JP4660808B2

JP4660808B2 - Foamable fluorescent magnetic powder for wet magnetic particle testing and its manufacturing method

Info

Publication number: JP4660808B2
Application number: JP2001197896A
Authority: JP
Inventors: 嘉高佐野; 知己河村
Original assignee: Marktec Corp
Current assignee: Marktec Corp
Priority date: 2001-06-29
Filing date: 2001-06-29
Publication date: 2011-03-30
Anticipated expiration: 2021-06-29
Also published as: JP2003014700A

Description

【０００１】
【産業上の利用分野】
本発明は、湿式磁粉探傷試験用発泡性蛍光磁粉に関するものであり、当該蛍光磁粉は、鉄鋼工場や自動車工場において実施されている湿式磁粉探傷試験方法に用いられる。
【０００２】
【従来の技術】
周知のとおり、鉄鋼工場においては角ビレットや丸ビレットなどの鋼材を被検査物として、自動車工場においてはナックルアームやシャフトなどの鋼製部品を被検査物として、それぞれＪＩＳ−Ｇ−０５６５−１９９２（鉄鋼材料の磁粉探傷試験方法及び磁粉模様の分類）に規定されている湿式磁粉探傷試験方法が実施されている。
【０００３】
前記湿式磁粉探傷試験方法は、通常、水１ｌ当り蛍光磁粉０．２〜１５ｇを分散させた磁粉液（当業界では「検査液」とも呼ばれている）を、磁化されている被検査物表面に接触させて当該蛍光磁粉を傷（欠陥部）に吸着させることによって探傷する試験方法である。
【０００４】
一般に、前記磁粉液の調製に当っては、市販の磁粉探傷試験用蛍光磁粉と市販の湿式磁粉探傷試験用磁粉分散剤とが使用されている。
【０００５】
前記市販磁粉探傷試験用蛍光磁粉は導磁性粒子粉末（純鉄粒子粉末、酸化鉄粒子粉末、ステンレススチール粒子粉末など）の各粒子表面に蛍光顔料又は蛍光染料を付着させた平均粒子径１〜２５μm の粉末であり、その代表的な市販品としては「スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製）」が挙げられる。
【０００６】
前記市販湿式磁粉探傷試験用磁粉分散剤には、液体タイプと粉末タイプとがあり、前者は水にＨＬＢ値８〜１４のノニオン系界面活性剤１〜２０重量％及びシリコン消泡剤０．１〜１０重量％を溶解乃至分散させたものであり、その代表的な市販品としては「スーパーマグナ（前出）磁粉分散剤ＢＣ−７００（商品名・マークテック株式会社製）」が挙げられ、後者は水溶性粒子粉末（例えば、トリポリリン酸ソーダ、亜硝酸ソーダなど）７０〜９９．４重量％にＨＬＢ値８〜１４の液状ノニオン系界面活性剤０．５〜２０重量％及びシリコン消泡剤０．１〜１０重量％を吸着させたものであり、その代表的な市販品としては「スーパーマグナ（前出）磁粉分散剤ＢＣ−１（商品名・マークテック株式会社製）・水溶性粒子粉末としてトリポリリン酸ソーダ粒子粉末が使用されている。」が挙げられる。
【０００７】
なお、液体タイプの湿式磁粉探傷試験用磁粉分散剤に関し、特公平２−５９４２６号公報には水、ノニオン系界面活性剤、シリコン消泡剤、防錆剤及びジメチルポリシロキサン−ポリオキシアルキレン共重合体からなるものが、特公平２−５２９８７号公報には水、ノニオン系界面活性剤、シリコン消泡剤及びセッケンからなるものがそれぞれ開示されており、粉体タイプの湿式磁粉探傷試験用磁粉分散剤に関し、特開平７−１２０４３７号公報（特許第２８１３９４８号）には５メッシュのフルイを通過する水溶性粒子粉末７０〜９９．４重量％、ＨＬＢ値８〜１４の液状ノニオン系界面活性剤０．５〜２０重量％及びシリコン消泡剤０．１〜１０重量％からなるものが、特開平８−３０４３４７号公報には１６メッシュのフルイを通過する水溶性粒子粉末７０〜９９．４重量％、ＨＬＢ値８〜１４の液状ノニオン系界面活性剤０．５〜２０重量％及びシリコン消泡剤０．１〜１０重量％からなる粉末状配合物１００重量部に対して２００メッシュのフルイを通過する水不溶性非磁性体粒子粉末２〜３０重量部を混合してなるものが、それぞれ開示されている。
【０００８】
水１ｌ当り蛍光磁粉０．２〜１５ｇを分散させた磁粉液の調製に当り、液体タイプの前記市販湿式磁粉探傷試験用磁粉分散剤並びに前掲各公報に開示されている各湿式磁粉探傷試験用磁粉分散剤を使用する場合には、水１ｌ当り分散剤濃度が１〜３％となるように添加されており、粉体タイプの前記市販湿式磁粉探傷試験用磁粉分散剤並びに前掲各公報に開示されている各湿式磁粉探傷試験用磁粉分散剤を使用する場合には、水１ｌ当りの有効成分（水溶性粒子粉末及び／又は水不溶性粒子粉末以外の成分：界面活性剤、シリコン消泡剤など）濃度が１〜３％となる量が添加されている。
【０００９】
湿式磁粉探傷試験方法の実施現場においては、前記市販磁粉探傷試験用蛍光磁粉と前記市販湿式磁粉探傷試験用磁粉分散剤とを使用して磁粉液が調製されているが、調製に当っては、蛍光磁粉と分散剤とを、それぞれ所定量秤取する秤量作業が必須である。
【００１０】
ところで、鉄鋼工場や自動車工場においては、分・秒・刻みの作業効率の向上がはかられており、前記秤量作業の簡略化が強く要望されている。
【００１１】
磁粉探傷試験用磁粉・湿式磁粉探傷試験用磁粉分散剤のメーカー側においては、前記要望に応えるべく、永年にわたる研究開発が続けられており、特公昭５０−４６９号公報や特開昭５７−１４１５４７号公報には、界面活性剤をあらかじめ磁粉に付着させてなる磁粉探傷試験用磁粉が開示されており、特公昭５６−４９３１１号公報や特公平３−４２４２７号公報には界面活性剤をバインダーとして磁粉を成型してなる磁粉探傷試験用磁粉成型物が開示されている。
【００１２】
前掲各公報に見られる通り、磁粉（蛍光磁粉又は非蛍光磁粉）に界面活性剤をあらかじめ付着させて置くことにより、磁粉探傷試験用磁粉自体に分散性を付与するという技術的手段は古くから提案されている。
【００１３】
しかし、磁粉探傷試験用蛍光磁粉を水に分散させるためには、ＨＬＢ値８〜１４の液状ノニオン系界面活性剤を用いる必要があり（因みに、米国軍隊規格ＭＩＬ−ＳＴＤ−１９４９Ａ：４，９，４項にはノニオン系界面活性剤を用いることとされている。）、当該界面活性剤は不揮発性の粘性液体であるため、これを付着させた蛍光磁粉は貯蔵中に凝集してしまうので、磁粉液調製時に充分な分散状態が得られないという問題点があり、また、当該界面活性剤は滲透性が強いので、これを付着させた蛍光磁粉は貯蔵中に顔料や染料の一部が剥離し、探傷時に剥離した蛍光顔料や蛍光染料がノイズとなって現れる（当業界では「バックグランド現象」と呼ばれている）ため、探傷精度が低下してしまうという問題点がある。事実、本発明者が知る限り、蛍光磁粉にＨＬＢ値８〜１４の液状ノニオン系界面活性剤をあらかじめ付着させてなる磁粉探傷試験用磁粉が実用されている例はない。
【００１４】
【発明が解決しようとする課題】
そこで、本発明は、ＨＬＢ値８〜１４の液状ノニオン系界面活性剤を用いているにもかかわらず、前記諸問題点が解決でき、前記秤量作業の簡略化という要望に応えることができると共に、磁粉液調製時により優れた水分散性を発揮できる湿式磁粉探傷試験用発泡性蛍光磁粉の提供を技術的課題とするものである。
【００１５】
【課題を解決するための手段】
前記本発明の技術的課題は、次のとおりの本発明によって達成できる。
【００１６】
即ち、本発明は、導磁性粒子粉末の各粒子表面に蛍光顔料又は蛍光染料を付着させた磁粉探傷試験用蛍光磁粉１００重量部とＨＬＢ値８〜１４の液状ノニオン系界面活性剤２０〜３０重量部とからなる泥状物に、トリポリ燐酸ソーダ粉末１７０〜２２０重量部と炭酸塩粉末又は炭酸水素塩粉末１５〜２５重量部と有機酸塩粉末２５〜３５重量部とを混合し、前記泥状物を粉末化してなる湿式磁粉探傷試験用発泡性蛍光磁粉である。
【００１７】
