CN102503137A - Calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and preparation method thereof - Google Patents
Calcium-aluminum-boron-silicon glass and fused quartz low-temperature co-fired ceramic material and preparation method thereof Download PDFInfo
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- 239000011521 glass Substances 0.000 title claims abstract description 59
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000005350 fused silica glass Substances 0.000 title claims abstract description 22
- -1 Calcium-aluminum-boron-silicon Chemical compound 0.000 title 1
- 238000002844 melting Methods 0.000 claims abstract description 59
- 239000000463 material Substances 0.000 claims abstract description 55
- 230000008018 melting Effects 0.000 claims abstract description 35
- 238000000498 ball milling Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- 239000000919 ceramic Substances 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- ULGYAEQHFNJYML-UHFFFAOYSA-N [AlH3].[Ca] Chemical compound [AlH3].[Ca] ULGYAEQHFNJYML-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000011049 filling Methods 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 239000005388 borosilicate glass Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 9
- 239000011230 binding agent Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000006060 molten glass Substances 0.000 claims abstract description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 9
- 239000002893 slag Substances 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 9
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- 238000005469 granulation Methods 0.000 claims description 3
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- 239000013078 crystal Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052802 copper Inorganic materials 0.000 abstract description 3
- 239000010949 copper Substances 0.000 abstract description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052737 gold Inorganic materials 0.000 abstract description 3
- 239000010931 gold Substances 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 3
- 239000004332 silver Substances 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 description 10
- 238000011161 development Methods 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000004100 electronic packaging Methods 0.000 description 3
- 238000004377 microelectronic Methods 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 239000006124 glass-ceramic system Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种钙铝硼硅系玻璃+熔融石英体系低温共烧陶瓷材料及其制备方法，其中钙铝硼硅低熔点玻璃相占总体材料的质量分数为50～70％。按低熔点玻璃相所需各氧化物的摩尔百分含量称取原料，在1500～1600C下保温3～5小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨制得平均粒度为1～3μm的玻璃粉；将熔融石英粉球磨后，得到平均粒度为3～5μm的熔融石英粉；将50～70％重量百分比的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入混合材料的重量的3％聚乙烯醇粘结剂，造粒干压后制成坯片；烧结制得低温共烧陶瓷材料。低温共烧陶瓷材料烧结温度低，与金、银、铜等导体材料共烧；所得材料致密化程度高，气孔率低，材料具有较低的热膨胀系数；工艺流程简单，成本低廉。
The invention relates to a low-temperature co-fired ceramic material of calcium aluminum borosilicate glass+fused quartz system and a preparation method thereof, wherein the mass fraction of calcium aluminum borosilicate low-melting glass phase in the overall material is 50-70%. Weigh the raw materials according to the mole percentage of each oxide required for the low-melting point glass phase, keep it warm at 1500-1600C for 3-5 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and ball mill it to obtain an average Glass powder with a particle size of 1 to 3 μm; fused silica powder with an average particle size of 3 to 5 μm after ball milling; 50 to 70% by weight of the low melting point glass phase and the high melting point ceramic filling phase are mixed evenly, Adding 3% polyvinyl alcohol binder by weight of the mixed material, granulating and dry-pressing to make a green sheet; sintering to make a low-temperature co-fired ceramic material. The low-temperature co-fired ceramic material has a low sintering temperature and is co-fired with conductor materials such as gold, silver, and copper; the obtained material has a high degree of densification, low porosity, and a low thermal expansion coefficient; the process is simple and the cost is low.
Description
技术领域 technical field
本发明涉及一种低热膨胀系数的低温共烧陶瓷材料及其制备方法，属于电子封装材料领域。The invention relates to a low-temperature co-fired ceramic material with a low thermal expansion coefficient and a preparation method thereof, belonging to the field of electronic packaging materials.
