KR20200133119A - Zirconium Based Ceramic Material and Method of Producing the same - Google Patents
Zirconium Based Ceramic Material and Method of Producing the same Download PDFInfo
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- KR20200133119A KR20200133119A KR1020190058013A KR20190058013A KR20200133119A KR 20200133119 A KR20200133119 A KR 20200133119A KR 1020190058013 A KR1020190058013 A KR 1020190058013A KR 20190058013 A KR20190058013 A KR 20190058013A KR 20200133119 A KR20200133119 A KR 20200133119A
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- 238000000034 method Methods 0.000 title claims description 22
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 title 1
- 229910010293 ceramic material Inorganic materials 0.000 title 1
- 229910052726 zirconium Inorganic materials 0.000 title 1
- 239000000919 ceramic Substances 0.000 claims abstract description 52
- 239000011324 bead Substances 0.000 claims abstract description 51
- 239000000843 powder Substances 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 4
- 239000000654 additive Substances 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 239000004615 ingredient Substances 0.000 claims description 16
- 239000003349 gelling agent Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 230000000996 additive effect Effects 0.000 claims description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 8
- 229910021193 La 2 O 3 Inorganic materials 0.000 claims description 7
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 7
- 229910006501 ZrSiO Inorganic materials 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 6
- 239000003381 stabilizer Substances 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- -1 Sb 2 O 3 Inorganic materials 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical class [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 claims description 4
- UHVMMEOXYDMDKI-JKYCWFKZSA-L zinc;1-(5-cyanopyridin-2-yl)-3-[(1s,2s)-2-(6-fluoro-2-hydroxy-3-propanoylphenyl)cyclopropyl]urea;diacetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O.CCC(=O)C1=CC=C(F)C([C@H]2[C@H](C2)NC(=O)NC=2N=CC(=CC=2)C#N)=C1O UHVMMEOXYDMDKI-JKYCWFKZSA-L 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 150000001860 citric acid derivatives Chemical class 0.000 claims description 3
- 239000005518 polymer electrolyte Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 238000005299 abrasion Methods 0.000 abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 20
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 5
- 235000015067 sauces Nutrition 0.000 description 3
- 229920001131 Pulp (paper) Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000679 carrageenan Substances 0.000 description 2
- 229920001525 carrageenan Polymers 0.000 description 2
- 229940113118 carrageenan Drugs 0.000 description 2
- 235000010418 carrageenan Nutrition 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
본 발명은 세륨 옥사이드가 첨가된 지르코니아 안정화 세라믹 비드 및 그 제조 방법에 관한 것이다.The present invention relates to a zirconia-stabilized ceramic bead to which cerium oxide is added and a method of manufacturing the same.
세라믹은 다른 재료에 비하여 고온강도, 내부식성, 내열성등 열적 기계적 물성이 우수함에도 불구하고, 취성 파괴에 매우 취약하며, 특히 순수 지르코니아 세라믹은 소결과정에서 불안정한 단사정상으로 변태하고 동시에 체적 팽창으로 인해 균열파괴가 발생되며, 내마모성에 중요한 인자인 경도가 낮아지게 되어 내마모성이 요구되는 제지용 펄프 제품과 금속, 비금속 채취 광산에는 치명적 결함이 된다. 따라서 균열파괴 발생을 억제하고, 경도가 우수하여 내마모성이 우수한 세라믹 비드의 제조가 요구된다.Although ceramic has superior thermal and mechanical properties such as high temperature strength, corrosion resistance, and heat resistance compared to other materials, it is very vulnerable to brittle fracture.In particular, pure zirconia ceramic transforms into an unstable monoclinic phase during sintering and cracks due to volume expansion. Destruction occurs, and the hardness, which is an important factor for abrasion resistance, decreases, resulting in a fatal defect in paper pulp products and metal and non-metal mining mines requiring wear resistance. Therefore, it is required to produce ceramic beads having excellent abrasion resistance by suppressing the occurrence of crack fracture and having excellent hardness.
본 발명의 목적은 경도가 우수하여 내마모성이 우수한 세라믹 비드 및 그 제조 방법을 제공하는 것이다.An object of the present invention is to provide a ceramic bead having excellent hardness and excellent abrasion resistance, and a method of manufacturing the same.
