WO2021189506A1 - 一种介电常数系列可调的低温共烧电介质材料及其制备方法 - Google Patents

一种介电常数系列可调的低温共烧电介质材料及其制备方法 Download PDF

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WO2021189506A1
WO2021189506A1 PCT/CN2020/082252 CN2020082252W WO2021189506A1 WO 2021189506 A1 WO2021189506 A1 WO 2021189506A1 CN 2020082252 W CN2020082252 W CN 2020082252W WO 2021189506 A1 WO2021189506 A1 WO 2021189506A1
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temperature
low
fired
silicon
dielectric material
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PCT/CN2020/082252
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French (fr)
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沓世我
王小舟
陈涛
刘芸
弗朗科姆·特里·詹姆士
付振晓
曹秀华
胡春元
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广东风华高新科技股份有限公司
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Priority to JP2021529074A priority Critical patent/JP7333147B2/ja
Priority to KR1020217015099A priority patent/KR102621058B1/ko
Priority to US17/246,742 priority patent/US20210309578A1/en
Publication of WO2021189506A1 publication Critical patent/WO2021189506A1/zh

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Definitions

  • the invention belongs to the technical field of ceramic materials, and specifically relates to a low-temperature co-fired dielectric material with adjustable dielectric constant series and a preparation method thereof.
  • the research on zirconia in low-temperature co-fired ceramic materials mainly focuses on the glass-ceramic system, that is, zirconia is used as a nucleating agent to control the crystallization of glass.
  • zirconia is used as a nucleating agent to control the crystallization of glass.
  • the content of zirconia added is usually 1%-10%, and there is generally an optimal value. If it deviates from this optimal value, it will cause obvious performance degradation, so the dielectric constant of the sample is relatively single.
  • the glass/ceramic composite system the glass is mainly used to reduce the sintering temperature, and the ceramic material mainly determines the performance after sintering. I. Choi et al.
  • the main phase is prepared by the fusion-quenching method to co-fire, and the obtained sample has a dielectric constant of about 9 and a dielectric loss.
  • the dielectric constant of these products is relatively single, due to the high glass phase
  • the dielectric composition is too high, so that the entire material system cannot achieve continuous control of the dielectric constant.
  • the integrated module of low-temperature co-fired ceramic materials often contains materials with different dielectric constants.
  • This method has two main drawbacks: one is because of some volatile components in the glass, such as B 2 O 3 and Bi 2 O 3 make the obtained glass powder deviate from the originally designed composition, which leads to the performance of the final sample is not as good as expected; the other is that this method is not suitable for preparing all glasses, such as CaO- SiO 2 glass etc.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a low-temperature co-fired dielectric material with adjustable dielectric constant series and a preparation method thereof.
  • the technical solution adopted by the present invention is: a low-temperature co-fired dielectric material with adjustable dielectric constant series, the low-temperature co-fired dielectric material includes a main phase of zirconia and a silicon-based amorphous phase filler, so The weight ratio of the main phase of zirconia to the silicon-based amorphous phase filler is: the main phase of zirconia: the silicon-based amorphous phase filler is 40-65:35-60; the SiO 2 is in the silicon-based amorphous phase filler.
  • the weight percentage content in the phase filler is ⁇ 50%.
  • the dielectric constant of the low-temperature co-fired dielectric material composed of the main phase of zirconia and the silicon-based amorphous phase filler is enhanced, and the dielectric constant can be adjusted in the range of 7-12.
  • the low-temperature co-fired dielectric material contains the following components by weight percentage: ZrO 2 40%-65%, SiO 2 27.03%-46.3%, Na 2 O 0.27%-0.46%, K 2 O 1.23% ⁇ 2.11%, CaO 0.73% ⁇ 1.26% and B 2 O 3 5.73% ⁇ 9.83%.
  • This material system has similar sintering characteristics and can avoid defects such as spalling and warping during co-firing.
  • the main phase of zirconium oxide is crystalline or amorphous.
