KR20160072109A - Phosphor-sheet evaluation method and manufacturing method - Google Patents

Abstract

A method of evaluating a phosphor sheet is a method of evaluating a phosphor sheet formed of a liquid composition containing a phosphor and a resin, comprising the steps of: placing a spacer on a substrate; injecting a liquid composition into the spacer to a predetermined height; And a measuring step of measuring the chromaticity of the liquid composition at a predetermined height.

Description

[0001] PHOSPHOR-SHEET EVALUATION METHOD AND MANUFACTURING METHOD [0002]

The present invention relates to a method of evaluating a phosphor sheet and a method of manufacturing the same, and more particularly, to a method of evaluating a phosphor sheet used in optical applications and a method of manufacturing the same.

Conventionally, a white light semiconductor device is known as a light emitting device capable of emitting light of high energy.

The white light semiconductor device includes, for example, an optical semiconductor element that emits blue light, and an encapsulant that encapsulates the optical semiconductor element and converts blue light (wavelength) into yellow light. So as to realize white light emission.

As such an encapsulating material for a white light semiconductor device, for example, a sealing sheet obtained by heat-curing a resin composition containing a silicone resin and a fluorescent material has been proposed (for example, see Patent Document 1).

Japanese Patent Application Laid-Open No. 2013-140848

However, in order to develop a good white color, the encapsulation sheet is required to have high precision in adjusting its chromaticity.

Therefore, a step of preparing a sealing sheet for trial production so as to express a desired chromaticity and evaluating its chromaticity is repeatedly carried out while changing the raw material composition (such as the content of the phosphor) of the sealing sheet. Then, the optimum raw material composition for achieving the desired chromaticity is determined.

However, the sealing sheet is obtained, for example, by applying a liquid composition containing a phosphor to a substrate and then curing (fully curing or semi-curing) by heating or the like. Therefore, at the start, a curing step such as heating is required, or it takes time to form the sealing sheet. In addition, since the encapsulating sheet provided at the start is hardened, there arises a problem that it needs to be discarded or reused.

It is an object of the present invention to provide a method of evaluating a phosphor sheet which can easily evaluate the chromaticity of the phosphor sheet and a method of manufacturing the phosphor sheet.

A method of evaluating a phosphor sheet of the present invention is a method of evaluating a phosphor sheet formed of a liquid composition containing a phosphor and a resin, comprising the steps of: arranging a spacer on a substrate; And a measuring step of measuring the chromaticity of the liquid composition at the predetermined height.

The evaluation method of the phosphor sheet of the present invention is preferably such that the substrate has the optical semiconductor element on its surface and the liquid composition is injected so as to cover the optical semiconductor element in the injection step.

Further, in the method of evaluating the phosphor sheet of the present invention, it is preferable that the measurement step is performed before the phosphor precipitates in the liquid composition after the implantation step.

The method for evaluating a phosphor sheet of the present invention may further comprise a cover placing step of placing the transparent cover so as to be in contact with the upper surface of the liquid composition at the predetermined height after the injection step and before the measuring step, .

The method for producing a phosphor sheet of the present invention may further comprise: an evaluation step of performing the evaluation method described above; a crystallization step of determining the composition of the liquid composition based on the evaluation method; And a forming step of forming the liquid composition in a sheet form.

Further, in the method for producing a phosphor sheet of the present invention, in the crystal step, the composition of the liquid composition is determined based on the evaluation method, the precrystallized liquid composition is precisely irradiated, and the composition of the liquid composition It is preferable to have a step of determining the temperature of the liquid.

INDUSTRIAL APPLICABILITY The method of evaluating a phosphor sheet of the present invention and the method of producing the same can measure the chromaticity of a phosphor sheet in a liquid phase in a composition containing a phosphor and a resin. Therefore, the curing step of the liquid composition can be dispensed with, and the phosphor sheet can be evaluated or manufactured simply and in a short time. In addition, since the material (composition) provided in the evaluation method can be reused, the yield is good.

1A is a process drawing (plan view) showing a first embodiment of a method for evaluating a phosphor sheet of the present invention. FIG. 1A is a substrate preparation process, FIG. 1B is a dam arrangement process, .
2A is a cross-sectional view corresponding to FIG. 1A, FIG. 2B is a cross-sectional view corresponding to FIG. 1B, FIG. 2C is a cross-sectional view corresponding to FIG. 1C .
3A is a process drawing (side view) showing a second embodiment of a method of evaluating a phosphor sheet of the present invention. Fig. 3A is a substrate preparation process, Fig. 3B is a spacer arrangement process, 3D shows a cover placing process, and Fig. 3E shows a measuring process.
4A to 4C of Fig. 4 are process charts showing one embodiment of the method for producing a phosphor sheet of the present invention, Fig. 4A shows a release type substrate preparation process, Fig. 4B shows a coating process, and Fig. 4C shows a sheet formation process.
5 is a schematic view for explaining the step of measuring the chromaticity in the first embodiment.

1A to 1C, the upper side of the drawing is referred to as the front side (one side in the first direction), the lower side of the drawing is referred to as the rear side (the other side in the first direction), the left side of the drawing is referred to as the left side (one side in the second direction) (One side in the third direction, one side in the thickness direction) and the inside of the paper is the lower side (the other side in the third direction and the other side in the thickness direction). 2A to 5 are also based on the directions of Figs. 1A to 1C.

[Evaluation method of phosphor sheet]

(First Embodiment)

A first embodiment of a method for evaluating a phosphor sheet in the present invention comprises a substrate preparation step, an identification step, a dam arrangement step, an injection step, a planarization step and a measurement step.

First, as shown in Figs. 1A and 2A, a substrate 1 is prepared (substrate preparation step).

The substrate 1 is formed of an insulating substrate, and is formed into a substantially rectangular flat plate shape when viewed in plan view, as shown in Fig. 1A. On the right front side and the left rear side of the base material 1, a piercing cutout is formed in a substantially U-shape on the inside.

The base material 1 has a plurality of (nine) optical semiconductor elements 2 and a plurality (two) of electrodes 3 on its upper surface (upper surface).

The optical semiconductor element 2 is, for example, a light emitting element (specifically, a blue LED or the like) that emits light such as blue light. The optical semiconductor element 2 is formed in a substantially rectangular shape in plan view and mounted on the base material 1. [ The optical semiconductor elements 2 are arranged and arranged substantially at the center of the upper surface of the substrate 1 in the front-rear direction (three rows) and in the left-right direction (three rows) with an interval therebetween.

