WO2016084722A1 - アルミナ焼結体及び光学素子用下地基板 - Google Patents

アルミナ焼結体及び光学素子用下地基板 Download PDF

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WO2016084722A1
WO2016084722A1 PCT/JP2015/082644 JP2015082644W WO2016084722A1 WO 2016084722 A1 WO2016084722 A1 WO 2016084722A1 JP 2015082644 W JP2015082644 W JP 2015082644W WO 2016084722 A1 WO2016084722 A1 WO 2016084722A1
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sintered body
alumina sintered
alumina
ppm
mass
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PCT/JP2015/082644
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English (en)
French (fr)
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潔 松島
守道 渡邊
佐藤　圭
七瀧　努
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日本碍子株式会社
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Priority to KR1020177006237A priority Critical patent/KR102376825B1/ko
Priority to CN201580047884.9A priority patent/CN107001148B/zh
Priority to JP2016561546A priority patent/JP6585620B2/ja
Publication of WO2016084722A1 publication Critical patent/WO2016084722A1/ja
Priority to US15/447,670 priority patent/US10138166B2/en

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Definitions

  • the present invention relates to an alumina sintered body and an optical element base substrate.
  • Patent Document 1 discloses that an oriented alumina sintered body produced using a plate-like alumina powder as part of a raw material exhibits excellent heat resistance and corrosion resistance.
  • Patent Document 1 Although a molded body using plate-like alumina powder as a part of the raw material is fired, the alumina purity is as low as less than 99.9% by mass and the firing temperature is as low as 1500 to 1750 ° C. Since it is fired under pressure, it is presumed that it is not sufficiently oriented. Moreover, since there is no description about translucency in patent document 1, it is estimated that the obtained oriented alumina sintered compact is opaque.
  • high-density polycrystalline alumina sintered body is known to exhibit translucency by reducing impurity concentration, arc tube for high-pressure sodium lamp, high heat-resistant window material, semiconductor device member, It is used for substrates for optical components.
  • this translucent alumina sintered body has been tried to control the crystal grain size or reduce the pores and impurity concentration, but the sufficient translucency is Not obtained.
  • One of the factors is birefringence derived from the crystal structure. It is known that the alumina sintered body has optical anisotropy in terms of crystal structure, and the translucency is limited when the orientation of polycrystalline alumina is low.
  • Non-Patent Document 1 translucency is improved by orienting a polycrystalline alumina sintered body by combining slip casting and magnetic field orientation.
  • the linear transmittance of the translucent alumina sintered body of Non-Patent Document 1 (in-line transmission is considered to be in-line transmission in Non-Patent Document 1), but is approximately 50 to 350-1000 nm. Only about 60%. For this reason, development of an alumina sintered body having better translucency has been desired.
  • the present invention has been made to solve such a problem, and has as its main object to provide an alumina sintered body having higher translucency than in the past.
  • This alumina sintered body is highly oriented because the degree of c-plane orientation is 90% or more, is high density because the number of pores is zero, and the total mass ratio of impurity elements other than Mg and C is 100 ppm. Since it is the following, it is highly pure. For this reason, the alumina sintered body of the present invention has higher translucency than conventional.
  • the base substrate for an optical element of the present invention is a substrate made of the above-described alumina sintered body of the present invention.
  • the optical element include LED, LD, solar cell, sensor, photodiode, optical member, window material and the like.
  • FIG. 2 is a schematic cross-sectional view of the light emitting element 10.
  • FIG. 2 is a schematic cross-sectional view of a horizontal light emitting element 20.
  • FIG. 4 is a schematic cross-sectional view showing a manufacturing process of the vertical light emitting device 30.
  • An appearance photograph of a sample of an alumina sintered body It is a schematic diagram of plate-like alumina particles, (a) is a plan view, (b) is a front view.
  • a high magnification photograph of a polished cross section of an alumina sintered body Explanatory drawing which shows a mode that the high magnification photograph was arranged so that it might become a continuous photograph.
  • the photograph which shows an example of the optical microscope image of the alumina sintered compact with a degranulation part.
  • the number of pores is zero when the cross section is polished by ion milling after being examined by ion milling, and the total mass ratio of impurity elements other than Mg and C is 100 ppm or less. It is.
  • the total mass ratio of impurity elements is the ICP (inductively coupled plasma) emission analysis, combustion (high frequency heating) -infrared absorption method, inert gas melting-thermal conductivity method, inert gas melting-non-described later. Quantitative values of elements detected by the dispersion-type infrared absorption method and thermal hydrolysis-ion chromatography were combined.
  • P is a value obtained from XRD of the alumina sintered body
  • P 0 is a value calculated from standard ⁇ -alumina (JCPDS card No. 46-1212).
  • the c-plane is the (006) plane of alumina.
  • the alumina sintered body of the present invention is a highly oriented alumina sintered body having a c-plane orientation degree of 90% or more.
  • the number of pores is counted as follows. That is, after polishing an arbitrary cross section of the alumina sintered body of the present invention by ion milling, the polished cross section is examined with a scanning electron microscope at a magnification of 5000 times, and the number of pores is counted. For example, a photograph obtained by enlarging a field of view of a length of 19.0 ⁇ m ⁇ 25.4 ⁇ m by a magnification of 5000 times with a scanning electron microscope on a polished electron microscope is continuous for 6 sheets in a vertical direction and 5 sheets in a horizontal direction (114 ⁇ m in length ⁇ 127 ⁇ m in width).
  • the reason for polishing by ion milling is that degranulation does not occur from the cross section.
  • An example of a polishing apparatus that uses ion milling is a cross section polisher manufactured by JEOL. Since the pores appear as black spots in the photograph magnified to a magnification of 5000 times, they can be sufficiently recognized visually.
  • the alumina sintered body of the present invention is a high-density alumina sintered body because the number of pores is zero.
  • Impurity elements (elements other than Mg and C in this case), depending on the element, ICP emission analysis, combustion (high-frequency heating)-infrared absorption method, thermal hydrolysis-ion chromatography, inert gas melting-thermal conductivity It can be quantified by adopting the method, inert gas melting-non-dispersive infrared absorption method.
  • S combustion (high-frequency heating)-infrared absorption method
  • N is inert gas melting-thermal conductivity method
  • H is inert gas melting-non-dispersive infrared absorption method
  • F thermal hydrolysis-ion chromatography method
  • Other elements can be quantified by ICP emission analysis.
  • the alumina sintered body of the present invention is a high-purity alumina sintered body because the total mass ratio of impurity elements other than Mg and C is 100 ppm or less.
  • the total mass ratio of the impurity elements is more preferably 50 ppm or less, and still more preferably 10 ppm or less.
  • the C content is preferably 30 to 70 ppm by mass.
  • C can be quantified by a combustion (high frequency heating) -infrared absorption method.
  • a combustion high frequency heating
  • the frequency at which the alumina particles shed from the surface is greatly reduced.
  • a film of a compound used for an optical element such as GaN is formed on the surface of the alumina sintered body after polishing, since the surface has almost no unevenness due to degranulation, the generated film is less likely to be defective. .
  • the alumina sintered body of the present invention preferably has an alumina content of 99.9% by mass or more.
  • the purity of alumina is determined by measuring the sum X of the mass% of impurity elements (including Mg and C in this case) in the sintered body and calculating 100-X.
  • the alumina sintered body of the present invention preferably has a linear transmittance of 70% or more at a wavelength of 350 to 1000 nm of a 0.2 mm thick sample taken out from the alumina sintered body.
  • the linear transmittance can be measured using a spectrophotometer (for example, Lambda 900, manufactured by Perkin Elmer).
  • Mg may be contained in a mass ratio of 1300 ppm or less (preferably 1150 ppm or less, more preferably 450 ppm or less, more preferably 120 ppm or less). This is because even when a light-emitting element such as an LED is produced using such an alumina sintered body, there is almost no influence of Mg.
  • the content of Mg is preferably 125 ppm or less by mass ratio.
  • Na flux is used, for example, when a film of GaN, AlN, InN or the like is formed on the alumina sintered body of the present invention by a flux method.
  • the alumina sintered body of the present invention When the alumina sintered body of the present invention is produced, the alumina is fired and sintered. If MgO is added to the alumina before sintering, densification proceeds due to the pore discharge effect of MgO during sintering. Therefore, it is preferable to add MgO to the mixed powder before sintering so that Mg contained in the alumina sintered body falls within the above-described mass ratio range.
