CN1332910C - Method for preparing high heatconducting aluminium nitride ceramic base sheets through powder metallurgical technique - Google Patents
Method for preparing high heatconducting aluminium nitride ceramic base sheets through powder metallurgical technique Download PDFInfo
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Abstract
The present invention belongs to the field of microelectronic packaging materials, particularly to a making method for an aluminum nitride ceramic base sheet with high thermal conduction through a powder metallurgical technology. In making the method, the ceramic base sheet with high thermal conduction is made through the five steps of powder preparation, glue addition, granulation, cold isostatic compaction, sintering and machine processing. In the making method, the main chemical components of used raw materials are 94 to 99 wt% of AlN and 1 to 6 wt% of sintering addition agent, wherein the sintering addition agent is one or more than one kind of Y2O3, Dy2O3, CaO, CaF2 and SrO. A binding agent used for the granulation of the powder is one kind of gasoline solution of buna with the concentration of 1 to 5 wt% and alcohol solution of ethyl cellulose and polyvinyl alcohol with the concentration of 1 to 12w%. Compared with the prior art, the present invention has the advantages of simple technology, easy control, good base sheet size adaptability, good base sheet size uniformity, high yield, high thermal conduction, good versatility and large-scale production suitability.
Description
Technical field
The invention belongs to the microelectronic packaging material field, be mainly used in the ceramic packing industry of microelectronics and power electronics industry, particularly a kind of method that adopts powder metallurgical technique to prepare high heat conduction aluminium nitride ceramic substrate.
Background technology
In the prior art, aluminium nitride material is low because of its thermal conductivity height, specific inductivity, thermal expansivity and silicon are complementary, advantage such as nontoxic becomes a kind of ideal electronic package material, can be used for instead of alumina and beryllium oxide material, and range of application is very wide.But the suitability for industrialized production technology of aluminium nitride chip does not obtain fine solution always, and the quality and the quantity of its high heat conduction substrate product all are difficult to satisfy the demand in market.Its major cause is that to prepare the aluminium nitride chip main method at present be casting method, as publication number is CN1557776A, open day be that on December 29th, 2004 and Granted publication number are CN1087010C, the day for announcing is that the patent on July 3rd, 2002 is described, at first the aluminium nitride slurry flow casting molding for preparing is prepared into biscuit film, biscuit film is prepared into aluminium nitride chip through binder removal, sintering.But casting method has its inherent shortcoming, and promptly the biscuit organic gel content of curtain coating is big, and the biscuit relative density is low, shrinks greatly in sintering process, lifts up song easily; And preparation also must increase stamping procedure during circular substrate, and the dimensional uniformity behind the sintering is difficult to guarantee that yield rate is lower simultaneously.Want to satisfy industrial production requirement, must look for another way.
Summary of the invention
The object of the present invention is to provide that a kind of technology is simple, easy to control, sizes of substrate adaptability and high conformity, yield rate height, thermal conductivity height, versatility be good, is applicable to that the employing powder metallurgical technique of large-scale production prepares the method for high heat conduction aluminium nitride ceramic substrate.
According to above-mentioned purpose, technical scheme of the present invention is to prepare aluminium nitride ceramic substrate with powder metallurgical technique, promptly by join powder, add the glue granulation, cold isostatic compaction, sintering, five steps of machining prepare the highly heat-conductive carbon/ceramic ceramic chip, its concrete steps are as follows:
1, the preparation of raw material powder: take by weighing an amount of AlN powder and sintering aid in proportion, in the mixer of packing into, add dehydrated alcohol by 1: 1 weight ratio, wet-mixed 5～15 hours is to evenly, then dry for standby;
2, add the glue granulation: the ratio in 400～600ml/kg in the confected materials powder adds the binding agent for preparing, after in mixed glue machine, mixing 0.5～2 hour, place baking oven at 40～80 ℃ of scope internal heating 10～40min, then with 100 mesh sieves screening granulation;
3, cold isostatic compaction: the powder after the granulation is packed in the flexible glue film, put into cold isostatic press compression moulding.The size of flexible glue film can be according to the diameter or the length and width size design of prepared substrate.Hydrostatic pressure is 150～220MPa, and the dwell time is 10～30min; Can require to carry out machining and shaping according to final sizes of substrate after the powder moulding;
4, sintering: with the blank of compression moulding 10
-1～10
-3Be heated to 500～800 ℃ through 2～4 hours under the pa state, be incubated 1～2 hour, so that remove the binding agent of adding; Feed nitrogen then, be warmed up to 1800～2400 ℃, be incubated 1.5～6 hours at 4～10 hours internal heating; Insulation finishes back outage, furnace cooling;
5, machining: the aluminium nitride blank that sinters is carried out machining by the desired size of substrate, the physical dimension that requires to substrate as cylindrical grinding or plane, cut into slices to the substrate thickness that needs with inner circle cutting machine again, grind then, polish, just obtain meeting the aluminium nitride chip of the high heat conduction of dimension precision requirement.