본 발명의 실시예에 따른 세라믹 비드 제조 방법은,Ceramic beads manufacturing method according to an embodiment of the present invention,
ZrO2 + HfO2, CeO2, Al2O3 및 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO에서 선택된 하나 이상의 산화물의 분말을 포함하는 수성 현탁액을 제조하는 단계(S10);ZrO 2 + HfO 2 , CeO 2 , Al 2 O 3 and Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 Preparing an aqueous suspension comprising a powder of one or more oxides selected from O 3 , ZnO, BaO, SrO, and CaO (S10);
상기 S10 단계에서 제조된 상기 현탁액을 과립 분체로 형성하는 단계(S20);Forming the suspension prepared in step S10 into granular powder (S20);
상기 S20 단계에서 얻어진 상기 과립 분체를 600~1000℃에서 열처리하는 단계; Heat-treating the granular powder obtained in step S20 at 600 to 1000°C;
상기 S30 단계에서 열처리된 상기 과립 분체를 구상의 형상을 나타내는 성형체로 제조하는 단계(S40); 및Manufacturing the granular powder heat-treated in step S30 into a molded body having a spherical shape (S40); And
상기 S40 단계에서 제조된 상기 성형체를 소결하는 단계(S50)를 포함하는 것을 특징으로 한다.It characterized in that it comprises a step (S50) of sintering the formed body manufactured in the step S40.
상기 S10의 현탁액은 건조 성분 함량이 50 중량% 내지 70 중량%의 범위인 것을 특징으로 한다.The suspension of S10 is characterized in that the dry ingredient content is in the range of 50% to 70% by weight.
상기 S30 단계에서 텀블링 공정을 이용하여 성형체를 구상의 형상으로 제조하는 것을 특징으로 한다.It characterized in that the formed body is manufactured in a spherical shape by using a tumbling process in step S30.
상기 S10 단계의 상기 현탁액은,The suspension of step S10,
건조 성분 중량에 대비 0 내지 5% 중량 농도의 분산제;A dispersant having a concentration of 0 to 5% by weight based on the weight of the dry ingredients;
건조 성분 중량에 대비 0 내지 10% 중량 농도의 결합제;0 to 10% by weight of the binder based on the weight of the dry ingredients;
건조 성분 중량에 대비 0 내지 3% 중량 농도의 점도 안정제; 또는A viscosity stabilizer having a concentration of 0 to 3% by weight based on the weight of the dry ingredients; or
건조 성분 중량에 대비 0 내지 3% 중량 농도의 겔화제(gelling agent)를 포함하는 것을 특징으로 한다.It characterized in that it contains a gelling agent (gelling agent) of 0 to 3% weight concentration relative to the weight of the dry ingredients.
상기 분산제 또는 상기 점도 안정제는, The dispersant or the viscosity stabilizer,
구연산 또는 암모늄 폴리카르복실산 계열, 구연산 또는 암모늄 사이트레이트 계열, 또는 고분자 전해질, 사이트레이트 계열을 포함하는 것을 특징으로 한다.It is characterized by including citric acid or ammonium polycarboxylic acid series, citric acid or ammonium citrate series, or a polymer electrolyte or citrate series.
상기 결합제 또는 상기 겔화제는, The binder or the gelling agent,
천연 카라기난 계열 또는 폴리비닐알코올 계열을 포함하는 것을 특징으로 한다.It is characterized in that it contains a natural carrageenan series or a polyvinyl alcohol series.
상기 S10 단계에서 ZrO2와 CeO2는 입자 크기가 1㎛ 내지 5㎛ 범위인 것을 특징으로 한다.In the step S10, ZrO 2 and CeO 2 have a particle size in the range of 1 μm to 5 μm.
상기 S40 단계에서,In step S40,
열처리된 상기 과립 분체는 텀블링 공정을 이용하여 구상의 형상을 나타내는 성형체로 제조되는 것을 특징으로 한다.The heat-treated granular powder is characterized in that it is manufactured into a molded body having a spherical shape using a tumbling process.
상기 S50 단계에서, In the step S50,
성형된 상기 성형체를 1000~1300℃의 온도에서 1시간 내지 5시간 동안 소결하는 것을 특징으로 한다.It characterized in that the molded body is sintered for 1 to 5 hours at a temperature of 1000 to 1300 °C.
