CN104810347B - Silicon carbide whisker/polymer composite material adapter plate and preparation method - Google Patents

Silicon carbide whisker/polymer composite material adapter plate and preparation method Download PDF

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Publication number
CN104810347B
CN104810347B CN201510119860.1A CN201510119860A CN104810347B CN 104810347 B CN104810347 B CN 104810347B CN 201510119860 A CN201510119860 A CN 201510119860A CN 104810347 B CN104810347 B CN 104810347B
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China
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silicon carbide
carbide whisker
polymer composite
composite material
adapter plate
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CN201510119860.1A
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CN104810347A (en
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张久斌
程萍
汪红
丁桂甫
王博
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Abstract

The present invention proposes a kind of silicon carbide whisker/polymer composite material adapter plate and preparation method, including metal column array and silicon carbide whisker/polymer composites film, wherein, the silicon carbide whisker prepared by the method for spin coating or electrophoresis/polymer composites film forms the matrix of pinboard, metal column array is regularly distributed in silicon carbide whisker/polymer composite material adapter plate matrix, and vertically therethrough.The present invention is using silicon carbide whisker/polymer composites as pinboard, compared with using straight polymer material or glass medium as pinboard, because the introducing of silicon carbide whisker makes the heat conductivility of polymer and mechanical performance has and significantly increased, but without increase technology difficulty, the overall performance of pinboard thus is improved, is expected to be used for industrialized production.