The height of the optical semiconductor element 2 is, for example, 50 占 퐉 or more, preferably 100 占 퐉 or more, for example, 500 占 퐉 or less, and preferably 400 占 퐉 or less. The distance between the optical semiconductor elements 2 is, for example, 0.1 mm or more, preferably 1 mm or more, and is, for example, 10 mm or less, preferably 5 mm or less.

The electrode 3 is formed in a substantially rectangular shape extending in the left-right direction. The two electrodes 3 are arranged so as to face the optical semiconductor element 2 and sandwich the optical semiconductor elements 2 therebetween so as to face each other in the longitudinal direction.

The height of the electrode 3 is, for example, 1 占 퐉 or more, preferably 3 占 퐉 or more, and is, for example, 50 占 퐉 or less, preferably 30 占 퐉 or less.

The optical semiconductor element 2 is wire-bonded to the electrode 3. Concretely, the wires 4 connect terminals (not shown) provided on the upper surface of the optical semiconductor element 2 adjacent in the front-rear direction, and also connect the terminals of the optical semiconductor element 2 and the light And the semiconductor element 2 and the electrode 3 adjacent in the front-rear direction are connected. Thereby, the optical semiconductor element 2 is electrically connected to the electrode 3 via the wire 4.

Subsequently, as shown by the imaginary line in Figs. 1A and 2A, after the substrate preparing step, the sealing area 5 is confirmed or determined (confirmation step).

As shown by the imaginary lines in Figs. 1A and 2A, in the encapsulation area 5, when the optical semiconductor element 2 is encapsulated by the phosphor sheet (reference numeral 6 in Fig. 4C which will be described later), the phosphor sheet 6 ) Is brought into contact with the upper surface of the base material (1).

The encapsulation area 5 is divided into a substantially rectangular shape at the approximate center of the upper surface of the base material 1 in the plan view and is arranged so as to include all the optical semiconductor elements 2 and a part of the electrodes 3 .

Next, as shown in Fig. 1B and Fig. 2B, a damper 7 as a spacer is disposed on the upper surface of the substrate 1. As shown in Fig.

The dam member 7 is formed in a substantially rectangular frame-like shape when viewed in plan view, and is formed in a shape surrounding the encapsulation area 5 in plan view when disposed on the upper surface of the base material 1. More specifically, the inner shape of the damper 7 is formed in the same shape as the encapsulation area 5 or larger than the encapsulation area 5 in plan view.

The damper 7 is formed of a transparent or semitransparent rubber such as silicone rubber, acrylic rubber, butyl rubber, nitrile rubber, chloroprene rubber, urethane rubber, natural rubber, styrene-butadiene rubber and the like .

The damper 7 is disposed on the upper surface of the base material 1 so as to surround the sealing area 5. At this time, the damper 7 is disposed so as not to create a gap between the upper surface of the base material 1 and the upper surface and the side surface of the electrode 3.

The height (length in the vertical direction) of the damper 7 is appropriately determined in accordance with the height or the like of the optical semiconductor element 2 and is set to, for example, one or more times, 1.5 times or more, for example, 20 times or less, preferably 15 times or less. Specifically, it is, for example, 100 占 퐉 or more, preferably 150 占 퐉 or more, and is, for example, 2000 占 퐉 or less, preferably 1500 占 퐉 or less.

The width of the rim of the damper 7 is, for example, 0.5 mm or more, preferably 1 mm or more, and is, for example, 10 mm or less, preferably 5 mm or less.

The area (internal area) enclosed by the dam member 7 is, for example, 1.0 to 1.2 times the area of the sealing area 5.

Subsequently, as shown in Figs. 1C and 2C, the liquid composition 8 is injected to the inside of the dam member up to a predetermined height (injection step).

In this step, first, the liquid composition (8) is prepared.

The liquid composition (8) contains a phosphor and a resin.

As the fluorescent substance, for example, a yellow fluorescent substance capable of converting blue light into yellow light can be given. Examples of such a fluorescent material include a fluorescent material doped with a metal atom such as cerium (Ce) or europium (Eu), for example, in a composite metal oxide or a metal sulfide.

Specific examples of the fluorescent material include Y ₃ Al ₅ O ₁₂ : Ce (YAG (yttrium aluminum garnet) Ce), (Y, Gd) ₃ Al ₅ O ₁₂ : Ce, Tb ₃ Al ₃ O ₁₂ (Sr, Ba) ₂ SiO (Ce, Ca ₃ Sc ₂ Si ₃ O ₁₂ : Ce, Lu ₂ CaMg ₂ (Si, Ge) ₃ O ₁₂ : Ce) _{4: Eu, Ca 3 SiO 4} Cl 2: Eu, Sr 3 SiO 5: Eu, Li 2 SrSiO 4: Eu, Ca 3 Si 2 O 7: example a silicate phosphor, for example, such as Eu CaAl ₁₂ O _19: Mn, SrAl ₂ O _4: example of the aluminate phosphor, for example, such as Eu ZnS: Cu, Al, CaS : Eu, CaGa 2 S 4: Eu, SrGa 2 S 4: e. sulfide phosphor, for example, such as Eu CaSi ₂ O ₂ N _2: such as _{Eu: Eu, SrSi 2 O 2} N 2: Eu, BaSi 2 O 2 N 2: Eu, Ca-α-SiAlON oxynitride phosphor, such as, for example, _{CaAlSiN 3: Eu, CaSi 5 N} 8 Nitride phosphors such as K ₂ SiF ₆ : Mn, K ₂ TiF ₆ : Mn, and the like. Preferably a garnet fluorescent material, more preferably Y ₃ Al ₅ O ₁₂ : Ce.

Such a fluorescent material may be used singly or in combination.

The phosphor is particulate, and its shape is not particularly limited, and examples thereof include a substantially spherical shape, a substantially flat plate shape, and a substantially needle shape.

The average particle size (average of the maximum length) of the phosphor is, for example, 0.1 μm or more, preferably 0.2 μm or more, more preferably 1 μm or more, and more preferably 500 μm or less, Or less. The average particle size of the phosphor particles is measured by a particle size distribution measuring apparatus.