상기 S10 단계 내지 S50 단계를 순차적으로 수행하여 제조된 세라믹 비드는 0.1mm 내지 5mm의 직경을 가지는 것을 특징으로 하는 세라믹 비드 제조 방법.The ceramic bead manufacturing method, characterized in that the ceramic bead manufactured by sequentially performing the steps S10 to S50 has a diameter of 0.1mm to 5mm.
본 발명의 다른 실시예에 따른 세라믹 비드는 총 100 중량%에 다음의 화학적 분석 결과를 나타낸다.Ceramic beads according to another embodiment of the present invention show the following chemical analysis results in a total of 100% by weight.
- ZrO2 + HfO2 : 70~78 중량%-ZrO 2 + HfO 2 : 70~78% by weight
- CeO2 : ≥ 22 중량%-CeO 2 : ≥ 22% by weight
- Al2O3 : ≥ 0.1 중량%-Al 2 O 3 : ≥ 0.1% by weight
- 첨가제 : ≥ 0.1 중량% -Additive: ≥ 0.1% by weight
- 불순물 : < 2.5 중량% -Impurities: <2.5% by weight
상기 첨가제는 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO 및 이들의 혼함물을 사용한다.The additives are Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 O 3 , ZnO, BaO, SrO, CaO and Use a mixture of these.
알루미나 및 첨가제의 조합은 지르코니아의 균열파괴의 발생을 억제시킨다. 따라서 1250℃와 같은 낮은 온도에서 소결되어 우수한 경도와 내마모성의 세라믹비드를 얻을 수 있다. The combination of alumina and additives suppresses the occurrence of zirconia cracking. Accordingly, ceramic beads having excellent hardness and wear resistance can be obtained by sintering at a low temperature such as 1250°C.
본 발명의 세라믹 비드는 다음의 조건이 필요하다. The ceramic bead of the present invention requires the following conditions.
- 알루미나 함량은 0.1 ~ 2.0 중량% 미만이고, -The alumina content is less than 0.1 to 2.0% by weight,
- 상기 첨가제의 함량은 0.1~2.0 중량% 미만이며, -The content of the additive is 0.1 to less than 2.0% by weight,
- 알루미나와 첨가제의 총 함량은 1.0~2.5 중량% 이고, -The total content of alumina and additives is 1.0 to 2.5% by weight,
- 상기 첨가제는 Fe2O3 및 / 또는 MnO2 이며, -The additive is Fe 2 O 3 and / or MnO 2 ,
- CeO2의 함량은 22 ~ 30 중량% 범위이다.-The content of CeO 2 is in the range of 22 to 30% by weight.
본 발명의 실시예에 따라 제조되는 세라믹 비드는, 특히 내마모성이 요구되는 나노그라인딩 또는 마이크로 분산 제지 펄프 제조용 및 금속과 비금속 채취 광산용으로 사용될 수 있다.The ceramic beads prepared according to an embodiment of the present invention may be used, in particular, for producing nano-grinding or micro-dispersed paper pulp requiring wear resistance, and for mining metals and non-metals.
도 1 은 본 발명의 실시예에 따른 세라믹 제조 방법을 나타내는 흐름도이다.
도 2 는 본 발명의 실시예에 따른 세라믹 제조 방법에 따라 제조된 세라믹 비드의 전자 현미경 사진을 나타낸다.1 is a flow chart showing a method of manufacturing a ceramic according to an embodiment of the present invention.
2 shows an electron micrograph of a ceramic bead manufactured according to a ceramic manufacturing method according to an embodiment of the present invention.
본 발명의 모든 세라믹 비드 조성은 비드 총 중량에 기초한 중량 백분율로 주어진다.All ceramic bead compositions of the present invention are given in weight percentage based on the total weight of the beads.
본 발명의 실시예에 따른 세라믹 비드는 총 100 중량%에 다음의 화학적 분석 결과를 나타낸다.The ceramic beads according to the embodiment of the present invention show the following chemical analysis results in a total of 100% by weight.