The used raw-material main chemical of above-mentioned preparation method is AlN94～99wt%, and all the other are sintering aid, and the Chemical Composition of sintering aid is Y
2O
3, Dy
2O
3, CaO, CaF
2, among the SrO any one or more, ratio is 1～6wt%; Wherein, the median size of AlN powder is 0.1～8 μ m, can adopt the powder that the self propagating high temperature synthesis method is produced or the reduction with carbon method is produced, and also can add the nanometer AlN of 0.1～10wt% with acceleration of sintering in the AlN powder.Sintering aid adopts commercially available chemically pure reagent, and addition can reduce with the reduction of AlN powder granularity.The used binding agent of powder granulation is that concentration is any in the spirituous solution of the gasoline solution of 1～5wt% sodium butadiene rubber or spirituous solution that concentration is 1～12wt% ethyl cellulose, polyvinyl alcohol.The present invention utilizes cold isostatic press compression moulding, and forming pressure is big, and biscuit is stressed respectively to unanimity, has guaranteed the consistence of performance.The common high temperature sintering furnace of sintering, logical nitrogen is protected.Shaping coreless grinding machine cylindrical grinding behind the sintering, is cut into slices by the thickness of substrate requirement with inner circle cutting machine to requiring size with the surface grinding machine face machined flat.
The present invention compared with prior art has the following advantages:
1, after the raw material granulation, the solvent of binding agent volatilizees fully substantially, does not participate in moulding process, but the biscuit direct sintering after the moulding;
2, the pressure during cold isostatic compaction is bigger, is generally 200Mpa, and the relative density of biscuit is higher after the moulding, helps densified sintering product, can prepare the substrate of high heat conduction;
3, biscuit is integral sintered, so the substrate of preparation does not have phenomenons such as warpage, the yield rate height;
4, size adaptability and high conformity.The physical dimension of substrate, thickness etc. can both accurately be guaranteed by machining means such as grindings;
5, can produce the goods of different shapes such as aluminium nitride crucible, temperature tube, insulating radiation plate simultaneously with this processing method, versatility is good, is suitable for large-scale industrial production.
Embodiment
According to preparation process of the present invention, choose different components and different technical parameters, prepare the aluminium nitride chip of three kinds of specifications and models altogether, preparation process is finished by operations such as joining powder, granulation, moulding, sintering, machining, and the density of substrate is all greater than 3.35g/cm
3, thermal conductivity is all greater than 190W/mK.The composition of material among the embodiment, processing parameter are as shown in table 1, and the performance of substrate is as shown in table 2.In order to compare, the substrate performance of Comparative Examples CN1087010C of the prior art, CN1557776A patent is listed in the table 2 simultaneously.Wherein sequence number 1-3 is the embodiment of the invention, and 4-7 is the prior art Comparative Examples.
