JP6423259B2 - Window member and lamp device - Google Patents

Description

  The present invention relates to a window member and a lamp device including a translucent member.

  Conventionally, for example, in a light extraction window of a lamp device such as a viewing window of a vacuum vessel for observing the inside of a vacuum vessel used in a semiconductor manufacturing apparatus or an electronic device, or a light irradiation device using a xenon lamp, for example, light transmission A window member using a translucent member mainly composed of sapphire, which has high properties and excellent thermal conductivity, is used.

  For example, a translucent member made of sapphire can be brazed with a metal frame by depositing a metallized layer on its surface. For example, it is made of sapphire as described in Patent Document 1 below. A viewing window that secures high airtightness by brazing the window member to a metal member has been proposed.

JP 2008-184691 A

  In recent years, for example, with the progress of miniaturization of devices such as a lamp device, the distance between the light emitter and the window member is close, and the temperature of the window member in use sometimes becomes higher than the conventional one. For example, sapphire is a member with excellent thermal conductivity and high heat dissipation effect, but when the temperature of the metallized layer and brazing material layer rises excessively, these metallized layer and brazing material layer react with components in the atmosphere (ie, corrosion). However, the bonding strength between the window member and the metal member may be reduced. When the thermal stress increases due to an excessive temperature rise, a decrease in bonding strength and an increase in thermal stress may cause a combination of the window member and the lamp device including the window member itself. The present invention aims to solve these problems.

  A window member according to one aspect of the present invention is a window member formed by joining a plate-like light-transmitting member and a frame-shaped body mainly composed of a metal having an inner surface surrounding a side surface of the light-transmitting member. The metallized layer formed on the side surface of the translucent member, the first metal layer mainly composed of nickel formed on the surface of the metallized layer, and the inner side surface of the frame-shaped body The light-transmitting member and the frame-shaped body are formed on the second metal layer containing nickel as a main component and containing phosphorus or boron, the first metal layer, and the second metal layer. And a brazing filler metal layer having silver as a main component.

  In the window member according to one embodiment of the present invention, the bonding strength between the translucent member and the frame-like body is difficult to decrease.

An example of the window member of this embodiment is shown, (a) is a plan view, (b) is a cross-sectional view taken along the line A-A 'of (a). The other example of the window member of this embodiment is shown, (a) is a top view, (b) is sectional drawing in the B-B 'line of (a). The other example of the window member of this embodiment is shown, (a) is a top view, (b) is a sectional view in the CC 'line of (a), (c) is an A section enlarged view of (b), (D) is the B section enlarged view of (b).

  Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings.

  1A and 1B show an example of a window member of the present embodiment. FIG. 1A is a plan view, and FIG. 1B is a cross-sectional view taken along line A-A ′ of FIG.

  2A and 2B show another example of the window member of the present embodiment. FIG. 2A is a plan view, and FIG. 2B is a cross-sectional view taken along line B-B ′ in FIG.

  The window member in the example shown in FIGS. 1 and 2 is formed by joining a plate-like translucent member 3 and a frame-like body 4 whose main component is a metal having an inner side surface surrounding a side surface 3d of the translucent member 3. A metallized layer 1 formed on the side surface 3d of the translucent member 3, a first metal layer 2 mainly composed of nickel, formed on the surface of the metallized layer 1, and a frame. The translucent member 3 is deposited on the second metal layer 6 containing nickel as a main component and containing phosphorus or boron, and the first metal layer 2 and the second metal layer 6, which are formed on the inner surface of the body 4. And a brazing filler metal layer 5 containing silver as a main component.

  Since the inner surface of the frame 4 is further provided with the second metal layer 6 containing nickel as a main component and containing phosphorus or boron as described above, the inner surface of the frame 4 is less likely to be oxidized. Even if exposed to the above, stress corrosion cracks starting from the inner surface are less likely to occur, and the bonding strength between the translucent member 3 and the frame-like body 4 is less likely to be reduced. The first metal layer 2 may be formed by plating a so-called nickel (Ni) plating material. The second metal layer 6 may be formed by plating a nickel plating material containing phosphorus or boron. Hereinafter, the first metal layer 2 is also referred to as the first plating layer 2, and the second metal layer 6 is also referred to as the second plating layer 6. The second metal layer 6 is not limited to being formed only on the inner side surface of the frame-like body 4, and is formed on the outer side surface of the frame-like body 4 or the entire surface of the frame-like body 4. May be.