- ZrO2 + HfO2 : 70~78 중량%-ZrO 2 + HfO 2 : 70~78% by weight
- CeO2 : ≥ 22 중량%-CeO 2 : ≥ 22% by weight
- Al2O3 : ≥ 0.1 중량%-Al 2 O 3 : ≥ 0.1% by weight
- 첨가제 : ≥ 0.1 중량% -Additive: ≥ 0.1% by weight
- 불순물 : < 2.5 중량% -Impurities: <2.5% by weight
상기 첨가제는 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO 및 이들의 혼함물을 사용한다.The additives are Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 O 3 , ZnO, BaO, SrO, CaO and Use a mixture of these.
알루미나 및 첨가제의 조합은 지르코니아의 균열파괴의 발생을 억제시킨다. 따라서 1250℃와 같은 낮은 온도에서 소결되어 우수한 경도와 내마모성의 세라믹비드를 얻을 수 있다. The combination of alumina and additives suppresses the occurrence of zirconia cracking. Accordingly, ceramic beads having excellent hardness and wear resistance can be obtained by sintering at a low temperature such as 1250°C.
본 발명의 세라믹 비드는 다음의 조건이 필요하다. The ceramic bead of the present invention requires the following conditions.
- 알루미나 함량은 0.1 ~ 2.0 중량% 미만이고, -The alumina content is less than 0.1 to 2.0% by weight,
- 상기 첨가제의 함량은 0.1~2.0 중량% 미만이며, -The content of the additive is 0.1 to less than 2.0% by weight,
- 알루미나와 첨가제의 총 함량은 1.0~2.5 중량% 이고, -The total content of alumina and additives is 1.0 to 2.5% by weight,
- 상기 첨가제는 Fe2O3 및 / 또는 MnO2 이며, -The additive is Fe2O3 and / or MnO2,
- CeO2의 함량은 22 ~ 30 중량% 범위이다.-The content of CeO 2 is in the range of 22 to 30% by weight.
"불순물"이라는 용어는 CeO2와 같이 원료 외의 제공되는 다른 모든 성분을 의미한다.The term "impurity" refers to all other ingredients provided other than raw materials, such as CeO 2 .
본 상세한 설명에 있어서, "첨가제"라는 용어는 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO 또는 이들의 혼합물을 의미한다.In this detailed description, the term "additive" is Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO2, Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 O 3 , ZnO, BaO, SrO, CaO or mixtures thereof.
세륨 옥사이드(CeO2)의 양은 본 발명의 세라믹 비드가 실질적으로 단사정(Monoclinic) 형태의 지르코니아를 가지지 않고 정방정(Tetragonal)과 입방정(Cubic) 형태를 지니도록 한다. 정방정과 입방정 형태를 지니기 위해서는 다른 산화물의 중량에 대비 최소한 CeO2 함량이 22 중량%가 필요하다.The amount of cerium oxide (CeO 2 ) is such that the ceramic beads of the present invention have substantially no monoclinic zirconia, but tetragonal and cubic crystal forms. In order to have a tetragonal crystal and a cubic crystal shape, at least 22% by weight of CeO 2 content is required relative to the weight of other oxides.
본 발명의 세라믹 비드를 제조방법은 다음과 같다.The method of manufacturing the ceramic bead of the present invention is as follows.
먼저, ZrO2 + HfO2, CeO2, Al2O3 및 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO에서 선택된 하나 이상의 산화물의 분말을 포함하는 수성 현탁액을 실온에서 제조한다(S10).First, ZrO 2 + HfO 2 , CeO 2 , Al 2 O 3 and Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , An aqueous suspension comprising a powder of at least one oxide selected from Sb 2 O 3 , ZnO, BaO, SrO and CaO is prepared at room temperature (S10).
이러한 성분 원(Source)은 총 불순물 함량이 본 발명의 세라믹 비드 성분의 건조 성분 (Dry matter) 중 2.5 중량% 미만으로 선택된다.This source of constituents is selected so that the total impurity content is less than 2.5% by weight of the dry matter of the ceramic bead component of the present invention.
상기 S10의 현탁액은 건조 성분 함량이 50% ~70%의 범위로 존재한다. The suspension of S10 has a dry ingredient content of 50% to 70%.
본 발명의 상기 S10의 현탁액은 다음의 성분을 함유할 수 있다. The suspension of S10 of the present invention may contain the following components.
