CN114031402A - 一种低温烧结微波介质材料MgZrNb2O8及其制备方法 - Google Patents
一种低温烧结微波介质材料MgZrNb2O8及其制备方法 Download PDFInfo
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Abstract
本发明属于电子材料及其制造领域,具体提供一种低温烧结微波介质材料MgZrNb2O8及其制备方法,用以解决微波介质材料MgZrNb2O8烧结温度过高、无法与Ag电极共烧形成LTCC陶瓷的问题。本发明通过在预合成MgZrNb2O8基料中添加ZnO‑B2O3玻璃作为助烧剂,大大降低微波介质材料MgZrNb2O8的烧结温度至925~975℃,进而实现与Ag电极共烧形成LTCC陶瓷;并且,微波介电性能仍然优异:介电常数为10~21、Q×f值为33000~40000GHz、谐振频率温度系数为‑80~‑70ppm/℃,在微波介质陶瓷中具有广阔的应用场景。另外,本发明提供低温烧结微波介质材料的制备方法,采用的传统固相法,工艺简单,易于工业化生产,并且低温烧结具有节省能源的显著优势。
Description
技术领域
本发明属于电子材料及其制造领域,涉及低温烧结微波介质材料,具体提供一种低温烧结微波介质材料MgZrNb2O8及其制备方法。
背景技术
低温烧结微波介质材料是目前微波元器件的研究热点,但是微波介质材料的烧结温度普遍偏高,如何降低烧结温度实现与Ag共烧成为研究难点,铌酸盐因其优异的微波性能吸引了众多国内外学者的广泛研究。
S.D.Ramarao,V.R.K.Murthy等人在文献“Crystal structure refinement andmicrowave dielectric properties of new low dielectric loss AZrNb2O8(A:Mn,Zn,Mgand Co)ceramics”中于1500℃的烧结温度下制备出MgZrNb2O8微波介质材料,其性能为εr=9.6、Q×f=58500GHz、τf=-31.5ppm/℃;但是,其烧结温度非常高(1500℃),根本无法与低电阻率的金属导体(银、铜等)共同烧结。
为了降低烧结温度,H.T.Wu等人在文献“Effect of H3BO3 addition on thesintering behavior and microwave dielectric properties of wolframite-typeMgZrNb2O8 ceramics”中通过在MgZrNb2O8陶瓷中添加H3BO3将烧结温度降低到1200℃,具体性能如下:εr=23.72、Q×f=58930、τf=-13.19ppm/℃;Xin Tang等人在文献“Low-Temperature Sintering and Microwave Dielectric Properties of MgZrNb2O8Ceramics with BaCu(B2O5)Addition”中通过在MgZrNb2O8陶瓷中添加BaCu(B2O5)成功地将烧结温度从1300℃降低到1100℃,在1100℃烧结温度下其微波性能为:εr=25.96、Q×f=65064GHz、τf=-47ppm/℃。上述两种方法虽然使MgZrNb2O8陶瓷的烧结温度有所降低,但是均没有将烧结温度降低到950℃,仍然没有办法与Ag电极共烧从而形成LTCC陶瓷。
基于此,本发明提供了一种低温烧结微波介质材料MgZrNb2O8及其制备方法。
发明内容
本发明的目的在于针对微波介质材料MgZrNb2O8烧结温度过高、无法与Ag电极共烧形成LTCC陶瓷的问题,提供一种低温烧结微波介质材料MgZrNb2O8及其制备方法,通过在预合成MgZrNb2O8基料中添加ZnO-B2O3玻璃作为助烧剂,大大降低微波介质材料MgZrNb2O8的烧结温度至925~975℃,进而实现与Ag电极共烧形成LTCC陶瓷。
