JP7328484B2 - 高熱膨張係数オルトリン酸塩遮熱コーティング材料及びその製造方法 - Google Patents
高熱膨張係数オルトリン酸塩遮熱コーティング材料及びその製造方法 Download PDFInfo
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Description
高熱膨張係数オルトリン酸塩遮熱コーティング材料であって、その一般的な化学式はReM3P3O12であり、立方晶系-43m点群に属し、結晶構造は珪蒼鉛石構造である。ここで、Reは希土類元素、Mはアルカリ土類金属である。
NdBa3P3O12、GdBa3P3O12、DyBa3P3O12、HoBa3P3O12、ErBa3P3O12のうちの1種類から選択される。
1:(4~8):(4~8)のモル比に従って、希土類酸化物、アルカリ土類金属含有化合物、P含有化合物を均一に混合し、マッフル炉に入れて1000℃~1100℃に加熱し、一定温度で4~6時間保持し、1回目の焼結を行い、予備焼結原料を得るステップ(1)と、
予備焼結原料を研磨して圧縮成形してマッフル炉に入れ、1300℃~1500℃に加熱し、2回目の焼結を行って純相材料を得るステップ(2)と、
純相材料に無水エタノールを添加し、湿式ボールミル粉砕法を使用して20~30時間ボールミル粉砕し、次に乾燥させ、研磨して、ふるいにかけた後にブランクに押し込むステップ(3)と、
ブランクをマッフル炉に入れ、1500℃~1700℃まで加熱し、空気雰囲気で高温反応を行い、反応が終了した後に炉内で冷却して、高熱膨張係数オルトリン酸塩遮熱コーティング材料を得るステップ(4)と、を含む。
酸化ネオジム、炭酸バリウム、リン酸二水素アンモニウムを原料としてNdBa3P3O12材料を調製するステップは、
Nd2O3、BaCO3及びNH4H2PO4を原料として、モル比1:6:6で混合したステップ(1)と、
ステップ(1)で調製した原料を均一に混合した後、アルミナるつぼ内に入れ、マッフル炉内に入れて1回目の焼結を行い、焼結温度は1000±50℃、温度を5時間一定に保って原料中のCO2、NH3及びH2Oを除去して予備焼結原料を得たステップ(2)と、
ステップ(2)における予備焼結原料を研磨し、棒状に押し込み、マッフル炉に入れて、1400℃の焼結温度で2回目の焼結を行い、純相材料を得たステップ(3)と、
純相材料に無水エタノールを添加し、48時間ボールミル粉砕して、無水エタノールの添加量と純相材料の質量比は1:3で、次に乾燥させたステップ(4)と、
ステップ(4)における粉末を十分に研磨し、ふるいにかけ(200メッシュ)、300MPa下でブランクに押し込んだステップ(5)と、
ブランクをマッフル炉に入れ、1600℃まで加熱し、空気雰囲気で高温反応を行い、反応時間は10時間で、そして炉内で冷却したステップ(6)と、
冷却後、反応物を取り出し、化学式NdBa3P3O12(略称:NdBP)の材料を得たステップ(7)と、を含む。
酸化ガドリニウム、炭酸バリウム、リン酸二水素アンモニウムを原料としてGdBa3P3O12材料を調製するステップは、
Gd2O3、BaCO3及びNH4H2PO4を原料として、モル比1:6:6で混合したステップ(1)と、
ステップ(1)で調製した原料を均一に混合した後、アルミナるつぼ内に入れ、マッフル炉内に入れて1回目の焼結を行い、焼結温度は1000±50℃、温度を5時間一定に保って原料中のCO2、NH3及びH2Oを除去して予備焼結原料を得たステップ(2)と、
ステップ(2)における予備焼結原料を研磨し、棒状に押し込み、マッフル炉に入れて、1400℃の焼結温度で2回目の焼結を行い、純相材料を得たステップ(3)と、
純相材料に無水エタノールを添加し、48時間ボールミル粉砕して、無水エタノールの添加量と純相材料の質量比は1:3で、次に乾燥させたステップ(4)と、
