JP4876351B2 - Shadow mask oxidation method - Google Patents
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- JP4876351B2 JP4876351B2 JP2001261311A JP2001261311A JP4876351B2 JP 4876351 B2 JP4876351 B2 JP 4876351B2 JP 2001261311 A JP2001261311 A JP 2001261311A JP 2001261311 A JP2001261311 A JP 2001261311A JP 4876351 B2 JP4876351 B2 JP 4876351B2
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【０００１】
【発明の属する技術分野】
本発明は、テレビ、コンピューター等のディスプレーのブラウン管中に用いられるシャドウマスクの処理方法に関するものである。
【０００２】
【従来の技術】
シャドウマスクは、金属薄板をエッチングすることにより製造されている。
金属薄板は、鉄材、鉄−ニッケル合金材、鉄−ニッケル−コバルト合金材が用いられている。いずれの場合でも鉄が材料の主成分である為、輸送や保管の際に多湿な環境であったりすると、錆が生じるという問題がある。
鉄の酸化物には、Ｆｅ2Ｏ3、Ｆｅ3Ｏ4、ＦｅＯ等がある。中でも、Ｆｅ2Ｏ3（赤錆）は、材料との密着力が弱い為、シャドウマスクがブラウン管に用いられた時に、赤錆がブラウン管内部で脱落し、シャドウマスク開孔部の目詰まりを起こすことがある。
これを防止する為に、Ｆｅ2Ｏ3（赤錆）を発生させない様に、脱落しにくい安定な酸化膜であるＦｅ3Ｏ4（黒錆）を優先的にシャドウマスクに形成させる対策（黒化処理）が採択されている。
また、シャドウマスクは、ブラウン管内で不必要な電子を遮る働きを行うが、この時、シャドウマスクが温度上昇し、熱膨張してしまい、画像の色ムラを起こすことがある。
上記温度上昇を防止する為に、熱輻射効率の高いＦｅ3Ｏ4（黒錆）をシャドウマスクに形成させる対策（黒化処理）が採択されている。
【０００３】
黒錆（Ｆｅ3Ｏ4）の形成方法としては、例えば、特開昭６４−３４９２号公報に開示されているように、従来の処理条件として、ＣＯ2、ＣＯの混合ガス中で約５８０℃に加熱すると記載されており、発熱型変性ガス雰囲気中で５００℃を超える温度で加熱するのが一般的である。
【０００４】
【発明が解決しようとする課題】
ところが、上記加熱条件により黒化処理を行うと、黒化膜として要求される熱輻射率≧０．６を得る為に、５０分以上の工業的には長い処理時間を必要とするという問題を有する。
また、混合ガスの組成によっては、Ｆｅ2Ｏ3（赤錆）が発生するという問題がある。
【０００５】
本発明は上記問題点に鑑み考案されたもので、脱落しにくい安定な酸化膜であるＦｅ3Ｏ4（黒錆）を優先的かつ短時間にシャドウマスクに形成するシャドウマスクの酸化処理方法を提供することを目的とする。
【０００６】
【課題を解決するための手段】
上記問題を解決するために、本発明のシャドウマスクの酸化処理方法においては、
シャドウマスクを、露点５０℃とした不活性ガスと水蒸気を含む雰囲気下で加熱処理する工程と、
不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む、露点５０℃とした混成ガスを流した雰囲気下で加熱処理する工程とを備え、
前記不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む雰囲気でのＨ2／Ｈ2Ｏ及びＣＯ／ＣＯ2値の両方が０．０１〜１．０であり、
前記加熱処理を４５０℃〜６５０℃で行うことを特徴とする。
【０００９】
【発明の実施の形態】
本発明のシャドウマスクの酸化処理方法は、シャドウマスクにＦｅ3Ｏ4（黒錆）を優先的に短時間に形成させる方法で、この技術を利用することにより、Ｆｅ2Ｏ3（赤錆）を含まない脱落しにくいＦｅ3Ｏ4（黒錆）からなる黒化膜をシャドウマスク上に優先的に短時間にできることが判明した。
具体的には、シャドウマスクを酸化力の強い不活性ガスと水蒸気を含む雰囲気下で加熱処理し、Ｆｅ2Ｏ3（赤錆）を含むが、短時間で要求熱輻射率を得る工程と、上記雰囲気中で加熱されたシャドウマスクを、不活性ガスと酸化性ガス及び還元性ガスを含む雰囲気下で加熱処理することによって、Ｆｅ2Ｏ3 （赤錆）をＦｅ3Ｏ4（黒錆）に変化させ、Ｆｅ2Ｏ3 （赤錆）を含まない脱落しにくいＦｅ3Ｏ4（黒錆）のみをシャドウマスク上に優先的に短時間に形成する方法である。
【００１０】
まず、シャドウマスクを、露点５０℃とした不活性ガスと水蒸気を含む雰囲気下で加熱処理し、さらに、不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む、露点５０℃とした混成ガスを流した雰囲気下で加熱処理することにより、短時間で要求熱輻射率を有するＦｅ3Ｏ4（黒錆）からなる黒化膜をシャドウマスク表面に形成するようにしたものである。
