CN103413780A - Method for manufacturing three-dimensional through hole interconnection structure based on molten glass skeleton - Google Patents

Method for manufacturing three-dimensional through hole interconnection structure based on molten glass skeleton Download PDF

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CN103413780A
CN103413780A CN 201310365926 CN201310365926A CN103413780A CN 103413780 A CN103413780 A CN 103413780A CN 201310365926 CN201310365926 CN 201310365926 CN 201310365926 A CN201310365926 A CN 201310365926A CN 103413780 A CN103413780 A CN 103413780A
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molten glass
silicon
silicon layer
glass
skeleton
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CN 201310365926
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Chinese (zh)
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CN103413780B (en )
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孙道恒
占瞻
周如海
李益盼
蔡建发
陈梦月
王凌云
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厦门大学
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Abstract

The invention discloses a method for manufacturing a three-dimensional through hole interconnection structure based on a molten glass skeleton, and relates to the interconnection technology of silicon through holes. Grooves are etched in a silicon layer, and silicon columns are formed. A screen printing plate with a pattern is made to align at the etched pattern of the silicon layer. Glass powder is arranged on the screen printing plate. The glass powder is extruded in the vertical direction to be filled into the grooves, and the screen printing plate is moved away. The glass powder on the surfaces of the tops of the silicon columns is removed. The silicon layer filled with the glass powder is heated and molten, no bubble exists inside the silicon layer, a molten glass structure is obtained after cooling, the silicon layer of the obtained molten glass structure is arranged in etching liquid, the remaining molten glass structure on the surfaces of the tops of the silicon columns is removed by the adoption of the wet etching technology, and the molten glass skeleton inside the grooves is obtained. By the adoption of the mechanical lapping mode, the lower portion of the silicon layer is machined in a thinned mode until the bottoms of the silicon columns are exposed out of the lower portion of the silicon layer, then, lapping damage is repaired by the adoption of the chemical mechanical polishing mode, and therefore the three-dimensional through hole interconnection structure based on the molten glass skeleton is obtained.

Description

一种基于熔融玻璃骨架的三维通孔互联结构制作方法技术领域 A three-dimensional structure manufacturing method of the through-hole interconnection Field based molten glass skeleton

[0001] 本发明涉及硅通孔互联技术,尤其是涉及一种基于熔融玻璃骨架的三维通孔互联结构的制作方法。 [0001] The present invention relates to silicon via interconnect technology, especially relates to a method for manufacturing a three-dimensional configuration of the through-hole interconnection based molten glass skeleton.

背景技术 Background technique

[0002] 基于硅通孔互联的三维集成是一种全新的封装技术,它可以提供垂直的方向的电学信号的互联,降低连线的寄生电容与功耗,提高传输速度。 [0002] TSV interconnect dimensional integration is based on a new packaging technology, it can provide a direction perpendicular to an electrical signal interconnections, reduce the parasitic capacitance of wiring and power consumption, increase the transmission speed. 同时可大大提升封装的密集度,减小芯片的尺寸,广泛应用于集成电路(IC)以及微机电系统(MEMS)的跨层连接。 At the same time can greatly enhance the package density, reducing the size of the chip, it is widely used in integrated circuits (IC) and cross-layer micro-electromechanical systems (MEMS) is connected.

[0003] 传统的硅通孔互联技术(TSV)制作方法主要包括:硅通孔的制作、硅通孔的绝缘和硅通孔的填充。 [0003] The conventional silicon vias interconnect technology (TSV) manufacturing method including: an insulating and filling the TSV produced, the TSV TSV. 其工艺流程参见图1,可以归纳为:步骤1,采用干法刻蚀工艺(DRIE)制备高深宽比的硅通孔,如图1 (a)所示;步骤2,采用等离子化学气相沉积在刻蚀硅片以及通孔内表面生长氮化硅薄膜(Si3N4)或者二氧化硅薄膜(SiO2),如图1 (b)所示;步骤3,通孔内制作种子层,如图1 (c)所示;步骤4,通孔内采用电镀工艺,完全填充金属,如图1 (d)所示;步骤5,采用机械研磨工艺,去除背面硅层,并且抛光,得到如图1 (e)所示硅通孔互联结构。 Referring to Figure 1 the process which can be summarized as follows: Step 1, using silicon vias (the DRIE) dry etching process preparing high aspect ratio, FIG. 1 (a) below; Step 2, by plasma chemical vapor deposition and etching the silicon nitride film growth surface of the through-hole (Si3N4) film or a silicon dioxide (SiO2), FIG. 1 (b) below; step 3, the through hole making the seed layer, as shown in FIG 1 (c ) shown; step 4, using the through-hole plating process, the metal is completely filled, as shown in FIG 1 (d) below; step 5, using mechanical polishing process, the back surface of the silicon layer is removed, and polishing, to give FIG 1 (e) TSV interconnect structure shown in FIG.