- 건조 성분 중량에 대비 0 내지 5% 중량 농도의 분산제; -A dispersant having a concentration of 0 to 5% by weight based on the weight of the dry ingredients;
- 건조 성분 중량에 대비 0 내지 10% 중량 농도의 결합제; -A binder in a concentration of 0 to 10% by weight based on the weight of the dry ingredients;
- 건조 성분 중량에 대비 0 내지 3% 중량 농도의 점도 안정제; -A viscosity stabilizer with a concentration of 0 to 3% by weight based on the weight of the dry ingredients;
- 건조 성분 중량에 대비 0 내지 3% 중량 농도의 겔화제(gelling agent). -A gelling agent having a concentration of 0 to 3% by weight based on the weight of the dry ingredients.
예로서, 다음이 언급될 수 있다.As an example, the following may be mentioned.
- 분산제 또는 점도 안정제로서, 구연산 또는 암모늄 폴리카르복실산 계열, 구연산 또는 암모늄 사이트레이트 계열, 또는 다른 고분자 전해질, 사이트레이트 계열을 포함할 수 있다. -As a dispersant or viscosity stabilizer, citric acid or ammonium polycarboxylic acid series, citric acid or ammonium citrate series, or other polymer electrolytes, citrate series may be included.
- 결합제와 겔화제로서, 천연 카라기난 계열과 폴리비닐알코올 계열을 포함할 수 있다. -As a binder and gelling agent, it may include natural carrageenan and polyvinyl alcohol.
이들 성분은 소결 제조 단계에서 모두 사라진다. 따라서 이들은 본 발명의 세라믹 비드의 성분에 기여하지 않는다. All of these components disappear during the sintering manufacturing step. Thus, they do not contribute to the composition of the ceramic beads of the present invention.
사용되는 ZrO2 분말 및 CeO2 분말은 1마이크로미터(um)에서 5um 범위의 크기를 갖는 것을 특징으로 한다.The ZrO 2 powder and CeO 2 powder used are characterized by having a size ranging from 1 micrometer (um) to 5 um.
S10 단계에서 제조된 현탁액을 Spray dryer로 통과시켜 과립 분체를 형성한다(S20). The suspension prepared in step S10 is passed through a spray dryer to form granular powder (S20).
얻어진 분체를 600~1000℃에서 열처리한다(S30). The obtained powder is heat-treated at 600 to 1000°C (S30).
열처리된 분체는 텀블링 공정을 이용하여 구상의 형상을 나타내는 성형체로 제조한다(S40).The heat-treated powder is manufactured into a molded body having a spherical shape using a tumbling process (S40).
구상으로 성형된 성형체를 1000~1300℃의 온도에서 소결한다(S50). 소결 지속 시간은 1시간 내지 5시간의 범위에 있다.The molded body molded into a spherical shape is sintered at a temperature of 1000 to 1300°C (S50). The sintering duration is in the range of 1 hour to 5 hours.
제조된 세라믹 비드는 0.1 밀리미터(mm)에서 5mm의 범위에 있는 직경을 가지고 있다.The prepared ceramic beads have a diameter in the range of 0.1 millimeter (mm) to 5 mm.
실시예Example
다음의 비한정적 실시예가 본 발명을 예시할 목적으로 주어진다.The following non-limiting examples are given for the purpose of illustrating the invention.
소결 세라믹 비드는 지르코니아 소스(1~5um)로부터, CeO2 소스(1~5um)로부터, 및 알루미나 소스(< 3um)로부터 제조하였다. 지르코니아 소스와 CeO2 소스의 순도는 99%를 이상이다. Sintered ceramic beads are from zirconia source (1-5um), CeO 2 It was prepared from a source (1-5 um) and from an alumina source (<3 um). Zirconia Sauce and CeO 2 The purity of the sauce is more than 99%.
상기 분말과 첨가제를 정제수와 함께 고형분 65 중량%으로 습식 분쇄하여 미세 결정립 크기는 D50 0.07um, 1um 이상 0%을 나타내도록 한다. 이 혼합 현탁액을 Spray dryer를 이용하여 건조된 과립 분체를 획득한다. The powder and additives are wet-milled with purified water to a solid content of 65% by weight, so that the fine grain size is D50 0.07um, 1um or more and 0%. The dried granular powder is obtained from this mixed suspension using a spray dryer.