背景技术 Background technique
随着微电子技术的迅速发展，电子线路日益向微型化、集成化的方向发展。而电子封装技术的发展没有与之形成配套，成为制约微电子技术继续发展的瓶颈。低温共烧陶瓷(LowTemperature Cofired Ceramics，LTCC)技术，作为近年来兴起的一种新的电子封装技术，受到了国内外科研人员的广泛重视和研究。它涉及电路设计，微波技术、材料科学等广泛领域。尤其是起到关键作用的材料技术得到了广泛的重视。With the rapid development of microelectronics technology, electronic circuits are increasingly miniaturized and integrated. However, the development of electronic packaging technology has not been matched with it, which has become a bottleneck restricting the continued development of microelectronic technology. Low Temperature Cofired Ceramics (LTCC) technology, as a new electronic packaging technology that has emerged in recent years, has received extensive attention and research by researchers at home and abroad. It involves a wide range of fields such as circuit design, microwave technology, and material science. In particular, material technology, which plays a key role, has received extensive attention.
LTCC技术主要具有以下几方面的技术优势：(1)LTCC可以直接与金属在大气中共烧，减少了工艺环节。(2)可采用低熔点、高电导率的金、银、铜等作为导线材料。因此降低了成本，又能获得良好的性能。(3)基板设计灵活。其中包括布线灵活，介电常数可调，层数可变等优势。LTCC technology mainly has the following technical advantages: (1) LTCC can be directly co-fired with metals in the atmosphere, reducing the process steps. (2) Gold, silver, copper, etc. with low melting point and high conductivity can be used as wire materials. Therefore, the cost is reduced and good performance can be obtained. (3) The substrate design is flexible. These include the advantages of flexible wiring, adjustable dielectric constant, and variable number of layers.
目前正在研究的和已经投入生产的主流LTCC材料主要分为两类，即微晶玻璃体系和玻璃+陶瓷体系。微晶玻璃系LTCC材料主要是通过玻璃的成核和结晶过程，得到致密的陶瓷材料。其缺点在于结晶过程难以控制，材料性能难以预测，尤其是介电损耗，工艺窗口窄，器件稳定性较差，不利于大批量生产。The mainstream LTCC materials currently being researched and put into production are mainly divided into two categories, namely the glass-ceramic system and the glass + ceramic system. Glass-ceramics-based LTCC materials are mainly obtained through the nucleation and crystallization process of glass to obtain dense ceramic materials. The disadvantages are that the crystallization process is difficult to control, the material properties are difficult to predict, especially the dielectric loss, the process window is narrow, and the device stability is poor, which is not conducive to mass production.
与之相比，玻璃+陶瓷体系材料具有以下优势：(1)更好地机械性能。由于玻璃量的减少，陶瓷填充相的加入提高了材料的机械性能。(2)较低的热膨胀系数、介电常数和介电损耗。(3)易操作，易控制。可通过选用合适的玻璃、陶瓷相，调整两者的比例控制所得材料的性质In contrast, glass + ceramic system materials have the following advantages: (1) better mechanical properties. The addition of the ceramic filler phase improves the mechanical properties of the material due to the reduced amount of glass. (2) Lower coefficient of thermal expansion, dielectric constant and dielectric loss. (3) Easy to operate and control. The properties of the obtained material can be controlled by selecting appropriate glass and ceramic phases and adjusting the ratio of the two
经过多年研究，LTCC技术已经日益成熟，而国内仍处于起步阶段。目前，材料的热机械性能是影响LTCC器件可靠性的主要因素，其中最关键的是热膨胀系数。LTCC封装材料与所载硅基板芯片材料热膨胀系数(3.5×10-6/℃)的匹配可减小机械应力，从而确保系统的热稳定性。因此开发具有低热膨胀系数的LTCC材料，对实现微电子产品的小型化，高性能和可靠性具有重大的意义。同时，LTCC材料应在较低温度下(＜1000℃)达到较高的致密度，一般情况下，材料的气孔率应小于5％。After years of research, LTCC technology has become increasingly mature, but it is still in its infancy in China. At present, the thermomechanical properties of materials are the main factors affecting the reliability of LTCC devices, the most critical of which is the thermal expansion coefficient. The matching of the thermal expansion coefficient (3.5×10 -6 /°C) between the LTCC packaging material and the loaded silicon substrate chip material can reduce mechanical stress, thus ensuring the thermal stability of the system. Therefore, the development of LTCC materials with low thermal expansion coefficient is of great significance to realize the miniaturization, high performance and reliability of microelectronic products. At the same time, the LTCC material should achieve higher density at a lower temperature (<1000°C), and generally, the porosity of the material should be less than 5%.