【００１１】
また、上記不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む雰囲気の組成比であるＣＯ／ＣＯ2及びＨ2／Ｈ2Ｏ値の両方が０．０１〜１．０になるようにする。
ここで、ＣＯ／ＣＯ2値が０．０１未満になると、シャドウマスクを加熱した際に、赤錆（Ｆｅ2Ｏ3）が発生してしまう場合があり、１．０以上になると、ＦｅＯが発生してしまう場合がある。
ＦｅＯは、化学的に不安定であり、Ｆｅ2Ｏ3（赤錆）に変化する可能性がある為、ＦｅＯが発生した状態は好ましくない。
また、Ｈ2／Ｈ2Ｏ値が０．０１未満になると、シャドウマスクを加熱した際に、Ｎｉが酸化してしまう場合があり、１．０以上になると、ＦｅＯが発生してしまう場合がある。
この様な理由から、ＣＯ／ＣＯ2及びＨ2／Ｈ2Ｏ値の両方が０．０１〜１．０であることが更に好ましい。
【００１２】
さらに、前記加熱処理を４５０℃〜６５０℃で行うようにする。
４５０℃以下の温度では、処理に時間を要することになり、６５０℃以上では、ＦｅＯが発生してしまう場合がある。その為、５５０℃〜６００℃で行うことがより好ましい。
【００１３】
【実施例】
以下実施例により本発明を詳細に説明する。
まず、処理すべきシャドウマスクとして、例えば、Ｎi＝３８％、Ｓi＝０．０５％、Ｃr＝０．１０％、Ｓ＝０．００３％Ｃ＝０．０１０％、Ｐ＝０．００５％、Ａl＝０．０３０％、Ｍn＝０．４０％（重量比）及び残部Ｆｅの材料組成比からなるシャドウマスクを準備した。
【００１４】
次に、上記シャドウマスクを内径５０ｍｍの加熱炉内に固定し、まず、露点を５０℃としたＮ2ガスを流しつつ６００℃で１５分間加熱処理を行い、さらに、炉内雰囲気の組成比が、ＣＯ／ＣＯ2及びＨ2／Ｈ2Ｏ値が、０．０１〜１．０になるように、ガス流量をＣＯ2ガス：１．２リットル／分、ＣＯガス：０．１５リットル／分、Ｈ2ガス：０．０５リットル／分及びＮ2ガス：７．６リットル／分とし、露点を５０℃とした混成ガスを流しつつ、６００℃で１５分間加熱処理を行った。
この混合ガスは、組成比にすると、ＣＯ2＝１１．８％、Ｈ2Ｏ＝１１．８％、ＣＯ＝１．５％、Ｈ2＝０．５％、Ｎ2＝７４．４％というものであった。
【００１５】
上記実施例で得られたシャドウマスクの黒化膜の熱輻射率の測定結果を表１に示す。
表１からも分かるように本発明の酸化処理法で形成した黒化膜の熱輻射率は熱処理時間３０分で０．６４が得られた。
比較例として、一般的に行われている発熱型変性ガスにて処理してシャドウマスク表面に形成した黒化膜の熱輻射率の測定結果も表１に併せて示す。一般的に行われている発熱型変性ガスによる処理は所望の熱輻射率（０．６以上）を得るのに５０分の処理時間を要した。
【００１６】
【表１】
上記実施例で得られたシャドウマスクの黒化膜のＸ線回折による構造解析結果を図１に示す。
上記実施例で得られたシャドウマスクの黒化膜には、Ｆｅ2Ｏ3（赤錆）の（１０４）面（２θ＝３３．１５１°）のピークが無く、Ｆｅ3Ｏ4（黒錆）の（３１１）面（２θ＝３５．４２１°）のピーク、Ｆｅ3Ｏ4（黒錆）の（４４０）面（２θ＝６２．５１２°）及びＦｅ3Ｏ4（黒錆）の（２２０）面（２θ＝３０．０９３°）のピークが存在していることを示している。
【００１８】
また、Ｆｅ3Ｏ4（黒錆）に粘着テープを圧着した後、Ｆｅ3Ｏ4（黒錆）から粘着テープを剥離した結果Ｆｅ3Ｏ4（黒錆）の粘着テープへの付着は見られなかった。酸化処理で形成されたＦｅ3Ｏ4（黒錆）が脱落しにくいことが確認された。
【００１９】
【発明の効果】
本発明のシャドウマスクの酸化処理方法により、シャドウマスクにＦｅ3Ｏ4（黒錆）からなる黒化膜を優先的に短時間に形成させることが可能となる。
これにより、Ｆｅ2Ｏ3（赤錆）を含まず、脱落しにくい安定な酸化膜であるＦｅ3Ｏ4（黒錆）を優先的にシャドウマスクに形成し、Ｆｅ2Ｏ3（赤錆）の粉によるシャドウマスクの目詰まりを防止でき、かつ、熱輻射率の要求を満たしたＦｅ3Ｏ4（黒錆）からなる黒化膜を従来の６割程度の時間（３０分間）で形成できる。
【図面の簡単な説明】
【図１】本発明のシャドウマスクの酸化処理方法により形成した黒化膜のＸ線回折による構造解析結果を示す説明図である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for processing a shadow mask used in a cathode ray tube of a display such as a television or a computer.
[0002]
[Prior art]
The shadow mask is manufactured by etching a metal thin plate.