  • the dielectric constants of monoclinic ZrO 2 ( ⁇ 20) and amorphous ZrO 2 ( ⁇ 22) are close. Choosing either or both can achieve the regulation of the dielectric constant between 7 and 12.
  • the silicon-based amorphous phase filler is glass or a mixture of amorphous phases.
  • the use of silicon-based amorphous phase does not need to go through a high-temperature melting process, which can avoid the volatilization of B 2 O 3.
  • the weight percentage content of Al element in the silicon-based amorphous phase filler is less than or equal to 0.01%.
  • the particle size of the ZrO 2 is 0.5 ⁇ m-10 ⁇ m.
  • the specific surface area within the particle size range of ZrO 2 is suitable, and the preparation of low-temperature co-fired dielectric materials with adjustable dielectric constant series can be realized at this ratio. More preferably, the particle size of the ZrO 2 is 1 ⁇ m to 5 ⁇ m.
  • the silicon-based amorphous phase filler can be prepared by mixing various components, or can be prepared by a wet chemical method.
  • the preparation method of the silicon-based amorphous phase filler includes the following steps:
  • the composition of the glass prepared by the traditional melting-quenching method often deviates from the originally designed glass composition. This is mainly due to the volatilization of some volatile components in the glass during the high-temperature melting process, such as B 2 O 3 and Bi 2 O 3 .
  • the above method can be used to synthesize silicon-based amorphous phase fillers under low temperature conditions ( ⁇ 700°C), which can effectively inhibit the volatilization of these components, so that the synthesized silicon-based amorphous phase fillers are closer to the designed components.
  • the salts corresponding to other elements other than silicon involved in the preparation method of the silicon-based amorphous phase filler are preferably soluble salts, and may be nitrates, acetates, etc. of Na, K, Ca, and B.
  • the volume ratio of the ethyl orthosilicate, alcohol and deionized water is 1:5-15:1.
  • the object of the present invention is also to provide a preparation method of the low-temperature co-fired dielectric material with adjustable dielectric constant series, the preparation method includes the following steps: a silicon-based amorphous phase filler and a main phase of zirconia are mixed and ball milled in proportion 6-24 hours, and then sintered at 800-900°C to obtain the low-temperature co-fired ceramic material with adjustable dielectric constant series.
  • the present invention provides a low-temperature co-fired dielectric material with adjustable dielectric constant series.
  • the present invention controls the ratio of the main phase of zirconia and the silicon-based amorphous phase filler, and the dielectric of the obtained material is
  • the constant is continuously adjustable in a wide range of 7-12, and the dielectric loss can be as low as 0.1%@1MHz.
  • This material system can be sintered at 800-900°C, can be co-fired compatible with silver electrodes, and can be used as a low-temperature co-fired dielectric material.
  • Figure 1 shows the dielectric properties of the samples described in Examples 1 to 4 (@1MHz);
  • picture (a) is the cross-section of the dry-pressed green sheet of silver electrode and powder in Example 3 after being co-fired at 850°C.
  • the SEM picture (b) is the silver content at each point in the picture (a).
  • An embodiment of the preparation method of the low-temperature co-fired dielectric material of the present invention includes the following steps:
  • the dielectric properties of the low-temperature co-fired dielectric material prepared in this embodiment are shown in FIG. 1, the dielectric constant is 8.89@1MHz, and the dielectric loss is 0.0012@1MHz.
  • the low-temperature co-fired dielectric material described in this embodiment and the silver electrode are tightly bonded after being co-fired, and no delamination, warpage, etc. occur.
  • An embodiment of the preparation method of the low-temperature co-fired dielectric material of the present invention includes the following steps:
  • the dielectric properties of the low-temperature co-fired dielectric material prepared in this embodiment are shown in FIG. 1, the dielectric constant is 10.48@1MHz, and the dielectric loss is 0.0011@1MHz.
  • the low-temperature co-fired dielectric material described in this embodiment and the silver electrode are tightly bonded after being co-fired, and no delamination, warpage, etc. occur.
