CN106304780B - Manufacturing process for high thermal conductivity graphite film - Google Patents

Manufacturing process for high thermal conductivity graphite film Download PDF

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Publication number
CN106304780B
CN106304780B CN201610696862.1A CN201610696862A CN106304780B CN 106304780 B CN106304780 B CN 106304780B CN 201610696862 A CN201610696862 A CN 201610696862A CN 106304780 B CN106304780 B CN 106304780B
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parts
graphite
degree
film
kept
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CN106304780A (en
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金闯
梁豪
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Sidike New Materials Jiangsu Co Ltd
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Sidike New Materials Jiangsu Co Ltd
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04Coating
    • C08J7/0427Coating with only one layer of a composition containing a polymer binder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1207Heat-activated adhesive
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00Constructional details common to different types of electric apparatus
    • H05K7/20Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • H05K7/205Heat-dissipating body thermally connected to heat generating element via thermal paths through printed circuit board [PCB]
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B32B27/18Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • BPERFORMING OPERATIONS; TRANSPORTING
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    • B32B27/00Layered products comprising a layer of synthetic resin
    • B32B27/28Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/281Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
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    • B32B37/02Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by a sequence of laminating steps, e.g. by adding new layers at consecutive laminating stations
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    • B32B37/14Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/15Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • B32B37/153Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is extruded and immediately laminated while in semi-molten state
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    • B32B37/15Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • B32B37/156Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is calendered and immediately laminated
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    • C04B35/52Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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    • C04B35/524Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from polymer precursors, e.g. glass-like carbon material
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    • C04B35/62218Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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    • C09J2467/005Presence of polyester in the release coating

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
  • Adhesives Or Adhesive Processes (AREA)
  • Adhesive Tapes (AREA)

Abstract

The present invention discloses a kind of manufacturing process for high thermal conductivity graphite film, the following steps are included: Kapton is risen to 250 DEG C from room temperature with 4 ~ 6 degree/min speed, kept for 0.9 ~ 1.1 hour, then with 2.5 ~ 3.5 degree/min, 400 DEG C are risen to, near room temperature after being kept for 1 hour;One layer graphite modified dose, which is coated with, in the upper and lower surfaces of the Kapton Jing Guo step 1 obtains treated Kapton;The graphite modified dose of group by following parts by weight is grouped as: 23 parts of benzophenone tetracarboxylic dianhydride, 12 parts of pyromellitic acid anhydride, 26.5 parts of diaminodiphenylmethane, 34 parts of dimethylformamide, 2.2 parts of ethylene glycol, 2 parts of dimethyl silicone polymer.The present invention is filled with the pin hole in heating process, improves crystallinity simultaneously, also overcome be heat-shrinked it is excessive caused by it is uneven, improve graphite linings biaxial tension performance.

