CN110862261A - 一种黄色氧化锆陶瓷用粉体及其制备方法和应用 - Google Patents
一种黄色氧化锆陶瓷用粉体及其制备方法和应用 Download PDFInfo
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 197
- 239000000919 ceramic Substances 0.000 title claims abstract description 89
- 239000000843 powder Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 34
- 238000000498 ball milling Methods 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002002 slurry Substances 0.000 claims abstract description 20
- 239000002270 dispersing agent Substances 0.000 claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 16
- 229910002637 Pr6O11 Inorganic materials 0.000 claims abstract description 15
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 14
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 14
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims description 20
- 229920000142 Sodium polycarboxylate Polymers 0.000 claims description 6
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 description 6
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- 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 2
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- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
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- 230000032683 aging Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
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- 238000001354 calcination Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- 230000005389 magnetism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- MMKQUGHLEMYQSG-UHFFFAOYSA-N oxygen(2-);praseodymium(3+) Chemical compound [O-2].[O-2].[O-2].[Pr+3].[Pr+3] MMKQUGHLEMYQSG-UHFFFAOYSA-N 0.000 description 1
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 description 1
- 229910003447 praseodymium oxide Inorganic materials 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910002076 stabilized zirconia Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 1
- 229910052845 zircon Inorganic materials 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种黄色氧化锆陶瓷用粉体的制备方法,特征是:包括S1:取如下质量份物料:0.28~0.32份MgO、0.19~0.25份Al2O3、0.33~0.37份SiO2、2.9~3.2份Y2O3、0.48~0.52份Pr6O11、95~96份ZrO2,搅拌形成混合料;S2:取如下质量份物料:10~14份研磨介质、1.2~1.5份去离子水及0.8~1.2份S1中混合料,放入球磨罐,加氨水调节pH至9~12,加入0.01~0.02份分散剂,将浆料球磨至D50≤0.4μm;S3:将S2中浆料在80~150℃下烘干,再研磨到D50≤0.2mm,得到产物粉体。其工艺极其简单、原料成本低。还提供一种通过上述制备方法制得的黄色氧化锆陶瓷用粉体,此粉体为紫灰色,烧结后形成黄色氧化锆陶瓷,不用染色;一种黄色氧化锆陶瓷,其力学性能优越,抗弯强度高、硬度高,断裂韧性好;一种黄色氧化锆陶瓷的制备方法,工艺简单、可操作性强。
Description
技术领域
本发明涉及氧化锆粉体制备技术领域,尤其涉及一种具有高强度高韧性的黄色氧化锆陶瓷用粉体及其制备方法和应用。
背景技术
目前,随着材料科学技术的不断发展进步,以氧化锆为原料的特种陶瓷以其具有的耐高温、耐腐蚀、耐磨等特性,在特定条件下又能显示电、磁、光、声等特殊功能。广泛应用于电子陶瓷、结构陶瓷、生物陶瓷、高级耐火材料等行业的产品,几乎遍及到了国民经济的各个领域。其中,陶瓷结构件的应用是特种陶瓷在我们生产生活中的一个重要方面。
在结构陶瓷方面,由于氧化锆陶瓷具有高韧性、高抗弯强度和高耐磨性,优异的隔热性能,热膨胀系数接近于钢等优点,因此被广泛应用于结构陶瓷领域。主要有:Y-TZP磨球、分散和研磨介质、喷嘴、球阀球座、氧化锆模具、微型风扇轴心、光纤插针、光纤套筒、拉丝模和切割工具、耐磨刀具、表壳及表带、高尔夫球的轻型击球棒及其它室温耐磨零器件等。
而结构件就要求材料有高的抗弯强度和韧性,并且对材料的加工性能要求很高,传统的3Y-TZP就是最简单的合成工艺(共沉淀法),其要想作出符合结构件用的氧化锆陶瓷粉体,对原料的纯度等要求很高,而且加工过程复杂(先原料溶解,共沉淀,再压滤,再煅烧,再球磨,再造粒),如果客户要求其他颜色如黄色,则还需要在结构件外表面涂黄色釉料,而且如果需要切割加工,则还需进一步重新上色处理等,工艺复杂、操作麻烦。
公开号为CN101143787A的中国专利公开了一种“高性能黄色氧化锆陶瓷超细粉的制备方法”,是将锆英砂或氧氯化锆溶液、氧化钇溶液、氧化镨溶液、氧化铝溶液混合配成氧化锆粉原料溶液,在其中滴加碳酸氢铵溶液,同时不断搅拌,反应生成的共沉淀化合物经过滤、干燥、煅烧得到氧化锆超细粉,由该粉体可以制备高性能黄色氧化锆陶瓷制品。此发明虽然通过在氧化锆陶瓷原料中加入镨、铝元素,降低了烧结温度,保证了烧结后陶瓷呈现黄色,但是其制备工艺较为复杂,原料成本高,不适宜大量生产,效益低。
发明内容
本发明的目的在于针对现有技术的不足,提供一种黄色氧化锆陶瓷用粉体的制备方法,其工艺极其简单、原料成本低。
还提供一种通过上述制备方法制得的黄色氧化锆陶瓷用粉体,此粉体为紫灰色,烧结后形成黄色氧化锆陶瓷,不用染色。
还提供一种黄色氧化锆陶瓷,其力学性能优越,抗弯强度高、硬度高,断裂韧性好。
