CN1318622C - Method for preparing silicon particle intensifying aluminum based compound material with highly volume fraction - Google Patents
Method for preparing silicon particle intensifying aluminum based compound material with highly volume fraction Download PDFInfo
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- CN1318622C CN1318622C CNB2005100240326A CN200510024032A CN1318622C CN 1318622 C CN1318622 C CN 1318622C CN B2005100240326 A CNB2005100240326 A CN B2005100240326A CN 200510024032 A CN200510024032 A CN 200510024032A CN 1318622 C CN1318622 C CN 1318622C
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- slurry
- volume fraction
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- silicon particle
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- 239000011856 silicon-based particle Substances 0.000 title claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 title abstract description 22
- 150000001875 compounds Chemical class 0.000 title description 9
- 239000002002 slurry Substances 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000002131 composite material Substances 0.000 claims abstract 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 230000002787 reinforcement Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 10
- 238000004100 electronic packaging Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000001746 injection moulding Methods 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 229910052710 silicon Inorganic materials 0.000 description 14
- 239000010703 silicon Substances 0.000 description 14
- 238000005516 engineering process Methods 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 6
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 239000004160 Ammonium persulphate Substances 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 4
- 235000019395 ammonium persulphate Nutrition 0.000 description 4
- 238000007872 degassing Methods 0.000 description 4
- 230000010358 mechanical oscillation Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001540 jet deposition Methods 0.000 description 1
- 229910000833 kovar Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000009715 pressure infiltration Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
一种高体积分数硅颗粒增强铝基复合材料的制备方法，首先采用凝胶注模成型工艺，在NaOH溶液中加入硅颗粒和分散剂四甲基氢氧化铵混和均匀，再先后加入丙烯酰胺，过硫酸铵和亚甲基双丙烯酰胺搅拌均匀，把浆料浇注到模具里面进行反复排气和振荡，除去浆料内部的气泡，得到无微裂纹和断裂且分布均匀的材料预制件，然后把干燥好的预制件装入容器中进行真空反压浸渗，制备出高体积分数(55-72%)硅颗粒增强铝基复合材料。本发明所制备的复合材料具有良好的导热和适宜的热膨胀性能，材料密度＜2.5g/cm3，具有容易加工、无环境污染和成本低廉等特点，在电子封装等领域中具有广泛的应用前景。A method for preparing a high volume fraction silicon particle reinforced aluminum matrix composite material. First, a gel injection molding process is adopted, and silicon particles and a dispersant tetramethylammonium hydroxide are added to the NaOH solution and mixed evenly, and then acrylamide is added successively. Stir ammonium persulfate and methylenebisacrylamide evenly, pour the slurry into the mold for repeated exhaust and vibration, remove the air bubbles inside the slurry, and obtain a material preform with no microcracks and fractures and even distribution, and then put the The dried preform is put into a container for vacuum back pressure impregnation to prepare a high volume fraction (55-72%) silicon particle reinforced aluminum matrix composite. The composite material prepared by the invention has good thermal conductivity and suitable thermal expansion performance, material density <2.5g/cm 3 , has the characteristics of easy processing, no environmental pollution and low cost, and has wide application prospects in the fields of electronic packaging and the like .
Description
Technical field
The present invention relates to the preparation method of a kind of high-volume fractional (55-72%) silicon particle intensifying aluminum based compound material, the matrix material that makes can be applicable to fields such as Electronic Packaging, belongs to technical field of function materials.
Background technology
Along with the fast development of modern integrated circuits technology, unicircuit is more and more harsher to the performance requriements of packaged material.Except that requiring material must possess certain intensity and the erosion resistance, the most important thing is to require material to have high thermal, low thermal expansivity and alap density.Electronic package material commonly used at present can not satisfy above-mentioned requirements fully.Thermal expansivity as Kovar can mate with Si, GaAs, but thermal conductivity is too low; W/Cu density is too big; Al/SiC
pThe problem that has processing difficulties again.In this case, new A l/Si
pElectronic package material is because of the low (＜2.5g/cm of its density
3), thermal conductivity is good, thermal expansivity is low, easy processing, non-environmental-pollution and characteristics such as with low cost become the emphasis that people pay close attention to.The Al/Si for preparing high-volume fractional at present
pThe technology of matrix material mainly contains three kinds: a kind of is powder metallurgy method; Another kind is the method for jet deposition; The third is that mold pressing prepares prefabricated component, adopts the method for infiltration then.The material density of preceding two kinds of methods preparation is not high, and there is the problem that easily produces tiny crack and fracture in the inhomogeneous and silicon grain of stress distribution in the third method in mold process.The problem that exists in the above technology has adverse influence to the heat conduction and the intensity of material.
Summary of the invention
The objective of the invention is to deficiency at existing technology of preparing, a kind of preparation method of silicon particle intensifying aluminum based compound material with highly volume fraction is proposed, silicon grain volume fraction height in the matrix material of preparing, even particle distribution, non-microcracked and fracture on the fragility silicon grain, material has heat conduction preferably and suitable hot expansibility, has a good application prospect in fields such as Electronic Packaging.