发明内容 Contents of the invention
本发明的目的是开发一种具有低热膨胀系数的低温共烧陶瓷材料。本发明的另一目的是提供一种工艺简单，成本低廉的该材料的制备方法。The object of the present invention is to develop a low temperature co-fired ceramic material with a low coefficient of thermal expansion. Another object of the present invention is to provide a preparation method of the material with simple process and low cost.
本发明的技术如下：The technology of the present invention is as follows:
一种钙铝硼硅系玻璃+熔融石英低温共烧陶瓷材料，低温共烧陶瓷材料包括低熔点玻璃相和高熔点陶瓷填充相，其中钙铝硼硅低熔点玻璃相占总体材料的质量分数为50～70％。A calcium aluminum borosilicate glass + fused silica low-temperature co-fired ceramic material, the low-temperature co-fired ceramic material includes a low melting point glass phase and a high melting point ceramic filling phase, wherein the mass fraction of the calcium aluminum borosilicate low melting point glass phase in the overall material is 50-70%.
所述的低温共烧陶瓷材料，低熔点玻璃相中各氧化物的摩尔百分含量如下：In the low-temperature co-fired ceramic material, the molar percentages of each oxide in the low-melting glass phase are as follows:
本发明的所述的低温共烧陶瓷材料的制备方法，步骤如下：The preparation method of the described low temperature co-fired ceramic material of the present invention, the steps are as follows:
(1)低熔点玻璃的原料准备：按低熔点玻璃相所需各氧化物的摩尔百分含量称取原料，并混合均匀；(1) raw material preparation of low-melting point glass: take the raw material according to the molar percentage of each oxide required for the low-melting point glass phase, and mix uniformly;
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1500～1600℃下保温3～5小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨，制得平均粒度为1～3μm的玻璃粉；(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, keep it warm at 1500-1600°C for 3-5 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, ball mill, and make Obtain glass powder with an average particle size of 1-3 μm;
(3)高熔点陶瓷填充相的制备：将熔融石英粉球磨后，得到平均粒度为3～5μm的熔融石英粉；(3) Preparation of high melting point ceramic filling phase: after ball milling fused silica powder, fused silica powder with an average particle size of 3-5 μm is obtained;
(4)材料成型：将50～70％重量百分比的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入混合材料的重量的3％聚乙烯醇粘结剂，造粒干压后制成坯片；(4) Material molding: After mixing 50-70% by weight of the low melting point glass phase and the high melting point ceramic filling phase, add 3% polyvinyl alcohol binder by weight of the mixed material, and make it after granulation and dry pressing Blank;
(5)烧结：将所得坯片在900～1000℃下烧结，制得低温共烧陶瓷材料。(5) Sintering: Sinter the obtained green sheet at 900-1000° C. to obtain a low-temperature co-fired ceramic material.
所述球磨的球料比为3∶1，球磨介质为去离子水。The ball-to-material ratio of the ball mill is 3:1, and the ball mill medium is deionized water.
所述的烧结工艺是，在保证不析出二氧化硅晶相的情况下，升温至所需温度，保温1小时后，在炉中自然冷却至室温。The sintering process is to raise the temperature to the required temperature under the condition of ensuring that no silicon dioxide crystal phase is precipitated, and then naturally cool to room temperature in a furnace after keeping the temperature for 1 hour.
本发明的优点在于：低温共烧陶瓷材料烧结温度低，在(900～1000)℃实现烧结，因此可与金、银、铜等导体材料共烧；所得材料致密化程度高，气孔率低，如图1所示；工艺流程简单，成本低廉；所得材料具有较低的热膨胀系数。The advantages of the present invention are: the sintering temperature of the low-temperature co-fired ceramic material is low, and the sintering is realized at (900-1000) °C, so it can be co-fired with conductor materials such as gold, silver, copper, etc.; the obtained material has a high degree of densification and a low porosity. As shown in Figure 1; the process flow is simple and the cost is low; the obtained material has a low coefficient of thermal expansion.
