CN105906331A - 一种大规格陶瓷基板、其制备方法以及生产线 - Google Patents

一种大规格陶瓷基板、其制备方法以及生产线 Download PDF

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CN105906331A
CN105906331A CN201610355830.5A CN201610355830A CN105906331A CN 105906331 A CN105906331 A CN 105906331A CN 201610355830 A CN201610355830 A CN 201610355830A CN 105906331 A CN105906331 A CN 105906331A
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oxide
ceramic
ceramic substrate
sintering equipment
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吴崇隽
孔丽萍
蔡斌斌
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Zhengzhou Zhongci Technology Co Ltd
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Abstract

本发明公开了一种大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.04‑0.14∶0.005‑0.018∶0.02‑0.06∶0.3‑0.9;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝93‑96%、二氧化硅0.5‑3%、氧化镁0.3‑2%、氧化钙0.2‑1%、氧化钇0.1‑2%、碳酸钡0.1‑2.5%、氧化锆0.05‑1%、氧化铋0.1‑2%同时公开了陶瓷基板的生产方法和所需的生产线。本发明陶瓷基板具有优良的机械强度,良好的导热特性;制备方法简单,成本低,生产线简单,不占用空间,有效提高产品质量。

Description

一种大规格陶瓷基板、其制备方法以及生产线
技术领域
本发明属于陶瓷基板技术领域,具体涉及一种大规格陶瓷基板、其制备方法以及生产线。
背景技术
近年来,LED照明、太阳能及风力发电等新能源产业蓬勃发展,这些产业都需要大功率电子电路。原用铝板涂硅油做LED电路基板因耐电压性能差、涂硅油后导热至6倍性差、硅油老化导致LED芯片光衰和死灯等问题,预计今明两年LED用的大规格电子陶瓷基板将以每年4的速度增长,高性能氧化铝电子陶瓷基板具有广阔的应用领域和巨大的市场空间。而全球只有德国赛琅泰克(CERAMTEC)、日本丸和(MARUWA)、日本京瓷(KYOCERA)等少数的厂商生产,国内只有极个别的厂家生产小规格的低端产品。小规格产品适用范围较小,并且工艺配方及设备不能用于大规格氧化铝陶瓷生产,因此急需开发一种大规格的陶瓷基板。
发明内容
本发明的目的在于提供一种大规格陶瓷基板、其制备方法以及生产线。
为实现上述目的,本发明采用如下技术方案:
一种大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.04-0.14∶0.005-0.018∶0.02-0.06∶0.3-0.9;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝93-96%、二氧化硅0.5-3%、氧化镁0.3-2%、氧化钙0.2-1%、氧化钇0.1-2%、碳酸钡0.1-2.5%、氧化锆0.05-1%、氧化铋0.1-2%。
所述陶瓷粉料中氧化铝的粒度为1.0-5.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为1.0-4.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1-1.8。
所述粘结剂为聚乙烯醇缩丁醛;所述分散剂为蓖麻油;所述增塑剂为邻苯二甲酸二丁酯。
上述大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机中,然后加入分散剂进行预分散,分散后加入球磨机中球磨30-50h至组织非常均匀,再在-0.01-0.15MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度20-50℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置的排胶区,在室温-500℃下排胶18-22h;然后进入烧结装置的升温高温区,在500-1600℃下烧结20-30h;接着进入烧结装置的降温区,在1600-900℃下烧结8-15h;再进入整平装置,在1300-1400℃下整平44-55h即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
上述方法得到的陶瓷基板可以根据客户要求用激光加工的方法进一步的进行刻化切割加工。
为了满足生产需求,本发明还提供了制备大规格陶瓷基板的生产线,包括高速分散机,高速分散机的出口依次连接有球磨机、真空脱泡装置、流延成型装置、敷粉装置、烧结装置和整平装置;所述烧结装置包括机架,机架的机头处设有推机,机架上设有炉膛,炉膛内设有传动辊,炉膛的出口和入口均设有与传动辊连接的固定板,固定板上沿传动辊传动方向设有两条平行的导轨;炉膛内设有加热装置,炉膛上方设有排气孔,排气孔通过管道连接换热器,换热器上连接有进水管道。
为了得到更好的大规格陶瓷基板,所述炉膛的膛壁由内到外依次为304不锈钢层、保温层和201不锈钢层;所述换热器为热管换热器。
优选的,为了对溶剂进行回收再利用,保护环境,所述流延成型装置连接有溶剂回收装置。
经检测,本发明大规格陶瓷基板的体积密度为3.65-3.75g/cm3,抗弯强度为250-450MPa,线膨胀系数((25-800℃)10-6):7.7-7.8,热导率为18-26w/(m·k),绝缘强度为15KV/mm,体积电阻率(25℃)为>1014Ω·cm,介电常数(ε(1MHz))为9.0,接电损耗((1MHz)/10-4)为3。综上所述本发明陶瓷基本各项性能良好。
