CN107139371A - Microwave forming method for Thermocurable polyimide sheet material - Google Patents
Microwave forming method for Thermocurable polyimide sheet material Download PDFInfo
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- CN107139371A CN107139371A CN201710479025.8A CN201710479025A CN107139371A CN 107139371 A CN107139371 A CN 107139371A CN 201710479025 A CN201710479025 A CN 201710479025A CN 107139371 A CN107139371 A CN 107139371A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
- B29C43/14—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles in several steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/36—Moulds for making articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/52—Heating or cooling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
- B29C2035/0855—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using microwave
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
- B29C2043/5816—Measuring, controlling or regulating temperature
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention belongs to polymer composite field shaping technique, and in particular to the microwave forming method for Thermocurable polyimide sheet material.This method weighs the ferroelectric ceramics powder, ground carbon fiber powder and Thermocurable polyimide powder of certain part by weight first, above raw material is added in mixer and carries out dry mixed, it is pre-stamped on cold press, then it is put into particular manufacturing craft in micro-wave oven, carry out microwave thermoforming, it is placed on afterwards on hot press and carries out thermocompression forming, then the demoulding is handled afterwards, you can obtain satisfactory Thermocurable polyimide sheet material.This method possesses that technique is simple, equipment is environmentally friendly, energy saving and easy-operating advantage, while can ensureing that the polyimide material properties after shaping can meet use requirement, moreover it is possible to greatly improve the production efficiency and quality stability of Thermocurable polyimide sheet material.
Description
Technical field
The invention belongs to polymer composite field shaping technique, and in particular to for Thermocurable polyimide sheet material
Microwave forming method.
Background technology
Polyimides refers on main chain that one containing imide ring (- CO-NH-CO-) birdss of the same feather flock together compound, wherein to contain phthaloyl
The polymer of imine structure is mostly important.Polyimides is as a kind of special engineered material, in the sixties in last century, polyimides
It is put into one of 21 century most promising engineering plastics.Polyimides can be divided into two kinds according to moulding process：Thermoplasticity and heat
Solidity.Due to containing the aromatic rings and imide group repeated in Thermocurable polyimide molecular structure so that the material has
Excellent mechanical performance, hot property, fire resistance, dielectric properties, environmental performance etc..But, although Thermocurable polyimide material
Material has above-mentioned excellent combination property, but its poor processability, difficult forming greatly limit its application field；Especially
Mechanically and electrically subdomains have more demands to high thickness PI sheet materials, but thickness is more than more than 35mm Thermocurable polyimide
Sheet material, current product qualification rate is even below 50%.The forming process of Thermocurable polyimide sheet material is that the generation of its strand is solidifying
Gel and the process of orientation, it is desirable to which forming temperature is high (being more than 400 DEG C), briquetting pressure is big (being more than 100MPa), so to equipment
Requirement it is very high.Current Thermocurable polyimide sheet material is the electrical heating method of forming using most forming methods, but due to electricity
Heating is to pass to polyimide material by external heat sources such as the gases after metal die or heating, easily cause material it is inside and outside by
Heat it is uneven, occur product " cold " center " phenomenon, this can cause shaping after sheet material occur being layered or cracking situation, and it is wear-resisting and
Mechanical performance can not meet use requirement.In addition, the electrical heating method of forming is also present, power consumption is big, time-consuming, and production efficiency is low to ask
Topic.How a kind of more simple and efficient forming method for Thermocurable polyimide sheet material is sought, so as to ensure shaping
While polyimide material properties afterwards can meet use requirement, its production efficiency and steady quality are greatly improved
Property, it is this area technical barrier urgently to be resolved hurrily in recent years.
The content of the invention
The purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art there is provided the microwave for Thermocurable polyimide sheet material
Forming method, this method possesses that technique is simple, equipment is environmentally friendly, energy saving and easy-operating advantage, can be after shaping is ensured
Polyimide material properties while can meet use requirement, moreover it is possible to greatly improve Thermocurable polyimide sheet material
Production efficiency and quality stability.