다음 상기 과립 분체를 얻기 위해 0.35mm의 직경을 갖는 이트리아 안정화 비드를 이용하여 15m/s의 선속도로 회전하는 고속 에너지밀 기기에서 1시간동안 분쇄 및 분산한다. Next, in order to obtain the granular powder, yttria stabilized beads having a diameter of 0.35 mm are pulverized and dispersed for 1 hour in a high-speed energy mill that rotates at a linear speed of 15 m/s.
이때 슬러리의 온도는 60℃를 유지한다. At this time, the temperature of the slurry is maintained at 60°C.
안정한 현탁액의 제조를 위해 건조 성분 중량 대비 5 중량%의 암모늄 폴리카르복실산형 분산제 ; 2 중량%의 구연산 암모늄계열의 포함하였다. 5% by weight of an ammonium polycarboxylic acid-type dispersant based on the weight of the dry ingredient for preparing a stable suspension; It contained 2% by weight of ammonium citrate.
안정한 현탁액에 겔화제를 함유하는 용액을 제조하였다. 겔화제로, 2 중량%의 카라기난 및 1 중량%의 폴리비닐알코올계열이 첨가되었다. A solution containing a gelling agent was prepared in a stable suspension. As a gelling agent, 2% by weight of carrageenan and 1% by weight of polyvinyl alcohol series were added.
상기 획득된 과립 분체는 600℃온도의 터널킬른에서 3시간동안 열처리하였다. The obtained granular powder was heat-treated for 3 hours in a tunnel kiln at a temperature of 600°C.
열처리된 과립분체는 텀블링기계에서 3mm 크기의 구형 형태의 성형체를 제조하였다. The heat-treated granular powder was prepared in a spherical shape of 3 mm in size by a tumbling machine.
구형 형태의 성형체는 1250℃온도의 터널킬른에서 3시간동안 소결되며, 첨가제의 조성에 따라 세라믹 비드의 밀도와 경도 그리고 내마모성이 달라진다. The spherical molded body is sintered in a tunnel kiln at a temperature of 1250℃ for 3 hours, and the density, hardness and wear resistance of the ceramic beads vary depending on the composition of the additive.
세라믹 비드의 밀도측정은 아르키케데스 원리를 이용하여 겉보기 밀도계를 사용하였다. The density measurement of ceramic beads was performed using an apparent density meter using the Archikedes principle.
세라믹 비드의 경도 측정은 마이크로비커스법을 이용하여 1kgf의 하중으로 측정하였다. The hardness of the ceramic beads was measured with a load of 1 kgf using the Micro Vickers method.
세라믹 비드의 마모율 측정은 500ml 횡성밀을 이용하여 정제수에 세라믹 비드 600 그램(g)을 회전속도 5미터(m/s)로 2시간 동안 가동하여 비드의 중량 손실로 마모율을 평가하였다. To measure the wear rate of ceramic beads, 600 grams (g) of ceramic beads in purified water were operated for 2 hours at a rotation speed of 5 meters (m/s) using a 500 ml horizontal mill, and the wear rate was evaluated by weight loss of the beads.
표 1은 상기 실시예에 따라 제조된 세라믹 비드의 조성에 따른 밀도, 경도, 마모율의 결과를 나타낸 표이다. Table 1 is a table showing the results of density, hardness, and wear rate according to the composition of ceramic beads prepared according to the above example.
표 1의 조성은 지르코니아 소스에 CeO2 소스를 22 중량%에서 30 중량% 범위이며, 첨가제의 총함량은 0.5 중량%에서 2.5 중량%를 첨가하였다. The composition of Table 1 is CeO 2 in zirconia source The sauce ranges from 22% to 30% by weight, and the total amount of additives is from 0.5% to 2.5% by weight added.
CeO2 첨가량이 증가할수록 높은 밀도의 CeO2로 인해 밀도가 증가하였다. 또한 Fe2O3와 MnO2 첨가 시 더 높은 밀도를 나타내었다.As the CeO 2 amount is increased, the density increase was due to the CeO 2 of high density. In addition, when Fe 2 O 3 and MnO 2 were added, the density was higher.
CeO2 첨가량에 따라 경도의 변화가 발생되었으며, 마모율 또한 변화가 동시에 발생되었다.The hardness was changed according to the amount of CeO 2 added, and the wear rate also changed at the same time.