本发明陶瓷基板具有优良的机械强度,良好的导热特性,适用于高温环境;具有耐抗侵蚀和磨耗性,高电气绝缘特性,良好表面特性,提供优异平面度与平坦度;抗震效果佳,低翘曲度,高温环境下稳定性稳定,可加工成各种复杂形状。本发明制备方法简单,采用流延法陶瓷基板,相比于干压、扎膜等成型工艺,流延法得到的基板组织非常均匀、致密,烧结后的晶粒均匀、气孔少、抗热震性好、导热性好、抗弯强度高、表面光洁,成本低。本发明的生产线简单,不占用空间,流延成型装置配备吸附冷凝式溶剂回收装置,烧结废气冷水冷凝的方式处理,有效提高产品质量并从源头减少污染物排放,达到国内清洁生产先进水平,适合工业使用。
附图说明
图1为本发明生产线结构示意图;
图2为本发明烧结装置结构示意图。
具体实施方式
下面结合实施例对本发明的技术方案及其有益效果做进一步的说明。实施例起解释说明作用,并不对本发明的的保护范围构成限定,任何基于本发明总体构思下的变化和修改应属本发明的保护范围之内。
如图1所示的大规格陶瓷基板的生产线,包括高速分散机1,高速分散机1的出口依次连接有球磨机2、真空脱泡装置3、流延成型装置4、敷粉装置5、烧结装置6和整平装置7,流延成型装置4连接有溶剂回收装置21;所述烧结装置6包括机架8,机架8的机头处设有推机9,机架8上设有炉膛10,炉膛10内设有传动辊11,炉膛10的出口和入口均设有与传动辊11连接的固定板12,固定板12上沿传动辊11传动方向设有两条平行的导轨13;炉膛10内设有加热装置14,炉膛10上方设有排气孔15,排气孔15通过管道连接换热器16,换热器16上连接有进水管道17。所述炉膛10的膛壁由内到外依次为304不锈钢层18、保温层19和201不锈钢层20;所述换热器16为热管换热器。
工作时,将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机2中球磨至组织非常均匀,再用真空脱泡装置3脱去气泡得陶瓷浆料;陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,流延成型的过程中溶剂回收装置21将溶剂回收并返回高速分散机进行再利用,陶瓷生坯用模具冲切成一定形状后再用敷粉装置5敷一层隔粘粉得到坯片;坯片放置在机架8上的固定板12的导轨13上,推机9将坯片推入炉膛10内,坯片在传动辊11的带动下移动,在炉膛10内的加热装置14的工作下加热,产生的废气通过排气孔15进入换热器16,与进水管道17进入换热器16的冷水进行换热,使废气的热量得以利用,产生的热水也可用于其他工序;经过炉膛10烧结的坯片再经过整平装置7整平即得符合生产需要的陶瓷基板。
下列为利用上述生产线生产大规格陶瓷基板的实施例,实施例中所述粘结剂为聚乙烯醇缩丁醛;所述分散剂为蓖麻油;所述增塑剂为邻苯二甲酸二丁酯。
实施例1
大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.04∶0.005∶0.02∶0.3;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝93%、二氧化硅0.5%、氧化镁0.3%、氧化钙0.2%、氧化钇2%、碳酸钡1.0%、氧化锆1%、氧化铋2%。
所述陶瓷粉料中氧化铝的粒度为1.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为1.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1。
大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机2中球磨30h至组织非常均匀,再经真空脱泡装置3在-0.01MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度20℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再经敷粉装置5敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置6的排胶区,在室温-500℃下排胶18h;然后进入烧结装置6的升温高温区,在500-1600℃下烧结20h;接着进入烧结装置6的降温区,在1600-900℃下烧结8h;再进入整平装置7,在1300℃下整平44h即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
实施例2
大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.14∶0.018∶0.06∶0.9;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝96%、二氧化硅0.5%、氧化镁0.3%、氧化钙0.2%、氧化钇1%、碳酸钡1.5%、氧化锆0.05%、氧化铋0.45%。
所述陶瓷粉料中氧化铝的粒度为5.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为4.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1.8。
大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机2中球磨50h至组织非常均匀,再经真空脱泡装置3在0.15MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度50℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再经敷粉装置5敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置6的排胶区,在室温-500℃下排胶22h;然后进入烧结装置6的升温高温区,在500-1600℃下烧结30h;接着进入烧结装置6的降温区,在1600-900℃下烧结15h;再进入整平装置7,在1400℃下整平55h即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