また、本発明は、導磁性粒子粉末の各粒子表面に蛍光顔料又は蛍光染料を付着させた磁粉探傷試験用蛍光磁粉１００重量部とＨＬＢ値８〜１４の液状ノニオン系界面活性剤２０〜３０重量部とからなる泥状物に、トリポリ燐酸ソーダ粉末１７０〜２２０重量部と炭酸塩粉末又は炭酸水素塩粉末１５〜２５重量部と有機酸塩粉末２５〜３５重量部とシリコン系消泡剤０．３〜１０重量部及び／又は防錆剤０．３〜１０重量部とを混合し、前記泥状物を粉末化してなる湿式磁粉探傷試験用発泡性蛍光磁粉である。
【００１８】
さらに、本発明は、導磁性粒子粉末の各粒子表面に蛍光顔料又は蛍光染料を付着させた磁粉探傷試験用蛍光磁粉１００重量部をＨＬＢ値８〜１４の液状ノニオン系界面活性剤２０〜３０重量部に分散させて泥状物とし、次いで当該泥状物にトリポリ燐酸ソーダ粉末１７０〜２２０重量部と炭酸塩粉末又は炭酸水素酸塩粉末１５〜２５重量部と有機酸粉末２５〜３５重量部とを添加して攪拌して、前記泥状物を粉末化することを特徴とする湿式磁粉探傷試験用発泡性蛍光磁粉の製造法である。
【００１９】
本発明の構成をより詳しく説明すれば次のとおりである。
【００２０】
先ず、本発明における磁粉探傷試験用蛍光磁粉としては、前記の市販磁粉探傷用蛍光磁粉を用いればよく、例えば、スーパーマグナ（前出）蛍光磁粉ＬＹ−１０（前出）が好適である。
【００２１】
また、本発明におけるＨＬＢ値８〜１４の液状ノニオン系界面活性剤としては、市販品を用いればよく、例えば、ニューコール８６４（商品名：日本乳化剤株式会社製：ＨＬＢ１３．８）やオクタポール５０（商品名：三洋化成株式会社製：ＨＬＢ１０．３）が好適である。
【００２２】
次に、本発明におけるトリポリ燐酸ソーダ粉末としては、使用時における溶解速度の面から１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過する粉末が好適であり、市販品から所要の粒子径のものを選定・入手して用いればよい。
【００２３】
また、本発明における炭酸塩粉末又は炭酸水素塩粉末としては、水中において有機酸と反応して炭酸ガスを発生するものであればよく、具体的には、市販の炭酸ナトリウム粉末、炭酸カリウム粉末、炭酸マグネシウム粉末、セスキ炭酸ナトリウム粉末、炭酸水素ナトリウム粉末等が挙げられ、これらの単独又は混合物を用いればよい。なお、目的物の使用時における溶解速度の面から１６メッシュのフルイ（前出）を通過する粒子粉末を選定・入手して用いることが好適である。
【００２４】
また、本発明における有機酸粉末としては、市販のコハク酸粉末、リンゴ酸粉末、洒石酸粉末、フマル酸粉末等が挙げられ、これらの単独又は混合物を用いればよい。なお、目的物の使用時における溶解速度の面から１６メッシュのフルイ（前出）を通過する粒子粉末を選定・入手して用いることが好適である。
【００２５】
本発明における前記磁粉探傷試験用蛍光磁粉、前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤、前記トリポリ燐酸ソーダ粉末、前記炭酸塩粉末又は炭酸水素塩粉末及び前記有機酸粉末の各配合量は重要である。
【００２６】
前記磁粉探傷試験用蛍光磁粉１００重量部の場合、前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤は２０重量部以上を必要とし、２０重量部未満では磁粉液調製時に蛍光磁粉を充分に分散させることが困難となり、調製した磁粉液の濡れ効果が不充分となる。３０重量部を越えて配合しても蛍光磁粉の分散性及び濡れ効果はさほど向上せず、目的物の粉体流動性に悪影響を及ぼすことになるので３０重量部以内に止めるべきである。
【００２７】
前記トリポリ燐酸ソーダ粉末は少なくとも１７０重量部以上を必要とし、１７０重量部未満では、前記磁粉探傷試験用蛍光磁粉１００重量部と前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤２０〜３０重量部とからなる泥状物を粉末化して充分な粉体流動性を付与することが困難となる。配合量の上限は、その他配合成分の各配合量割合から定まるが、１７０〜２２０重量部の範囲内であれば充分な粉体流動性を付与することができる。
【００２８】
なお、ＨＬＢ８〜１４の液状ノニオン系界面活性剤を付着させた蛍光磁粉をそのままの状態にて放置した場合には、前述のとおり、貯蔵中に該界面活性剤が蛍光磁粉粒子同志を結びつけるため該蛍光磁粉が塊状に凝集してしまい、また、当該界面活性剤が蛍光磁粉粒子表面の蛍光顔料層又は蛍光染料層に滲過するため蛍光顔料又は蛍光染料の一部が剥離してしまうが、前記トリポリ燐酸塩粉末が混在している場合には、該トリポリ燐酸塩粉末は吸油量が大きいので、蛍光磁粉粒子に付着している当該界面活性剤を吸収し担持するから、当該凝集を抑制でき、また、当該剥離も抑制できる。
【００２９】
前記炭酸塩又は炭酸水素塩粉末と前記有機酸粉末との使用割合は、特に重要であり、前者：後者＝１：１〜３の比率にて使用する必要があり、前者：後者＝１：１未満の場合には、前記トリポリ燐酸ソーダ粉末が溶解している磁粉液のｐＨ値がアルカリ性を呈するために前者と後者との間で反応が起こらないので目的物に自己発泡性を付与することができず、また、前者：後者＝１：３以上の場合には、前記トリポリ燐酸ソーダ粉末が溶解している磁粉液のｐＨ値が酸性を呈するために被検査物である鋼材や鋼製部品に錆を発生させる危険がある。
【００３０】
従って、前記炭酸塩粉末又は炭酸水素塩粉末を１５〜２５重量部配合すると共に前記有機酸粉末を２５〜３５重量部配合する。なお、両者の配合量の各上限はその他の配合成分量から定まる。
【００３１】
前記炭酸塩粉末又は炭酸水素塩粉末と有機酸粉末との各配合量の範囲内において調節することによって前記トリポリ燐酸塩粉末が溶解している磁粉液のｐＨ値を中性〜弱アルカリ性にすることができる。
【００３２】
前記各配合成分を前記配合量にて配合してなる本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉は、磁粉液調製時において水中に投入すれば自己発泡して速やかに溶解し、溶解後には殆んど泡立ちは認められないが、蛍光磁粉を分散させた後の泡立ちを充分に抑制する必要がある場合には、前記の市販磁粉液用分散剤と同様にシリコン系消泡剤を配合することができる。
【００３３】
本発明におけるシリコン系消泡剤としては、市販品を用いればよく、例えば、シリコン消泡剤ＫＭ５０８（商品名：信越化学株式会社製）やシリコン消泡剤ＫＭ５３１（商品名：信越化学株式会社製）が好適である。
【００３４】
前記シリコン系消泡剤は０．３重量部以上を必要とし、０．３重量部未満では、消泡効果が得られ難く、通常、１〜５重量部程度を配合すれば充分であり、１０重量部を越えて配合する必要はない。
【００３５】
また、前記トリポリ燐酸ソーダ粉末が防錆力を有しているので、通常は防錆剤を配合する必要はないが、被検査物の材質に応じて強い防錆力が要求される場合には、防錆剤を配合することもできる。
【００３６】
本発明における防錆剤としては、市販の亜硝酸ソーダ粉末やグルコン酸ソーダ粉末が好適であり、通常、０．３〜１０重量部程度を配合すれば充分であり、１０重量部を越えて配合する必要はない。
【００３７】
本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉の製造法は、次のとおりである。
【００３８】
先ず、第１工程として、前記磁粉探傷試験用蛍光磁粉及び前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤を、それぞれ所定量秤取して容器（例えば、ステンレス製タンク）に投入し、攪拌器（例えば、電動ミキサー）を用いて充分に混合・攪拌して泥状物とする。
【００３９】
次いで、第２工程として、当該タンクに前記トリポリ燐酸ソーダ粉末、前記炭酸塩粉末又は前記炭酸水素塩粉末、前記有機酸塩粉末及び必要に応じて配合される前記シリコン消泡剤及び／又は前記防錆剤を、それぞれ所定量秤取して追加投入し、さらに充分に混合・攪拌して粉末化すれば目的物が得られる。なお、粉末化状態は目視及び指触によって行なえばよい。
【００４０】