The density of the phosphor is, for example, 1.0 g / cm ³ or more, preferably 2.0 g / cm ³ or more, and 8.0 g / cm ³ or less, preferably 6.0 g / cm ³ or less.

The content ratio of the phosphor is appropriately adjusted so that the light emitted from the optical semiconductor element 2 and passing through the phosphor sheet 6 becomes white and is added to the liquid composition 8 in an amount of, for example, 1% by mass or more, 2 mass% or more, for example, 50 mass% or less, preferably 30 mass% or less.

The resin is, for example, a transparent encapsulating resin used as an encapsulating material for encapsulating the optical semiconductor element 2, and examples of the encapsulating resin include a thermoplastic resin that is plasticized by heating, for example, For example, an active energy ray-curable resin which is cured by irradiation with active energy rays (for example, ultraviolet ray, electron beam, or the like).

Examples of the thermoplastic resin include vinyl acetate resin, ethylene-vinyl acetate copolymer (EVA), vinyl chloride resin, EVA-vinyl chloride resin copolymer and the like.

Examples of the curable resin such as a thermosetting resin and an active energy ray-curable resin include a silicone resin, an epoxy resin, a polyimide resin, a phenol resin, a urea resin, a melamine resin, and an unsaturated polyester resin.

As such encapsulating resin, a curable resin such as a thermosetting resin and an active energy ray-curable resin may be preferably used, and a thermosetting resin is more preferable, and a silicone resin is more preferable.

Examples of the encapsulating resin composition containing a silicone resin as the encapsulating resin include a thermosetting silicone resin composition such as a two-step curing-type silicone resin composition and a first-stage curing-type silicone resin composition.

The two-step curable silicone resin composition is a thermosetting silicone resin having a two-step reaction mechanism and being B-staged (semi-cured) in the first-step reaction and C-staged (fully cured) in the second-step reaction . On the other hand, the one-stage curing-type silicone resin is a thermosetting silicone resin which has a one-step reaction mechanism and is completely cured in the first-step reaction.

The B stage is a state in which the thermosetting silicone resin composition is in a state between the liquid phase A stage and the fully cured C stage and the cure and gelation proceed slightly and the elastic modulus is smaller than the elastic modulus of the C stage.

Examples of the uncured product (before curing in the first step) of the two-step curable silicone resin composition include a condensation reaction / addition reaction curable silicone resin composition.

The condensation reaction / addition reaction curable silicone resin composition is a thermosetting silicone resin composition capable of undergoing a condensation reaction and an addition reaction by heating, more concretely, a condensation reaction can be carried out by heating to form a B stage (semi-cured) (Fully cured) by an additional reaction (specifically, hydrosilylation reaction) by heating the same to give a thermosetting silicone resin composition.

Examples of such a condensation reaction / addition reaction curable silicone resin composition include a first silicone resin composition containing a siloxane endopoly polysiloxane, an alkenyl group-containing trialkoxysilane, an organohydrogensiloxane, a condensation catalyst, and a hydrosilylation catalyst Condensation reaction and addition reaction A curing type silicone resin composition such as a polysiloxane having a silanol group, a silicon compound containing an ethylenically unsaturated hydrocarbon group, an epoxy group-containing silicon compound, an organohydrogensiloxane, a condensation catalyst and an addition catalyst (hydrosilylation A second condensation reaction / addition reaction curing type silicone resin composition containing a catalyst, for example, a siloxane type silicone oil having a single terminal group, an alkenyl group-containing dialkoxyalkylsilane, an organohydrogensiloxane, a condensation catalyst and a hydrosilylation catalyst A third condensation reaction / addition reaction curable silicone resin composition containing A fourth condensation reaction / addition reaction containing an organopolysiloxane having at least two alkenylsilyl groups in one molecule, an organopolysiloxane having at least two hydrosilyl groups in one molecule, a hydrosilylation catalyst and a curing retarder A curable silicone resin composition, for example, a composition comprising at least two ethylenically unsaturated hydrocarbon groups and at least two hydrosilyl groups in one molecule and not containing a first organopolysiloxane or ethylenically unsaturated hydrocarbon group, A fifth condensation reaction / addition reaction curing type silicone resin composition containing a second organopolysiloxane in a molecule, a hydrosilylation catalyst and a hydrosilylation inhibitor, for example, at least two ethylenically unsaturated hydrocarbon groups and at least two silanol groups And a first organopolysiloxane , A sixth condensation reaction / addition reaction curing type silicone resin composition containing a second organopolysiloxane not containing an ethylenically unsaturated hydrocarbon group and having at least two hydrosilyl groups in one molecule, a hydrosilylation inhibitor and a hydrosilylation catalyst , A seventh condensation reaction / addition reaction curing type silicone resin composition containing, for example, a silicon compound, and a boron compound or an aluminum compound, for example, a polycondensation reaction and a polycondensation reaction containing a polyaluminosiloxane and a silane coupling agent A reactive curing type silicone resin composition and the like.

These condensation reaction / addition reaction curable silicone resin compositions may be used alone or in combination of two or more.

Examples of the first-stage curable silicone resin composition include an addition curing-type silicone resin composition.

The addition reaction-curable silicone resin composition contains, for example, an ethylenically unsaturated hydrocarbon group-containing polysiloxane to be a main agent and an organohydrogensiloxane to be a crosslinking agent.

The content of the resin is, for example, not less than 30 mass%, preferably not less than 50 mass%, and not more than 85 mass%, preferably not more than 75 mass%, for example, with respect to the liquid composition (8).

On the other hand, the liquid composition (8) may contain a filler in an appropriate ratio, if necessary.

Examples of the filler include silicon fine particles, glass, alumina, silica (fused silica, crystalline silica, ultrafine crystalline amorphous silica and hydrophobic ultra fine silica), titania, zirconia, talc, clay, barium sulfate, These fillers may be used alone or in combination of two or more. Preferably silicon fine particles.

The silicon fine particles are fine particles of a polysiloxane (after curing) having a crosslinking structure, and examples thereof include polysilsesquioxane fine particles. In consideration of hardness (reinforcing effect), preferably, the polymethylsilsesquioxane fine particles . Thereby, the hardness of the liquid composition 8 can be improved, and the luminance of the optical semiconductor element device can be improved.

The refractive index of the silicon fine particle is, for example, 1.39 or more, preferably 1.40 or more, and is, for example, 1.43 or less, preferably 1.42 or less.

