WO2021185075A1 - 一种ltcc微波介质材料及其制备方法 - Google Patents

一种ltcc微波介质材料及其制备方法 Download PDF

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WO2021185075A1
WO2021185075A1 PCT/CN2021/078758 CN2021078758W WO2021185075A1 WO 2021185075 A1 WO2021185075 A1 WO 2021185075A1 CN 2021078758 W CN2021078758 W CN 2021078758W WO 2021185075 A1 WO2021185075 A1 WO 2021185075A1
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microwave dielectric
powder
dielectric material
glass
ball mill
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PCT/CN2021/078758
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English (en)
French (fr)
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陈涛
程凯
曹秀华
沓世我
付振晓
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广东风华高新科技股份有限公司
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Priority to KR1020217024601A priority Critical patent/KR102618234B1/ko
Priority to JP2021544937A priority patent/JP7254195B2/ja
Priority to US17/389,334 priority patent/US20210355035A1/en
Publication of WO2021185075A1 publication Critical patent/WO2021185075A1/zh

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Definitions

  • the invention belongs to the technical field of microwave dielectric materials, and specifically relates to an LTCC microwave dielectric material with a temperature coefficient of resonance frequency close to zero and a preparation method thereof.
  • LTCC Low-temperature co-fired ceramic material
  • Q value that is, low loss
  • materials are required to have a near-zero resonance frequency temperature coefficient.
  • the Chinese invention patent with the application number "200910113981.X” combines Ba 5-x La x Ti x Nb x O 15 with BaCuB 2 O 5 and BaWO4 to obtain a low-temperature sintered microwave dielectric ceramic with a Qf value higher than 10000GHz, and The temperature coefficient of the resonance frequency is close to zero; however, due to the high dielectric constant of Ba 5-x La x Ti x Nb x O 15, the dielectric constant of the system is relatively high (35-45), which does not meet the requirements of low dielectric constant. For this reason, it is necessary to develop a new composite material system to meet the needs of LTCC microwave dielectric ceramics with low dielectric constant and near zero temperature coefficient of resonance frequency.
  • the purpose of the present invention is to overcome the above-mentioned shortcomings of the prior art and provide an LTCC microwave dielectric material with a temperature coefficient of resonant frequency close to zero.
  • an LTCC microwave dielectric material the material composition of the LTCC microwave dielectric material is as follows: a Ba 5 Si 8 O 21 +(1-a)(Mg x Ca y Sr z Ba 1-xyz )WO 4 +Ba-B-Si glass; where 0.4 ⁇ a ⁇ 0.8, 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1.
  • the present invention combines a barium silicate Ba 5 Si 8 O 21 with a positive resonance frequency temperature coefficient and a low dielectric constant and a tungstate (Mg x Ca y Sr z Ba 1-xyz ) with a negative resonance frequency temperature coefficient.
  • WO 4 composite, low melting point Ba-B-Si glass is added to reduce the sintering temperature of the system, and LTCC microwave dielectric ceramics with low dielectric constant and near zero resonance frequency temperature coefficient are obtained, which are suitable for high-frequency communication and radio frequency fields.