なお、前記工程順序は重要であり、第１工程と第２工程とを同時に実施する場合、換言すれば、各配合成分を同時に混合する場合には、前記トリポリ燐酸ソーダ粉末に吸収・担持されている前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤に前記磁粉探傷試験用蛍光磁粉の粒子が付着してしまうので該蛍光磁粉の各粒子を該界面活性剤で被覆できず、当該蛍光磁粉の粒子同志が接触している部分が生じるため、後出比較例１に見られるとおり、目的物に充分な探傷能力を付与できず（調製した磁粉液の分散性及び濡れ性が悪い）、また、目的物に充分な保存安定性を付与できない（貯蔵中に蛍光磁粉の粒子同志が直接接触している部分が凝集する）。一方、第１工程において当該蛍光磁粉と当該界面活性剤とを混合・攪拌して泥状物とした後に第２工程に移行する場合には、当該蛍光磁粉の各粒子を当該界面活性剤で被覆できるので、当該蛍光磁粉の粒子同志が直接接触しないから、後出発明の実施の形態並びに各実施例に見られるとおり、目的物に充分な探傷能力及び充分な保存安定性を付与できる。
【００４１】
本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉の使用方法は極めて簡易であり、所要量を水に投入して混合・攪拌すれば、当該発泡性蛍光磁粉が水中で自己発泡するので、配合成分中の前記トリポリ燐酸ソーダ粉末、前記炭酸塩粉末又は前記炭酸水素塩粉末及び前記有機酸塩粉末は速やかに溶解し、配合成分中の前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤は速やかに溶解乃至分散し、配合成分中の前記磁粉探傷試験用蛍光磁粉は速やかに分散して、前記した市販磁粉探傷試験用蛍光磁粉と市販湿式磁粉探傷試験用磁粉分散剤とを用いる場合と変らない磁粉液が調製できる。
【００４２】
なお、本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉を構成する配合成分の各配合量が前記のとおりであるから、当該発泡性蛍光磁粉は約３〜４ｇ当り前記磁粉探傷試験用蛍光磁粉１ｇを含んでいる。
【００４３】
【発明の実施の形態】
湿式磁粉探傷試験用発泡性蛍光磁粉の製造：スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製・四三酸化鉄粒子粉末の各粒子表面に合成樹脂バインダーを用いて蛍光顔料を付着させたもの）１００重量部及びニューコール８６４（商品名・日本乳化株式会社製・ＨＬＢ１３．８の液状ノニオン系界面活性剤）２０重量部をステンレス製タンクに投入し、電動ミキサーを用いて充分に混合・攪拌して泥状物とする。
【００４４】
次いで、１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過するトリポリ燐酸ソーダ粉末（住友化学工業株式会社製）１７０重量部、炭酸水素ナトリウム粉末（旭硝子株式会社製）１５重量部及び洒石酸粉末（扶桑化学株式会社製）２５重量部を当該タンクに追加投入し、充分に混合・攪拌して前記泥状物を粉末化して湿式磁粉探傷試験用発泡性蛍光磁粉約３３０重量部を得た。
【００４５】
粉末化状態評価試験：ここに得た発泡性蛍光磁粉をガラス容器に入れ、当該ガラス容器を水平位置から徐々に傾斜させて容器内の粉末状分散剤に流動が生じた時の角度を測定し、５５度未満の角度で流動が生じたものを「○（良好）」、５５度以上の角度で流動が生じたものを「×（悪い）」と評価した。その結果「○」であった。
【００４６】
発泡性評価試験：ここに得た発泡性蛍光磁粉３．３ｇを水１ｌが入っているガラスビーカーに投入し、攪拌しない状態下において目視にて観察し、泡が生じたものを「○（良い）」、泡が生じなかったものを「×（悪い）」と評価した。その結果は「○」であった。
【００４７】
分散性評価試験：ここに得た発泡性蛍光磁粉３．３ｇ（蛍光磁粉含有量：１ｇ）を水１ｌが入っているガラスビーカーに投入し、マドラーを用いて攪拌して磁粉液を調製した。
【００４８】
一方、スーパーマグナ（前出）蛍光磁粉ＬＹ−１００（前出）１ｇとスーパーマグナ（登録商標）磁粉分散剤ＢＣ−１（商品名・マークテック株式会社製・トリポリ燐酸ソーダー粉末にＨＬＢ８〜１４の液状ノニオン系界面活性剤を吸着・担持させたもの）２ｇとを混合し、該混合物を水１ｌが入っているガラスビーカーに投入し、マドラーを用いて攪拌して比較用磁粉液を調製した。
【００４９】
前記両磁粉液の分散状態を、暗所における紫外線灯の照射下において目視にて観察し、充分に分散している比較用磁粉液の分散状態と同等の分散状態を視認した場合には「○（良い）」、比較用磁粉液の分難状態より劣る分散状態を視認した場合には「×（悪い）」と評価した。その結果は「○」であった。
【００５０】
探傷能力評価試験：ここに得た発泡性蛍光磁粉３．３ｇ（蛍光磁粉含有量：１ｇ）を水１ｌが入っているガラスビーカーに投入し、マドラーを用いて攪拌して磁粉液を調製した。
【００５１】
一方、スーパーマグナ（前出）蛍光磁粉ＬＹ−１００（前出）１ｇとスーパーマグナ（前出）磁粉分散剤ＢＣ−１（前出）２ｇとを混合し、該混合物を水１ｌが入っているガラスビーカーに投入し、マドラーを用いて攪拌して比較用磁粉液を調製した。
【００５２】
前記両磁粉液を使用して次のとおりの湿式磁粉探傷試験方法を実施した。
【００５３】
ＪＩＳ−０５６５−１９９２規格のＡ型試験片（円型・ＡＩ−１５／１００、ＡＩ−３０／１００）を被検査物とし、該試験片を鋼製角型ビレットに貼り付け、該角型ビレットを磁器通電法によって磁化して当該試験片に磁粉液を散布し、暗所において紫外線灯下で試験面を目視にて観察した。その結果、明瞭な欠陥指示模様が観察できた比較用磁粉液と同等の明瞭な欠陥指示模様が観察できた場合には「○（良い）」、比較用磁粉液を使用した欠陥指示模様に比較して不明瞭な欠陥指示模様を視認した場合には「×（悪い）」と評価した。その結果は「○」であった。
【００５４】
保存安定性評価試験：ここに得た発泡性蛍光磁粉を室内・常温（約２５℃）にて１ケ月間放置した後、当該発泡性蛍光磁粉３．３ｇを水１ｌが入っているガラスビーカーに投入し、マドラーを用いて攪拌して磁粉液を調製した後、攪拌しない状態にて、暗所における紫外線灯の照射下において目視にて観察し、凝集が発生していない場合には「○（良い）」、凝集が発生している場合には「×（悪い）」と評価した。その結果は「○」であった。
【００５５】
【作用】
本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉は、その配合成分中に前記ＨＬＢ値８〜１４の液状ノニオン系界面活性剤を含んでいるから、磁粉液調製時に水に投入して混合・攪拌するだけで磁粉液が調製でき、また、当該界面活性剤が配合成分中の前記トリポリ燐酸塩粉末に吸着・担持されているから保存安定性に優れている。
【００５６】
さらに、その配合成分中に前記炭酸塩粉末又は前記炭酸水素塩粉末と前記有機酸粉末とを含んでいるから、水に投入されると水中で該炭酸塩粉末又は該炭酸水素塩粉末と該有機酸とが反応して炭酸ガスを発生するので発泡する。この発泡現象によって各配合成分の溶解・分散が促進されるから、強力な攪拌を行わなくても、蛍光磁粉が充分に分散している磁粉液が調製できる。
【００５７】
なお、水中における前記炭酸塩粉末又は前記炭酸水素塩粉末と前記有機酸粉末との反応は吸熱反応であるため前記トリポリ燐酸ソーダ粉末と水との反応による発熱が抑制できるから、調製中における磁粉液の昇温が抑制される。
【００５８】
【実施例】
以下に、実施例及び比較例を挙げる。
【００５９】
実施例１
【００６０】
湿式磁粉探傷試験用発泡性蛍光磁粉の製造：スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製・四三酸化鉄粒子粉末の各粒子表面に合成樹脂バインダーを用いて蛍光顔料を付着させたもの）１００重量部及びニューコール８６４（商品名・日本乳化株式会社製・ＨＬＢ１３．８の液状ノニオン系界面活性剤）３０重量部をステンレス製タンクに投入し、電動ミキサーを用いて充分に混合・攪拌して泥状物とする。
【００６１】
次いで、１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過するトリポリ燐酸ソーダ粉末（住友化学工業株式会社製）２２０重量部、炭酸マグネシウム粉末（株式会社トクヤマ製）２５重量部、コハク酸粉末（扶桑化学株式会社製）３５重量部及びシリコン消泡剤ＫＭ５０８（商品名・信越化学株式会社製）５重量部を当該タンクに追加投入し、充分に混合・攪拌して前記泥状物を粉末化して湿式磁粉探傷試験用発泡性蛍光磁粉約４１５重量部を得た。なお、当該発泡性蛍光磁粉は４．１５ｇ当り磁粉探傷用蛍光磁粉（前記スーパーマグナ蛍光磁粉ＬＹ−１０）１ｇを含んでいる。
