CN114409413A - 氮化硅陶瓷基板及其制造方法 - Google Patents
氮化硅陶瓷基板及其制造方法 Download PDFInfo
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- CN114409413A CN114409413A CN202111472033.2A CN202111472033A CN114409413A CN 114409413 A CN114409413 A CN 114409413A CN 202111472033 A CN202111472033 A CN 202111472033A CN 114409413 A CN114409413 A CN 114409413A
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- silicon nitride
- ceramic substrate
- nitride ceramic
- sintering
- temperature
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 title claims abstract description 141
- 229910052581 Si3N4 Inorganic materials 0.000 title claims abstract description 137
- 239000000758 substrate Substances 0.000 title claims abstract description 111
- 239000000919 ceramic Substances 0.000 title claims abstract description 84
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 239000000654 additive Substances 0.000 claims abstract description 17
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims description 92
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 45
- 238000000034 method Methods 0.000 claims description 32
- 229910052799 carbon Inorganic materials 0.000 claims description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 22
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 239000011230 binding agent Substances 0.000 claims description 21
- 238000000465 moulding Methods 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000004014 plasticizer Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 13
- 238000005498 polishing Methods 0.000 claims description 12
- 239000012752 auxiliary agent Substances 0.000 claims description 11
- 238000005266 casting Methods 0.000 claims description 9
- 238000004080 punching Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 230000000996 additive effect Effects 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- 239000011256 inorganic filler Substances 0.000 claims description 6