ステップ(4)における粉末を十分に研磨し、ふるいにかけ(200メッシュ)、300MPa下でブランクに押し込んだステップ(5)と、
ブランクをマッフル炉に入れ、1600℃まで加熱し、空気雰囲気で高温反応を行い、反応時間は10時間で、そして炉内で冷却したステップ(6)と、
冷却後、反応物を取り出し、化学式GdBa3P3O12(略称:GdBP)の材料を得たステップ(7)と、を含む。
酸化ディスプロシウム、炭酸バリウム、リン酸二水素アンモニウムを原料としてDyBa3P3O12材料を調製するステップは、
Dy2O3、BaCO3及びNH4H2PO4を原料として、モル比1:6:6で混合したステップ(1)と、
ステップ(1)で調製した原料を均一に混合した後、アルミナるつぼ内に入れ、マッフル炉内に入れて1回目の焼結を行い、焼結温度は1000±50℃、温度を5時間一定に保って原料中のCO2、NH3及びH2Oを除去して予備焼結原料を得たステップ(2)と、
ステップ(2)における予備焼結原料を研磨し、棒状に押し込み、マッフル炉に入れて、1400℃の焼結温度で2回目の焼結を行い、純相材料を得たステップ(3)と、
純相材料に無水エタノールを添加し、48時間ボールミル粉砕して、無水エタノールの添加量と純相材料の質量比は1:3で、次に乾燥させたステップ(4)と、
ステップ(4)における粉末を十分に研磨し、ふるいにかけ(200メッシュ)、300MPa下でブランクに押し込んだステップ(5)と、
ブランクをマッフル炉に入れ、1600℃まで加熱し、空気雰囲気で高温反応を行い、反応時間は10時間で、そして炉内で冷却したステップ(6)と、
冷却後、反応物を取り出し、化学式DyBa3P3O12(略称:DyBP)の材料を得たステップ(7)と、を含む。
酸化ホルミウム、炭酸バリウム、リン酸二水素アンモニウムを原料としてHoBa3P3O12材料を調製するステップは、
Ho2O3、BaCO3及びNH4H2PO4を原料として、モル比1:6:6で混合したステップ(1)と、
ステップ(1)で調製した原料を均一に混合した後、アルミナるつぼ内に入れ、マッフル炉内に入れて1回目の焼結を行い、焼結温度は1000±50℃、温度を5時間一定に保って原料中のCO2、NH3及びH2Oを除去して予備焼結原料を得たステップ(2)と、
ステップ(2)における予備焼結原料を研磨し、棒状に押し込み、マッフル炉に入れて、1400℃の焼結温度で2回目の焼結を行い、純相材料を得たステップ(3)と、
純相材料に無水エタノールを添加し、48時間ボールミル粉砕して、無水エタノールの添加量と純相材料の質量比は1:3で、次に乾燥させたステップ(4)と、
ステップ(4)における粉末を十分に研磨し、ふるいにかけ(200メッシュ)、300MPa下でブランクに押し込んだステップ(5)と、
ブランクをマッフル炉に入れ、1600℃まで加熱し、空気雰囲気で高温反応を行い、反応時間は10時間で、そして炉内で冷却したステップ(6)と、
冷却後、反応物を取り出し、化学式HoBa3P3O12(略称:HoBP)の材料を得たステップ(7)と、を含む。
酸化エルビウム、炭酸バリウム、リン酸二水素アンモニウムを原料としてErBa3P3O12材料を調製するステップは、
Er2O3、BaCO3及びNH4H2PO4を原料として、モル比1:6:6で混合したステップ(1)と、
ステップ(1)で調製した原料を均一に混合した後、アルミナるつぼ内に入れ、マッフル炉内に入れて1回目の焼結を行い、焼結温度は1000±50℃、温度を5時間一定に保って原料中のCO2、NH3及びH2Oを除去して予備焼結原料を得たステップ(2)と、
ステップ(2)における予備焼結原料を研磨し、棒状に押し込み、マッフル炉に入れて、1400℃の焼結温度で2回目の焼結を行い、純相材料を得たステップ(3)と、
純相材料に無水エタノールを添加し、48時間ボールミル粉砕して、無水エタノールの添加量と純相材料の質量比は1:3で、次に乾燥させたステップ(4)と、