The composition of table 1 embodiment of the invention, process parameter table
| Sequence number | 1 | 2 | 3 | ||
| The embodiment of the invention | Material composition (wt%) | AlN+3％Y 2O 3 | AlN+1.5％Y 2O 3+2.5％ Dy 2O 3 | AlN+2.0％Y 2O 3+1.5％ CaO+1.0％CaF 2+0.5％ SrO | |
| Powder mean particle sizes | 0.5μm | 3μm | 6μm | ||
| The binding agent kind | The gasoline solution of 4.5wt% sodium butadiene rubber | The spirituous solution of 3.5wt% ethyl cellulose | The spirituous solution of 7.5wt% polyvinyl alcohol | ||
| The binding agent add-on | 450ml/kg | 520ml/kg | 550ml/kg | ||
| Join powder | Wet-mixed | 10 hours | 7 hours | 13 hours | |
| Add the glue granulation | Mix the glue time | 1.0 hour | 0.5 hour | 1.5 hour | |
| Bake out temperature | 75℃ | 50℃ | 60℃ | ||
| Drying time | 40min | 30min | 15min | ||
| Cold isostatic compaction | Moulding process | 215MPa*10min | 200MPa*15min | 180MPa*30min | |
| Sintering | Binder removal technology | 10 -1* was 770 ℃ in Pa*3 hour | 10 -2* was 680 ℃ in Pa*2 hour | 10 -3* was 550 ℃ in Pa*4 hour | |
| Soaking time | 2 hours | 1.5 hour | 1 hour | ||
| Heat-up time | 5 hours | 7 hours | 9 hours | ||
| Sintering process | 2000 ℃ of * 3 hours | 1850 ℃ of * 6 hours | 2150 ℃ of * 1.5 hours | ||
| The sintering briquette size | Φ41*80mm | 52*52*65mm | 152*27*20mm | ||
| Sizes of substrate | Φ40*1.5mm | 50.8*50.8*1.0mm | 150*25*1.5mm | ||
The substrate performance comparison table of table 2 embodiment of the invention and prior art Comparative Examples
| Sequence number | Sintering briquette density | Thermal conductivity | |
| The embodiment of the invention | 1 | 3.39g/cm 3 | 220W/m·K |
| 2 | 3.36g/cm 3 | 198W/m·K | |
| 3 | 3.38g/cm 3 | 210W/m·K | |
| Comparative Examples CN1087010C | 4 | 3.35g/cm 3 | 165W/m·K |
| 5 | 3.33g/cm 3 | 190W/m·K | |
| 6 | 3.34g/cm 3 | 110W/m·K | |
| Comparative Examples CN1557776A | 7 | - | 138W/m·K |
Claims (3)
1, adopt powder metallurgical technique to prepare the method for high heat conduction aluminium nitride ceramic substrate, it is characterized in that this method comprise join powder, add the glue granulation, cold isostatic compaction, sintering, five steps of machining, its concrete steps are as follows:
The preparation of A, raw material powder: take by weighing an amount of AlN powder and sintering aid in proportion, in the mixer of packing into, add dehydrated alcohol by 1: 1 weight ratio, wet-mixed 5～15 hours is to evenly, then dry for standby;
B, add the glue granulation: the ratio in 400～600ml/kg in the confected materials powder adds the binding agent for preparing, after in mixed glue machine, mixing 0.5～2 hour, place baking oven at 40～80 ℃ of scope internal heating 10～40min, then with 100 mesh sieves screening granulation;
C, cold isostatic compaction: the powder after the granulation is packed in the flexible glue film, put into cold isostatic press compression moulding; The size of flexible glue film can be according to the diameter or the length and width size design of prepared substrate; Hydrostatic pressure is 150～220MPa, and the dwell time is 10～30min; Can require to carry out machining and shaping according to final sizes of substrate after the powder moulding;
D, sintering: with the blank of compression moulding 10
-1～10
-3Be heated to 500～800 ℃ through 2～4 hours under the Pa state, be incubated 1～2 hour, so that remove the binding agent of adding; Feed nitrogen then, be warmed up to 1800～2400 ℃, be incubated 1.5～6 hours at 4～10 hours internal heating; Insulation finishes back outage, furnace cooling;
E, machining: the aluminium nitride blank that sinters is carried out machining by the desired size of substrate, the physical dimension that cylindrical grinding or plane require to substrate, cut into slices to the substrate thickness that needs with inner circle cutting machine again, grind then, polish, just obtain meeting the aluminium nitride chip of the high heat conduction of dimension precision requirement.
