CN106816204A - 一种适配氮化铝基材的浆料及其制备方法 - Google Patents
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Abstract
本发明公开了一种适配氮化铝基材的浆料及其制备方法,所述的浆料包括以下质量百分比成分:玻璃粉30‑40%,氧化钌粉24‑42%,有机溶剂混合物28‑37%,助剂1‑3%;所述有机溶剂混合物包括松油醇、丁基卡必醇、丁基卡必醇醋酸酯、邻苯二甲酸二丁酯、柠檬酸三丁酯和乙基纤维素。该浆料的制备方法是按质量百分比,称取玻璃粉、有机溶剂混合物和氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。本发明适配氮化铝基材的浆料采用低软化点的玻璃粉,配以选取的有机溶剂混合物,可降低浆料的烧结温度,所得烧结浆料层具有电阻低、重烧电阻变化率小于3%的优异性能。同时,该浆料不含铅,且具有优异的丝印性能,完全适合用作大功率密度(>80W/cm2)发热器件。
Description
技术领域
本发明涉及一种浆料,尤其涉及一种适配氮化铝基材的浆料及其制备方法。
背景技术
氮化铝材料具有优异的导热和电绝缘性能,因此,它成为新兴的电热发热器件用基材的重要选择。相对于不锈钢基材,氮化铝材料的优势明显,不需要覆盖介质层就能直接使用,极高的导热系数意味着基材在极短时间内便能受热均匀。然而,一些条件下,需要在氮化铝材料涂覆含有氧化钌的浆料涂层,但在750℃以上时,氮化铝会与氧化钌产生化学反应释放出氮气,因此,现有的含有氧化钌的浆料难以适用于氮化铝基材使用工艺(850℃左右)。
发明内容
未解决上述问题,本发明提供一种适配氮化铝基材的浆料及其制备方法,具体方案如下:
一种适配氮化铝基材的浆料,包括以下质量百分比成分:
所述玻璃粉的软化点低于450℃,优选为420-450℃;所述有机溶剂混合物包括松油醇、丁基卡必醇、丁基卡必醇醋酸酯、邻苯二甲酸二丁酯、柠檬酸三丁酯和乙基纤维素,粘度为20-50Pa·s。
进一步的,所述玻璃粉包括二氧化硅、氧化铋、氧化硼、氧化钡和三氧化二铁;所述玻璃粉粒度10μm以内。
优选的,所述玻璃粉由以下质量百分比成分:
优选的,所述有机溶剂混合物由以下质量百分比成分组成:
优选的,所述氧化钌粉的纯度均大于99.9%,粒度小于8μm。
进一步的,所述助剂包括分散剂、润湿剂和流平剂;优选的,所述分散剂、润湿剂和流平剂在浆料中的质量百分比分别为:
分散剂 0.5-1.5%
润湿剂 0.5-1.5%
流平剂 0.3-0.7%。
优选的,所述浆料固含量为65%-73%;烧结温度为650-750℃,优选为700℃。
上述适配氮化铝基材的浆料的制备方法包括以下步骤:
A)配制有机相:按质量百分比,称取松油醇、丁基卡必醇、丁基卡必醇醋酸酯、邻苯二甲酸二丁酯、柠檬酸三丁酯和乙基纤维素,置于分散罐中搅拌分散4h以上,得到有机溶剂混合物。
B)配制浆料:按质量百分比,称取玻璃粉、有机溶剂混合物、助剂和氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
进一步的,所述步骤B)中,玻璃粉的制备方法如下:按质量百分比,将18-26%的二氧化硅、45-58%的氧化铋、10-15%的氧化硼、14-20%的氧化钡、3-6%的三氧化二铁混匀后升温至1100-1500℃熔融保温15-30min,然后将熔融液水淬得到玻璃料,再将玻璃料粉碎并球磨成所需粒度的玻璃粉。
本发明适配氮化铝基材的浆料采用低软化点(450℃以下)的玻璃粉,配以选取的有机溶剂混合物,可降低浆料的烧结温度。该浆料丝印于氮化铝片状陶瓷表面,经过650-750℃烧结5-20min,所得烧结浆料层具有电阻低、重烧(650-750℃烧结5-20min)后电阻变化率小于3%的优异性能。同时,该浆料不含铅,且具有优异的丝印性能,完全适合用作大功率密度(>80W/cm2)发热器件。
具体实施方式
为了更充分理解本发明的技术内容,下面结合具体实施例对本发明的技术方案进一步介绍和说明。
实施例1
按以下步骤制备适配氮化铝基材的浆料。
制备玻璃粉:按质量百分比,称取分析纯级18-26%的二氧化硅、45-58%的氧化铋、10-15%的氧化硼、14-20%的氧化钡、3-6%的三氧化二铁混匀后转移至刚玉坩埚或铂金坩埚,置于箱式电阻炉中升温至1100-1500℃熔融保温15-30min,然后将熔融液水淬得到玻璃料,再将玻璃料粉碎并球磨成所需粒度10μm以内的玻璃粉。
配制有机相:按质量百分比,称取15-25%的松油醇、20-30%的丁基卡必醇、30-50%的丁基卡必醇醋酸酯、8-15%的邻苯二甲酸二丁酯、8-12%的柠檬酸三丁酯和4-8%的乙基纤维素,置于分散罐中搅拌分散4h以上,得到透明的有机溶剂混合物。
配制浆料:按质量百分比,称取30-40%制备的玻璃粉、28-37%配置的有机溶剂混合物、1-3%助剂和24-42%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