【００６２】
ここに得た発泡性蛍光磁粉について、前出発明実施の形態における各評価試験と同じ評価試験を行った結果は、次のとおりであった。
【００６３】
粉末化状態評価試験：「○」、発泡性評価試験：「○」、分散性評価試験：「○」、探傷能力評価試験：「○」、保存安定性評価試験：「○」。
【００６４】
実施例２
【００６５】
湿式磁粉探傷試験用発泡性蛍光磁粉の製造：スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製・四三酸化鉄粒子粉末の各粒子表面に合成樹脂バインダーを用いて蛍光顔料を付着させたもの）１００重量部及びニューコール８６４（商品名・日本乳化株式会社製・ＨＬＢ１３．８の液状ノニオン系界面活性剤）２５重量部をステンレス製タンクに投入し、電動ミキサーを用いて充分に混合・攪拌して泥状物とする。
【００６６】
次いで、１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過するトリポリ燐酸ソーダ粉末（住友化学工業株式会社製）２２０重量部、炭酸水素ナトリウム粉末（旭硝子株式会社製）２５重量部、フマル酸粉末（扶桑化学株式会社製）２５重量部、シリコン消泡剤ＫＭ５０８（商品名・信越化学株式会社製）５重量部及び亜硝酸粉末５重量部を当該タンクに追加投入し、充分に混合・攪拌して前記泥状物を粉末化して湿式磁粉探傷試験用発泡性蛍光磁粉約３８５重量部を得た。なお、当該発泡性蛍光磁粉は３．８５ｇ当り磁粉探傷用蛍光磁粉（前記スーパーマグナ蛍光磁粉ＬＹ−１０）１ｇを含んでいる。
【００６７】
ここに得た発泡性蛍光磁粉について、前出発明実施の形態における各評価試験と同じ評価試験を行った結果は、次のとおりであった。
【００６８】
粉末化状態評価試験：「○」、発泡性評価試験：「○」、分散性評価試験：「○」、探傷能力評価試験：「○」、保存安定性評価試験：「○」。
【００６９】
比較例１
【００７０】
湿式磁粉探傷試験用発泡性蛍光磁粉の製造：スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製・四三酸化鉄粒子粉末の各粒子表面に合成樹脂バインダーを用いて蛍光顔料を付着させたもの）１００重量部、ニューコール８６４（商品名・日本乳化株式会社製・ＨＬＢ１３．８の液状ノニオン系界面活性剤）２０重量部、１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過するトリポリ燐酸ソーダ粉末（住友化学工業株式会社製）１７０重量部、炭酸ナトリウム粉末（旭硝子株式会社製）１５重量部及び洒石酸粉末（扶桑化学株式会社製）２５重量部をステンレスタンクに投入し、電動ミキサーを用いて充分に混合・攪拌して比較用発泡性蛍光磁粉約３３０重量部を得た。なお、この比較用発泡性蛍光磁粉は３．３ｇ当り磁粉探傷用蛍光磁粉（前記スーパーマグナ蛍光磁粉ＬＹ−１０）１ｇを含んでいる。
【００７１】
ここに得た比較用発泡性蛍光磁粉について、前出発明実施の形態における各評価試験と同じ評価試験を行った結果は、次のとおりであった。
【００７２】
粉末化状態評価試験：「○」、発泡性評価試験：「○」、分散性評価試験：「○」、探傷能力評価試験：「×」、保存安定性評価試験：「×」。
【００７３】
比較例２
【００７４】
湿式磁粉探傷試験用発泡性蛍光磁粉の製造：スーパーマグナ（登録商標）蛍光磁粉ＬＹ−１０（商品名・マークテック株式会社製・四三酸化鉄粒子粉末の各粒子表面に合成樹脂バインダーを用いて蛍光顔料を付着させたもの）１００重量部及びニューコール８６４（商品名・日本乳化株式会社製・ＨＬＢ１３．８の液状ノニオン系界面活性剤）２５重量部をステンレス製タンクに投入し、電動ミキサーを用いて充分に混合・攪拌して泥状物とする。
【００７５】
次いで、１６メッシュのフルイ（目開き１０００μm ・ＪＩＳ−Ｚ−８８０１）を通過するトリポリ燐酸ソーダ粉末（住友化学工業株式会社製）１７０重量部及びシリコン消泡剤ＫＭ５０８（商品名・信越化学株式会社製）５重量部を当該タンクに追加投入し、充分に混合・攪拌して前記泥状物を粉末化して比較用発泡性蛍光磁粉約３８５重量部を得た。なお、比較用蛍光磁粉は３ｇ当り磁粉探傷蛍光磁粉（前記スーパーマグナ蛍光磁粉ＬＹ−１０）１ｇを含んでいる。
【００７６】
ここに得た比較用発泡性蛍光磁粉について、前出発明実施の形態における各評価試験と同じ評価試験を行った結果は、次のとおりであった。
【００７７】
粉末化状態評価試験：「○」、発泡性評価試験：「×」、分散性評価試験：「×」、探傷能力評価試験：「○」、保存安定性評価試験：「○」。
【００７８】
【発明の効果】
本発明によれば、磁粉液調製時における秤量作業が簡略化できると共に、水中投入時に自己発泡によって優れた水分散性を発揮し、強力な攪拌を行わなくても、蛍光磁粉が充分に分散している磁粉液が容易に調製でき（因みに、鉄鋼工場においては、一時に数千リットルの磁粉液が調製される場合もあり、かゝる場合には強力な攪拌が必要とされているので、磁粉液調製時に強力な攪拌を必要としない点は、特筆すべき効果といえる）、しかも、貯蔵時においては優れた保存安定性を具備している湿式磁粉探傷試験用発泡性蛍光磁粉が提供できる。
【００７９】
また、本発明に係る湿式磁粉探傷試験用発泡性蛍光磁粉は、その各配合成分材料が市販品から容易に入手できると共に、特別な技術・装置を必要とせずに簡易に製造できる。
【００８０】
従って、本発明は鉄鋼工場や自動車工場における湿式磁粉探傷試験方法の作業効率の向上に大きく貢献できるものであり、その産業利用性は非常に大きい。[0001]
[Industrial application fields]
The present invention relates to a foamable fluorescent magnetic powder for a wet magnetic particle flaw detection test, and the fluorescent magnetic powder is used in a wet magnetic particle flaw detection test method implemented in a steel factory or an automobile factory.
[0002]
[Prior art]
As is well known, steel products such as square billets and round billets are used as inspection objects in steel factories, and steel parts such as knuckle arms and shafts are used as inspection objects in automobile factories. JIS-G-0565-1992 ( A wet magnetic particle testing method defined in (Magnetic particle testing method of iron and steel materials and classification of magnetic powder pattern) has been implemented.
[0003]
The wet magnetic particle flaw detection test method is usually performed by magnetizing a magnetic powder liquid (also called “inspection liquid” in the industry) in which 0.2 to 15 g of fluorescent magnetic powder is dispersed per liter of water. This is a test method for flaw detection by bringing the fluorescent magnetic powder into contact with a flaw and adsorbing the fluorescent magnetic powder to a flaw (defect portion).