为实现上述目的,本发明采用的技术方案如下:
一种低温烧结微波介质材料,其特征在于,所述低温烧结微波介质材料由MgZrNb2O8与ZnO-B2O3玻璃组成,其中,ZnO-B2O3玻璃占总料的比例为20~40wt%,MgZrNb2O8占总料的比例为60~80wt%。
进一步的,上述低温烧结微波介质材料MgZrNb2O8的制备方法,其特征在于,包括以下步骤:
步骤1:将分析纯4MgCO3·Mg(OH)2·5H2O、ZrO2、Nb2O5粉体按化学式MgZrNb2O8的摩尔比进行配料;
步骤2:将混合料球磨、烘干、过筛,得到干燥粉体;
步骤3:将步骤2得干燥粉体置于高温烧结炉中,以3min/℃升温速率升温至1200℃,预烧4小时,获得主晶相MgZrNb2O8的预烧料;
步骤4:将纯ZnO与H3BO3粉体按照质量比为3:5通过玻璃加工工艺制备成ZnO-B2O3玻璃;
步骤5:将预烧料与ZnO-B2O3玻璃混合,并再次球磨、烘干、过筛,得干燥粉体;
步骤6:将步骤5得干燥粉体用丙烯酸造粒,并在10~20MPa下压制成生坯;
步骤7:将生坯置于烧结炉中,以3min/℃升温速率升温至925~975℃,烧结4小时,得到所述的微波介质材料。
进一步的,所述步骤2与步骤5中,球磨工艺具体为:按照原料:去离子水:锆球为1:2:5的质量比将混合料于尼龙罐中球磨6小时,烘干工艺具体为:100℃烘干。
本发明的有益效果在于:
1.本发明提供了一种低温烧结微波介质材料,通过在预合成MgZrNb2O8基料中添加ZnO-B2O3玻璃作为助烧剂,由于在烧结过程中低熔点氧化物B2O3在800℃形成液相加快传质,从而加快晶粒生长,在主晶相MgZrNb2O8外引入新的次晶相Zn3(BO2)2与Zn4O(BO2)6,极大的降低了烧结温度,实现了925~975℃的低温烧结,尤其是950℃的低温烧结,能够实现与Ag电极共烧形成LTCC陶瓷。
2.本发明提供的低温烧结微波介质材料,由于助烧剂的引入,微波介质材料的微波介电性能(如Q×f值)存在一定下降,但微波介电性能仍然优异:介电常数为10~21、Q×f值为33000~40000GHz、谐振频率温度系数为-80~-70ppm/℃,在微波介质陶瓷中具有广阔的应用场景:如在MgZrNb2O8基料中添加30wt%的ZnO-B2O3时能够在950℃烧结并获得Q×f值为39325GHz。
3.本发明提供的低温烧结微波介质材料,采用的传统固相法,工艺简单,易于工业化生产,并且低温烧结具有节省能源的显著优势。
附图说明
图1为实施例3中950℃烧结微波介质材料MgZrNb2O8的XRD图。
图2为实施例3中950℃烧结微波介质材料MgZrNb2O8的SEM图。
图3为实施例5中975℃烧结微波介质材料MgZrNb2O8的XRD图。
图4为实施例5中975℃烧结微波介质材料MgZrNb2O8的SEM图。
具体实施方式
下面结合附图和实施例对本发明做进一步详细说明。
本发明共提供六个实施例,每个实施例中,低温烧结微波介质材料由MgZrNb2O8与Zn O-B2O3玻璃组成,其中,ZnO-B2O3玻璃为xwt%,x=25、30、35;低温烧结微波介质材料均采用相同制备方法制备,具体包括以下步骤:
步骤1:将分析纯4MgCO3·Mg(OH)2·5H2O、ZrO2、Nb2O5粉体按化学式MgZrNb2O8的摩尔比进行配料;
步骤2:按照原料:去离子水:锆球为1:2:5的质量比将混合料于尼龙罐中球磨6小时,然后料浆在100℃烘干,并将干燥粉体通过80目的筛网;
步骤3:将步骤2干燥粉体置于烧结炉中,得在1200℃预烧4小时,获得主晶相为MgZrNb2O8的预烧料;
步骤4:将纯ZnO与H3BO3粉体按照质量比为3:5通过常规的玻璃加工工艺制备成ZnO-B2O3玻璃;
步骤5:将预烧料与25~35wt%的ZnO-B2O3玻璃混合;按照预烧料:锆球:去离子水为1:5:2的质量比加工混合料于尼龙罐中球磨4小时,然后料浆在100℃烘干;