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000009736 wetting Methods 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- 239000012766 organic filler Substances 0.000 claims description 4
- 239000011265 semifinished product Substances 0.000 claims description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 239000000571 coke Substances 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- 239000000853 adhesive Substances 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 1
- 238000012216 screening Methods 0.000 claims 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000000843 powder Substances 0.000 description 21
- 238000010438 heat treatment Methods 0.000 description 14
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 description 12
- 229910002804 graphite Inorganic materials 0.000 description 9
- 239000010439 graphite Substances 0.000 description 9
- 229910052582 BN Inorganic materials 0.000 description 8
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- -1 polytetrafluoroethylene Polymers 0.000 description 8
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 8
- 239000004810 polytetrafluoroethylene Substances 0.000 description 8
- 238000005096 rolling process Methods 0.000 description 8
- 229910052814 silicon oxide Inorganic materials 0.000 description 8
- 238000004321 preservation Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000000704 physical effect Effects 0.000 description 4
- 229910021426 porous silicon Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000004359 castor oil Substances 0.000 description 3
- 235000019438 castor oil Nutrition 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000003746 surface roughness Effects 0.000 description 3
- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229920000881 Modified starch Polymers 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 2
- 239000011268 mixed slurry Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000012297 crystallization seed Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
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Abstract
本发明公开了一种氮化硅陶瓷基板,包括按质量分数占氮化硅陶瓷基板总体质量50%‑90%的氮化硅空心球体,剩余为添加剂和/或助剂以及无法去除的杂质。本发明氮化硅陶瓷基板,通过将氮化硅空心球体设置为主要材料,因其空心从而具备良好的导热率、密度较小和较低的相对介电常数,同时制备工艺简单,易于大批量生产。本发明还公开了上述氮化硅陶瓷基板的制造方法。
Description
技术领域
本发明涉及陶瓷基板材料技术领域,特别指一种氮化硅陶瓷基板及其制造方法。
背景技术
目前,随着电子产品的日益更新,对于电路基板的需求越来越高。其中,绝缘性,相对介电常数,导热率参数是电路基板特别关注的性能参数。随着集成度,大功率集成电路的出现,传统的PCB基板已经不能满足需求导热率以及可靠性的需求。目前,氮化硅陶瓷基板由于其出色的导热率被认为是未来大功率集成电路的主要基板选择,但相对介电常数较高,若在微波集成电路中使用,则会产生较大的电磁干扰,极大地影响电路性能,进而遏制了其在大功率微波集成电路中的应用。基于此,如公开号为CN102320856A的中国发明专利公开说明书公开了一种制备多孔氮化硅陶瓷材料的方法,包括如下步骤:a)将淀粉与水在40~90℃下搅拌,制得预凝胶化淀粉;b)向预凝胶化淀粉中加入氮化硅、烧结助剂、粘结剂及消泡剂,球磨使混合均匀,制得混合浆料;c)将步骤b)制得的混合浆料浇注成型,进行脱气、固化、使样品完全冻结及冷冻干燥处理,制得多孔氮化硅陶瓷坯体;d)升温脱除步骤c)制得的多孔氮化硅陶瓷坯体中的有机挥发物;e)进行烧结,烧结后样品随炉冷却,即得所述的多孔氮化硅陶瓷材料。上述方法一定程度上可以降低相对介电常数,提升其在大功率微波集成电路中的应用。但是,上述方案工艺过程复杂,徒增较高的成本,而且具备过多无法去除的杂质,影响了电路基板的可靠性。
而在公开号为CN02800712.3的中国发明专利公开说明书中,公开了一种多孔性陶瓷及其制造方法,其介电损失较小,但是其制作过程需要使用稀土材料,成本较高。因而,如何制备兼具绝缘性好,相对介电常数低,导热率高,质量轻,且成本低,制造方法简单,易于大批量生产的氮化硅陶瓷基板成为了业内亟需解决的技术问题。
发明内容
发明目的:为了克服现有技术中存在的不足,本发明提供一种相对介电常数低,导热率高,质量轻,且成本低,制造方法简单,易于大批量生产的氮化硅陶瓷基板。
技术方案:一种氮化硅陶瓷基板,包括:
按质量分数占氮化硅陶瓷基板总体质量50%-90%的氮化硅空心球体,剩余为添加剂和/或助剂以及无法去除的杂质。
进一步地,所述氮化硅空心球体占氮化硅陶瓷基板质量分数的60%-80%。
进一步地,氮化硅空心球体的直径范围为0.1μm-1000μm。
进一步地,氮化硅空心球体的壁厚范围为0.05μm -500μm。
进一步地,所述添加剂和/或助剂至少包括有机填料、无机填料、粘结剂、增塑剂、烧结剂中的一种或几种。
进一步地,所述氮化硅空心球体的气孔体积占所述氮化硅陶瓷基板总体积比例气孔率为15%-65%。
进一步地,所述氮化硅空心球体的气孔体积占所述氮化硅陶瓷基板总体积比例气孔率为30%-45%。
一种氮化硅陶瓷基板的制造方法,包括以下步骤:
将混合比例为质量份数60-65份的二氧化硅空心球体、20-26份的碳源、5-10份的烧结助剂、5-10份的氮化硅磨球和20-26份的无水乙醇球磨充分混合制得原料;
蒸发去除原料中的无水乙醇并过筛,过筛孔径为50μm -150μm;
在氮气环境下进行高温烧结成型得到氮化硅陶瓷基板。
进一步地,所述碳源为焦炭、碳粉、蔗糖、葡萄糖等含碳物中的一种或几种。
进一步地,氮气为高纯度氮气,氮气压力(0.2-4 MPa),流量1L/min-5L/min。
进一步地,烧结时加入按质量份数5-20份的催化剂。
进一步地,烧结助剂至少包括氧化铝、氧化钇、氧化镁中的一种。
进一步地,所述烧结成型的方法包括但不限于流延成型、干压成型。
进一步地,将所述原料过筛后,还包括以下步骤:
将所述原料润湿并加入烧结助剂、塑性剂、粘结剂混合球磨,混合均匀;
利用成型方法使基板成型,按需求抛光、打孔,并依次将基板金属化、排胶后得到半成品,进行第一次烧结;
再进行第二次烧结并保温后即得所需氮化硅陶瓷基板。
进一步地,所述第一次烧结中温度为1000-1300摄氏度,并保温2h-6h。
进一步地,所述第二次烧结中温度为1700-1900摄氏度,并保温4h-48h。
有益效果:本发明氮化硅陶瓷基板,通过将氮化硅空心球体设置为主要材料,因其空心从而具备良好的导热率、密度较小和较低的相对介电常数,同时制备工艺简单,易于大批量生产。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本发明提供了一种氮化硅陶瓷基板,包括:
