JP2021508948A - 耐久性および耐薬品性が向上した淡色磁性粒子 - Google Patents
耐久性および耐薬品性が向上した淡色磁性粒子 Download PDFInfo
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Abstract
【選択図】図3
Description
酸化ジルコニウム(ZrO 2 )および銀(Ag)コーティング層が形成された磁性粒子の製造
磁性基材(substrate)としてAlNiCo、FeCrCo、CuNiFe磁性コアを準備し、それぞれの磁性コアに酸化ジルコニウムコーティング層および銀コーティング層を形成した。
下記の[表1]の組成によって原料粉末(アルミニウム粉末、ニッケル粉末、コバルト粉末、チタン粉末、銅粉末および鉄粉末、原料粉末の純度≧99.9%)を混合し、不活性雰囲気で溶解した後、凝固させてインゴットを製造した。
原料粉末の組成を下記の[表2]のように準備した以外は、AlNiCoの製造と同じ方法でFeCrCoを製造した。
原料粉末の組成を下記の[表3]のように準備した以外は、AlNiCoの製造と同じ方法でCuNiFeを製造した。
エタノールに磁性コア1g、蒸留水1mlを投入した後、超音波を照射して分散させた。ジルコニウムブトキシド(Zirconium‐tert‐butoxide)(Aldrich)1mlとエタノール170mlを混合し、ゆっくり投入した。85℃の温度で300rpmの回転速度で3時間撹拌した。酸化ジルコニウムコーティング層(11.2nm)からなる粒子を磁石で分離し、エタノールで2回洗浄した後、乾燥した。
蒸留水1200mlに硝酸銀(AgNO3)21gと水酸化ナトリウム(NaOH)4gを投入した後、水酸化アンモニウム(NH4OH)34mLを投入し、褐色の沈殿が透明な銀アミン錯体溶液に変化するように撹拌した。3に維持される銀アミン錯体溶液に酸化ジルコニウムコーティング層が形成された粒子60gを投入した後、300rpmの速度で30分間撹拌した。蒸留水400mlにグルコース20g、酒石酸カリウム1.5gを溶解した溶液(3)を二酸化チタンシェルがコーティングされたコア粒子が分散した銀アミン錯体溶液(3)に投入した後、300rpmの速度で1時間撹拌し、酸化ジルコニウムコーティング層が形成されたコア粒子に平均100nmの厚さ、銀の含有量が磁性コア重量に対して15.6重量%である銀コーティング層を形成した。次に、製造された磁性粒子を磁石で分離した後、エタノールで2回洗浄し、60で乾燥した。
酸化チタン(TiO 2 )、二酸化ケイ素(SiO 2 )および銀(Ag)コーティング層が形成された磁性粒子の製造
磁性コアとして、実施例と同様に製造したAlNiCo、CuNiFe、FeCrCoを使用し、磁性コアに酸化チタン(TiO2)および二酸化ケイ素(SiO2)コーティング層を形成した後、銀コーティング層を形成した。酸化チタンコーティング層および二酸化ケイ素コーティング層は、下記のように形成し、銀コーティング層は、実施例と同じ方法で形成した。
磁性コアに対して、磁性コア粒子1g、TBOT(tetrabuthoxy titanium)(Aldrich)1ml、蒸留水1mlにエタノール170mlを投入した後、85の温度で300rpmの回転速度で2時間撹拌し、コア粒子の表面に酸化チタンコーティング層(12.5nmの厚さ)を形成した。酸化チタンコーティング層が形成されたコア粒子を磁石で分離して回収した後、エタノールで2回洗浄および乾燥した。
磁性コアに対して、磁性コア粒子1g、TEOS(Tetraethly orthosilicate)(Aldrich)1ml、蒸留水1mlにエタノール170mlを投入した後、85の温度で300rpmの回転速度で2時間撹拌し、コア粒子表面に酸化チタンコーティング層(10.5nmの厚さ)を形成した。酸化チタンコーティング層が形成されたコア粒子を磁石で分離して回収した後、エタノールで2回洗浄および乾燥した。
以上の実施例および比較例によって製造した磁性粒子10重量%を有価証書用のセキュリティインクと混合し、アプリケータを用いて紙に展色した後、48時間以上乾燥し、反射率、耐光性、耐アルカリ性、耐酸性および磁性特性を測定した。測定結果は、[表5]〜[表13]のとおりである。磁性粒子と混合したインクの組成は、下記の[表4]のとおりである。
反射率測定装置(Varian、Cary 5000)を用いて反射率を測定した。
耐光性は、ISO2835に準じて測定し、耐光性実験装置(Atlas、Ci4000 Xenon Weather‐Ometer)を用いて240時間実験を実施した。
耐アルカリ性は、1M KOH溶液を使用して23℃で100時間測定した。
耐酸性は、磁性粒子10gを0.1M HCl溶液に2分間沈殿させた後、VSM(vibrating sample magnetometer、Lakeshore、7400series)を用いて磁性粒子の磁性特性の変化を測定した。
Claims (10)
- 磁性コアと、
前記磁性コアに形成された酸化ジルコニウムコーティング層と、
前記酸化ジルコニウムコーティング層に形成された銀コーティング層とを含む、磁性粒子。 - 前記銀コーティング層は、磁性コアの重量に対する銀の含有量が10〜20重量%である、請求項1に記載の磁性粒子。
- 前記磁性粒子の反射率は、900nmの波長で45〜75%である、請求項2に記載の磁性粒子。
- 前記磁性粒子の酸化ジルコニウムコーティング層の一部の表面が外部に露出している、請求項3に記載の磁性粒子。
- 前記磁性粒子の銀コーティング層の厚さは、50〜120nmである、請求項4に記載の磁性粒子。
- 前記磁性コアは、粒度分布D90が8〜15μmである、請求項1に記載の磁性粒子。
- Fe、Cu、Al、Ni、Co、Nb、Nd、Si、B、CrおよびSmからなる群から選択される1種以上を含む磁性コアである、請求項1に記載の磁性粒子。
- 前記磁性コアは、AlNiCo、FeCrCoまたはCuNiFeである、請求項1に記載の磁性粒子。
- 請求項1から8のいずれか一項に記載の磁性粒子を含む、セキュリティインク。
- 請求項9に記載のセキュリティインクが適用されている、有価証券。
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PCT/KR2018/013521 WO2019132232A1 (ko) | 2017-12-29 | 2018-11-08 | 내구성 및 내화학성이 향상된 담색 자성입자 |
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KR102559246B1 (ko) * | 2018-10-19 | 2023-07-25 | 한국조폐공사 | AlNiCo계 자성 입자를 포함하는 스크린 인쇄용 보안 잉크 조성물 |
KR102559243B1 (ko) * | 2018-10-19 | 2023-07-25 | 한국조폐공사 | AlNiCo계 자성 입자를 포함하는 보안 잉크 조성물 |
KR102217912B1 (ko) | 2019-07-29 | 2021-02-19 | 한국조폐공사 | AlNiCo계 경자성체 입자 및 그 제조 방법 |
JP2022128629A (ja) * | 2021-02-24 | 2022-09-05 | 日鉄鉱業株式会社 | 明度が高い半硬質磁性粉体とその合成方法 |
GB202217404D0 (en) * | 2022-11-21 | 2023-01-04 | Univ Swansea | Conductive ink |
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