  • the weight of the Ba-B-Si glass is 2-15% of the total weight of Ba 5 Si 8 O 21 and Mg x Ca y Sr z Ba 1-xyz . This choice can better reduce the sintering temperature of the system.
  • the present invention also provides a method for preparing the LTCC microwave dielectric material, which includes the following steps:
  • step (3) Combine the Ba 5 Si 8 O 21 powder obtained in step (1), the (Mg x Ca y Sr z Ba 1-xyz ) WO 4 powder obtained in step (2), and the Ba-Si 8 O 21 powder obtained in step (3).
  • B-Si glass powder is added to the ball mill tank, zirconia balls and deionized water are added, ball milled for 2-6 hours, taken out, dried, and powdered to obtain porcelain powder for preparing LTCC microwave dielectric ceramics;
  • step (4) PVA solution is added to the porcelain powder obtained in step (4) to granulate, and compressed into a cylindrical block, sintered at 850-900 DEG C, and kept for 0.5-3h to obtain LTCC microwave dielectric ceramics.
  • the Ba-B-Si glass in the step (3) is prepared by the following method:
  • a solid phase method is used to synthesize barium silicate Ba 5 Si 8 O 21 with a positive resonance frequency temperature coefficient ( ⁇ f) and tungstate AWO 4 with a negative ⁇ f (A can be an alkaline earth metal element Any one or a combination of more than one), using a high-temperature melting method to prepare Ba-B-Si (BBS) low-melting glass; by controlling the content of Ba 5 Si 8 O 21 and AWO 4 to adjust ⁇ f to near zero, passing BBS Glass addition reduces the sintering temperature of the system to below 900°C, and a low dielectric constant LTCC microwave dielectric ceramic with ⁇ f close to zero is obtained.
  • the sieving in the step (1) and step (2) is: sieving through a 200-mesh sieve.
  • the weight of the PVA solution is 7-10 wt% of the weight of the porcelain powder.
  • the raw materials in the step (2) are MgO, CaCO 3 , SrCO 3 , BaCO 3 and WO 3 .
  • the raw materials in the step (1) are BaCO 3 and SiO 2 .
  • the raw materials used in this application are synthesized by solid phase method, the process is simple, and suitable for industrial production.
  • the synthesized Ba 5 Si 8 O 21 , (Mg x Ca y Sr z Ba 1-xyz )WO 4 and Ba-B-Si glass dielectric The constant is low.
  • the LTCC microwave dielectric ceramics obtained by compounding have a low dielectric constant.
  • the material composition of the LTCC microwave dielectric material in the examples of this application is as follows: a Ba 5 Si 8 O 21 +(1-a)(Mg x Ca y Sr z Ba 1-xyz )WO 4 +Ba-B-Si glass ; Wherein, 0.4 ⁇ a ⁇ 0.8, 0 ⁇ x ⁇ 1, 0 ⁇ y ⁇ 1, 0 ⁇ z ⁇ 1; the weight of the Ba-B-Si glass is Ba 5 Si 8 O 21 , Mg x Ca y Sr 2-15% (b%) of the sum of z Ba 1-xyz weight;
  • the material components and properties of the LTCC microwave dielectric materials of the specific embodiments are shown in Table 1.
  • the dielectric constant and Qf value are obtained by the parallel plate reflection method using a network analyzer; the ⁇ f value is based on the formula It is calculated that T2 and T1 are 80°C and 25°C, respectively, and f2 and f1 are the resonance frequencies of the sample at temperatures T2 and T1, respectively.
  • the LTCC microwave dielectric ceramic obtained in this application has a relatively low dielectric constant.

