CN117142851A - 一种防辐射陶瓷及其制备方法 - Google Patents
一种防辐射陶瓷及其制备方法 Download PDFInfo
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- CN117142851A CN117142851A CN202311176826.9A CN202311176826A CN117142851A CN 117142851 A CN117142851 A CN 117142851A CN 202311176826 A CN202311176826 A CN 202311176826A CN 117142851 A CN117142851 A CN 117142851A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 230000003471 anti-radiation Effects 0.000 title description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- 230000005855 radiation Effects 0.000 claims abstract description 42
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 32
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 26
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 15
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002210 silicon-based material Substances 0.000 claims abstract description 15
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052796 boron Inorganic materials 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 11
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 8
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 238000001746 injection moulding Methods 0.000 claims abstract description 8
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000008595 infiltration Effects 0.000 claims abstract description 6
- 238000001764 infiltration Methods 0.000 claims abstract description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 10
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims description 7
- 229910052912 lithium silicate Inorganic materials 0.000 claims description 7
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 7
- 239000012279 sodium borohydride Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
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- 230000000630 rising effect Effects 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000004111 Potassium silicate Substances 0.000 claims description 2
- 239000004115 Sodium Silicate Substances 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 2
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 2
- 235000019794 sodium silicate Nutrition 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 6
- 238000003801 milling Methods 0.000 claims 2
- 230000010355 oscillation Effects 0.000 claims 1
- 230000003204 osmotic effect Effects 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 20
- 230000006378 damage Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 150000001639 boron compounds Chemical class 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract description 2
- 230000002411 adverse Effects 0.000 abstract 1
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- 239000003758 nuclear fuel Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000005260 corrosion Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- -1 Magnesium oxide Cerium oxide Lithium nitrate Sodium hydroxide Sodium Chemical compound 0.000 description 1
- 208000019155 Radiation injury Diseases 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
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- 150000002500 ions Chemical class 0.000 description 1
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- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
本发明涉及一种防辐射陶瓷及其制备方法,属于陶瓷的技术领域。本发明采用高稳定性、高密度的氧化锆、氧化镁和氧化铈,有效抗击辐射损伤;加入硼化合物和含硅化合物,增强陶瓷材料的防辐射能力;采用注塑成形,成型效率高,产品成型质量均匀性好;烧结前进行热处理和渗透处理,加上烧结温度较低,避免陶瓷材料的结构破坏和晶粒长大的负面影响。所述防辐射陶瓷包括以下原料:氧化锆、氧化镁、氧化铈、硝酸锂、氢氧化钠、含硼化合物、含硅化合物和钛酸钡。所述制备方法包括1)将原料混合研磨得到混合颗粒;2)加入氢氧化钠和去离子水混合,静置后烘干,得到预制物;3)加入甲醇超声震荡离心后进行干燥,得到陶瓷粉料;4)注塑成形后进行烧结。
Description
技术领域
本发明属于陶瓷的技术领域,涉及一种防辐射陶瓷及其制备方法。
背景技术
防辐射陶瓷是一种特种功能材料,可以对电子、离子等辐射粒子进行屏蔽,保护人体安全,主要应用在核工业和核燃料循环领域、医疗领域、航空航天、电子和光学领域。核工业和核燃料循环领域:在核工业和核燃料循环领域,防辐射陶瓷材料广泛应用于核反应堆中的衬垫、反应容器、管道和金属封闭体等部件中,要求这些陶瓷零部件具备很好的耐辐射性能,能够抵御核反应堆中的辐射环境,减少辐射对人类和环境的危害。医疗领域:在医疗领域,防辐射陶瓷材料也广泛应用于高能辐射治疗设备中,要求陶瓷材料具有良好的辐射防护性能,以保护医护人员和患者免受辐射伤害。其他领域:在某些工业领域,如航空航天、电子和光学等领域,以避免辐射对精密仪器、设备和元器件等的影响。
因此,为了满足不同领域中的不同需求,陶瓷需要具备不同的防辐射性能。常见的防辐射性能包括高温耐辐射性、抗辐射能力、辐射吸收能力,此外陶瓷还需具备良好的力学性质。
市面的防辐射陶瓷热存在以下缺陷:
(1)稳定性差:一些防辐射陶瓷材料在遇到高温场合时,容易出现裂纹、脱落、变形等失效现象,降低了材料的耐承载能力和使用寿命;(2)导热性能差:由于防辐射陶瓷材料多为非晶态或微晶态陶瓷,晶粒大小较小,而且热导率较低,因此热传导能力较差,不利于高温场合的应用;(3)防护性能有限:对于高能量的辐射,现有的防辐射陶瓷材料防护能力有限,需要进一步改进和提升。
发明内容
本发明的目的在于提供一种防辐射陶瓷及其制备方法,采用高稳定性、高密度的氧化锆、氧化镁和氧化铈材料,能够有效抗击辐射损伤;加入硼化合物和含硅化合物,可以增强陶瓷材料的防辐射能力;采用注塑成形,成型效率高,产品成型质量均匀性好;采用回收热量,能够有效地降低工艺能耗;烧结前进行热处理和渗透处理,加上烧结温度较低,能够避免陶瓷材料的结构破坏和晶粒长大的负面影响。