附图说明 Description of drawings
图1为本发明中实施例3中低温共烧陶瓷材料的SEM图。Fig. 1 is an SEM image of the low temperature co-fired ceramic material in Example 3 of the present invention.
具体实施方式 Detailed ways
实施例1：Example 1:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1500℃下保温4小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为3μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1500° C. for 4 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (the ball-to-material ratio is 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 3 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为4μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: After ball milling the purchased fused silica powder (the ratio of ball to material is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 4 μm is obtained
(4)材料成型：将70wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入3wt％聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material molding: after mixing evenly 70wt% of the low-melting point glass phase and the high-melting point ceramic filling phase, add 3wt% polyvinyl alcohol binder, granulate and dry-press to make green sheets.
(5)烧结：将所得坯片在900℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: sinter the obtained green sheet at 900° C., keep it warm for 1 hour, and then naturally cool it to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为4.70×10-6/℃。该材料的气孔率为18.6％。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 4.70×10 -6 /°C. The material has a porosity of 18.6%.
实施例2：Example 2:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1550℃下保温4小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为1μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1550° C. for 4 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (the ball-to-material ratio is 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 1 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为3μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: After ball milling the purchased fused silica powder (the ball-to-material ratio is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 3 μm is obtained
(4)材料成型：将70wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入混合均匀后材料的重量的3％的聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material forming: After mixing evenly the low-melting-point glass phase and the high-melting-point ceramic filling phase of 70wt%, add 3% polyvinyl alcohol binder of the weight of the material after mixing, and make a billet after granulation and dry pressing piece.
(5)烧结：将所得坯片在900℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: sinter the obtained green sheet at 900° C., keep it warm for 1 hour, and then naturally cool it to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为6.2×10-6/℃。该材料的气孔率为1.1％。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 6.2×10 -6 /°C. The material has a porosity of 1.1%.
实施例3：Example 3:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1550℃下保温5小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为1.5μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1550° C. for 5 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (the ball-to-material ratio is 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 1.5 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为4μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: After ball milling the purchased fused silica powder (the ratio of ball to material is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 4 μm is obtained
(4)材料成型：将70wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入3wt％聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material molding: after mixing evenly 70wt% of the low-melting point glass phase and the high-melting point ceramic filling phase, add 3wt% polyvinyl alcohol binder, granulate and dry-press to make green sheets.
(5)烧结：将所得坯片在900℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: sinter the obtained green sheet at 900° C., keep it warm for 1 hour, and then naturally cool it to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为4.80×10-6/℃。该材料的气孔率为2.2％。本实例的SEM图见附图1。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 4.80×10 -6 /°C. The material has a porosity of 2.2%. The SEM picture of this example is shown in accompanying
实施例4：Example 4:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1600℃下保温3小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为3μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1600° C. for 3 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (ball-to-material ratio: 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 3 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为5μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: after ball milling the purchased fused silica powder (the ratio of ball to material is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 5 μm is obtained
(4)材料成型：将70wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入3wt％聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material molding: after mixing evenly 70wt% of the low-melting point glass phase and the high-melting point ceramic filling phase, add 3wt% polyvinyl alcohol binder, granulate and dry-press to make green sheets.
(5)烧结：将所得坯片在900℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: sinter the obtained green sheet at 900° C., keep it warm for 1 hour, and then naturally cool it to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为7.95×10-6/℃。该材料的气孔率为2.9％。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 7.95×10 -6 /°C. The material has a porosity of 2.9%.
实施例5：Example 5:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1550℃下保温4小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为1μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1550° C. for 4 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (the ball-to-material ratio is 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 1 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为3μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: After ball milling the purchased fused silica powder (the ball-to-material ratio is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 3 μm is obtained
(4)材料成型：将50wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入3wt％聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material molding: After mixing 50wt% of the low-melting point glass phase and the high-melting point ceramic filling phase evenly, add 3wt% polyvinyl alcohol binder, granulate and dry-press to make green sheets.