The average particle size (average of the maximum length) of the filler is, for example, not less than 0.2 탆, preferably not less than 0.5 탆, and is, for example, not more than 40 탆, preferably not more than 10 탆.

The average particle size of the filler is measured by a particle size distribution measuring apparatus.

The content of the filler is, for example, not less than 10% by mass, preferably not less than 20% by mass and not more than 50% by mass, and preferably not more than 40% by mass, relative to the liquid composition (8).

To the liquid composition 8, known additives such as a modifier, a surfactant, a dye, a pigment, an anti-discoloration agent, and an ultraviolet absorber may be added in an appropriate ratio.

To the liquid composition 8, known additives such as a silane coupling agent, an anti-aging agent, a modifier, a surfactant, a dye, a pigment, an anti-discoloration agent, and an ultraviolet absorber may be added in an appropriate ratio, if necessary.

In order to prepare the liquid composition (8), the above-mentioned components are compounded in the above mixing ratio and mixed.

The mixing conditions are, for example, 10 占 폚 or higher, preferably 15 占 폚 or higher, and, for example, 40 占 폚 or lower, preferably 35 占 폚 or lower.

Further, the liquid composition (8) is defoamed, if necessary, after its preparation.

Examples of the defoaming method include a known defoaming method such as stirring defoaming, vacuum defoaming (vacuum defoaming), centrifugal defoaming, and ultrasonic defoaming.

The viscosity of the liquid composition 8 is, for example, 0.1 Pa · s or more, preferably 1 Pa · s or more at 25 ° C., for example, 10 Pa · s or less, s or less.

The density of the liquid composition (8) is, for example, and 0.8g / cm ³ or more, preferably 1.0g / cm ³ or more, and, for example 5.0g / cm ³ or less, preferably 4.0g / cm ³ Or less.

Subsequently, the liquid composition 8 is injected into the inside of the damper 7. Specifically, the liquid composition 8 is injected into the encapsulation area 5 so as to have a predetermined height.

Examples of the method of injecting the liquid composition 8 include coating, spraying, dropping, and the like.

The liquid composition 8 is preferably injected so as to cover the optical semiconductor element 2 and the wire 4.

The height of the injected liquid composition 8 (the distance from the upper surface of the substrate 1 to the upper surface of the liquid composition 8) is the thickness of the desired phosphor sheet. Specifically, the height is equal to or lower than the height of the damper 7, and is, for example, 300 占 퐉 or more, preferably 500 占 퐉 or more, and is, for example, 5000 占 퐉 or less, preferably 2000 占 퐉 or less.

The height of the liquid composition 8 can be measured with a laser displacement meter (LT-9030M, manufactured by KEITH).

Then, the upper surface (upper surface) of the liquid composition 8 is made flat (planarization step, not shown).

The planarization process may be, for example, a method of setting the liquid composition 8 for a predetermined time, a method of making the upper surface of the liquid composition 8 uniform by using a jig such as tweezers, and the like. Preferably, the liquid composition 8 is allowed to stand for a predetermined time.

The settling time is, for example, less than the time required for the phosphor to precipitate in the liquid composition (8). That is, after the implantation step, the measurement step is performed before the phosphor in the liquid composition 8 is settled.

The settling time is preferably set so that the time required for the phosphor to precipitate in the liquid composition 8 at a distance of 100 m from the upper surface of the liquid composition 8 (that is, until a supersaturated layer of 100 m is formed Of the time). Hereinafter, this time is referred to as the " permitted time Tmax ".

The time during which the phosphor precipitates is appropriately determined according to the kind of the phosphor and the liquid composition 8, and is determined, for example, by the following Stokes equation.

Vs: termination speed (m / s)

Dp: Particle size of the phosphor (m)

ρp: density of phosphor (kg / m ³ )

? f: density (kg / m ³ ) of the liquid composition (8)

?: viscosity (Pa · s) of the liquid composition (8)

g: weight acceleration (m / s ² )

Then, the permissible standing time Tmax is calculated from the above equation by the following equation.

Tmax = 0.000184? / {Dp ² (? P-? F)}

More specifically, the settling time is preferably set to be shorter than the allowable settling time Tmax, and is set to, for example, 1 minute or longer, preferably 5 minutes or longer, for example, 10 hours or shorter, preferably 1 hour or shorter to be.

On the other hand, in the injection step, the liquid composition 8 may be injected to a predetermined height at a time, or it may be injected by dividing the liquid composition 8 in several steps, and the step of injecting may be performed between the injection steps.

Thereby, it is possible to obtain the measurement sample 20 having the base material 1, the damper 7 disposed on the base material 1, and the liquid composition 8 injected into the inside of the damper 7.

Then, the chromaticity of the liquid composition 8 at a predetermined height is measured (measurement step).

The chromaticity CIE value of the liquid composition 8 is measured by, for example, emitting light from the optical semiconductor element 2 of the measurement sample 20 and measuring light transmitted through the liquid composition 8. [

As a method of measuring the chromaticity of the liquid composition 8, for example, there is a method of measurement by a total luminous flux measuring system using an integrating hemisphere. Specifically, this will be described later in Examples.

The chromaticity CIE value is appropriately determined according to the kind of the phosphor to be used. For example, when a red phosphor is used as the phosphor, it is, for example, 0.300 to 0.400.

Then, the chromaticity of the liquid composition 8 obtained by the above measuring step is regarded as the chromaticity of the phosphor sheet 6 (described later), and the chromaticity of the phosphor sheet 6 is evaluated. That is, the chromaticity of the liquid composition 8 is taken as the chromaticity of the phosphor sheet 6.

This evaluation method is suitably used as a method of evaluating a phosphor sheet for directly forming a phosphor sheet on a substrate on which an optical semiconductor element is mounted.

(Modification of First Embodiment)

In the embodiment of Fig. 1A, the optical semiconductor element 2 is connected to the electrode 3 by wire bonding. For example, although not shown, the optical semiconductor element 2 is flip-chip mounted on the substrate 1 .

Although the planarization process is performed in the embodiment of Figs. 1A to 1C, the planarization process can be performed immediately after the implantation process, for example, although not shown.

In the evaluation method of the first embodiment, a planarization step is preferably performed. Thereby, the chromaticity of the liquid composition 8 having a uniform surface can be measured, and the chromaticity of the phosphor sheet 6 can be more accurately evaluated.

