CN105598014B - Two layers of method prepares the flexible amination device without glue polyimide copper clad lamination - Google Patents
Two layers of method prepares the flexible amination device without glue polyimide copper clad lamination Download PDFInfo
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- CN105598014B CN105598014B CN201610061761.7A CN201610061761A CN105598014B CN 105598014 B CN105598014 B CN 105598014B CN 201610061761 A CN201610061761 A CN 201610061761A CN 105598014 B CN105598014 B CN 105598014B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0433—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being a reactive gas
- B05D3/0453—After-treatment
- B05D3/046—Curing or evaporating the solvent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1085—Polyimides with diamino moieties or tetracarboxylic segments containing heterocyclic moieties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/40—Metallic substrate based on other transition elements
- B05D2202/45—Metallic substrate based on other transition elements based on Cu
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
Two layers of method prepares the flexible amination device without glue polyimide copper clad lamination, for independently of the nitrogen high temperature oven (400) except polyamic acid coating and drying device, furnace body (10) with top-opening type, furnace body mouth be sealed with heat insulation furnace cover (20), be additionally provided with vacuum system (40), inflated with nitrogen system, circulating fan system (60), for baking oven power supply, heating and cooling and carry out gas control control system, be placed in furnace interior be used for unreel dress polyimide copper clad lamination material volume (80) rack (70).Special nitrogen high temperature oven heat insulation effect of the invention is good, temperature is uniform, it accurate can control heating and imidizate is completed in thermostatic control, annealing is completed in certain temperature by the control that cools down again, it just can guarantee that copper-clad plate has good dimensional stability and higher peel strength in this way, meanwhile offline amination device of the invention is lower than the equipment cost of one, efficient, energy consumption is small, amination effect is good.
Description
Technical field
The present invention relates to the amination dresses that flexible printed wiring board field more particularly to two layers of method prepare flexible glue-free copper coated plate
It sets.
Background technology
Polyimide copper clad lamination is obtained in fields such as telecommunication, computer, automobiles and is answered extensively with its unique property of interconnections
With the whole world is with 10%~15% annual growth sustainable growth, and global dosage is more than 1,500,000,000 dollars within 2013.There is glue polyamides at present
Imines copper-clad plate is due to its flexility, and heat resistance, dimensional stability is bad, and application field is very limited.And without glue polyamides
Compared with imines copper-clad plate has glue polyimide copper clad lamination with tradition, heat resistance is greatly improved, and the region service life of destroying or force to yield substantially carries
Height, Rigid Flex realize high density interconnection, substantially increase the connection efficiency of circuit.
Currently, external nearly all use two layers of method production without glue system polyimide copper clad lamination, according to difference in two layers of method
Technique is divided into as 4 kinds of manufacturing methods, i.e.,：The tape casting, metallikon, chemical plating/galvanoplastic and laminating method, but the above method is required for
The special import equipment of costliness, of high cost, existing equipment are substantially integrated amination curing apparatus, and complex process, speed is slow, efficiency
Low, high energy consumption.Also, the dimensional stability of no glue system polyimide copper clad lamination is a huge test.Polyimides will be with
Copper is combined together, since the coefficient of thermal expansion (CET) of the two is different, by cold and hot effect, especially by polyamides Asia
The precursor polyamic acid of amine will occur in high temperature hot-imide postcooling because of the mismatch of the two coefficient of thermal expansion
Warpage, cracking even delamination, cause the poor dimensional stability of existing glue-free copper coated plate.The process of front and obtained copper-clad plate are again
Good, last aminating process, which is dealt with improperly, may also lead to that all that has been achieved is spoiled.
Invention content
No glue system polyimide copper clad lamination composite material is can guarantee the technical problem to be solved in the present invention is to provide a kind of
High-dimensional stability and equipment is simple, two layers of method at low cost prepare the offline amination device without glue system polyimide copper clad lamination；
The amination device heat insulation effect is good and sealing effect is good.
In order to solve the above technical problem, the present invention provides in order to solve the above-mentioned technical problem, two layers of method of the invention
The flexible amination method without glue polyimide copper clad lamination is prepared, steps are as follows：It will remove completely made of winding after residual solvent
Polyamic acid copper-clad plate roll good is put into special nitrogen high temperature oven 400, first carries out baking oven heating：With 30 degrees Celsius/it is small
When speed rise to 180 degrees Celsius, then constant temperature 4 hours, then rise to 330-340 degrees Celsius in 2 hours；Constant temperature carries out for 1 hour again
Imidizate；Then temperature-fall period is carried out：270 degrees Celsius were down to by the thermostat temperature of imidizate with 1 hour time, constant temperature
2 hours, then be cooled to 200 degrees Celsius in 2 hours, then natural cooling to get to two layer method flexibilities without glue polyimide copper clad lamination,
Its dimensional stability is in ± 5/10000.
