CN116217255B - 一种5g信号基站用高精度陶瓷材料及其制备方法 - Google Patents
一种5g信号基站用高精度陶瓷材料及其制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 229920002050 silicone resin Polymers 0.000 claims abstract description 44
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 29
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 29
- -1 magnesium lanthanum aluminate Chemical class 0.000 claims abstract description 27
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims abstract description 20
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 29
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000000919 ceramic Substances 0.000 claims description 16
- 235000015895 biscuits Nutrition 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- 239000002184 metal Substances 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 7
- 238000000748 compression moulding Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 150000004703 alkoxides Chemical class 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 3
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- BCWYYHBWCZYDNB-UHFFFAOYSA-N propan-2-ol;zirconium Chemical compound [Zr].CC(C)O.CC(C)O.CC(C)O.CC(C)O BCWYYHBWCZYDNB-UHFFFAOYSA-N 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 30
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 3
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
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Abstract
本发明涉及陶瓷材料领域,具体为一种5G信号基站用高精度陶瓷材料及其制备方法,以重量份数计,包括以下制备原料:α‑氧化铝90‑95份、氟化铝6‑8份、铝酸镁镧0.2‑0.8份、乙烯基液体硅树脂3‑5份、有机溶剂80‑120份,本发明所制备的陶瓷材料具有良好的力学性能和较低的线性收缩率,可以满足高精度陶瓷材料的生产需求。
Description
技术领域
本发明涉及陶瓷材料领域,具体为一种5G信号基站用高精度陶瓷材料及其制备方法。
背景技术
5G信号基站是5G网络的核心设备,提供无线覆盖,实现有线通信网络与无线终端之间的无线信号传输,5G信号基站建设时需要大量使用高精度的陶瓷材料,这些高精度陶瓷材料对尺寸要求较为严格,如果在生产时线性收缩率过大会在其内部产生内应力,导致尺寸变形影响精度,严重的甚至产生裂纹,不符合5G信号基站的建设规格要求,迟滞了5G信号基站的建设进度。
发明内容
发明目的:针对上述技术问题,本发明提出了一种5G信号基站用高精度陶瓷材料及其制备方法。
所采用的技术方案如下:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝90-95份、氟化铝6-8份、铝酸镁镧0.2-0.8份、乙烯基液体硅树脂3-5份、有机溶剂80-120份。
进一步地,以重量份数计,包括以下制备原料:
α-氧化铝95份、氟化铝8份、铝酸镁镧0.6份、乙烯基液体硅树脂5份、有机溶剂100份。
进一步地,所述乙烯基液体硅树脂为金属烷氧基化合物改性乙烯基液体硅树脂。
进一步地,所述金属烷氧基化合物改性乙烯基液体硅树脂的制备方法如下:
将乙烯基三乙氧基硅烷、甲苯混合搅拌均匀,滴加稀盐酸,滴毕后升温至40-50℃反应8-12h后,继续升温至85-95℃反应1-3h,恢复室温后分离出有机相,减压浓缩得到液体乙烯基硅树脂,氮气保护下,将得到的液体乙烯基硅树脂用甲苯溶解后,加入金属烷氧基化合物,升温至55-65℃反应6-10h减压旋蒸即可。
进一步地,所述金属烷氧基化合物为锆烷氧基化合物。
进一步地,所述锆烷氧基化合物为锆酸四正丙酯或锆酸四异丙酯。
进一步地,所述金属烷氧基化合物的用量为所述液体乙烯基硅树脂质量的5-12%。
进一步地,所述稀盐酸的质量浓度为0.5-1%。
进一步地,所述有机溶剂的沸点≤100℃。