In the embodiment of Figs. 1A to 1C, after the dam arrangement process, the weighing process of the base material 1 may be performed while the subsequent injection process and measurement process are performed.

In the evaluation method of the first embodiment, preferably, the injection step and the measurement step are carried out while the weight of the base material 1 is measured. According to this embodiment, the weight of the liquid composition 8 injected by the injection step can be accurately measured. Therefore, in carrying out the next evaluation method, when preparing the liquid composition (8), the weight of the liquid composition (8) measured in the previous time can be referred to, and an accurate evaluation method can be continuously performed have.

As a method for measuring the weight of the base material 1, for example, there can be mentioned a method of placing the base material 1 on a weight measuring instrument such as a balance.

Although not shown in the evaluation method of the first embodiment, a cover arranging step of disposing a transparent cover on the upper surface of the damper 7 so as to cover the liquid composition 8 immediately before or after the planarizing step .

The transparent cover has a transparent flat plate shape, and its outer periphery is formed in the same shape as the outer periphery of the damper 7 when projected in the thickness direction. The transparent cover is formed of, for example, glass.

(Second Embodiment)

3A to 3E, members similar to those of the first embodiment of Figs. 1A to 1C are denoted by the same reference numerals, and the details thereof are omitted.

The second embodiment of the evaluation method of the phosphor sheet 6 in the present invention comprises a substrate preparation step, a spacer arrangement step, an injection step, a cover arrangement step and a measurement step.

First, as shown in Fig. 3A, a substrate 1a is prepared (substrate preparation step).

The base material 1a is a base material on which an optical semiconductor element is not mounted, has a transparent flat plate shape, and is formed of, for example, glass.

Subsequently, as shown in Fig. 3B, the spacers 14 are arranged on the upper surface of the base material 1a. The substrate 1a may be subjected to a releasing treatment.

The spacer 14 of the second embodiment may be the damper 7 of the first embodiment or may be of a different shape than the damper 7 of the first embodiment. That is, for example, the spacers 14 of the second embodiment may be two rod-like members sandwiching the liquid composition 8 and disposed opposite to each other.

The height (vertical length) of the spacer 14 is, for example, 100 占 퐉 or larger, preferably 150 占 퐉 or larger, and is, for example, 2000 占 퐉 or smaller, preferably 1500 占 퐉 or smaller. The width of the spacer 14 is, for example, 0.5 mm or more, preferably 1 mm or more, and is, for example, 10 mm or less, preferably 5 mm or less.

The spacers 14 are formed of transparent or translucent rubber or the like as illustrated in the damper 7.

Next, as shown in Fig. 3C, the liquid composition 8 is injected to the inside of the spacer 14 to a predetermined height (injection step).

The method of injecting the liquid composition 8 is the same as that of the liquid composition 8 of the first embodiment.

Preferably, the liquid composition 8 is injected into the interior of the spacer 14 so as to be at the same height as or higher than the spacer 14.

The height of the injected liquid composition 8 (the distance from the upper surface of the substrate 1a to the upper surface of the liquid composition 8) is the thickness of the desired phosphor sheet. Specifically, it is 300 탆 or more, preferably 500 탆 or more, for example, 5000 탆 or less, and preferably 2,000 탆 or less.

Next, as shown in Fig. 3D, the transparent cover 9 is disposed so as to be in contact with the upper surface of the liquid composition 8 at a predetermined height (cover arranging step).

Specifically, the transparent cover 9 is arranged to be in contact with the upper surface of the spacer 14. Thereby, the upper surface of the liquid composition 8 comes into contact with the lower surface of the transparent cover 9.

The transparent cover 9 has a transparent flat plate shape and is formed in the same shape as the base material 1a when projected in the thickness direction. The transparent cover 9 is formed of, for example, glass.

Thereby, the base material 1a, the spacer 14 disposed on the base material 1a, the liquid composition 8 injected into the spacer 14, and the transparent cover (not shown) disposed on the upper surface of the spacer 14 9 can be obtained.

Next, as shown in Fig. 3E, the chromaticity of the liquid composition 8 at a predetermined height is measured (measurement step).

For example, the chromaticity CIE-y value of the liquid composition 8 is measured by irradiating the measurement specimen 20a with predetermined light and measuring the light transmitted through the measurement specimen 20a.

Specifically, the light transmitting portion 10 is disposed above the transparent cover 9, and the light receiving portion 11 is disposed below the base material 1a. Then, the excitation light 12 is irradiated from the transparent portion 10 toward the liquid composition 8. Then, the measurement can be performed by measuring the excitation light 12 passing through the liquid composition 8 and received by the light-receiving unit 11.

By considering the value of the chromaticity CIE (in particular, the CIE-y value) of the liquid composition 8 obtained by this measuring step as the value of the chromaticity CIE of the phosphor sheet 6 (in particular, the CIE-y value) And the value of the chromaticity CIE of the sheet 6 is evaluated. That is, the value of the chromaticity CIE of the liquid composition 8 is taken as the value of the chromaticity CIE of the phosphor sheet 6.

This evaluation method can be suitably used as a method of evaluating a transfer-use phosphor sheet for transferring to a substrate on which an optical semiconductor element is mounted to seal an optical semiconductor element.

This evaluation method can also be suitably used as a method for evaluating the encapsulating phosphor sheet including the optical semiconductor element and the phosphor sheet for encapsulating the optical semiconductor element. The encapsulant phosphor sheet is transferred to a substrate, so that the optical semiconductor device can be mounted on the substrate and the optical semiconductor device in which the phosphor sheet is encapsulated in the optical semiconductor element.

(Modification of Second Embodiment)

In the embodiment of Figs. 3A to 3E, the cover arranging step is performed. However, a measurement step can be performed after the injection step, for example, although not shown, without performing the cover arranging step.

In the evaluation method of the second embodiment, a cover arrangement step is preferably carried out. Thereby, the chromaticity of the liquid composition 8 having a uniform surface can be measured, and the chromaticity of the phosphor sheet 6 can be more accurately evaluated.

[Production method of phosphor sheet]

The method for producing the phosphor sheet 6 in the present invention includes an evaluation step, a crystal step, a preparation step and a formation step.

First, the aforementioned evaluation method is performed (evaluation step).