  Here, the metallized layer 1 includes, for example, molybdenum as a main component and manganese.

The translucent member 3 can be made of glass, ceramics, single crystal, or the like. When the translucent member 3 is made of ceramics, the ceramics are, for example, yttrium aluminum garnet (YAG), magnesium aluminate (MgAl ₂ O ₄ ), aluminum nitride (AlN), magnesium difluoride (MgF _2). ), Lithium fluoride (LiF), calcium difluoride (CaF ₂ ), barium difluoride (BaF ₂ ), or the like may be used. Moreover, what is necessary is just to comprise the translucent member 3 with a sapphire, for example, when using the translucent member which consists of a single crystal as the translucent member 3. FIG. Here, it is preferable that the translucent member 3 is mainly composed of sapphire, and the frame body 4 is mainly composed of an Fe—Ni—Co alloy, an Fe—Ni alloy, or a Cu—W alloy. The linear expansion coefficient of sapphire at 40 to 400 ° C. is 7.7 × 10 ⁻⁶ / ° C. (direction parallel to the c-axis) and 7.7 × 10 ⁻⁶ / ° C. (direction perpendicular to the c-axis), each linear expansion coefficient of the Fe-Ni-Co alloy, Fe-Ni alloy and Cu-W alloy in the above temperature ^{range, 4.9 × 10 -6 /℃,5.0×10 -6 /} ℃ , 6.4 × 10 ⁻⁶ / ° C., the difference in linear expansion coefficient between sapphire and the alloy is small, and distortion due to residual stress generated after joining with a brazing material is difficult to occur.

In addition, the main component in each member which comprises the window member 10 of this embodiment is a component which occupies 70 mass% or more with respect to a total of 100 mass% of the component which comprises a member. When the member is made of metal, the content of each metal is determined using an ICP emission spectroscopic analyzer or a fluorescent X-ray analyzer, and 70% by mass or more with respect to the total of 100% by mass of the components constituting the member. Is the main component. In addition, when the member is made of a compound, the compound is identified using an X-ray diffractometer (XRD), and the inclusion of the metal constituting the compound using an ICP emission spectroscopic analyzer or a fluorescent X-ray analyzer What is necessary is just to obtain | require an amount and to convert into the identified compound.

  Further, in the window member 10b shown in FIG. 2, each shape of the translucent member 3 and the frame body 4 constituting the window member 10a shown in FIG. 1 is a square plate shape and a rectangular frame shape, respectively. The shape of the translucent member 3 is a disc shape, and the shape of the frame-like body 4 is an annular shape.

  According to the configuration of the window member 10b shown in FIG. 2, both the translucent member 3 and the frame-like body 4 have the inside of the side surface 3d and the frame-like body 4 of the translucent member 3 even in an environment where heating and cooling are repeated. Since there are no corners where stress concentration is likely to occur on the side surfaces, cracks are less likely to occur.

  Here, the metallized layer 1 has a thickness of, for example, 10 μm or more and 30 μm or less. Moreover, when the translucent member 3 is disk shape, a diameter is 20 mm or more and 30 mm or less, and thickness is 1 mm or more and 5 mm or less. When the frame-like body 4 is annular, the inner diameter and the outer diameter are 20 mm or more and 30 mm or less, 21 mm or more and 31 mm or less, respectively, and the thickness is 3 mm or more and 8 mm or less.

  The first plating layer 2 preferably has a thickness of 3 μm or more and 9 μm or less. If the thickness of the first plating layer 2 is 3 μm or more, the risk of exposing the metallized layer 1 is reduced even if there is a portion where the height difference of the surface of the first plating layer 2 is large. Adhesiveness is ensured, and the bonding strength of the brazing material layer 5 to the first plating layer 2 can be maintained high. On the other hand, if the thickness of the first plating layer 2 is 9 μm or less, the residual stress in the first plating layer 2 is unlikely to increase even if heating and cooling are repeated, so that the first plating layer 2 is peeled off from the metallized layer 1. It becomes difficult.

  The second plating layer 6 preferably has a thickness of 3 μm or more and 9 μm or less. If the thickness of the second plating layer 6 is 3 μm or more, even if there is a portion where the height difference of the inner surface of the frame 4 is large, the possibility that the frame 4 will be exposed is reduced. Even when exposed to the above, stress corrosion cracking starting from the inner surface of the frame 4 is further less likely to occur. On the other hand, if the thickness of the second plating layer 6 is 9 μm or less, the residual stress in the second plating layer 6 is hardly increased even if heating and cooling are repeated, so that the second plating layer 6 is peeled off from the frame-like body 4. It becomes difficult to do.