  • An embodiment of the preparation method of the low-temperature co-fired dielectric material of the present invention includes the following steps:
  • the dielectric properties of the low-temperature co-fired dielectric material prepared in this embodiment are shown in FIG. 1, the dielectric constant is 11.11@1MHz, and the dielectric loss is 0.0006@1MHz.
  • An embodiment of the preparation method of the low-temperature co-fired dielectric material of the present invention includes the following steps:
  • the dielectric properties of the low-temperature co-fired dielectric material prepared in this embodiment are shown in FIG. 1, and the dielectric loss is 0.0004@1MHz.
  • the low-temperature co-fired dielectric material described in this embodiment and the silver electrode are tightly bonded after being co-fired, and no delamination, warpage, etc. occur.

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Abstract

一种介电常数系列可调的低温共烧电介质材料，所述低温共烧电介质材料包含氧化锆主相和硅基非晶相填充料，所述氧化锆主相和硅基非晶相填充料的重量之比为：氧化锆主相：硅基非晶相填充料＝40～65：35～60；所述SiO 2在所述硅基非晶相填充料中的重量百分含量≥50％。通过控制氧化锆主相和硅基非晶相填充料的比例，所得材料的介电常数在7～12较宽的范围内连续可调，而且介电损耗可低至0.1％@1MHz。该材料体系可在800～900℃烧结，能够与银电极兼容共烧，可以用作低温共烧电介质材料。还公开了所述介电常数系列可调的低温共烧电介质材料的制备方法。

Description

一种介电常数系列可调的低温共烧电介质材料及其制备方法 技术领域
本发明属于陶瓷材料技术领域，具体涉及一种介电常数系列可调的低温共烧电介质材料及其制备方法。
背景技术
随着半导体技术的发展，主动元件的封装已经得到了快速的发展。然而在实际器件应用中，被动元件(电容、电感等)的数量通常比主动元件要多十倍以上。如此大的被动原件的数量制约着器件的小型化发展。低温共烧陶瓷技术因其独特的三维立体结构，已经成为目前最有前景的被动元件封装技术。常用的低温共烧陶瓷材料主要基于微晶玻璃体系和玻璃/陶瓷复合体系。目前对于氧化锆在低温共烧陶瓷材料中的研究主要集中在微晶玻璃体系，即氧化锆作为成核剂来控制玻璃的晶化。对于不同组分的玻璃，加入的氧化锆的含量通常在1％～10％，而且一般存在最佳值。如果偏离这个最佳值，则会引起明显的性能退化，所以样品的介电常数相对单一。对于玻璃/陶瓷复合体系，其中的玻璃主要用来降低烧结温度，而陶瓷材料主要决定烧结后的性能。I.Choi等人曾尝试将ZrO 2作为陶瓷填充材料与钙铝硼硅酸盐玻璃主相(由熔融-淬火法制备主相共烧，所得的样品介电常数在9左右，而且介电损耗偏高(tanδ＝0.006)。