최고의 경도와 내마모성을 나타내는 조성은 CeO2 첨가량이 27 중량%이었으며, CeO2가 27~28 중량% 범위에서 가장 안정한 경도, 마모율을 나타내었다.The composition showing the highest hardness and abrasion resistance was the addition amount of CeO 2 at 27% by weight, and CeO 2 showed the most stable hardness and wear rate in the range of 27 to 28% by weight.
CeO2 첨가량이 22 ~ 30 중량%에서는 지르코니아 결정상은 안정적인 정방정상과 입방정상이 공존하였다.When CeO 2 was added in an amount of 22 to 30% by weight, the zirconia crystal phase coexisted with a stable tetragonal crystal and cubic crystal.
CeO2 첨가량이 증가할수록 낮은 온도에서 제조될 수 있어 우수한 내마모성을 나타내었다.As the amount of CeO 2 increased, it could be prepared at a lower temperature, thus exhibiting excellent wear resistance.
한편, 도 2는 CeO2 첨가량에 따른 지르코니아 세라믹 비드를 나타낸 사진으로 CeO2 첨가량이 27 중량%일때 에 도시된 바와 같이, 단사정(Monoclinic) 형태의 지르코니아를 가지지 않고 정방정(Tetragonal)과 입방정(Cubic) 형태를 가지는 것을 알 수 있다.On the other hand, Fig. 2, not having the monoclinic (Monoclinic) forms of zirconia tetragonal (Tetragonal) and cubic crystal as shown in the CeO 2 amount is 27% by weight when a photograph showing the zirconia ceramic beads in accordance with the CeO 2 amount ( Cubic) shape.
Claims (17)
상기 S10 단계에서 제조된 상기 현탁액을 과립 분체로 형성하는 단계(S20);
상기 S20 단계에서 얻어진 상기 과립 분체를 600~1000℃에서 열처리하는 단계;
상기 S30 단계에서 열처리된 상기 과립 분체를 구상의 형상을 나타내는 성형체로 제조하는 단계(S40); 및
상기 S40 단계에서 제조된 상기 성형체를 소결하는 단계(S50)를 포함하는 세라믹 비드 제조 방법.ZrO 2 + HfO 2 , CeO 2 , Al 2 O 3 and Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 Preparing an aqueous suspension comprising a powder of one or more oxides selected from O 3 , ZnO, BaO, SrO, and CaO (S10);
Forming the suspension prepared in step S10 into granular powder (S20);
Heat-treating the granular powder obtained in step S20 at 600 to 1000°C;
Manufacturing the granular powder heat-treated in step S30 into a molded body having a spherical shape (S40); And
Ceramic bead manufacturing method comprising the step (S50) of sintering the formed body manufactured in the step S40.
상기 S10의 현탁액은 건조 성분 함량이 50 중량% 내지 70 중량%의 범위인 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
The suspension of S10 is a method for producing ceramic beads, characterized in that the dry component content is in the range of 50% to 70% by weight.
상기 S30 단계에서 텀블링 공정을 이용하여 성형체를 구상의 형상으로 제조하는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
Ceramic bead manufacturing method, characterized in that the formed body is manufactured in a spherical shape by using a tumbling process in step S30.
상기 S10 단계의 상기 현탁액은,
건조 성분 중량에 대비 0 내지 5% 중량 농도의 분산제;
건조 성분 중량에 대비 0 내지 10% 중량 농도의 결합제;
건조 성분 중량에 대비 0 내지 3% 중량 농도의 점도 안정제; 또는
건조 성분 중량에 대비 0 내지 3% 중량 농도의 겔화제(gelling agent)를 포함하는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
The suspension of step S10,
A dispersant having a concentration of 0 to 5% by weight based on the weight of the dry ingredients;
0 to 10% by weight of the binder based on the weight of the dry ingredients;
A viscosity stabilizer having a concentration of 0 to 3% by weight based on the weight of the dry ingredients; or
Ceramic bead production method comprising a gelling agent (gelling agent) of 0 to 3% by weight based on the weight of the dry ingredients.
상기 분산제 또는 상기 점도 안정제는,
구연산 또는 암모늄 폴리카르복실산 계열, 구연산 또는 암모늄 사이트레이트 계열, 또는 고분자 전해질, 사이트레이트 계열을 포함하는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 4,
The dispersant or the viscosity stabilizer,
A method for producing ceramic beads comprising citric acid or ammonium polycarboxylic acid series, citric acid or ammonium citrate series, or a polymer electrolyte and citrate series.