In order to realize the amination method, the present invention provides a kind of dedicated amination device, the amination device is independent
Nitrogen high temperature oven 400 except polyamic acid coating and drying device；The nitrogen high temperature oven 400, baking oven are open-top
Formula, including furnace body 10, salable heat insulation furnace cover 20 in furnace body mouth, the vacuum system 40 vacuumized for baking oven, be baking oven nitrogen charging
The inflated with nitrogen system of gas, circulating fan system 60, for baking oven power supply, heating and cooling and the control system for carrying out gas control；Also wrap
It includes and is placed in the rack 70 that furnace interior is used for unreeling dress polyimide copper clad lamination material volume 80；
The furnace body 10 be vertical hollow circle tube, the furnace body 10 from outside to inside successively include furnace shell 11, insulating layer 12,
Outer thermal insulation layer 13, heating element 14, inner insulating layer 15, the outer thermal insulation layer 13, heating element 14, inner insulating layer 15 constitute stove
Courage, the rack 70 are placed in the flue；
A hydraulicefficiency elevation structure 30 is connected in the furnace body lateral wall, the lifting arm 33 on top is laterally connected in described
The top of heat insulation furnace cover 20, so that 20 lock sealing of the heat insulation furnace cover in furnace body top open part or opens it；
The vacuum system 40 includes the vacuum pump 41 being placed in outside furnace body, and 42 one end of vacuum line is communicated in vacuum pump,
The other end is communicated in the flue, and connector is equipped with valve 43；
The inflated with nitrogen system, including be opened in flue and air inlet 51, air valve, the pipe of furnace body external air source can be connected to
Road；
The circulating fan system 60 is by motor 61 and is connected to the fan blade 62 of motor output end, described to be into fan blade
Two, it is symmetricly set on the both sides of bottom of furnace body；
The rack 70 is supported in the chassis 71 of bottom of furnace body by connection, and be connected to chassis top, can accept it is multiple
The frame 72 of roll good forms.
The present invention further provides the amination stoves of more leakproofness：It is equipped in the downside of the bell 20 and furnace body contact position
One circle groove 23, groove is interior to be equipped with fluid sealant 21, in the periphery of fluid sealant, in being respectively equipped with as fluid sealant on bell and furnace body
More water cooling tubes 22 of cooling effect.
The heating element 14 of the furnace body is heating wire, is equipped on the inner insulating layer 15 of furnace body multiple convenient for into flue
The through-hole 151 of space heat transfer.
Beneficial effects of the present invention are mainly described below:
For the dimensional stability of no glue system polyimide copper clad lamination, the main method of solution makes to be combined with each other
The coefficient of thermal expansion of two kinds of materials is close as possible, and influence material thermal expansion coefficient (CTE) because being known as chemical constitution and aggregation
The aspect of state two, after chemical constitution determination, state of aggregation is then determined by more factors, such as solvent for use, is synthesized
Journey, coating method, drying program, imidizate program, annealing conditions etc..
Before amination of the present invention, the copper-clad plate front and continued drying effect of polyamic acid solution coating is as shown in Table 1.
Table one
| Dry front density (g/100cm2) | 1.832 | 1.82 | 1.812 | 1.834 | 1.816 |
| Dry density (g/100cm below2) | 1.771 | 1.755 | 1.753 | 1.774 | 1.755 |
The present invention is will to be completely dried and carry out imidizate, annealing without the Texturized copper-clad plate material volume of copper foil.It is existing
Imidizate complexity, speed are very slow in technology, and production capacity is low, and special nitrogen high temperature oven heat insulation effect of the invention is good, temperature is equal
It is even, it accurate can control heating and imidizate is completed in thermostatic control, then annealing is completed in certain temperature by cooling down to control, this
Sample just can guarantee that copper-clad plate has good dimensional stability and higher peel strength, meanwhile, it is of the invention offline (to refer to and be coated with
It is not one with drying) amination device is lower than the equipment cost of one, efficient, energy consumption is small, amination effect is good.
