CN112299828A - 一种应用于5g太阳能手机的透明陶瓷背板的制备方法 - Google Patents
一种应用于5g太阳能手机的透明陶瓷背板的制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 239000011268 mixed slurry Substances 0.000 claims abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 238000001746 injection moulding Methods 0.000 claims abstract description 10
- -1 rare earth ions Chemical class 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 8
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- 235000015895 biscuits Nutrition 0.000 claims abstract description 4
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- 238000010438 heat treatment Methods 0.000 claims description 38
- 238000000034 method Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
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- 229910052596 spinel Inorganic materials 0.000 claims description 5
- 229910026161 MgAl2O4 Inorganic materials 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 4
- 229910052906 cristobalite Inorganic materials 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 229910052682 stishovite Inorganic materials 0.000 claims description 4
- 229910052905 tridymite Inorganic materials 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 238000005266 casting Methods 0.000 abstract description 4
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- YWYZEGXAUVWDED-UHFFFAOYSA-N triammonium citrate Chemical compound [NH4+].[NH4+].[NH4+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O YWYZEGXAUVWDED-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
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- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
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- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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Abstract
本发明公开了一种应用于5G太阳能手机的透明陶瓷背板的制备方法,它包括以下步骤:按照稀土离子掺杂的透明陶瓷材料分子式中各元素的化学计量比称取原料粉体,将原料粉体、烧结助剂、溶剂、磨球放入球磨罐中,球磨混合得混合浆料;混合浆料干燥、过筛、煅烧得到凝胶注模成型的原料粉;使用上述原料粉配制凝胶成型体系所需浆料,真空除泡后注入手机背板模具中,室温下凝胶固化成型,脱模坯体并干燥;将干燥后的陶瓷素坯依次进行排胶、真空烧结、精密加工和抛光处理,得到透明陶瓷背板。本发明结合了陶瓷手机背板的材料优势和凝胶注模成型特点,制备得到满足5G太阳能手机背板所需的透明、高太阳能利用率要求的陶瓷背板。