  3A and 3B show another example of the window member of the present embodiment, in which FIG. 3A is a plan view, FIG. 3B is a sectional view taken along the line CC ′ of FIG. 3A, and FIG. Part (d) is an enlarged view of part B of (b).

  According to the window member 10c of the example shown in FIG. 3, the translucent member 3 includes the inclined surfaces 3c and 3g at the outer edge portions of at least one of the main surfaces 3a and 3b. The plated layer 2 is continuously formed from the side surface 3d to at least a part of the inclined surfaces 3c and 3g. That is, inclined surfaces 3c and 3g, which are so-called chamfered surfaces, are provided between the main surfaces 3a and 3b and the side surface 3d.

  With such a configuration, it is possible to increase the amount of brazing material on the main surfaces 3a and 3b side including the inclined surfaces 3c and 3g, so that the brazing material layer 5 can perform the heating and cooling repeatedly. Since the effect | action which relieve | moderates the increase in a thermal stress becomes high, it becomes difficult to produce the crack which makes the outer surface 3d of the translucent member 3 a starting point.

  From the viewpoint described above, it is preferable that the brazing filler metal layer 5 of the window member 10c is continuously applied from a region corresponding to the side surface of the first plating layer 2 to a region corresponding to the inclined surfaces 3c and 3g. .

  Here, the thickness of the metallized layer 1 on the inclined surfaces 3c and 3g is, for example, 10 μm or more and 30 μm or less. Moreover, the thickness of the first plating layer 2 on the inclined surfaces 3c and 3g is, for example, 3 μm or more and 9 μm or less.

  Further, the metallized layer 1 and the first plating layer 2 are formed in a region occupying an area of at least 40% of the surface area of the inclined surfaces 3c and 3g, starting from the intersection lines 3e and 3h between the inclined surfaces 3c and 3g and the outer surface 3d. Is preferably formed on the inclined surfaces 3c and 3g. That is, the metallized layer 1 and the first plating layer 2 are preferably formed on the portion of the inclined surfaces 3c and 3g on the outer surface 3d side including the intersecting lines 3e and 3h. The area of the plating layer 2 is preferably 40% or more of the entire surface area of each of the inclined surfaces 3c and 3g. When the metallized layer 1 and the first plating layer 2 are applied to the entire inclined surfaces 3c and 3g, the metallized layer 1 and the first plated layer 2 are formed on the entire main surfaces 3a and 3b of the window member 10 in the formation process of these layers. 1 plating layer 2 is easy to wet and spread, and there is a possibility that an extra step of removing metallized layer 1 and first plating layer 2 spreading on main surface 3a and main surface 3b may be required. The metallized layer 1 and the first plating layer 2 are formed in a region of 40% or more and 70% or less of the entire surface area from the portion of the inclined surfaces 3c and 3g on the outer surface 3d side including the intersecting lines 3e and 3h. Is preferred.

Further, according to the window member 10 of the present embodiment, the angles θ ₁ and θ ₂ formed by the main surfaces 3a and 3b and the inclined surfaces 3c and 3g are preferably 120 ° or more and 150 ° or less. When the angles θ ₁ and θ ₂ are 120 ° or more, even if heating and cooling are repeated, stress concentration is generated on the intersecting lines 3e and 3h between the main surfaces 3a and 3b of the translucent member 3 and the inclined surfaces 3c and 3g. Therefore, cracks starting from the intersection lines 3e and 3h are less likely to occur. On the other hand, when the angles θ ₁ and θ ₂ are 150 ° or less, the amount of the brazing material between the translucent member 3 and the frame-like body 4 can be increased. Therefore, even if heating and cooling are repeated, the brazing material layer 5 As a result, the effect of alleviating the increase in thermal stress is increased, so that cracks starting from the side surface 3d of the translucent member 3 are less likely to occur.

Further, according to the window member 10 of the present embodiment, the widths L ₁ and L ₂ of the inclined surfaces 3c and 3g are 0.2 mm or more and 0.4 mm or less in a plan view perpendicular to the main surfaces 3a and 3b. Is preferred.