Abstract

一种LTCC微波介质材料的组分如下：a Ba 5Si 8O 21+(1-a)(Mg xCa ySr zBa 1-x-y-z)WO 4+Ba-B-Si玻璃；其中，0.4≤a≤0.8，0≤x≤1，0≤y≤1，0≤z≤1。通过调整Ba 5Si 8O 21及(Mg xCa ySr zBa 1-x-y-z)WO 4的含量，可将谐振频率温度系数调节到近零，适用于高频通讯及射频领域。同时，还公开一种LTCC微波介质材料的制备方法。

Description

一种LTCC微波介质材料及其制备方法 技术领域
本发明属于微波介质材料技术领域，具体涉及一种谐振频率温度系数近零的LTCC微波介质材料及其制备方法。
背景技术
随着5G通讯及万物互联时代的到来，高频应用成为趋势。小型化、高集成度和高可靠性成为5G通信器件的典型特点。用于5G通信器件集成技术的关键介质材料-低温共烧陶瓷材料(LTCC)成为研究热点。为减少信号传输损耗，加快信号传输速度，需要LTCC材料具备较低的介电常数及较高的Q值(即低损耗)；为提高信号传输的稳定性，需要材料具备近零的谐振频率温度系数。
申请号为“200910113981.X”的中国发明专利，将Ba 5-xLa xTi xNb xO 15与BaCuB 2O 5及BaWO4复合，得到了Qf值高于10000GHz的低温烧结微波介质陶瓷，且其谐振频率温度系数近零；但由于Ba 5-xLa xTi xNb xO 15介电常数较高，导致体系介电常数较高(35～45)，不符合低介电常数要求。为此，需开发新的复合材料体系，以满足低介电常数，且谐振频率温度系数近零的LTCC微波介质陶瓷需求。
发明内容
基于此，本发明的目的在于克服上述现有技术的不足之处而提供一种谐振频率温度系数近零的LTCC微波介质材料。
为实现上述目的，本发明所采取的技术方案为：一种LTCC微波介质材料，所述LTCC微波介质材料的材料组分如下：a Ba 5Si 8O 21+(1-a)(Mg xCa ySr zBa 1-x-y-z)WO 4+Ba-B-Si玻璃；其中，0.4≤a≤0.8，0≤x≤1，0≤y≤1，0≤z≤1。
本发明通过将具有正谐振频率温度系数且介电常数较低的钡硅酸盐Ba 5Si 8O 21与具有负谐振频率温度系数的钨酸盐(Mg xCa ySr zBa 1-x-y-z)WO 4复合，通 过低熔点Ba-B-Si玻璃添加来降低体系烧结温度，得到了低介电常数，且谐振频率温度系数近零的LTCC微波介质陶瓷，适用于高频通讯及射频领域。
优选地，所述Ba-B-Si玻璃的重量为Ba 5Si 8O 21、Mg xCa ySr zBa 1-x-y-z重量之和的2～15％。这一选择可以更好的降低体系的烧结温度。
同时，本发明还提供一种所述的LTCC微波介质材料的制备方法，包括如下步骤：
(1)按照化学计量比Ba 5Si 8O 21称取原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，球磨4-12h，取出、烘干、过筛，将过筛后的粉末在1100-1250℃下煅烧，保温1-5h，冷却至室温，得到Ba 5Si 8O 21粉体；
(2)按照化学计量比(Mg xCa ySr zBa 1-x-y-z)WO 4称取原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨4-12h，取出、烘干、过筛，将过筛后的粉末在700-1000℃下煅烧，保温1-5h，冷却至室温，得到(Mg xCa ySr zBa 1-x-y-z)WO 4粉体；
(3)将Ba-B-Si玻璃放入球磨罐中，加入氧化锆球和去离子水，球磨2-6h，取出、烘干，得到Ba-B-Si玻璃粉；
(4)将步骤(1)得到的Ba 5Si 8O 21粉体、步骤(2)得到的(Mg xCa ySr zBa 1-x-y-z)WO 4粉体、步骤(3)得到的Ba-B-Si玻璃粉加入球磨罐中，加入氧化锆球和去离子水，球磨2-6h，取出、烘干、打粉，得到用于制备LTCC微波介质陶瓷的瓷粉；
(5)在步骤(4)所得瓷粉中添加PVA溶液造粒，并压制成圆柱状块体，在850-900℃下烧结，保温0.5-3h，得到LTCC微波介质陶瓷。
优选地，所述步骤(3)中的Ba-B-Si玻璃通过以下方法制备所得：
以SiO 2、H 3BO 3、BaCO 3、Na 2CO 3、Li 2CO 3、BaCO 3、SrCO 3、K 2CO 3、Al 2O 3、MgO、TiO 2为原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨1-4h，取出、烘干，将烘干后的粉末在1200-1500℃下熔融，保温1-3h，将玻璃液高温取出，倒入去离子水中淬火，得到Ba-B-Si玻璃。
本申请制备方法中，采用固相法合成谐振频率温度系数(τf)为正值的钡硅酸盐Ba 5Si 8O 21及τf为负值的钨酸盐AWO 4(A可以是碱土金属元素中的任意 一种或一种以上的组合)，采用高温熔融法制备Ba-B-Si(BBS)低熔点玻璃；通过控制Ba 5Si 8O 21及AWO 4的含量调节τf近零，通过BBS玻璃添加将体系烧结温度降低到900℃以下，得到τf近零的低介电常数LTCC微波介质陶瓷。