To achieve the above object, present invention employs following technical scheme：
A kind of microwave forming method for Thermocurable polyimide sheet material, it is characterised in that comprise the following steps：
1), batch mixing
Remove the raw material of row parts by weight：
10~35 parts of ferroelectric ceramics powder；
0~15 part of ground carbon fiber powder；
50~90 parts of Thermocurable polyimide powder；
Above raw material is added in mixer, 5~10 minutes are stirred under 300~500RPM rotating speeds, then 100~
Stirred 10~15 minutes under 200RPM rotating speeds, compound is taken out stand-by；
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 260~300 DEG C is protected, and dries 1~1.5
Hour；
3) it is, pre-stamped
Weigh the process step 2 of constant weight) dry compound, be put into particular manufacturing craft die cavity and carried out using press
It is pre-stamped；Slow pressurization in three times, first time pressure is 30~50MPa, and second is 50~100MPa, and third time pressure is
100~150MPa；Followed by that particular manufacturing craft is locked, compound is maintained in particular manufacturing craft, pressurize 5~15 minutes, stand-by；
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of compound in micro-wave oven, close fire door, microwave frequency be adjusted to
2450MHZ, when furnace temperature rises to 405 DEG C~415 DEG C, closes microwave rf generator, and is incubated 15~60 minutes, and electricity is closed afterwards
Source；
5), thermocompression forming, the demoulding
By step 4) in particular manufacturing craft taken out from micro-wave oven, and place it on hot press, 405 DEG C of temperature~
Initial compression is to 50MPa at 415 DEG C；Particular manufacturing craft is unlocked, property is pressurized to 120~150MPa again, heat-insulation pressure keeping 10~
30 minutes, stop heating；When mold temperature is reduced to below 100 DEG C, the demoulding obtains Thermocurable polyimide sheet material.
It is preferred that, 35~55 μm of the particle size range of the Thermocurable polyimide powder, range of number-average molecular weight 0.4~
2.5 ten thousand, dielectric constant range 2.8~4, dielectric loss scope 0.005~0.01.
It is preferred that, the ferroelectric ceramics powder at least includes CaCu 3 Ti 4 O and barium strontium titanate；Ferroelectric ceramics powder diameter model
Enclose 5~20 μm, dielectric constant range 104~105, dielectric loss scope 0.01~0.05.
It is preferred that, 5~12 μm of the diameter range of the ground carbon fiber powder, draw ratio scope 6：1~8：1, stretching is strong
Degree >=2GPa, Young's modulus >=250GPa.
It is preferred that, the particular manufacturing craft includes the exterior mould of barrel chamber vertical setting and is respectively cooperating with two ends of exterior mould
The upper holder block and lower lock block at place, upper holder block and the lower lock block profile are block in the step of two-period form, each briquetting it is small-bore
In the insertion outer die casing barrel chamber that section is coincide and accordingly seam is constituted between the shoulder of briquetting and the respective barrel end of exterior mould to coordinate；Push
The clamping screw for locking lower lock block, exterior mould and upper holder block in vertical, clamping screw are connected with the shoulder of block
Axis vertical extends through exterior mould barrel and upper holder block and constitutes screw thread between the locking nut at upper holder block top surface
Coordinate；Arrangement isolates mutual cushion block, and at least external mold between upper holder block and compound and between lower lock block and compound
Contacted with compound one section of stack shell on cylinder is made up of ceramic material.
It is preferred that, in vertical, the exterior mould is cut into three sections of cylinders by twice horizontal plane parallel to each other
Three sections of tube structures are respectively designated as epimere mould cylinder, stage casing ceramic die cylinder and lower die cylinder, the stage casing ceramic die by structure
The height that the inner tube wall of cylinder constitutes the contact surface that is in contact with compound and stage casing ceramic die cylinder is higher than upper holder block and lower lock block
Spacing between adjacent surface.