When the widths L ₁ and L ₂ are 0.2 mm or more, the amount of the brazing material between the translucent member 3 and the frame-like body 4 can be increased. Therefore, even if heating and cooling are repeated, the thermal stress is caused by the brazing material layer 5. Since the effect | action which relieve | moderates an increase becomes high, it becomes difficult to produce the crack which makes the side 3d of the translucent member 3 a starting point. On the other hand, if the widths L ₁ and L ₂ are 0.4 mm or less, the possibility that a part of the main surfaces 3a and 3b of the translucent member 3 is covered with the brazing material is reduced, so that translucency is maintained. Can do.

  Further, according to the window member 10 of the present embodiment, the arithmetic average roughness Ra of the inclined surfaces 3c, 3g is preferably 0.15 μm or more and 0.35 μm or less. When the arithmetic average roughness Ra of the inclined surfaces 3c and 3g is 0.15 μm or more, the bonding strength between the translucent member 3 and the metallized layer 1 can be maintained high due to the anchor effect. On the other hand, if the arithmetic average roughness Ra of the inclined surfaces 3c and 3g is 0.35 μm or less, the metallized layer 1 can be formed thin, so that the residual stress generated in the metallized layer 1 even if heating and cooling are repeated. Is suppressed, and the metallized layer 1 and the first plated layer 2 are less likely to be peeled off.

Here, the arithmetic average roughness Ra of the inclined surfaces 3c and 3g is determined by JIS B in the portion of the surfaces of the inclined surfaces 3c and 3g where other layers such as the metallized layer 1 and the first plating layer 2 are not deposited. Measurement may be performed in accordance with 0601-2013. If the measurement length and cut-off value are 0.25 mm and 0.8 mm, respectively, and the measurement is performed using a stylus type surface roughness meter, for example, the stylus tip radius is on the inclined surfaces 3c and 3g. A 2 μm stylus is applied, the stylus scanning speed is set to 0.5 mm / second, and the average value of each of four locations obtained by this measurement is taken as the value of the arithmetic average roughness Ra.

  The window member described above can be used in a lamp device or the like provided with the window member and a light emitter described above. For example, a light emitter such as a xenon lamp emits a lot of heat during light emission. The transmission window that protects the heating element and transmits light is often at a high temperature. When used for a long period of time, the joint is likely to deteriorate or crack due to corrosion. As described above, the lamp device using the window member of the present embodiment is less susceptible to stress corrosion cracking starting from the inner surface even when exposed to the air atmosphere for a long period of time. Since it is configured to include the window member and the light emitter of the embodiment, it can be used for a long period of time, and the replacement frequency of the window member can be reduced. The window member is not limited to a lamp device or the like, and may be used for a window member for a vacuum apparatus such as a plasma processing apparatus or other devices.

  In addition, when the window member of this embodiment is used for a xenon lamp device, the window member has an inclined surface at the outer edge portion of both main surfaces, and the main surface on the side exposed to the atmosphere and the inclined surface The angle formed between the main surface exposed to xenon and the inclined surface is 120 ° to 150 °, and the angle formed between the main surface exposed to the atmosphere and the inclined surface is It is preferable that the angle is smaller than the angle formed between the exposed main surface and the inclined surface. By reducing the angle formed between the main surface on the side exposed to the atmosphere and the inclined surface, it is possible to suppress the deterioration of the brazing material caused by exposure to the atmosphere.

Next, an example of the manufacturing method of the window member of this embodiment is demonstrated. First, the metallized layer 1 containing molybdenum as a main component and containing manganese is formed on the side surface 3d of the plate-like translucent member 3 made of ceramics or glass by the Telefunken method. A first plating layer 2 (first metal layer 2) containing nickel as a main component and containing phosphorus or boron is sequentially formed on the surface of the metallized layer 1 by electroless plating. Further, the inner surface of the frame 4 mainly composed of Fe-Ni-Co alloy, Fe-Ni alloy or Cu-W alloy is mainly composed of nickel by electroless plating or electrolytic plating, and phosphorous. Alternatively, the second plating layer 6 (second metal layer 6) containing boron is formed. Specifically, in the case where the second plating layer 6 containing nickel as a main component and containing phosphorus is formed by electroless plating, for example, nickel sulfate, sodium hypophosphite, and succinic acid are contained at 60 ° C. or higher. What is necessary is just to immerse the translucent member 3 and the frame-shaped body 4 in the electroless nickel plating solution heated at 90 degrees C or less. In the case where the second plating layer 6 containing nickel as a main component and containing phosphorus is formed by electrolytic plating, for example, the pH containing nickel sulfate, nickel chloride, boric acid, citrate and phosphorous acid is 2.4. The translucent member 3 and the frame-like body 4 are immersed in an electrolytic nickel plating solution heated to 50 ° C. or higher and 65 ° C. or lower, and the current density is 0.1 A / dm ² or more and 20 A. / Dm ² or less may be set. In particular, the current density is preferably 1 A / dm ² or more and 2 A / dm ² or less.