本发明的目的可以通过以下技术方案实现:
一种防辐射陶瓷,所述防辐射陶瓷按重量份数包括以下原料:氧化锆50-75份、氧化镁10-25份、氧化铈10-25份、硝酸锂0.15-0.5份、氢氧化钠2-4份、含硼化合物1-5份、含硅化合物5-15份以及钛酸钡1-5份。
作为本发明的一种优选技术方案,所述含硼化合物为硼酸和硼氢化钠中的一种或两种;所述含硅化合物为硅酸锂、硅酸钾、硅酸钠和二氧化硅中的一种或多种。
本发明方案公开了一种防辐射陶瓷的制备方法,包括以下步骤:
1)将氧化锆、氧化镁、氧化铈、含硼化合物、含硅化合物混合均匀,筛选后放入球磨罐中研磨,并在其中加入硝酸锂,混合均匀,得到混合颗粒;
2)向混合颗粒加入氢氧化钠和去离子水,搅拌混合均匀,在室温下静置后,置于烘箱中烘干,得到预制物;
3)将预制物加入甲醇中,超声震荡进行离心,取固体置于烘箱中干燥后,得到陶瓷粉料;
4)将陶瓷粉料注入注塑机中,压制成形体,将形体置于烧结炉中进行烧结。
作为本发明的一种优选技术方案,在步骤1)中,所述研磨条件为以100rpm的转速研磨4-5h。
作为本发明的一种优选技术方案,在步骤2)中,所述静置时间为12-15h,所述烘箱烘干条件为在50-60℃下烘干2-3h,所述去离子水的加入量为刚好淹没混合颗粒和氢氧化钠。
作为本发明的一种优选技术方案,在步骤3)中,所述超声震荡时间为2-3h,所述离心时间为10-20min,所述干燥条件为在105-115℃下干燥2-3h。
作为本发明的一种优选技术方案,在步骤4)中,所述烧结炉烧结条件为升温速度5℃/min,升温至1350℃烧结4-5h。
作为本发明的一种优选技术方案,在步骤4)的压制成形体后,还依次包括步骤41)渗透处理和步骤42)热处理。
作为本发明的一种优选技术方案,所述步骤42)热处理为将渗透处理后的所述形体置于热处理炉中,在300-320℃加热2-3h后,在热处理炉中进行冷却,热处理炉散出的热量通过换热器收集后,得到回收热量。
作为本发明的一种优选技术方案,所述步骤41)渗透处理为将所述形体置于浓度为0.1-0.2mol/L的硝酸中,通过所述回收热量加热至150℃,维持温度1-2h后,降温至90-110℃,加入EDTA,反应1-2h,然后将其取出,用水冲洗干净;其中,所述硝酸与所述形体的质量比为1:20;所述EDTA与所述形体的质量比为3-5:100。
本发明的有益效果:
1、硝酸可以与陶瓷材料表面的氧化物反应,使表面产生溶解和清晰化作用,使陶瓷表面更加平滑,硝酸可以与陶瓷材料之间产生强烈的氢键作用,促进材料微观结构的改变,增加陶瓷材料的强度和硬度,同时增加陶瓷材料的抗裂和抗磨损性能;EDTA与陶瓷材料中的金属离子反应,具体为:氧化锆、氧化铈、含硅化合物中含有金属离子,可以与EDTA发生配位作用;而含硼化合物中硼元素则可以与EDTA发生络合反应,形成稳定的络合物,增加渗透液的渗透深度和陶瓷材料的硬度。
2、热处理可以依靠气流减少陶瓷坯体表面的水分含量,改善内外含水量分布的不均匀性,使得坯体在烧结过程中更加均匀地挥发水分,从而提高烧结效率和陶瓷材料的性能。
3、氧化锆主要提供材料的高稳定性和抗辐射性能;氧化镁能够提高材料的密度和硬度,同时具有一定的防辐射能力;氧化铈主要起到稳定作用;含硼化合物和含硅化合物能够协同增强陶瓷材料的防辐射性能;其中,硼化合物、氢氧化钠以及EDTA都可以对抗辐射,使得材料的防辐射性能更优;硝酸锂则用于混合颗粒的制备,加入适量的硝酸锂可以促进混合颗粒的均匀分散;通过上述成分协同增效,使得本发明方案制备的陶瓷的性能优越,包括优秀力学性能(强度、硬度和韧性)、高稳定性、抗腐蚀性强、防辐射性能。
具体实施方式
为更进一步阐述本发明为实现预定发明目的所采取的技术手段及功效,以下结合实施例,对依据本发明的具体实施方式、结构、特征及其功效,详细说明如下。
实施例1
一种防辐射陶瓷,按重量份数包括以下原料:氧化锆50份、氧化镁10份、氧化铈10份、硝酸锂0.15份、氢氧化钠2份、硼氢化钠1-5份、硅酸锂5份以及钛酸钡1份。
一种防辐射陶瓷的制备方法,包括以下步骤:
1)将氧化锆、氧化镁、氧化铈、含硼化合物、含硅化合物混合均匀,筛选后放入球磨罐中以100rpm的转速研磨4h,并在其中加入硝酸锂,混合均匀,得到混合颗粒;
2)向混合颗粒中加入氢氧化钠和去离子水,搅拌混合均匀,在室温下静置12h后,置于烘箱中在50℃下烘干2h,得到预制物;其中,所述去离子水的加入量为刚好淹没混合颗粒和氢氧化钠;
3)将预制物加入甲醇中,超声震荡2h进行离心10min,取固体置于烘箱中在105℃下干燥2h后,得到陶瓷粉料;
4)将陶瓷粉料注入注塑机中,压制成形体,置于浓度为0.1mol/L的硝酸中,通过所述回收热量加热至150℃,维持温度1h后,降温至90℃,加入EDTA,反应1h,然后将其取出,用水冲洗干净,将冲洗干净后所述形体置于热处理炉中,在300℃加热2h后,在热处理炉中进行冷却,将热处理后的所述形体置于烧结炉中进行烧结;