按质量分数占氮化硅陶瓷基板总体质量50%-90%的氮化硅空心球体,剩余为添加剂和/或助剂以及无法去除的杂质。优选地,所述氮化硅空心球体占氮化硅陶瓷基板质量分数的60%-80%。氮化硅空心球体的直径范围为0.1μm-1000μm,直径越小,基板的初始粗糙度越低,后续加工难度越低。氮化硅空心球体的壁厚范围为0.05μm-500μm,壁厚越厚,则基板的物理性能越好。所述添加剂和/或助剂至少包括有机填料、无机填料、粘结剂、增塑剂、烧结剂中的一种或几种。具体地,参见以下实施例:
实施例1:
本实施例氮化硅陶瓷基板包括按质量分数占氮化硅陶瓷基板总体质量50%的氮化硅空心球体、25%的添加剂和25%的助剂。在本实施例中,添加剂为钛或其他金属类无机填料,用以提升物理性能,助剂为粘结剂、烧结剂和增塑剂,以利于基板成型。
本实施例氮化硅陶瓷基板的氮化硅空心球体的气孔体积占氮化硅陶瓷基板总体积比例气孔率为15%,经测试,导热率可达30W m -1K -1,介电常数7.5,介电损耗0.0001,绝缘耐力20kV/mm,电气电阻值10-14Ω・cm,破坏韧性为3 MPa/m,氮化硅陶瓷基板的弹性模量为36000 MPa,弯曲强度为700MPa。
实施例2:本实施例氮化硅陶瓷基板包括按质量分数占氮化硅陶瓷基板总体质量60%的氮化硅空心球体、30%的添加剂和10%的助剂。在本实施例中,添加剂为聚氨酯等合成树脂类有机填料,用以提升物理性能,助剂为粘结剂和增塑剂,以利于基板成型。
本实施例氮化硅陶瓷基板的氮化硅空心球体的气孔体积占氮化硅陶瓷基板总体积比例气孔率为30%,经测试,导热率可达55W m -1K -1,介电常数6.5,介电损耗0.0005,绝缘耐力16kV/mm,电气电阻值5*10-16Ω・cm,破坏韧性为5 MPa/m,氮化硅陶瓷基板的弹性模量为30000 MPa,弯曲强度为1500MPa。
实施例3:本实施例氮化硅陶瓷基板包括按质量分数占氮化硅陶瓷基板总体质量70%的氮化硅空心球体、10%的添加剂和20%的助剂。在本实施中,采用的添加剂为无机盐类无机填料,助剂为粘结剂和烧结剂,以利于基板成型。
本实施例氮化硅陶瓷基板的氮化硅空心球体的气孔体积占氮化硅陶瓷基板总体积比例气孔率为45%,经测试,导热率可达80W m -1K -1,介电常数6,介电损耗0.001,绝缘耐力12kV/mm,电气电阻值10-15Ω・cm,破坏韧性为7MPa/m,氮化硅陶瓷基板的弹性模量为24000 MPa,弯曲强度为1500MPa。
实施例4:本实施例氮化硅陶瓷基板包括按质量分数占氮化硅陶瓷基板总体质量80%的氮化硅空心球体、5%的添加剂和15%的助剂。在本实施例中,采用的添加剂为石墨或其他碳类或碳化物无机填料,采用的添加剂为助剂为烧结剂和增塑剂,以利于基板成型。
本实施例氮化硅陶瓷基板的氮化硅空心球体的气孔体积占氮化硅陶瓷基板总体积比例气孔率为60%,经测试,导热率可达105W m -1K -1,介电常数5.5,介电损耗0.005,绝缘耐力8kV/mm,电气电阻值5*10-15Ω・cm,破坏韧性为9MPa/m,氮化硅陶瓷基板的弹性模量为18000 MPa,弯曲强度为700MPa。
实施例5:本实施例氮化硅陶瓷基板包括按质量分数占氮化硅陶瓷基板总体质量90%的氮化硅空心球体和10%的助剂。在本实施例中,添加剂为聚酯纤维类合成树脂材料,用以提升物理性能,助剂为粘结剂和增塑剂,以利于基板成型。
本实施例氮化硅陶瓷基板的氮化硅空心球体的气孔体积占氮化硅陶瓷基板总体积比例气孔率为65%,经测试,导热率可达120W m -1K -1,介电常数4.5,介电损耗0.01,绝缘耐力5kV/mm,电气电阻值10-14Ω・cm,破坏韧性为10 MPa/m,氮化硅陶瓷基板的弹性模量为12000 MPa,弯曲强度为1500MPa。
本发明氮化硅陶瓷基板,通过将氮化硅空心球体设置为主要材料,因其空心从而具备良好的导热率、密度较小和较低的相对介电常数,同时制备工艺简单,易于大批量生产。
本发明还提供上述氮化硅陶瓷基板的制造方法,包括以下步骤:
S100:将混合比例为质量份数60-65份的二氧化硅空心球体、20-26份的碳源、5-10份的烧结助剂、5-10份的氮化硅磨球和无水乙醇球磨充分混合制得原料;
S200:蒸发去除原料中的无水乙醇并过筛,过筛孔径为50μm-150μm;
S300:在氮气环境下进行高温烧结成型得到氮化硅陶瓷基板。
具体地,在步骤S100中,将氧化硅空心球体、氮化硅磨球、碳源、烧结助剂和无水乙醇装入聚四氟乙烯球磨罐,滚动球磨,混合均匀。用旋转蒸发仪将原料中的乙醇除去,并过筛。置于涂敷氮化硼的石墨坩埚中,为了防止烧结原料受到污染和反应,再使用多功能炉在氮气环境下进行烧结。其中,球磨时间12h-48h,以得到充分球磨混合。高温条件为1650-1850摄氏度,以保证充分受热反应。