实施例3
大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.1∶0.01∶0.04∶0.6;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝95%、二氧化硅1%、氧化镁1%、氧化钙0.5%、氧化钇1%、碳酸钡0.45%、氧化锆0.05%、氧化铋1%。
所述陶瓷粉料中氧化铝的粒度为3.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为2.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1.5。
大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机2中球磨40h至组织非常均匀,再经真空脱泡装置3在0.1MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度30℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再经敷粉装置5敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置6的排胶区,在室温-500℃下排胶20h;然后进入烧结装置6的升温高温区,在500-1600℃下烧结25h;接着进入烧结装置6的降温区,在1600-900℃下烧结10h;再进入整平装置7,在1350℃下整平50h即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
实施例4
大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.08∶0.012∶0.05∶0.7;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝94%、二氧化硅1%、氧化镁0.5%、氧化钙0.5%、氧化钇0.5%、碳酸钡2.5%、氧化锆0.9%、氧化铋0.1%。
所述陶瓷粉料中氧化铝的粒度为2.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为3.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1.2。
大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机中球磨45h至组织非常均匀,再经真空脱泡装置3在0.05MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度25℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再经敷粉装置5敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置6的排胶区,在室温-500℃下排胶21h;然后进入烧结装置6的升温高温区,在500-1600℃下烧结27h;接着进入烧结装置6的降温区,在1600-900℃下烧结12h;再进入整平装置7,在1370℃下整平即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
实施例5
大规格陶瓷基板,由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.12∶0.009∶0.05∶0.5;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝93%、二氧化硅1.5%、氧化镁1.2%、氧化钙0.3%、氧化钇1.24%、碳酸钡2.5%、氧化锆0.06%、氧化铋0.2%。
所述陶瓷粉料中氧化铝的粒度为2.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为2.5μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1.6。
大规格陶瓷基板的制备方法,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机1中,然后加入分散剂进行预分散,分散后加入球磨机2中球磨35h至组织非常均匀,再在0.05MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度35℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型装置4得厚度均匀、表面光洁、分切成卷的陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再经敷粉装置5敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置6的排胶区,在室温-500℃下排胶19h;然后进入烧结装置6的升温高温区,在500-1600℃下烧结23h;接着进入烧结装置6的降温区,在1600-900℃下烧结9h;再进入整平装置7,在1300-1400℃下整平48h即得平整、光洁、热震性优良的陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
本发明实施例1-5中产品性能的测试方式和测试设备如下:
1、用GF-300D型密度仪测试成瓷密度;
2、用Agilent网络分析仪,采用闭腔法测试圆柱样品的介电性能,测试频率范围在1MHz~20MHz
3、用SANS万能实验机,三点弯曲法测试条样抗弯强度。
4、用耐驰LFA 447热导测试仪测试热导率。
经检测,实施例1-5中陶瓷基板的成瓷密度、介电性能、抗弯强度、热导率数结果详细见下表:
由上表可知,本发明大规格陶瓷基板均匀、致密,具有优良的抗弯强度,良好的导热特性,适用于高温环境;具有耐抗侵蚀和磨耗性,高电气绝缘特性,高温环境下稳定性稳定,可加工成各种复杂形状,适合作为大功率电路的基板。