The beneficial effects of the present invention are：
1), abandon traditional electrical heating method of forming and prepare such as shaping back plate caused by Thermocurable polyimide sheet material
Material occurs being layered or ftractureed and defect that preparation efficiency is low.One aspect of the present invention is high by being added in polyimide matrix
The ceramic material of dielectric constant, to improve the dielectric constant of composite polyimide material, 10~30, realization are brought up to from 2.8~4
The huge improvement of polyimide material absorbing property, provides operational feasibility for the shaping of its microwave, realizes polyimides material
The diversity of the forming method of material.And on the other hand, then using outside microwave source, make polyimide material self-heating, with
Ensure that material is heated evenly from inside to outside, forming temperature can be reached simultaneously, and be molded under pressure, it is final to cause after shaping
Polyimide material be not in the phenomenons such as layering, cracking, and wear-resisting and mechanical performance etc. can meet use requirement.
To sum up, the present invention possess that technique is simple, equipment is environmentally friendly, energy saving and advantage easy to operate, heat can be greatly improved
The production efficiency and quality stability of solidity polyimides sheet material.Its one side breaches high thickness Thermocurable polyimide sheet material
Forming technique barrier, solve the technological difficulties of high thickness sheet material layering easy to crack；On the other hand as microwave equipment is molded
The amplification in space, it is possible to achieve the mass shaping of Thermocurable polyimide material, substantially increases the life of polyimide material
Efficiency is produced, so as to reduce production cost, this obviously also can play very big to the popularization and application of Thermocurable polyimide material
Facilitation.
2), on the basis of said structure, the present invention has also carried out certain restriction to the construction of particular manufacturing craft.Actually make
Used time, it is contemplated that particular manufacturing craft needs to carry out a series of locking, pressurize or even microwave hyperthermia operation, therefore, a side of the invention
Face is coordinated using the seam of the stabilization between upper holder block, exterior mould and lower lock block, to ensure the reliable operation during mould use
Property；On the other hand, by clamping screw collocation locking nut, to realize the quick lock in and unblock effect of foregoing particular manufacturing craft
Really.What is more important, for the stage casing of exterior mould, namely stage casing ceramic die cylinder part, should be made using ceramic material, from
And the premium properties such as high-k, low lossy microwave, temperature coefficient be small of ceramics itself is utilized, to realize to inside ceramics
Being rapidly heated and heat insulation effect for compound, finally make it that the functional reliability and efficiency of whole technique are effectively carried
Rise.
Brief description of the drawings
Fig. 1 is the structure sectional view of particular manufacturing craft.
The actual corresponding relation of each label of the present invention and component names is as follows：
10- exterior moulds
11- epimeres mould cylinder 12- stage casings ceramic die cylinder 13- lower die cylinders
20- upper holder block 30- lower lock blocks
41- clamping screw 42- locking nut 50- cushion blocks
Embodiment
For ease of understanding, described further below is made to the concrete structure and working method of the present invention herein：
The principle of polyimide material microwave heating is：When polar molecule dielectric and non-polar molecule dielectric are placed in microwave
When in electromagnetic field, existing dipole or the dipole of formation are rearranged in dielectric material, and with high-frequency alternating electromagnetic field
Swung with the speed of up to several hundred million times per second；Molecule will be rearranged with the direction for the high-frequency electric field being continually changing, just necessary
Overcome interference and obstruction that the original warm-up movement of molecule and molecule are acted on each other, produce the effect similar to friction, realize and divide
" stirring " of sub- level, so as to produce substantial amounts of heat.The present invention is exactly using outside microwave source, so that polyimide material
Self-heating, and then material is heated evenly from inside to outside, forming temperature can be reached simultaneously, and be molded under pressure,
It is final to obtain required Thermocurable polyimide sheet material.
The whole method flow of the present invention comprises the following steps：
1), batch mixing
Remove the raw material of row parts by weight：
10~35 parts of ferroelectric ceramics powder；
0~15 part of ground carbon fiber powder；
50~90 parts of Thermocurable polyimide powder；
Wherein：
35~55 μm of the particle size range of Thermocurable polyimide powder, range of number-average molecular weight 0.4~2.5 ten thousand, dielectric is normal
Number scope 2.8~4, dielectric loss scope 0.005~0.01.Ferroelectric ceramics powder at least includes CaCu 3 Ti 4 O and barium strontium titanate；
5~20 μm of ferroelectric ceramics powder diameter scope, dielectric constant range 104~105, dielectric loss scope 0.01~0.05.Grind
5~12 μm of the diameter range of carbon fiber powder, draw ratio scope 6：1~8：1, tensile strength >=2GPa, Young's modulus >=
250GPa。
Above raw material is added it in mixer, stirs 5~10 minutes, then exists under 300~500RPM rotating speeds
Stirred 10~15 minutes under 100~200RPM rotating speeds, compound is taken out stand-by.