2, employing powder metallurgical technique according to claim 1 prepares the method for high heat conduction aluminium nitride ceramic substrate, it is characterized in that the used raw-material main chemical of aforesaid method is AlN94～99wt%, and all the other are sintering aid; The Chemical Composition of sintering aid is Y
2O
3, Dy
2O
3, CaO, CaF
2, among the SrO any one or more, ratio is 1～6wt%; Wherein, the median size of AlN powder is 0.1～8 μ m.
3, employing powder metallurgical technique according to claim 1 prepares the method for high heat conduction aluminium nitride ceramic substrate, it is characterized in that the used binding agent of powder granulation is that concentration is any in the spirituous solution of the gasoline solution of 1～5wt% sodium butadiene rubber or spirituous solution that concentration is 1～12wt% ethyl cellulose, polyvinyl alcohol.
Priority Applications (1)
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|---|---|---|---|
| CNB2005100730503A CN1332910C (en) | 2005-05-31 | 2005-05-31 | Method for preparing high heatconducting aluminium nitride ceramic base sheets through powder metallurgical technique |
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|---|---|---|---|
| CNB2005100730503A CN1332910C (en) | 2005-05-31 | 2005-05-31 | Method for preparing high heatconducting aluminium nitride ceramic base sheets through powder metallurgical technique |
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| CN1686944A CN1686944A (en) | 2005-10-26 |
| CN1332910C true CN1332910C (en) | 2007-08-22 |
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Families Citing this family (11)
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|---|---|---|---|---|
| CN101985396B (en) * | 2010-11-03 | 2013-03-20 | 刘述江 | Method for preparing aluminum nitride ceramic substrate by clinker slicing |
| CN102581271A (en) * | 2012-03-30 | 2012-07-18 | 吉林大学 | Powder metallurgy material mixing method |
| CN103121848B (en) * | 2013-02-25 | 2015-08-19 | 潮州三环（集团）股份有限公司 | A kind of aluminum nitride ceramic substrate sintering process |
| CN103539457A (en) * | 2013-09-29 | 2014-01-29 | 合肥工业大学 | Preparation method of AlN ceramic base plate for microelectronic packaging |
| CN106830945A (en) * | 2016-11-30 | 2017-06-13 | 莱鼎电子材料科技有限公司 | It is a kind of to add the method that composite sintering agent prepares high heat conduction aluminium nitride ceramic substrate |
| CN108147821B (en) * | 2017-12-21 | 2021-04-27 | 北京华进创威电子有限公司 | Preparation method of high-purity porous aluminum nitride crystal material source |
| CN109400175B (en) * | 2018-11-15 | 2020-07-31 | 中国科学院上海硅酸盐研究所 | Preparation method of high-thermal-conductivity silicon nitride ceramic substrate material |
| CN109809833B (en) * | 2019-04-01 | 2021-09-28 | 河北工业大学 | Composite phase-change material and preparation method thereof |
| CN110628223A (en) * | 2019-11-01 | 2019-12-31 | 银川艾森达新材料发展有限公司 | Heat-conducting filler |
| CN115261747B (en) * | 2021-04-29 | 2023-08-22 | 苏州铜宝锐新材料有限公司 | Powder metallurgy composite functional material, manufacturing method and application thereof |
| US20230069395A1 (en) * | 2021-08-30 | 2023-03-02 | Applied Materials, Inc. | Stress treatments for cover wafers |
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| JPS58162675A (en) * | 1982-03-23 | 1983-09-27 | Ricoh Co Ltd | Ink medium |
| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Method for manufacturing high-heat conductivity aluminium nitride ceramics |
| JP2004192872A (en) * | 2002-12-09 | 2004-07-08 | Toshiba Ceramics Co Ltd | Aluminum nitride heater |
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2005
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58162675A (en) * | 1982-03-23 | 1983-09-27 | Ricoh Co Ltd | Ink medium |
| CN1130607A (en) * | 1995-11-17 | 1996-09-11 | 清华大学 | Method for manufacturing high-heat conductivity aluminium nitride ceramics |
| JP2004192872A (en) * | 2002-12-09 | 2004-07-08 | Toshiba Ceramics Co Ltd | Aluminum nitride heater |
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