(5)烧结：将所得坯片在1000℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: sinter the obtained green sheet at 1000° C., keep it warm for 1 hour, and then naturally cool it to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为4.95×10-6/℃。该材料的气孔率为4.4％。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 4.95×10 -6 /°C. The material has a porosity of 4.4%.
实施例6：Embodiment 6:
本发明具体实施例中，钙铝硼硅玻璃中各氧化物的摩尔百分比含量如下：In a specific embodiment of the present invention, the mole percentage content of each oxide in calcium aluminum borosilicate glass is as follows:
本实施例中低温共烧陶瓷材料的制备方法，包括以下步骤：The preparation method of the low-temperature co-fired ceramic material in this embodiment comprises the following steps:
(1)低熔点玻璃的原料准备：按上述各氧化物的摩尔百分含量称取低熔点钙铝硼硅玻璃所需原料，并混合均匀。(1) Raw material preparation for low melting point glass: Weigh the raw materials required for low melting point calcium aluminum borosilicate glass according to the mole percentage of each oxide mentioned above, and mix them evenly.
(2)低熔点玻璃的制备：将上述混合均匀的混合物装入坩埚，在1550℃下保温5小时，将熔融的玻璃液直接倒入去离子水中，得到玻璃渣，球磨后(球料比为3∶1，球磨介质为去离子水)，制得平均粒度为1.5μm的玻璃粉。(2) Preparation of low-melting point glass: put the above-mentioned homogeneously mixed mixture into a crucible, heat it at 1550° C. for 5 hours, pour the molten glass liquid directly into deionized water to obtain glass slag, and after ball milling (the ball-to-material ratio is 3:1, the ball milling medium is deionized water), and the glass powder with an average particle size of 1.5 μm is obtained.
(3)高熔点陶瓷填充相的制备：将购得的熔融石英粉球磨后(球料比为3∶1，球磨介质为去离子水)，得到平均粒度为4μm的熔融石英粉(3) Preparation of high melting point ceramic filling phase: after ball milling the purchased fused silica powder (the ratio of ball to material is 3:1, and the ball milling medium is deionized water), the fused silica powder with an average particle size of 4 μm is obtained
(4)材料成型：将60wt％的低熔点玻璃相和高熔点陶瓷填充相混合均匀后，加入3wt％聚乙烯醇粘结剂，造粒干压后制成坯片。(4) Material forming: after mixing 60wt% of low melting point glass phase and high melting point ceramic filling phase evenly, adding 3wt% polyvinyl alcohol binder, granulating and dry pressing to make green sheet.
(5)烧结：将所得坯片在950℃下烧结，保温1小时后，在炉中自然冷却至室温，制得低温共烧陶瓷材料。(5) Sintering: The obtained green sheet was sintered at 950° C., kept for 1 hour, and then naturally cooled to room temperature in a furnace to obtain a low-temperature co-fired ceramic material.
本实施例中所制得低温共烧陶瓷材料的热膨胀系数为4.75×10-6/℃。该材料的气孔率为1.3％。The coefficient of thermal expansion of the low temperature co-fired ceramic material prepared in this example is 4.75×10 -6 /°C. The material has a porosity of 1.3%.
本发明提出的一种钙铝硼硅系玻璃+熔融石英体系低温共烧陶瓷材料及其制备方法，已通过实施例进行了描述，相关技术人员明显能在不脱离本发明的内容、精神和范围内对本文所述的内容进行改动或适当变更与组合，来实现本发明。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，他们都被视为包括在本发明的精神、范围和内容中。A low-temperature co-fired ceramic material of calcium aluminum borosilicate glass + fused silica system proposed by the present invention and its preparation method have been described through the examples, and those skilled in the art can clearly understand the present invention without departing from the content, spirit and scope of the present invention. Changes or appropriate changes and combinations are made to the content described herein to realize the present invention. In particular, it should be pointed out that all similar substitutions and modifications would be obvious to those skilled in the art, and they are all considered to be included in the spirit, scope and content of the present invention.
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