CN115259844B - 一种陶瓷材料及其制备方法和应用 - Google Patents
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims abstract description 34
- 239000013078 crystal Substances 0.000 claims description 24
- 238000013003 hot bending Methods 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 238000010438 heat treatment Methods 0.000 claims description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 13
- 239000010439 graphite Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000000137 annealing Methods 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 229910018068 Li 2 O Inorganic materials 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 238000002834 transmittance Methods 0.000 claims description 5
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 claims description 4
- 238000003426 chemical strengthening reaction Methods 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 claims description 3
- 238000005342 ion exchange Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 238000005728 strengthening Methods 0.000 claims description 3
- 238000010408 sweeping Methods 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 2
- 238000005452 bending Methods 0.000 claims description 2
- 238000005034 decoration Methods 0.000 claims description 2
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 abstract description 24
- 239000011148 porous material Substances 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 229910052582 BN Inorganic materials 0.000 description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 1
- HEHRHMRHPUNLIR-UHFFFAOYSA-N aluminum;hydroxy-[hydroxy(oxo)silyl]oxy-oxosilane;lithium Chemical compound [Li].[Al].O[Si](=O)O[Si](O)=O.O[Si](=O)O[Si](O)=O HEHRHMRHPUNLIR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 229910052670 petalite Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
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Abstract
本发明公开了一种陶瓷材料及其制备方法和应用,该陶瓷材料在可见光波段透过率为5%‑65%,Lab值的L值为50‑100,a值为‑5至+5,b值为‑5至+15;雾度≥50%;密度介于2.3g/cm3‑2.7g/cm3,相对介电常数为5‑6。可以代替氧化锆陶瓷用作手机背板或可穿戴设备的背板或笔记本电脑触控板或平板电脑背板。
Description
技术领域
本发明属于特种陶瓷材料领域,具体涉及一种陶瓷材料及其制备方法和应用。
背景技术
21世纪背景下,手机、笔记本等终端的外观设计材料,需要满足尽量降低对电磁信号的屏蔽,具有优良的抗摔性能,同时要求美丽的外观,例如手机背板,通常会采用塑料、玻璃或氧化锆陶瓷,其中氧化锆陶瓷是目前现有技术下最高端的材料,它以温润如玉的质感以及抗摔性能以及纯洁的白色被人们所喜爱,但是与此同时,人们也在迫切的寻找其他的材料,在达到氧化锆陶瓷的各项优异性能的同时可以更好的提升他的抗摔性能以及尽量降低它的介电常数、降低材料成本、降低材料重量迫在眉睫。
