JP5786756B2 - Method for producing phosphor powder - Google Patents
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Description
本発明は、蛍光体粉末の製造方法に関する。 The present invention relates to a method for producing a phosphor powder.
従来の蛍光体粉末の製造方法として、蛍光体粉末又はその原料化合物に炭素を添加し、還元することにより、原料化合物に含有される酸素を除去する方法が知られている（例えば、特許文献１、２参照）。 As a conventional method for producing a phosphor powder, a method of removing oxygen contained in a raw material compound by adding carbon to the phosphor powder or its raw material compound and reducing it is known (for example, Patent Document 1). 2).
特許文献１によれば、ＡｌＮ：Ｅｕ、Ｓｉ蛍光体を製造した後、ＡｌＮ：Ｅｕ、Ｓｉ蛍光体に対して０．０３〜０．１ｗｔ％の高純度カーボンを添加し、アニール処理を行う。
According to
また、特許文献２によれば、蛍光体の原料混合物を焼成する際に、炭素若しくは炭素含有化合物からなる容器、発熱体、又は断熱材から生じる微量の炭素を蛍光体の原料混合物に添加する。
According to
一般に、所望の粒径の蛍光体粉末を得るためには、製造した蛍光体粉末を分級し、所望の粒径を有する粒子を選出する。このとき、所望したものと異なる粒径を有する粒子は、通常、廃棄されるため、製造した蛍光体粉末の粒径のばらつきが大きいほど蛍光体粉末の歩留まりが低下し、製造コストが高くなる。そのため、蛍光体粉末は、粒径が小さいだけでなく、ばらつきが小さいことが求められる。 In general, in order to obtain a phosphor powder having a desired particle size, the produced phosphor powder is classified, and particles having a desired particle size are selected. At this time, since particles having a particle size different from that desired are usually discarded, the larger the variation in the particle size of the manufactured phosphor powder, the lower the yield of the phosphor powder and the higher the manufacturing cost. Therefore, the phosphor powder is required not only to have a small particle size but also to have a small variation.
そこで、本発明の目的は、粒径が小さく、かつ粒径のばらつきの小さい蛍光体粉末を製造することにある。 Accordingly, an object of the present invention is to produce a phosphor powder having a small particle size and a small variation in particle size.
上記目的を達成するため、本発明の一態様は、蛍光体原料に炭素原料として粉末状のＣを３０ｍｏｌ％以上添加して前駆体を形成する工程と、
前記前駆体を焼成し、蛍光体粉末を得る工程と、
を含み、
前記焼成の直後の前記蛍光体粉末の粒度分布における、体積基準のアンダーサイズ累積が９０％の粒径であるＤ９０と１０％の粒径であるＤ１０との差が、前記蛍光体粉末がＣａＡｌＳｉＮ ３ ：Ｅｕの粉末である場合は４１μｍ以下であり、（Ｂａ，Ｓｒ） ２ ＳｉＯ ４ ：Ｅｕの粉末である場合は５０μｍ以下であることにより、前記蛍光体粉末に粉砕処理及び分級処理を施さない、
蛍光体粉末の製造方法を提供する。
In order to achieve the above object, one embodiment of the present invention includes a step of forming a precursor by adding 30 mol% or more of powdery C as a carbon raw material to a phosphor raw material,
Firing the precursor to obtain a phosphor powder;
Including
In the particle size distribution of the phosphor powder immediately after the firing, the difference between D90 having a particle size with a volume-based undersize accumulation of 90% and D10 having a particle size of 10% is that the phosphor powder is CaAlSiN 3. : 41 μm or less in the case of Eu powder, (Ba, Sr) 2 SiO 4 : 50 μm or less in the case of Eu powder, so that the phosphor powder is not subjected to pulverization and classification,
A method for producing a phosphor powder is provided.
前記蛍光体粉末がＣａＡｌＳｉＮ ３ ：Ｅｕの粉末である場合の前記Ｄ９０とＤ１０との差が、２８μｍ以下であってもよい。 The difference between D90 and D10 when the phosphor powder is CaAlSiN 3 : Eu powder may be 28 μm or less.
前記蛍光体粉末がＣａＡｌＳｉＮ ３ ：Ｅｕの粉末である場合の前記Ｄ９０とＤ１０との差が、２０μｍ以下であってもよい。 The difference between D90 and D10 in the case where the phosphor powder is CaAlSiN 3 : Eu powder may be 20 μm or less.