  • the alumina sintered body of the present invention is preferably not eroded by Na flux when GaN or the like is formed by the Na flux method.
  • the degree of erosion of the alumina sintered body by the flux can be evaluated by the following method. From the minimum value of linear transmittance at a wavelength of 350 to 1000 nm of a 0.2 mm thick sample taken out from the alumina sintered body before being immersed in the Na flux, the sample after being immersed in Na flux at 870 ° C. in nitrogen for 120 hours. A value obtained by subtracting the minimum value of the linear transmittance at a wavelength of 350 to 1000 nm of a 0.2 mm thick sample taken out from the alumina sintered body is calculated. If this value is 5% or less, it can be said that it is difficult to be eroded by the flux. In other words, an alumina sintered body in which the above value is 5% or less is preferable.
  • the alumina sintered body of the present invention can be used as a base substrate for forming a film, for example, as a base substrate for forming a film of GaN, ZnO, AlN, SiC, InN or the like.
  • the alumina sintered body of the present invention is preferably mechanically polished before the film formation. In this way, since the surface unevenness is eliminated, it is easy to form a film and it is difficult to cause defects in the film. In the case of mechanical polishing, if particles having high hardness (for example, alumina particles) are used, there is a risk of detaching from the surface. Considering this point, it is preferable to use the alumina sintered body of the present invention that contains 30 to 70 ppm of C by mass. In this way, the frequency of grain removal by mechanical polishing can be greatly reduced.
  • the alumina sintered body of the present invention can be produced, for example, by molding and firing a mixed powder obtained by mixing a plate-like alumina powder and a fine alumina powder having an average particle size smaller than that of the plate-like alumina powder.
  • a mixed powder of plate-like alumina powder and fine alumina powder the plate-like particles are easily oriented during molding (tape molding, extrusion molding, casting molding, injection molding, uniaxial press molding, etc.).
  • the plate-like alumina powder becomes a seed crystal (template)
  • the fine alumina powder becomes a matrix
  • the template grows homoepitaxially while taking in the matrix.
  • TGG Temporated Grain Growth
  • the fine structure of the obtained alumina sintered body can be controlled by the particle size and mixing ratio of the plate-like alumina powder and the fine alumina powder, and it becomes denser than the case of firing the plate-like alumina powder alone. It is easy to improve the degree of orientation.
  • firing is performed by pressure firing (for example, hot press firing or HIP firing).
  • pressure firing for example, hot press firing or HIP firing
  • a capsule method can also be used.
  • the firing temperature is preferably 1750 to 2000 ° C.
  • the pressure is preferably 50 kgf / cm 2 or more in the case of the hot press firing, 200 kgf / cm 2 or more is more preferable.
  • Pressure when the HIP sintering is preferably 1000 kgf / cm 2 or more, 2,000 kgf / cm 2 or more is more preferable.
  • the content of the plate-like alumina powder in the mixed powder is not particularly limited and may be 100% by mass, but is preferably 0.1 to 50% by mass.
  • the content of the plate-like alumina powder is more preferably 0.1 to 15% by mass, still more preferably 0.5 to 5% by mass, and particularly preferably 1.5 to 5% by mass. By doing so, the degree of c-plane orientation obtained is sufficiently high, and the amount of expensive plate-like alumina used is relatively small, which is advantageous in terms of cost. Further, from the viewpoint of promoting densification, an appropriate amount of a sintering aid may be added to the mixed powder.
  • oxides such as MgO, ZrO 2 , Y 2 O 2 , CaO, SiO 2 , TiO 2 , Fe 2 O 3 , Mn 2 O 3 , La 2 O 3 , AlF 3 , MgF 2 , Examples thereof include at least one selected from fluorides such as YbF 3 . Of these, MgO, CaO, SiO 2 and La 2 O 3 are preferable, and MgO is particularly preferable. From the viewpoint of increasing the degree of orientation of the obtained alumina sintered body, the thickness of the particles constituting the plate-like alumina powder is preferably larger than the average particle size of the fine alumina powder particles.
  • the particle size of the plate surface of the plate-like particles constituting the plate-like alumina powder is preferably larger from the viewpoint of high orientation, preferably 1.5 ⁇ m or more, more preferably 5 ⁇ m or more, further preferably 10 ⁇ m or more, 15 ⁇ m or more is particularly preferable.
  • the particle size of the plate surface is small, and 30 ⁇ m or less is preferable.
  • the particle size of the plate surface is preferably 1.5 to 20 ⁇ m in order to achieve both high orientation and densification.
  • the purity of the plate-like alumina powder is preferably 99% by mass or more, more preferably 99.9% by mass or more, and further preferably 99.99% by mass or more.
  • an impurity element that volatilizes and disappears during firing may be included, and for example, an element such as F or S may be included.
  • High purity plate-like alumina powder can be produced by the following procedure. That is, first, at least one transition alumina powder selected from the group consisting of gibbsite, boehmite and ⁇ -alumina and AlF 3 powder are mixed so that the AlF 3 content is 0.25% by mass or more.
  • the total of elements other than Al, O, Mg, N, and Re (Re: rare earth element) is preferably 1% by mass or less.
  • the material of the container is preferably Al 2 O 3 having a purity of 99.5% by mass or more.
  • the mixed powder is put in a container and covered, or the mixed powder is put in a container and sealed, or the mixed powder is sealed in a container made of a porous material and heat treated at 750 to 1650 ° C.
  • a plate-like alumina powder composed of ⁇ -alumina particles is obtained.
  • a mixed powder obtained by mixing the plate-like alumina powder and the fine alumina powder may be molded and fired to obtain an alumina sintered body.
  • an alumina sintered body may be obtained by molding and firing a mixed powder obtained by mixing a plate-like alumina powder annealed at 900 to 1350 ° C. in the atmosphere, an inert atmosphere or a vacuum atmosphere, and fine alumina powder.
  • the plate-like alumina powder may be pulverized before mixing with the fine alumina powder.
  • the base substrate for an optical element of the present invention is a substrate made of the above-described alumina sintered body of the present invention.
  • the optical element include a light emitting element and a light receiving element.
  • a GaN layer on the base substrate for optical elements of the present invention, it can be used as a light-emitting substrate for LEDs and the like that is large and inexpensive compared to the case where sapphire is used for the base substrate. Since the base substrate for optical elements of the present invention has a high degree of orientation of alumina, a dense GaN layer can be formed. In addition to the GaN layer, a ZnO layer, an AlN layer, an InN layer, or the like can be formed.
  • the light emitting element 10 includes a base substrate 12 and a light emitting functional layer 14 formed on the base substrate 12.
  • the light emitting functional layer 14 emits light based on the light emission principle of the LED by applying a voltage.
  • the p-type layer 14a, the active layer 14b, and the n-type layer 14c are stacked in this order from the side close to the base substrate 12. ing.
  • the light emitting functional layer 14 is made of a GaN-based material, a ZnO-based material, an AlN-based material, or the like.
  • the horizontal light-emitting element 20 is formed on the outer periphery of the light-emitting functional layer 14 of the light-emitting element 10 so that the surface of the n-type layer 14c is a stepped surface, and on the stepped surface of the n-type layer 14c.
  • a cathode electrode 22 is attached, and an anode electrode pad 25 is provided on the surface of the p-type layer 14a via a translucent anode electrode 24.
  • the vertical light emitting element 30 has the mounting substrate 16 attached to the surface of the n-type layer 14c of the light emitting functional layer 14 via the cathode electrode 34 and the surface of the p-type layer 14a via the anode electrode 32.
  • the vertical light emitting element 30 is formed by forming an anode electrode 32 on the surface of the p-type layer 14a of the light emitting element 10, bonding the anode electrode 32 to the mounting substrate 16, and removing the base substrate 12 by a laser lift-off method.
  • the cathode electrode 34 is formed on the surface of the n-type layer 14c. According to the vertical light emitting element 30, a current flows in the normal direction of the light emitting functional layer 14.
  • the laser lift-off method can be used in this way because the base substrate 12 has a large linear transmittance and high translucency.
  • TM-300D high-purity ⁇ -alumina powder
  • IPA isopropyl alcohol
  • the total mass ratio of impurity elements other than F, H, C, and S contained in the obtained mixed powder was 1000 ppm or less.
  • 300 g of the obtained mixed powder was put in a sheath made of high-purity alumina having a purity of 99.5% by mass (volume: 750 cm 3 ), covered with a lid made of high-purity alumina having a purity of 99.5% by mass, and airflowing in an electric furnace. , 900 ° C. for 3 hours.