Subsequently, the composition of the liquid composition 8 is determined based on the above-described evaluation method (the first embodiment or the second embodiment) (crystal step). That is, this evaluation method is repeatedly carried out while changing the composition (such as the content of the phosphor) of the liquid composition 8. Then, the optimum composition (such as the content of the phosphor) for achieving the desired chromaticity is determined.

The respective components and blending of the liquid composition 8 and the chromaticity of the liquid composition 8 are as described above.

Subsequently, the liquid composition 8 is prepared again according to the determined composition of the liquid composition 8 (preparation process). The method of preparing the liquid composition (8) is the same as the preparation method described above.

Subsequently, the liquid composition is formed into a sheet (forming step).

4A), a step of applying the liquid composition 8 onto the release substrate 13 (Fig. 4B), and a step of curing the liquid composition 8 (Fig. 4C). Thus, the phosphor sheet 6 can be produced from the liquid composition 8.

As the release substrate 13, for example, a polyester film (for example, a polyethylene terephthalate film), a polycarbonate film, a polyolefin film (for example, a polyethylene film or a polypropylene film), a polystyrene film, , A fluororesin film, and the like.

On the other hand, on the upper surface of the release substrate 13 (the surface on the side where the phosphor sheet 6 is formed), a releasing treatment is carried out if necessary in order to increase releasability from the phosphor sheet 6.

The thickness of the release substrate 13 is not particularly limited, but is 20 to 100 m, for example, from the viewpoints of handleability and cost.

As a coating method, a known coating method such as an applicator, a cast, a spin, and a roll may be used.

The curing method (semi-curing or fully curing) is determined depending on the type of the resin contained in the liquid composition 8, for example, when the resin is a thermosetting resin, heating.

The heating conditions are determined depending on the type of the thermosetting resin. For example, when the resin is the second-stage curable silicone resin composition and the semi-cured (B-stage) phosphor sheet 6 is produced, for example, the temperature is 80 ° C or higher, preferably 110 ° C or higher , For example, 200 占 폚 or lower, and preferably 180 占 폚 or lower. The heating time is 1 minute or longer, preferably 5 minutes or longer, and is, for example, 1 hour or shorter, preferably 0.5 hour or shorter.

When the resin is the first-stage curable silicone resin composition and the phosphor sheet of the fully cured state (C stage) is produced, the heating temperature is, for example, 80 DEG C or higher, preferably 100 DEG C or higher, For example, 200 DEG C or lower, preferably 180 DEG C or lower. The heating time is, for example, 5 minutes or longer, preferably 10 minutes or longer, and is, for example, 10 hours or shorter, preferably 5 hours or shorter.

The thickness of the obtained phosphor sheet 6 is, for example, 100 占 퐉 or more, preferably 200 占 퐉 or more, and, for example, 2000 占 퐉 or less, preferably 1500 占 퐉 or less.

This phosphor sheet 6 is used, for example, in applications such as optical electronic devices, and specifically, can be used as a sealing sheet for sealing the optical semiconductor element 2. [ Particularly, it can be suitably used for a white light semiconductor device which emits white light by providing a blue LED and converting blue light.

According to the evaluation method of the phosphor sheet 6, the chromaticity of the phosphor sheet 6 formed of the liquid composition 8 can be evaluated by measuring the chromaticity of the liquid composition 8. That is, the value of the chromaticity of the liquid composition 8 can be equal to the value of the chromaticity of the phosphor sheet 6.

This is because the liquid crystal composition 8 is semi-cured or fully cured by heating or the like to produce the phosphor sheet 6, and the present inventors have found that the liquid composition 8 and the semi-cured or completely cured (For example, the CIE-y value) is substantially not changed. That is, it is found that the chromaticity of the liquid composition 8 can be regarded as the chromaticity of the phosphor sheet 6.

Therefore, in the evaluation of the phosphor sheet 6, the phosphor sheet 6 can be evaluated without the curing step of the liquid composition 8, and the phosphor sheet 6 can be evaluated easily and in a short time. In addition, since the material (composition) provided in the evaluation method can be reused as it is, the yield is good.

According to the method for producing the phosphor sheet 6, the composition of the liquid composition 8 is determined based on the evaluation method, and the phosphor sheet 6 is produced from the liquid composition 8 having this composition. The phosphor sheet 6 can be manufactured easily and in a short time. Also, the yield of the phosphor sheet 6 is good.

(Modification Example of Evaluation Process)

In the above-described embodiment, the composition of the liquid composition 8 is directly determined (that is, determined in advance) based on the above-described evaluation method (the first embodiment or the second embodiment) Although not shown, for example, the composition of the liquid composition may be determined through a precise irradiation process of the liquid composition based on the evaluation method described above. That is, the composition of the liquid composition may be tentatively determined based on the above-described evaluation method, and the composition of the liquid composition may be determined by precisely irradiating the tentatively determined liquid composition.

In this modified example, first, the composition of the liquid composition is tentatively determined based on the evaluation method described above (a tentative fixing step). Specifically, the above-described evaluation method is repeated while changing the composition of the liquid composition (the content of the phosphor, etc.). Then, the optimum composition (the content of the phosphor, etc.) for achieving the desired chromaticity is determined.

The respective components and blending of the liquid composition 8 and the chromaticity of the liquid composition 8 are as described above.

Subsequently, the uncertain liquid composition is precisely inspected (precise irradiation step). Concretely, the phosphor sheet 6 (prototype) is started from the liquid composition 8 according to the composition of the temporarily determined liquid composition 8, and the chromaticity of the prototype is evaluated.

When the liquid composition 8 is a composition that can be completely cured (C-staged), the prototype of the C-stage is started (manufactured).

Subsequently, on the basis of the evaluation of the prototype, the composition of the liquid composition 8 is determined (principal determination step). Specifically, when the measured value of the chromaticity of the prototype is within the target range, the composition of the liquid composition 8 is determined. On the other hand, if the measured value of the chromaticity of the prototype is outside the target range, the composition of the liquid composition 8 is modified and determined to be the target chromaticity from the composition and evaluation.