本発明によれば、粒径が小さく、かつ粒径のばらつきの小さい蛍光体粉末を製造することができる。 According to the present invention, a phosphor powder having a small particle size and a small variation in particle size can be produced.
〔実施の形態〕
図１は、実施の形態に係る蛍光体粉末の製造工程を表すフローチャートである。蛍光体粉末は、例えば、窒化物を母物質とするＣａＡｌＳｉＮ３：Ｅｕ等の窒化物蛍光体や、酸化物を母物質とする（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ等の酸化物蛍光体の粉末である。以下、図１のフローチャートに従って、蛍光体粉末の製造工程について説明する。
Embodiment
FIG. 1 is a flowchart showing a manufacturing process of a phosphor powder according to an embodiment. The phosphor powder is, for example, a nitride phosphor such as CaAlSiN 3 : Eu using nitride as a base material, or an oxide phosphor such as (Ba, Sr) 2 SiO 4 : Eu using oxide as a base material. It is a powder. Hereinafter, the manufacturing process of the phosphor powder will be described with reference to the flowchart of FIG.
まず、蛍光体の原料、及び炭素原料を化学量論比に従って秤量する（ステップＳ１）。 First, the phosphor raw material and the carbon raw material are weighed according to the stoichiometric ratio (step S1).
炭素原料として粉末状のＣを用いる場合は、蛍光体の原料に対して１０ｍｏｌ％以上の炭素原料を混合することが好ましく、蛍光体の原料に対して３０ｍｏｌ％以上の炭素原料を混合することがより好ましい。炭素原料として粉末状のＣ３Ｎ４を用いる場合は、蛍光体の原料に対して１０ｍｏｌ％以上の炭素原料を混合することが好ましい。また、炭素原料としてチップ状のＣを用いる場合は、蛍光体の原料に対して１０ｍｏｌ％以上の炭素原料を混合することが好ましい。 When powdered C is used as the carbon material, it is preferable to mix 10 mol% or more of the carbon material with respect to the phosphor material, and to mix 30 mol% or more of the carbon material with respect to the phosphor material. More preferred. When powdered C 3 N 4 is used as the carbon material, it is preferable to mix 10 mol% or more of the carbon material with respect to the phosphor material. Further, when chip-like C is used as the carbon raw material, it is preferable to mix 10 mol% or more of the carbon raw material with respect to the phosphor raw material.
次に、秤量した蛍光体の原料及び炭素原料を混合して前駆体を形成する（ステップＳ２）。 Next, a precursor is formed by mixing the weighed phosphor material and carbon material (step S2).
次に、前駆体をルツボに入れて電気炉で加熱し、焼成して、蛍光体粉末を得る（ステップＳ３）。焼成条件は、温度、時間、圧力が、それぞれ１６００〜２３００℃、１〜２４時間、０〜１ＭＰａであることが好ましい。また、Ｎ２ガス等の不活性ガス雰囲気下で焼成を行うことが好ましい。 Next, the precursor is put in a crucible, heated in an electric furnace, and baked to obtain a phosphor powder (step S3). As for the firing conditions, the temperature, time, and pressure are preferably 1600 to 2300 ° C., 1 to 24 hours, and 0 to 1 MPa, respectively. Moreover, it is preferable to perform baking in an inert gas atmosphere such as N 2 gas.
本実施の形態に係る蛍光体粉末は、焼成直後の粒径のばらつきが小さい（粒度分布の均一性が高い）ため、最終的に得られる蛍光体粉末の粒径のばらつきも小さい。そのため、分級により除外され、廃棄される粉末が少なく、蛍光体粉末の歩留まりが高い。その結果、蛍光体粉末の製造コストを下げることができる。さらに、焼成後の粒径のばらつきが十分に小さい場合は、分級工程を省略することができる。 Since the phosphor powder according to the present embodiment has a small variation in particle size immediately after firing (high uniformity of particle size distribution), the variation in the particle size of the finally obtained phosphor powder is also small. Therefore, there are few powders that are excluded and discarded by classification, and the yield of the phosphor powder is high. As a result, the manufacturing cost of the phosphor powder can be reduced. Furthermore, when the particle size variation after firing is sufficiently small, the classification step can be omitted.