优选地，所述步骤(1)、步骤(2)中的过筛为：过200目筛。
优选地，所述步骤(5)中，PVA溶液的重量为瓷粉重量的7-10wt％。
优选地，所述步骤(2)中的原料为MgO、CaCO 3、SrCO 3、BaCO 3和WO 3。
优选地，所述步骤(1)中的原料为BaCO 3和SiO 2。
相对于现有技术，本发明的优势在于：
本申请所用原材料通过固相法合成，工艺简单、适合工业生产，所合成的Ba 5Si 8O 21、(Mg xCa ySr zBa 1-x-y-z)WO 4及Ba-B-Si玻璃介电常数较低，经复合后得到的LTCC微波介质陶瓷具备较低的介电常数，通过调整Ba 5Si 8O 21及(Mg xCa ySr zBa 1-x-y-z)WO 4的含量，可将谐振频率温度系数调节到近零，适用于高频通讯及射频领域。
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。
本申请实施例中的LTCC微波介质材料的材料组分如下：a Ba 5Si 8O 21+(1-a)(Mg xCa ySr zBa 1-x-y-z)WO 4+Ba-B-Si玻璃；其中，0.4≤a≤0.8，0≤x≤1，0≤y≤1，0≤z≤1；所述Ba-B-Si玻璃的重量为Ba 5Si 8O 21、Mg xCa ySr zBa 1-x-y-z重量之和的2～15％(b％)；
本申请实施例中的LTCC微波介质材料的制备方法如下：
(1)按照化学计量比Ba 5Si 8O 21称取BaCO 3及SiO 2原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨4-12h，取出、烘干、过200目筛，将过筛后的粉末放到氧化铝坩埚中，在马弗炉中以1100-1250℃煅烧，保温1-5h，冷却至室温，得到Ba 5Si 8O 21粉体；
(2)按照化学计量比(Mg xCa ySr zBa 1-x-y-z)WO 4取MgO、BaCO 3、SrCO 3、BaCO 3及WO 3原料(其中0≤x≤1，0≤y≤1，0≤z≤1)，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨4-12h，取出、烘干、过200目筛，将过筛后的粉末放到氧化铝坩埚中，在马弗炉中以700-1000℃煅烧，保温1-5h，冷却至室温，得到(Mg xCa ySr zBa 1-x-y-z)WO 4粉体；
(3)按照配比SiO 2(45.8wt％)、H 3BO 3(39.6wt％)、BaCO 3(5.3wt％)、Na 2CO 3(1.6wt％)、Li 2CO 3(0.7wt％)、BaCO 3(1.5wt％)、SrCO 3(1.1wt％)、K 2CO 3(1.9wt％)、Al 2O 3(1.2wt％)、MgO(0.8wt％)、TiO 2(0.5wt％)，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨1-4h，取出、烘干，将烘干后的粉末放到氧化铝坩埚中，在高温炉中1200-1500℃熔融，保温1-3h，将玻璃液高温取出，倒入去离子水中淬火，得到Ba-B-Si玻璃，将Ba-B-Si玻璃放入球磨罐中，加入氧化锆球和去离子水，行星球磨2-6h，取出、烘干，得到Ba-B-Si玻璃粉；
(4)按照a Ba 5Si 8O 21+(1-a)(Mg xCa ySr zBa 1-x-y-z)WO 4+b wt％Ba-B-Si玻璃的比例称取上述所Ba 5Si 8O 21、(Mg xCa ySr zBa 1-x-y-z)WO 4及Ba-B-Si玻璃粉体，其中0.4≤a≤0.8，2≤b≤15；将称量好的粉体倒入球磨罐中，加入氧化锆球和去离子水，行星球磨2-6h，取出、烘干、打粉，得到用于制备LTCC微波介质陶瓷的瓷粉；
(5)在上述瓷粉中添加7-10wt％的PVA溶液造粒并压制成圆柱状块体，在850-900℃之间烧结，保温0.5-3h，得到LTCC微波介质陶瓷。
具体各实施例LTCC微波介质材料的材料组分及性能如表1所示，其中，介电常数及Qf值采用网络分析仪，以平行板反射法测试得到；τf值根据公式
Figure PCTCN2021078758-appb-000001
计算得到，其中，T2和T1分别为80℃及25℃，f2和f1分别为温度T2及T1下样品的谐振频率。
表1 具体实施例材料组分及对应样品微波介电性能
Figure PCTCN2021078758-appb-000002
Figure PCTCN2021078758-appb-000003
从表1可以看出，本申请得到的LTCC微波介质陶瓷具备较低的介电常数，通过调整Ba 5Si 8O 21及(Mg xCa ySr zBa 1-x-y-z)WO 4的含量，可将谐振频率温度系数调节到近零，适用于高频通讯及射频领域。
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 (8)