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 260~300 DEG C is protected, and dries 1~1.5
Hour.
3) it is, pre-stamped
Weigh the process step 2 of constant weight) compound dried, take the top board and corresponding pad of particular manufacturing craft apart
Plate, so that compound is put into particular manufacturing craft die cavity, the position of compound is referring between two groups of cushion blocks 50 in Fig. 1
X wire segment mark position.Afterwards, particular manufacturing craft is reclosed, and it is pre-stamped using being carried out on press.Slow pressurization in three times,
First time pressure is 30~50MPa, and second is 50~100MPa, and third time pressure is 100~150MPa；Lock is utilized followed by
The screw thread each other of tight bolt 41 and locking nut 42 coordinates, thus particular manufacturing craft is locked, referring in particular to shown in Fig. 1, to incite somebody to action
Compound is maintained in particular manufacturing craft.It is stand-by by particular manufacturing craft pressurize 5~15 minutes.
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of compound in micro-wave oven, close fire door, microwave frequency be adjusted to
2450MHZ, when furnace temperature rises to 405 DEG C~415 DEG C, closes microwave rf generator, and is incubated 15~60 minutes, and electricity is closed afterwards
Source.
5), thermocompression forming, the demoulding
By step 4) in particular manufacturing craft taken out from micro-wave oven, and place it on hot press, 405 DEG C of temperature~
Initial compression is to 50MPa at 415 DEG C；Locking nut 42 is shed, to loosen top board 20, cushion block 50, exterior mould 10 and to push
Plate 30, again property be pressurized to 120~150MPa, heat-insulation pressure keeping 10~30 minutes stops heating；When mold temperature is reduced to 100
When below DEG C, the demoulding obtains Thermocurable polyimide sheet material.
For ease of further understanding, specific examples below is remake out herein to illustrate：
Embodiment 1：
1), batch mixing
The CaCu 3 Ti 4 O powder of 10 parts by weight and the Thermocurable polyimide powder of 50 parts by weight are weighed, three are added it to
Tie up in mixer, stir 10 minutes, then stirred 15 minutes under 150RPM rotating speeds under 300RPM rotating speeds, taken out stand-by.
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 300 DEG C is protected, dries 1 hour.
3) it is, pre-stamped
By step 2) in obtained dried compound add in the die cavity of particular manufacturing craft, be placed on press and carry out precompressed
System, first is pressurized to 30MPa, and 60MPa is pressurized to for the second time, and 100MPa, pressurize 8 minutes, by particular manufacturing craft are pressurized to for the third time
Locked, material is maintained in particular manufacturing craft, after release, stand-by.
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of polyimide material in special microwave oven, fire door is closed, by microwave
Frequency is adjusted to 2450MHZ, when furnace temperature rises to 405 DEG C, closes microwave rf generator, and is incubated 20 minutes, closes power supply.
5), thermocompression forming, the demoulding
It is rapid from micro-wave oven to take out particular manufacturing craft, and place it on hot press (temperature is up to 410 DEG C), it is preliminary to add
50MPa is pressed onto, particular manufacturing craft locking device is shed, property is pressurized to 120MPa again, heat-insulation pressure keeping 10 minutes stops adding
Heat, when particular manufacturing craft temperature is reduced to below 100 DEG C, polyimides sheet material is taken out in the demoulding.
By identifying that plate surface is smooth to the polyimides, uniform color has no layering and ftractureed, performance mirror
Surely use requirement is met.
Embodiment 2：
1), batch mixing
Weigh the heat of the CaCu 3 Ti 4 O powder of 35 parts by weight, the ground carbon fiber powder of 15 parts by weight, and 90 parts by weight
Solidity polyimide powder, is added it in three-dimensional mixer, is stirred 5 minutes under 500RPM rotating speeds, then in 200RPM
Stir 10 minutes, take out stand-by under rotating speed.