  • the air flow rate was 25000 cc / min.
  • the heat-treated powder was annealed in air at 1150 ° C.
  • the average particle diameter, average thickness, and aspect ratio of the particles were determined by observing 100 arbitrary particles in the plate-like alumina powder with a scanning electron microscope (SEM).
  • SEM scanning electron microscope
  • the average particle size is the average value of the major axis length of the particle plate surface
  • the average thickness is the average value of the minor axis length (thickness) of the particle
  • the aspect ratio is the average particle size / average thickness.
  • FIG. 6 is a schematic view of plate-like alumina particles, where (a) is a plan view and (b) is a front view.
  • the plate-like alumina particles have a substantially hexagonal shape when viewed in plan, the particle diameter is as shown in FIG. 6 (a), and the thickness is as shown in FIG. 6 (b).
  • the obtained plate-like alumina powder was ⁇ -alumina, and impurity elements other than F, C, and S were 10 ppm or less.
  • the mass proportion of F contained in the plate-like alumina powder was determined by a thermal hydrolysis-ion chromatography method and found to be 24 ppm.
  • the mass ratio of C and S was determined by combustion (high frequency heating) -infrared absorption method.
  • C was 240 ppm
  • S was below the detection limit
  • the purity of the plate-like alumina powder was 99.97% by mass. there were.
  • BM-2 manufactured by Sekisui Chemical Co., Ltd.
  • 7.8 parts by mass di (2-ethylhexyl) phthalate (manufactured by Kurokin Kasei) as a plasticizer, 3.9 parts by mass, and sorbitan trioleate (Leodol SP) as a dispersant -O30, manufactured by Kao Corporation) and 2-ethylhexanol as a dispersion medium were added and mixed.
  • the amount of the dispersion medium was adjusted so that the slurry viscosity was 20000 cP.
  • the slurry thus prepared was formed into a sheet shape on a PET film by a doctor blade method so that the thickness after drying was 20 ⁇ m.
  • the obtained tape was cut into a circular shape with a diameter of 50.8 mm (2 inches), then laminated 150 sheets, placed on an Al plate with a thickness of 10 mm, and then placed in a package to make the inside vacuum. Packed.
  • This vacuum pack was hydrostatically pressed at a pressure of 100 kgf / cm 2 in 85 ° C. warm water to obtain a disk-shaped molded body.
  • N inert gas melting-thermal conductivity method
  • H inert gas melting-non-dispersive infrared absorption method
  • F thermal hydrolysis-ion chromatography method other than the above Elements (mainly Si, Fe, Ti, Na, Ca, Mg, K, P, V, Cr, Mn, Co, Ni, Cu, Zn, Y, Zr, Pb, Bi, Li, Be, B, Cl, Sc, Ga, Ge, As, Se, Br, Rb, Sr, Nb, Mo, Ru, Rh, Pd, Ag, Cd, In, Sn, Sb, Te, Cs, Ba, Hf, Ta, W, Ir, Pt, Au, Hg, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu): ICP emission analysis
  • the Al 2 O 3 content (mass%) of the alumina sintered body was determined by 100-X by measuring the sum X of the mass% of elements other than Al and O in the sintered body in the above (2).
  • the Al 2 O 3 content of the alumina sintered body of Experimental Example 1 was 99.98% by mass.
  • alumina sintered body was cut into a size of 10 mm ⁇ 10 mm, and fixed to the outermost peripheral portion of a ⁇ 68 mm metal surface plate every 90 °, and on the SiC polishing paper, Lapping (preliminary polishing) was performed for 10 minutes at # 800 and for 5 minutes at # 1200 with only the load of the polishing jig applied (1314 g in total). Thereafter, lapping using diamond abrasive grains was performed on a ceramic surface plate. The lapping was performed at an abrasive grain size of 1 ⁇ m for 30 minutes and then at an abrasive grain size of 0.5 ⁇ m for 2 hours.
  • the 10 mm ⁇ 10 mm sintered body (sample) after polishing was washed with acetone, ethanol, and ion-exchanged water for 3 minutes in this order, and then optionally 20 with an optical microscope (Nikon, MM-60) at a magnification of 100 times. The location was observed and the number of sheddings was counted.
  • the alumina sintered body of Experimental Example 1 the number of samples in which degranulation occurred at 10 or more locations was 0 out of 20 (0/20).
  • An example of an optical microscope image of an alumina sintered body having a grain-removal portion is shown in FIG.
  • the obtained alumina sintered body was examined for corrosion resistance against Na flux, equivalent to the actual GaN growth conditions.
  • the alumina sintered body was placed at the bottom of a cylindrical flat bottom alumina crucible having an inner diameter of 80 mm and a height of 45 mm, and then the melt composition was filled in the crucible in a glove box.
  • the composition of the melt composition was 60 g of metal Ga, 60 g of metal Na, and 1.85 g of germanium tetrachloride.
  • the alumina crucible was placed in a refractory metal container and sealed, and then placed on a table where the crystal growth furnace could be rotated. After raising the temperature and pressure to 870 ° C.
  • the solution was rotated while maintaining for 120 hours. Then, it was gradually cooled to room temperature over 3 hours, and the container was taken out from the crystal growth furnace.
  • the surface of the alumina sintered body after the corrosion resistance test was ultrasonically cleaned with ethanol, and then the linear transmittance was measured in the same manner as in (5) above. After the corrosion resistance test of the alumina sintered body of Experimental Example 1, the linear transmittance at a wavelength of 350 to 1000 nm was 72.6% or more.
  • Example 2 In producing an alumina sintered body, the following points are set to 1.
  • an alumina sintered body was produced in the same manner as in Experimental Example 1 except that HIP firing was employed after performing atmospheric pressure atmospheric firing instead of hot pressing.
  • the conditions for atmospheric pressure atmospheric firing were held at 1350 ° C. for 4 hours.
  • the HIP firing conditions were such that Ar was used as a pressure medium and the pressure was maintained at 1800 ° C. for 2 hours at 185 MPa.
  • the characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 3 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that 1.5 parts by mass of the plate-like alumina powder and 98.5 parts by mass of the fine granular alumina powder were used in the tape molding of (2). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 4 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that the firing holding time was 2 hours in the firing of (3). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 5 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that the firing holding time was 8 hours in the firing of (3). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 6 In producing an alumina sintered body, the following points are set to 1. In Example 2 except that 60 mass ppm of SiO 2 powder and 60 mass ppm of CaO powder were added in addition to magnesium oxide powder as a sintering aid to 100 mass parts of the mixed alumina powder in the tape molding of (2). Similarly, an alumina sintered body was produced. About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 7 In producing an alumina sintered body, the following points are set to 1. In Example 2 except for adding 120 mass ppm of SiO 2 powder and 120 mass ppm of CaO powder in addition to magnesium oxide powder as a sintering aid to 100 mass parts of the mixed alumina powder in the tape molding of (2), Similarly, an alumina sintered body was produced. About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 8 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1, except that a commercially available plate-like alumina powder (YFA10030, manufactured by Kinsei Matech) was used instead of the plate-like alumina powder produced in (1). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 9 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that the firing temperature was set to 1700 ° C. in the firing of (3). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 10 In producing an alumina sintered body, the following points are set to 1. In the firing of (3), an alumina sintered body was produced in the same manner as in Experimental Example 1 except that the firing temperature was 1700 ° C. in atmospheric pressure. About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 11 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that the firing temperature was 1900 ° C. in the firing of (3). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 12 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1, except that 0.25 parts by mass of magnesium oxide was added to 100 parts by mass of the mixed alumina powder in the tape molding of (2). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 13 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1, except that 0.015 parts by mass of graphite powder was added to 100 parts by mass of the mixed alumina powder in the tape molding of (2). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 14 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1, except that 0.005 parts by mass of graphite powder was added to 100 parts by mass of the mixed alumina powder in the tape molding of (2). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • Example 15 In producing an alumina sintered body, the following points are set to 1. An alumina sintered body was produced in the same manner as in Experimental Example 1 except that 0.02 parts by mass of graphite powder was added to 100 parts by mass of the mixed alumina powder in the tape molding of (2). About the obtained alumina sintered body, the above 2. The characteristics (1) to (7) were determined. The results are shown in Table 1.
  • the c-plane orientation degree was 90% or more, the number of pores was 0, and the total of impurity elements other than Mg and C was 100 ppm or less.