[0004]
Generally, in the preparation of the magnetic powder solution, commercially available fluorescent magnetic powder for magnetic particle flaw detection test and commercially available magnetic powder dispersant for wet magnetic powder flaw detection test are used.
[0005]
The commercially available magnetic particle for magnetic particle flaw detection test has an average particle diameter of 1 to 25 μm in which a fluorescent pigment or a fluorescent dye is adhered to the surface of each particle of a conductive particle powder (pure iron particle powder, iron oxide particle powder, stainless steel particle powder, etc.). As a representative commercially available product, “Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktech Co., Ltd.)” can be mentioned.
[0006]
The commercially available magnetic powder dispersant for wet magnetic particle flaw detection test includes a liquid type and a powder type. The former is 1 to 20% by weight of a nonionic surfactant having an HLB value of 8 to 14 and a silicon antifoaming agent 0.1. 10 wt% is dissolved or dispersed, and as a typical commercially available product, "Super Magna (supra) magnetic powder dispersant BC-700 (trade name, manufactured by Mark Tech Co., Ltd.)" can be mentioned, The latter is a water-soluble particle powder (for example, sodium tripolyphosphate, sodium nitrite, etc.) 70 to 99.4% by weight, 0.5 to 20% by weight of a liquid nonionic surfactant having an HLB value of 8 to 14 and a silicon antifoaming agent. 0.1 to 10% by weight is adsorbed, and a typical commercially available product is “Super Magna (supra) magnetic powder dispersant BC-1 (trade name, manufactured by Marktec Co., Ltd.) / Water-soluble particles. Tripo as powder Soda particles phosphoric acid is used. "And the like.
[0007]
Incidentally, regarding a liquid type magnetic particle dispersant for wet magnetic particle flaw detection test, Japanese Patent Publication No. 2-59426 discloses water, nonionic surfactant, silicon antifoaming agent, rust preventive agent and dimethylpolysiloxane-polyoxyalkylene copolymer. The union is made up of 2- 52987 Japanese Patent Application Laid-Open No. 7-120437 discloses a powder type wet magnetic particle flaw detection magnetic powder dispersant for water, a nonionic surfactant, a silicon antifoaming agent and soap. Patent No. 2813948) discloses a water-soluble particle powder passing through a 5-mesh sieve of 70 to 99.4% by weight, a liquid nonionic surfactant having an HLB value of 8 to 14 and 0.5 to 20% by weight, and a silicon antifoaming agent. Japanese Patent Application Laid-Open No. 8-304347 discloses a liquid nonionic interface having 70 to 99.4% by weight of water-soluble particle powder passing through a 16 mesh sieve and an HLB value of 8 to 14. Water-insoluble non-magnetic particles passing through a 200-mesh sieve with respect to 100 parts by weight of a powdery composition comprising 0.5 to 20% by weight of an activator and 0.1 to 10% by weight of a silicon antifoaming agent Made by mixing the powder 2 to 30 parts by weight is disclosed, respectively.
[0008]
In the preparation of a magnetic powder liquid in which 0.2 to 15 g of fluorescent magnetic powder is dispersed per 1 liter of water, the liquid type magnetic powder dispersant for commercially available wet magnetic particle flaw detection test and each magnetic powder for wet magnetic particle flaw detection test disclosed in the above publications When a dispersant is used, it is added so that the dispersant concentration is 1 to 3% per liter of water, and is disclosed in the above-mentioned powder type magnetic powder dispersant for commercial wet magnetic particle flaw detection test and the above-mentioned publications. When using a magnetic powder dispersant for each wet magnetic particle testing, the active ingredients per 1 liter of water (components other than water-soluble particle powder and / or water-insoluble particle powder: surfactant, silicon antifoaming agent, etc.) An amount that gives a concentration of 1 to 3% is added.
[0009]
In the implementation site of the wet magnetic particle flaw detection test method, the magnetic powder liquid is prepared using the fluorescent magnetic powder for the commercial magnetic particle flaw detection test and the magnetic powder dispersant for the commercially available wet magnetic particle flaw detection test. Weighing work for weighing a predetermined amount of each of the fluorescent magnetic powder and the dispersant is essential.
[0010]
By the way, in steel factories and automobile factories, improvement in work efficiency in minutes, seconds and increments is being attempted, and simplification of the weighing work is strongly desired.
[0011]
The manufacturers of magnetic powder for magnetic particle flaw detection testing and magnetic powder dispersants for wet magnetic particle flaw detection testing have continued research and development for many years in order to meet the above demands. Japanese Patent Publication No. 50-469 and Japanese Patent Application Laid-Open No. 57-141547. Japanese Patent Publication No. 56-49311 and Japanese Patent Publication No. 3-42427 disclose a magnetic powder for magnetic particle flaw detection test in which a surfactant is previously adhered to the magnetic powder. A magnetic powder molded product for a magnetic particle flaw detection test formed by molding magnetic powder is disclosed.
[0012]
As seen in the above-mentioned publications, the technical means of imparting dispersibility to the magnetic powder for magnetic particle flaw detection has been proposed for a long time by attaching a surfactant to magnetic powder (fluorescent magnetic powder or non-fluorescent magnetic powder) in advance. Has been.
[0013]
However, in order to disperse the magnetic powder for magnetic particle testing in water, it is necessary to use a liquid nonionic surfactant having an HLB value of 8 to 14 (U.S. military standard MIL-STD-1949A: 4, 9, In item 4, a nonionic surfactant is supposed to be used.) Since the surfactant is a non-volatile viscous liquid, the fluorescent magnetic powder to which it is attached will aggregate during storage. There is a problem that a sufficiently dispersed state cannot be obtained at the time of preparing the magnetic powder solution, and the surfactant is strong in permeability, so that the fluorescent magnetic powder to which this is attached peels off part of the pigment or dye during storage However, since the fluorescent pigment or fluorescent dye peeled off during the flaw detection appears as noise (referred to as “background phenomenon” in the industry), there is a problem that the flaw detection accuracy is lowered. In fact, as far as the present inventor knows, there is no practical example of magnetic powder for magnetic particle flaw detection test in which a liquid nonionic surfactant having an HLB value of 8 to 14 is attached to fluorescent magnetic powder in advance.
[0014]
[Problems to be solved by the invention]
Therefore, the present invention can solve the above-mentioned problems despite the use of a liquid nonionic surfactant having an HLB value of 8 to 14, and can meet the demand for simplification of the weighing operation. An object of the present invention is to provide a foamable fluorescent magnetic powder for wet magnetic particle flaw detection test that can exhibit better water dispersibility when preparing a magnetic powder.
[0015]
[Means for Solving the Problems]
The technical problem of the present invention can be achieved by the present invention as follows.
[0016]
That is, in the present invention, 100 parts by weight of a fluorescent magnetic powder for magnetic particle flaw detection in which a fluorescent pigment or fluorescent dye is attached to the surface of each particle of the magnetically conductive particle powder and a liquid nonionic surfactant having an HLB value of 8 to 14 are 20 to 30 weights. The slurry is composed of 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or bicarbonate powder, and 25 to 35 parts by weight of organic acid salt powder. It is a foamable fluorescent magnetic powder for wet magnetic particle flaw detection test, which is obtained by powdering a product.
[0017]
The present invention also provides 100 parts by weight of a fluorescent magnetic powder for magnetic particle flaw detection in which a fluorescent pigment or a fluorescent dye is attached to the surface of each particle of the magnetically conductive particle powder, and a liquid nonionic surfactant having an HLB value of 8 to 14 to 20 to 30 weights. In addition, 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or hydrogencarbonate powder, 25 to 35 parts by weight of organic acid salt powder, and a silicon-based antifoaming agent. 3 to 10 parts by weight and / or rust inhibitor 0.3 to 10 parts by weight are mixed, and the muddy matter is pulverized to form a foamable fluorescent magnetic powder for a wet magnetic particle flaw detection test.
[0018]
Furthermore, in the present invention, 100 parts by weight of fluorescent magnetic powder for magnetic particle flaw detection test, in which a fluorescent pigment or fluorescent dye is adhered to the surface of each particle of the magnetically conductive particle powder, is a liquid nonionic surfactant having an HLB value of 8 to 14 to 20 to 30 weights. The slurry is dispersed in a part to obtain a muddy substance, and then the muddy substance is added with 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or bicarbonate powder, and 25 to 35 parts by weight of organic acid powder. Is added and stirred to pulverize the mud, which is a method for producing a foamable fluorescent magnetic powder for wet magnetic particle flaw detection test.