Description
技术领域
本发明涉及陶瓷背板技术领域,具体涉及一种应用于5G太阳能手机的透明陶瓷背板的制备方法。
背景技术
手机背板是手机的重要零件,随着科技的飞速发展,人们对电子产品的要求也越来越高,其中消费者对手机背板质量和外观的要求也越来越高。目前手机背板材料主要为塑料、金属、玻璃和陶瓷。其中,由于陶瓷背板具有耐磨性好、硬度高、散热性强、穿透力强等特点,正成为手机企业产业链进军5G时代的重要材料。特别是具有高对称性的立方晶体结构的陶瓷,不仅可减少双折射,具有良好的透光性,也利于工信部提出的3300-3600MHz和4800-5000MHz的5G毫米波频率信号传输。更主要的是,为了适应未来太阳能和5G手机的发展需要,必然要求陶瓷手机背板具有透明、高光能利用率、易传输5G毫米波的特性。
然而,目前尚未发现采用透明陶瓷生产的用于5G太阳能的手机背板。而且研究发现此技术领域申请的专利不多,主要紧密相关的有专利CN 110217985 A公开了一种低膨胀系数透明微晶玻璃及其制品的生产方法,可以制成超薄、高强度透明微晶玻璃的5G手机背板等。又如:专利CN 108947539 A提供一种氮化硅陶瓷材料的制备方法并用于手机背板。专利CN 107347103 A公开了一种采用玻璃热弯机一体热弯成型手机玻璃后盖的制备方法。而在手机背板的透明陶瓷成型过程中,凝胶注模成型具有高素坯强度、可机加工、净几尺寸、便于成型像手机背板这类需要开孔、开槽等复杂结构的陶瓷器件。因此,针对未来5G高频毫米波和和绿色能源时代对手机背板的综合功能要求,结合透明陶瓷材料的优良性能和凝胶注模成型技术特点非常有利于透明陶瓷手机背板的制备。
发明内容
本发明的目的是提供一种应用于5G太阳能手机的透明陶瓷背板的制备方法。
为实现上述目的,本发明采用的技术方案如下:一种应用于5G太阳能手机的透明陶瓷背板的制备方法,包括如下步骤:
步骤一、按照稀土离子掺杂的透明陶瓷材料分子式中各元素的化学计量比称取原料粉体,除杂预处理,所述透明陶瓷材料具有立方、六方或等轴晶体结构;
步骤二、将所述原料粉体混合并加入烧结助剂、磨球、溶剂组成预混液,放入球磨罐中混合球磨,得到混合浆料;
步骤三、球磨结束后将混合浆料烘干,过筛,再放入马弗炉中煅烧,得到凝胶注模成型的陶瓷原料粉;
步骤四、使用上述原料粉配制凝胶成型体系所需浆料,真空除泡后注入手机背板模具中,室温下凝胶固化成型,3~6h后脱模坯体并干燥;
步骤五、将干燥后的陶瓷素坯依次进行排胶、真空烧结、精密加工和抛光处理,得到透明陶瓷背板。
优选的,步骤一中,所述透明陶瓷材料为YAG(Y3Al5O12,钇铝石榴石)、MgAl2O4(镁铝尖晶石)、Al2O3(氧化铝)中的一种或多种,所述稀土离子为Er3+、Tm3+和Ho3+中的一种或多种,稀土离子掺杂量为1~5at%。
优选的,步骤二中,所述烧结助剂为MgO和/或SiO2,烧结助剂的加入量为陶瓷原料粉体总质量的0.5%;所述磨球为Al2O3磨球,球料比为1~3:1;所述溶剂为无水乙醇;球磨转速为120~160r/min,球磨时间为24~36h。
优选的,步骤三中,所述烘干的温度为40~120℃,时间为24~48h。
优选的,步骤三中,所述过筛的筛网目数为100~200目。
优选的,步骤三中,所述煅烧的温度为800~1000℃,保温时间为8~24h。
优选的,步骤四中,所述的凝胶成型体系为AM(丙烯酰胺)、PIBM(异丁烯和马来酸酐的共聚物)和MAM(甲基丙烯酰胺)凝胶体系中的一种。
优选的,步骤四中,所述脱模坯体先室温干燥2~6h再于40~60℃烘箱中继续干燥6~8h。
优选的,步骤五中,所述排胶的参数为:室温下以升温速率为0.5~2℃/min,升温到450℃,再以升温速率为0.5~3℃/min升温到800℃,并在800℃保温2~6h。
优选的,步骤五中,所述真空烧结的参数为:首先按5~10℃/min从室温升温到200℃并保温10~30min,其次按10~20℃/min升温到1000℃并保温10~30min,然后按1~5℃/min升温到1600~1800℃并保温4~8h,最后以5~10℃/min降温到室温,整个烧结过程中真空度保持在1×10-2~1×10-5Pa。
与现有技术相比,本发明具有如下有益效果:
1.本发明提供的制备方法,结合了陶瓷手机背板的材料优势和凝胶注模成型特点,利用高对称的六方或立方晶系陶瓷材料,通过凝胶注模成型均匀的掺杂高吸收太阳能的稀土离子达到较高的光能利用率以满足5G太阳能手机背板所需的透明、高太阳能利用率的要求,具备高强度、高硬度、高热导率特性、高电阻率、低介电常数和介电损耗以及优良的透波性能,具有满足未来5G通信及绿色能源的双重要求。
2.本发明提供的制备方法,工艺简单高效,可实现工业化。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明。
以下实施例中所使用的原料粉体均为高纯纳米粉体,纯度>99.99%。
实施例1