总的来说，尽管有研究者对氧化锆在低温共烧陶瓷中的应用做了一些研究和探索，但这些产品的介电常数相对单一，由于玻璃相的高介电成分太高，从而使整个材料系统无法实现介电常数可连续调控。在低温共烧陶瓷材料的集成模块中常包含不同介电常数的材料，如果这些材料都是基于不同的材料体系，那么在共烧时由于它们之间烧结特性的不同，往往会引发层裂、翘曲等缺陷。但如果能基于同一材料体系开发出介电常数系列可调的配方，则可以有效地避免这类问题。另外，目前基于玻璃/陶瓷复合的LTCC材料中，几乎所有的玻璃都是由熔融-淬火法制得。这种方法有两个主要的弊端：一是因为玻璃中一些易挥发的组分，比如B 2O 3和Bi 2O 3，使得到的玻璃粉与最初设计的组分有偏差，进而导致最终样 品性能不及预期效果；另一个是这种方法并不适用于制备所有玻璃，比如CaO-SiO 2玻璃等。
发明内容
本发明的目的在于克服现有技术存在的不足之处而提供一种介电常数系列可调的低温共烧电介质材料及其制备方法。
为实现上述目的，本发明采取的技术方案为：一种介电常数系列可调的低温共烧电介质材料，所述低温共烧电介质材料包含氧化锆主相和硅基非晶相填充料，所述氧化锆主相和硅基非晶相填充料的重量之比为：氧化锆主相：硅基非晶相填充料40～65：35～60；所述SiO 2在所述硅基非晶相填充料中的重量百分含量≥50％。
氧化锆主相和硅基非晶相填充料组成的低温共烧电介质材料介电常数可调性增强，可实现介电常数在7～12的调控。
优选地，所述低温共烧电介质材料包含以下重量百分含量的组分：ZrO 240％～65％、SiO 227.03％～46.33％、Na 2O 0.27％～0.46％、K 2O 1.23％～2.11％、CaO 0.73％～1.26％和B 2O 35.73％～9.83％。该材料体系具有相似的烧结特性，共烧时可以避免层裂、翘曲等缺陷。
优选地，所述氧化锆主相为晶态或者非晶态。单斜ZrO 2(～20)和非晶ZrO 2(～22)的介电常数接近，选择任意一种或两种都能实现介电常数在7～12的调控。
优选地，所述硅基非晶相填充料为玻璃或者非晶相的混合物。选用硅基非晶相则不需要经过高温熔融过程，可以避免B 2O 3的挥发。
优选地，所述硅基非晶相填充料中，Na和K的原子比为：Na/K＝1:2～4。在上述比值下可以减少介电损耗。
优选地，所述硅基非晶相填充料中Al元素的重量百分含量≤0.01％。
优选地，所述ZrO 2的颗粒尺寸为0.5μm～10μm。在ZrO 2的颗粒尺寸范围内 的比表面积合适，在该配比下能实现介电常数系列可调的低温共烧电介质材料的制备。更优选地，所述ZrO 2的颗粒尺寸为1μm～5μm。
所述硅基非晶相填充料可以由各组分的混合而成，也可以由湿化学法制备。优选地，所述硅基非晶相填充料的制备方法包括以下步骤：
S1：将正硅酸乙酯溶于酒精和去离子水的混合溶液中；
S2:调节溶液pH至1～3；
S3:加入玻璃粉元素对应的盐，在60～80℃加热并搅拌均匀；
S4:调节溶液pH至6～8使其凝胶，将凝胶烘干并在600～750℃煅烧，即得所述玻璃粉。
传统的熔融-淬火法制备的玻璃的组分往往会与最初设计的玻璃组分有偏差，这主要是由于玻璃中一些易挥发的组分在高温熔融过程中的挥发，比如B 2O 3和Bi 2O 3。采用上述方法可以在低温条件下(～700℃)合成硅基非晶相填充料，可有效抑制这些组分的挥发，使得合成的硅基非晶相填充料更接近设计的组分。
所述硅基非晶相填充料的制备方法中涉及的除硅以外其他元素对应的盐，优选可溶性盐，可以为Na、K、Ca、B的硝酸盐、醋酸盐等。
优选地，步骤S1中，所述正硅酸乙酯、酒精和去离子水的体积比为：1：5～15：1。
本发明的目的还在于提供所述介电常数系列可调的低温共烧电介质材料的制备方法，所述制备方法包括以下步骤：将硅基非晶相填充料和氧化锆主相按比例混合球磨6～24小时，然后在800～900℃下烧结，得所述介电常数系列可调的低温共烧陶瓷材料。