炭素の添加により蛍光体粉末の粒径のばらつきが小さくなる機構は明らかではないが、焼成時に炭化物や炭酸化物等の炭素含有化合物が生成され、蛍光体の粒成長を阻害することによると推測される。 The mechanism by which the variation in the particle size of the phosphor powder is reduced by the addition of carbon is not clear, but it is presumed that carbon-containing compounds such as carbides and carbonates are generated during firing and inhibit the phosphor grain growth. The
炭素の添加により蛍光体粉末の粒径のばらつきが小さくなるという効果は、酸化物蛍光体よりも、窒化物蛍光体において顕著に現れる。これは、酸化物蛍光体においては、一部の炭素が酸化物の還元に用いられることによると考えられる。すなわち、一部の炭素が酸素と結合して二酸化炭素等として排出されるため、炭素含有化合物の生成量が少なくなり、窒化物蛍光体の場合ほどには粒成長が阻害されないものと考えられる。 The effect that the variation in the particle size of the phosphor powder is reduced by the addition of carbon is more noticeable in the nitride phosphor than in the oxide phosphor. This is considered to be due to the fact that part of carbon is used for oxide reduction in oxide phosphors. In other words, since a part of carbon is combined with oxygen and discharged as carbon dioxide or the like, the amount of carbon-containing compound produced is reduced, and it is considered that grain growth is not inhibited as much as in the case of a nitride phosphor.
なお、蛍光体粉末の粒径のばらつきを小さくするためには、還元により酸素を除去するために用いられる炭素原料の量（例えば、粉末状のＣで蛍光体の原料に対して０．０３〜０．１ｗｔ％）では不十分である。これは、微量の炭素では炭素含有化合物がほとんど生成されず、粒成長が阻害されないためと考えられる。 In order to reduce the variation in the particle size of the phosphor powder, the amount of the carbon raw material used for removing oxygen by reduction (for example, 0.03 to 0.03 of the phosphor raw material in the form of powder C). 0.1 wt%) is insufficient. This is presumably because a very small amount of carbon produces almost no carbon-containing compound and does not inhibit grain growth.
蛍光体粉末の粒径のばらつきの指標として、Ｄ９０とＤ１０の差であるＤ９０−Ｄ１０の値を用いることができる。ここで、Ｄ９０は、体積基準のアンダーサイズ累積（粒径の小さいものからの累計）が９０％での粒径を表し、Ｄ１０は、体積基準のアンダーサイズ累積が１０％での粒径を表す。Ｄ９０−Ｄ１０の値が小さいほど、粒径のばらつきが小さい。 A value of D90-D10 that is a difference between D90 and D10 can be used as an index of variation in particle diameter of the phosphor powder. Here, D90 represents the particle size when the volume-based undersize accumulation (cumulative from the smaller particle size) is 90%, and D10 represents the particle size when the volume-based undersize accumulation is 10%. . The smaller the value of D90-D10, the smaller the variation in particle size.
例えば、蛍光体粉末が窒化物蛍光体粉末である場合のＤ９０−Ｄ１０の値は４１μｍ以下であり、好ましくは２８μｍ以下、より好ましくは２０μｍ以下である。また、蛍光体粉末が酸化物蛍光体粉末である場合のＤ９０−Ｄ１０の値は５０μｍ以下であり、好ましくは４７μｍ以下である。 For example, when the phosphor powder is a nitride phosphor powder, the value of D90-D10 is 41 μm or less, preferably 28 μm or less, more preferably 20 μm or less. Further, when the phosphor powder is an oxide phosphor powder, the value of D90-D10 is 50 μm or less, preferably 47 μm or less.
また、本実施の形態に係る蛍光体粉末は、焼成直後の粒径が小さい。このため、焼成後の蛍光体粉末の粒径が十分に小さく、所望の粒径が得られている場合は、粉砕処理を省略することができる。 Moreover, the phosphor powder according to the present embodiment has a small particle size immediately after firing. For this reason, when the particle size of the phosphor powder after firing is sufficiently small and a desired particle size is obtained, the pulverization treatment can be omitted.
ここで、体積基準のアンダーサイズ累積が５０％での粒径Ｄ５０（メジアン径とも呼ばれる）の値を粒径分布の指標として用いることができる。 Here, the value of the particle diameter D50 (also called the median diameter) when the volume-based undersize accumulation is 50% can be used as an index of the particle size distribution.