[0004]目前,由于TSV制作方法中的干法刻蚀技术已经可以制作小直径、高深宽比的通孔,故主要限制硅通孔互联的是生长绝缘层的可靠性以及电镀工艺两个方面。 [0004] Currently, due to the dry etching of TSV fabrication method already made a small diameter, high aspect ratio through-holes, it is mainly restricted TSV interconnect insulating layer is grown as well as the reliability of the plating process both . 如公开号为CN101540295B的中国专利,发明名称为“一种TSV通孔的绝缘层的制备方法”中提出高深宽比的通孔会对生长的绝缘层性能造成影响,进而导致粘附性下降最终失效;如公开号为CN1260398C的中国专利,发明名称为“电解铜电镀液”中提出,电镀工艺也会由于通孔尺寸缩小而难度增加。 As disclosed in Chinese patent No. CN101540295B, entitled "method for preparing an insulating layer TSV vias' properties of the insulating layer in the through hole made high aspect ratio will affect the growth, eventually leading to decreased adhesion failure; the Chinese Patent Publication No., entitled CN1260398C as "electrolytic copper plating solution" in the proposed plating process will be reduced in size since the through hole more difficult.

[0005] 玻璃粉是一种广泛应用于涂·覆浆料等方面的颗粒态玻璃,其尺寸可依据制备工艺从微米级到纳米级变化,且其熔融温度以及热膨胀系数能够通过改变配比成分进行调节。 [0005] The glass frit is a widely used particulate glass-coated areas slurry coating and the like, which may be prepared according the size from the micron to nanometer process level changes, and the melting temperature and the thermal expansion coefficient is possible by changing the composition ratio adjusted.

发明内容 SUMMARY

[0006] 本发明的目的在于克服传统TSV制作方法中存在生长层绝缘性能弱,电镀工艺加工困难、成本高、可靠性差等问题,提供一种可制作小线宽、可靠性高基于熔融玻璃骨架的三维通孔互联结构制作方法。 [0006] The object of the present invention to overcome the weak growth layer insulating properties, processing difficulties electroplating process, high costs, poor reliability, to provide a line width can be made small, and high reliability based on the skeleton of the molten glass present in the conventional manufacturing method TSV a method of making a three-dimensional network structure through holes.

[0007] 本发明所述基于熔融玻璃骨架的三维通孔互联结构制作方法,包括以下步骤: [0007] A method for fabricating a three-dimensional network structure of the present invention is a through hole-based skeleton molten glass, comprising the steps of:

[0008] I)在硅层上,刻蚀出沟槽,同时形成凸起的硅柱; [0008] I) on the silicon layer, etching trenches, while forming a silicon pillar projection;

[0009] 2)将带有图案的丝网版与硅层刻蚀后的图案对准,保证丝网版上镂空图案覆盖于刻蚀出的沟槽上,硅层其余区域部分被丝网版保护;将玻璃粉置于丝网版上,再采用平板在竖直方向反复挤压,使玻璃粉填充沟槽,然后刮去多余玻璃粉,并移走丝网版; [0009] 2) The screen plate after the silicon layer is etched with a pattern of pattern alignment, to ensure that the screen plate covers the hollow pattern etched trenches, remaining portions of the silicon layer is screen area Edition protection; glass frit is placed on the screen plate, and then re-pressing by plate in the vertical direction, so that the glass frit filling the trench, and then scrape off the excess glass frit, and removing the screen plate;

[0010] 3)采用粘性胶纸粘附去除硅柱顶部表面存在的玻璃粉; [0010] 3) The removal of the viscous adhesive tape present in the glass frit top surface of the silicon column;