Description of the drawings
With reference to the accompanying drawings and detailed description, the present invention is described in further detail：
Fig. 1 is that two layers of method of the present invention prepares the flexible production line schematic diagram without glue polyimide copper clad lamination.
Fig. 2 is the nitrogen high temperature oven schematic diagram of the present invention.
Fig. 3 is the portions A enlarged drawing in Fig. 2.
Specific implementation mode
Embodiment 1
As shown in Figure 1, two layers of method of the present invention prepares the flexible production line without glue polyimide copper clad lamination, include system successively
The reaction system 100 of standby polyamic acid solution, the coating system 200 that polyamic acid solution is applied to copper foil, will be after coating
Copper-clad plate under high tension the high-tension drying cylinder 300 of redrying, by roll good carry out imidizate special nitrogen high temperature
Baking oven 400.
Equipment in the prior art can be used in the reaction system 100 for preparing polyamic acid solution, coating system 200,
The equipment that wherein existing coating applications can be used in coating system 200；And the parameter and special nitrogen high temperature of high-tension drying cylinder 300 are dried
Case 400 is then special designs of the present invention.
The high-tension drying cylinder 300 is undertaken on 200 end of coating system, and the cylinder structure that paper industry uses can be used,
Such as the copper heat conduction cylinder body that can be rotated around its axle center, but the present invention has found the Parameter Conditions to the drying cylinder through many experiments
Necessary particular/special requirement, such as drying cylinder diameter, surface state, surface temperature difference range, static balancing value etc..In the present embodiment, it dries
A diameter of 1.5 meters of the drying section that cylinder is contacted with copper-clad plate, cylinder surface are electroplate with the layers of chrome of 0.08-0.1mm thickness and do mirror
Reason, uniformly distributed heating element in cylinder body, the cylinder surface temperature difference within 3 degree, be undertaken on to copper-clad plate high-tension cylinder surface into
Row heat drying.The static balancing of cylinder body is required in 40g or less so that tension is more uniform.
As shown in Fig. 2, the nitrogen high temperature oven 400 includes furnace body 10, salable heat insulation furnace cover 20 in furnace body, to dry
Vacuum system 40 that case vacuumizes, the inflation system for baking oven inflated with nitrogen, circulating fan system 60, be baking oven power supply, heating and cooling,
The control system of gas control；It further include the rack 70 for being placed in bottom in furnace body；The furnace body 10 is vertical hollow circle tube, institute
State furnace body 10 from outside to inside successively include furnace shell 11, insulating layer 12, outer thermal insulation layer 13, heating element 14, inner insulating layer 15, it is described
Outer thermal insulation layer 13, heating element 14, inner insulating layer 15 constitute flue, and the heating element 14 of the furnace body is heating wire, for stove
Temperature is more uniform in courage, and multiple through-holes 151 convenient for heat transfer are equipped with around furnace body inside wall, on inner insulating layer 15.Institute
State the rack 16 for being equipped in flue and being supported in bottom of furnace body；A hydraulicefficiency elevation structure 30, packet are connected in the furnace body lateral wall
The hydraulic cylinder 31 for being connected to the furnace body side is included, the piston 32 of hydraulic cylinder is connected to the lower end of longitudinal extension bar 33, and longitudinal
Be fixedly connected on the lifting arm 33 at the top of the upper end of telescopic rod 33, to by hydraulic piston 32 drive lifting arm rise or under
Drop, so that 20 lock sealing of the heat insulation furnace cover in furnace body top open part or opens it.The vacuum system 40 includes
The vacuum pump 41 being placed in outside furnace body, 42 one end of vacuum line are communicated in vacuum pump, and the other end is communicated in the flue, connector
Equipped with valve 43；(not entirely shown in figure, the nitrogen inflation with reference to related field in the prior art is the nitrogen inflation system
System), including be opened in flue and air inlet 51, air valve, the pipeline of furnace body external air source can be connected to；The circulating fan system
System 60 is by motor 61 and is connected to the fan blade 62 of motor output end, and described into fan blade is two, is symmetricly set on bottom of furnace body
Both sides；The rack 70 includes the chassis 71 that connection is supported in bottom of furnace body, and is connected to the frame 72 on chassis top, can
Accept multiple polyimide copper clad lamination material volumes 80.In order to preferably seal, it is equipped in the downside of the bell and furnace body contact position
One circle groove, fluid sealant 21 is equipped in groove, the periphery of fluid sealant, in being respectively equipped with as fluid sealant on bell and furnace body it is cold
But the more water cooling tubes 22 acted on are unlikely to damage to allow fluid sealant to keep lower temperature.