[0019]
The configuration of the present invention will be described in more detail as follows.
[0020]
First, as the fluorescent magnetic powder for magnetic particle flaw detection test in the present invention, the above-mentioned fluorescent magnetic powder for magnetic particle flaw detection may be used. For example, Super Magna (supra) fluorescent magnetic powder LY-10 (supra) is suitable.
[0021]
As the liquid nonionic surfactant having an HLB value of 8 to 14 in the present invention, a commercially available product may be used. For example, New Coal 864 (trade name: Nippon Emulsifier Co., Ltd .: HLB 13.8) or Octapol 50 (Product name: Sanyo Chemical Co., Ltd .: HLB10.3) is preferred.
[0022]
Next, the sodium tripolyphosphate powder in the present invention is preferably a powder that passes through a 16-mesh sieve (aperture 1000 μm · JIS-Z-8801) in view of the dissolution rate at the time of use. A particle having a particle size may be selected and obtained.
[0023]
The carbonate powder or bicarbonate powder in the present invention may be any powder that reacts with an organic acid in water to generate carbon dioxide gas. Specifically, commercially available sodium carbonate powder, potassium carbonate powder, A magnesium carbonate powder, a sesquisodium carbonate powder, a sodium hydrogencarbonate powder etc. are mentioned, These may be used individually or in mixture. In addition, it is preferable to select and obtain a particle powder that passes through a 16-mesh sieve (described above) in view of the dissolution rate when the target product is used.
[0024]
Moreover, as an organic acid powder in this invention, commercially available succinic acid powder, malic acid powder, aragonic acid powder, fumaric acid powder, etc. are mentioned, These may be used individually or in mixture. In addition, it is preferable to select and obtain a particle powder that passes through a 16-mesh sieve (described above) in view of the dissolution rate when the target product is used.
[0025]
The blending amounts of the magnetic powder for magnetic particle testing in the present invention, the liquid nonionic surfactant having the HLB value of 8 to 14, the sodium tripolyphosphate powder, the carbonate powder or the bicarbonate powder, and the organic acid powder are as follows: is important.
[0026]
In the case of 100 parts by weight of the magnetic powder for magnetic particle testing, the liquid nonionic surfactant having an HLB value of 8 to 14 needs to be 20 parts by weight or more, and if it is less than 20 parts by weight, the fluorescent magnetic powder is sufficiently dispersed when the magnetic powder is prepared. This makes it difficult to wet the prepared magnetic powder solution. Even if it exceeds 30 parts by weight, the dispersibility and the wetting effect of the fluorescent magnetic powder are not improved so much and it adversely affects the powder flowability of the target product, so it should be stopped within 30 parts by weight.
[0027]
The sodium tripolyphosphate powder requires at least 170 parts by weight, and if it is less than 170 parts by weight, 100 parts by weight of the fluorescent magnetic powder for magnetic particle testing and 20-30 parts by weight of a liquid nonionic surfactant having an HLB value of 8-14. It becomes difficult to pulverize the mud consisting of the above and impart sufficient powder fluidity. The upper limit of the blending amount is determined from the proportions of the other blending components, but sufficient powder fluidity can be imparted if it is within the range of 170 to 220 parts by weight.
[0028]
In addition, when the fluorescent magnetic powder to which the liquid nonionic surfactant of HLB 8-14 is adhered is left as it is, the surfactant binds the fluorescent magnetic powder particles during storage as described above. The fluorescent magnetic powder aggregates in a lump, and the surfactant permeates into the fluorescent pigment layer or fluorescent dye layer on the surface of the fluorescent magnetic powder particle, so that part of the fluorescent pigment or fluorescent dye peels off, When the tripolyphosphate powder is mixed, since the tripolyphosphate powder has a large oil absorption amount, it absorbs and carries the surfactant adhering to the fluorescent magnetic powder particles, so that the aggregation can be suppressed, Moreover, the said peeling can also be suppressed.
[0029]
The use ratio of the carbonate or hydrogen carbonate powder and the organic acid powder is particularly important, and it is necessary to use the former: the latter = 1: 1 to 3, and the former: the latter = 1: 1. If it is less than the above, since the pH value of the magnetic powder solution in which the sodium tripolyphosphate powder is dissolved exhibits alkalinity, there is no reaction between the former and the latter, so that self-foaming property can be imparted to the target product. In addition, when the former: latter = 1: 3 or more, the pH value of the magnetic powder solution in which the sodium tripolyphosphate powder is dissolved is acidic, so that the steel material or the steel part which is the object to be inspected is used. Risk of rusting.
[0030]
Accordingly, 15 to 25 parts by weight of the carbonate powder or bicarbonate powder is blended and 25 to 35 parts by weight of the organic acid powder is blended. In addition, each upper limit of both compounding quantities is decided from the amount of other compounding components.
[0031]
Making the pH value of the magnetic powder solution in which the tripolyphosphate powder is dissolved neutral to weakly alkaline by adjusting within the range of the blending amount of the carbonate powder or bicarbonate powder and the organic acid powder. Can do.
[0032]
The foamable fluorescent magnetic powder for wet magnetic particle flaw detection test according to the present invention, which is obtained by blending each of the above-mentioned blending components in the above blending amount, is self-foamed and quickly dissolves when dissolved in water during the preparation of the magnetic powder solution. Almost no foaming is observed, but when it is necessary to sufficiently suppress foaming after the fluorescent magnetic powder is dispersed, a silicone-based antifoaming agent is blended in the same manner as the above-mentioned dispersing agent for magnetic powder liquid. can do.
[0033]
Commercially available products may be used as the silicon-based antifoaming agent in the present invention. For example, silicon antifoaming agent KM508 (trade name: manufactured by Shin-Etsu Chemical Co., Ltd.) and silicon antifoaming agent KM531 (trade name: manufactured by Shin-Etsu Chemical Co., Ltd.) ) Is preferred.
[0034]
The silicon-based antifoaming agent requires 0.3 parts by weight or more, and if it is less than 0.3 parts by weight, it is difficult to obtain an antifoaming effect. Usually, it is sufficient to add about 1 to 5 parts by weight. It is not necessary to add more than part by weight.
[0035]
In addition, since the sodium tripolyphosphate powder has rust preventive power, it is usually not necessary to add a rust preventive, but when strong rust preventive power is required depending on the material of the object to be inspected. A rust preventive agent can also be blended.
[0036]
As the rust preventive agent in the present invention, commercially available sodium nitrite powder or sodium gluconate powder is suitable, and it is usually sufficient to add about 0.3 to 10 parts by weight, and it exceeds 10 parts by weight. do not have to.
[0037]
The production method of the foamable fluorescent magnetic powder for wet magnetic particle flaw detection test according to the present invention is as follows.
[0038]
First, as a first step, a predetermined amount of each of the magnetic powder for magnetic particle flaw detection test and the liquid nonionic surfactant having an HLB value of 8 to 14 is weighed and put into a container (for example, a stainless steel tank), and stirred. Mix thoroughly and stir using a vessel (for example, an electric mixer) to make a mud.
[0039]
Next, as a second step, the sodium tripolyphosphate powder, the carbonate powder or the hydrogen carbonate powder, the organic acid salt powder, and the silicon antifoam and / or the antibacterial compounded as necessary in the tank. A desired amount can be obtained by weighing out a predetermined amount of each of the rusting agents, adding the rusting agent, and further mixing and stirring to powder. In addition, what is necessary is just to perform a powdered state by visual observation and finger touch.
[0040]
Note that the order of the steps is important, and when the first step and the second step are performed simultaneously, in other words, when the blending components are mixed at the same time, they are absorbed and supported on the sodium tripolyphosphate powder. The particles of the fluorescent magnetic powder for magnetic particle flaw detection test adhere to the liquid nonionic surfactant having an HLB value of 8 to 14, so that the particles of the fluorescent magnetic powder cannot be coated with the surfactant. Since a portion where the particles are in contact with each other is produced, as seen in Comparative Example 1 described later, sufficient flaw detection ability cannot be imparted to the target (the prepared magnetic powder solution has poor dispersibility and wettability). Sufficient storage stability cannot be imparted to the target product (the part where the particles of the fluorescent magnetic powder are in direct contact is aggregated during storage). On the other hand, when moving to the second step after mixing and stirring the fluorescent magnetic powder and the surfactant in the first step to form a mud, each particle of the fluorescent magnetic powder is coated with the surfactant. Therefore, since the particles of the fluorescent magnetic powder are not in direct contact with each other, sufficient flaw detection ability and sufficient storage stability can be imparted to the object as will be seen in the embodiments and examples of the invention.