[0011] 4)在真空条件下,将填充有玻璃粉硅层进行加热,使玻璃粉完全熔融,并且内部无气泡,再冷却至室温,得到熔融玻璃结构,该熔融玻璃结构包括硅柱顶部表面残留熔融玻璃以及沟槽内的熔融玻璃骨架; [0011] 4) under vacuum, filled with glass frit silicon layer is heated to completely melt the glass frit, and the inner bubble-free, and then cooled to room temperature to obtain a molten glass structure, the molten glass surface of the silicon pillar structure includes a top the residue of molten glass and the molten glass within the trench skeleton;

[0012] 5)将得到熔融玻璃结构的硅层置于腐蚀液中,采用湿法腐蚀工艺去除硅柱顶部表面残留的熔融玻璃结构,得到沟槽内的熔融玻璃骨架; [0012] 5) The resulting molten glass disposed silicon layer structure etching solution, wet etching process to remove the top surface of the molten glass structure remaining silicon pillars to obtain molten glass skeleton within the trench;

[0013] 6)采用机械研磨方式,将硅层下部减薄加工至暴露出硅柱底部,再采用化学机械抛光方式修复研磨损伤,从而获得所述基于熔融玻璃骨架的三维通孔互联结构。 [0013] 6) using a mechanical grinding method, the lower silicon layer is thinned to expose the silicon to the bottom of the column processing, and then chemical mechanical polishing abrasive damage repair mode, so as to obtain a three-dimensional structure of interconnecting through hole-based molten glass skeleton.

[0014] 在步骤I)中,所述硅层可为硅片、SOI片或表面加工有集成电路的标准硅片。 [0014] In step I), the silicon layer may be a silicon wafer, the SOI substrate or a surface processed with a standard silicon integrated circuit. 硅层最好在制作硅柱的区域采用局部高掺杂,这样使制作出来的硅柱具有更好的导电性。 Preferably the silicon layer using a local highly doped region produced in the silicon pillar, so that the silicon pillar having produced the better conductivity. 所述沟槽和硅柱可采用光刻与DRI的组合工艺制成。 The trenches and the silicon column may be employed in combination with a lithographic process DRI made.

[0015] 在步骤2)中,所述玻璃粉采用纳米级颗粒的玻璃粉,玻璃粉的热膨胀系数与硅层接近,这样可减少所造成的内应力;在玻璃粉填充沟槽的过程中,在控制竖直方向平板挤压压力的同时,可采用机械振动等辅助分散方式,使玻璃粉完全填充沟槽。 [0015] In step 2), the glass frit glass frit using nanoscale particles, glass frit and the coefficient of thermal expansion close to the silicon layer, which can reduce the internal stress caused; glass frit in the process of filling the trench, while controlling the vertical direction of the plate pressing pressure, vibration and other auxiliary machinery can be employed in a decentralized manner, in the frit completely fill the trenches.

[0016] 在步骤4)中,所述加热是将填充有玻璃粉的硅层置于真空管式炉内进行加热,在真空条件下,加热温度最好高于玻璃粉熔融温度100〜200°c。 [0016] In step 4), the heating of the glass frit is filled with a silicon layer disposed vacuum heating furnace, under vacuum, heating temperature is preferably higher than the melting temperature of the glass frit 100~200 ° c .

[0017] 在步骤5)中,所述腐蚀液最好为氢氟酸溶液。 [0017] In step 5), preferably the etching solution is hydrofluoric acid solution.