Description

Silicon carbide whisker/polymer composite material adapter plate and preparation method
Technical field
The present invention is that the carbonization of microelectronics system chips and PCB substrate interconnection is particularly used on a kind of pinboard Silicon wafer palpus/polymer composite material adapter plate, belong to integrated circuit or Discrete device packaging technical field.
Background technology
In technical field of integrated circuits, it is necessary to which chip is connected with PCB substrate, with the development of encapsulation technology, there is height The pinboard of the characteristics such as thermal conductivity factor, high-k, low thermal coefficient of expansion, high density, high rigidity arises.Wherein TSV Pinboard is the developing direction of current relatively main flow, and it, which has, can be achieved fine linewidth and line spacing, can meet highdensity turn Ability is connect, but because some critical technological points, such as through hole formation are more difficult, dielectric layer deposition is difficult, via metal filling is difficult, Thus the formation efficiency of this method is relatively low, does not possess the ability of large-scale production also at present.
In order to overcome problem present in TSV pinboard techniques, utility model patent CN201994289U is using encapsulating gold Belong to the polymer of post array as pinboard.The pinboard of this structure is compared with TSV pinboards, although reducing technique hardly possible Degree, but heat conductivility due to polymer and mechanical strength are weaker than silicon, limit the performance of pinboard.
To strengthen the heat conductivility and mechanical property of polymer, Chinese invention patent 103325754A discloses one kind and is based on Polymer composite material adapter plate of CNT enhancing and preparation method thereof, the patent is to pass through carbon nanotubes reinforced polymer The heat conduction of pinboard and mechanical property.And the present invention is then proposed with the heat conduction of silicon carbide whisker enhancing polymer pinboard and power Performance is learned, due to belonging to two kinds of different reinforcing materials, there is also difference by the preparation technology of pinboard.
The content of the invention
The purpose of the present invention is the deficiency for polymer pinboard, proposes a kind of silicon carbide whisker/polymer composite Expect pinboard and preparation method thereof, because the heat conductivility of conventional polymeric materials is poor, and the silicon carbide whisker/polymerization invented Thing composite has higher heat conductivility, while has preferable mechanical performance, is expected to realize commercial application.
The present invention provides a kind of silicon carbide whisker/polymer composite material adapter plate, including metal column array and carbonization Silicon wafer palpus/polymer composites film, wherein, the silicon carbide whisker/polymer prepared by the method for spin coating or electrophoresis is multiple Condensation material film forms the matrix of pinboard, and metal column array is regularly distributed on silicon carbide whisker/polymer composites switching In plate matrix, and vertically therethrough.
Preferably, a diameter of 10~150 μm of the metal column, it is highly 100~300 μm.
Preferably, the metal for forming metal column array is one kind of copper, nickel, titanium, chromium or alloy.
Preferably, described silicon carbide whisker/polymer composite film is as pinboard matrix, its height and metal column Height is consistent substantially, is 100~300 μm.
Preferably, described polymer is using one kind in electrophoretic paint, polyimides, epoxy resin, SU-8.
Preferably, the silicon carbide whisker is prepared including gas phase carbon source method, solid-phase carbon source method and phase carbon source method Silicon carbide whisker.
The present invention provides a kind of preparation method of silicon carbide whisker/polymer composite material adapter plate, comprises the following steps：
Step 1, the preparation of metal column array
One layer of photoetching positive photoresist of spin coating, drying are used as sacrifice layer on a glass substrate, the sputtering seed layer Cr/ on sacrifice layer Cu, then get rid of one layer of photoresist on the seed layer again and dry, or one layer of dry film is pasted in Cr/Cu Seed Layers, by photoetching, show Shadow is patterned to photoresist or dry film, exposes a diameter of 10~150 μm of circular Cr/Cu Seed Layers region, then passes through perseverance Stream plating forms metal column array, is highly 100~300 μm, then removes the unnecessary photoresist or dry in Cr/Cu Seed Layers Film, and it is cleaned by ultrasonic metal column array with deionized water, in 100-250 DEG C of drying；
Step 2, the preparation of silicon carbide whisker/polymer composite film
By way of electrophoresis and spin coating, by silicon carbide whisker/polymer composites uniform fold in above-mentioned band metal In the substrate of post array, ensure that the thickness of composite coating is close with the height of metal column array, then dried at 100-250 DEG C It is dry；The top of pinboard is processed by shot blasting, metal top end is exposed from silicon carbide whisker/polymer composites.
Step 3, the formation of silicon carbide whisker/polymer composite material adapter plate
Sacrifice layer is removed, the pinboard with metal column array and glass substrate are departed from, pinboard bottom is polished, gone Except Seed Layer, expose metal column, so as to finally give silicon carbide whisker/polymer composite material adapter plate.
Described metal column array is regularly arranged by multiple metal columns, vertically through compound by carborundum/polymer Material pinboard matrix.
To strengthen the heat conductivility and intensity of polymer, the present invention proposes a kind of silicon carbide whisker/polymer composite Expect pinboard.Silicon carbide whisker is that a kind of a diameter of nanoscale is similar with diamond to micron-sized mono-crystlling fibre, crystal structure Seemingly, chemical impurity is few in crystal, and no grain boundary, crystal structure defects are few, crystalline phase uniform component, has high thermal conductivity coefficient (83.6W/mK), low-thermal-expansion rate (4.4 × 10-6℃-1), high-melting-point (temperature is up to 2700 DEG C), low-density (3.21g/ cm3), high intensity (tensile strength 2100kg/cm2), high elastic modulus (modulus of elasticity 9 × 104kg/cm2) and it is wear-resisting, resistance to The characteristics such as burn into oxidation-resistance property is strong.Using silicon carbide whisker can improve in pinboard the heat conductivility of polymer and Mechanical performance, improve the capacity of heat transmission and mechanical strength of pinboard.
