JP2007045683A - Glass powder for use in electrode support rod, electrode support rod, and manufacturing method for them - Google Patents

Glass powder for use in electrode support rod, electrode support rod, and manufacturing method for them Download PDF

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JP2007045683A
JP2007045683A JP2005234168A JP2005234168A JP2007045683A JP 2007045683 A JP2007045683 A JP 2007045683A JP 2005234168 A JP2005234168 A JP 2005234168A JP 2005234168 A JP2005234168 A JP 2005234168A JP 2007045683 A JP2007045683 A JP 2007045683A
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glass
electrode support
glass powder
support rod
powder
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Seiichi Hanada
誠一 花田
Shigehiko Fujizu
成彦 藤津
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Nippon Electric Glass Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide an electrode support rod which is free from the occurrence of chipping or breaking even when heated for the purpose of inserting an electrode thereinto. <P>SOLUTION: The method for manufacturing a glass powder for an electrode support rod comprises a process of melting a glass raw material, a process of solidifying the molten glass, a process of pulverizing the resultant glass into a powder and a process of classifying the glass powder, characterized by choosing, in the glass powder classification process, the glass powder having a particle diameter of 200 μm or less; and the glass powder for an electrode support rod is manufactured by using a manufacturing method comprising a process of melting a glass raw material, a process of solidifying the molten glass, a process of pulverizing the glass into a powder, a process of classifying the glass powder, characterized by choosing, in the classification process, the glass powder having a particle diameter of 200 μm or less. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、電極支持棒用ガラス粉末、電極支持棒およびそれらの製造方法に関するものである。   The present invention relates to a glass powder for an electrode support bar, an electrode support bar, and a method for producing them.

陰極線管は、フェイスパネル、ファンネルおよびネック管が封着され、フェイスパネルの内面に塗布された蛍光体に、ネック管に配設された電子銃から電子を放射することで蛍光体が発光して画像を表示するディスプレイ装置である。   A cathode ray tube has a face panel, a funnel and a neck tube sealed, and the phosphor emits light by emitting electrons from the electron gun disposed on the neck tube to the phosphor applied to the inner surface of the face panel. A display device that displays an image.

電子銃は、次のようにしてネック管に固定される。まず、ネック管の内表面に固定されたガラス製の電極支持棒を加熱軟化して、電極を電極支持棒の内部に挿通し、固定する。その後、電子銃を電極から通電できるようにネック管内に装着し、固定する。   The electron gun is fixed to the neck tube as follows. First, the glass electrode support rod fixed to the inner surface of the neck tube is heated and softened, and the electrode is inserted into the electrode support rod and fixed. Thereafter, the electron gun is mounted and fixed in the neck tube so that electricity can be applied from the electrode.

電極支持棒は、以下のようにして作製される。   The electrode support rod is produced as follows.

まず、所定のガラス組成となるようにガラス原料を溶融炉で溶融した後、溶融ガラスを溶融炉から流し出してガラスを固化させる。   First, after melting a glass raw material in a melting furnace so as to have a predetermined glass composition, the molten glass is poured out of the melting furnace to solidify the glass.

次に、固化したガラスを粉砕し、分級してガラス粉末を作製する。   Next, the solidified glass is pulverized and classified to produce glass powder.

最後に、ガラス粉末に有機バインダーや顔料を加えて顆粒状に造粒し、金型に充填してプレス成形した後、焼成して電極支持棒を作製する（例えば、特許文献１参照。）。   Finally, an organic binder or pigment is added to glass powder, granulated into granules, filled in a mold, press-molded, and fired to produce an electrode support rod (see, for example, Patent Document 1).

このような用途には、例えば、質量％表示でＳｉＯ2 ７４〜８５％、Ｂ2Ｏ3 １４〜２５％、Ｒ2Ｏ（Ｒ＝Ｌｉ、ＮａおよびＫ） ０．０５〜５％、ＭｇＯ ０〜０．５％、Ａｌ2Ｏ3 ０．２〜０．９％の成分を含有するガラス粉末が使用される（特許文献２参照。）。
特開２００１−１８０９７３号公報 特開２００１−１８０９６８号公報 For such applications, for example, SiO 2 74 to 85%, B 2 O 3 14 to 25%, R 2 O (R = Li, Na and K) 0.05 to 5% in terms of mass%, MgO 0 Glass powder containing components of ˜0.5% and Al 2 O 3 0.2 to 0.9% is used (see Patent Document 2).
JP 2001-180973 A JP 2001-180968 A

電極支持棒には、電極を挿通するために加熱軟化する際に折れたり欠けたりしないことが要求されるが、加熱した際に折れたり欠けたりする場合があった。   The electrode support rod is required not to be broken or chipped when heated and softened in order to pass through the electrode, but may be folded or chipped when heated.