例えば、蛍光体粉末が窒化物蛍光体粉末である場合のＤ５０の値は１９μｍ以下であり、好ましくは１５μｍ以下である。また、蛍光体粉末が酸化物蛍光体粉末である場合のＤ５０の値は２４μｍ以下であり、好ましくは２２μｍ以下である。 For example, when the phosphor powder is a nitride phosphor powder, the value of D50 is 19 μm or less, preferably 15 μm or less. Further, when the phosphor powder is an oxide phosphor powder, the value of D50 is 24 μm or less, preferably 22 μm or less.
上記のＤ１０、Ｄ５０、Ｄ９０の値は、蛍光体粉末を解砕した後、レーザー回折・散乱法等により測定することができる。解砕は、粒子の凝集を解く処理であり、粒径を小さくするための粉砕とは異なる。 The values of D10, D50, and D90 can be measured by a laser diffraction / scattering method or the like after pulverizing the phosphor powder. Crushing is a process that breaks up the agglomeration of particles and is different from crushing to reduce the particle size.
次に、蛍光体粉末に粉砕処理を施し、微粒化する（ステップＳ４）。ただし、上述のように、ステップＳ３の焼成直後の蛍光体粉末の粒径が十分に小さく、所望の粒径が得られている場合は、粉砕処理を省略することができる。 Next, the phosphor powder is pulverized and atomized (step S4). However, as described above, when the particle size of the phosphor powder immediately after firing in step S3 is sufficiently small and a desired particle size is obtained, the pulverization process can be omitted.
次に、蛍光体粉末を水又は酸水溶液を用いて洗浄し（ステップＳ５）、乾燥させる（ステップＳ６）。 Next, the phosphor powder is washed with water or an acid aqueous solution (step S5) and dried (step S6).
次に、蛍光体粉末を分級し、所望の粒径を有する粒子を選出する（ステップＳ７）。ただし、上述のように、ステップＳ３の焼成直後の蛍光体粉末の粒径のばらつきが十分に小さく、所望の均一性が得られている場合は、分級処理を省略することができる。 Next, the phosphor powder is classified, and particles having a desired particle diameter are selected (step S7). However, as described above, when the variation in the particle diameter of the phosphor powder immediately after firing in step S3 is sufficiently small and the desired uniformity is obtained, the classification process can be omitted.
実施例１として、上記実施の形態によって製造したＣａＡｌＳｉＮ３：Ｅｕからなる窒化物蛍光体粉末の評価結果を以下に述べる。 As Example 1, the evaluation results of the nitride phosphor powder made of CaAlSiN 3 : Eu manufactured according to the above embodiment will be described below.
実施例１においては、Ｃａ３Ｎ２、ＡｌＮ、Ｓｉ３Ｎ４、及びＥｕ２Ｏ３をＣａＡｌＳｉＮ３：Ｅｕ蛍光体の原料として用いて、粉末状のＣ、チップ状のＣ、及び粉末状のＣ３Ｎ４を炭素原料として用いた。 In Example 1, using Ca 3 N 2 , AlN, Si 3 N 4 , and Eu 2 O 3 as raw materials for the CaAlSiN 3 : Eu phosphor, powder C, chip C, and powder C 3 N 4 was used as a carbon raw material.
以下、実施例１において製造した、炭素原料を添加していないＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末を試料Ａ、１０ｍｏｌ％の粉末状のＣを添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末を試料Ｂ、３０ｍｏｌ％の粉末状のＣを添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末を試料Ｃ、１０ｍｏｌ％の粉末状のＣ３Ｎ４を添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末を試料Ｄ、１８．８ｍｏｌ％のチップ状のＣを添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末を試料Ｅと記載する。 Hereinafter, CaAlSiN 3 : Eu phosphor powder prepared in Example 1 to which no carbon raw material was added was added to sample A, and 10 mol% of powdered C was added to sample B, 30 mol% of CaAlSiN 3 : Eu phosphor powder. CaAlSiN that the addition of powdery C 3: Eu phosphor powder samples C, 10 mol% of powdered C 3 N 4 CaAlSiN 3 with the addition of: Eu phosphor powder sample D, 18.8mol% of the chip- The CaAlSiN 3 : Eu phosphor powder to which C was added is referred to as Sample E.