热碳还原法为氧化硅与碳与氮气在高温下烧结发生的氧化还原反应,生成氮化硅以及一氧化碳气体。方程式如下:
进一步地,所述碳源为焦炭、碳粉、蔗糖、葡萄糖等含碳物中的一种或几种,所述碳源成本较为低廉,可进一步降低制备成本。并且在制备过程中需保持碳源充足且过量。
进一步地,氮气为高纯度氮气,氮气压力设定为0.2-4 MPa,流量1L/min-5L/min,以满足制备过程中氮气充足,二氧化硅与氮气、碳源充分反应。
进一步地,烧结时加入按质量份数5-20份的催化剂,具体的可以为铁以加速反应。
进一步地,烧结助剂至少包括氧化铝、氧化钇、氧化镁中的一种。烧结方法包括但不限于气压烧结、热压烧结、热等静压烧结、常压烧结等。其中,在烧结温度最高时保温2-12h。其中,剩余的碳源,可在空气中600摄氏度,除碳4小时,以保证碳充分与二氧化硅反应。
在S300中,成型方法包括但不限于流延成型、干压成型等陶瓷成型方法。具体地,还包括以下步骤:
S310: 将经步骤S200所得原料润湿并加入烧结助剂、塑性剂、粘结剂混合球磨,混合均匀。具体地,可装入聚四氟乙烯球磨罐进行滚动球磨。
S320:利用成型方法使基板成型,按需求抛光、打孔,并依次将基板金属化、排胶后得到半成品,进行烧结。具体地,将所述半成品置于涂敷氮化硼的石墨坩埚中,使用多功能炉在氮气环境下进行烧结。
S330:烧结保温后即得所需氮化硅陶瓷基板。
烧结分为两次,S320中烧结温度为1000-1300摄氏度进行预烧结,保温2h-6h;S330中进行1700-1900摄氏度烧结,保温4-48h。
具体地,排胶方法包括但不限于热脱脂法等陶瓷排胶方法。
具体地,烧结助剂包含但不限于氧化铝、氧化钇、氧化镁等有机或无机助剂两种甚至三种混合使用。纯度99.9%以上,粒径20-500nm。
具体地,烧结方法包括但不限于气压烧结、热压烧结、热等静压烧结、常压烧结等。
具体地,成型方法包括但不限于流延成型、干压成型等陶瓷成型方法。
上述方法成本较低,无需成本高昂的稀土原料,且制备过程较为简单,仅需球磨混合和烧结即可,对于设备和人员的要求较低,适宜于大规模推广。
进一步地,本发明还提供具体的实施例如下:
实施例1:
本实施例选用直径0.1 μm的市售空心二氧化硅球体,纯度为95%,气孔率为20%,密度为2 g/cm3。碳源选用市售碳粉,粉末状,200目。Al2O3–Y2O3作为烧结助剂,纯度99.9%,粒径500nm。
首先,为了获得氮化硅空心球体粉料,将空心氧化硅球体、氮化硅磨球、碳源、烧结助剂和无水乙醇装入聚四氟乙烯球磨罐(型号QM-QX4),滚动球磨 12 h,混合均匀。其中,混合材料的质量分数分别为氧化硅球体64.3%,碳粉25.7%,烧结助剂5%,氮化硅磨球5%。原料混合均匀后,用旋转蒸发仪将浆料中的酒精除去,干燥后过 100 目筛(孔径 150 μm)。将过筛后的粉体置于涂敷氮化硼的石墨坩埚中,使用多功能炉(型号High multi–5000 )进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为1MPa,烧结温度为1650摄氏度,保温2小时。烧结后,通入空气,降温至600摄氏度,除碳保温4小时,获得氮化硅空心球体粉料。空心结构的氮化硅球体,气孔率(所以空心球的气孔体积占总体积比例)为15%。
氮化硅球体的直径范围为0.2 μm。空心球体的壁厚度为0.15 μm。
将氮化硅空心球体粉料用水润湿并加入分散剂蓖麻油、烧结助剂Al2O3–Y2O3、塑性剂二丙二醇二苯甲酸酯、粘结剂聚乙烯醇缩丁醛混合装入聚四氟乙烯球磨罐,滚动球磨12h,混合均匀。其中,混合比例为质量分数80%氮化硅空心球体粉料,5%烧结助剂、5%塑性剂、5%粘结剂、5%氮化硅磨球。通过流延机流延成平整膜带(型号LY-250-02-P)。后进行干燥使溶剂蒸发,粘结剂在陶瓷粉末之间形成网状结构,得到陶瓷生坯。利用打孔机进行打孔,基板通过丝网印刷进行金属化,后进行加热排胶,加热温度无1摄氏度/分钟到300度,后0.5摄氏度/分钟到700摄氏度,后1摄氏度/分钟到900摄氏度。将排胶后的生坯置于涂敷氮化硼的石墨坩埚中,使用多功能炉在氮气环境下进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为2MPa,烧结分为两次,首先,温度为1000摄氏度进行预烧结,保温2h,后进行1800摄氏度烧结,保温12h。对成型基板进行化学机械抛光,抛光精度为50 nm。得到氮化硅陶瓷基板。
氮化硅球体所占基板的质量分数为85%,密度为2.45 g/cm3,基板的导热率为120W·M-1K-1。介电常数为7.5,介电损耗为0.0001。基板的电气电阻值10-16Ω・cm,绝缘耐力20kV/mm。基板的弯曲强度为700 MPa。基板的破坏韧性为3 MPa/m,弹性模量为36000 MPa。经抛光,表面粗糙为50 nm,满足高精度的需求。