Description

Manufacturing process for high thermal conductivity graphite film
Technical field
The present invention relates to a kind of high thermal conductivity graphite films, belong to double faced adhesive chip technology field.
Background technique
With modern microelectronic technology high speed development, electronic equipment (such as laptop, mobile phone, tablet computer) is increasingly Become ultra-thin, light, this structure significantly improves electronic equipment internal power density, and generated heat is not easy in operation It is discharged, is easy to accumulate rapidly and form high temperature.On the other hand, high temperature can reduce the performance of electronic equipment, reliability and use the longevity Life.Therefore, Current electronic industry proposes increasingly higher demands for the heat sink material as heat control system core component, urgently It needs a kind of high-efficiency heat conduction, light material to transfer heat away from rapidly, ensures that electronic equipment operates normally.
Kapton is mostly used for flexible circuit board in the prior art, is obtained although having using polyimide film sintered Graphite heat radiation fin, to be covered on heat source, but be constrained to Kapton product quality and performances the good and the bad not Together, influenced the performance of the two-sided pad pasting heat dissipation performance of heat dissipation, there are following technical problems: heat dissipation is uneven, adhesive tape easily occurs Hot-spot, the heat dissipation performance of product is unstable, reliability performance is poor, is unfavorable for product quality management control, influences the competition of product Power.
Summary of the invention
It is an object of the present invention to provide a kind of manufacturing process for high thermal conductivity graphite film, this is used for the system of high thermal conductivity graphite film It makes technique and improves heating conduction in the vertical direction and the horizontal direction, avoid adhesive tape hot-spot, realize adhesive tape thermal conductivity While the uniformity of energy, heat dissipation performance stability, the reliability of product are improved, the cost of product is greatly reduced.
In order to achieve the above objectives, the technical solution adopted by the present invention is that: a kind of manufacturing process for high thermal conductivity graphite film, The high thermal conductivity graphite film fits between radiating piece and heat generating components, and the high thermal conductivity graphite film includes light strippable PET film With re-release type PET film, this light strippable PET film and re-release and be disposed with the first thermally conductive adhesive layer, stone between type PET film Layer of ink and the second thermally conductive adhesive layer;The graphite linings are obtained by following process, this process the following steps are included:
Step 1: Kapton is risen to 250 DEG C from room temperature with 4 ~ 6 degree/min speed, kept for 0.9 ~ 1.1 hour, Then with 2.5 ~ 3.5 degree/min, 400 DEG C are risen to, is down to room temperature after being kept for 1 hour;
Step 2: the upper and lower surfaces in the Kapton Jing Guo step 1 are coated with one layer of graphite modified dose of acquisition Treated Kapton;
The graphite modified dose of group by following parts by weight is grouped as: 23 parts of benzophenone tetracarboxylic dianhydride, Pyromellitic Acid 12 parts of dianhydride, 26.5 parts of diaminodiphenylmethane, 34 parts of dimethylformamide, 2.2 parts of ethylene glycol, dimethyl silicone polymer 2 Part;
Step 3: rising to 800 DEG C with the speed of 4 ~ 6 degree/min, kept for 0.9 ~ 1.1 hour;Again with the speed of 9 ~ 11 degree/min Degree rises to 1200 DEG C, cooling after being kept for 0.9 ~ 1.1 hour, to obtain the carbonized film of pre-burned;
Step 4: rolling the carbonized film of the pre-burned of the step 3 using calender;
Step 5: rising to 2400 DEG C with the speed of 19 ~ 21 degree/min, kept for 0.9 ~ 1.1 hour, then with 19 ~ 21 degree/min Speed rise to 2900 DEG C, it is cooling after being kept for 1.8 ~ 2.2 hours, to obtain the graphite film of main firing;
Step 6: then the graphite film of the resulting main firing of step 5 carries out calendering to obtain the graphite linings.
Further improved scheme is as follows in above-mentioned technical proposal:
In l above scheme, graphite modified dose of the viscosity is 30000 ~ 48000cP.
Since above-mentioned technical proposal is used, the present invention has following advantages and effect compared with prior art:
The present invention is used for the manufacturing process of high thermal conductivity graphite film, and graphite linings are coated with one layer by upper and lower surfaces in structure Graphite modified dose of Kapton is prepared, and improves heating conduction in the vertical direction and the horizontal direction, avoids glue Band hot-spot, realizes the uniformity of adhesive tape heating conduction;Secondly, it is located at graphite modified dose of Kapton surface By benzophenone tetracarboxylic dianhydride, pyromellitic acid anhydride, diaminodiphenylmethane, dimethylformamide, ethylene glycol, poly dimethyl Siloxanes composition, is coated on Kapton, and the pin hole being filled in heating process improves crystallinity simultaneously, also gram It is excessive caused uneven to have taken thermal contraction, has improved graphite linings biaxial tension performance;Again, Kapton surface has Graphite modified dose, graphite linings and thermally conductive adhesive layer heating conduction in two-sided pad pasting are improved, and described pre- using calender calendering The carbonized film of firing, the volume contraction for avoiding fold and being graphitized in sintering process, improves compactness and crystallinity, into one Step improves heating conduction in the vertical direction and the horizontal direction.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment: a kind of manufacturing process for high thermal conductivity graphite film, the high thermal conductivity graphite film fit in radiating piece and Between heat generating components, the high thermal conductivity graphite film includes light strippable PET film and re-releases type PET film, this light strippable PET film And it re-releases and is disposed with the first thermally conductive adhesive layer, graphite linings and the second thermally conductive adhesive layer between type PET film;The graphite linings Obtained by following process, this process the following steps are included:
Step 1: Kapton is risen to 250 DEG C from room temperature with 4 ~ 6 degree/min speed, kept for 0.9 ~ 1.1 hour, Then with 2.5 ~ 3.5 degree/min, 400 DEG C are risen to, is down to room temperature after being kept for 1 hour;
Step 2: the upper and lower surfaces in the Kapton Jing Guo step 1 are coated with one layer of graphite modified dose of acquisition Treated Kapton, the graphite modified dose of group by following parts by weight are grouped as, as shown in table 1:
Table 1
Note: graphite modified dose of viscosity of embodiment is 32000CP;
Step 3: rising to 800 DEG C with the speed of 4 ~ 6 degree/min, kept for 0.9 ~ 1.1 hour;Again with the speed of 9 ~ 11 degree/min Degree rises to 1200 DEG C, cooling after being kept for 0.9 ~ 1.1 hour, to obtain the carbonized film of pre-burned;
Step 4: rolling the carbonized film of the pre-burned of the step 3 using calender;
Step 5: rising to 2400 DEG C with the speed of 19 ~ 21 degree/min, kept for 0.9 ~ 1.1 hour, then with 19 ~ 21 degree/min Speed rise to 2900 DEG C, it is cooling after being kept for 1.8 ~ 2.2 hours, to obtain the graphite film of main firing;
Step 6: then the graphite film of the resulting main firing of step 5 carries out calendering to obtain the graphite linings.
The step 6 is obtained into graphite linings and carries out calendering process.
The grammes per square metre of above-mentioned light 1 peeling force of strippable PET film is 5 ~ 10g/m2, gram for re-releasing 2 peeling force of type PET film Weight is 50 ~ 100g/m2
When using the above-mentioned manufacturing process for high thermal conductivity graphite film, graphite linings are coated with by upper and lower surfaces in structure One layer graphite modified dose of Kapton is prepared, and improves heating conduction in the vertical direction and the horizontal direction, keeps away Exempt from adhesive tape hot-spot, realizes the uniformity of adhesive tape heating conduction;Secondly, its graphite for being located at Kapton surface changes Property agent is by benzophenone tetracarboxylic dianhydride, pyromellitic acid anhydride, diaminodiphenylmethane, dimethylformamide, ethylene glycol, poly- two Methylsiloxane composition, is coated on Kapton, and the pin hole being filled in heating process improves crystallinity simultaneously, It is excessive caused uneven to also overcome thermal contraction, improves graphite linings biaxial tension performance;Again, Kapton surface With graphite modified dose, graphite linings and thermally conductive adhesive layer heating conduction in two-sided pad pasting are improved, and institute is rolled using calender The carbonized film for stating pre-burned, the volume contraction for avoiding fold and being graphitized in sintering process, improves compactness and crystallinity, Further improve heating conduction in the vertical direction and the horizontal direction.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (1)