  • the C content was 30 to 70 ppm, the Mg content was 125 ppm or less, and the linear transmittance at 350 to 1000 nm before immersion of Na flux was 70% or more. Further, the decrease amount of the minimum value of the linear transmittance at 350 to 1000 nm before and after the Na flux immersion was 5% or less. Little shedding was observed.
  • the alumina sintered body of Experimental Example 7 had a c-plane orientation degree of 90% or more, a C content of 30 to 70 ppm, and a Mg content of 125 ppm or less.
  • the total of impurity elements exceeded 100 ppm, and the linear transmittance at 350 to 1000 nm before immersion of Na flux was 25.6% or more. This is considered to be caused by an excessive amount of SiO 2 or CaO added.
  • the alumina sintered body of Experimental Example 8 had a c-plane orientation degree of 90% or more, a C content of 30 to 70 ppm, a Mg content of 125 ppm or less, and 0 pores.
  • the total of impurity elements exceeded 100 ppm, and the linear transmittance at 350 to 1000 nm before immersion of Na flux was 1.1% or more. This is thought to be due to the use of commercially available plate-like alumina powder.
  • the alumina sintered bodies of Experimental Examples 9 and 10 had a c-plane orientation degree as low as 30.7 to 70.7%, and a linear transmittance at 350 to 1000 nm before immersion of Na flux was as low as 0%. This is thought to be because the firing temperature after tape molding was not appropriate.
  • the alumina sintered bodies of Experimental Examples 11 to 13 had a c-plane orientation degree of 90% or more, 0 pores, and no impurity elements other than Mg and C.
  • the C content was 30 to 70 ppm
  • the linear transmittance at 350 to 1000 nm before immersion of Na flux was 60% or more (Experimental Examples 11 and 13 were 70% or more), and almost no degranulation was observed.
  • the alumina sintered body of Experimental Example 12 had a high Mg content of 1132 ppm, the linear transmittance at 350 to 1000 nm after immersion in Na flux was zero.
  • the alumina sintered bodies of Experimental Examples 14 and 15 had a c-plane orientation degree of 90% or more, 0 pores, and no impurity elements other than Mg and C. Further, the Mg content was 125 ppm or less, and the linear transmittance before immersion of Na flux was 70% or more. Furthermore, the amount of decrease in linear transmittance before and after immersion in Na flux was 5% or less. However, since the C content was 20 ppm and 80 ppm, a relatively large amount of degranulation was observed.
  • Experimental Examples 1 to 15 correspond to the examples of the present invention.
  • the present invention is not limited to these examples, and can be carried out in various modes as long as they belong to the technical scope of the present invention.
  • the present invention can be used for, for example, a base substrate for an optical element.
  • the optical element include LED, LD, solar cell, sensor, photodiode, optical member, window material and the like.

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Abstract

　本発明のアルミナ焼結体は、板面に対してＸ線を照射したときの２θ＝２０°～７０°の範囲におけるＸ線回折プロファイルを用いてロットゲーリング法により求めたｃ面配向度が９０％以上であり、板面と垂直な方向で切断した断面をＡｒ+イオンビームと遮蔽板を用いて研磨したあと走査型電子顕微鏡にて倍率５０００倍で調べたときの気孔の数がゼロであり、Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下のものである。このアルミナ焼結体は、高配向、高密度、高純度であるため、従来に比べて高い透光性を有している。

Description

アルミナ焼結体及び光学素子用下地基板
　本発明は、アルミナ焼結体及び光学素子用下地基板に関する。
　機械的強度や絶縁性、耐熱衝撃性、耐食性に優れた材料として、多結晶アルミナ（Ａｌ2Ｏ3）焼結体が広く用いられている。この多結晶アルミナ焼結体は、微細構造を制御することで構成粒子の結晶方位を特定方位に揃える（配向させる）ことで機械的強度や耐熱衝撃性、耐食性が向上することが知られている。これは、破壊靱性や誘電率、熱伝導率、熱膨張率に結晶方位による異方性があるためである。例えば、特許文献１では、板状アルミナ粉末を原料の一部に用いて作製した配向アルミナ焼結体が優れた耐熱性や耐食性を示すことが開示されている。特許文献１では、板状アルミナ粉末を原料の一部に用いた成形体を焼成しているものの、アルミナ純度が９９．９質量％未満と低い上、焼成温度が１５００～１７５０℃と低くしかも常圧で焼成しているため、十分に配向していないと推測される。また、特許文献１には、透光性について記載がないことから、得られた配向アルミナ焼結体は不透明なものと推測される。