When forming the second plating layer 6 containing nickel as a main component and containing boron by electroless plating, a nickel compound such as nickel sulfate and a boron-based reducing agent such as sodium borohydride and dimethylamine borane are included. What is necessary is just to immerse the translucent member 3 and the frame-shaped body 4 in the electroless nickel plating solution heated at 60 degreeC or more and 90 degrees C or less. When the second plating layer 6 containing nickel as a main component and containing boron is formed by electrolytic plating, for example, an amine-added hydrogen compound such as nickel sulfate, nickel chloride, boric acid and trimethylamine, triethylamine borane, dimethylamine borane is used. The translucent member 3 and the frame-like body 4 are immersed in an electrolytic nickel plating solution having a pH of 1.5 to 6 and heated to a temperature of 40 ° C. or higher and 70 ° C. or lower, and the current density is 1 A / dm. ² or 5A / dm ² may be set below.

  Here, in order to obtain the window members 10a and 10b in which the thicknesses of the first plating layer 2 and the second plating layer 6 are 3 μm or more and 9 μm or less, they are immersed in the electroless nickel plating solution for 35 minutes or more and 65 minutes or less. Good.

  Further, the translucent member 3 includes inclined surfaces 3c and 3g at the outer edge portions of at least one of the main surfaces 3a and 3b, and the metallized layer 1 and the first plating layer 2 are formed from the side surface 3d to the inclined surfaces 3c, 3c, In order to obtain the window member 10c formed continuously over at least a part of 3g, the translucent member 3 provided with the inclined surfaces 3c and 3g is prepared, and the same method as described above may be used.

  Here, in order to obtain the window member 10c having the arithmetic average roughness Ra of the inclined surfaces 3c and 3g of 0.15 μm or more and 0.35 μm or less, for example, diamond abrasive grains having a particle size of 325 or more and 400 or less were fixed. What is necessary is just to grind the outer edge part of at least any one of the main surfaces 3a and 3b by using an electrodeposition grindstone and setting the rotation speed of the electrodeposition grindstone to 2300 rpm or more and 2600 rpm or less.

  Then, after weighing and mixing so that the ratios of the silver and copper powders are 72% by mass and 28% by mass, respectively, a resin or inorganic compound flux and an organic solvent are added and kneaded to obtain a brazing material paste. After producing and applying this brazing paste to the surface of at least one of the first plating layer 2 and the second plating layer 6 by any method such as screen printing, pressure printing, and brush coating, 120 Dry at a temperature of from 150 ° C. to 150 ° C.

  Here, 2 parts by mass or more and 5 parts by mass or less of titanium, hafnium, zirconium, niobium, or a hydride thereof may be added to and mixed with 100 parts by mass of the silver and copper powders in total. Furthermore, it is preferable to add and mix 1 to 10 parts by mass of indium or tin with 100 parts by mass of each of the silver and copper powders, which reduces the bonding temperature and the hardness of the brazing material layer. Can be.

  Then, after drying the brazing material paste, the window member 10 of the present embodiment in which the translucent member 3 and the frame-like body 4 are joined by heat treatment at, for example, 780 ° C. or more and 900 ° C. or less. Can be obtained.

  Alternatively, after placing the brazing material paste obtained by the above-described method on one end face of the first plating layer 2 and the second plating layer 6, by irradiating the brazing material with a laser and utilizing wet spreading, The window member 10 of this embodiment in which the translucent member 3 and the frame-like body 4 are joined can be obtained.

  Examples of the present invention will be specifically described below, but the present invention is not limited to these examples.

  First, an annular frame 4 having a Fe—Ni—Co alloy as a main component is prepared, and the contents of nickel and phosphorus are 93% by mass and 7% by mass, respectively, on the inner surface by electroless plating. The second plating layer 6 is formed and the sample No. It was set to 1. As a specific method of electroless plating, the frame 4 was immersed in an electroless nickel plating solution heated to 75 ° C. containing nickel sulfate, sodium hypophosphite and succinic acid for 30 minutes.

  As a comparative example, an annular frame 4 without the second plating layer 6 was prepared, and sample No. 2.