[0018] 与现有技术比较,本发明的有益效果如下: [0018] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0019] 本发明所述的基于熔融玻璃骨架的三维通孔互联结构制作方法,利用了玻璃粉对微加工中刻蚀沟槽进行填充,并且经过后续烧结、减薄工艺,获得一类基于熔融玻璃骨架的三维通孔互联结构。 [0019] The present invention method for manufacturing a three-dimensional network structure of the molten glass through hole based on the skeleton, the use of glass frit micromachining etching groove is filled, and through subsequent sintering, the thinning process, to obtain a class of molten three-dimensional structure of the glass through-hole interconnect backbone. 由于采用熔融玻璃粉作为通孔结构骨架,体硅作为电连接结构。 Since the molten glass powder employed as the structural framework of the through holes, electrical connection structure as bulk silicon. 因此不需要生长绝缘层,简化了工艺步骤;与传统硅通孔绝缘化后金属填充工艺中密度受限制、绝缘性差、连接可靠性低相比,极大的提高了通孔互联技术的通孔密度、电学连接可靠性以及具有更好的绝缘性。 Growth insulating layer is not necessary, the process is simplified steps; TSV after the conventional insulated metal filling process density is limited, poor insulation, the connection reliability is low compared to the through-hole greatly improves the through-hole interconnect technology density, electrical connection reliability and a better insulation. 可应用于集成电路以及微机电系统跨层连接的通孔互联制作。 It can be used in integrated circuits and interconnecting vias produced across the MEMS layer connection.

附图说明 BRIEF DESCRIPTION

[0020] 图1为现有常用的硅通孔互联结构制作工艺流程示意图。 [0020] FIG. 1 is a schematic view of the conventional production process commonly TSV interconnect structure. 图1中各标记表示: Figure 1 each denote:

1.刻蚀槽;2.娃柱;5.绝缘层;6.种子层;7.电镀金属;01.娃片。 1. etched grooves; 2. baby column; 5. insulating layer; 6 seed layer;. Metal plating 7; 01 baby sheet.

[0021] 图2为本发明所述的基于熔融玻璃骨架的三维通孔互联结构实施例制作流程示意图。 [0021] FIG. 2 based on the three-dimensional structure of the molten glass through hole interconnect backbone schematic diagram of the production process embodiment of the present invention. 图2中各标记表示:1.刻蚀槽;2.硅柱;3.纳米玻璃粉;4.熔融玻璃结构;401.熔融玻璃骨架;402.硅柱顶部表面残留熔融玻璃;01.硅片;02.丝网版;03.平板。 FIG 2 each denote: 1 etch tank; second silicon pillar; 3 nanometers glass frit; molten glass structure 4; 401 skeleton molten glass; a top surface of the silicon pillar 402 remained molten glass; wafer 01...... ; 02 screen version; 03 flat.

[0022] 图3为采用本发明所述的基于熔融玻璃骨架的三维通孔互联结构实施例制作方法所得到的产品结构不意图。 [0022] FIG. 3 is not intended product structure produced using the method of Example of the obtained through hole interconnect structure based on a three-dimensional skeleton of the molten glass of the present invention. 图3中各标记表不:2.娃柱;401.熔融玻璃骨架;01.娃片。 In Figure 3 each mark table is not: baby column 2; 401 skeleton molten glass; baby sheet 01..

[0023] 图4为硅柱上端带有残留熔融玻璃结构的三维通孔互联结构断面SEM示意图。 [0023] FIG. 4 is an SEM schematic cross section of a three-dimensional structure of the through-hole interconnection structure remained molten glass with a silicon column end. 图4中各标记表示:2.硅柱;401.熔融玻璃骨架;402.硅柱顶部表面残留熔融玻璃。 In FIG. 4 each denote: a second silicon pillar; 401 skeleton molten glass; a top surface of the silicon pillar 402 remained molten glass....

具体实施方式 detailed description

[0024] 参见图2,本发明所述的基于熔融玻璃骨架的三维通孔互联结构实施例制作流程,包括以下步骤: [0024] Referring to Figure 2, the production process of the present invention based on the embodiment of the three-dimensional structure of the through-hole interconnection molten glass skeleton, comprising the steps of:

[0025] I)在硅片01上采用光刻与DRIE的组合工艺加工,得到沟槽I和硅柱2,如图2(a)所示; [0025] I) using a combination of DRIE and photolithography processing technology on a silicon wafer 01, to obtain silicon pillar I and grooves (a), 2, 2;