发明内容
为了找到与氧化锆陶瓷相似外观的替代材料,同时提供更好的抗摔性能并尽量降低其介电常数,降低材料成本,降低材料重量,本发明提供了一种陶瓷材料及其制备方法和应用,具体技术方案如下:
一种陶瓷材料,其在可见光波段透过率为5%-65%,Lab值的L值为50-100,a值为-5至+5,b值为-5至+15;雾度≥50%;密度介于2.3g/cm3-2.7g/cm3,相对介电常数为5-6。
进一步的,该陶瓷材料的晶体类型为二硅酸锂和锂铝硅石,结晶度≥90%,晶体尺寸为90-400nm,晶体形貌为带孔类球形。
更进一步的,该材料的断裂韧性≥2MPa×m1/2。
优选地,该陶瓷材料由67-73wt%SiO2,5-9wt%Al2O3,0-1wt%TiO2,0-1wt%CaO,9-13wt%Li2O,0.1-1.5wt%Na2O,0.1-1wt%K2O,3-6wt%P2O5,3-9wt%ZrO2,0-1wt%BaO,0-3wt%MgO,0-2wt%ZnO和0-2wt%Sb2O3经过高温熔融退火后再经热弯处理后制得。
一种陶瓷材料的制备方法,包括以下步骤:
步骤1:67-73wt%SiO2,5-9wt%Al2O3,0-1wt%TiO2,0-1wt%CaO,9-13wt%Li2O,0.1-1.5wt%Na2O,0.1-1wt%K2O,3-6wt%P2O5,3-9wt%ZrO2,0-1wt%BaO,0-3wt%MgO,0-2wt%ZnO和0-2wt%Sb2O3混合均匀,后分4-8次放入铂金坩埚中,1300-1650℃条件下融化30h后浇筑成型;
步骤2:将步骤1浇筑成型的块料投入退火炉中,500℃条件下保温24h,再经5h后随炉按30℃/min的降温速率降至室温后取出切成片状;
步骤3:将步骤2得到的片状材料在室温条件下放入晶化炉中,以1-20℃/min的梯度升温至600-1000℃,在600-1000℃下保温30-180min,保温结束后,以10-30℃/min的降温速率降至室温后取出;
步骤4:将步骤3得到的陶瓷片进行CNC及抛光、扫边处理;
步骤5:将步骤4得到的陶瓷片放入2D或3D石墨模具中,再将装有陶瓷片的石墨模具放入热弯机中进行热弯,热弯机按照30-100℃/min的升温速率升温至700-900℃,并在700-900℃的温度下保持5-30min,后按照50-100℃/min的降温速率降至室温后取出陶瓷片,然后将得到的陶瓷片进行抛光,即制得目标产品,陶瓷片实现3D外形的同时完成第二段热处理长晶。该步骤将传统的两步法先成核后长晶结合为一步,本发明原料组成中提高了氧化锆的占比,二氧化锆是一种好的成核剂,因而成核的温度区间与长晶的温度区间重叠区域更大,进而可以一步完成成核和长晶过程,节约了生产成本,经过本步骤处理的陶瓷材料的透过率为5-65%,结晶度已经到达89%以上;
优选的,步骤5中使用的模具为石墨模具,石墨模具在700-900℃下会氧化,通过热弯机的热弯炉中充入氮气,避免石墨模具的氧化,该步骤中没有使用耐高温的氮化硼模具;同时采用单片进行热处理,没有采用叠片的方案,没有使用氮化硼类的脱模剂,避免氮化硼在高温下受热分解产生氧化硼类的物质渗入玻璃内部影响晶粒的生长,本申请陶瓷的母坯的晶体生长不会与模具材料或脱模剂材料发生反应,从而在该热处理的温度和时间下晶体粒径较小,又因为二硅酸锂和锂铝硅石晶体形成的小尺寸阶段,因而晶体形貌依然为类球形;特别地,该步骤中在热弯处理时,在热弯机中持续充入氮气以防止石墨模具的氧化,保持热弯机腔内压力维持在0.01-0.02Mpa的正压;热弯处理700-900℃期间给石墨模具施压,压强值为0.1-1Mpa。
优选地,还包括步骤6:将步骤5得到的陶瓷片放入含有硝酸钾、硝酸钠、硝酸锂的强化盐中在400-500℃条件下保温3-5h进行离子交换,进行化学强化。
进一步地,还包括步骤7:将步骤6得到的陶瓷片进行表面装饰。
一种上述陶瓷材料的应用,其用作手机背板或可穿戴设备的背板或笔记本电脑触控板或平板电脑背板。
本发明中使用67-73wt%SiO2,5-9wt%Al2O3,0-1wt%TiO2,0-1wt%CaO,9-13wt%Li2O,0.1-1.5wt%Na2O,0.1-1wt%K2O,3-6wt%P2O5,3-9wt%ZrO2,0-1wt%BaO,0-3wt%MgO,0-2wt%ZnO和0-2wt%Sb2O3作为原料,将热处理融合在热弯处理步骤,在陶瓷体内形成以透锂长石和二硅酸锂为主要晶相的陶瓷材料,晶体的形貌为带孔类球形,类球形形貌的晶体使陶瓷内部的微裂纹在扩展时遇到晶体会发生微裂纹的方向转变,从而降低微裂纹进一步扩展的动能。晶体的尺寸介于90-400nm之间,同时晶体在长大的过程中大的晶体会与小的晶体生长成一体,因为单独的晶体形状为类球形,所以球形与球形的交界处就会在晶界处形成气孔,气孔的尺寸在1-5nm,因为有气孔的存在,进一步降低了材料整体的密度;另一方面,处于90-400nm尺寸的晶体与可见光的380-780nm波段一定程度的重叠,可以对光进行有效地遮蔽通过,从而形成透过率在5%-65%的白色抗摔陶瓷。
同时,本发明的陶瓷材料相比于氧化锆陶瓷的相对分子质量低,其密度介于2.3g/cm3-2.7g/cm3,相比于氧化锆陶瓷的5g/cm3-6g/cm3,更为轻质。
本发明的有益技术效果为该陶瓷材料在可见光波段透过率为5%-65%,Lab值的L值为50-100,a值为-5至+5,b值为-5至+15;雾度≥50%;密度介于2.3g/cm3-2.7g/cm3,相对介电常数为5-6,断裂韧性≥2MPa×m1/2,密度介于2.3g/cm3-2.7g/cm3,可以代替氧化锆陶瓷用作手机背板或可穿戴设备的背板或笔记本电脑触控板或平板电脑背板。