本发明的有益效果在于：本发明提供了一种介电常数系列可调的低温共烧电介质材料，本发明通过控制氧化锆主相和硅基非晶相填充料的比例，所得材料的介电常数在7～12较宽的范围内连续可调，而且介电损耗可低至0.1％@1MHz。该材料体系可在800～900℃烧结，能够与银电极兼容共烧，可以用作 低温共烧电介质材料。
附图说明
图1为实施例1～4所述样品的介电性能(@1MHz)；
图2中，图(a)为实施例3中银电极与粉末干压成的生片在850℃共烧后的横截面的SEM图(b)为图(a)中各点位置的银含量。
具体实施方式
为更好的说明本发明的目的、技术方案和优点，下面将结合具体实施例对本发明作进一步说明。
实施例1
本发明所述低温共烧电介质材料的制备方法的一种实施例，本实施例所述低温共烧电介质材料的制备方法包括以下步骤：
将9.3mL的正硅酸乙酯溶于酒精(100mL)和去离子水(9.3mL)的混合溶液中；为促进水解，加入硝酸调节溶液pH至1左右并搅拌；待溶液澄清后，加入0.07g NaNO 3、0.24g KNO 3、0.28g Ca(NO 3) 2·4H 2O和0.92g HBO 3溶液，剧烈搅拌并在75℃加热，然后加入氨水调节pH至7左右形成凝胶，所得凝胶烘干后在700℃煅烧2h，得硅基非晶相填充料；最后称量49.81％的ZrO 2(颗粒尺寸为5μm)和50.19％的硅基非晶相填充料进行球磨混料18小时，干燥后在7MPa下干压成片并在850℃烧结，得所述低温共烧陶瓷材料。
本实施例制得的低温共烧电介质材料的介电性能如图1所示，介电常数为8.89@1MHz，介电损耗为0.0012@1MHz。本实施例所述低温共烧电介质材料与银电极共烧后结合紧密，没有发生层裂、翘曲等现象。
实施例2
本发明所述低温共烧电介质材料的制备方法的一种实施例，本实施例所述低温共烧电介质材料的制备方法包括以下步骤：
将9.3mL的正硅酸乙酯溶于酒精(93mL)和去离子水(9.3mL)的混合溶液中；为促进水解，加入硝酸调节溶液pH至1左右并搅拌，待溶液澄清后，加入0.07g NaNO 3、0.24g KNO 3、0.28g Ca(NO 3) 2·4H 2O和0.92g HBO 3溶液，剧烈搅拌并在80℃加热；然后加入氨水调节pH至7左右形成凝胶，所得凝胶烘干后在700℃煅烧2h，得硅基非晶相填充料；最后称量55％的ZrO 2(颗粒尺寸为5μm)和45％的硅基非晶相填充料进行球磨混料15小时。干燥后在7MPa下干压成片并在850℃烧结，得所述低温共烧陶瓷材料。
本实施例制得的低温共烧电介质材料的介电性能如图1所示，介电常数为10.48@1MHz，介电损耗为0.0011@1MHz。本实施例所述低温共烧电介质材料与银电极共烧后结合紧密，没有发生层裂、翘曲等现象。
实施例3
本发明所述低温共烧电介质材料的制备方法的一种实施例，本实施例所述低温共烧电介质材料的制备方法包括以下步骤：
将9.3mL的正硅酸乙酯溶于酒精(100mL)和去离子水(9.3mL)的混合溶液中；为促进水解，加入硝酸调节溶液pH至1左右并搅拌；待溶液澄清后，加入0.07g NaNO 3、0.24g KNO 3、0.28g Ca(NO 3) 2·4H 2O和0.92g HBO 3溶液，剧烈搅拌并在60℃加热；然后加入氨水调节pH至7左右形成凝胶，所得凝胶烘干后在700℃煅烧2h，得硅基非晶相填充料；最后称量60％的ZrO 2(颗粒尺寸为5μm)和40％的硅基非晶相填充料进行球磨混料16小时，干燥后在7MPa下干压成片并在850℃烧结，得所述低温共烧陶瓷材料。
本实施例制得的低温共烧电介质材料的介电性能如图1所示，介电常数为11.11@1MHz，介电损耗为0.0006@1MHz。
为了验证该组分与银电极共烧的兼容性，我们用5％的聚乙烯醇缩丁醛(PVB)溶液对球磨后的氧化锆和玻璃的混合粉末进行造粒，然后在7MPa下干压成片，再在其表面涂上银电极，最后在850℃烧结。图2中，图(a)是银电极和生片共烧后横截面的SEM图，可以看到银电极和陶瓷结合紧密，没有脱层或者裂缝现象，图(b)显示银的含量在银电极/陶瓷界面处急剧下降，表明烧结过 程中没有发生扩散。
实施例4
本发明所述低温共烧电介质材料的制备方法的一种实施例，本实施例所述低温共烧电介质材料的制备方法包括以下步骤：