其中热处理炉散出的热量通过换热器收集后,得到回收热量;
其中,所述硝酸与所述形体的质量比为1:20;所述EDTA与所述形体的质量比为3:100。
其中,所述烧结炉烧结条件为升温速度5℃/min,升温至1350℃烧结4h。
实施例2
一种防辐射陶瓷,按重量份数包括以下原料:氧化锆62份、氧化镁17份、氧化铈17份、硝酸锂0.3份、氢氧化钠3份、硼氢化钠3份、硅酸锂10份以及钛酸钡3份。
一种防辐射陶瓷的制备方法,包括以下步骤:
1)将氧化锆、氧化镁、氧化铈、含硼化合物、含硅化合物混合均匀,筛选后放入球磨罐中以100rpm的转速研磨4.5h,并在其中加入硝酸锂,混合均匀,得到混合颗粒;
2)向混合颗粒加入氢氧化钠和去离子水,搅拌混合均匀,在室温下静置13h后,置于烘箱中在55℃下烘干2.5h,得到预制物;其中,所述去离子水的加入量为刚好淹没混合颗粒和氢氧化钠;
3)将预制物加入甲醇中,超声震荡2.5h进行离心15min,取固体置于烘箱中在110℃下干燥2.5h后,得到陶瓷粉料;
4)将陶瓷粉料注入注塑机中,压制成形体,置于浓度为0.15mol/L的硝酸中,通过所述回收热量加热至150℃,维持温度1.5h后,降温至100℃,加入EDTA,反应1-2h,然后将其取出,用水冲洗干净,将冲洗干净后所述形体置于热处理炉中,在310℃加热2.5h后,在热处理炉中进行冷却,将热处理后的所述形体置于烧结炉中进行烧结;
其中热处理炉散出的热量通过换热器收集后,得到回收热量;
其中,所述硝酸与所述形体的质量比为1:20;所述EDTA与所述形体的质量比为4:100。
其中,所述烧结炉烧结条件为升温速度5℃/min,升温至1350℃烧结4.5h。
实施例3
一种防辐射陶瓷,按重量份数包括以下原料:氧化锆75份、氧化镁25份、氧化铈25份、硝酸锂0.5份、氢氧化钠4份、硼氢化钠5份、硅酸锂15份以及钛酸钡5份。
一种防辐射陶瓷的制备方法,包括以下步骤:
1)将氧化锆、氧化镁、氧化铈、含硼化合物、含硅化合物混合均匀,筛选后放入球磨罐中以100rpm的转速研磨5h,并在其中加入硝酸锂,混合均匀,得到混合颗粒;
2)向混合颗粒加入氢氧化钠和去离子水,搅拌混合均匀,在室温下静置15h后,置于烘箱中在60℃下烘干3h,得到预制物;其中,所述去离子水的加入量为刚好淹没混合颗粒和氢氧化钠;
3)将预制物加入甲醇中,超声震荡3h进行离心20min,取固体置于烘箱中在115℃下干燥3h后,得到陶瓷粉料;
4)将陶瓷粉料注入注塑机中,压制成形体,置于浓度为0.2mol/L的硝酸中,通过所述回收热量加热至150℃,维持温度2h后,降温至110℃,加入EDTA,反应2h,然后将其取出,用水冲洗干净,将冲洗干净后所述形体置于热处理炉中,在320℃加热3h后,在热处理炉中进行冷却,将热处理后的所述形体置于烧结炉中进行烧结;
其中热处理炉散出的热量通过换热器收集后,得到回收热量;
其中,所述硝酸与所述形体的质量比为1:20;所述EDTA与所述形体的质量比为5:100。
其中,所述烧结炉烧结条件为升温速度5℃/min,升温至1350℃烧结5h。
对比例1-8
与实施例2相比,不同之处在于,氧化锆、氧化镁、氧化铈、硝酸锂、氢氧化钠、硼氢化钠、硅酸锂以及钛酸钡的用量(重量份)如表1所示,其余组分、制备步骤和参数均一致。
表1
氧化锆 | 氧化镁 | 氧化铈 | 硝酸锂 | 氢氧化钠 | 硼氢化钠 | 硅酸锂 | 钛酸钡 | |
对比例1 | 0 | 17 | 17 | 0.3 | 3 | 3 | 10 | 3 |
对比例2 | 62 | 0 | 17 | 0.3 | 3 | 3 | 10 | 3 |
对比例3 | 62 | 17 | 0 | 0.3 | 3 | 3 | 10 | 3 |
对比例4 | 62 | 17 | 17 | 0 | 3 | 3 | 10 | 3 |
对比例5 | 62 | 17 | 17 | 0.3 | 0 | 3 | 10 | 3 |
对比例6 | 62 | 17 | 17 | 0.3 | 3 | 0 | 10 | 3 |
对比例7 | 62 | 17 | 17 | 0.3 | 3 | 3 | 0 | 3 |
对比例8 | 62 | 17 | 17 | 0.3 | 3 | 3 | 10 | 0 |
对比例9
与实施例2相比,不同之处在于,所述防辐射陶瓷的制备方法不进行步骤41),其余组分、制备步骤和参数均一致。
对比例10
与实施例2相比,不同之处在于,所述防辐射陶瓷的制备方法不进行步骤42),其余组分、制备步骤和参数均一致。
将实施例1-3和对比例1-10制备的防辐射陶瓷分别硬度检测、X射线防护屏蔽检测,测试如下:
硬度检测:
采用显微维氏硬度计测量材料的维氏硬度,载荷为10N,加载时间为5S,硬度值是测量五次的平均值。
X射线防护屏蔽检测:
按国家标准《GBZ/T147—2002 X射线防护材料衰减性能的测定》进行防辐射性能测试,使用(120KV、附加过滤为2 .50mmAl)标准X射线进行X射线防护屏蔽检测。
其测试结果如表2所示。
表2
硬度Hv(GPa) | 铅当量值(mmPb) | |