On the production line, the step of being prepared without glue polyimide copper clad lamination with two layers method, is as follows：
1) in a kettle, by monomer aromatic diamines 3,4- diaminodiphenyl ethers, p-phenylenediamine and 2- (4- aminophenyls)-
3 kinds of substances of 5- aminobenzimidazoles are according to 2:2:1 molar ratio is dissolved in handled through molecular sieve dehydration, water content and is less than 100ppm
N,N-Dimethylformamide solvent in, be cooled to -10 degree left and right, point 5 batches are added with diamines substance total amount etc. in 5 hours
Mole pyromellitic acid anhydride maintains -10 degree left and right, reacts 40 hours, and it is 15 grams/100 milliliters that polymerization, which generates solid content,
The number-average molecular weight of polyamic acid solution, obtained polyamic acid is 51000~66000, and molecular weight distributing index is<1.4, be
The polyamic acid solution of high molecular weight, low profile exponent.
2) the thermal instability deaeration agent that weight percentage is 0.2% is added into polyimide solution, stirs evenly,
The thermal instability deaeration agent refers to resolvent deaeration agent during heating so that sub- without glue polyamides finally obtaining
It is not remained in amine copper-clad plate.The thermal instability deaeration agent of the present invention uses 920 photocurings of TEGO Airex of Di Gao companies
The special antifoaming agent of coating can also use 370 solvent type levelling agents of TEGO Flow, the TEGO Flow 300 of Di Gao companies molten
940 solvent type of dosage form levelling agent or TEGO Airex, no-solvent type coating deaeration agent.
3) polyamic acid solution that step 2) obtains is coated on the speed of 6m/min on 18 microns of thick copper foils.Coating
Coating apparatus general in the prior art can be used, when being dried to 89% solvent of removing during coating with 140 degrees Celsius,
Then it proceeds as follows,
3) speed in 180 degrees Celsius, 4m/min on special drying line is dried, and is removed residual solvent completely, is wound into
1000m/ volumes of web-like.
4) roll good is put into special nitrogen high temperature oven, is heated up with following process：With the speed of 30 degrees Celsius/hour
180 degrees Celsius are risen to, then constant temperature 4 hours, rises to 330 degrees Celsius within 2 hours；Then constant temperature carries out imidizate in 1 hour；Then
Carry out temperature-fall period：270 degrees Celsius were down to by 330 degrees Celsius with 1 hour time, constant temperature 2 hours is cooled to 200 in 2 hours and takes the photograph
Family name's degree, then natural cooling is to obtain two layers of method non-gel flexible copper-clad plate, and various performance detections the results are shown in Table shown in three.In addition,
The data such as experiment parameter are with reference to table two.
Embodiment 2
The content of embodiment 2 is roughly the same with embodiment 1.Except that：
Fragrant amine aqueous solution is 3 kinds of substances in embodiment 1 in step 1), and it is 4 to match:4:1, it is -8 degrees Celsius to be cooled to temperature
Left and right, equimolar bibenzene tetracarboxylic dianhydride is added in point 8 batches in 8 hours, and it is 45 to maintain for -8 degrees centigrade reaction time
Hour, it is 12 grams/100 milliliters, molecular weight 53000-69000 that obtained polyamic acid contains admittedly, and molecular weight distributing index is small
In 1.4.
Copper thickness in step 2) is 12mm, coating speed 9m/min, when coating drying temperature be 130 degree, removing
81% solvent, the drying cylinder diameter in step 4) are 2 meters, the temperature of high-tension dryer surface drying is 190 degrees Celsius, speed is
3m/min, it is 1500m/ volumes to wind；According to the heating and cooling process of embodiment 1, process centre 1 hour temperature of constant temperature when imidizate
Degree is 335 degree, and obtained non-gel flexible copper-clad plate, various performance detections the results are shown in Table shown in three.In addition, the data such as experiment parameter
With reference to table two.
Embodiment 3
The content of embodiment 3 is roughly the same with embodiment 1.Except that：
Fragrant amine aqueous solution is 3 kinds of substances in embodiment 1 in step 1), and it is 6 to match:6:1 cooling temperature is -5 degrees Celsius,
Equimolar 4-4 biphenyl ether dianhydrides are added in point 10 batches in 10 hours, and it is 50 hours to maintain -5 degrees Celsius of reaction time, is obtained
Containing admittedly for polyamic acid is 13 grams/100 milliliters, molecular weight 51000-64000, and molecular weight distributing index is less than 1.4.