For realizing such purpose, the present invention at first prepares high-volume-fraction Si particulate prefabricated component non-microcracked and that rupture and be evenly distributed with gel injection molding and forming technology, adopt the method for vacuum back-pressure infiltration then, prepare high-volume fractional (55-72vol%) silicon particle intensifying aluminum based compound material.Concrete preparation technology mainly comprises the steps:
1, select for use NaOH and deionized water preparation certain volume, the pH value is 9.6 solution.According to the volume fraction of the matrix material that will prepare, adding volume in above-mentioned solution is the 1.06-2.01 silicon grain doubly and the Tetramethylammonium hydroxide that accounts for silicon grain weight 0.05-0.1% of solution, stirs the slurry that obtains mixing 30 minutes;
2, in above-mentioned slurry, add the acrylamide that accounts for silicon grain weight 0.8%, stirred 5 minutes; And then add ammonium persulphate that accounts for silicon grain weight 0.06% and the methylene-bisacrylamide that accounts for silicon grain weight 0.01%, evenly stirred 5 minutes; The slurry that obtains is poured into the mould the inside, then mould is put into and carried out vacuum exhaust 2 minutes in the vacuum apparatus, take out the mould that slurry is housed then and carried out mechanical oscillation 1 minute, exhaust and vibration are 3 times so repeatedly, remove the inner bigger bubble that exists of slurry.
3, the mould that slurry is housed after the degasification being placed on temperature is 60 ℃ of loft drier the insides, sloughs mould after dry 2 hours, and adjusting the loft drier temperature then is 120 ℃, continues dry 12 hours;
4, the good prefabricated component of drying is packed in the container, carry out the infiltration of aluminium liquid in vacuum back-pressure device, the phase volume fraction that is enhanced is the silicon particle intensifying aluminum based compound material of 55-72%.
There is not the particle agglomeration phenomenon in the utilization Tetramethylammonium hydroxide as dispersion agent in the inventive method in the prefabricated component of preparing.Because there is not pressure process, so do not have tiny crack and phenomenon of rupture on the silicon grain in the prefabricated component of preparing.Prepared matrix material has good heat conduction and suitable hot expansibility, and the density of material is lower, has easy processing, non-environmental-pollution and characteristics such as with low cost, is with a wide range of applications in fields such as Electronic Packaging.
Embodiment
Further describe technical scheme of the present invention below by specific embodiment.
Embodiment 1:
1, selecting NaOH and deionized water secure ph for use is 9.6 solution 14.5ml, then 36g silicon grain (mean diameter is 30 μ m) and 0.036g Tetramethylammonium hydroxide is joined in the above-mentioned solution, stirs 30 minutes, obtains mixed uniform slurry;
2, in above-mentioned slurry, add the acrylamide of 0.28g, stirred 5 minutes; And then add the ammonium persulphate of 0.021g and the methylene-bisacrylamide of 0.0036g, evenly stirred 5 minutes; The slurry that obtains is poured in the mould, then mould is put into and carried out vacuum exhaust 2 minutes in the vacuum apparatus, take out the mould that slurry is housed then and carried out mechanical oscillation 1 minute, exhaust and vibration are 3 times so repeatedly, remove the inner bigger bubble that exists of slurry;
3, the mould that slurry is housed after the degasification being placed on temperature is 60 ℃ of loft drier the insides, sloughs mould after dry 2 hours, and adjusting the loft drier temperature then is 120 ℃, continues dry 12 hours;
4, the good prefabricated component of drying is packed in certain container, in vacuum back-pressure device, carry out the infiltration of aluminium liquid.Prepare the wild phase volume fraction and be 55vol% and have good heat conduction and the silicon particle intensifying aluminum based compound material of suitable hot expansibility.Density of material＜25g/cm
3
Embodiment 2:
1, selecting NaOH and deionized water secure ph for use is 9.6 solution 10.6ml, with the silicon grain of 36g (weight proportion of big or small silicon grain is: 60 μ m: 10 μ m=8: 2) and the 0.027g Tetramethylammonium hydroxide join in the above-mentioned solution, stirred 30 minutes, and obtained mixed uniform slurry;
2, in above-mentioned slurry, add the acrylamide of 0.28g, stirred 5 minutes; And then add the ammonium persulphate of 0.021g and the methylene-bisacrylamide of 0.0036g, evenly stirred 5 minutes; The slurry that obtains is poured in the mould, mould is put into carried out vacuum exhaust 2 minutes in the vacuum apparatus then, take out the mould that slurry is housed then and carried out mechanical oscillation 1 minute, exhaust and vibration are 3 times so repeatedly, remove slurry inner exist than air pocket;
3, the mould that slurry is housed after the degasification being placed on temperature is 60 ℃ of loft drier the insides, sloughs mould after dry 2 hours, and adjusting the loft drier temperature then is 120 ℃, continues dry 12 hours;
4, the good prefabricated component of drying is packed in certain container, in vacuum back-pressure device, carry out the infiltration of aluminium liquid.Prepare the wild phase volume fraction and be 67vol% and have good heat conduction and the silicon particle intensifying aluminum based compound material of suitable hot expansibility.