实施例2:
本实施例选用直径50 μm的市售空心二氧化硅球体,纯度为95%,气孔率为50%,密度为1.2 g/cm3。碳源选用市售碳粉,粉末状,200目。Al2O3–Y2O3作为烧结助剂,纯度99.9%,粒径500nm。
首先,为了获得氮化硅空心球体粉料,将空心氧化硅球体、氮化硅磨球、碳源、烧结助剂和无水乙醇装入聚四氟乙烯球磨罐(型号QM-QX4),滚动球磨12 h,混合均匀。其中,混合材料的质量分数分别为氧化硅球体64.3%,碳粉25.7%,烧结助剂5%,氮化硅磨球5%。原料混合均匀后,用旋转蒸发仪将浆料中的酒精除去,干燥后过100目筛(孔径 150 μm)。将过筛后的粉体置于涂敷氮化硼的石墨坩埚中,使用多功能炉(型号High multi–5000 )进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为1MPa,烧结温度为1650摄氏度,保温2小时。烧结后,通入空气,降温至600摄氏度,除碳保温4小时,获得氮化硅空心球体粉料。空心结构的氮化硅球体,气孔率(所以空心球的气孔体积占总体积比例)为35%。氮化硅球体的直径约为50 μm。空心球体的壁厚度为15 μm。
将氮化硅空心球体粉料用水润湿并加入分散剂蓖麻油、烧结助剂Al2O3–Y2O3、塑性剂二丙二醇二苯甲酸酯、粘结剂聚乙烯醇缩丁醛混合装入聚四氟乙烯球磨罐,滚动球磨12h,混合均匀。其中,混合比例为质量分数75%氮化硅空心球体粉料,5%烧结助剂、5%塑性剂、10%粘结剂、5%氮化硅磨球。
通过流延机流延成平整膜带(型号LY-250-02-P)。后进行干燥使溶剂蒸发,粘结剂在陶瓷粉末之间形成网状结构,得到陶瓷生坯。利用打孔机进行打孔,基板通过丝网印刷进行金属化,后进行加热排胶,加热温度无1摄氏度/分钟到300度,后0.5摄氏度/分钟到700摄氏度,后1摄氏度/分钟到900摄氏度。将排胶后的生坯置于涂敷氮化硼的石墨坩埚中,使用多功能炉在氮气环境下进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为2MPa,烧结分为两次,首先,温度为1000摄氏度进行预烧结,保温2h,后进行1800摄氏度烧结,保温12h。对成型基板进行化学机械抛光,抛光精度为100 nm。得到氮化硅陶瓷基板。
氮化硅球体所占基板的质量分数为80%,密度为1.85 g/cm3,基板的导热率为80W·M-1K-1。介电常数为6.5,介电损耗为0.001。基板的电气电阻值5*10-15Ω・cm,绝缘耐力15kV/mm。基板的弯曲强度为1000 MPa。基板的破坏韧性为5 MPa/m,弹性模量为24000 MPa。经抛光,表面粗糙为100 nm,满足高精度的需求。
实施例3:
本实施例选用直径100 μm的市售空心二氧化硅球体,纯度为95%,气孔率为80%,密度为0.6 g/cm3。碳源选用市售碳粉,粉末状,200目。Al2O3–Y2O3作为烧结助剂,纯度99.9%,粒径500nm。
首先,为了获得氮化硅空心球体粉料,将空心氧化硅球体、氮化硅磨球、碳源、烧结助剂和无水乙醇装入聚四氟乙烯球磨罐(型号QM-QX4),滚动球磨12 h,混合均匀。其中,混合材料的质量分数分别为氧化硅球体64.3%,碳粉25.7%,烧结助剂5%,氮化硅磨球5%。原料混合均匀后,用旋转蒸发仪将浆料中的酒精除去,干燥后过100目筛(孔径 150 μm)。将过筛后的粉体置于涂敷氮化硼的石墨坩埚中,使用多功能炉(型号High multi–5000 )进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为1MPa,烧结温度为1650摄氏度,保温2小时。烧结后,通入空气,降温至600摄氏度,除碳保温4小时,获得氮化硅空心球体粉料。空心结构的氮化硅球体,气孔率(所以空心球的气孔体积占总体积比例)为35%。氮化硅球体的直径约为100 μm。空心球体的壁厚度为30 μm。
将氮化硅空心球体粉料用水润湿并加入分散剂蓖麻油、烧结助剂Al2O3–Y2O3、塑性剂二丙二醇二苯甲酸酯、粘结剂聚乙烯醇缩丁醛混合装入聚四氟乙烯球磨罐,滚动球磨12h,混合均匀。其中,混合比例为质量分数70%氮化硅空心球体粉料,10%烧结助剂、5%塑性剂、10%粘结剂、5%氮化硅磨球。