  And sample no. 1 and the surface of the second plating layer 6 and the sample No. 2 was measured by energy dispersive X-ray spectroscopy (EDX), and then sample No. 2 was measured. 1 and 2 were kept at 200 ° C. for 24 hours in an air atmosphere. And after finishing this holding | maintenance, again sample No. 1 and the surface of the second plating layer 6 and the sample No. The respective oxygen concentrations on the inner side surface of the frame body 4 of No. 2 were measured, and the difference in oxygen concentration before and after holding was shown in Table 1.

  As shown in Table 1, sample no. 1 is formed by forming the second plating layer 6 on the inner surface of the frame-like body 4, and therefore, sample No. 1 without the second plating layer 6 even when exposed to high temperatures. It turns out that it is harder to oxidize than 2, and it becomes difficult to produce a crack over a long period of time. From this result, the sample No. 1 in which the translucent member 3 on which the metallized layer 1 and the first plating layer 2 were formed was joined by the brazing material layer 5 was obtained. When comparing Nos. 1 and 2, Sample No. 1 is Sample No. It can be said that even when exposed to an air atmosphere for a longer time than 2, the bonding strength is unlikely to decrease.

  First, a disc-shaped translucent member 3 made of sapphire is prepared, and a metallized layer 1 having molybdenum and manganese contents of 80% by mass and 20% by mass is formed on the side surface 3d by the Telefunken method, respectively. The first plating layer 2 having a nickel and phosphorus content of 93% by mass and 7% by mass, respectively, was sequentially formed by electrolytic plating. In addition, an annular frame 4 made of an Fe—Ni—Co alloy is prepared, and the inner surface thereof has nickel and phosphorus contents of 93 mass% and 7 mass%, respectively, by electroless plating. Two plating layers 6 were formed. As a specific method of electroless plating, the translucent member 3 was immersed in the electroless nickel plating solution used in Example 1 for the time shown in Table 2, and the frame 4 was immersed for 80 minutes.

  Then, after weighing and mixing so that the ratios of the silver and copper powders are 72% by mass and 28% by mass, respectively, a resin or inorganic compound flux and an organic solvent are added and kneaded to obtain a paste-like brazing material Was made. After this brazing material is placed on one end face of the first plating layer 2 and the second plating layer 6, the brazing material is irradiated with a laser so that the sample No. 1 which is the window member 10 b shown in FIG. 3-7 were obtained.

  Then, the shear strength of the brazing filler metal layer 5 with respect to the first plating layer 2 was measured along the thickness direction of each sample, and the shear strength is shown in Table 2. In Examples 2 and 3, this shear strength is the bonding strength.

A cycle different from the sample whose shear strength was measured was held at 90 ° C. for 30 minutes, and then held at −40 ° C. for 30 minutes. It was. After carrying out this temperature cycle test, the cross section perpendicular to the thickness direction of the window member was polished to a mirror surface, the thickness of the first plating layer 2 on this mirror surface was measured, and the values are shown in Table 3. In addition, the presence or absence of peeling of the first plating layer 2 was observed, and it was shown in Table 2 as being present in samples in which peeling was observed and absent in samples in which peeling was not observed. In addition, the measurement and observation of the thickness of the 1st plating layer 2 made the magnification 100 times using the optical microscope. The thickness of the second plating layer 6 on the mirror surface was 12 μm.

  As shown in Table 2, in Sample Nos. 4 to 6, since the thickness of the first plating layer 2 is 3 μm or more and 9 μm or less, the bonding strength of the brazing material layer 5 to the first plating layer 2 is high, and heating and cooling are performed. It turns out that the 1st plating layer 2 is hard to peel even if it repeats.

  The disc-shaped translucent member 3 made of sapphire, in which the first plating layer 2 is formed on the outer side surface 3d through the metallized layer 1 by the method shown in Example 2, and the second plating layer 6 on the inner side surface An annular frame 4 made of the formed Fe—Ni—Co alloy was obtained. However, the translucent member 3 was immersed in the electroless nickel plating solution used in Example 2 for 80 minutes, and the frame 4 was immersed in the time shown in Table 3.

  And by the method shown in Example 2, the translucent member 3 and the frame-like body 4 were joined using the brazing material, so that the sample No. 1 as the window member 10b shown in FIG. 8-12 were obtained.