　一方、高密度の多結晶アルミナ焼結体は、不純物濃度を低減することにより透光性が発現することが知られており、高圧ナトリウムランプ用発光管や高耐熱窓材、半導体装置用部材、光学部品用基板等に用いられている。この透光性アルミナ焼結体は、透光性を向上させるために、結晶粒径を制御したり気孔や不純物濃度を低減したりすることが試され得ているが、十分な透光性は得られていない。その要因の一つに、結晶構造に由来する複屈折が挙げられる。アルミナ焼結体は、結晶構造上、光学的異方性を持っており、多結晶アルミナの配向性が低い場合には、透光性が制限されることが知られている。例えば、非特許文献１では、多結晶アルミナ焼結体をスリップキャストと磁場配向とを組み合わせることで配向させることにより、透光性を向上させている。
特許第２９１６６６４号
Journal of American Ceramic Society 91[10] pp3431-3433(2008)
　しかしながら、非特許文献１の透光性アルミナ焼結体の直線透過率（非特許文献１にはin-line transmissionとあるが正しくはin-line transmittanceと思われる）は３５０～１０００ｎｍで概ね５０～６０％程度しかない。そのため、より透光性の優れたアルミナ焼結体の開発が望まれていた。
　本発明はこのような課題を解決するためになされたものであり、従来より透光性の高いアルミナ焼結体を提供することを主目的とする。
　本発明のアルミナ焼結体は、Ｘ線を照射したときの２θ＝２０°～７０°の範囲におけるＸ線回折プロファイルを用いてロットゲーリング法により求めたｃ面配向度が９０％以上の面を有し、任意の断面をイオンミリングによって研磨したあと走査型電子顕微鏡にて倍率５０００倍で調べたときの気孔の数がゼロであり，Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下のものである。このアルミナ焼結体は、ｃ面配向度が９０％以上であるため高配向であり、気孔の数がゼロであるため高密度であり、Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下であるため高純度である。そのため、本発明のアルミナ焼結体は、従来に比べて高い透光性を有している。
　本発明の光学素子用下地基板は、上述した本発明のアルミナ焼結体からなる基板である。光学素子としては、例えばＬＥＤ、ＬＤ、太陽電池、センサ、フォトダイオード、光学部材、窓材等が挙げられる。
ＴＧＧ法でアルミナ焼結体を作製する工程の模式図。 発光素子１０の概略断面図。 横型発光素子２０の概略断面図。 縦型発光素子３０の製造工程を示す概略断面図。 アルミナ焼結体のサンプルの外観写真。 板状アルミナ粒子の模式図であり、（ａ）は平面図、（ｂ）は正面図。 アルミナ焼結体の研磨された断面の高倍率写真。 高倍率写真を連続的な写真となるように並べた様子を示す説明図。 脱粒部のあるアルミナ焼結体の光学顕微鏡像の一例を示す写真。
　本発明のアルミナ焼結体は、Ｘ線を照射したときの２θ＝２０°～７０°の範囲におけるＸ線回折プロファイルを用いてロットゲーリング法により求めたｃ面配向度が９０％以上の面を有し、任意の断面をイオンミリングによって研磨したあと走査型電子顕微鏡にて倍率５０００倍で調べたときの気孔の数がゼロであり、Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下である。なお、本発明では不純物元素の質量割合の合計は後述するＩＣＰ（誘導結合プラズマ）発光分析、燃焼（高周波加熱）－赤外線吸収法、不活性ガス融解－熱伝導度法、不活性ガス融解－非分散型赤外線吸収法、熱加水分解－イオンクロマトグラフ法で検出された元素の定量値を合算したものとした。
　ｃ面配向度は、ＸＲＤ装置（例えばリガク製、ＲＩＮＴ－ＴＴＲ　ＩＩＩ）を用いてアルミナ焼結体の所定の断面（例えばｃ面に平行な断面）を平滑に研磨加工した後、その面に対してＸ線を照射したときの２θ＝２０°～７０°の範囲におけるＸ線回折プロファイルを用いて、以下の式により算出する。式中、Ｐはアルミナ焼結体のＸＲＤから得られた値であり、Ｐ0は標準α－アルミナ（ＪＣＰＤＳカードＮｏ．４６－１２１２）から算出された値である。ｃ面とはアルミナの（００６）面である。本発明のアルミナ焼結体は、ｃ面配向度が９０％以上の高配向なアルミナ焼結体である。
Figure JPOXMLDOC01-appb-M000001
　気孔の数は、以下のようにしてカウントする。すなわち、本発明のアルミナ焼結体の任意の断面をイオンミリングによって研磨したあと、その研磨した断面を走査型電子顕微鏡にて倍率５０００倍で調べて、気孔の数をカウントする。例えば、研磨した断面を走査型電子顕微鏡にて縦１９．０μｍ×横２５．４μｍの視野を５０００倍に拡大した写真を、縦６枚分、横５枚分（縦１１４μｍ×横１２７μｍ）で連続的な写真となるように３０枚撮影し、その３０枚について気孔の数を目視でカウントする。イオンミリングによって研磨するのは、断面から脱粒が生じないからである。なお、イオンミリングを用いる研磨装置としては、例えば、日本電子製のクロスセクションポリッシャが挙げられる。倍率５０００倍に拡大した写真では気孔は黒点として現れるため、目視で十分認識することができる。本発明のアルミナ焼結体は、気孔の数がゼロであるため高密度なアルミナ焼結体である。
　不純物元素（ここではＭｇ，Ｃ以外の元素）は、元素に応じて、ＩＣＰ発光分析、燃焼（高周波加熱）－赤外線吸収法、熱加水分解－イオンクロマトグラフ法、不活性ガス融解－熱伝導度法、不活性ガス融解－非分散型赤外線吸収法を採用して定量することができる。例えば、Ｓは燃焼（高周波加熱）－赤外線吸収法、Ｎは不活性ガス融解－熱伝導度法、Ｈは不活性ガス融解－非分散型赤外線吸収法、Ｆは熱加水分解－イオンクロマトグラフ法、その他の元素はＩＣＰ発光分析で定量することができる。本発明のアルミナ焼結体は、Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下であるため、高純度のアルミナ焼結体である。不純物元素の合計の質量割合は５０ｐｐｍ以下がより好ましく、１０ｐｐｍ以下が更に好ましい。
　本発明のアルミナ焼結体において、Ｃの含有量は質量割合で３０～７０ｐｐｍであることが好ましい。Ｃは、燃焼（高周波加熱）－赤外線吸収法により定量することができる。こうすれば、このアルミナ焼結体の表面を凹凸のないように砥粒を用いて研磨加工した場合に、表面からアルミナ粒子が脱粒する頻度が大幅に低減される。例えば、このアルミナ焼結体の研磨加工後の表面にＧａＮなどの光学素子に用いられる化合物の膜を生成する場合、脱粒に起因する凹凸が表面にほとんどないため、生成した膜に欠陥が生じにくい。
　本発明のアルミナ焼結体は、アルミナ含有量が９９．９質量％以上であることが好ましい。アルミナの純度は、便宜上、焼結体中の不純物元素（ここではＭｇ，Ｃを含む）の質量％の和Ｘを測定し、１００－Ｘにより求めることとする。
　本発明のアルミナ焼結体は、該アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率が７０％以上であることが好ましい。このように透光性の高いアルミナ焼結体は従来知られていないため種々の分野で利用されることが期待される。直線透過率は、分光光度計（例えばＰｅｒｋｉｎ　Ｅｌｍｅｒ製、Ｌａｍｂｄａ９００）を用いて測定することができる。
　本発明のアルミナ焼結体において、Ｍｇは質量割合で１３００ｐｐｍ以下（好ましくは１１５０ｐｐｍ以下、より好ましくは４５０ｐｐｍ以下、更に好ましくは１２０ｐｐｍ以下）含まれていてもよい。こうしたアルミナ焼結体を用いてＬＥＤ等の発光素子を作製してもＭｇの影響がほとんどないからである。但し、Ｎａフラックスに対する耐食性の観点からは、Ｍｇの含有量は質量割合で１２５ｐｐｍ以下であることが好ましい。Ｎａフラックスは、例えば、本発明のアルミナ焼結体上にＧａＮやＡｌＮ、ＩｎＮなどの膜をフラックス法で形成する際に利用される。本発明のアルミナ焼結体を作製する際にはアルミナを焼成して焼結させるが、焼結前にアルミナにＭｇＯを添加すれば、焼結時にＭｇＯの気孔排出効果により緻密化が進む。そのため、アルミナ焼結体に含まれるＭｇが上述した質量割合の範囲に収まるように、焼結前にＭｇＯを混合粉末に添加するのが好ましい。
　本発明のアルミナ焼結体は、Ｎａフラックス法によりＧａＮなどを成膜する場合、Ｎａフラックスにより浸食されないことが好ましい。フラックスによるアルミナ焼結体の浸食の程度は下記のような手法で評価することができる。Ｎａフラックスに浸漬する前の前記アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率の最小値から、窒素中８７０℃のＮａフラックスに１２０時間浸漬した後の前記アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率の最小値を差し引いた値を算出する。この値が５％以下であるとフラックスによって浸食されにくいということができる。言い換えると、上記の値が５％以下となるようなアルミナ焼結体が好ましい。