図２及び図３は、実施例１に係る試料Ａ、Ｂ、Ｃ、Ｄ、Ｅの焼成直後の体積基準の粒度分布を表すグラフである。ここで、図２は頻度分布を表し、図３は累積分布を表す。 2 and 3 are graphs showing the volume-based particle size distribution immediately after firing Samples A, B, C, D, and E according to Example 1. FIG. Here, FIG. 2 represents a frequency distribution, and FIG. 3 represents a cumulative distribution.
図２及び３の粒度分布は、各試料を解砕した後、レーザー回折・散乱法により測定した。測定において、イオン交換水を溶媒として用いた。 The particle size distributions in FIGS. 2 and 3 were measured by a laser diffraction / scattering method after each sample was crushed. In the measurement, ion exchange water was used as a solvent.
図２から、炭素を添加したいずれの蛍光体粉末も、炭素を添加していない蛍光体粉末よりも曲線のピーク位置が小粒径側にあり、また、曲線の形状がシャープである。このことから、炭素を添加したいずれの蛍光体粉末も、炭素を添加していない蛍光体粉末よりも頻度の最も高い粒径が小さく、また、粒径のばらつきが小さいことがわかる。 As can be seen from FIG. 2, in any phosphor powder to which carbon is added, the peak position of the curve is closer to the smaller particle size than the phosphor powder to which no carbon is added, and the shape of the curve is sharp. From this, it can be seen that any phosphor powder to which carbon is added has the smallest frequency of particle size and the variation in particle size is smaller than the phosphor powder to which no carbon is added.
また、各蛍光体粉末のＤ１０、Ｄ５０、Ｄ９０を図３から求めることができる。Ｄ１０、Ｄ５０、Ｄ９０は、それぞれ各曲線における体積基準の累計（％）が１０、５０、９０であるときの粒径（μｍ）である。各蛍光体粉末のＤ１０、Ｄ５０、Ｄ９０、及びＤ９０−Ｄ１０の値（μｍ）を表１に示す。 Further, D10, D50, and D90 of each phosphor powder can be obtained from FIG. D10, D50, and D90 are particle diameters (μm) when the volume-based cumulative (%) in each curve is 10, 50, and 90, respectively. Table 1 shows the values (μm) of D10, D50, D90, and D90-D10 of each phosphor powder.
炭素を添加したいずれのＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末も、炭素を添加していないＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末よりもＤ９０−Ｄ１０の値が小さく、粒径のばらつきが小さいことがわかる。 It can be seen that any CaAlSiN 3 : Eu phosphor powder to which carbon is added has a smaller value of D90-D10 and less variation in particle size than the CaAlSiN 3 : Eu phosphor powder to which no carbon is added.
表１は、炭素を添加した全ての試料、試料Ｂ、Ｃ、Ｄ、ＥのＤ９０−Ｄ１０の値が４１μｍ以下であり、試料Ｃ、Ｄ、ＥのＤ９０−Ｄ１０の値が２８μｍ以下であり、試料ＣのＤ９０−Ｄ１０の値が２０μｍ以下であることを示している。 Table 1 shows that the values of D90-D10 of all the samples added with carbon, samples B, C, D, and E are 41 μm or less, and the values of D90-D10 of samples C, D, and E are 28 μm or less. It shows that the value of D90-D10 of sample C is 20 μm or less.
また、表１は、炭素を添加した全ての試料、試料Ｂ、Ｃ、Ｄ、ＥのＤ５０の値が１９μｍ以下であり、試料ＣのＤ５０の値が１５μｍ以下であることを示している。 Table 1 shows that the D50 values of all the samples to which carbon was added, Samples B, C, D, and E were 19 μm or less, and the D50 value of Sample C was 15 μm or less.
図４は、試料Ａ、Ｂ、Ｃの粒度分布を図１から抜き出したグラフである。 FIG. 4 is a graph obtained by extracting the particle size distribution of Samples A, B, and C from FIG.