As the metal thin plate, an iron material, an iron-nickel alloy material, or an iron-nickel-cobalt alloy material is used. In any case, since iron is the main component of the material, there is a problem that rust occurs when it is in a humid environment during transportation and storage.
Examples of iron oxides include Fe 2 O 3 , Fe 3 O 4 , and FeO. Among them, Fe 2 O 3 (red rust) has a weak adhesion to the material, so when a shadow mask is used for a cathode ray tube, the red rust may fall off inside the cathode ray tube and clog the shadow mask opening. is there.
In order to prevent this, a measure to preferentially form Fe 3 O 4 (black rust), which is a stable oxide film that does not easily fall off, on the shadow mask to prevent generation of Fe 2 O 3 (red rust) (blackening) Processing) has been adopted.
In addition, the shadow mask functions to block unnecessary electrons in the cathode ray tube. At this time, the shadow mask rises in temperature and thermally expands, which may cause color unevenness in the image.
In order to prevent the above temperature rise, a measure (blackening treatment) is adopted in which Fe 3 O 4 (black rust) having high thermal radiation efficiency is formed on the shadow mask.
[0003]
As a method for forming black rust (Fe 3 O 4 ), for example, as disclosed in Japanese Patent Application Laid-Open No. 64-3492, as a conventional treatment condition, about 580 ° C. in a mixed gas of CO 2 and CO. In general, heating is performed at a temperature exceeding 500 ° C. in an exothermic modified gas atmosphere.
[0004]
[Problems to be solved by the invention]
However, when the blackening treatment is performed under the above heating conditions, in order to obtain the thermal emissivity ≧ 0.6 required for the blackening film, an industrially long treatment time of 50 minutes or more is required. Have.
Further, depending on the composition of the mixed gas, there is a problem that Fe 2 O 3 (red rust) is generated.
[0005]
The present invention has been devised in view of the above problems, and provides a shadow mask oxidation method for preferentially and quickly forming Fe 3 O 4 (black rust), which is a stable oxide film that does not easily fall off, in a shadow mask. The purpose is to provide.