再提供一种黄色氧化锆陶瓷的制备方法,工艺简单、可操作性强。
为实现上述目的,本发明首先提供如下技术方案:一种黄色氧化锆陶瓷用粉体的制备方法,包括如下具体制备步骤:
步骤S1:称取包括如下质量份的物料:0.28~0.32质量份MgO、0.19~0.25质量份Al2O3、0.33~0.37质量份SiO2、2.9~3.2质量份Y2O3、0.48~0.52质量份Pr6O11、95~96质量份ZrO2,搅拌形成混合料;
步骤S2:称取包括如下质量份的物料:10~14质量份研磨介质、1.2~1.5质量份去离子水以及0.8~1.2质量份的步骤1中所述的混合料,放入到球磨罐中,加入适量氨水调节pH值至9~12,再加入0.01~0.02质量份分散剂,然后将球磨罐内浆料球磨至D50≤0.4μm;
步骤S3:将步骤S2中球磨后的浆料在80~150℃的条件下烘干,再干法研磨到D50≤0.2mm,得到产物粉体,即为黄色氧化锆陶瓷用粉体。
优选地,步骤S1:称取包括如下质量份的物料:0.3质量份MgO、0.22质量份Al2O3、0.35质量份SiO2、0.31质量份Y2O3、0.5质量份Pr6O11、95.5质量份ZrO2,搅拌形成混合料。
优选地,步骤S1中所述的Al2O3为γ晶型的氧化铝,所述的ZrO2为单斜氧化锆。
优选地,步骤S2中所述的分散剂为聚羧酸钠盐型分散剂。
优选地,步骤S1中所述的MgO、Al2O3、SiO2、Y2O3、Pr6O11以及ZrO2原料均为干燥粉末,其称取的质量误差在±5%以内。
优选地,步骤S2中所述的研磨介质为氧化锆研磨珠,所述的研磨罐为氧化锆材质。
优选地,步骤S2中所述的氨水的纯度为工业级以上。
优选地,步骤S1中所述的原料的纯度在工业级以上。
本发明还提供一种黄色氧化锆陶瓷用粉体,所述的粉体是通过上述的粉体制备方法制备的。
本发明还提供一种黄色氧化锆陶瓷用粉体的应用,具体涉及通过上述粉体制备得到一种黄色氧化锆陶瓷,所述的黄色氧化锆陶瓷的抗弯强度平均在1010MPa左右,硬度计断裂韧性在11MPa·m1/2左右,维氏硬度为1148~1150kgf/mm2。
本发明还提供一种制备上述黄色氧化锆陶瓷的方法,包括以下制备步骤:
步骤A:粉体烧结,称取定量的的步骤S3中制得的产物粉体,将称得的粉体在4~6MPa压强下压制成片,在1400~1420℃下保温2~3h,得到黄色固体,即为氧化锆陶瓷。
优选地,对步骤A中制得的氧化锆陶瓷进行抗弯强度、断裂韧性及硬度测试,测得氧化锆陶瓷的抗弯强度平均在1010MPa左右,硬度计断裂韧性在11MPa·m1/2左右,维氏硬度为1148~1150kgf/mm2。
优选地,步骤A中硬度的测试采用维氏硬度方法测算,抗弯强度测试采用双轴抗弯强度测试标准,所述双轴抗弯强度的测试采用GB30367-2013/ISO6872:2008标准,断裂韧性的测试采用压痕法。
本发明的有益效果至少包括:
(1)本发明的配方,只需要买廉价的单斜氧化锆和对应的氧化物组份,按照特定比例球磨,就可以做出适合结构件使用的粉体,而且粉体烧结后力学性能优异,烧结后的陶瓷体内外无色差,均为黄色,方便加工处理。是可以作为结构件用的廉价且性能优异的陶瓷粉体。
(2)本发明的工艺过程简单,所需原料不需要合成,成本低廉;用本发明方法制备的粉体烧结出的陶瓷体为黄色,陶瓷体内外颜色一致,解决了部分氧化铈稳定氧化锆由于烧结气氛的影响导致陶瓷体内外颜色不一致;此外本发明的粉体烧结出的黄色陶瓷,其双轴抗弯强度能达到1000MPa以上,断裂韧性能达到10.96MPa·m1/2,已经优于目前大部分的氧化钇稳定氧化锆粉体的烧结力学性能。在结构件和需要美观效果的地方前景可观。
附图说明
图1A实施例1制备的粉体XRD图。
图1B实施例1制备的陶瓷体XRD图。
图2A实施例2制备的粉体XRD图。
图2B实施例2制备的陶瓷体XRD图。
图3A实施例3制备的粉体XRD图。
图3B实施例3制备的陶瓷体XRD图。
具体实施方式
下面结合附图及实施方式对本发明做进一步说明。
一种黄色氧化锆陶瓷用粉体的制备方法,包括如下具体制备步骤:
步骤S1:原料选取,称取包括如下质量份的物料:0.28~0.32份MgO,0.19~0.25份Al2O3,0.33~0.37份SiO2,2.9~3.2份Y2O3,0.48~0.52份Pr6O11,95~96份ZrO2;将称取好的原料放入容器中均匀搅拌,形成混合料;
步骤S2:研磨,称取包括如下质量份的物料:10~14份研磨介质、1.2~1.5份去离子水以及0.8~1.2份步骤1中所述的混合料,将称取的物料放入到球磨罐中,加入适量氨水调节pH值至9~12,再加入0.01~0.02质量份的分散剂,然后将球磨罐内浆料球磨至浆料D50≤0.4μm;
步骤S3:烘干再研磨,将步骤S2中球磨后的浆料在80~150℃的条件下干燥处理,烘干后的块体再干法研磨到D50≤0.2mm,得到的产物粉体即为黄色氧化锆陶瓷用粉体。
进一步地,步骤S1:称取包括如下质量份的物料:0.3质量份MgO、0.22质量份Al2O3、0.35质量份SiO2、0.31质量份Y2O3、0.5质量份Pr6O11、95.5质量份ZrO2,搅拌形成混合料。
进一步地,步骤S1中所述的Al2O3为γ晶型的氧化铝,所述的ZrO2为单斜氧化锆。
进一步地,步骤S2中所述的分散剂为聚羧酸钠盐型分散剂。
进一步地,步骤S1中所述的MgO、Al2O3、SiO2、Y2O3、Pr6O11以及ZrO2原料均为干燥粉末,由于各种氧化物原料都在配方中起到关键性作用,所以对原料的称量要求特别准确,称取质量误差在±5%以内。
进一步地,步骤S2中所述的研磨介质为氧化锆研磨珠,所述的研磨罐为氧化锆材质。
进一步地,步骤S2中所述的氨水的纯度为工业级以上。
进一步地,步骤S1中所述的原料的纯度在工业级以上。
本发明还提供一种黄色氧化锆陶瓷用粉体,所述的粉体是通过上述氧化锆陶瓷用粉体的制备方法制备的。
本发明还提供一种黄色氧化锆陶瓷用粉体的应用,具体涉及通过上述粉体制备得到一种黄色氧化锆陶瓷,所述氧化锆陶瓷的抗弯强度平均在1010MPa左右,硬度计断裂韧性在11MPa·m1/2左右,维氏硬度为1148~1150kgf/mm2。
本发明还提供一种制备黄色氧化锆陶瓷的方法,包括以下制备步骤:
步骤A:粉体烧结,称取定量的的步骤S3中制得的氧化锆陶瓷用粉体,将称得的粉体在4~6MPa压强下压制成直径为18~23mm的圆形薄片,在1400~1420℃下保温2~3h,得到黄色固体即为氧化锆陶瓷。
进一步地,对步骤A中制得的氧化锆陶瓷进行抗弯强度、断裂韧性及硬度测试,测得氧化锆陶瓷的抗弯强度平均在1010MPa左右,硬度计断裂韧性在11MPa·m1/2左右,维氏硬度为1148~1150kgf/mm2。
进一步地,步骤A中硬度的测试采用维氏硬度方法测算,抗弯强度测试采用双轴抗弯强度测试标准,所述双轴抗弯强度的测试采用GB30367-2013/ISO6872:2008标准,断裂韧性的测试采用压痕法。
实施例1
一种黄色氧化锆陶瓷用粉体的制备方法,包括如下制备步骤:
步骤S1:原料选取,分别称取工业级以上纯度的MgO:0.3g,Al2O3:0.25g,SiO2:0.35g,Y2O3:3.1g,Pr6O11:0.51g,ZrO2:95.5g,其中Al2O3为γ晶体,ZrO2为纯单斜氧化锆,将上述称取好的原料倒入氧化锆材质的球磨罐中均匀搅拌,形成混合料;
步骤S2:球磨,向球磨罐中分别加入1200g氧化锆研磨珠和150g去离子水,再加入适量工业级纯度以上的氨水调节pH值到11(误差允许范围内),再加入1.5g的聚羧酸钠盐型分散剂,在本实施例中具体可以为日本圣诺普科SN-DISPERSANT 5040型号的分散剂,然后将球磨罐内的浆料球磨至浆料D50为0.36μm;
步骤S3:烘干再研磨,将步骤S2中球磨后的浆料在100℃的条件下干燥处理,烘干后的块体进行干法研磨,同时用孔径为0.2mm的筛网过筛,得到的产物粉体即为黄色氧化锆陶瓷用粉体,其通常呈紫灰色。
还提供一种利用上述的黄色氧化锆陶瓷用粉体制备黄色氧化锆陶瓷的方法,包括以下制备步骤:
