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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Abstract
The present invention relates to a method for preparing a silicon particle intensifying aluminum based compound material with high volume fraction. Firstly, a gel-casting process is adopted, silicon particles and tetramethylammonium hydroxide as a dispersing agent are added to a NaOH solution, and the silicon particles, the tetramethylammonium hydroxide and the NaOH solution are uniformly mixed; acrylamide, ammonium persulfate and methylene bisacrylamide are added successively, and the mixed solution, the acrylamide, the ammonium persulfate and the methylene bisacrylamide are uniformly stirred so as to obtain slurry; the slurry is cast in a mold, and air bubbles in the slurry are removed by repeated air exhaust and oscillation so as to obtain a prefabricated member of the material, which has the advantages of no microcrack and fracture, and uniform distribution; then, the dried prefabricated member is loaded into a container, and infiltrated by vacuum counterpressure so as to prepare the silicon particle intensifying aluminum based compound material with high volume fraction (55 to 72%). The compound material prepared by the present invention has the characteristics of favorable thermal conductivity, suitable thermal expansion, easy processing, no environmental pollution, low cost, wide application prospect in electronic packaging and other fields, etc., and the density of the compound material is less than 2.5 g/cm<3>.
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)
1, a kind of preparation method of silicon particle intensifying aluminum based compound material with highly volume fraction is characterized in that comprising the steps:
1) selecting NaOH and deionized water secure ph for use is 9.6 solution, volume fraction according to 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, stirred 30 minutes, and obtained mixed uniform slurry;
2) in above-mentioned slurry, add the acrylamide account for silicon grain weight 0.8%, stirs and add ammonium persulphate that accounts for silicon grain weight 0.06% and the methylene-bisacrylamide that accounts for silicon grain weight 0.01% after 5 minutes again, evenly stirred 5 minutes; The slurry that obtains is poured into the mould the inside, 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 the inner bubble that exists of slurry;
3) 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%.
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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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| 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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| CN1670229A CN1670229A (en) | 2005-09-21 |
| CN1318622C true CN1318622C (en) | 2007-05-30 |
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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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| CN1670229A (en) | 2005-09-21 |
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