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 300 DEG C is protected, dries 1 hour.
3) it is, pre-stamped
By step 2) in obtained dried compound add in the die cavity of particular manufacturing craft, be placed on press and carry out precompressed
System, first is pressurized to 40MPa, and 100MPa is pressurized to for the second time, and 150MPa, pressurize 15 minutes, by die for special purpose are pressurized to for the third time
Tool is locked, and material is maintained in particular manufacturing craft, after release, stand-by.
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of polyimide material in special microwave oven, fire door is closed, by microwave
Frequency is adjusted to 2450MHZ, when furnace temperature rises to 415 DEG C, closes microwave rf generator, and is incubated 40 minutes, closes power supply.
5), thermocompression forming, the demoulding
It is rapid from micro-wave oven to take out particular manufacturing craft, and place it on hot press (temperature is up to 410 DEG C), it is preliminary to add
50MPa is pressed onto, particular manufacturing craft locking device is shed, property is pressurized to 150MPa again, heat-insulation pressure keeping 30 minutes stops adding
Heat, when particular manufacturing craft temperature is reduced to below 100 DEG C, polyimides sheet material is taken out in the demoulding.
By identifying that plate surface is smooth to the polyimides, uniform color has no layering and ftractureed, performance mirror
Surely use requirement is met.
Embodiment 3：
1), batch mixing
Weigh the heat of the CaCu 3 Ti 4 O powder of 15 parts by weight, the ground carbon fiber powder of 35 parts by weight, and 60 parts by weight
Solidity polyimide powder, is added it in three-dimensional mixer, is stirred 5 minutes under 400RPM rotating speeds, then in 100RPM
Stir 15 minutes, take out stand-by under rotating speed.
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 270 DEG C is protected, dries 1 hour.
3) it is, pre-stamped
By step 2) in obtained dried compound add in the die cavity of particular manufacturing craft, be placed on press and carry out precompressed
System, first is pressurized to 40MPa, and 60MPa is pressurized to for the second time, and 120MPa, pressurize 10 minutes, by particular manufacturing craft are pressurized to for the third time
Locked, material is maintained in particular manufacturing craft, after release, stand-by.
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of polyimide material in special microwave oven, fire door is closed, by microwave
Frequency is adjusted to 2450MHZ, when furnace temperature rises to 410 DEG C, closes microwave rf generator, and is incubated 40 minutes, closes power supply.
5), thermocompression forming, the demoulding
It is rapid from micro-wave oven to take out particular manufacturing craft, and place it on hot press (temperature is up to 410 DEG C), it is preliminary to add
50MPa is pressed onto, particular manufacturing craft locking device is shed, property is pressurized to 150MPa again, heat-insulation pressure keeping 20 minutes stops adding
Heat, when particular manufacturing craft temperature is reduced to below 100 DEG C, polyimides sheet material is taken out in the demoulding.
By identifying that plate surface is smooth to the polyimides, uniform color has no layering and ftractureed, performance mirror
Surely use requirement is met.
It in summary it can be seen, the polyimides sheet material manufactured using the microwave method of forming of present disclosure, its smooth in appearance,
Uniform color, have no cracking and be layered.The present invention possesses that technique is simple, equipment is environmentally friendly, energy saving and easy-operating advantage, can
While can meet use requirement in the polyimide material properties after ensureing shaping, moreover it is possible to greatly improve thermosetting
The production efficiency and quality stability of polyimides sheet material.