Copper thickness in step 2) is 12mm, and drying temperature is 160 degree, speed 12m/min when coating, removing 80%
Solvent；Drying cylinder diameter in step 4) is 2.5 meters, the temperature of high-tension dryer surface drying be 200 degree, speed 2m/
Min, it is 2000m/ volumes to wind；According to the heating and cooling process of embodiment 1, process centre 1 hour temperature of constant temperature when imidizate
It it is 340 degree, obtained non-gel flexible copper-clad plate, various performance detections the results are shown in Table shown in three.In addition, the data such as experiment parameter are joined
According to table two.
Embodiment 4
Content in the present embodiment 4 is roughly the same with embodiment 3.Except that：
When step 1) prepares polyamic acid solution, the aromatic diamines used is 2 kinds of chemical substances：3,4- diaminodiphenyl ethers
It is with molecular structureCAS accession number is 2- (4- aminophenyls) -5- ammonia of 7621-86-5
Base benzimidazole, proportioning are 1:1.Used aromatic dianhydride is bibenzene tetracarboxylic dianhydride.Obtained polyamic acid contains admittedly
13.5 grams/100 milliliters, molecular weight 50000-65000, molecular weight distributing index are less than 1.4；Coating temperature is 120 Celsius
Degree, speed 6m/min remove 80% solvent；It is 200 degrees Celsius that in cylinder dried, speed, which is 3m/min, temperature,；After amination
Obtained non-gel flexible polyimide copper clad lamination, various performance detections the results are shown in Table shown in three.In addition, the data such as experiment parameter are joined
According to table two.
Embodiment 5
Content in the present embodiment 5 is roughly the same with embodiment 4.Except that：
The aromatic diamines used are same as Example 4 for 2 kinds of chemical substances, and proportioning is adjusted to 1:1.1.Obtained polyamides
Amino acid is solid to be contained for 12.8 grams/100 milliliters, molecular weight 51000-68000, molecular weight distributing index less than 1.4；In cylinder dried
It is 180 degrees Celsius that Shi Sudu, which is 2m/min, temperature,；The non-gel flexible polyimide copper clad lamination finally obtained, various performance detections
The results are shown in Table shown in three.In addition, the data such as experiment parameter are with reference to table two.
Embodiment 6
Content in the present embodiment 6 is roughly the same with embodiment 4.Except that：
The aromatic diamines used are same as Example 4 for 2 kinds of chemical substances, and proportioning is adjusted to 1:1.2.What is obtained is poly-
Amic acid is solid containing being 14 grams/100 milliliters, molecular weight 51000-67000, and molecular weight distributing index is less than 1.4；It is dry in drying cylinder
It is 180 degrees Celsius that speed, which is 4m/min, temperature, when dry；The non-gel flexible polyimide copper clad lamination finally obtained, various performance inspections
That surveys the results are shown in Table shown in three.In addition, the data such as experiment parameter are with reference to table two.
Embodiment 7
Content in the present embodiment 7 is roughly the same with embodiment 2, the difference is that the aromatic diamines used is 2 kinds of chemistry
Substance：P-phenylenediamine and molecular structure areCAS accession number is the 2- (4- of 7621-86-5
Aminophenyl) -5- aminobenzimidazoles, proportioning is 1:1.Used tetracid dianhydride is 3,3 ', 4,4 ' --- benzophenone tetracid two
Acid anhydride, it is 11.6 grams/100 milliliters, molecular weight 52000-69000 that obtained polyamic acid contains admittedly, and molecular weight distributing index is less than
1.4；The drying cylinder speed of second segment drying is 1m/min, temperature is 200 degrees Celsius；The non-gel flexible coated polyimide finally obtained
Copper coin, various performance detections the results are shown in Table shown in three.In addition, the data such as experiment parameter are with reference to table two.
Embodiment 8
Content in the present embodiment 8 is roughly the same with embodiment 7, and aromatic diamines use same 2 kinds of chemical substance,
Proportioning is adjusted to 1:1.1.The solid of obtained polyamic acid contains for 11 grams/100 milliliters, molecular weight 52000-65000, molecular weight
Profile exponent is less than 1.4；The non-gel flexible polyimide copper clad lamination finally obtained, various performance detections the results are shown in Table three institutes
Show.In addition, the data such as experiment parameter are with reference to table two.