　本発明のアルミナ焼結体は、膜を形成するための下地基板として利用可能であり、例えば、ＧａＮ，ＺｎＯ，ＡｌＮ，ＳｉＣ，ＩｎＮなどを成膜するための下地基板として利用可能である。本発明のアルミナ焼結体は、成膜する前に表面を機械研磨することが好ましい。こうすれば、表面の凹凸がなくなるため、成膜しやすいし膜に欠陥が生じにくい。機械研磨の際、硬度の高い粒子（例えばアルミナ粒子）を用いると表面から脱粒するおそれがある。この点を考慮して、本発明のアルミナ焼結体としてＣが質量割合で３０～７０ｐｐｍ含まれるものを利用することが好ましい。こうすれば、機械研磨による脱粒の頻度を大幅に低減することができる。
　本発明のアルミナ焼結体は、例えば、板状アルミナ粉末と平均粒径が板状アルミナ粉末よりも小さい微細アルミナ粉末とを混合した混合粉末を成形、焼成することにより製造することができる。板状アルミナ粉末と微細アルミナ粉末の混合粉末を成形することにより、成形時（テープ成形、押出成形、鋳込み成形、射出成形、一軸プレス成形等）に板状粒子が配向しやすくなる。また、焼成時に、板状アルミナ粉末が種結晶（テンプレート）となり、微細アルミナ粉末がマトリックスとなって、テンプレートがマトリックスを取り込みながらホモエピタキシャル成長する。こうした製法は、ＴＧＧ（Ｔｅｍｐｌａｔｅｄ　Ｇｒａｉｎ　Ｇｒｏｗｔｈ）法と呼ばれる。ＴＧＧ法でアルミナ焼結体を作製する工程の模式図を図１に示す。ＴＧＧ法では、板状アルミナ粉末と微細アルミナ粉末の粒径や混合比によって、得られるアルミナ焼結体の微細構造を制御することができ、板状アルミナ粉末単体を焼成する場合に比べて緻密化しやすく、配向度が向上しやすい。
　ＴＧＧ法では、加圧焼成（例えばホットプレス焼成やＨＩＰ焼成など）にて焼成する。なお、加圧焼成前に常圧予備焼成を行ってもよい。ＨＩＰ焼成を行うときにはカプセル法を用いることもできる。焼成温度は１７５０～２０００℃が好ましい。ホットプレス焼成の場合の圧力は５０ｋｇｆ／ｃｍ2以上が好ましく、２００ｋｇｆ／ｃｍ2以上がより好ましい。ＨＩＰ焼成の場合の圧力は１０００ｋｇｆ／ｃｍ2以上が好ましく、２０００ｋｇｆ／ｃｍ2以上がより好ましい。混合粉末中の板状アルミナ粉末の含有量は、特に限定されるものではなく、１００質量％でもよいが、０．１～５０質量％が好ましい。０．１質量％未満だと得られるアルミナ焼結体のｃ面配向度が高くなりにくく、５０質量％を超えるとアルミナが焼結しにくくなるおそれがあるからである。板状アルミナ粉末の含有量は、０．１～１５質量％がより好ましく、０．５～５質量％が更に好ましく、１．５～５質量％が特に好ましい。こうすれば、得られるｃ面配向度が十分高くなるし、高価な板状アルミナの使用量が比較的少ないためコスト的に有利である。また、緻密化を進める観点では、混合粉末に焼結助剤を適量添加してもよい。焼結助剤としては、ＭｇＯ、ＺｒＯ2、Ｙ2Ｏ2、ＣａＯ、ＳｉＯ2、ＴｉＯ2、Ｆｅ2Ｏ3、Ｍｎ2Ｏ3、Ｌａ2Ｏ3等の酸化物、ＡｌＦ3、ＭｇＦ2、ＹｂＦ3等のフッ化物などから選ばれる少なくとも１種が挙げられる。このうち、ＭｇＯ、ＣａＯ、ＳｉＯ2、Ｌａ2Ｏ3が好ましく、ＭｇＯが特に好ましい。得られるアルミナ焼結体の配向度を上げるという観点からすると、板状アルミナ粉末を構成する粒子の厚みは微細アルミナ粉末の粒子の平均粒径より大きいことが好ましい。また、板状アルミナ粉末を構成する板状粒子の板面の粒径は高配向化の観点からは大きい方が好ましく、１．５μｍ以上が好ましく、５μｍ以上がより好ましく、１０μｍ以上が更に好ましく、１５μｍ以上が特に好ましい。但し、緻密化の観点では板面の粒径が小さい方が好ましく、３０μｍ以下が好ましい。こうしたことから、高配向と緻密化を両立するには板面の粒径が１．５～２０μｍであることが好ましい。
　ここで、板状アルミナ粉末は高純度のものを用いることが好ましい。板状アルミナ粉末の純度は９９質量％以上が好ましく、９９．９質量％以上がより好ましく、９９．９９質量％以上が更に好ましい。但し、焼成中に揮発消失する不純物元素は含んでいてもよく、例えばＦやＳなどの元素は含まれていてもよい。高純度の板状アルミナ粉末は、以下の手順で製造することができる。すなわち、まず、ギブサイト、ベーマイト及びγ－アルミナからなる群より選ばれる少なくとも１種の遷移アルミナ粉末とＡｌＦ3粉末とを、ＡｌＦ3の含有率が０．２５質量％以上となるように混合して、Ｆ，Ｈ，Ｃ，Ｓ以外の不純物元素の質量割合の合計が１０００ｐｐｍ以下の混合粉末を得る。この混合粉末中に種結晶としてα－アルミナ粒子を添加することが好ましい。次に、容器として、混合粉末に含まれるＡｌＦ3の質量を容器の体積で除した値（＝ＡｌＦ3質量／容器体積）が１×１０-4ｇ／ｃｍ3以上になるものを用意する。容器は、Ａｌ，Ｏ，Ｍｇ，Ｎ，Ｒｅ（Ｒｅ：希土類元素）以外の元素の合計が１質量％以下であることが好ましい。容器の材質は、純度９９．５質量％以上のＡｌ2Ｏ3が好ましい。そして、混合粉末を容器に入れて蓋をするか、混合粉末を容器に入れて密閉するか、又は混合粉末を多孔質材料からなる容器に閉じ込め、７５０～１６５０℃で熱処理することにより板状のα－アルミナ粒子で構成された板状アルミナ粉末を得る。この板状アルミナ粉末と微細アルミナ粉末とを混合した混合粉末を成形、焼成してアルミナ焼結体としてもよい。あるいは、板状アルミナ粉末を大気、不活性又は真空の雰囲気下で９００～１３５０℃でアニール処理したものと微細アルミナ粉末とを混合した混合粉末を成形、焼成してアルミナ焼結体としてもよい。板状アルミナ粉末は、微細アルミナ粉末と混合する前に粉砕してもよい。
　本発明の光学素子用下地基板は、上述した本発明のアルミナ焼結体からなる基板である。光学素子としては、発光素子や受光素子が挙げられる。例えば、本発明の光学素子用下地基板にＧａＮ層を成膜することで、サファイアを下地基板に用いた場合に比べて大型で安価なＬＥＤ等の発光基板として用いることができる。本発明の光学素子用下地基板は、アルミナの配向度が高いため緻密なＧａＮ層を形成することができる。なお、ＧａＮ層のほかにＺｎＯ層，ＡｌＮ層，ＩｎＮ層なども形成することができる。
　本発明の光学素子用下地基板を発光素子に利用した例を以下に示す。発光素子１０は、図２に示すように、下地基板１２と、下地基板１２上に形成された発光機能層１４とを備えている。発光機能層１４は、電圧を印加することによりＬＥＤの発光原理に基づき発光するものであり、ここでは下地基板１２に近い側からｐ型層１４ａ、活性層１４ｂ、ｎ型層１４ｃの順に積層されている。この発光機能層１４は、ＧａＮ系材料、ＺｎＯ系材料、ＡｌＮ系材料などで作製されている。
　横型発光素子２０は、図３に示すように、発光素子１０のうち発光機能層１４の外周部にｎ型層１４ｃの表面が段差面となるように形成され、ｎ型層１４ｃの段差面にカソード電極２２が取り付けられ、ｐ型層１４ａの表面に透光性アノード電極２４を介してアノード電極パッド２５が設けられたものである。この横型発光素子２０によれば、発光機能層１４の法線方向だけでなく、水平方向にも電流が流れる。
　縦型発光素子３０は、図４に示すように、発光機能層１４のｎ型層１４ｃの表面にカソード電極３４、ｐ型層１４ａの表面にアノード電極３２を介して実装基板１６が取り付けられたものである。この縦型発光素子３０は、発光素子１０のｐ型層１４ａの表面にアノード電極３２を形成し、実装基板１６にアノード電極３２を接合し、下地基板１２をレーザリフトオフ法で除去し、露出したｎ型層１４ｃの表面にカソード電極３４を形成することにより作製される。この縦型発光素子３０によれば、発光機能層１４の法線方向に電流が流れる。このようにレーザリフトオフ法が利用できるのは、下地基板１２の直線透過率が大きく透光性が高いからである。
［実験例１］
１．アルミナ焼結体の作製
（１）板状アルミナ粉末の作製
　高純度γ－アルミナ粉末（ＴＭ－３００Ｄ、大明化学製）９６質量部と、高純度ＡｌＦ3粉末（関東化学製、鹿特級）４質量部と、種結晶として高純度α－アルミナ粉末（ＴＭ－ＤＡＲ、大明化学製、Ｄ５０＝１μｍ）０．１７質量部とを、溶媒をＩＰＡ（イソプロピルアルコール）としてφ２ｍｍのアルミナボールを用いて５時間ポットミルで混合した。得られた混合粉末中に含まれるＦ，Ｈ，Ｃ，Ｓ以外の不純物元素の質量割合の合計は１０００ｐｐｍ以下であった。得られた混合粉末３００ｇを純度９９．５質量％の高純度アルミナ製のさや（容積７５０ｃｍ3）に入れ、純度９９．５質量％の高純度アルミナ製の蓋をして電気炉内でエアフロー中、９００℃、３時間熱処理した。エアの流量は２５０００ｃｃ／ｍｉｎとした。熱処理後の粉末を大気中、１１５０℃で４０時間アニール処理した後、φ２ｍｍのアルミナボールを用いて４時間粉砕して平均粒径２μｍ、厚み０．２μｍ、アスペクト比１０の板状アルミナ粉末を得た。粒子の平均粒径、平均厚み、アスペクト比は、走査型電子顕微鏡（ＳＥＭ）で板状アルミナ粉末中の任意の粒子１００個を観察して決定した。平均粒径は、粒子板面の長軸長の平均値、平均厚みは、粒子の短軸長（厚み）の平均値、アスペクト比は、平均粒径／平均厚みである。図６は、板状アルミナ粒子の模式図であり、（ａ）は平面図、（ｂ）は正面図である。板状アルミナ粒子は、平面視したときの形状が略六角形状であり、その粒径は図６（ａ）に示したとおりであり、厚みは図６（ｂ）に示したとおりである。得られた板状アルミナ粉末は、α－アルミナであり、Ｆ，Ｃ，Ｓ以外の不純物元素は１０ｐｐｍ以下であった。この板状アルミナ粉末中に含まれるＦの質量割合を、熱加水分解－イオンクロマトグラフ法により求めたところ、２４ｐｐｍであった。また、Ｃ，Ｓの質量割合を、燃焼（高周波加熱）－赤外線吸収法で求めたところ、Ｃは２４０ｐｐｍ、Ｓは検出限界以下であり、この板状アルミナ粉末の純度は９９．９７質量％であった。