ステップ(4)における粉末を十分に研磨し、ふるいにかけ(200メッシュ)、300MPa下でブランクに押し込んだステップ(5)と、
ブランクをマッフル炉に入れ、1600℃まで加熱し、空気雰囲気で高温反応を行い、反応時間は10時間で、そして炉内で冷却したステップ(6)と、
冷却後、反応物を取り出し、化学式ErBa3P3O12(略称:ErBP)の材料を得たステップ(7)と、を含む。
1、実施例1~5のReM3P3O12遮熱コーティング材料に対してXRD試験を実行し、試験結果を図1に示す。
2、実施例1~5のReBa3P3O12遮熱コーティング材料の硬度を図2に、弾性率を図3に、TG-DTA曲線を図4に、熱膨張係数を図5に、熱伝導率を図6に示す。
Claims (8)
- NdBa 3 P 3 O 12 、GdBa 3 P 3 O 12 、DyBa 3 P 3 O 12 、HoBa 3 P 3 O 12 、ErBa 3 P 3 O 12 のうちの1種類から選択される高熱膨張係数オルトリン酸塩遮熱コーティング材料であって、立方晶系-43m点群に属し、結晶構造は珪蒼鉛石構造である高熱膨張係数オルトリン酸塩遮熱コーティング材料。
- 1:(4~8):(4~8)のモル比に従って、希土類酸化物、アルカリ土類金属含有化合物、P含有化合物を均一に混合し、マッフル炉に入れて1000℃~1100℃に加熱し、一定温度で4~6時間保持し、1回目の焼結を行い、予備焼結原料を得るステップ(1)と、 予備焼結原料を研磨して圧縮成形してマッフル炉に入れ、1300℃~1500℃に加熱し、2回目の焼結を行って純相材料を得るステップ(2)と、
純相材料に無水エタノールを添加し、湿式ボールミル粉砕法を使用して20~30時間ボールミル粉砕し、次に乾燥させ、研磨して、ふるいにかけた後にブランクに押し込むステップ(3)と、
ブランクをマッフル炉に入れ、1500℃~1700℃まで加熱し、空気雰囲気で高温反応を行い、反応が終了した後に炉内で冷却して、高熱膨張係数オルトリン酸塩遮熱コーティング材料を得るステップ(4)と、を含む請求項1に記載の高熱膨張係数オルトリン酸塩遮熱コーティング材料の製造方法。 - ステップ(1)において、希土類酸化物、アルカリ土類金属含有化合物、P含有化合物のモル比は1:6:6であることを特徴とする請求項2に記載の製造方法。
- ステップ(1)において、希土類酸化物は、Y2O3、La2O3、Nd2O3、Sm2O3、Gd2O3、Dy2O3、Ho2O3、Er2O3又はYb2O3のうちの1種類、または任意の2種類または2種類以上の組み合わせであり、希土類酸化物の純度は99.99%以上であり、アルカリ土類金属含有化合物は、BaCO3又はSrCO3又はBaCO3のうちの1種類、および2種類又は以上の組み合わせであり、P含有化合物はリン酸二水素アンモニウムであることを特徴とする請求項2に記載の製造方法。
- ステップ(1)において、希土類酸化物、炭酸塩、リン酸二水素アンモニウムの粒度は50~100μm、1回目の焼結温度は1000℃、恒温時間は5時間、1回目の焼結加熱速度は8~12℃/minであることを特徴とする請求項2に記載の製造方法。
- ステップ(2)において、2回目の焼結温度は1400℃、恒温時間は5時間、2回目の焼結の加熱速度は8~12℃/minであることを特徴とする請求項2に記載の製造方法。
- ステップ(3)において、無水エタノールの添加量と純相材料の質量比は1:(2~6)であり、ブランクに押し込む圧力は200~350MPaであることを特徴とする請求項2に記載の製造方法。
- ステップ(4)において、高温反応温度は1600~1700℃、加熱速度は1~3℃/min、高温反応時間は≧5時間であり、好ましくは、高温反応時間は8~20hであることを特徴とする請求項2に記載の製造方法。
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