一种应用于5G太阳能手机的透明陶瓷背板的制备方法,它包括以下步骤:
步骤一、按照1%Er3+:YAG分子式中各元素的化学计量比分别称量高纯纳米Y2O3粉体21.47g、高纯纳米α-Al2O3粉体28.53g,高纯纳米Er2O3粉体0.5g;
步骤二、使用烧结助剂SiO2 0.25g、高纯Al2O3磨球150g、无水乙醇60ml、充分搅拌后放入球磨罐中,在120r/min的转速下混合球磨36h后得到混合浆料;
步骤三、将混合浆料置于40℃恒温烘箱中烘48h后过筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到800℃,保温8h后自然冷却,作为凝胶注模成型的原料粉;
步骤四、采用AM凝胶注模体系,在11.5g的去离子水中,加入AM有机单体2.5g,交联剂N,N-亚甲基双丙烯酰胺(MBAM)0.208g,用氨水调节pH到10,采用柠檬酸铵分散剂0.15g,并加入原料粉50g后充分球磨,制备固含量为50vol.%的陶瓷浆料;再用真空除泡机进行除泡处理后加入0.25g的APS引发剂,充分搅拌后注入手机背板玻璃模具中;室温下自然凝胶固化,3h后脱模坯体并进行干燥处理:室温先干燥2h后,放入40℃烘箱中保温8h;,
步骤五、干燥后进行排胶处理,从室温开始以2℃/min升温速度到450℃,再以1.5℃/min升温速度到800℃,并保温2h;最后真空烧结,室温开始以10℃/min升温到200℃,保温30min,再次按10℃/min升温到1000℃并保温10min,然后按5℃/min升温到1750℃并保温6h,最后以5℃/min降温到室温,整个烧结过程中真空度保持在1×10-2Pa。再经过精密加工和抛光处理,得到透明陶瓷手机背板。
表1是5G手机测试信号通过8mm厚陶瓷背板(实施例1制备)的实验测试结果,经5G信号测试确认,本实施例制备的透明陶瓷背板对5G通讯信号无屏蔽。
表1 5G信号测试结果
网络名称/信号类型 | 信号强度(无屏蔽) | 信号强度(有陶瓷屏蔽) |
中国电信/SA | 107dBm 33asu | 107dBm 33asu |
中国移动/NSA | 122dBm 33asu | 122dBm 33asu |
实施例2
一种应用于5G太阳能手机的透明陶瓷背板的制备方法,它包括以下步骤:
步骤一、按照5%Tm3+:MgAl2O4分子式分别称量纳米MgAl2O4粉体50g和高纯纳米Tm2O3粉体2.5g;
步骤二、使用烧结助剂MgO 0.05g、高纯Al2O3磨球120g、无水乙醇80ml、充分搅拌后放入球磨罐中,在140r/min的转速下混合球磨32h后得到混合浆料;
步骤三、将混合浆料置于120℃恒温烘箱中烘24h后过筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到1000℃,保温24h后自然冷却,作为凝胶注模成型的原料粉;
步骤四、采用PIBM凝胶注模体系,在12g的去离子水中,加入Isobam104#0.15g,用四甲基氢氧化铵调节pH到11,采用柠檬酸铵分散剂0.10g,并加入原料粉50g后充分球磨,制备固含量为48vol.%的陶瓷浆料,再用真空除泡机进行除泡处理迅速注入手机背板硅胶模具中;室温下自然凝胶固化,5h后脱模坯体并进行干燥处理:室温先干燥4h后,放入50℃烘箱中保温7h。
步骤五、干燥后进行排胶处理,从室温开始以1℃/min升温速度到450℃,再以3℃/min升温速度到800℃,并保温6h;最后真空烧结,室温开始以5℃/min升温到200℃,保温10min,再次按20℃/min升温到1000℃并保温30min,然后按1℃/min升温到1800℃并保温4h,最后以10℃/min降温到室温,整个烧结过程中真空度保持在1×10-5Pa。再经过精密加工和抛光处理,得到透明陶瓷手机背板。。
表2是5G手机测试信号通过8mm厚陶瓷背板(实施例2制备)的实验测试结果,经5G信号测试确认,本实施例制备的透明陶瓷背板对5G通讯信号无屏蔽。
表2 5G信号测试结果
网络名称/信号类型 | 信号强度(无屏蔽) | 信号强度(有陶瓷屏蔽) |
中国电信/SA | 107dBm 33asu | 107dBm 33asu |
中国移动/NSA | 122dBm 33asu | 122dBm 33asu |
实施例3
一种应用于5G太阳能手机的透明陶瓷背板的制备方法,它包括以下步骤:
步骤一、按照2%Ho3+:Al2O3分子式分别称量高纯纳米α-Al2O3粉体50g和高纯纳米Ho2O3粉体1.0g;
步骤二、使用烧结助剂SiO2 0.15g和MgO 0.1g、高纯Al2O3磨球100g、无水乙醇70ml、充分搅拌后放入球磨罐中,在160r/min的转速下混合球磨24h后得到混合浆料;
步骤三、将混合浆料置于100℃恒温烘箱中烘36h后过筛,将过筛后的粉体置于马弗炉中煅烧,从室温升温到900℃,保温12h后自然冷却,作为凝胶注模成型的原料粉;