[0026] 2)采用带有镂空图案、厚度为200 μ m丝网版02,使其与硅片01对准,保证镂空图案与硅片Ol刻蚀硅柱区域对齐,而硅片01其余区域被丝网版保护。 [0026] 2) The remaining hollow pattern region having a thickness of 200 μ m screen plate 02, so that it is aligned with the wafer 01, and the wafer to ensure Ol hollow pattern etched silicon pillar region alignment, the wafer 01 protected screen version. 选用纳米玻璃粉3(熔点530°C,热膨胀系数4.0)置于丝网版02内,采用平板03竖直方向往复运动,反复挤压纳米玻璃粉3,使沟槽内完全填充纳米玻璃粉3,并且利用刀片刮去高于丝网版的纳米玻璃粉3,如图2(b)所示; Selection nano 3 glass frit (m.p. 530 ° C, the thermal expansion coefficient of 4.0) was placed inside the screen plate 02 by plate 03 reciprocates in the vertical direction, the re-pressing nano 3 glass frit, glass frit, so that complete filling of the trench 3 nanometers , and with a blade to scrape the screen plate above the glass frit nano 3, FIG. 2 (b) below;

[0027] 3)采用粘性胶纸,粘去硅柱2顶部表面大部分的纳米玻璃粉3,如图2(c)所示; [0027] 3) using a viscous adhesive tape, adhered to the surface of the silicon pillar glass frit most 2 nanometers top 3, FIG. 2 (c) below;

[0028] 4)将加工硅片01置于真空退火炉中,在KT2Pa的条件下,加热至630°C,保温2h,保证纳米玻璃粉3完全熔融并且内部无气泡,得到如图2 (d)所示熔融玻璃结构4,其中包括硅柱2顶部表面残留熔融玻璃402,以及沟槽I内的熔融玻璃骨架401 ; [0028] 4) The processed wafer 01 in a vacuum annealing furnace, at KT2Pa heated to 630 ° C, incubated 2h, ensure that the glass frit nano 3 completely melted and no air bubbles inside, to give FIG 2 (d ) shown in molten glass structure 4, which includes a top surface of the silicon column 2 remained molten glass 402, and the molten glass within the trench skeleton I 401;

[0029] 5)将加热后的硅片01静置于HF酸溶液中,控制腐蚀时间,使硅柱2顶部表面熔融玻璃402完全腐蚀,得到如图2(e)所示沟槽I内的玻璃骨架401 ; [0029] 5) The wafer was heated 01 stand in HF solution, etching time is controlled so that the top surface of the molten silicon pillar 2 402 etched glass, to give the 2 (e) in the trench I shown in FIG. a glass skeleton 401;

[0030] 6)采用研磨工艺将硅片01底部减薄至暴露出硅柱2底部,并采用化学机械抛光修复研磨造成的表面损伤,得到如图2(f)所示本发明所述的基于熔融玻璃骨架的三维通孔互联结构。 [0030] 6) a grinding process using a silicon wafer is thinned to expose the bottom of the silicon pillar 01 to the bottom 2, and the use of chemical mechanical polishing repair surface damage caused by grinding, to obtain the present invention based on FIG. 2 (f) shown in FIG. three-dimensional structure of the molten glass through-hole interconnect backbone.

[0031] 参见图3,图3为采用本发明所述的基于熔融玻璃骨架的三维通孔互联结构实施例制作方法所得到的产品结构示意图。 [0031] Referring to FIG. 3, FIG. 3 is a schematic three-dimensional product structure manufacturing method of the through-hole interconnect structure based on the embodiment of the molten glass skeleton obtained using the present invention.

[0032] 参见图4,图4为制作过程中硅柱2顶部表面残留熔融玻璃402的三维通孔互联结构的断面SEM示意图。 [0032] Referring to Figure 4, a schematic cross section of FIG. 4 SEM dimensional interconnect structure through hole 402 of the molten glass 2 is a top surface of the silicon pillar residue production process.

Claims (6)

