加工を行い1mmの平板状ジルコニア質焼結体を得た。
図11は第1実施形態のタブレット型端末を示す図である。
図12は第2実施形態の腕時計を示す図である。
2 筐体
3 腕時計
4 時計部材(時計側)
Claims (17)
- ジルコニア質焼結体と繊維強化プラスチックスが積層し、互いに密着固定されてなる厚み2mm以下の複合プレートであって、ジルコニア質焼結体と繊維強化プラスチックスとの厚み比率(ジルコニア質焼結体厚み/繊維強化プラスチックス厚み)が0.01~1であり、且つ、複合プレートの見かけ密度が4.3g/cm3以下である複合プレート。
- ジルコニア質焼結体と繊維強化プラスチックスが積層し、互いに密着固定されてなる厚み2mm以下の複合プレートであって、ジルコニア質焼結体の表面凹凸の差の最大値が、1cm2あたり50μm以下である複合プレート。
- ジルコニア質焼結体と繊維強化プラスチックスとの厚み比率(ジルコニア質焼結体厚み/繊維強化プラスチックス厚み)が0.01~1である請求項2記載の複合プレート。
- 複合プレートの見かけ密度が4.3g/cm3以下である請求項2又は3に記載の複合プレート。
- ジルコニア質焼結体と繊維強化プラスチックスが積層し、互いに白色接着剤によって密着固定されてなる2mm以下の複合プレートであって、ジルコニア質焼結体表面の色調(L*、a*、b*)がL*=86~94、a*=-1~+1、b*=-1~+1の範囲の白色を呈する請求項1~4のいずれかに記載の複合プレート。
- ジルコニア質焼結体が、ジルコニアに対して2~10mol%のイットリアを含有するジルコニアである請求項1~5のいずれかに記載の複合プレート。
- ジルコニア質焼結体が、白色顔料、遷移金属酸化物、着色顔料からなる群より選ばれる少なくとも1種を含有するジルコニアである請求項1~6のいずれかに記載の複合プレート。
- ジルコニア質焼結体の相対密度が97%以上である請求項1~7のいずれかに記載の複合プレート。
- ジルコニア質焼結体のビッカース硬度が1000以上である請求項1~8のいずれかに記載の複合プレート。
- 繊維強化プラスチックスが、ガラス繊維強化プラスチックス又は炭素繊維強化プラスチックスである請求項1~9のいずれかに記載の複合プレート。
- 130gの鋼球を自由落下させる試験において、破壊高さが10cm以上である高耐衝撃性を示す請求項1~10のいずれかに記載の複合プレート。
- 複合プレートの厚みが0.1~1.5mmである請求項1~11のいずれかに記載の複合プレート。
- 複合プレートの見掛け密度が0.9~4.3g/cm3である請求項1~12のいれかに記載の複合プレート。
- 請求項1から13のいずれかに記載の複合プレートを製造する方法であって、
ジルコニア質焼結体と繊維強化プラスチックスを、エポキシ系熱硬化型接着剤を用いて300℃以下の温度で接合する複合プレートの製造方法。 - ジルコニア質焼結体が、ジルコニア粉末と有機バインダーを混合したスラリーを厚さ1mm以下のグリーンシートに成膜し、次いで1300~1500℃で焼結したものである請求項14に記載の複合プレートの製造方法。
- 請求項1~13のいずれかに記載の複合プレートを用いた携帯用電子機器の筐体。
- 請求項1~13のいずれかに記載の複合プレートを用いた時計部材。
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JP6064567B2 (ja) | 2017-01-25 |
TW201433454A (zh) | 2014-09-01 |
CN104903096B (zh) | 2017-06-23 |
EP2930018A1 (en) | 2015-10-14 |
US20150283791A1 (en) | 2015-10-08 |
US10682831B2 (en) | 2020-06-16 |
JP2014113726A (ja) | 2014-06-26 |
TWI636873B (zh) | 2018-10-01 |
EP2930018B1 (en) | 2019-10-02 |
KR102120321B1 (ko) | 2020-06-08 |
CN104903096A (zh) | 2015-09-09 |
KR20150092143A (ko) | 2015-08-12 |
EP2930018A4 (en) | 2016-06-01 |
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