将9.3mL的正硅酸乙酯溶于酒精(100mL)和去离子水(9.3mL)的混合溶液中；为促进水解，加入硝酸调节溶液pH至1左右并搅拌；待溶液澄清后，加入0.07g NaNO 3、0.24g KNO 3、0.28g Ca(NO 3) 2·4H 2O和0.92g HBO 3溶液，剧烈搅拌并在60℃加热；然后加入氨水调节pH至7左右形成凝胶，所得凝胶烘干后在700℃煅烧2h，得硅基非晶相填充料；最后称量65％的ZrO 2(颗粒尺寸为5μm)和35％的硅基非晶相填充料进行球磨混料15小时，干燥后在7MPa下干压成片并在850℃烧结，得所述低温共烧陶瓷材料。
本实施例制得的低温共烧电介质材料的介电性能如图1所示，介电损耗为0.0004@1MHz。本实施例所述低温共烧电介质材料与银电极共烧后结合紧密，没有发生层裂、翘曲等现象。
最后所应当说明的是，以上实施例仅用以说明本发明的技术方案而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

  1. 一种介电常数系列可调的低温共烧电介质材料，其特征在于，所述低温共烧电介质材料包含氧化锆主相和硅基非晶相填充料，所述氧化锆主相和硅基非晶相填充料的重量之比为：氧化锆主相：硅基非晶相填充料＝40～65：35～60；所述SiO 2在所述硅基非晶相填充料中的重量百分含量≥50％。
  2. 如权利要求1所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述低温共烧电介质材料包含以下重量百分含量的组分：ZrO 240％～65％、SiO 227.03％～46.33％、Na 2O 0.27％～0.46％、K 2O 1.23％～2.11％、CaO 0.73％～1.26％和B 2O 35.73％～9.83％。
  3. 如权利要求1或2所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述氧化锆主相为晶态或者非晶态。
  4. 如权利要求1或2所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述硅基非晶相填充料为玻璃或者非晶相的混合物。
  5. 如权利要求2所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述硅基非晶相填充料中，Na和K的原子比为：Na/K＝1:2～4。
  6. 如权利要求2所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述硅基非晶相填充料中Al元素的重量百分含量≤0.01％。
  7. 如权利要求2所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述ZrO 2的颗粒尺寸为0.5μm～10μm；优选地，所述ZrO 2的颗粒尺寸为1μm～5μm。
  8. 如权利要求1所述介电常数系列可调的低温共烧电介质材料，其特征在于，所述硅基非晶相填充料的制备方法包括以下步骤：
    S1：将正硅酸乙酯溶于酒精和去离子水的混合溶液中；
    S2:调节溶液pH至1～3；
    S3:加入玻璃粉元素对应的盐，在60～80℃加热并搅拌均匀；
    S4:调节溶液pH至6～8使其凝胶，将凝胶烘干并在600～750℃煅烧，即得所述玻璃粉。
  9. 如权利要求1所述介电常数系列可调的低温共烧电介质材料，其特征在于，步骤S1中，所述正硅酸乙酯、酒精和去离子水的体积比为：1：5～15：1。
  10. 如权利要求1～9中任一项所述介电常数系列可调的低温共烧电介质材料的制备方法，其特征在于，包括以下步骤：将硅基非晶相填充料和氧化锆主相按比例混合球磨6～24小时，然后在800～900℃下烧结，得所述介电常数系列可调的低温共烧陶瓷材料。
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