1. a kind of manufacturing process for high thermal conductivity graphite film, the high thermal conductivity graphite film fit in radiating piece and heat generating components it Between, the high thermal conductivity graphite film includes light strippable PET film and re-releasing type PET film, this light strippable PET film and re-releases type The first thermally conductive adhesive layer, graphite linings and the second thermally conductive adhesive layer are disposed between PET film;It is characterized by: the graphite Layer obtained by following process, this process the following steps are included:
Step 1: Kapton is risen to 250 DEG C from room temperature with 4 ~ 6 degree/min speed, kept for 0.9 ~ 1.1 hour, then With 2.5 ~ 3.5 degree/min, 400 DEG C are risen to, is down to room temperature after being kept for 1 hour;
Step 2: the upper and lower surfaces in the Kapton Jing Guo step 1 are coated with one layer graphite modified dose and are handled Kapton afterwards;
The graphite modified dose of group by following parts by weight is grouped as: 23 parts of benzophenone tetracarboxylic dianhydride, pyromellitic acid anhydride 12 parts, 26.5 parts of diaminodiphenylmethane, 34 parts of dimethylformamide, 2.2 parts of ethylene glycol, 2 parts of dimethyl silicone polymer;
Step 3: rising to 800 DEG C with the speed of 4 ~ 6 degree/min, kept for 0.9 ~ 1.1 hour;Again with the speed liter of 9 ~ 11 degree/min It is cooling after being kept for 0.9 ~ 1.1 hour to 1200 DEG C, to obtain the carbonized film of pre-burned;
Step 4: rolling the carbonized film of the pre-burned of the step 3 using calender;
Step 5: rising to 2400 DEG C with the speed of 19 ~ 21 degree/min, kept for 0.9 ~ 1.1 hour, then with the speed of 19 ~ 21 degree/min Degree rises to 2900 DEG C, cooling after being kept for 1.8 ~ 2.2 hours, to obtain the graphite film of main firing;
Step 6: then the graphite film of the resulting main firing of step 5 carries out calendering to obtain the graphite linings;The graphite The viscosity of modifying agent is 30000 ~ 48000cP.
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