步骤四、采用MAM凝胶注模体系,在10g的去离子水中,加入MAM有机单体2.2g,交联剂二丙烯基酒石酸二酰胺(DATDA)0.2g,用四甲基氢氧化铵调节pH到11,加入原料粉50g后充分球磨,制备固含量为52vol.%的陶瓷浆料。再用真空除泡机进行除泡处理后加入0.3g的引发剂,充分搅拌后注入手机背板不锈钢模具中;室温下自然凝胶固化,6h后脱模坯体并进行干燥处理:室温先干燥6h后,放入60℃烘箱中保温6h;
步骤五、干燥后进行排胶处理,从室温开始以1℃/min升温速度到450℃,再以2℃/min升温速度到800℃,并保温4h;最后真空烧结,室温开始以8℃/min升温到200℃,保温20min,其次按15℃/min升温到1000℃并保温20min,然后按4℃/min升温到1600℃并保温8h,最后以8℃/min降温到室温,整个烧结过程中真空度保持在1×10-3Pa。再经过精密加工和抛光处理,得到透明陶瓷手机背板。
表3是5G手机测试信号通过8mm厚陶瓷背板(实施例3制备)的实验测试结果,经5G信号测试确认,本实施例制备的透明陶瓷背板对5G通讯信号无屏蔽。
表3 5G信号测试结果
网络名称/信号类型 | 信号强度(无屏蔽) | 信号强度(有陶瓷屏蔽) |
中国电信/SA | 107dBm 33asu | 107dBm 33asu |
中国移动/NSA | 122dBm 33asu | 122dBm 33asu |
Claims (10)
1.一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,包括如下步骤:
步骤一、按照稀土离子掺杂的透明陶瓷材料分子式中各元素的化学计量比称取原料粉体,除杂预处理,所述透明陶瓷材料具有立方、六方或等轴晶体结构;
步骤二、将所述原料粉体混合并加入烧结助剂、磨球、溶剂组成预混液,放入球磨罐中混合球磨,得到混合浆料;
步骤三、球磨结束后将混合浆料烘干,过筛,再放入马弗炉中煅烧,得到凝胶注模成型的陶瓷原料粉;
步骤四、使用上述原料粉配制凝胶成型体系所需浆料,真空除泡后注入手机背板模具中,室温下凝胶固化成型,3~6h后脱模坯体并干燥;
步骤五、将干燥后的陶瓷素坯依次进行排胶、真空烧结、精密加工和抛光处理,得到透明陶瓷背板。
2.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤一中,所述透明陶瓷材料为YAG、MgAl2O4、Al2O3中的一种或多种,所述稀土离子为Er3+、Tm3+和Ho3+中的一种或多种,稀土离子掺杂量为1~5at%。
3.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤二中,所述烧结助剂为MgO和/或SiO2,烧结助剂的加入量为陶瓷原料粉体总质量的0.5%;所述磨球为Al2O3磨球,球料比为1~3:1;所述溶剂为无水乙醇;球磨转速为120~160r/min,球磨时间为24~36h。
4.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤三中,所述烘干的温度为40~120℃,时间为24~48h。
5.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤三中,所述过筛的筛网目数为100~200目。
6.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤三中,所述煅烧的温度为800~1000℃,保温时间为8~24h。
7.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤四中,所述的凝胶成型体系为丙烯酰胺、PIBM和甲基丙烯酰胺凝胶体系中的一种。
8.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤四中,所述脱模坯体先室温干燥2~6h再于40~60℃烘箱中继续干燥6~8h。
9.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤五中,所述排胶的参数为:室温下以升温速率为0.5~2℃/min升温到450℃,再以升温速率为0.5~3℃/min升温到800℃,并在800℃保温2~6h。
10.根据权利要求1所述的一种应用于5G太阳能手机的透明陶瓷背板的制备方法,其特征在于,步骤五中,所述真空烧结的参数为:首先按5~10℃/min从室温升温到200℃并保温10~30min,其次按10~20℃/min升温到1000℃并保温10~30min,然后按1~5℃/min升温到1600~1800℃并保温4~8h,最后以5~10℃/min降温到室温,整个烧结过程中真空度保持在1×10-2~1×10-5Pa。
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