Claims (6)
1. a kind of microwave forming method for Thermocurable polyimide sheet material, it is characterised in that comprise the following steps：
1), batch mixing
Remove the raw material of row parts by weight：
10~35 parts of ferroelectric ceramics powder；
0~15 part of ground carbon fiber powder；
50~90 parts of Thermocurable polyimide powder；
Above raw material is added in mixer, 5~10 minutes are stirred under 300~500RPM rotating speeds, then 100~
Stirred 10~15 minutes under 200RPM rotating speeds, compound is taken out stand-by；
2), dry
By step 1) obtained compound is put into the baking oven that the nitrogen that furnace temperature is 260~300 DEG C is protected, and dries 1~1.5 small
When；
3) it is, pre-stamped
Weigh the process step 2 of constant weight) dry compound, be put into particular manufacturing craft die cavity and using press carry out precompressed
System；Slow pressurization in three times, first time pressure is 30~50MPa, is for second 50~100MPa, third time pressure is 100~
150MPa；Followed by that particular manufacturing craft is locked, compound is maintained in particular manufacturing craft, pressurize 5~15 minutes, stand-by；
4), microwave is molded
By step 3) in be put into equipped with the particular manufacturing craft of compound in micro-wave oven, close fire door, microwave frequency be adjusted to
2450MHZ, when furnace temperature rises to 405 DEG C~415 DEG C, closes microwave rf generator, and is incubated 15~60 minutes, and electricity is closed afterwards
Source；
5), thermocompression forming, the demoulding
By step 4) in particular manufacturing craft taken out from micro-wave oven, and place it on hot press, in temperature 405 DEG C~415
Initial compression is to 50MPa at DEG C；Particular manufacturing craft is unlocked, property is pressurized to 120~150MPa, 10~30 points of heat-insulation pressure keeping again
Clock, stops heating；When mold temperature is reduced to below 100 DEG C, the demoulding obtains Thermocurable polyimide sheet material.
2. the microwave forming method according to claim 1 for Thermocurable polyimide sheet material, it is characterised in that：It is described
35~55 μm of the particle size range of Thermocurable polyimide powder, range of number-average molecular weight 0.4~2.5 ten thousand, dielectric constant range 2.8
~4, dielectric loss scope 0.005~0.01.
3. the microwave forming method according to claim 1 for Thermocurable polyimide sheet material, it is characterised in that：It is described
Ferroelectric ceramics powder at least includes CaCu 3 Ti 4 O and barium strontium titanate；5~20 μm of ferroelectric ceramics powder diameter scope, dielectric constant model
Enclose 104~105, dielectric loss scope 0.01~0.05.
4. the microwave forming method according to claim 1 for Thermocurable polyimide sheet material, it is characterised in that：It is described
5~12 μm of the diameter range of ground carbon fiber powder, draw ratio scope 6：1~8：1, tensile strength >=2GPa, Young's modulus >=
250GPa。
5. the microwave forming method for Thermocurable polyimide sheet material according to claim 1 or 2 or 3 or 4, its feature
It is：The particular manufacturing craft includes the exterior mould (10) of barrel chamber vertical setting and is respectively cooperating with (10) two ends of exterior mould
Upper holder block (20) and lower lock block (30), the upper holder block (20) and lower lock block (30) profile be block in the step of two-period form,
The respective barrel end of the shoulder and exterior mould (10) of the small-bore section of identical interior and corresponding briquetting of insertion outer die casing barrel chamber of each briquetting
Between constitute seam coordinate；It is connected with the shoulder of lower lock block (30) for locking lower lock block (30), exterior mould in vertical
(10) and upper holder block (20) clamping screw (41), clamping screw (41) axis vertical extend through exterior mould (10) barrel and
Upper holder block (20) simultaneously constitutes screw thread cooperation between the locking nut (42) at upper holder block (20) top surface；Upper holder block (20) is with mixing
Close between expecting and lower lock block (30) is arranged between compound and isolates mutual cushion block (50), and at least on exterior mould (10)
Contacted with compound one section of stack shell be made up of ceramic material.
6. the microwave forming method according to claim 5 for Thermocurable polyimide sheet material, it is characterised in that：In lead
Hang down on direction, the exterior mould (10) is cut into three sections of tube structures by twice horizontal plane parallel to each other, by three sections of cylinders
Body structure is respectively designated as epimere mould cylinder (11), stage casing ceramic die cylinder (12) and lower die cylinder (13), the stage casing ceramic die cylinder
(12) inner tube wall constitutes the contact surface being in contact with compound and the height of stage casing ceramic die cylinder is higher than upper holder block (20) with
Spacing between the adjacent surface of briquetting (30).
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| CN113580454A (en) * | 2021-08-17 | 2021-11-02 | 江苏泰氟隆科技有限公司 | Manufacturing process of polyimide plate processed by multilayer vacuum hot press |
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