Embodiment 3:
1, selecting NaOH and deionized water secure ph for use is 9.6 solution 7.7ml, with the silicon grain of 36g (weight proportion of big or small silicon grain is: 60 μ m: 10 μ m=8: 2) and the 0.018g Tetramethylammonium hydroxide join in the above-mentioned solution, stirred 30 minutes, and obtained mixed uniform slurry;
2, in above-mentioned slurry is above-mentioned, add the acrylamide of 0.28g, stirred 5 minutes; And then add the ammonium persulphate of 0.021g and the methylene-bisacrylamide of 0.0036g, evenly stirred 5 minutes; The slurry that obtains is poured into the mould the inside, then mould is put into and carried out vacuum exhaust 2 minutes in the vacuum apparatus, take out the mould that slurry is housed then and carried out mechanical oscillation 1 minute, exhaust and vibration are 3 times so repeatedly, remove the inner bigger bubble that exists of slurry;
3, the mould that slurry is housed after the degasification being placed on temperature is 60 ℃ of loft drier the insides, sloughs mould after dry 2 hours, and adjusting the loft drier temperature then is 120 ℃, continues dry 12 hours;
4, the good prefabricated component of drying is packed in certain container, in vacuum back-pressure device, carry out the infiltration of aluminium liquid.Prepare the wild phase volume fraction and be 72vol% and have good heat conduction and the silicon particle intensifying aluminum based compound material of suitable hot expansibility.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100240326A CN1318622C (en) | 2005-02-24 | 2005-02-24 | Method for preparing silicon particle intensifying aluminum based compound material with highly volume fraction |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100240326A CN1318622C (en) | 2005-02-24 | 2005-02-24 | Method for preparing silicon particle intensifying aluminum based compound material with highly volume fraction |
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| Publication Number | Publication Date |
|---|---|
| CN1670229A CN1670229A (en) | 2005-09-21 |
| CN1318622C true CN1318622C (en) | 2007-05-30 |
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| CNB2005100240326A Expired - Fee Related CN1318622C (en) | 2005-02-24 | 2005-02-24 | Method for preparing silicon particle intensifying aluminum based compound material with highly volume fraction |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8795695B2 (en) | 2011-08-15 | 2014-08-05 | The Procter & Gamble Company | Personal care methods |
| US9333151B2 (en) | 2011-04-04 | 2016-05-10 | The Procter & Gamble Company | Home care articles and methods |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104611590B (en) * | 2015-01-21 | 2017-06-13 | 上海交通大学 | High-volume fractional primary silicon reinforced aluminum matrix composites dilution extruding filtering preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6228299B1 (en) * | 1997-09-16 | 2001-05-08 | Ut-Battelle, Llc | Gelcasting compositions having improved drying characteristics and machinability |
| CN1328167A (en) * | 2001-06-07 | 2001-12-26 | 上海交通大学 | Semi-solid coagulation method for preparing antiwear Zn-Al alloy containing high-volume-fraction Si |
| CN1393572A (en) * | 2001-06-22 | 2003-01-29 | 中国科学院金属研究所 | SiAl alloy with low expansibility and high thermal conductivity |
-
2005
- 2005-02-24 CN CNB2005100240326A patent/CN1318622C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6228299B1 (en) * | 1997-09-16 | 2001-05-08 | Ut-Battelle, Llc | Gelcasting compositions having improved drying characteristics and machinability |
| CN1328167A (en) * | 2001-06-07 | 2001-12-26 | 上海交通大学 | Semi-solid coagulation method for preparing antiwear Zn-Al alloy containing high-volume-fraction Si |
| CN1393572A (en) * | 2001-06-22 | 2003-01-29 | 中国科学院金属研究所 | SiAl alloy with low expansibility and high thermal conductivity |
Non-Patent Citations (1)
| Title |
|---|
| 高含量Si_p/Al复合材料的无压浸渗机制 胡锐 朱冠勇 白海琪 李金山 傅恒志，中国有色金属学报，第14卷第11期 2004 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9333151B2 (en) | 2011-04-04 | 2016-05-10 | The Procter & Gamble Company | Home care articles and methods |
| US9592181B2 (en) | 2011-04-04 | 2017-03-14 | The Procter & Gamble Company | Personal care articles and methods |
| US8795695B2 (en) | 2011-08-15 | 2014-08-05 | The Procter & Gamble Company | Personal care methods |
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| Publication number | Publication date |
|---|---|
| CN1670229A (en) | 2005-09-21 |
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