図４からわかるように、粉末状のＣの添加量の増加に伴い、曲線のピーク位置が小粒径側にシフトし、また、曲線の形状がシャープになっている。このことから、頻度の最も高い粒径が小さくなり、また、粒径のばらつきが小さくなることがわかる。 As can be seen from FIG. 4, the peak position of the curve shifts to the small particle size side as the amount of powdered C added increases, and the shape of the curve becomes sharper. From this, it can be seen that the most frequent particle size becomes smaller and the variation in particle size becomes smaller.
また、図２からわかるように、粉末状のＣ３Ｎ４を添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末と、チップ状のＣを添加したＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末も、炭素を添加していないＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末よりも、頻度の最も高い粒径が小さく、また、粒径のばらつきが小さい。このことから、粒径のばらつきを小さくするためにＣａＡｌＳｉＮ３：Ｅｕ蛍光体粉末に添加される炭素原料の組成や形状は、限定されないといえる。 Moreover, as can be seen from FIG. 2, CaAlSiN added powdered C 3 N 4 3: Eu as the phosphor powder, CaAlSiN added with chipped C 3: Eu phosphor powder even without the addition of carbon Compared to CaAlSiN 3 : Eu phosphor powder, the most frequent particle size is small and the variation in particle size is small. From this, it can be said that the composition and shape of the carbon raw material added to the CaAlSiN 3 : Eu phosphor powder in order to reduce the variation in particle size are not limited.
実施例２として、上記実施の形態によって製造した（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ（ＢＯＳ）からなる酸化物蛍光体粉末の評価結果を以下に述べる。 As Example 2, the evaluation results of the oxide phosphor powder made of (Ba, Sr) 2 SiO 4 : Eu (BOS) manufactured according to the above embodiment will be described below.
実施例２においては、ＢａＣＯ３、ＳｒＣＯ３、ＳｉＯ２、Ｅｕ２Ｏ３、及び融剤としてのハロゲン化合物を混合したものを（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体の原料として用いて、粉末状のＣを炭素原料として用いた。実施例２において製造した（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体の具体的な組成は、（Ｂａ０．９０Ｓｒ０．１０）１．９２ＳｉＯ４：Ｅｕ０．０８である。 In Example 2, a mixture of BaCO 3 , SrCO 3 , SiO 2 , Eu 2 O 3 and a halogen compound as a flux was used as a raw material for (Ba, Sr) 2 SiO 4 : Eu phosphor, Powdered C was used as a carbon raw material. The specific composition of the (Ba, Sr) 2 SiO 4 : Eu phosphor produced in Example 2 is (Ba 0.90 Sr 0.10 ) 1.92 SiO 4 : Eu 0.08 .
以下、実施例２において製造した、炭素原料を添加していない（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体粉末を試料Ｆ、１０ｍｏｌ％の粉末状のＣを添加した（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体粉末を試料Ｇ、３０ｍｏｌ％の粉末状のＣを添加した（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体粉末を試料Ｈと記載する。 Hereinafter, (Ba, Sr) 2 SiO 4 : Eu phosphor powder produced in Example 2 without addition of carbon raw material was added to sample F, 10 mol% of powdered C (Ba, Sr) 2 SiO 4 : Eu phosphor powder is referred to as sample G, and (Ba, Sr) 2 SiO 4 : Eu phosphor powder added with 30 mol% of powdery C is referred to as sample H.
図５及び図６は、実施例２に係る試料Ｆ、Ｇ、Ｈの焼成直後の体積基準の粒度分布を表すグラフである。ここで、図５は頻度分布を表し、図６は累積分布を表す。 5 and 6 are graphs showing the volume-based particle size distribution immediately after firing Samples F, G, and H according to Example 2. FIG. Here, FIG. 5 represents a frequency distribution, and FIG. 6 represents a cumulative distribution.
図５及び６の粒度分布は、各試料を解砕した後、レーザー回折・散乱法により測定した。測定において、イオン交換水を溶媒として用いた。 The particle size distributions in FIGS. 5 and 6 were measured by laser diffraction / scattering method after crushing each sample. In the measurement, ion exchange water was used as a solvent.
図５からわかるように、粉末状のＣの添加量の増加に伴い、曲線の形状がシャープになっており、粒径のばらつきが小さくなることがわかる。なお、粒径の変化は、実施例１の酸化物蛍光体粉末ほど大きくはない。 As can be seen from FIG. 5, as the amount of powdery C added increases, the shape of the curve becomes sharper and the variation in particle size becomes smaller. The change in particle size is not as great as that of the oxide phosphor powder of Example 1.