本発明は、電極を挿通するために加熱しても折れや欠けが発生しない電極支持棒を提供することを目的とする。   An object of the present invention is to provide an electrode support rod that does not break or chip even when heated to insert an electrode.

本発明者等は、上記事情を鑑みて鋭意検討を行なった結果、電極支持棒用ガラス粉末に、ガラス原料の未溶解物や侵食された溶融炉の耐火物が混入している場合があり、これが電極支持棒の折れや欠けの原因となっていることと、混入した未溶解物や耐火物の粒径が２００μｍ以下であると折れや欠けが発生しないことを突き止め、本発明として提案するものである。   As a result of intensive studies in view of the above circumstances, the present inventors may have mixed unmelted glass raw materials and eroded melting furnace refractories in the electrode support rod glass powder, Ascertaining that this is the cause of breakage and chipping of the electrode support rod, and that no breakage or chipping occurs when the particle size of the mixed undissolved material or refractory is 200 μm or less, and is proposed as the present invention. It is.

すなわち、本発明の電極支持棒用ガラス粉末の製造方法は、ガラス原料を溶融する工程、溶融ガラスを固化する工程、ガラスを粉砕して粉末にする工程およびガラス粉末を分級する工程を備え、ガラス粉末の分級工程において粒径が２００μｍ以下のガラス粉末を選択することを特徴とする。   That is, the method for producing a glass powder for an electrode support bar of the present invention comprises a step of melting a glass raw material, a step of solidifying molten glass, a step of crushing glass into powder, and a step of classifying glass powder. In the powder classification step, glass powder having a particle size of 200 μm or less is selected.

また、本発明の電極支持棒用ガラス粉末は、ガラス原料を溶融する工程、溶融ガラスを固化する工程、ガラスを粉砕して粉末にする工程およびガラス粉末を分級する工程を備え、分級工程において粒径２００μｍ以下のガラス粉末を選択する製造方法を用いて製造されたことを特徴とする。   The glass powder for electrode support rods of the present invention comprises a step of melting a glass raw material, a step of solidifying molten glass, a step of crushing glass into powder, and a step of classifying glass powder. It was manufactured using the manufacturing method which selects the glass powder of a diameter of 200 micrometers or less.

また、本発明の電極支持棒の製造方法は、ガラス原料を溶融する工程、溶融ガラスを固化する工程、ガラスを粉砕して粉末にする工程およびガラス粉末を分級する工程を含有し、ガラス粉末の分級工程において粒径２００μｍ以下のガラス粉末を選択する製造方法を用いて製造された電極支持棒用ガラス粉末に有機バインダーを添加して攪拌することによって均一なスラリーを作製する工程、スラリーを噴霧・乾燥してガラス粉末顆粒を作製する工程、金型にガラス粉末顆粒を充填しプレス成形して電極支持棒の前駆体を作製する工程および前駆体を焼成する工程を備えることを特徴とする。   In addition, the method for producing an electrode support rod of the present invention includes a step of melting a glass raw material, a step of solidifying molten glass, a step of crushing glass into powder, and a step of classifying glass powder. A step of preparing a uniform slurry by adding an organic binder to the glass powder for an electrode support bar manufactured using a manufacturing method for selecting a glass powder having a particle size of 200 μm or less in the classification step, and spraying the slurry The method includes a step of producing glass powder granules by drying, a step of filling a glass powder granule in a mold and press-molding to produce a precursor of an electrode support rod, and a step of firing the precursor.