[0041]
The use method of the foamable fluorescent magnetic powder for wet magnetic particle flaw detection test according to the present invention is very simple, and if the required amount is added to water and mixed and stirred, the foamable fluorescent magnetic powder is self-foamed in water. The sodium tripolyphosphate powder, carbonate powder or bicarbonate powder and organic acid salt powder in the component dissolve quickly, and the liquid nonionic surfactant having an HLB value of 8 to 14 in the blending component quickly dissolves. The magnetic powder for magnetic particle flaw detection test in the blending component is quickly dispersed, and is the same as the case of using the above-mentioned fluorescent magnetic powder for magnetic particle flaw detection test and the magnetic powder dispersing agent for commercially available wet magnetic particle flaw detection test. A magnetic powder solution can be prepared.
[0042]
In addition, since each compounding quantity of the compounding component which comprises the foamable fluorescent magnetic powder for wet magnetic particle flaw detection tests which concerns on this invention is as above-mentioned, the said foamable fluorescent magnetic powder is the said fluorescent magnetic powder for magnetic particle flaw detection tests per about 3-4g. Contains 1g.
[0043]
DETAILED DESCRIPTION OF THE INVENTION
Production of foaming fluorescent magnetic powder for wet magnetic particle flaw detection test: Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktec Co., Ltd., using synthetic resin binder on each particle surface of iron trioxide powder) 100 parts by weight of a fluorescent pigment attached) and 20 parts by weight of New Coal 864 (trade name, manufactured by Nippon Emulsion Co., Ltd., HLB 13.8 liquid nonionic surfactant) are placed in a stainless steel tank, and an electric mixer is installed. Mix thoroughly and stir to make a mud.
[0044]
Next, 170 parts by weight of sodium tripolyphosphate powder (manufactured by Sumitomo Chemical Co., Ltd.) passing through a 16 mesh sieve (aperture 1000 μm · JIS-Z-8801), 15 parts by weight of sodium hydrogen carbonate powder (manufactured by Asahi Glass Co., Ltd.) An additional 25 parts by weight of fumaric acid powder (manufactured by Fuso Chemical Co., Ltd.) is added to the tank, and the mixture is thoroughly mixed and stirred to pulverize the mud to obtain about 330 parts by weight of foamable fluorescent magnetic powder for wet magnetic particle testing. Got.
[0045]
Powdered state evaluation test: Put the foamable fluorescent magnetic powder obtained here into a glass container, gradually tilt the glass container from the horizontal position, and measure the angle when the powdered dispersant in the container has flowed. A sample having a flow at an angle of less than 55 degrees was evaluated as “◯ (good)”, and a sample having a flow at an angle of 55 degrees or more was evaluated as “x (bad)”. As a result, it was “◯”.
[0046]
Foamability evaluation test: 3.3 g of the foamable fluorescent magnetic powder obtained here was put into a glass beaker containing 1 l of water and visually observed under a state where stirring was not performed. ) ", And no foam was evaluated as" x (bad) ". The result was “◯”.
[0047]
Dispersibility evaluation test: 3.3 g of the foamable fluorescent magnetic powder obtained here (fluorescent magnetic powder content: 1 g) was put into a glass beaker containing 1 l of water, and stirred using a mudler to prepare a magnetic powder.
[0048]
On the other hand, 1 g of Super Magna (supra) fluorescent magnetic powder LY-100 (supra) and Super Magna (registered trademark) magnetic powder dispersant BC-1 (trade name, manufactured by Marktec Co., Ltd., tripolyphosphate soda powder with HLB 8-14 2 g of liquid nonionic surfactant adsorbed / supported) was mixed, and the mixture was put into a glass beaker containing 1 l of water, and stirred using a mudler to prepare a comparative magnetic powder.
[0049]
When the dispersion state of both magnetic powder liquids was visually observed under the irradiation of an ultraviolet lamp in a dark place, and a dispersion state equivalent to the dispersion state of the sufficiently dispersed magnetic powder liquid for comparison was visually confirmed, (Good) ”was evaluated as“ × (bad) ”when a dispersed state inferior to the difficult state of the magnetic powder for comparison was visually confirmed. The result was “◯”.
[0050]
Flaw detection ability evaluation test: 3.3 g of the foamable fluorescent magnetic powder obtained here (fluorescent magnetic powder content: 1 g) was put into a glass beaker containing 1 l of water, and stirred using a mudler to prepare a magnetic powder solution.
[0051]
On the other hand, 1 g of Super Magna (supra) fluorescent magnetic powder LY-100 (supra) and 2 g of Super Magna (previous) magnetic powder dispersant BC-1 (supra) are mixed, and the mixture contains 1 l of water. The glass powder was put into a glass beaker and stirred using a mudler to prepare a comparative magnetic powder solution.
[0052]
The following wet magnetic particle flaw detection test method was carried out using the both magnetic powder solutions.
[0053]
JIS-0565-1992 standard type A test piece (circular type, AI-15 / 100, AI-30 / 100) was used as an object to be inspected, and the test piece was attached to a steel square billet. Was magnetized by a porcelain energization method, and a magnetic powder solution was sprayed on the test piece, and the test surface was visually observed in the dark under an ultraviolet lamp. As a result, when a clear defect indication pattern equivalent to the comparative magnetic powder solution in which a clear defect indication pattern could be observed was observed, “○ (good)” was compared with the defect indication pattern using the comparative magnetic powder solution. When an unclear defect indication pattern was visually recognized, it was evaluated as “× (bad)”. The result was “◯”.
[0054]
Storage stability evaluation test: After the foamable fluorescent magnetic powder obtained here is left indoors at room temperature (about 25 ° C) for 1 month, 3.3 g of the foamable fluorescent magnetic powder is placed in a glass beaker containing 1 liter of water. After the magnetic powder solution was prepared by stirring with a mudler, it was visually observed under ultraviolet light irradiation in a dark place with no stirring. “Good” ”, and“ × (bad) ”when aggregation occurred. The result was “◯”.
[0055]
[Action]
The foamable fluorescent magnetic powder for wet magnetic particle flaw detection test according to the present invention contains a liquid nonionic surfactant having an HLB value of 8 to 14 in the blending component. A magnetic powder solution can be prepared only by stirring, and since the surfactant is adsorbed and supported on the tripolyphosphate powder in the blending component, it is excellent in storage stability.
[0056]
Further, since the carbonate powder or the hydrogen carbonate powder and the organic acid powder are included in the blending components, the carbonate powder or the hydrogen carbonate powder and the organic powder in water when put into water. The acid reacts to generate carbon dioxide, which causes foaming. Since the foaming phenomenon promotes dissolution and dispersion of each compounding component, a magnetic powder liquid in which the fluorescent magnetic powder is sufficiently dispersed can be prepared without performing strong stirring.
[0057]
Since the reaction between the carbonate powder or the bicarbonate powder and the organic acid powder in water is an endothermic reaction, heat generation due to the reaction between the sodium tripolyphosphate powder and water can be suppressed. Temperature rise is suppressed.
[0058]
【Example】
Examples and comparative examples are given below.
[0059]
Example 1
[0060]
Production of foaming fluorescent magnetic powder for wet magnetic particle flaw detection test: Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktec Co., Ltd., using synthetic resin binder on each particle surface of iron trioxide powder) 100 parts by weight of fluorescent pigments) and 30 parts by weight of New Coal 864 (trade name, manufactured by Nippon Emulsion Co., Ltd., HLB 13.8 liquid nonionic surfactant) are put into a stainless steel tank, and an electric mixer is installed. Mix thoroughly and stir to make a mud.
[0061]
Next, 220 parts by weight of sodium tripolyphosphate powder (manufactured by Sumitomo Chemical Co., Ltd.) passing through a 16 mesh sieve (aperture 1000 μm, JIS-Z-8801), 25 parts by weight of magnesium carbonate powder (manufactured by Tokuyama Co., Ltd.), kohaku 35 parts by weight of acid powder (manufactured by Fuso Chemical Co., Ltd.) and 5 parts by weight of silicon antifoaming agent KM508 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.) are added to the tank, and the mixture is stirred and mixed well. Was powdered to obtain about 415 parts by weight of foamable fluorescent magnetic powder for wet magnetic particle testing. The foamable fluorescent magnetic powder contains 1 g of magnetic powder flaw detecting fluorescent magnetic powder (super magna fluorescent magnetic powder LY-10) per 4.15 g.