附图说明
图1为本发明实施例1制得的陶瓷材料SEM照片;
图2为本发明实施例2制得的陶瓷材料SEM照片。
具体实施方式
实施例1
第一步:将71wt%SiO2,9wt%Al2O3,0.05wt%CaO,11.71wt%Li2O,0.2wt%Na2O,0.5wt%K2O,1wt%P2O5,6wt%ZrO2,0.03wt%BaO,0.51wt%MgO粉料先混合均匀,然后分次放入铂金坩埚中,在1300-1650℃的条件下融化30h后浇筑成型;
第二步:将浇筑成型的块料3min之内放入退火炉中,500℃条件下保温24h进行退火处理,5h之后随炉按照每分钟30℃的条件下随炉降至室温后取出;
第三步:将取出的块体通过线切割成90*180*0.7mm的片状;
第四步:将第三步得到的片状材料室温下放入晶化炉中以1℃/min的梯度升温至设定温度600℃,然后在设定温度下保温30min,保温结束后,以10℃/min的降温速率降至室温后取出;
第五步:将第四步得到的陶瓷片按照要求的尺寸形状进行CNC及抛光、扫边处理;
第六步:将第五步得到的陶瓷片放入3D石墨模具中,再将装有陶瓷片的石墨模具放入热弯机中进行热弯,热弯机按照30℃/min的升温速率升温至700℃,并在700℃的温度下保持5min,然后按照50℃/min的降温速率降至室温后取出,实现模具外形的同时完成第二段热处理;
第七步:将第六步得到的陶瓷进行进一步的抛光处理,以抛除热弯带来的模印、麻点;
第八步:将第七步得到的陶瓷材料放入含有硝酸钾、硝酸钠、硝酸锂的强化盐中在450℃条件下保温4h进行离子交换,进行化学强化,得最终产品。
实施例1-7的实验参数及测试结果如下表所示。
Claims (9)
1.一种陶瓷材料的制备方法,其特征在于包括以下步骤:
步骤1:将67-73wt%SiO 2 , 9wt%Al 2 O 3 , 0.05wt%CaO,12.71-13wt%Li 2 O,0.2wt%Na 2 O,0.5wt%K 2 O,1wt%P 2 O 5 ,3-9wt%ZrO 2 ,0.03wt%BaO,0.22-2.22wt%MgO和0-0.1wt%ZnO混合均匀,为保证充分均匀融化,先后分4-8次放入铂金坩埚中,1300-1650℃条件下保温30h以融化,后浇筑成型;
步骤2:将步骤1浇筑成型的块料投入退火炉中,500℃条件下保温24h,再随炉按30℃/min的降温速率降至室温后取出切成片状;
步骤3:将步骤2得到的片状材料在室温条件下放入晶化炉中,以10-20℃/min的梯度升温至850-1000℃,在850-1000℃下保温110-180min,保温结束后,以20-30℃/min的降温速率降至室温后取出;
步骤4:将步骤3得到的陶瓷片进行CNC及抛光、扫边处理;
步骤5:将步骤4得到的陶瓷片单片放入2D或3D石墨模具中,再将装有陶瓷片的石墨模具放入热弯机中进行热弯,热弯机按照80-100℃/min的升温速率升温至700-900℃,并在700-900℃的温度下保持10-30min,后按照90-100℃/min的降温速率降至室温后取出陶瓷片 ,然后将得到的陶瓷片进行抛光,即制得目标产品,制得陶瓷材料在可见光波段透过率为5%-65%,Lab值的L值为50-100,a值为-5至+5,b值为-5至+15;雾度≥50%;密度介于2.3g/cm 3 -2.7g/cm 3 ,相对介电常数为5-6。
2.根据权利要求1所述的陶瓷材料的制备方法,其特征在于还包括步骤6:将步骤5得到的陶瓷片放入含有硝酸钾、硝酸钠、硝酸锂的强化盐中在400-500℃条件下保温3-5h进行离子交换,进行化学强化。
3.根据权利要求2所述的陶瓷材料的制备方法,其特征在于还包括步骤7:将步骤6得到的陶瓷片进行表面装饰。
4.根据权利要求1所述的陶瓷材料的制备方法,其特征在于步骤5中在热弯处理时,在热弯机中持续充入氮气以防止石墨模具的氧化,热弯机炉腔应持续保持正压,压力值为0.01-0.02Mpa;热弯处理700-900℃期间给石墨模具施压,压力值为0.1-1Mpa。
5.一种如权利要求1所述的方法制得的陶瓷材料,其特征在于其在可见光波段透过率为5%-65%,Lab值的L值为50-100,a值为-5至+5,b值为-5至+15;雾度≥50%;密度介于2.3g/cm 3 -2.7g/cm 3 ,相对介电常数为5-6。
6.根据权利要求5所述的陶瓷材料,其特征还在于该材料晶体类型为二硅酸锂和锂铝硅石,结晶度≥90%,晶体尺寸为90-400nm,晶体形貌为类球形。
7.根据权利要求5或6所述的陶瓷材料,其特征在于该材料的断裂韧性≥2MPa×m 1/2 。
8.根据权利要求7所述的陶瓷材料,其特征还在于其由67-73wt%SiO 2 , 9wt%Al 2 O3 , 0.05wt%CaO,12.71-13wt%Li 2 O,0.2 wt%Na 2 O,0.5wt%K 2 O,1wt%P 2 O 5 ,3-9wt%ZrO 2 ,0.03wt%BaO,0.22-2.22wt%MgO和0-0.1wt%ZnO经过高温熔融退火后再经热弯处理后制得。
9.一种如权利要求5或6或8所述的陶瓷材料的应用,其用作手机背板或可穿戴设备的背板或笔记本电脑触控板或平板电脑背板。
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