また、本発明の電極支持棒は、ガラス原料を溶融する工程、溶融ガラスを固化する工程、ガラスを粉砕して粉末にする工程およびガラス粉末を分級する工程を含有し、ガラス粉末の分級工程において粒径２００μｍ以下のガラス粉末を選択する製造方法を用いて製造された電極支持棒用ガラス粉末に有機バインダーを添加して攪拌することによって均一なスラリーを作製する工程、スラリーを噴霧・乾燥してガラス粉末顆粒を作製する工程、金型にガラス粉末顆粒を充填しプレス成形して電極支持棒の前駆体を作製する工程および前駆体を焼成する工程を備える製造方法を用いて製造されたことを特徴とする。   The electrode support rod of the present invention includes a step of melting a glass raw material, a step of solidifying molten glass, a step of crushing glass into powder and a step of classifying glass powder. The step of preparing a uniform slurry by adding an organic binder to the glass powder for electrode support rods produced by using the production method for selecting a glass powder having a particle size of 200 μm or less, and stirring and spraying and drying the slurry It was manufactured using a manufacturing method including a step of manufacturing glass powder granules, a step of filling a glass powder granule into a mold and press forming to prepare a precursor of an electrode support rod, and a step of firing the precursor. Features.

本発明の電極支持棒は、粒径が２００μｍ以下のガラス粉末を用いて作製されるため、加熱しても折れや欠けが発生しない。   Since the electrode support rod of the present invention is produced using glass powder having a particle size of 200 μm or less, it does not break or chip even when heated.

溶融炉から流し出したガラスにはガラス原料の未溶解物、例えばシリカやアルミナ、または溶融炉から侵食された耐火物が混入していることがある。   Glass that has flowed out of the melting furnace may contain unmelted glass raw materials such as silica and alumina, or refractory eroded from the melting furnace.

ガラス中に未溶解物や耐火物が存在した状態でガラス粉末に粉砕すると、ガラスよりも未溶解物や耐火物の方が硬いため粉砕されにくく、大きな粒径のまま残存しやすい。   When pulverized into glass powder in the presence of undissolved material or refractory in glass, the undissolved material or refractory is harder than glass because it is harder than glass and tends to remain as a large particle size.

これまで、ガラス中に未溶解物や耐火物が存在していても、ガラス粉末を製造する工程ではｍｍ単位のように粗大な粒子以外は取り除かれることはなかったが、本発明では粉末に粉砕した後に分級することで粒径が２００μｍよりも大きな未溶解物や耐火物が取り除かれる。未溶解物や耐火物とガラス粉末との熱膨張係数の差が、加熱時に折れや欠けが発生する原因となるため、折れや欠けの発生を防止することができる。   So far, even if undissolved materials and refractories existed in the glass, in the process of producing the glass powder, particles other than coarse particles such as mm have not been removed. Then, the unclassified substance and the refractory having a particle size larger than 200 μm are removed by classification. Since the difference in thermal expansion coefficient between the undissolved material or refractory and the glass powder causes breakage or chipping during heating, the occurrence of folding or chipping can be prevented.

なお、粒径が２００μｍ以下の未溶解物や耐火物は、折れや欠けを発生させるほど大きな歪が生じない。   It should be noted that undissolved materials and refractories having a particle size of 200 μm or less are not so strained as to cause breakage or chipping.

ガラス粉末の粒径を２００μｍ以下にするために、篩を用いる。ガラス粉末の粒径は１８０μｍ以下であるとより好ましく、１５０μｍ以下であるとさらに好ましい。   A sieve is used to make the particle size of the glass powder 200 μm or less. The particle size of the glass powder is more preferably 180 μm or less, and further preferably 150 μm or less.

ガラス粉末のＤ50は、１０〜３０μｍであることが好ましい。１０μｍよりも小さいと粉砕に時間やコストがかかるとともに取り扱いにくくなるため好ましくない。また、３０μｍよりも大きいと電極支持棒の前駆体の空隙が大きくなるため前駆体の強度が低く破損しやすい。 D 50 of the glass powder is preferably 10 to 30 [mu] m. If it is smaller than 10 μm, it takes time and cost for pulverization and is difficult to handle. On the other hand, if it is larger than 30 μm, the gap of the precursor of the electrode support rod becomes large, so the strength of the precursor is low and it is easily damaged.

本発明の電極支持棒用ガラス粉末の製造方法について説明する。   The manufacturing method of the glass powder for electrode support bars of this invention is demonstrated.