步骤A:粉体烧结,称取1.1g的上述步骤S3中制得的黄色氧化锆陶瓷用粉体,将称得的粉体在4MPa压强下压制4个直径为20mm的圆形薄片,然后将薄片放置到电热炉中以1.5℃/min的升温速度升温至1400℃,保温2h后自然降温,得到的黄色固体薄片,即为氧化锆陶瓷。将薄片取出后按照GB30367-2013/ISO6872:2008标准测其双轴抗弯强度、按照阿基米德原理测密度、测其维氏硬度,并根据压痕法公式计算断裂韧性,数据如表1所示。其抗弯强度平均值达到1079MPa,断裂韧性达到10.96MPa·m1/2,密度达到6.05g/cm3。
实施例2
一种黄色氧化锆陶瓷用粉体的制备方法,包括如下制备步骤:
步骤S1:原料选取,分别称取工业级以上纯度的MgO:0.23g,Al2O3:0.16g,SiO2:0.27g,Y2O3:2.4g,Pr6O11:0.4g,ZrO2:78.54g,其中Al2O3为γ晶体,ZrO2为纯单斜氧化锆,将上述称取好的原料倒入氧化锆材质的球磨罐中均匀搅拌,形成混合料;
步骤S2:球磨,向球磨罐中分别加入1000g氧化锆研磨珠和120g去离子水,再加入适量工业级纯度以上的氨水调节pH值到9(误差允许范围内),再加入1g的聚羧酸钠盐型分散剂,在本实施例中具体可以为南通市晗泰化工有限公司生产的HT-5050型号的高效分散剂,然后将球磨罐内的浆料球磨至浆料D50为0.3μm;
步骤S3:烘干再研磨,将步骤S2中球磨后的浆料在80℃的条件下干燥处理,烘干后的块体进行干法研磨,同时用孔径为0.2mm的筛网过筛,得到的紫灰色粉体即为黄色氧化锆陶瓷用粉体。
还提供一种利用上述的黄色氧化锆陶瓷用粉体制备黄色氧化锆陶瓷的方法,包括以下制备步骤:
步骤A:粉体烧结,称取1.5g的上述步骤S3中制得的黄色氧化锆陶瓷用粉体,将称得的粉体在5MPa压强下压制4个直径为18mm的圆形薄片,然后将薄片放置到电热炉中以1.5℃/min的升温速度升温至1410℃,保温2.5h后自然降温,得到的黄色固体薄片,即为氧化锆陶瓷。将薄片取出后按照GB30367-2013/ISO6872:2008标准测其双轴抗弯强度、按照阿基米德原理测密度,测其维氏硬度,并根据压痕法公式计算断裂韧性,数据如表1所示。其抗弯强度平均值达到957MPa,断裂韧性达到9.65MPa·m1/2,密度达到6.06g/cm3。
表1-黄色陶瓷片力学性能测试数据:
实施例3
一种黄色氧化锆陶瓷用粉体的制备方法,包括如下制备步骤:
步骤S1:原料选取,分别称取工业级以上纯度的MgO:0.38g,Al2O3:0.29g,SiO2:0.44g,Y2O3:3.81g,Pr6O11:0.62g,ZrO2:114.4g,其中Al2O3为γ晶体,ZrO2为纯单斜氧化锆,将上述称取好的原料倒入氧化锆材质的球磨罐中均匀搅拌,形成混合料;
步骤S2:球磨,向球磨罐中分别加入1400g氧化锆研磨珠和150g去离子水,再加入适量工业级纯度以上的氨水调节pH值到12(误差允许范围内),再加入2g的聚羧酸钠盐型分散剂,在本实施例中具体可以为日本圣诺普科SN-DISPERSANT 5040型号的分散剂,然后将球磨罐内的浆料球磨至浆料D50为0.3μm;
步骤S3:烘干再研磨,将步骤S2中球磨后的浆料在150℃的条件下干燥处理,烘干后的块体进行干法研磨,同时用孔径为0.15mm的筛网过筛,得到的紫灰色产物粉体即为黄色氧化锆陶瓷用粉体。
还提供一种利用上述的黄色氧化锆陶瓷用粉体制备黄色氧化锆陶瓷的方法,包括以下制备步骤:
步骤A:粉体烧结,称取1.5g的上述步骤S3中制得的黄色氧化锆陶瓷用粉体,将称得的粉体在6MPa压强下压制4个直径为23mm的圆形薄片,然后将薄片放置到电热炉中以1.5℃/min的升温速度升温至1420℃,保温2h后自然降温,得到的黄色固体薄片,即为氧化锆陶瓷。将薄片取出后按照GB30367-2013/ISO6872:2008标准测其双轴抗弯强度、按照阿基米德原理测密度,测其维氏硬度,并根据压痕法公式计算断裂韧性,数据如表1所示。其抗弯强度平均值达到996MPa,断裂韧性达到10.19MPa·m1/2,密度达到6.06g/cm3。