本发明还提供了一种5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别干燥后混合得到第一粉料,将乙烯基液体硅树脂用有机溶剂稀释后与所述第一粉料混合球磨后干燥除去有机溶剂得到第二粉料,将所述第二粉料模压成型得到陶瓷素坯,将所述陶瓷素坯加热烧结,加热烧结时先一段升温至600-650℃,保温烧结90-120min,再二段升温至800-850℃,保温烧结90-120min,再三段升温至1400-1450℃,保温烧结120-180min,最后随炉冷却至室温即可。
本发明的有益效果:
本发明提供了一种5G信号基站用高精度陶瓷材料,液体硅树脂是一种以-Si-O-Si-为主链的半无机半有机类型的高聚物,在一定条件下会发生交联反应,形成三维网状结构的产物,将其与α-氧化铝、氟化铝、铝酸镁镧混合,这种三维网状结构会将这些陶瓷粉料包覆在其中,形成具有一定形状和强度的颗粒,在烧结过程中,发生分解并以SiO2/-Si-O-C-的形式保留,形成氧化铝-SiO2-氟化铝三元体系,在高温烧结时原位生成莫来石晶须,生成的莫来石晶须穿插在陶瓷材料内部,起到支撑和架桥作用,并且乙烯基液体硅树脂在高温烧结过程中氧化分解产生气体,这些气体的连续溢出抵消了陶瓷材料内部致密化产生的内应力,降低了线性收缩率,提高了生产精度,发明人以金属烷氧基化合物对液体硅树脂进行改性,经酯交换反应后在高聚物链中引入金属元素,在烧结时能够形成金属氧化物对陶瓷材料进行增韧增强,而铝酸镁镧能够促进陶瓷材料的烧结致密化,并细化晶粒,提高致密度和力学强度。
附图说明
图1为本发明实施例1中高精度陶瓷材料的微观形貌图;
由图中可以看到,生成的莫来石晶须穿插在陶瓷材料内部,起到支撑和架桥作用。
具体实施方式
实施例中未注明具体条件者,按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者,均为可以通过市售购买获得的常规产品。本发明未提及的技术均参照现有技术。
实施例1:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝95份、氟化铝8份、铝酸镁镧0.6份、乙烯基液体硅树脂5份、丙酮100份。
其中,乙烯基液体硅树脂为锆酸四正丙酯改性乙烯基液体硅树脂,制备方法如下:
将1kg乙烯基三乙氧基硅烷、10L甲苯加入到带冷凝管的反应釜中,开启搅拌使之混合均匀,用滴液漏斗将285mL质量浓度为1%的稀盐酸滴加到反应釜中,滴毕后开启加热升温至45℃搅拌反应10h后,继续升温至95℃搅拌反应2h,关闭加热,自然恢复室温后分离出有机相,用无水硫酸钠干燥后,减压旋蒸得到液体乙烯基硅树脂,氮气保护下,将得到的液体乙烯基硅树脂用适量甲苯溶解后,加入其质量10%的锆酸四正丙酯,开启加热升温至60℃反应8h后,反应液转移至旋转蒸发仪,减压旋蒸即可。
上述5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别于100℃干燥10h后混合得到第一粉料,将制备的锆酸四正丙酯改性乙烯基液体硅树脂用丙酮稀释后与第一粉料混合球磨15h后85℃干燥24h除去丙酮得到第二粉料,将第二粉料转移至模具中15MPa压力下模压成型80s得到陶瓷素坯,将所得陶瓷素坯在空气氛围下加热烧结,加热烧结时先以10℃/min的速度一段升温至650℃,保温烧结100min,再以5℃/min的速度二段升温至820℃,保温烧结120min,再以2℃/min的速度三段升温至1430℃,保温烧结150min,最后随炉冷却至室温即可。
实施例2:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝95份、氟化铝8份、铝酸镁镧0.8份、乙烯基液体硅树脂5份、丙酮120份。
其中,乙烯基液体硅树脂为锆酸四正丙酯改性乙烯基液体硅树脂,制备方法同实施例1;
上述5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别于100℃干燥10h后混合得到第一粉料,将制备的锆酸四正丙酯改性乙烯基液体硅树脂用丙酮稀释后与第一粉料混合球磨15h后85℃干燥24h除去丙酮得到第二粉料,将第二粉料转移至模具中15MPa压力下模压成型80s得到陶瓷素坯,将所得陶瓷素坯在空气氛围下加热烧结,加热烧结时先以10℃/min的速度一段升温至650℃,保温烧结120min,再以5℃/min的速度二段升温至850℃,保温烧结120min,再以2℃/min的速度三段升温至1450℃,保温烧结180min,最后随炉冷却至室温即可。
实施例3:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝90份、氟化铝6份、铝酸镁镧0.2份、乙烯基液体硅树脂3份、丙酮80份。
其中,乙烯基液体硅树脂为锆酸四正丙酯改性乙烯基液体硅树脂,制备方法同实施例1;
上述5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别于100℃干燥10h后混合得到第一粉料,将制备的锆酸四正丙酯改性乙烯基液体硅树脂用丙酮稀释后与第一粉料混合球磨15h后85℃干燥24h除去丙酮得到第二粉料,将第二粉料转移至模具中15MPa压力下模压成型80s得到陶瓷素坯,将所得陶瓷素坯在空气氛围下加热烧结,加热烧结时先以10℃/min的速度一段升温至600℃,保温烧结90min,再以5℃/min的速度二段升温至800℃,保温烧结90min,再以2℃/min的速度三段升温至1400℃,保温烧结120min,最后随炉冷却至室温即可。