[0006]
[Means for Solving the Problems]
In order to solve the above problem, in the shadow mask oxidation treatment method of the present invention,
Heat-treating the shadow mask in an atmosphere containing an inert gas and water vapor with a dew point of 50 ° C .;
A step of heat-treating in an atmosphere of flowing a mixed gas containing an inert gas and H 2 , H 2 O, CO and CO 2 and having a dew point of 50 ° C.,
Both the H 2 / H 2 O and CO / CO 2 values in an atmosphere containing the inert gas and H 2 , H 2 O, CO and CO 2 are 0.01 to 1.0,
The heat treatment is performed at 450 ° C. to 650 ° C.
[0009]
DETAILED DESCRIPTION OF THE INVENTION
The shadow mask oxidation method of the present invention is a method in which Fe 3 O 4 (black rust) is preferentially formed in a shadow mask in a short time. By utilizing this technique, Fe 2 O 3 (red rust) is reduced. It has been found that a blackening film made of Fe 3 O 4 (black rust) that does not contain and does not easily fall off can be preferentially formed on the shadow mask in a short time.
Specifically, the shadow mask is heat-treated in an atmosphere containing an inert gas having strong oxidizing power and water vapor, and contains Fe 2 O 3 (red rust). Fe 2 O 3 (red rust) is changed to Fe 3 O 4 (black rust) by heat-treating a shadow mask heated in an atmosphere in an atmosphere containing an inert gas, an oxidizing gas, and a reducing gas. In this method, only Fe 3 O 4 (black rust) that does not contain Fe 2 O 3 (red rust) and does not easily fall off is preferentially formed on the shadow mask in a short time.
[0010]
First, the shadow mask was heat-treated in an atmosphere containing an inert gas and water vapor with a dew point of 50 ° C., and further a dew point of 50 ° C. containing an inert gas and H 2 , H 2 O, CO, and CO 2 . A blackening film made of Fe 3 O 4 (black rust) having the required heat radiation rate is formed on the shadow mask surface in a short time by heat treatment in an atmosphere in which a mixed gas flows.
[0011]
Further, both the CO / CO 2 and H 2 / H 2 O values, which are the composition ratio of the inert gas and the atmosphere containing H 2 , H 2 O, CO, and CO 2 , are 0.01 to 1.0. Like that.
Here, when the CO / CO 2 value is less than 0.01, red rust (Fe 2 O 3 ) may be generated when the shadow mask is heated, and when it is 1.0 or more, FeO is generated. May end up.
Since FeO is chemically unstable and may change to Fe 2 O 3 (red rust), the state where FeO is generated is not preferable.
When the H 2 / H 2 O value is less than 0.01, Ni may be oxidized when the shadow mask is heated, and when it is 1.0 or more, FeO may be generated. is there.
For these reasons, it is more preferable that both the CO / CO 2 and H 2 / H 2 O values are 0.01 to 1.0.
[0012]
Further, the heat treatment is performed at 450 ° C. to 650 ° C.
If the temperature is 450 ° C. or lower, the treatment takes time, and if it is 650 ° C. or higher, FeO may be generated. Therefore, it is more preferable to carry out at 550 ° C to 600 ° C.
[0013]
【Example】
Hereinafter, the present invention will be described in detail by way of examples.
First, as a shadow mask to be processed, for example, Ni = 38%, Si = 0.05%, Cr = 0.10%, S = 0.003% C = 0.010%, P = 0.005%, A shadow mask having a material composition ratio of Al = 0.030%, Mn = 0.40% (weight ratio) and the balance Fe was prepared.
[0014]
Next, the shadow mask is fixed in a heating furnace having an inner diameter of 50 mm. First, heat treatment is performed at 600 ° C. for 15 minutes while flowing N 2 gas with a dew point of 50 ° C., and the composition ratio of the atmosphere in the furnace is further increased. , CO 2 gas: 1.2 liters / minute, CO gas: 0.15 liters / minute, so that CO / CO 2 and H 2 / H 2 O values are 0.01 to 1.0 Heat treatment was performed at 600 ° C. for 15 minutes while flowing a mixed gas with H 2 gas: 0.05 liter / min and N 2 gas: 7.6 liter / min and a dew point of 50 ° C.
This mixed gas has a composition ratio of CO 2 = 11.8%, H 2 O = 11.8%, CO = 1.5%, H 2 = 0.5%, N 2 = 74.4%. It was a thing.