また、各蛍光体粉末のＤ１０、Ｄ５０、Ｄ９０を図６から求めることができる。各蛍光体粉末のＤ１０、Ｄ５０、Ｄ９０、及びＤ９０−Ｄ１０の値（μｍ）を表２に示す。 Moreover, D10, D50, and D90 of each phosphor powder can be obtained from FIG. Table 2 shows the values (μm) of D10, D50, D90, and D90-D10 of each phosphor powder.
炭素を添加したいずれの（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体粉末も、炭素を添加していない（Ｂａ，Ｓｒ）２ＳｉＯ４：Ｅｕ蛍光体粉末よりもＤ９０−Ｄ１０の値が小さく、粒径のばらつきが小さいことがわかる。 Any (Ba, Sr) 2 SiO 4 : Eu phosphor powder added with carbon has a smaller value of D90-D10 than (Ba, Sr) 2 SiO 4 : Eu phosphor powder without carbon added, It can be seen that the variation in particle size is small.
表２は、炭素を添加した全ての試料、試料Ｇ、Ｈ、のＤ９０−Ｄ１０の値が５０μｍ以下であり、試料ＨのＤ９０−Ｄ１０の値が４７μｍ以下であることを示している。 Table 2 shows that the values of D90-D10 of all the samples to which carbon was added, samples G and H are 50 μm or less, and the values of D90-D10 of sample H are 47 μm or less.
また、表２は、炭素を添加した全ての試料、試料Ｇ、ＨのＤ５０の値が２４μｍ以下であり、試料ＨのＤ５０の値が２２μｍ以下であることを示している。 Table 2 shows that the D50 values of all the samples to which carbon was added, the samples G and H are 24 μm or less, and the D50 value of the sample H is 22 μm or less.
本発明は、上記の実施の形態及び実施例に限定されず、発明の主旨を逸脱しない範囲内において種々変形実施が可能である。 The present invention is not limited to the embodiments and examples described above, and various modifications can be made without departing from the spirit of the invention.
また、上記の実施の形態及び実施例は特許請求の範囲に係る発明を限定するものではない。また、実施の形態及び実施例の中で説明した特徴の組合せの全てが発明の課題を解決するための手段に必須であるとは限らない点に留意すべきである。 Moreover, said embodiment and Example do not limit the invention which concerns on a claim. It should be noted that not all combinations of features described in the embodiments and examples are necessarily essential to the means for solving the problems of the invention.
Claims (3)
前記前駆体を焼成し、蛍光体粉末を得る工程と、
を含み、
前記焼成の直後の前記蛍光体粉末の粒度分布における、体積基準のアンダーサイズ累積が９０％の粒径であるＤ９０と１０％の粒径であるＤ１０との差が、前記蛍光体粉末がＣａＡｌＳｉＮ ３ ：Ｅｕの粉末である場合は４１μｍ以下であり、（Ｂａ，Ｓｒ） ２ ＳｉＯ ４ ：Ｅｕの粉末である場合は５０μｍ以下であることにより、前記蛍光体粉末に粉砕処理及び分級処理を施さない、
蛍光体粉末の製造方法。 Adding 30 mol% or more of powdered C as a carbon raw material to the phosphor raw material to form a precursor;
Firing the precursor to obtain a phosphor powder;
Including
In the particle size distribution of the phosphor powder immediately after the firing, the difference between D90 having a particle size with a volume-based undersize accumulation of 90% and D10 having a particle size of 10% is that the phosphor powder is CaAlSiN 3. : 41 μm or less in the case of Eu powder, (Ba, Sr) 2 SiO 4 : 50 μm or less in the case of Eu powder, so that the phosphor powder is not subjected to pulverization and classification,
Method for producing phosphor powder.
請求項１に記載の蛍光体粉末の製造方法。 The difference between D90 and D10 when the phosphor powder is CaAlSiN 3 : Eu powder is 28 μm or less,
The manufacturing method of the fluorescent substance powder of Claim 1.
請求項１又は２に記載の蛍光体粉末の製造方法。 The difference between D90 and D10 when the phosphor powder is CaAlSiN 3 : Eu powder is 20 μm or less,
The manufacturing method of the fluorescent substance powder of Claim 1 or 2.
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