  And the shear strength of the brazing filler metal layer 5 with respect to the 2nd plating layer 6 was measured along the thickness direction of each sample. In addition, a temperature cycle test was performed by the same method as shown in Example 2. After carrying out this temperature cycle test, the cross section perpendicular to the thickness direction of the window member was polished to a mirror surface, the thickness of the second plating layer 6 on this mirror surface was measured, and the values are shown in Table 3. In addition, the presence or absence of peeling of the second plating layer 6 was observed, and it was shown in Table 3 as being present in samples in which peeling was observed and absent in samples in which peeling was not observed. In addition, the measurement and observation of the thickness of the 2nd plating layer 6 made the magnification 100 times using the optical microscope. The thickness of the first plating layer 2 on the mirror surface was 12 μm.

  As shown in Table 3, Sample No. In Nos. 9 to 11, since the thickness of the second plating layer 6 is not less than 3 μm and not more than 9 μm, the bonding strength of the brazing material layer 5 to the second plating layer 6 is high, and the second plating layer 6 can be repeatedly heated and cooled. It turns out that it is hard to peel.

  First, a disc-shaped translucent member 3 made of sapphire is prepared, and an electrodeposited grindstone to which diamond abrasive grains having a particle size shown in Table 4 are fixed is used. , 3b were polished to obtain inclined surfaces 3c, 3g.

  The metallized layer 1 having a molybdenum and manganese content of 80% by mass and 20% by mass, respectively, is formed on the outer surface 3d by the Telefunken method, and the nickel and phosphorus contents are 93% by mass and 7% by electroless plating, respectively. % Of the first plating layer 2 was sequentially formed. At the same time, the second intermediate layer 7 and the third metal layer 8 were sequentially formed on the inclined surfaces 3c and 3g.

  In addition, an annular frame 4 made of an Fe—Ni—Co alloy is prepared, and the inner surface thereof has nickel and phosphorus contents of 93 mass% and 7 mass%, respectively, by electroless plating. Two plating layers 6 were formed. As a specific method of electroless plating, as a specific method of electroless plating, the translucent member and the frame 4 were both immersed in the electroless nickel plating solution used in Example 1 for 50 minutes. .

  Then, after weighing and mixing so that the ratios of the silver and copper powders are 72% by mass and 28% by mass, respectively, a resin or inorganic compound flux and an organic solvent are added and kneaded to obtain a paste-like brazing material Was made. After this brazing material is placed on one end face of the first plating layer 2 and the second plating layer 6, the brazing material is irradiated with a laser so that the sample No. 1 in the window member 10 c shown in FIG. 13-27 were obtained.

  Here, Sample No. The brazing filler metal layer 5 of 13 to 27 is continuously applied from the region corresponding to the side surface of the first plating layer 2 to the region corresponding to the inclined surfaces 3c and 3g using an optical microscope. Confirmed as double. Sample No. In Nos. 13 to 27, the metallized layer 1 and the first layer 1 are formed in a region occupying an area of about 60% of the surface area of the inclined surfaces 3c and 3g starting from the intersection lines 3e and 3h between the inclined surfaces 3c and 3g and the outer surface 3d. A plating layer 2 and a brazing material layer 5 are formed. That is, sample no. In Nos. 13 to 27, the metallized layer 1 and the first plating layer 2 are formed only in an area of about 60% of the inclined surfaces 3c and 3g on the outer surface 3d side including the intersecting lines 3e and 3h. .

  As a comparative example, the sample No. 1 which is the window member 10b shown in FIG. 28 was produced by the method described above.

  Then, after each sample was held at 90 ° C. for 30 minutes and then held at −40 ° C. for 30 minutes, a cycle of 1200, 1400, 1600, and 1800 cycles was performed. After carrying out these temperature cycle tests, the cross section perpendicular to the thickness direction of the window member 10c is polished to a mirror surface, and the presence or absence of cracks starting from the outer surface 3d of the translucent member 3 on this mirror surface is determined using an optical microscope. Table 5 shows that the sample was observed with a magnification of 100 times, and was present for samples in which cracks were observed, but not for samples in which cracks were not observed.

In addition, the radial cross section of the window member is polished to a mirror surface, and the angle θ ₁ (θ ₂ ) and width L ₁ (L ₂ ) on the mirror surface are measured with an optical microscope at a magnification of 100 times, and the values are It is shown in Table 4.

Further, the arithmetic average roughness Ra of the inclined surface 3c (3g) was measured according to JIS B 0601-2013. Specifically, the measurement length and cut-off value were set to 0.25 mm and 0.8 mm, respectively, and measurement was performed using a stylus type surface roughness meter. The stylus tip radius was measured on the inclined surface 3c (3g). A 2 μm stylus was applied, and the scanning speed of the stylus was set to 0.5 mm / second. The average value of each of four locations obtained by this measurement is shown in Table 4 as the value of arithmetic average roughness Ra.