通过流延机流延成平整膜带(型号LY-250-02-P)。后进行干燥使溶剂蒸发,粘结剂在陶瓷粉末之间形成网状结构,得到陶瓷生坯。利用打孔机进行打孔,基板通过丝网印刷进行金属化,后进行加热排胶,加热温度无1摄氏度/分钟到300度,后0.5摄氏度/分钟到700摄氏度,后1摄氏度/分钟到900摄氏度。将排胶后的生坯置于涂敷氮化硼的石墨坩埚中,使用多功能炉在氮气环境下进行烧结。烧结的环境为高纯度氮气(99%),气压恒定为2MPa,烧结分为两次,首先,温度为1000摄氏度进行预烧结,保温2h,后进行1800摄氏度烧结,保温12h。对成型基板进行化学机械抛光,抛光精度为150 nm。得到氮化硅陶瓷基板。
氮化硅球体所占基板的质量分数为75%,密度为1.15 g/cm3,基板的导热率为30W·M-1K-1。介电常数为5.5,介电损耗为0.01。基板的电气电阻值10-14Ω・cm,绝缘耐力10kV/mm。基板的弯曲强度为1300 MPa。基板的破坏韧性为8 MPa/m,弹性模量为12000 MPa。经抛光,表面粗糙为150 nm,满足高精度的需求。
以上所述仅是本发明的优选实施方式,应当指出:对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (16)
1.一种氮化硅陶瓷基板,其特征在于,包括:
按质量分数占氮化硅陶瓷基板总体质量50%-90%的氮化硅空心球体,剩余为添加剂和/或助剂以及无法去除的杂质。
2.根据权利要求1所述的氮化硅陶瓷基板,其特征在于:所述氮化硅空心球体占氮化硅陶瓷基板质量分数的60%-80%。
3.根据权利要求1所述的氮化硅陶瓷基板,其特征在于:氮化硅空心球体的直径范围为0.1μm-1000μm。
4.根据权利要求3所述的氮化硅陶瓷基板,其特征在于:氮化硅空心球体的壁厚范围为0.05μm -500μm。
5.根据权利要求4所述的氮化硅陶瓷基板,其特征在于:所述添加剂和/或助剂至少包括有机填料、无机填料、粘结剂、增塑剂、烧结剂中的一种或几种。
6.根据权利要求1所述的氮化硅陶瓷基板,其特征在于:所述氮化硅空心球体的气孔体积占所述氮化硅陶瓷基板总体积比例气孔率为15%-65%。
7.根据权利要求6所述的氮化硅陶瓷基板,其特征在于:所述氮化硅空心球体的气孔体积占所述氮化硅陶瓷基板总体积比例气孔率为30%-45%。
8.一种氮化硅陶瓷基板的制造方法,其特征在于,包括以下步骤:
将混合比例为质量份数60-65份的二氧化硅空心球体、20-26份的碳源、5-10份的烧结助剂、5-10份的氮化硅磨球和20-26份的无水乙醇球磨充分混合制得原料;
蒸发去除原料中的无水乙醇并过筛,过筛孔径为50μm -150μm;
在氮气环境下进行高温烧结成型得到氮化硅陶瓷基板。
9.根据权利要求8所述制造方法,其特征在于,所述碳源为焦炭、碳粉、蔗糖、葡萄糖等含碳物中的一种或几种。
10.根据权利要求8所述制造方法,其特征在于,氮气为高纯度氮气,氮气压力为0.2-4MPa,流量1L/min-5L/min。
11.根据权利要求8所述制造方法,其特征在于,烧结时加入按质量份数5-20份的催化剂。
12.根据权利要求8所述制造方法,其特征在于,烧结助剂至少包括氧化铝、氧化钇、氧化镁中的一种。
13.根据权利要求8所述制造方法,其特征在于,所述烧结成型的方法包括但不限于流延成型、干压成型。
14.根据权利要求8所述制造方法,其特征在于,将所述原料过筛后,还包括以下步骤:
将所述原料润湿并加入烧结助剂、塑性剂、粘结剂混合球磨,混合均匀;
利用成型方法使基板成型,按需求抛光、打孔,并依次将基板金属化、排胶后得到半成品,进行第一次烧结;
再进行第二次烧结并保温后即得所需氮化硅陶瓷基板。
15.根据权利要求14所述制造方法,其特征在于,所述第一次烧结中温度为1000-1300摄氏度,并保温2h-6h。
16.根据权利要求14所述制造方法,其特征在于,所述第二次烧结中温度为1700-1900摄氏度,并保温4h-48h。
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CN109987944A (zh) * | 2019-03-06 | 2019-07-09 | 清华大学 | 一种高导热氮化硅陶瓷基板及其制备方法 |
CN113620716A (zh) * | 2021-09-02 | 2021-11-09 | 北京中材人工晶体研究院有限公司 | 一种氮化硅陶瓷基板及其制备方法 |
CN113773092A (zh) * | 2021-08-17 | 2021-12-10 | 广东工业大学 | 氮化硅陶瓷基板生坯及其制备方法、陶瓷基板 |
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CN109987944A (zh) * | 2019-03-06 | 2019-07-09 | 清华大学 | 一种高导热氮化硅陶瓷基板及其制备方法 |
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