步骤6:将干燥粉体用丙烯酸造粒,并在10~20MPa下压制成生坯;
步骤7:将生坯在烧结炉中于925~975℃烧结4小时,得到所述的微波介质材料。
上述六个实施例的具体工艺参数及微波介电性能如下表所示:
编号 | 组成 | 烧结温度 | 烧结时长 | ε<sub>r</sub> | Q×f(GHz) | τ<sub>f</sub>(ppm/℃) |
实施例1 | 0wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 1340 | 4 | 26.63 | 53195 | -55.80 |
实施例2 | 25wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 950 | 4 | 18.94 | 36742 | -72.12 |
实施例3 | 30wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 950 | 4 | 20.47 | 39325 | -74.65 |
实施例4 | 35wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 950 | 4 | 19.24 | 33742 | -78.54 |
实施例5 | 25wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 975 | 4 | 19.87 | 36110 | -72.46 |
实施例6 | 30wt.%ZnO-B<sub>2</sub>O<sub>3</sub> | 975 | 4 | 18.29 | 34197 | -75.03 |
上述六个实施例中,实施例3制备得低温烧结微波介质材料的XRD图如图1所示、SEM图如图2所示,由图可见,所述微波介质材料的主晶相为MgZrNb2O8,添加ZnO-B2O3后形成少量的Zn3(BO2)2和Zn4O(BO2)6;实施例5制备得低温烧结微波介质材料的XRD图如图3所示、SEM图如图4所示,其结果呈现与图1与图2基本相同。
以上所述,仅为本发明的具体实施方式,本说明书中所公开的任一特征,除非特别叙述,均可被其他等效或具有类似目的的替代特征加以替换;所公开的所有特征、或所有方法或过程中的步骤,除了互相排斥的特征和/或步骤以外,均可以任何方式组合。
Claims (3)
1.一种低温烧结微波介质材料,其特征在于,所述低温烧结微波介质材料由MgZrNb2O8与ZnO-B2O3玻璃组成,其中,
ZnO-B2O3玻璃占总料的比例为20~40wt%,
MgZrNb2O8占总料的比例为60~80wt%。
2.按权利要求1所述低温烧结微波介质材料的制备方法,其特征在于,包括以下步骤:
步骤1:将分析纯4MgCO3·Mg(OH)2·5H2O、ZrO2、Nb2O5粉体按化学式MgZrNb2O8的摩尔比进行配料;
步骤2:将混合料球磨、烘干、过筛,得到干燥粉体;
步骤3:将步骤2得干燥粉体置于高温烧结炉中,以3min/℃升温速率升温至1200℃,预烧4小时,获得主晶相MgZrNb2O8的预烧料;
步骤4:将纯ZnO与H3BO3粉体按照质量比为3:5通过玻璃加工工艺制备成ZnO-B2O3玻璃;
步骤5:将预烧料与ZnO-B2O3玻璃混合,并再次球磨、烘干、过筛,得干燥粉体;
步骤6:将步骤5得干燥粉体用丙烯酸造粒,并在10~20MPa下压制成生坯;
步骤7:将生坯置于烧结炉中,以3min/℃升温速率升温至925~975℃,烧结4小时,得到所述的微波介质材料。
3.按权利要求2所述低温烧结微波介质材料的制备方法,其特征在于,所述步骤2与步骤5中,球磨工艺具体为:按照原料:去离子水:锆球为1:2:5的质量比将混合料于尼龙罐中球磨6小时,烘干工艺具体为:100℃烘干。
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