  As shown in Tables 4 and 5, Sample No. The translucent members 3 of 13 to 27 are provided with inclined surfaces 3c and 3g at outer edges of at least one of the main surfaces 3a and 3b, and the metallized layer 1 and the first plating layer 2 are inclined from the side surface 3d. The brazing material layer 5 is continuously formed from the region corresponding to the side surface of the first plating layer to the region corresponding to the inclined surfaces 3c and 3g. Therefore, sample no. It can be seen that cracks starting from the outer surface 3d are less likely to occur than 28.

Sample Nos. 16, 17, 18, 21, 24 having the same width L ₁ (L ₂ ) and the same arithmetic average roughness Ra of the inclined surface 3c (3g) but different angles θ ₁ (θ ₂ ). When comparing 25,
Sample No. 17,18,21,24, since the angle θ ₁ (θ ₂₎ is less than 0.99 ° 120 ° or more, the angle θ ₁ (θ ₂₎ is outside this range Sample No. It can be seen that cracks starting from the intersecting portion 3e (3h) and the outer side surface 3d are less likely to occur than 16 and 25.

In addition, the sample No. ₁ in which the angle θ ₁ (θ ₂ ) and the arithmetic mean roughness Ra of the inclined surface 3c (3g) are the same and the width L ₁ (L ₂ ) is different. When comparing 19 to 23, the width L ₁ (L ₂ ) is 0.2 m.
m and 0.4 mm or less. Samples Nos. 20 to 23 are out of this range. It can be seen that cracks starting from the outer surface 3d are less likely to occur than 19.

In addition, the sample No. ₁ in which the angle θ ₁ (θ ₂ ) and the width L ₁ (L ₂ ) are the same and the arithmetic mean roughness Ra of the inclined surface 3c (3g) is different. 13, 14, 15, 26, and 27, Sample No. in which the arithmetic average roughness Ra of the inclined surface 3 c (3 g) is 0.15 μm or more and 0.35 μm or less. Samples Nos. 13, 14, 15, and 26 are sample Nos. Outside this range. It can be seen that the metallized layer 1 and the first plated layer 2 are less likely to peel than 27.

  In the present embodiment, the case where the first plating layer 2 is mainly composed of nickel and contains phosphorus is shown. However, the same result is obtained when the first plating layer 2 is mainly composed of nickel and contains boron. It goes without saying that it is obtained.

DESCRIPTION OF SYMBOLS 1 Metallization layer 2 1st plating layer 3 Translucent member 4 Frame-like body 5 Brazing material layer 6 2nd plating layer 10 Window member

Claims (8)

A window member formed by joining a plate-like light-transmitting member and a frame-shaped body mainly composed of a metal having an inner surface surrounding a side surface of the light-transmitting member,
A metallized layer formed on the side surface of the translucent member;
A first metal layer mainly composed of nickel formed on the surface of the metallized layer;
A second metal layer formed on the inner surface of the frame-like body and containing nickel or phosphorus or boron as a main component;
A window comprising: a brazing material layer mainly composed of silver, which is attached to the first metal layer and the second metal layer and joins the translucent member and the frame-like body. Element.   2. The translucent member is mainly composed of sapphire, and the frame body is composed mainly of an Fe—Ni—Co alloy, an Fe—Ni alloy, or a Cu—W alloy. The window member described. The translucent member includes an inclined surface at an outer edge portion of at least one of the main surfaces,
The window member according to claim 1, wherein the metallized layer and the first metal layer are continuously formed from the side surface to at least a part of the inclined surface. The window member according to claim 3, wherein the brazing material layer is continuously applied from a region corresponding to the side surface of the first metal layer to a region corresponding to the inclined surface.   The window member according to claim 3 or 4, wherein an angle formed between the main surface and the inclined surface is 120 ° or more and 150 ° or less. In a plan view perpendicular to the main surface,
The window member according to any one of claims 3 to 5, wherein a width of the inclined surface is 0.2 mm or more and 0.4 mm or less.   The window member according to claim 3, wherein an arithmetic average roughness Ra of the inclined surface is 0.15 μm or more and 0.35 μm or less.   A lamp device comprising the window member according to any one of claims 1 to 7 and a light emitter.

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