Embodiment 9
Content in the present embodiment 9 is roughly the same with embodiment 7, and aromatic diamines use same 2 kinds of chemical substance,
Proportioning is adjusted to 1:1.2.The solid of obtained polyamic acid contains for 10.8 grams/100 milliliters, molecular weight 53000-66000, molecule
It measures profile exponent and is less than 1.4；The non-gel flexible polyimide copper clad lamination finally obtained, various performance detections the results are shown in Table three institutes
Show.In addition, the data such as experiment parameter are with reference to table two.
Claims (1)
1. two layers of method prepares the flexible amination device without glue polyimide copper clad lamination, which is characterized in that the amination device is only
Stand on the nitrogen high temperature oven (400) except polyamic acid coating and drying device；The nitrogen high temperature oven (400) is open-top
Formula, including furnace body (10), salable heat insulation furnace cover (20) in furnace body mouth, the vacuum system (40) vacuumized for baking oven, be to dry
The inflated with nitrogen system of case inflated with nitrogen, circulating fan system (60), for baking oven power supply, heating and cooling and the control system for carrying out gas control
System；It further include the rack (70) for being placed in furnace interior and being used for unreeling dress polyimide copper clad lamination material volume (80)；
The furnace body (10) is vertical hollow circle tube, and the furnace body (10) includes furnace shell (11), insulating layer successively from outside to inside
(12), outer thermal insulation layer (13), heating element (14), inner insulating layer (15, the outer thermal insulation layer (13), heating element (14), it is interior every
Thermosphere (15) constitutes flue, and the rack (70) is placed in the flue；
A hydraulicefficiency elevation structure (30) is connected in the furnace body lateral wall, the lifting arm (33) on top is laterally connected in described
The top of heat insulation furnace cover (20), so that the heat insulation furnace cover (20) lock sealing in furnace body top open part or opens it；
The vacuum system (40) includes the vacuum pump (41) being placed in outside furnace body, and vacuum line (42) one end is communicated in vacuum
Pump, the other end are communicated in the flue, and connector is equipped with valve (43)；
The inflated with nitrogen system, including be opened in flue and air inlet (51), air valve, the pipeline of furnace body external air source can be connected to；
The circulating fan system (60) is by motor (61) and is connected to the fan blade (62) of motor output end and forms, the wind
Leaf (62) is two, is symmetricly set on the both sides of bottom of furnace body；
The rack (70) is supported in the chassis (71) of bottom of furnace body by connection, and be connected to chassis top, can accept it is multiple
The frame (72) of roll good forms；
It is equipped with a circle groove (23) in the downside of the bell (20) and furnace body contact position, fluid sealant (21) is housed in groove,
The periphery of fluid sealant, in being respectively equipped with as fluid sealant on bell and furnace body cooling effect more water cooling tubes (22)；
The heating element (14) of the furnace body is heating wire, is equipped on the inner insulating layer (15) of furnace body multiple convenient for into flue
The through-hole (151) of space heat transfer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610061761.7A CN105598014B (en) | 2016-01-28 | 2016-01-28 | Two layers of method prepares the flexible amination device without glue polyimide copper clad lamination |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610061761.7A CN105598014B (en) | 2016-01-28 | 2016-01-28 | Two layers of method prepares the flexible amination device without glue polyimide copper clad lamination |
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| CN105598014A CN105598014A (en) | 2016-05-25 |
| CN105598014B true CN105598014B (en) | 2018-11-09 |
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| CN116714287A (en) * | 2023-08-08 | 2023-09-08 | 杭州锐健马斯汀医疗器材有限公司 | Heat treatment apparatus and heat treatment method suitable for absorbable material |
Citations (4)
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| JP2004019958A (en) * | 2002-06-12 | 2004-01-22 | Matsushita Electric Ind Co Ltd | Drying equipment, drying method, and manufacturing device and manufacturing method of magnetic recording medium |
| CN102072620A (en) * | 2011-01-28 | 2011-05-25 | 福建南平南孚电池有限公司 | Vacuum baking oven for pole pieces of battery |
| CN203216244U (en) * | 2013-03-20 | 2013-09-25 | 东莞市力嘉电池有限公司 | Lithium-ion battery vacuum baking device |
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