まず、ガラス原料を所定の組成となるように調合し、アルミナ耐火物等で内壁が覆われた溶融炉に投入し、１６００℃程度で溶融する。   First, a glass raw material is prepared so as to have a predetermined composition, charged into a melting furnace whose inner wall is covered with an alumina refractory or the like, and melted at about 1600 ° C.

次に、溶融ガラスを溶融炉から流し出し、固化した後に粗粉砕して粒径２〜３ｍｍ程度のカレットを作製する。   Next, the molten glass is poured out of the melting furnace, solidified and then coarsely pulverized to produce a cullet having a particle size of about 2 to 3 mm.

続いて、カレットを、ボールミル、ハンマーミル、磨砕器等を用いてＤ50が１０〜３０μｍとなるように粉砕する。 Subsequently, the cullet is pulverized using a ball mill, a hammer mill, a grinder or the like so that D 50 is 10 to 30 μm.

最後に、前記粉砕物を目間隔が例えば１５０μｍの篩を通して、所望の粒径を有するガラス粉末を作製する。   Finally, the pulverized product is passed through a sieve having a mesh interval of, for example, 150 μm to produce a glass powder having a desired particle size.

次に、電極支持棒の作製方法について説明する。   Next, a method for producing an electrode support rod will be described.

上述したガラス粉末に有機バインダーや顔料を添加して均一に攪拌してスラリーを作製し、スラリーを噴霧・乾燥してＤ50が１１０〜１８０μｍのガラス粉末顆粒を作製する。 An organic binder and a pigment are added to the glass powder described above and uniformly stirred to prepare a slurry, and the slurry is sprayed and dried to prepare glass powder granules having a D 50 of 110 to 180 μm.

続いて、金型にガラス粉末顆粒を充填し、プレス成形して電極支持棒の前駆体を作製する。   Subsequently, the mold is filled with glass powder granules and press-molded to prepare an electrode support rod precursor.

最後に、前駆体を９００〜１０００℃で焼成し、脱バインダーして電極支持棒を作製する。   Finally, the precursor is calcined at 900 to 1000 ° C. and debindered to produce an electrode support rod.

なお、ガラス粉末の組成は、質量％表示でＳｉＯ2 ７４〜８５％、Ｂ2Ｏ3 １４〜２５％、Ｒ2Ｏ（Ｒ＝Ｌｉ、ＮａおよびＫ） ０．０５〜５％、ＭｇＯ ０〜０．５％、Ａｌ2Ｏ3 ０．２〜０．９％の成分を含有すると熱膨張係数や軟化点等の点から好ましい。 The composition of the glass powder, SiO 2 seventy-four to eighty-five% represented by mass%, B 2 O 3 14~25%, R 2 O (R = Li, Na and K) 0.05 to 5%, MgO 0 to Containing components of 0.5% and Al 2 O 3 0.2 to 0.9% is preferable from the viewpoint of thermal expansion coefficient and softening point.

以下、本発明を実施例および比較例を用いて詳細に説明する。   Hereinafter, the present invention will be described in detail using examples and comparative examples.

［実施例］
まず、質量％表示でＡｌ2Ｏ3 ０．３％、ＳｉＯ2 ７５％、Ｂ2Ｏ3 ２０％、Ｎａ2Ｏ ４．０％、Ｋ2Ｏ ０．７％の組成となるようにガラス原料を調合し、白金ルツボに投入し、電気炉において１６００℃で３時間放置し、溶融ガラスとした。 [Example]
First, a glass raw material having a composition of Al 2 O 3 0.3%, SiO 2 75%, B 2 O 3 20%, Na 2 O 4.0%, K 2 O 0.7% in terms of mass%. Was put into a platinum crucible and allowed to stand at 1600 ° C. for 3 hours in an electric furnace to obtain molten glass.

次に、溶融ガラスをカーボン板の上に流し出し、固化した後に粒径が２〜３ｍｍ程度となるように粗粉砕してカレットを作製した。   Next, the molten glass was poured out on a carbon plate, solidified, and then coarsely pulverized so as to have a particle size of about 2 to 3 mm to prepare a cullet.

続いて、前記カレットをボールミルを用いて平均粒径１０μｍ程度まで粉砕してガラス粉末を作製し、目開きが１５０μｍの篩を用いて篩を通過したガラス粉末を収集した。   Subsequently, the cullet was pulverized to an average particle size of about 10 μm using a ball mill to produce a glass powder, and the glass powder that passed through the sieve was collected using a sieve having an opening of 150 μm.