按以下步骤制备玻璃粉、有机溶剂混合物和助剂,用于制备实施例2-6的适配氮化铝基材的浆料。
制备玻璃粉:按质量百分比,称取分析纯级20%的二氧化硅、50%的氧化铋、10%的氧化硼、15%的氧化钡、5%的三氧化二铁混匀后转移至刚玉坩埚或铂金坩埚,置于箱式电阻炉中升温至1150℃熔融保温20min,然后将熔融液水淬得到玻璃料,再将玻璃料粉碎并球磨成所需粒度10μm以内的玻璃粉。
配制有机相:按质量百分比,称取20%的松油醇、25%的丁基卡必醇、30%的丁基卡必醇醋酸酯、10%的邻苯二甲酸二丁酯、10%的柠檬酸三丁酯和5%的乙基纤维素,置于分散罐中搅拌分散4h,得到透明的有机溶剂混合物。
制备助剂:将分散剂、润湿剂和流平剂按质量比2:2:1混合配置成助剂。
实施例2
按质量百分比,称取40%上述制备的玻璃粉、33%上述配置的有机溶剂混合物、3%助剂和24%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
实施例3
按质量百分比,称取38%上述制备的玻璃粉、33%上述配置的有机溶剂混合物、2%助剂和27%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
实施例4
按质量百分比,称取35%上述制备的玻璃粉、32.5%上述配置的有机溶剂混合物、1.5%助剂和31%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
实施例5
按质量百分比,称取32%上述制备的玻璃粉、31.5%上述配置的有机溶剂混合物、1.5%助剂和35%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
实施例6
按质量百分比,称取30%上述制备的玻璃粉、29%上述配置的有机溶剂混合物、1.0%助剂和40%的纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
将上述实施例2-6制备的浆料分别丝印于氮化铝片状陶瓷表面,经过700℃烧结10min,冷却后测定浆料层的电阻R1;测定电阻后,再将带有烧结浆料层的氮化铝片状陶瓷经过700℃烧结10min重烧,冷却后测定浆料层的电阻R2;计算重烧后电阻变化率=(R2-R1)/R1*100%;具体结果如表1所示:
表1
试验一:玻璃粉软化点试验
按表2试验例1-10所示的成分质量比称取分析纯级的二氧化硅、氧化铋、氧化硼、氧化钡、三氧化二铁混匀后转移至刚玉坩埚或铂金坩埚,置于箱式电阻炉中升温至1150℃熔融保温20min,然后将熔融液水淬得到玻璃料,再将玻璃料粉碎并球磨成所需粒度10μm以内的玻璃粉。分别测定试验例1-10所得玻璃粉的软化点,结果如表2所示:
表2
试验二:高软化点玻璃粉制备浆料的烧结试验
选取软化点为550℃的玻璃粉,玻璃粉粒度10μm以内。
按以下步骤制备有机溶剂混合物和助剂,用于制备试验例11-16的的浆料。
配制有机相:按质量百分比,称取20%的松油醇、25%的丁基卡必醇、30%的丁基卡必醇醋酸酯、10%的邻苯二甲酸二丁酯、10%的柠檬酸三丁酯和5%的乙基纤维素,置于分散罐中搅拌分散4h,得到透明的有机溶剂混合物。
制备助剂:将分散剂、润湿剂和流平剂按质量比2:2:1混合配置成助剂。
按表3试验例11-16所示的成分质量比称取高软化点玻璃粉、有机溶剂混合物、助剂和纯度大于99.9%、粒度小于8μm的氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,分别得到对应试验例11-16的浆料,将上述试验例11-16制备的浆料分别丝印于氮化铝片状陶瓷表面进行烧结,分别测定试验例11-16所得浆料的烧结温度,结果如表3所示:
表3
表3的测试结果可知,采用高软化点玻璃粉,则必须要提高烧结温度,也就是要超过750℃,然而750℃以上氮化铝和氧化钌会发生化学反应,所以高软化点玻璃粉在该体系中是无法被采用的。所以,本发明的玻璃粉是在结合氮化铝基材和氧化钌特征的基础上开发的,而高软化点玻璃粉不能满足该浆料体系的特征需求。
以上所述仅以实施例来进一步说明本发明的技术内容,以便于读者更容易理解,但不代表本发明的实施方式仅限于此,任何依本发明所做的技术延伸或再创造,均受本发明的保护。
Claims (10)
1.一种适配氮化铝基材的浆料,其特征在于,包括以下质量百分比成分:
所述玻璃粉的软化点低于450℃;所述有机溶剂混合物包括松油醇、丁基卡必醇、丁基卡必醇醋酸酯、邻苯二甲酸二丁酯、柠檬酸三丁酯和乙基纤维素。
2.根据权利1所述的适配氮化铝基材的浆料,其特征在于:所述玻璃粉包括二氧化硅、氧化铋、氧化硼、氧化钡和三氧化二铁;所述玻璃粉粒度10μm以内。
3.根据权利2所述的适配氮化铝基材的浆料,其特征在于:所述玻璃粉由以下质量百分比成分:
4.根据权利3所述的适配氮化铝基材的浆料,其特征在于:所述有机溶剂混合物由以下质量百分比成分组成:
5.根据权利4所述的适配氮化铝基材的浆料,其特征在于:所述氧化钌粉的纯度均大于99.9%,粒度小于8μm。