[0015]
Table 1 shows the measurement results of the thermal emissivity of the blackened film of the shadow mask obtained in the above example.
As can be seen from Table 1, the heat emissivity of the blackened film formed by the oxidation treatment method of the present invention was 0.64 after a heat treatment time of 30 minutes.
As a comparative example, Table 1 also shows the measurement results of the thermal emissivity of the blackened film formed on the surface of the shadow mask by treatment with a general exothermic denatured gas. In general, the treatment with the exothermic denatured gas takes a treatment time of 50 minutes to obtain a desired heat radiation rate (0.6 or more).
[0016]
[Table 1]
FIG. 1 shows the structural analysis result by X-ray diffraction of the blackened film of the shadow mask obtained in the above example.
The blackened film of the shadow mask obtained in the above example does not have a peak of (104) plane (2θ = 33.151 °) of Fe 2 O 3 (red rust), and Fe 3 O 4 (black rust) has no peak. Peak of (311) plane (2θ = 35.421 °), (440) plane of Fe 3 O 4 (black rust) (2θ = 62.512 °) and (220) plane of Fe 3 O 4 (black rust) It shows that a peak (2θ = 30.093 °) exists.
[0018]
Furthermore, after bonding the adhesive tape to the Fe 3 O 4 (black rust), Fe 3 adhesion of O 4 from (black rust) to the adhesive tape as a result of peeling off the adhesive tape Fe 3 O 4 (black rust) is observed There wasn't. It was confirmed that Fe 3 O 4 (black rust) formed by the oxidation treatment was not easily dropped off.
[0019]
【Effect of the invention】
With the shadow mask oxidation treatment method of the present invention, it becomes possible to preferentially form a blackened film made of Fe 3 O 4 (black rust) on the shadow mask in a short time.
As a result, Fe 3 O 4 (black rust), which is a stable oxide film that does not contain Fe 2 O 3 (red rust) and is difficult to fall off, is preferentially formed on the shadow mask, and Fe 2 O 3 (red rust) powder Therefore, a blackened film made of Fe 3 O 4 (black rust) that satisfies the requirement of thermal radiation rate can be formed in about 60% of the time (30 minutes).
[Brief description of the drawings]
FIG. 1 is an explanatory view showing a structural analysis result by X-ray diffraction of a blackened film formed by an oxidation treatment method for a shadow mask of the present invention.
Claims (1)
不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む、露点５０℃とした混成ガスを流した雰囲気下で加熱処理する工程とを備え、
前記不活性ガスとＨ2、Ｈ2Ｏ、ＣＯ及びＣＯ2を含む雰囲気でのＨ2／Ｈ2Ｏ及びＣＯ／ＣＯ2値の両方が０．０１〜１．０であり、
前記加熱処理を４５０℃〜６５０℃で行うことを特徴とするシャドウマスクの酸化処理方法。Heat-treating the shadow mask in an atmosphere containing an inert gas and water vapor with a dew point of 50 ° C . ;
Inert gas and H 2, H 2 O, including CO and CO 2, e Preparations and heating treatment in an atmosphere of flowing a dew point 50 ° C. and were mixed gas,
Wherein both the inert gas and H 2, H 2 O, H 2 / H 2 O and CO / CO 2 value in an atmosphere containing CO and CO 2 is Ri der 0.01 to 1.0,
A shadow mask oxidation treatment method, wherein the heat treatment is performed at 450 ° C. to 650 ° C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001261311A JP4876351B2 (en) | 2001-08-30 | 2001-08-30 | Shadow mask oxidation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001261311A JP4876351B2 (en) | 2001-08-30 | 2001-08-30 | Shadow mask oxidation method |
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| JP2003073797A JP2003073797A (en) | 2003-03-12 |
| JP4876351B2 true JP4876351B2 (en) | 2012-02-15 |
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| JP4702095B2 (en) * | 2006-02-24 | 2011-06-15 | 住友金属工業株式会社 | Method for producing Cr-containing nickel-base alloy tube |
| JP4702096B2 (en) * | 2006-02-24 | 2011-06-15 | 住友金属工業株式会社 | Method for producing Cr-containing nickel-base alloy tube |
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