  1. 1.一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,包括以下步骤: 1)在娃层上,刻蚀出沟槽,同时形成凸起的娃柱; 2)将带有图案的丝网版与硅层刻蚀后的图案对准,保证丝网版上镂空图案覆盖于刻蚀出的沟槽上,硅层其余区域部分被丝网版保护;将玻璃粉置于丝网版上,再采用平板在竖直方向反复挤压,使玻璃粉填充沟槽,然后刮去多余玻璃粉,并移走丝网版; 3)采用粘性胶纸粘附去除硅柱顶部表面存在的玻璃粉; 4)在真空条件下,将填充有玻璃粉硅层进行加热,使玻璃粉完全熔融,并且内部无气泡,再冷却至室温,得到熔融玻璃结构,该熔融玻璃结构包括硅柱顶部表面残留熔融玻璃以及沟槽内的熔融玻璃骨架; 5)将得到熔融玻璃结构的硅层置于腐蚀液中,采用湿法腐蚀工艺去除硅柱顶部表面残留的熔融玻璃结构,得到沟槽内 1. A three-dimensional structure manufacturing method of the through-hole interconnect backbone based molten glass, characterized by comprising the steps of: 1) layer on a baby, etched trenches, while forming convex baby column; 2) the tape the patterned silicon layer screen plate with the etched pattern alignment, to ensure that the screen plate covers the hollow pattern etched trenches, remaining region of the silicon layer is partially protected screen version; frit disposed the screen plate, and then re-pressing by plate in the vertical direction, so that the glass frit filling the trench, and then scrape off the excess glass frit, and removing the screen plate; 3) removing the adhesive tape sticky surface of the top silicon pillar the presence of glass frit; 4) under vacuum, filled with glass frit silicon layer is heated to completely melt the glass frit, and the inner bubble-free, and then cooled to room temperature to obtain a molten glass structure, the structure comprising a silicon pillar molten glass the residue of molten glass, and the top surface of the molten glass within the trench skeleton; 5) the resulting silicon layer is melted in the glass structure is placed in an etching solution, wet etching process to remove the top surface of the molten glass structure remaining silicon pillars to obtain the trench 熔融玻璃骨架; 6)采用机械研磨方式,将硅层下部减薄加工至暴露出硅柱底部,再采用化学机械抛光方式修复研磨损伤,从而获得本发明所述的基于熔融玻璃骨架的三维通孔互联结构。 Molten glass skeleton; 6) using a mechanical grinding method, the lower silicon layer is thinned to expose the bottom silicon pillar processing, then using chemical mechanical polishing abrasive damage repair embodiment, the present invention is to obtain a three-dimensional through-hole based on the molten glass skeleton interconnect structure.
  2. 2.如权利要求1所述的一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,在步骤I)中,所述硅层为硅片、SOI片或表面加工有集成电路的标准硅片。 2. one of the claims 1 through hole interconnection method of manufacturing three-dimensional structures based on the skeleton of the molten glass, characterized in that, in step I), the silicon layer is a silicon wafer, the SOI substrate has an integrated circuit or surface finish standard silicon.
  3. 3.如权利要求1所述的一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,在步骤I)中,所述硅层在制作硅柱的区域采用局部高掺杂,所述沟槽和硅柱采用光刻工艺与DRIE的组合工艺制成。 3. The one-dimensional claim 1 through hole interconnect structure fabrication method based on the skeleton of the molten glass, characterized in that, in step I), the silicon layer using a local highly doped region produced in the silicon pillar, the trenches and the silicon column using a combination of photolithography technology and DRIE process is made.
  4. 4.如权利要求1所述的一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,在步骤2)中,所述玻璃粉采用纳米级颗粒的玻璃粉,玻璃粉的热膨胀系数与硅层接近。 As claimed in one of the thermal expansion of the glass frit of claim 1 three-dimensional structure manufacturing method of the through-hole interconnect backbone based molten glass, wherein, in step 2), the glass frit glass frit using nanoscale particles, coefficient close to silicon layer.
  5. 5.如权利要求1所述的一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,在步骤4)中,所述加热是将填充有玻璃粉的硅层置于真空管式炉内进行加热,在真空条件下,加热温度高于玻璃粉熔融温度100〜200°C。 5. one of the claims 1 through hole interconnection method of manufacturing three-dimensional structures based on the skeleton of the molten glass, wherein, in step 4), the heating of the glass frit is filled with the silicon layer vacuum disposed formula the furnace was heated under vacuum conditions, temperature above the melting temperature of the glass frit 100~200 ° C.
  6. 6.如权利要求1所述的一种基于熔融玻璃骨架的三维通孔互联结构制作方法,其特征在于,在步骤5)中,所述腐蚀液为氢氟酸溶液。 One of the claims 1 6. The method of manufacturing three-dimensional network structure of the through-hole of the molten glass-based skeleton, wherein, in step 5), the etching solution is hydrofluoric acid solution.
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