前記ガラス粉末を６００ｇ、純水を７００ｇおよびポリエチレングリコールを３０ｇ添加して攪拌混合してスラリーを作製し、スプレードライヤーを用いて前記スラリーを噴霧乾燥し、平均粒径が１５０μｍ程度の顆粒を作製した。   600 g of the glass powder, 700 g of pure water and 30 g of polyethylene glycol were added and mixed by stirring to prepare a slurry, and the slurry was spray-dried using a spray drier to prepare granules having an average particle size of about 150 μm. .

最後に、前記顆粒を金型に充填してからプレス成形し、その成形体を９７０℃において焼成することによって電極支持棒（４×４×４０ｍｍ）を１０本作製した。   Finally, the granules were filled into a mold and press-molded, and the molded body was fired at 970 ° C., thereby producing 10 electrode support bars (4 × 4 × 40 mm).

［比較例１］
実施例で作製したガラス粉末に平均粒径２５０μｍのシリカを３ｇ添加した以外は実施例と同様の手順で電極支持棒を１０本作製した。なお、シリカ粉末の添加は、未溶解物の混入を再現したものである。 [Comparative Example 1]
Ten electrode support bars were prepared in the same procedure as in the example except that 3 g of silica having an average particle size of 250 μm was added to the glass powder prepared in the example. The addition of silica powder reproduces the mixing of undissolved substances.

［比較例２］
目開きが５００μｍの篩を用いた以外は実施例と同様の手順で電極支持棒を１０本作製した。 [Comparative Example 2]
Ten electrode support bars were produced in the same procedure as in the example except that a sieve having an opening of 500 μm was used.

各電極支持棒をバーナーで９７０℃まで加熱した後、水中に投入して折れや欠けを評価した。   Each electrode support rod was heated to 970 ° C. with a burner and then poured into water to evaluate breakage and chipping.

実施例は、１０本の電極支持棒において全く「折れ」や「欠け」が見られなかったのに対して、比較例１は６本の電極支持棒において、比較例２では２本の電極支持棒において「折れ」または「欠け」が発生した。   In the example, no “folding” or “chip” was found in the 10 electrode support bars, whereas in Comparative Example 1, 6 electrode support bars were used, and in Comparative Example 2, 2 electrode supports were supported. A “break” or “chip” occurred in the bar.

Claims (4)

ガラス原料を溶融する工程、溶融ガラスを固化する工程、ガラスを粉砕して粉末にする工程およびガラス粉末を分級する工程を備え、分級工程において粒径が２００μｍ以下のガラス粉末を選択することを特徴とする電極支持棒用ガラス粉末の製造方法。   It comprises a step of melting a glass raw material, a step of solidifying molten glass, a step of crushing glass into powder and a step of classifying glass powder, and selecting a glass powder having a particle size of 200 μm or less in the classification step A method for producing a glass powder for an electrode support bar. 請求項１に記載の電極支持棒用ガラス粉末の製造方法を用いて製造されたことを特徴とする電極支持棒用ガラス粉末。   A glass powder for an electrode support bar produced by the method for producing a glass powder for an electrode support bar according to claim 1. 請求項２に記載の電極支持棒用ガラス粉末に有機バインダーを添加して攪拌することによって均一なスラリーを作製する工程、スラリーを噴霧・乾燥してガラス粉末顆粒を作製する工程、金型にガラス粉末顆粒を充填しプレス成形して電極支持棒の前駆体を作製する工程および前駆体を焼成する工程を備えることを特徴とする電極支持棒の製造方法。   A step of preparing a uniform slurry by adding an organic binder to the glass powder for an electrode support bar according to claim 2 and stirring, a step of spraying and drying the slurry to prepare a glass powder granule, a glass in a mold A method for producing an electrode support rod, comprising: a step of filling a powder granule and press-molding to prepare a precursor of an electrode support rod; and a step of firing the precursor. 請求項３に記載の電極支持棒の製造方法を用いて製造されたことを特徴とする電極支持棒。   An electrode support bar manufactured using the method for manufacturing an electrode support bar according to claim 3.
JP2005234168A 2005-08-12 2005-08-12 Glass powder for use in electrode support rod, electrode support rod, and manufacturing method for them Pending JP2007045683A (en)

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