Compared with prior art, the present invention has following beneficial effect：
The present invention uses silicon carbide whisker/polymer composites as pinboard, with using straight polymer material or glass Glass medium is compared as pinboard, because the introducing of silicon carbide whisker makes the heat conductivility of polymer and mechanical performance have significantly Ground improves, but without increase technology difficulty, thus the overall performance of pinboard is improved, it is expected to be used for industrial metaplasia Production.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention Protection domain.
Embodiment 1
Silicon carbide whisker/electrophoretic paint composite pinboard is prepared with the method for the present invention, is comprised the following steps：
1. the preparation of copper post array
The photoetching positive photoresist of about 5~10 μm of the thickness of spin coating one drying, is splashed as sacrifice layer on sacrifice layer on a glass substrate Seed Layer Cr/Cu is penetrated, then the dry film of 250~300 μ m-thicks is attached on Seed Layer Cr/Cu, photoetching, development, makes dry film figure Change, expose a diameter of 120~180 μm of circular Cr/Cu regions.Using the substrate of glass with graphical Seed Layer as negative electrode, with copper Plate is anode, applies 5~10mA/cm between electrodes2Constant-current supply, at room temperature plating formed height be 250~300 μm copper post array；Then the dry film in Cr/Cu Seed Layers is removed, and is cleaned by ultrasonic copper post array with deionized water, 100~ 150 DEG C of 30~40min of drying；
2. the electrophoretic deposition of silicon carbide whisker/electrophoretic paint composite
Configure silicon carbide whisker/electrophoretic paint mixing electrophoresis liquid：By 100g electrophoretic paints black wash, 500g electrophoretic paints emulsion and 600g Deionized water adds beaker, at room temperature using magnetic stirrer 24h, cures electrophoresis liquid, then adds certain The treated silicon carbide whisker suspension with electric charge is measured, is uniformly mixed.
Using the above-mentioned substrate with copper post array as negative electrode, using stainless steel or titanium sheet as anode, two electrodes are put into carbon In SiClx whisker/electrophoretic paint mixing electrophoresis liquid, apply constant voltage between electrodes and carry out electrodeposition coated film, until silicon carbide whisker The coating film thickness of palpus/electrophoretic paint should be basically identical with height of the copper pillar, about 250~300 μm, 150~200 DEG C dry 60~ 80min.
3. the formation of silicon carbide whisker/polymer composite material adapter plate
The top of pinboard is processed by shot blasting, copper post array top is exposed from silicon carbide whisker/electrophoretic paint.So Photoetching glue victim layer is removed with acetone afterwards, the pinboard with copper post array and glass substrate are departed from, pinboard bottom is thrown Light, Seed Layer is removed, exposes copper post, so as to finally give silicon carbide whisker/electrophoretic paint composite pinboard.
By taking thick 250 microns of pinboard as an example, the yield strength of straight polymer composite pinboard is 30MPa, Young Modulus is 1.5GPa, thermal conductivity factor 0.2w/m.k, and the yield strength of silicon carbide whisker/polymer composite material adapter plate is 40MPa, Young's modulus 2-5GPa, thermal conductivity factor 0.5-1.2w/m.k, therefore silicon carbide whisker/polymerization proposed by the present invention The mechanical property of thing composite pinboard, heat conductivility are all greatly improved.
Embodiment 2
Silicon carbide whisker/composite polyimide material pinboard is prepared with the method for the present invention, is comprised the following steps：
It is step 2 in the present embodiment, 4 identical with above-described embodiment.The difference is that step 1 and 3, is introduced such as respectively Under：
1. the preparation of copper post array
One layer of photoetching positive photoresist sacrifice layer of spin coating on a glass substrate, the sputtering seed layer Cr/Cu on sacrifice layer, is then being planted The photoetching positive photoresist of one layer of 30~50 μ m-thick of spin coating again in sublayer, photoetching, development, makes photoetching offset plate figure, expose a diameter of 20~ 30 μm of circular Cr/Cu regions.Using the substrate of glass with graphical Seed Layer as negative electrode, using nickel plate as anode, two electrodes it Between apply 5~10mA/cm2Constant-current supply, plating at room temperature forms height about 30~50 μm of nickel post array；By nickel post Polish and expose, then the photoresist of 30 microns of one thickness of spin coating, photoetching (alignment), development, the nickel post for electroplating 30~50 μm high, so Repeatedly, until the height of nickel post is 120~200 μm.
2. the preparation of silicon carbide whisker/composite polyimide material
The mixed sols of silicon carbide whisker/polyimides is prepared first：A certain amount of silicon carbide whisker is added to polyamides In imines, it is sufficiently mixed with Ball Milling, forms silicon carbide whisker/polyimides complex sol.
The substrate with nickel post is placed on photoresist spinner, by adjusting rotating speed and time, in substrate surface spin coating thickness about For 120~200 μm of silicon carbide whisker/polyimide composite film, 150~200min is dried at 250~300 DEG C.
3. the formation of silicon carbide whisker/composite polyimide material pinboard
The top of pinboard is processed by shot blasting, copper post array top is exposed from silicon carbide whisker/polyimides. Then acetone removes photoetching glue victim layer, and the pinboard with copper post array and glass substrate are departed from, and pinboard bottom is thrown Light, Seed Layer is removed, exposes copper post, so as to finally give silicon carbide whisker/composite polyimide material pinboard.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow Ring the substantive content of the present invention.