  1. 一种LTCC微波介质材料，其特征在于，所述LTCC微波介质材料的材料组分如下：a Ba 5Si 8O 21+(1-a)(Mg xCa ySr zBa 1-x-y-z)WO 4+Ba-B-Si玻璃；其中，0.4≤a≤0.8，0≤x≤1，0≤y≤1，0≤z≤1。
  2. 如权利要求1所述的LTCC微波介质材料，其特征在于，所述Ba-B-Si玻璃的重量为Ba 5Si 8O 21、Mg xCa ySr zBa 1-x-y-z重量之和的2～15％。
  3. 一种如权利要求1或2所述的LTCC微波介质材料的制备方法，其特征在于，包括如下步骤：
    (1)按照化学计量比Ba 5Si 8O 21称取原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，球磨4-12h，取出、烘干、过筛，将过筛后的粉末在1100-1250℃下煅烧，保温1-5h，冷却至室温，得到Ba 5Si 8O 21粉体；
    (2)按照化学计量比(Mg xCa ySr zBa 1-x-y-z)WO 4称取原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨4-12h，取出、烘干、过筛，将过筛后的粉末在700-1000℃下煅烧，保温1-5h，冷却至室温，得到(Mg xCa ySr zBa 1-x-y-z)WO 4粉体；
    (3)将Ba-B-Si玻璃放入球磨罐中，加入氧化锆球和去离子水，球磨2-6h，取出、烘干，得到Ba-B-Si玻璃粉；
    (4)将步骤(1)得到的Ba 5Si 8O 21粉体、步骤(2)得到的(Mg xCa ySr zBa 1-x-y-z)WO 4粉体、步骤(3)得到的Ba-B-Si玻璃粉加入球磨罐中，加入氧化锆球和去离子水，球磨2-6h，取出、烘干、打粉，得到用于制备LTCC微波介质陶瓷的瓷粉；
    (5)在步骤(4)所得瓷粉中添加PVA溶液造粒，并压制成圆柱状块体，在850-900℃下烧结，保温0.5-3h，得到LTCC微波介质陶瓷。
  4. 如权利要求3所述的LTCC微波介质材料的制备方法，其特征在于，所述步骤(3)中的Ba-B-Si玻璃通过以下方法制备所得：
    以SiO 2、H 3BO 3、BaCO 3、Na 2CO 3、Li 2CO 3、BaCO 3、SrCO 3、K 2CO 3、Al 2O 3、MgO、TiO 2为原料，将称量好的原料倒入球磨罐中，加入氧化锆球和去离子水，行星球磨1-4h，取出、烘干，将烘干后的粉末在1200-1500℃下熔融，保温1-3h， 将玻璃液高温取出，倒入去离子水中淬火，得到Ba-B-Si玻璃。
  5. 如权利要求3所述的LTCC微波介质材料的制备方法，其特征在于，所述步骤(1)、步骤(2)中的过筛为：过200目筛。
  6. 如权利要求3所述的LTCC微波介质材料的制备方法，其特征在于，所述步骤(5)中，PVA溶液的重量为瓷粉重量的7-10wt％。
  7. 如权利要求3所述的LTCC微波介质材料的制备方法，其特征在于，所述步骤(2)中的原料为MgO、CaCO 3、SrCO 3、BaCO 3和WO 3。
  8. 如权利要求3所述的LTCC微波介质材料的制备方法，其特征在于，所述步骤(1)中的原料为BaCO 3和SiO 2。
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