[0062]
About the foamable fluorescent magnetic powder obtained here, the result of having performed the same evaluation test as each evaluation test in above-mentioned invention embodiment was as follows.
[0063]
Powdered state evaluation test: “◯”, Foamability evaluation test: “O”, Dispersibility evaluation test: “O”, Flaw detection ability evaluation test: “O”, Storage stability evaluation test: “O”.
[0064]
Example 2
[0065]
Production of foaming fluorescent magnetic powder for wet magnetic particle flaw detection test: Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktec Co., Ltd., using synthetic resin binder on each particle surface of iron trioxide powder) 100 parts by weight of a fluorescent pigment attached) and 25 parts by weight of New Coal 864 (trade name, manufactured by Nippon Emulsion Co., Ltd., HLB 13.8 liquid nonionic surfactant) are placed in a stainless steel tank, and an electric mixer is installed. Mix thoroughly and stir to make a mud.
[0066]
Next, 220 parts by weight of sodium tripolyphosphate powder (manufactured by Sumitomo Chemical Co., Ltd.) passing through a 16 mesh sieve (aperture 1000 μm · JIS-Z-8801), 25 parts by weight of sodium hydrogen carbonate powder (manufactured by Asahi Glass Co., Ltd.), Add 25 parts by weight of fumaric acid powder (manufactured by Fuso Chemical Co., Ltd.), 5 parts by weight of silicon antifoam KM508 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.) and 5 parts by weight of nitrous acid powder to the tank and mix thoroughly. Stirring and pulverizing the muddy material to obtain about 385 parts by weight of foamable fluorescent magnetic powder for wet magnetic particle testing. The foamable fluorescent magnetic powder contains 1 g of magnetic powder flaw detecting fluorescent magnetic powder (the super magna fluorescent magnetic powder LY-10) per 3.85 g.
[0067]
About the foamable fluorescent magnetic powder obtained here, the result of having performed the same evaluation test as each evaluation test in above-mentioned invention embodiment was as follows.
[0068]
Powdered state evaluation test: “◯”, Foamability evaluation test: “O”, Dispersibility evaluation test: “O”, Flaw detection ability evaluation test: “O”, Storage stability evaluation test: “O”.
[0069]
Comparative Example 1
[0070]
Production of foaming fluorescent magnetic powder for wet magnetic particle flaw detection test: Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktec Co., Ltd., using synthetic resin binder on each particle surface of iron trioxide powder) 100 parts by weight of fluorescent pigment attached), New Coal 864 (trade name, manufactured by Nippon Emulsion Co., Ltd., HLB13.8 liquid nonionic surfactant), 20 parts by weight, 16 mesh sieve (opening 1000 μm, JIS) -Z-8801) 170 parts by weight of sodium tripolyphosphate powder (manufactured by Sumitomo Chemical Co., Ltd.), 15 parts by weight of sodium carbonate powder (manufactured by Asahi Glass Co., Ltd.) and 25 parts by weight of fumaric acid powder (manufactured by Fuso Chemical Co., Ltd.) Part was put into a stainless steel tank and sufficiently mixed and stirred using an electric mixer to obtain about 330 parts by weight of comparative foamable fluorescent magnetic powder. This comparative foaming fluorescent magnetic powder contains 1 g of magnetic powder flaw detection fluorescent magnetic powder (super magna fluorescent magnetic powder LY-10) per 3.3 g.
[0071]
About the comparative foamable fluorescent magnetic powder obtained here, the result of having performed the same evaluation test as each evaluation test in above-mentioned embodiment of the invention was as follows.
[0072]
Powdered state evaluation test: “◯”, Foamability evaluation test: “O”, Dispersibility evaluation test: “O”, Flaw detection ability evaluation test: “×”, Storage stability evaluation test: “×”.
[0073]
Comparative Example 2
[0074]
Production of foaming fluorescent magnetic powder for wet magnetic particle flaw detection test: Super Magna (registered trademark) fluorescent magnetic powder LY-10 (trade name, manufactured by Marktec Co., Ltd., using synthetic resin binder on each particle surface of iron trioxide powder) 100 parts by weight of fluorescent pigment attached) and 25 parts by weight of New Coal 864 (trade name, manufactured by Nippon Emulsion Co., Ltd., HLB 13.8 liquid nonionic surfactant) are placed in a stainless steel tank, and an electric mixer is installed. Mix thoroughly and stir to make a mud.
[0075]
Next, 170 parts by weight of tripolyphosphate soda powder (manufactured by Sumitomo Chemical Co., Ltd.) passing through a 16 mesh sieve (aperture 1000 μm, JIS-Z-8801) and silicon antifoam KM508 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.) ) 5 parts by weight were additionally charged into the tank and thoroughly mixed and stirred to powder the mud to obtain about 385 parts by weight of a comparative foamable fluorescent magnetic powder. The comparative fluorescent magnetic powder contains 1 g of magnetic particle flaw detection fluorescent magnetic powder (the super magna fluorescent magnetic powder LY-10) per 3 g.
[0076]
About the comparative foamable fluorescent magnetic powder obtained here, the result of having performed the same evaluation test as each evaluation test in above-mentioned embodiment of the invention was as follows.
[0077]
Powdered state evaluation test: “◯”, foamability evaluation test: “×”, dispersibility evaluation test: “×”, flaw detection ability evaluation test: “◯”, storage stability evaluation test: “◯”.
[0078]
【The invention's effect】
According to the present invention, it is possible to simplify the weighing work at the time of preparing the magnetic powder solution, and to exhibit excellent water dispersibility by self-foaming when thrown into water, and the fluorescent magnetic powder is sufficiently dispersed without performing strong stirring. The magnetic powder solution can be easily prepared (by the way, in a steel factory, thousands of liters of magnetic powder solution may be prepared at one time, and in such cases, strong stirring is required. The fact that strong stirring is not required when preparing the magnetic powder solution is a remarkable effect), and in addition, it is possible to provide a foaming fluorescent magnetic powder for wet magnetic particle flaw detection tests that has excellent storage stability during storage. .
[0079]
Further, the foamable fluorescent magnetic powder for wet magnetic particle flaw detection test according to the present invention can be easily produced without requiring any special technique / equipment while each compounding component material can be easily obtained from commercial products.
[0080]
Therefore, the present invention can greatly contribute to the improvement of the working efficiency of the wet magnetic particle testing method in steel factories and automobile factories, and its industrial applicability is very large.

Claims

A muddy state comprising 100 parts by weight of fluorescent magnetic powder for magnetic particle flaw detection test, in which a fluorescent pigment or fluorescent dye is attached to the surface of each particle of the magnetically conductive particle powder, and 20-30 parts by weight of a liquid nonionic surfactant having an HLB value of 8-14. To the product, 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or bicarbonate powder and 25 to 35 parts by weight of organic acid salt powder are mixed to powder the mud. Foamable fluorescent magnetic powder for wet magnetic particle testing.

A muddy state comprising 100 parts by weight of fluorescent magnetic powder for magnetic particle flaw detection test, in which a fluorescent pigment or fluorescent dye is attached to the surface of each particle of the magnetically conductive particle powder, and 20-30 parts by weight of a liquid nonionic surfactant having an HLB value of 8-14. In addition, 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or bicarbonate powder, 25 to 35 parts by weight of organic acid salt powder, 0.3 to 10 parts by weight of silicon-based antifoaming agent, and Foamable fluorescent magnetic powder for wet magnetic particle flaw detection test obtained by mixing 0.3 to 10 parts by weight of a rust inhibitor and powdering the mud.

100 parts by weight of fluorescent magnetic powder for magnetic particle flaw detection test, in which a fluorescent pigment or fluorescent dye is attached to the surface of each particle of the magnetically conductive particle powder, is dispersed in 20-30 parts by weight of a liquid nonionic surfactant having an HLB value of 8-14. Then, 170 to 220 parts by weight of sodium tripolyphosphate powder, 15 to 25 parts by weight of carbonate powder or hydrogencarbonate powder, and 25 to 35 parts by weight of organic acid powder are added to the mud and stirred. A method for producing foamable fluorescent magnetic powder for wet magnetic particle flaw detection test, characterized in that the mud is pulverized.