（２）テープ成形
　上記（１）で作製した板状アルミナ粉末５質量部と、微細アルミナ粉末（ＴＭ－ＤＡＲ、平均粒径０．１μｍ、大明化学製）９５質量部とを混合した。この混合アルミナ粉末１００質量部に対し、酸化マグネシウム（５００Ａ、宇部マテリアルズ製）０．０２５質量部と、グラファイト粉末（ＵＦ－Ｇ５、昭和電工製）０．０１質量部と、バインダーとしてポリビニルブチラール（品番ＢＭ－２、積水化学工業製）７．８質量部と、可塑剤としてジ（２－エチルヘキシル）フタレート（黒金化成製）３．９質量部と、分散剤としてトリオレイン酸ソルビタン（レオドールＳＰ－Ｏ３０、花王製）２質量部と、分散媒として２－エチルヘキサノールとを加えて混合した。分散媒の量は、スラリー粘度が２００００ｃＰとなるように調整した。このようにして調製されたスラリーを、ドクターブレード法によってＰＥＴフィルムの上に乾燥後の厚さが２０μｍとなるようにシート状に成形した。得られたテープを口径５０．８ｍｍ（２インチ）の円形に切断した後１５０枚積層し、厚さ１０ｍｍのＡｌ板の上に載置した後、パッケージに入れて内部を真空にすることで真空パックとした。この真空パックを８５℃の温水中で１００ｋｇｆ／ｃｍ2の圧力にて静水圧プレスを行い、円板状の成形体を得た。
（３）焼成
　得られた成形体を脱脂炉中に配置し、６００℃で１０時間の条件で脱脂を行った。得られた脱脂体を黒鉛製の型を用い、ホットプレスにて窒素中１８００℃で４時間、面圧２００ｋｇｆ／ｃｍ2の条件で焼成し、アルミナ焼結体を得た。得られたアルミナ焼結体のサンプルの外観写真を図５に示した。図５に描かれたＮＧＫのロゴ入りマークは日本碍子（株）の登録商標である。
２．アルミナ焼結体の特性
（１）ｃ面配向度の算出
　得られたアルミナ焼結体の配向度を確認するため、ＸＲＤによりｃ面配向度を測定した。円板状のアルミナ焼結体の上面に対して平行になるように研磨加工した後、その研磨面に対してＸＲＤ装置（リガク製、ＲＩＮＴ－ＴＴＲ　ＩＩＩ）を用いてＸ線を照射したときの２θ＝２０～７０°の範囲でＸＲＤプロファイルを測定した。具体的には、ＣｕＫα線を用いて電圧５０ｋＶ、電流３００ｍＡという条件で測定した。ｃ面配向度は、ロットゲーリング法によって算出した。具体的には、以下の式により算出した。実験例１のアルミナ焼結体のｃ面配向度は９９．７％であった。
Figure JPOXMLDOC01-appb-M000002
（２）純度－その１
　アルミナ焼結体を純度９９．９％のアルミナ乳鉢で粉砕した後、Ａｌ，Ｏ以外の元素について、下記方法により定量分析した。そして、アルミナ焼結体中のＭｇ，Ｃ以外の不純物元素の合計の質量割合（ｐｐｍ）、アルミナ焼結体に含まれるＭｇ，Ｃそれぞれの質量割合（ｐｐｍ）を求めた。実験例１のアルミナ焼結体のＭｇ，Ｃ以外の不純物元素は、いずれも含まれておらず（検出限界以下）、Ｍｇが１１２ｐｐｍ、Ｃが４０ｐｐｍ検出された。
　Ｃ，Ｓ：燃焼（高周波加熱）－赤外線吸収法
　Ｎ：不活性ガス融解－熱伝導度法
　Ｈ：不活性ガス融解－非分散型赤外線吸収法
　Ｆ：熱加水分解－イオンクロマトグラフ法
　上記以外の元素（主にＳｉ，Ｆｅ，Ｔｉ，Ｎａ，Ｃａ，Ｍｇ，Ｋ，Ｐ，Ｖ，Ｃｒ，Ｍｎ，Ｃｏ，Ｎｉ，Ｃｕ，Ｚｎ，Ｙ，Ｚｒ，Ｐｂ，Ｂｉ，Ｌｉ，Ｂｅ，Ｂ，Ｃｌ，Ｓｃ，Ｇａ，Ｇｅ，Ａｓ，Ｓｅ，Ｂｒ，Ｒｂ，Ｓｒ，Ｎｂ，Ｍｏ，Ｒｕ，Ｒｈ，Ｐｄ，Ａｇ，Ｃｄ，Ｉｎ，Ｓｎ，Ｓｂ，Ｔｅ，Ｃｓ，Ｂａ，Ｈｆ，Ｔａ，Ｗ，Ｉｒ，Ｐｔ，Ａｕ，Ｈｇ，Ｌａ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｔｂ，Ｄｙ，Ｈｏ，Ｅｒ，Ｔｍ，Ｙｂ，Ｌｕ）：ＩＣＰ発光分析
（３）純度－その２
　アルミナ焼結体のＡｌ2Ｏ3含有量（質量％）は、上記（２）で焼結体中のＡｌ，Ｏ以外の元素の質量％の和Ｘを測定し、１００－Ｘにより求めた。実験例１のアルミナ焼結体のＡｌ2Ｏ3含有量は９９．９８質量％であった。
（４）気孔（密度）
　得られたアルミナ焼結体の任意の断面をクロスセクションポリッシャ（ＣＰ）（日本電子製、ＩＢ－０９０１０ＣＰ）で研磨した。ＣＰはイオンミリングの範疇に属する。ＣＰを用いたのは、研磨面に脱粒が生じないからである。得られた断面を走査型電子顕微鏡（日本電子製、ＪＳＭ－６３９０）にて撮影した。具体的には、図７のような縦１９．０μｍ×横２５．４μｍの視野を倍率５０００倍で撮影した写真を、図８のように縦６枚分、横５枚分連続的な写真（縦１１４μｍ×横１２７μｍ）となるように並べ、目視により気孔の数をカウントした。気孔と気孔でない部分とは、明暗がはっきりしているため目視で容易に区別することができる。実験例１のアルミナ焼結体で確認された気孔数は０個であった。
（５）脱粒
　得られたアルミナ焼結体を、１０ｍｍ×１０ｍｍの大きさに切り出し、φ６８ｍｍの金属製定盤の最外周部に９０°おきに４個固定し、ＳｉＣ研磨紙上で、金属製定盤と研磨治具の荷重のみ（合わせて１３１４ｇ）をかけた状態で＃８００で１０分、＃１２００で５分ラップ研磨（予備研磨）した。その後、セラミック定盤上でダイヤモンド砥粒を用いたラップ研磨を行った。ラップ研磨は、砥粒サイズ１μｍで３０分、その後、砥粒サイズ０．５μｍで２時間行った。研磨後の１０ｍｍ×１０ｍｍの焼結体（試料）をアセトン、エタノール、イオン交換水の順でそれぞれ３分間洗浄した後、光学顕微鏡（ニコン製、ＭＭ－６０）にて倍率１００倍で任意の２０箇所を観察し、脱粒の数を数えた。実験例１のアルミナ焼結体につき、脱粒が１０箇所以上生じた試料は２０個中０個であった（０／２０）。脱粒部のあるアルミナ焼結体の光学顕微鏡像の一例を図９に示した。
（６）直線透過率
　得られたアルミナ焼結体２０個のうち、光学顕微鏡で確認した脱粒の個数が最も少なかった試験片を分光光度計（Ｐｅｒｋｉｎ　Ｅｌｍｅｒ製、Ｌａｍｂｄａ９００）を用いて波長３５０～１０００ｎｍにおける直線透過率を測定した。実験例１のアルミナ焼結体の波長３５０～１０００ｎｍにおける直線透過率は７６．２％以上であった。
（７）Ｎａフラックス耐食性
　得られたアルミナ焼結体を、実際のＧａＮ育成条件と同等としてＮａフラックスに対する耐食性を調べた。アルミナ焼結体を内径８０ｍｍ、高さ４５ｍｍの円筒平底のアルミナ坩堝の底部分に設置し、次いで融液組成物をグローブボックス内で坩堝内に充填した。融液組成物の組成は、金属Ｇａ６０ｇ、金属Ｎａ６０ｇ、四塩化ゲルマニウム１．８５ｇとした。このアルミナ坩堝を耐熱金属製の容器に入れて密閉した後、結晶育成炉の回転が可能な台上に設置した。窒素雰囲気中で８７０℃、４．０ＭＰａまで昇温加圧後、１２０時間保持しつつ溶液を回転させた。その後、３時間かけて室温まで徐冷し、結晶育成炉から容器を取り出した。耐食性試験後のアルミナ焼結体の表面をエタノールを用いて超音波洗浄した後、直線透過率を上記（５）と同様にして測定した。実験例１のアルミナ焼結体の耐食性試験後の、波長３５０～１０００ｎｍにおける直線透過率は７２．６％以上であった。
Figure JPOXMLDOC01-appb-T000003