On the other hand, in the present crystal process, the composition of the liquid composition 8 can be determined by considering the relationship between the thickness and chromaticity of the phosphor sheet 6. Specifically, two or more prototypes (for example, a first prototype and a second prototype) are fabricated, a calibration curve is prepared based on the thickness and chromaticity of the first prototype and the second prototype, and based on the calibration curve, The thickness of the phosphor sheet 6 corresponding to the chromaticity is obtained. Then, it is determined whether or not it is possible to produce the phosphor sheet 6 having the target chromaticity by adjusting the thickness of the phosphor sheet. When it is determined as possible, the composition is determined. More specifically, the method described in, for example, Japanese Patent Application Laid-Open No. 2014-96491 can be determined by reference.

In this modified example, since the phosphor sheet 6 (prototype) is actually started, the phosphor sheet 6 having the target chromaticity can be manufactured more accurately.

Example

EXAMPLES The present invention will be described in more detail with reference to the following examples and comparative examples, but the present invention is not limited to them at all. The numerical values of the embodiments shown below can be replaced with the numerical values described in the above embodiments (that is, the upper limit value or the lower limit value).

(Example 1)

As the substrate 1, an insulating substrate 1 shown in Figs. 1A and 2A (outer dimensions of 22 mm x 20 mm) was prepared. On the other hand, nine blue LEDs (optical semiconductor elements 2, height 150 m) are mounted at substantially equal intervals of three rows by three rows at the center of the substrate 1, and these nine blue LEDs are arranged in the front- Two electrodes 3 (height 1 mu m) were arranged.

Subsequently, as shown by the imaginary line in Figs. 1A and 2A, the encapsulation area 5 is divided into a plane of 13.5 mm in the forward and backward direction and 12.5 mm in the left and right direction so as to include a part of the nine blue LEDs and the electrode 3 It was decided to be rectangular.

Next, as the damper 7, the size of the inner rim is 13.5 mm (forward and backward length) x 12.5 mm (lateral length) x 700 um (height), and the size of the outer rim is 15.5 mm mm (length in the left-right direction) × 700 μm (height). As shown in Figs. 1B and 2B, the damper 7 is formed so that the upper surface of the substrate 1, the upper surface and the side surface of the electrode 3 are spaced apart from each other by a gap (not shown) so that the inner rim thereof coincides with the outer periphery of the sealing area 5 Place it so that it does not occur.

Subsequently, 0.38 g of a YAG fluorescent substance ("YAG432", particle diameter of 8.9 μm, density of 4.5 (g / cm ³ ), Nemoto LUMMaterial Co., (Silicone resin) and 3.00 g of silicone microparticles ("TOUSPLE 2000B", Momentive Performance Materials Japan Co., Ltd.) were mixed and stirred for 5 minutes with a spatula, followed by stirring with Mazerusta Followed by stirring and defoaming for 3 minutes to prepare a liquid composition (8). The viscosity (25 캜) of the liquid composition 8 was 2 Pa · s and the density was 1.2 g / cm ³ .

Subsequently, as shown in Figs. 1C and 2C, the liquid composition 8 was injected into the sealing area 5 inside the damper 7 by a syringe until a height of 600 mu m from the upper surface of the substrate 1 .

At this time, the liquid composition 8 was allowed to stand for 10 minutes until the upper surface of the liquid composition 8 became flat. On the other hand, since the allowable settling time Tmax was calculated to be 369 hours from the above-described Stokes equation, the settled time was within the allowable settled time. The base material 1 into which the liquid composition 8 was injected into the dam member 7 to a height of 600 mu m was used as the measurement sample 20.

Then, the chromaticity of the measurement sample 20 was measured using a whole-beam measuring system.

5, the liquid composition 8 is placed on the lowest side of the integral hemispherical unit 22 (trade name: 150 mm general purpose compact integrate, manufactured by Lap Spares) so that the liquid material composition 8 is on the bottom side and the base material 1 is on the bottom side And the measurement sample 20 was placed.

The integral hemispherical unit 22 has a diameter of 150 mm, the inner surface of its hemispherical portion 22a is a specular surface treated with barium sulfate, and the inner surface of the cap portion 22b is a specular surface treated with aluminum. The cap portion 22b is provided with a small window 23 for receiving light at a position 7.5 mm away from the center thereof.

Then, the measurement sample 20 was made to emit light at a voltage of 9 V and a current of 0.02 A. The light emitted from the measurement sample 20 is received by the light receiving head 24 through the light receiving window 23. [ The received light was detected by a spectrophotometer (trade name: MC-9800, manufactured by OTSUKA ELECTRONICS CO., LTD.) Connected to the light-receiving head 24 (not shown) to obtain the chromaticity CIE-y value. The chromaticity CIE-y value at this time was 0.319.

Example 2

The liquid composition (8) of Example 2 was prepared in the same manner as in Example 1 except that 0.48 g of the phosphor, 6.52 g of the silicone resin and 3.00 g of the silicon fine particles were blended with the liquid composition (8) of Example 1.

The same procedure as in Example 1 was carried out except that the liquid composition (8) of Example 2 was used, and the chromaticity CIE-y value of the liquid composition (8) was determined. The chromaticity CIE-y value was 0.352.

Example 3

A liquid composition (8) of Example 3 was prepared in the same manner as in Example 1 except that 0.58 g of the fluorescent substance, 6.42 g of the silicone resin and 3.00 g of the silicon fine particles were blended with the liquid composition (8) of Example 1.

The same procedure as in Example 1 was carried out except that the liquid composition (8) of Example 3 was used to obtain the chromaticity CIE-y value of the liquid composition (8). The chromaticity CIE-y value was 0.387.

Comparative Example 1

The liquid composition (8) of Example 1 was formed on a sheet having a thickness of 600 mu m using an applicator. Subsequently, heat treatment at 135 占 폚 for 20 minutes was carried out to obtain a semi-cured state. The semi-cured phosphor sheet 6 was cut into a size of 13.5 mm x 12.5 mm. The cut fluorescent material sheet 6 was brought into close contact with the sealing area 5 of the same base material 1 as in Example 1 to seal the optical semiconductor element 2. Then, the chromaticity was measured in the same manner as in Example 1. The chromaticity CIE-y value was 0.319.

Comparative Example 2

The liquid composition (8) of Example 2 was formed on a sheet having a thickness of 600 mu m using an applicator. Subsequently, heat treatment at 135 占 폚 for 20 minutes was carried out to obtain a semi-cured state. The semi-cured phosphor sheet 6 was cut into a size of 13.5 mm x 12.5 mm. The cut fluorescent material sheet 6 was brought into close contact with the sealing area 5 of the same base material 1 as in Example 1 to seal the optical semiconductor element 2. Then, the chromaticity was measured in the same manner as in Example 1. The chromaticity CIE-y value was 0.352.