Claims (7)

1.一种大规格陶瓷基板,其特征在于:由陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂制成,所述陶瓷粉料、粘结剂、分散剂、增塑剂和溶剂的重量比为1∶0.04-0.14∶0.005-0.018∶0.02-0.06∶0.3-0.9;其中所述陶瓷粉料由以下重量百分比的原料组成:氧化铝93-96%、二氧化硅0.5-3%、氧化镁0.3-2%、氧化钙0.2-1%、氧化钇0.1-2%、碳酸钡0.1-2.5%、氧化锆0.05-1%、氧化铋0.1-2%。
2.如权利要求1所述的一种大规格陶瓷基板,其特征在于,所述陶瓷粉料中氧化铝的粒度为1.0-5.0μm,二氧化硅、氧化镁、氧化钙、氧化钇、碳酸钡、氧化锆、氧化铋的粒度均为为1.0-4.0μm;所述溶剂由无水乙醇和丁酮组成,无水乙醇和丁酮的重量比为1∶1-1.8。
3.如权利要求2所述的一种大规格陶瓷基板,其特征在于,所述粘结剂为聚乙烯醇缩丁醛;所述分散剂为蓖麻油;所述增塑剂为邻苯二甲酸二丁酯。
4.权利要求1-3任一所述大规格陶瓷基板的制备方法,其特征在于,包括以下步骤:
(1)将陶瓷粉料、粘结剂、增塑剂和溶液混合后加入高速分散机中,然后加入分散剂进行预分散,分散后加入球磨机中球磨30-50h,再在-0.01-0.15MPa下脱去气泡得陶瓷浆料,陶瓷浆料的温度20-50℃,粘度≤2500mp.s;
(2)将陶瓷浆料经流延成型得陶瓷生坯,陶瓷生坯用模具冲切成一定形状后再敷一层隔粘粉得到坯片;
(3)将坯片放入烧结装置的排胶区,在室温-500℃下排胶18-22h;然后进入烧结装置的升温高温区,在500-1600℃下烧结20-30h;接着进入烧结装置的降温区,在1600-900℃下烧结8-15h;再进入整平装置,在1300-1400℃下整平44-55h即得陶瓷基板;其中所述烧结装置排胶区和升温高温区的升温速率为2-5℃/min,烧结装置降温区的降温速率为2-5℃/min。
5.制备权利要求1-3任一所述的大规格陶瓷基板的生产线,其特征在于,包括高速分散机,高速分散机的出口依次连接有球磨机、真空脱泡装置、流延成型装置、敷粉装置、烧结装置和整平装置;所述烧结装置包括机架,机架的机头处设有推机,机架上设有炉膛,炉膛内设有传动辊,炉膛的出口和入口均设有与传动辊连接的固定板,固定板上沿传动辊传动方向设有两条平行的导轨;炉膛内设有加热装置,炉膛上方设有排气孔,排气孔通过管道连接换热器,换热器上连接有进水管道。
6.如权利要求5所述的制备大规格陶瓷基板的生产线,其特征在于,所述炉膛的膛壁由内到外依次为304不锈钢层、保温层和201不锈钢层;所述换热器为热管换热器。
7.如权利要求6所述的制备大规格陶瓷基板的生产线,其特征在于,所述流延成型装置连接有溶剂回收装置。
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WO2019030025A1 (en) * 2017-08-08 2019-02-14 Morgan Advanced Ceramics, Inc CERAMIC MATERIALS READY FOR LEACHING FOR MOLDING
CN108058264A (zh) * 2017-12-04 2018-05-22 南充三环电子有限公司 一种陶瓷基板坯体的敷粉工艺和系统
CN108863323A (zh) * 2018-08-14 2018-11-23 中铭富驰(苏州)纳米高新材料有限公司 一种用于电子烟雾化器发热模块的基板材料及其制备方法
CN110330317A (zh) * 2019-07-23 2019-10-15 南充三环电子有限公司 一种氧化锆复合氧化铝陶瓷烧结体、其制备方法及应用
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CN112863793A (zh) * 2021-01-12 2021-05-28 南充三环电子有限公司 一种大规格的陶瓷基板
CN116041085A (zh) * 2022-10-25 2023-05-02 山东中为电子科技有限公司 一种可优化陶瓷基板翘曲的多孔陶瓷盖板及其应用
CN116041085B (zh) * 2022-10-25 2024-04-12 山东中为电子科技有限公司 一种可优化陶瓷基板翘曲的多孔陶瓷盖板及其应用
CN115925399A (zh) * 2022-11-01 2023-04-07 南充三环电子有限公司 一种抗热震陶瓷基板及其制备方法
CN115925399B (zh) * 2022-11-01 2023-12-12 南充三环电子有限公司 一种抗热震陶瓷基板及其制备方法

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