상기 결합제 또는 상기 겔화제는,
천연 카라기난 계열 또는 폴리비닐알코올 계열을 포함하는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 4,
The binder or the gelling agent,
Ceramic beads manufacturing method comprising a natural carrageenan series or polyvinyl alcohol series.
상기 S10 단계에서 ZrO2와 CeO2는 입자 크기가 1㎛ 내지 5㎛ 범위인 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
In the step S10, ZrO 2 and CeO 2 have a particle size in the range of 1 μm to 5 μm.
상기 S40 단계에서,
열처리된 상기 과립 분체는 텀블링 공정을 이용하여 구상의 형상을 나타내는 성형체로 제조되는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
In step S40,
The heat-treated granular powder is a ceramic bead manufacturing method, characterized in that it is manufactured into a molded body having a spherical shape using a tumbling process.
상기 S50 단계에서,
성형된 상기 성형체를 1000~1300℃의 온도에서 1시간 내지 5시간 동안 소결하는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
In the step S50,
Ceramic bead manufacturing method, characterized in that the molded body is sintered for 1 hour to 5 hours at a temperature of 1000 ~ 1300 ℃.
상기 S10 단계 내지 S50 단계를 순차적으로 수행하여 제조된 세라믹 비드는 0.1mm 내지 5mm의 직경을 가지는 것을 특징으로 하는 세라믹 비드 제조 방법.The method of claim 1,
The ceramic bead manufacturing method, characterized in that the ceramic bead manufactured by sequentially performing the steps S10 to S50 has a diameter of 0.1mm to 5mm.
상기 첨가제는 Fe2O3, MnO2, ZrSiO4, SiO2, Y2O3, La2O3, MgO, NnO2, CuO, TiO2, Sb2O3, ZnO, BaO, SrO, CaO 및 이들의 혼합물 중 선택된 어느 하나 이상인 것을 특징으로 하는 세라믹 비드.The method of claim 11,
The additives are Fe 2 O 3 , MnO 2 , ZrSiO 4 , SiO 2 , Y 2 O 3 , La 2 O 3 , MgO, NnO 2 , CuO, TiO 2 , Sb 2 O 3 , ZnO, BaO, SrO, CaO and Ceramic beads, characterized in that at least any one selected from these mixtures.
Al2O3 함량이 0.1 이상 2.0 중량% 미만인 것을 특징으로 하는 세라믹 비드.The method of claim 11,
Ceramic beads, characterized in that the Al 2 O 3 content is 0.1 or more and less than 2.0% by weight.
상기 첨가제 함량은 0.1 이상 2.0 중량% 미만인 것을 특징으로 하는 세라믹 비드.The method of claim 11,
Ceramic beads, characterized in that the additive content is 0.1 or more and less than 2.0% by weight.
상기 Al2O3 와 상기 첨가제 함량은 1.0 ~ 2.5 중량% 인 것을 특징으로 하는 세라믹 비드.The method of claim 11,
Ceramic beads, characterized in that the content of the Al 2 O 3 and the additive is 1.0 to 2.5% by weight.
상기 첨가제는 Fe2O3 또는 MnO2 인 것을 특징으로 하는 세라믹 비드.The method of claim 15,
Ceramic beads, characterized in that the additive is Fe 2 O 3 or MnO 2 .
상기 CeO2의 함량은 22 ~ 30 중량% 인 것을 특징으로 하는 세라믹 비드.
The method of claim 11,
Ceramic beads, characterized in that the content of the CeO 2 is 22 to 30% by weight.
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| KR19980032186A (en) | 1996-10-01 | 1998-07-25 | 니이하라고이치 | Zirconia-based ceramic materials and preparation method thereof |
| KR20060003984A (en) | 2004-07-06 | 2006-01-12 | 케이지케미칼 주식회사 | Production method of ceramic bead |
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| KR19980032186A (en) | 1996-10-01 | 1998-07-25 | 니이하라고이치 | Zirconia-based ceramic materials and preparation method thereof |
| KR20060003984A (en) | 2004-07-06 | 2006-01-12 | 케이지케미칼 주식회사 | Production method of ceramic bead |
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