［実験例２］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成においてホットプレスの代わりに、常圧大気焼成を実施した後に、ＨＩＰ焼成を採用したこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。常圧大気焼成の条件は、１３５０℃で４時間保持とした。また、ＨＩＰ焼成の条件は、Ａｒを圧力媒体とし、圧力１８５ＭＰａで１８００℃、２時間保持とした。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例３］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において板状アルミナ粉末を１．５質量部、微細粒状アルミナ粉末を９８．５質量部用いた以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例４］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成において焼成保持時間を２時間にしたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例５］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成において焼成保持時間を８時間にしたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例６］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対し、焼結助剤として酸化マグネシウム粉末のほかにＳｉＯ2粉末を６０質量ｐｐｍ、ＣａＯ粉末を６０質量ｐｐｍ加えた以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例７］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対し、焼結助剤として酸化マグネシウム粉末のほかにＳｉＯ2粉末を１２０質量ｐｐｍ、ＣａＯ粉末を１２０質量ｐｐｍ加えた以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例８］
　アルミナ焼結体を作製するにあたり、実験例１の１．（１）で作製した板状アルミナ粉末の代わりに、市販の板状アルミナ粉末（ＹＦＡ１００３０、キンセイマテック製）を用いたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例９］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成において焼成温度を１７００℃としたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１０］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成において常圧大気中で焼成温度を１７００℃としたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１１］
　アルミナ焼結体を作製するにあたり、実験例１の１．（３）の焼成において焼成温度を１９００℃としたこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１２］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対し酸化マグネシウムを０．２５質量部添加したこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１３］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対しグラファイト粉末を０．０１５質量部添加したこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１４］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対しグラファイト粉末を０．００５質量部添加したこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［実験例１５］
　アルミナ焼結体を作製するにあたり、実験例１の１．（２）のテープ成形において混合アルミナ粉末１００質量部に対しグラファイト粉末を０．０２質量部添加したこと以外は、実験例１と同様にしてアルミナ焼結体を作製した。得られたアルミナ焼結体につき、上記２．（１）～（７）の特性を求めた。その結果を表１に示した。
［評価］
　実験例１～６のアルミナ焼結体は、ｃ面配向度が９０％以上、気孔数は０個、Ｍｇ，Ｃ以外の不純物元素の合計は１００ｐｐｍ以下であった。また、Ｃの含有量は３０～７０ｐｐｍ、Ｍｇの含有量が１２５ｐｐｍ以下、Ｎａフラックス浸漬前の３５０～１０００ｎｍにおける直線透過率が７０％以上であった。更に、Ｎａフラックス浸漬前後の３５０～１０００ｎｍにおける直線透過率の最小値の減少量は５％以下であった。脱粒もほとんどみられなかった。
　実験例７のアルミナ焼結体は、ｃ面配向度が９０％以上、Ｃの含有量が３０～７０ｐｐｍ、Ｍｇの含有量が１２５ｐｐｍ以下であったが、気孔が確認され、Ｍｇ，Ｃ以外の不純物元素の合計は１００ｐｐｍを超え、Ｎａフラックス浸漬前の３５０～１０００ｎｍにおける直線透過率は２５．６％以上であった。これは、ＳｉＯ2やＣａＯの添加量が多すぎたことが原因と考えられる。
　実験例８のアルミナ焼結体は、ｃ面配向度が９０％以上、Ｃの含有量が３０～７０ｐｐｍ、Ｍｇの含有量が１２５ｐｐｍ以下、気孔が０個であったが、Ｍｇ，Ｃ以外の不純物元素の合計は１００ｐｐｍを超え、Ｎａフラックス浸漬前の３５０～１０００ｎｍにおける直線透過率は１．１％以上であった。これは、市販の板状アルミナ粉末を用いたことが原因と考えられる。
　実験例９，１０のアルミナ焼結体は、ｃ面配向度が３０．７～７０．７％と低く、Ｎａフラックス浸漬前の３５０～１０００ｎｍにおける直線透過率が０％と低かった。これは、テープ成形後の焼成温度が適切でなかったことが原因と考えられる。
　実験例１１～１３のアルミナ焼結体は、ｃ面配向度が９０％以上、気孔数は０個、Ｍｇ，Ｃ以外の不純物元素は含有していなかった。また、Ｃの含有量は３０～７０ｐｐｍ、Ｎａフラックス浸漬前の３５０～１０００ｎｍにおける直線透過率が６０％以上（実験例１１，１３は７０％以上）で、脱粒もほとんどみられなかった。但し、実験例１２のアルミナ焼結体は、Ｍｇの含有量が１１３２ｐｐｍと多かったことから、Ｎａフラックス浸漬後の３５０～１０００ｎｍにおける直線透過率はゼロであった。
　実験例１４，１５のアルミナ焼結体は、ｃ面配向度が９０％以上、気孔数は０個、Ｍｇ，Ｃ以外の不純物元素は含有していなかった。また、Ｍｇの含有量が１２５ｐｐｍ以下、Ｎａフラックス浸漬前の直線透過率が７０％以上であった。更に、Ｎａフラックス浸漬前後の直線透過率の減少量が５％以下であった。但し、Ｃの含有量が２０ｐｐｍ及び８０ｐｐｍだったため、脱粒が比較的多くみられた。
　なお、実験例１～１５のうち、本発明の実施例に相当するのは実験例１～６，１１～１５である。本発明は、これらの実施例に何ら限定されるものではなく、本発明の技術的範囲に属する限り、種々の態様で実施することができる。
　本出願は、２０１４年１１月２８日に出願された日本国特許出願第２０１４－２４１６８３号を優先権主張の基礎としており、引用によりその内容の全てが本明細書に含まれる。
　本発明は、例えば光学素子用下地基板に利用可能である。光学素子としては、例えばＬＥＤ、ＬＤ、太陽電池、センサ、フォトダイオード、光学部材、窓材等が挙げられる。
１０　発光素子、１２　下地基板、１４　発光機能層、１４ａ　ｐ型層、１４ｂ　活性層、１４ｃ　ｎ型層、１６　実装基板、２０　横型発光素子、２２　カソード電極、２４　透光性アノード電極、２５　アノード電極パッド、３０　縦型発光素子、３２　アノード電極、３４　カソード電極。

Claims (6)

  1. 　Ｘ線を照射したときの２θ＝２０°～７０°の範囲におけるＸ線回折プロファイルを用いてロットゲーリング法により求めたｃ面配向度が９０％以上の面を有し、
    　任意の断面をイオンミリングによって研磨したあと走査型電子顕微鏡にて倍率５０００倍で調べたときの気孔の数がゼロであり、
    　Ｍｇ，Ｃ以外の不純物元素の合計の質量割合が１００ｐｐｍ以下である、
    　アルミナ焼結体。
  2. 　Ｃの含有量が質量割合で３０～７０ｐｐｍである、
    　請求項１に記載のアルミナ焼結体。
  3. 　前記アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率が７０％以上である、
    　請求項１又は２に記載のアルミナ焼結体。
  4. 　Ｍｇの含有量が質量割合で１２５ｐｐｍ以下である、
    　請求項１～３のいずれか１項に記載のアルミナ焼結体。
  5. 　Ｎａフラックスに浸漬する前の前記アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率の最小値から、窒素中８７０℃のＮａフラックスに１２０時間浸漬した後の前記アルミナ焼結体から取り出した厚み０．２ｍｍの試料の波長３５０～１０００ｎｍにおける直線透過率の最小値を差し引いた値が５％以下である、
    　請求項４に記載のアルミナ焼結体。
  6. 　請求項１～５のいずれか１項に記載のアルミナ焼結体からなる光学素子用下地基板。
PCT/JP2015/082644 2014-11-28 2015-11-20 アルミナ焼結体及び光学素子用下地基板 WO2016084722A1 (ja)

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