实施例1 | 17.7 | 0.90 |
实施例2 | 16.2 | 0.81 |
实施例3 | 17.1 | 0.85 |
对比例1 | 14.7 | 0.51 |
对比例2 | 15.2 | 0.43 |
对比例3 | 13.2 | 0.41 |
对比例4 | 14.9 | 0.51 |
对比例5 | 11.8 | 0.48 |
对比例6 | 13.1 | 0.55 |
对比例7 | 14.2 | 0.57 |
对比例8 | 15.5 | 0.49 |
对比例9 | 13.5 | 0.67 |
对比例10 | 12.8 | 0.62 |
从表2测试结果可知,实施例1-3与对比例1-8相比,实施例1-3制备的防辐射陶瓷具有高硬度的机械性能和抗辐射性能;其原因是氧化锆主要提供材料的高稳定性和抗辐射性能;氧化镁能够提高材料的密度和硬度,同时具有一定的防辐射能力;氧化铈主要起到稳定作用;含硼化合物和含硅化合物能够协同增强陶瓷材料的防辐射性能;其中,硼化合物、氢氧化钠以及EDTA都可以对抗辐射,使得材料的防辐射性能更优;硝酸锂则用于混合颗粒的制备,加入适量的硝酸锂可以促进混合颗粒的均匀分散;通过上述成分协同增效,使得本发明方案制备的陶瓷的性能优越,包括优秀力学性能(强度、硬度和韧性)、高稳定性、抗腐蚀性强、防辐射性能。
实施例1-3与对比例9-10相比可知,实施例1-3制备的防辐射陶瓷具有显著的机械性能和抗辐射性能;其原因是实施例1-3的步骤42)热处理:可以改善陶瓷的晶界和微观结构,提高陶瓷的稳定性和抗损伤性,从而增强其抗辐射能力;实施例1-3的步骤41)渗透处理:通过填补陶瓷体表层的孔隙,可以提高其致密度和损伤阈值,减少裂纹的自发展和扩展,从而增强其抗辐射性能。
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭示如上,然而并非用以限定本发明,任何本领域技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容做出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简介修改、等同变化与修饰,均仍属于本发明技术方案的范围内。
Claims (10)
1.一种防辐射陶瓷,其特征在于,所述防辐射陶瓷按重量份数包括以下原料:氧化锆50-75份、氧化镁10-25份、氧化铈10-25份、硝酸锂0.15-0.5份、氢氧化钠2-4份、含硼化合物1-5份、含硅化合物5-15份以及钛酸钡1-5份。
2.根据权利要求1所述的一种防辐射陶瓷,其特征在于:所述含硼化合物为硼酸和硼氢化钠中的一种或两种;所述含硅化合物为硅酸锂、硅酸钾、硅酸钠和二氧化硅中的一种或多种。
3.一种如权利要求1~2任一项所述的防辐射陶瓷的制备方法,其特征在于,所述制备方法包括以下步骤:
1)将氧化锆、氧化镁、氧化铈、含硼化合物、含硅化合物混合均匀,筛选后放入球磨罐中研磨,并在其中加入硝酸锂,混合均匀,得到混合颗粒;
2)向混合颗粒中加入氢氧化钠和去离子水,搅拌混合均匀,在室温下静置后,置于烘箱中烘干,得到预制物;
3)将预制物加入甲醇中,超声震荡后进行离心,取固体置于烘箱中干燥后,得到陶瓷粉料;
4)将陶瓷粉料注入注塑机中,压制成形体,将形体置于烧结炉中进行烧结。
4.根据权利要求3所述的一种防辐射陶瓷的制备方法,其特征在于:在步骤1)中,所述研磨条件为以100rpm的转速研磨4-5h。
5.根据权利要求3所述的一种防辐射陶瓷的制备方法,其特征在于:在步骤2)中,所述静置时间为12-15h,所述烘箱烘干条件为在50-60℃下烘干2-3h,所述去离子水的加入量为刚好淹没混合颗粒和氢氧化钠。
6.根据权利要求3所述的一种防辐射陶瓷的制备方法,其特征在于:在步骤3)中,所述超声震荡时间为2-3h,所述离心时间为10-20min,所述干燥条件为在105-115℃下干燥2-3h。
7.根据权利要求3所述的一种防辐射陶瓷的制备方法,其特征在于:在步骤4)中,所述烧结炉烧结条件为升温速度5℃/min,升温至1350℃烧结4-5h。
8.根据权利要求3所述的一种防辐射陶瓷的制备方法,其特征在于:在步骤4)的压制成形体后,还依次包括步骤41)渗透处理和步骤42)热处理。
9.根据权利要求8所述的一种防辐射陶瓷的制备方法,其特征在于:所述步骤42)热处理为将渗透处理后的形体置于热处理炉中,在300-320℃加热2-3h后,在热处理炉中进行冷却,热处理炉散出的热量通过换热器收集后,得到回收热量。
10.根据权利要求9所述的一种防辐射陶瓷的制备方法,其特征在于:所述步骤41)渗透处理为将所述形体置于浓度为0.1-0.2mol/L的硝酸中,通过所述回收热量加热至150℃,维持温度1-2h后,降温至90-110℃,加入EDTA,反应1-2h,然后将其取出,用水冲洗干净;其中,所述硝酸与所述形体的质量比为1:20;所述EDTA与所述形体的质量比为3-5:100。
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