在本发明中,由于制备粉体用的单斜氧化锆占主要成分,其粉体的XRD图(图1A、图2A、图3A)只能看到氧化锆的单斜峰。其中MgO、SiO2、Y2O3和Pr6O11均能起到稳定氧化锆到亚稳四方相的作用;其最终的陶瓷烧结体的XRD图(图1B、图2B、图3B)中四方相的含量达到95%,但是还是存在微量的单斜相,这跟具体的球磨工艺能否达到充分混合有关;
在本发明中,Al2O3能起到降低陶瓷烧结温度,同时也能提高耐老化性能,而MgO加入一定比例的量,能提高其耐热震性能;Pr6O11加入一定比例的量,能够使粉体制备出的陶瓷体变为金黄色,而且通过微调Pr6O11的添加量,能够使粉体或者陶瓷体呈现出不同深度的黄色表现。
总之,通过本发明中工艺方法的操作,可以得到高抗弯强度和高断裂韧性的黄色氧化锆陶瓷用粉体,在结构件陶瓷领域具有很好的应用。
以上实施方式仅用于说明本发明,而并非对本发明的限制,有关技术领域普通技术人员,在不脱离本发明精神和范围的情况下,还可以做出各种变化和变型,因此所有等同的技术方案也属本发明的范畴,本发明专利保护范围应由权利要求限定。
Claims (10)
1.一种黄色氧化锆陶瓷用粉体的制备方法,其特征在于,包括如下制备步骤:
步骤S1:称取包括如下质量份的物料:0.28~0.32质量份MgO、0.19~0.25质量份Al2O3、0.33~0.37质量份SiO2、2.9~3.2质量份Y2O3、0.48~0.52质量份Pr6O11、95~96质量份ZrO2,搅拌形成混合料;
步骤S2:称取包括如下质量份的物料:10~14质量份研磨介质、1.2~1.5质量份去离子水及0.8~1.2质量份的步骤1中所述的混合料,放入到球磨罐中,加入适量氨水调节pH值至9~12,再加入0.01~0.02质量份的分散剂,然后将球磨罐内浆料球磨至D50≤0.4μm;
步骤S3:将步骤S2中球磨后的浆料在80~150℃的条件下烘干,再干法研磨到D50≤0.2mm,得到产物粉体。
2.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S1:称取包括如下质量份的物料:0.3质量份MgO、0.22质量份Al2O3、0.35质量份SiO2、0.31质量份Y2O3、0.5质量份Pr6O11、95.5质量份ZrO2,搅拌形成混合料。
3.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S1中所述的Al2O3为γ晶型的氧化铝。
4.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S1中所述的ZrO2为单斜氧化锆。
5.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S2中所述的研磨介质为氧化锆研磨珠,所述的研磨罐为氧化锆材质。
6.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S2中所述的分散剂为聚羧酸钠盐型分散剂。
7.根据权利要求1所述的黄色氧化锆陶瓷用粉体的制备方法,其特征在于,步骤S1中所述的MgO、Al2O3、SiO2、Y2O3、Pr6O11以及ZrO2均为干燥粉末,其称取的质量误差在±5%以内。
8.一种黄色氧化锆陶瓷用粉体,其特征在于,所述的粉体是通过权利要求1至7中任一项所述的制备方法制备的。
9.一种黄色氧化锆陶瓷,其特征在于,所述的黄色氧化锆陶瓷是通过权利要求8所述的粉体制备的。
10.一种制备权利要求9所述的黄色氧化锆陶瓷的方法,其特征在于,包括以下制备步骤:
步骤A:粉体烧结,称取定量的步骤S3中制得的产物粉体,将称得的粉体在4~6MPa压强下压制成片,在1400~1420℃下烧结2~3h,得到黄色固体。
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