Claims (8)

  1. A kind of 1. preparation method of silicon carbide whisker/polymer composite material adapter plate, it is characterised in that the silicon carbide whisker Palpus/polymer composite material adapter plate, including metal column array and silicon carbide whisker/polymer composites film, wherein, The silicon carbide whisker prepared by the method for spin coating or electrophoresis/polymer composites film forms the matrix of pinboard, metal Post array is regularly distributed in silicon carbide whisker/polymer composite material adapter plate matrix, and vertically therethrough；
    It the described method comprises the following steps：
    Step 1, the preparation of metal column array
    One layer of photoetching positive photoresist of spin coating, drying are used as sacrifice layer on a glass substrate, the sputtering seed layer Cr/Cu on sacrifice layer, so Get rid of one layer of photoresist on the seed layer again afterwards and dry, or one layer of dry film is pasted in Cr/Cu Seed Layers, pass through photoetching, development pair Photoresist or dry film are patterned, and expose circular Cr/Cu Seed Layers region, then electroplate to form metal column array by constant current, Then the unnecessary photoresist or dry film in Cr/Cu Seed Layers are removed, and is cleaned by ultrasonic metal column array with deionized water, then is dried It is dry；
    Step 2, the preparation of silicon carbide whisker/polymer composite film
    By way of electrophoresis and spin coating, by silicon carbide whisker/polymer composites uniform fold in above-mentioned band metal column battle array In the substrate of row, ensure that the thickness of composite coating is close with the height of metal column array, then dry；The top of pinboard is entered Row polishing, metal top end is exposed from silicon carbide whisker/polymer composites；
    Step 3, the formation of silicon carbide whisker/polymer composite material adapter plate
    Sacrifice layer is removed, the pinboard with metal column array and glass substrate are departed from, pinboard bottom is polished, removal kind Sublayer, expose metal column, so as to finally give silicon carbide whisker/polymer composite material adapter plate.
  2. 2. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim 1, its feature exist In in the first step, exposing the circular Cr/Cu Seed Layers area that circular Cr/Cu Seed Layers region refers to expose a diameter of 10~150 μm Domain.
  3. 3. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim 1 or 2, its feature It is, in step 1 and step 2, drying refers to carry out drying and processing at 100~250 DEG C.
  4. 4. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim 1, its feature exist In：A diameter of 10~150 μm of the metal column, it is highly 100~300 μm.
  5. 5. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim 1, its feature exist In：The metal for forming metal column array is one kind of copper, nickel, titanium, chromium or alloy.
  6. 6. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim 1, its feature exist In：Silicon carbide whisker/the polymer composite film keeps one substantially as pinboard matrix, its height and the height of metal column Cause, be 100~300 μm.
  7. 7. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim any one of 1-6, its It is characterised by：The polymer is using one kind in electrophoretic paint, polyimides, epoxy resin, SU-8.
  8. 8. the preparation method of silicon carbide whisker/polymer composite material adapter plate according to claim any one of 1-6, its It is characterised by：The silicon carbide whisker includes the carbonization that gas phase carbon source method, solid-phase carbon source method and phase carbon source method are prepared Silicon wafer must it is any.
CN201510119860.1A 2015-03-18 2015-03-18 Silicon carbide whisker/polymer composite material adapter plate and preparation method Expired - Fee Related CN104810347B (en)

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CN106206543A (en) * 2016-08-04 2016-12-07 上海交通大学 Based on nano aluminum nitride/composite polyimide material keyset and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103060890A (en) * 2013-01-22 2013-04-24 华南理工大学 Method for synthesizing nano silicon carbide crystal whiskers
CN103325754A (en) * 2013-05-22 2013-09-25 上海交通大学 Enhanced polymer composite material adapter plate based on carbon nano tube and preparation method thereof

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JPS63312328A (en) * 1987-06-15 1988-12-20 Tokai Carbon Co Ltd Production of polyimide polymer reinforced with sic whisker

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103060890A (en) * 2013-01-22 2013-04-24 华南理工大学 Method for synthesizing nano silicon carbide crystal whiskers
CN103325754A (en) * 2013-05-22 2013-09-25 上海交通大学 Enhanced polymer composite material adapter plate based on carbon nano tube and preparation method thereof

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