实施例4:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝95份、氟化铝6份、铝酸镁镧0.8份、乙烯基液体硅树脂3份、丙酮120份。
其中,乙烯基液体硅树脂为锆酸四正丙酯改性乙烯基液体硅树脂,制备方法同实施例1;
上述5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别于100℃干燥10h后混合得到第一粉料,将制备的锆酸四正丙酯改性乙烯基液体硅树脂用丙酮稀释后与第一粉料混合球磨15h后85℃干燥24h除去丙酮得到第二粉料,将第二粉料转移至模具中15MPa压力下模压成型80s得到陶瓷素坯,将所得陶瓷素坯在空气氛围下加热烧结,加热烧结时先以10℃/min的速度一段升温至600℃,保温烧结120min,再以5℃/min的速度二段升温至800℃,保温烧结120min,再以2℃/min的速度三段升温至1400℃,保温烧结180min,最后随炉冷却至室温即可。
实施例5:
一种5G信号基站用高精度陶瓷材料,以重量份数计,包括以下制备原料:
α-氧化铝90份、氟化铝8份、铝酸镁镧0.2份、乙烯基液体硅树脂5份、丙酮80份。
其中,乙烯基液体硅树脂为锆酸四正丙酯改性乙烯基液体硅树脂,制备方法同实施例1;
上述5G信号基站用高精度陶瓷材料的制备方法:
将α-氧化铝、氟化铝、铝酸镁镧分别于100℃干燥10h后混合得到第一粉料,将制备的锆酸四正丙酯改性乙烯基液体硅树脂用丙酮稀释后与第一粉料混合球磨15h后85℃干燥24h除去丙酮得到第二粉料,将第二粉料转移至模具中15MPa压力下模压成型80s得到陶瓷素坯,将所得陶瓷素坯在空气氛围下加热烧结,加热烧结时先以10℃/min的速度一段升温至650℃,保温烧结90min,再以5℃/min的速度二段升温至850℃,保温烧结90min,再以2℃/min的速度三段升温至1450℃,保温烧结120min,最后随炉冷却至室温即可。
对比例1:
与实施例1基本相同,区别在于,不加入铝酸镁镧。
对比例2:
与实施例1基本相同,区别在于,用市售乙烯基液体硅树脂(得尔塔DT-10050)代替所制备的锆酸四正丙酯改性乙烯基液体硅树脂。
性能测试:
将本发明实施例1-5及对比例1-2所制备的陶瓷材料作为试样,采用游标卡尺测量试样烧结前后的尺寸,计算线性收缩率,单位%,在万能试验机上采取三点弯曲法测量试样的抗弯强度,跨距为30mm,加载速率为0.5mm/min,单位MPa,用压痕法测量并计算试样的断裂韧性,单位MPa·m1/2,测试结果见下表1:
表1:
抗弯强度 | 断裂韧性 | 线性收缩率 | |
实施例1 | 166.2 | 3.05 | 0.36 |
实施例2 | 163.7 | 2.96 | 0.42 |
实施例3 | 159.3 | 2.84 | 0.44 |
实施例4 | 162.9 | 3.01 | 0.38 |
实施例5 | 165.5 | 3.03 | 0.37 |
对比例1 | 130.4 | 2.16 | 0.38 |
对比例2 | 126.8 | 2.01 | 1.03 |
由上表1可知,本发明所制备的陶瓷材料具有良好的力学性能和较低的线性收缩率,可以满足高精度陶瓷材料的生产需求。
以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (7)
1.一种5G信号基站用高精度陶瓷材料,其特征在于,以重量份数计,包括以下制备原料:
α-氧化铝90-95份、氟化铝6-8份、铝酸镁镧0.2-0.8份、乙烯基液体硅树脂3-5份、有机溶剂80-120份;
所述乙烯基液体硅树脂为金属烷氧基化合物改性乙烯基液体硅树脂;
所述金属烷氧基化合物改性乙烯基液体硅树脂的制备方法如下:
将乙烯基三乙氧基硅烷、甲苯混合搅拌均匀,滴加稀盐酸,滴毕后升温至40-50℃反应8-12h后,继续升温至85-95℃反应1-3h,恢复室温后分离出有机相,减压浓缩得到液体乙烯基硅树脂,氮气保护下,将得到的液体乙烯基硅树脂用甲苯溶解后,加入金属烷氧基化合物,升温至55-65℃反应6-10h减压浓缩即可;
所述金属烷氧基化合物为锆烷氧基化合物。
2.如权利要求1所述的5G信号基站用高精度陶瓷材料,其特征在于,以重量份数计,包括以下制备原料:
α-氧化铝95份、氟化铝8份、铝酸镁镧0.6份、乙烯基液体硅树脂5份、有机溶剂100份。
3.如权利要求1所述的5G信号基站用高精度陶瓷材料,其特征在于,所述锆烷氧基化合物为锆酸四正丙酯或锆酸四异丙酯。
4.如权利要求1所述的5G信号基站用高精度陶瓷材料,其特征在于,所述金属烷氧基化合物的用量为所述液体乙烯基硅树脂质量的5-12%。
5.如权利要求1所述的5G信号基站用高精度陶瓷材料,其特征在于,所述稀盐酸的质量浓度为0.5-1%。
6.如权利要求1所述的5G信号基站用高精度陶瓷材料,其特征在于,所述有机溶剂的沸点≤100℃。
7.一种如权利要求1-6中任一项所述的5G信号基站用高精度陶瓷材料的制备方法,其特征在于,将α-氧化铝、氟化铝、铝酸镁镧分别干燥后混合得到第一粉料,将乙烯基液体硅树脂用有机溶剂稀释后与所述第一粉料混合球磨后干燥除去有机溶剂得到第二粉料,将所述第二粉料模压成型得到陶瓷素坯,将所述陶瓷素坯加热烧结,加热烧结时先一段升温至600-650℃,保温烧结90-120min,再二段升温至800-850℃,保温烧结90-120min,再三段升温至1400-1450℃,保温烧结120-180min,最后随炉冷却至室温即可。
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