6.根据权利5所述的适配氮化铝基材的浆料,其特征在于:所述助剂包括分散剂、润湿剂和流平剂。
7.根据权利6所述的适配氮化铝基材的浆料,其特征在于:所述分散剂、润湿剂和流平剂在浆料中的质量百分比分别为:
分散剂 0.5-1.5%
润湿剂 0.5-1.5%
流平剂 0.3-0.7%。
8.根据权利7所述的适配氮化铝基材的浆料,其特征在于:所述浆料固含量为65%-73%。
9.一种如权利要求1-8任意一项所述适配氮化铝基材的浆料的制备方法,其特征在于,包括以下步骤:
A)配制有机相:按质量百分比,称取松油醇、丁基卡必醇、丁基卡必醇醋酸酯、邻苯二甲酸二丁酯、柠檬酸三丁酯和乙基纤维素,置于分散罐中搅拌分散4h以上,得到有机溶剂混合物。
B)配制浆料:按质量百分比,称取玻璃粉、有机溶剂混合物、助剂和氧化钌粉,经过搅拌、三辊研磨、过滤及脱泡工序,得到所需的浆料。
10.根据权利9所述适配氮化铝基材的浆料的制备方法,其特征在于,所述步骤B)中,玻璃粉的制备方法如下:按质量百分比,将18-26%的氧化硅、45-58%的氧化铋、10-15%的氧化硼、14-20%的氧化钡、3-6%的三氧化二铁混匀后升温至1100-1500℃熔融保温15-30min,然后将熔融液水淬得到玻璃料,再将玻璃料粉碎并球磨成所需粒度的玻璃粉。
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CN114538932A (zh) * | 2022-03-21 | 2022-05-27 | 福建华清电子材料科技有限公司 | 一种共烧氮化铝陶瓷基板的制备方法 |
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US6406646B1 (en) * | 1999-12-17 | 2002-06-18 | Daejoo Fine Chemical Co., Ltd. | Resistive paste for the formation of electrically heat-generating thick film |
US20030000938A1 (en) * | 2000-12-01 | 2003-01-02 | Yanling Zhou | Ceramic heater, and ceramic heater resistor paste |
US20140110637A1 (en) * | 2010-12-28 | 2014-04-24 | E I Du Pont De Nemours And Company | Thick film resistive heater compositions comprising ag & ruo2, and methods of making same |
CN105810291A (zh) * | 2016-04-07 | 2016-07-27 | 东莞珂洛赫慕电子材料科技有限公司 | 一种中低阻段大功率厚膜电路稀土电阻浆料及其制备方法 |
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US6406646B1 (en) * | 1999-12-17 | 2002-06-18 | Daejoo Fine Chemical Co., Ltd. | Resistive paste for the formation of electrically heat-generating thick film |
US20030000938A1 (en) * | 2000-12-01 | 2003-01-02 | Yanling Zhou | Ceramic heater, and ceramic heater resistor paste |
US20140110637A1 (en) * | 2010-12-28 | 2014-04-24 | E I Du Pont De Nemours And Company | Thick film resistive heater compositions comprising ag & ruo2, and methods of making same |
CN105810291A (zh) * | 2016-04-07 | 2016-07-27 | 东莞珂洛赫慕电子材料科技有限公司 | 一种中低阻段大功率厚膜电路稀土电阻浆料及其制备方法 |
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CN114538932A (zh) * | 2022-03-21 | 2022-05-27 | 福建华清电子材料科技有限公司 | 一种共烧氮化铝陶瓷基板的制备方法 |
CN114538932B (zh) * | 2022-03-21 | 2022-12-06 | 福建华清电子材料科技有限公司 | 一种共烧氮化铝陶瓷基板的制备方法 |
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