Comparative Example 3

The liquid composition (8) of Example 3 was formed on a sheet having a thickness of 600 mu m using an applicator. Subsequently, heat treatment at 135 占 폚 for 20 minutes was carried out to obtain a semi-cured state. The semi-cured phosphor sheet 6 was cut into a size of 13.5 mm x 12.5 mm. The cut fluorescent material sheet 6 was brought into close contact with the sealing area 5 of the same base material 1 as in Example 1 to seal the optical semiconductor element 2. Then, the chromaticity was measured in the same manner as in Example 1. The chromaticity CIE-y value was 0.387.

<Review>

From the above results, the chromaticity in the liquid composition was the same as the chromaticity in the semi-cured state. Therefore, it was confirmed that the evaluation of the chromaticity of the phosphor sheet 6 in the semi-cured state was possible by the evaluation method of the present invention.

Example 4

As the substrate 1a, a slide glass was prepared (Fig. 3A).

Next, as the spacer 14, a silicone rubber having an inner rim of 30 mm x 30 mm x 175 m (height) and an outer rim of 31 mm x 31 mm x 175 m (height) was prepared. This spacer 14 was disposed so as not to create a gap on the upper surface of the transparent substrate 1a (Fig. 3B).

2.5 g of a YAG fluorescent substance ("YAG432", particle diameter of 8.9 μm, density of 4.5 (g / cm ³ ), Nemoto LUMI MATERIAL CO., LTD.) And silicone resin ("LR7665", addition reaction curing type silicone resin composition, manufactured by Asahi Kasei ), And the mixture was stirred with a spatula for 5 minutes and then subjected to stirring defoaming with Mazerusta (Kurabo Industries, Ltd.) for 3 minutes to prepare a liquid composition (8) of Example 4.

Subsequently, the liquid composition 8 was taken out with a syringe and injected into the spacer 14 until the height became 175 mu mm (Fig. 3C).

Next, as the transparent cover 9, the same slide glass as that of the transparent substrate 1a was prepared and disposed so as to contact the upper surface of the spacer 14 (Fig. 3D). The transparent base material 1a into which the liquid composition 8 was injected into the spacer 14 to a height of 175 mu m was used as a measurement sample 20a.

Then, the chromaticity of this measurement specimen 20a was measured.

Specifically, as shown in Fig. 3E, the transparent portion 10 is disposed above the transparent cover 9, and the light receiving portion 11 (light receiving head) is disposed below the transparent substrate 1a. As the light source here, an inspection LED (manufactured by CISCO) was used. A spectrophotometer (trade name: MC-9800, manufactured by OTSUKA ELECTRONICS CO., LTD.) Was used as a measuring instrument for measuring the excitation light 12 received by the transparent portion 10. The spot size of the transparent portion 10 was 1 mm and the distance from the transparent portion 10 to the upper surface of the liquid composition 8 was 1 mm.

Then, the excitation light 12 (447 nm, half-width of 20 nm) was irradiated from the transparent portion 10 toward the liquid composition 8. Subsequently, the excitation light 12 passed through the liquid composition 8 and received by the light receiving section 11 was measured by a spectrophotometer. The chromaticity CIE-y value was 0.358.

Comparative Example 4

The liquid sample 8 is heated and cured on a hot plate at 105 DEG C for 10 minutes before the chromaticity measurement in Example 4 so as to obtain the phosphor sheet 6 of the fully cured state (C stage) (Thickness: 175 mu m).

The chromaticity was measured in the same manner as in Example 4 with respect to the measurement specimen 20a subjected to the heat curing. The chromaticity CIE-y value was 0.355.

<Review>

From the above results, the chromaticity in the liquid composition was within 1% with respect to the chromaticity in the cured phosphor sheet 6, and the chromaticity of both was almost the same. Therefore, it was confirmed that the evaluation of the chromaticity of the phosphor sheet 6 in a cured state was possible by the evaluation method of the present invention.

While the present invention has been described as an exemplary embodiment of the present invention, it is to be understood that the present invention is by no means restricted to such examples. Variations of the invention which will be apparent to those skilled in the art are included in the later claims.

The method for evaluating the phosphor sheet of the present invention and the method for producing the same can be applied to various industrial products, and can be used for optical applications such as white light semiconductor devices.

1: substrate
1a: substrate
2: optical semiconductor element
6: phosphor sheet
7: Damage
8: Liquid composition
9: Transparent cover
14: Spacer

Claims (6)

A method for evaluating a phosphor sheet formed of a liquid composition containing a phosphor and a resin,
A spacer arranging step of disposing a spacer on a substrate,
An injecting step of injecting the liquid composition to a predetermined height into the spacer, and
A measurement step of measuring the chromaticity of the liquid composition at the predetermined height
Wherein the phosphor sheet has a surface roughness of at least 20 占 퐉. The method according to claim 1,
Wherein the substrate has an optical semiconductor element on its surface,
Wherein the liquid composition is injected so as to cover the optical semiconductor element in the injection step. The method according to claim 1,
The method for evaluating a phosphor sheet according to any one of claims 1 to 3, wherein the measurement step is performed before the phosphor precipitates in the liquid composition after the implantation step. The method according to claim 1,
Wherein the substrate is a transparent substrate,
Further comprising a cover placing step of arranging the transparent cover so as to be in contact with the upper surface of the liquid composition at the predetermined height after the injection process and before the measurement process. An evaluation step of performing a method of evaluating a phosphor sheet formed of a liquid composition containing a phosphor and a resin,
A crystallization step of determining the composition of the liquid composition based on the evaluation method,
A preparing step of preparing a liquid composition according to the determined composition of the liquid composition, and
A forming step of forming the liquid composition into a sheet form
And,
The above-
A spacer arranging step of disposing a spacer on a substrate,
An injecting step of injecting the liquid composition to a predetermined height into the spacer, and
A measurement step of measuring the chromaticity of the liquid composition at the predetermined height
Wherein the phosphor sheet is formed on the surface of the phosphor sheet. 6. The method of claim 5,
And a step of determining the composition of the liquid composition by precisely irradiating the preliminarily determined liquid composition on the basis of the evaluation method and determining the composition of the liquid composition .

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