CN102391646A - Enhanced high-insulation composite material and preparation method thereof - Google Patents
Enhanced high-insulation composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an enhanced high-insulation composite material and a preparation method thereof. The composite material comprises matrix resin and an additive, wherein the matrix resin is micron polyimide (PI); the additive is nano zinc oxide (ZnO); and the composite material comprises 90 to 99 % of PI and 1 to 10 % of ZnO. The preparation method for the enhanced high-insulation composite material comprises the following steps of dispersing ZnO; performing surface treatment; performing PI moulding powder pretreatment; mixing two kinds of raw material powder through liquid phase; stirring quickly; drying; performing cold press moulding; and performing high-temperature moulding. The composite material prepared by the method has high insulativity and excellent heating conductivity and can be applied in the application field of engineering with high insulativity requirement on a polymer material and high working temperature of the material, so that the insulation structure size is shrunk, the insulation design requirement of the system is guaranteed, and the problem of the service life of equipment caused by heating and ageing of the material can be solved.
Description
Technical field
The invention belongs to the polymer composites technical field, be specifically related to high insulating composite material of a kind of enhancement type and preparation method thereof.
Background technology
The extensive application of polymeric media in electric and electronic technical field, and be accompanied by the microminiaturization development of power electronic equipment, the polymeric media insulating property have been proposed increasingly high requirement.Therefore, when reaching the equipment microminiaturization through reducing the insulation system size, the strength of electric field that dielectric bore can further increase, and causes insulating material partial breakdown even whole possibility increasing of burning.Simultaneously, the polymeric media of high insulating property has relatively poor thermal conductivity usually, causes equipment heat in service to scatter and disappear and makes the material long term operation at comparatively high temps, and this lasting heating is aging can to badly influence insulating material performance and life-span.Polyimide PI is a kind of common special engineering plastics, is widely used in special dimensions such as microelectronics as structured material and functional material.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art; The object of the present invention is to provide high insulating composite material of a kind of enhancement type and preparation method thereof; Adopt the matrix material of the inventive method preparation to have the enhanced high insulating property; Heat conductivility can be used for the equipment such as power electronics of the high insulating requirements of needs than the obvious improvement of straight polymer simultaneously, thereby guarantees the design requirements of equipment integral insulating.
In order to achieve the above object, the technical scheme that the present invention adopted is:
The high insulating composite material of a kind of enhancement type; Said matrix material comprises matrix resin and additive; Said matrix resin is polyimide PI; Said additive is zinc oxide ZnO, and the mass percent of each component is in this matrix material: polyimide PI is 90～99%, zinc oxide ZnO is 1%～10%.
Said matrix resin is micron order polyimide PI, and said additive is Nano-class zinc oxide ZnO.
The mass percent of each component is in the said matrix material: polyimide PI is 92～98%, zinc oxide ZnO is 2%～8%.
The mass percent of each component is in the said matrix material: polyimide PI is 96%, zinc oxide ZnO is 4%.
A kind of method for preparing above-mentioned matrix material comprises the steps:
Step 1:ZnO disperses and surface treatment; Take by weighing the zinc oxide ZnO powder of powder diameter less than the preset quality of 100nm; Adding volume is in the alcohol of 5～10 times of zinc oxide ZnO powder volumes; Suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 30～60min then; In suspension-s, add the coupling agent account for zinc oxide ZnO quality 1～5% in the ultrasonic vibration process, disperseed after the suspension-s that will add coupling agent subsequently places baking oven that alcohol is dried and surface treatment after zinc oxide ZnO raw material;
The pre-treatment of polyimide PI moulding powder takes by weighing the polyimide PI moulding powder of powder diameter less than the preset quality of 20 μ m, is placed on then and dries 12～24h in the baking oven, and bake out temperature is 70～90 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 1%～10% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 2～4 times of mixture volumes, stirs 30～60min and obtains finely dispersed suspension-s, puts into baking oven then and dries;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 8～12MPa, the time length is 15s, colds pressing repeatedly 3～5 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 8～12MPa; Mold temperature is that sectional heats up and insulation; The final molding temperature is 320～340 ℃, lowers the temperature naturally with body of heater afterwards, obtains finished product.
The described coupling agent of step 1 is silane coupling agent KH550.
It is 80～100 ℃ that the suspension-s of the said adding coupling agent of step 1 places the bake out temperature of baking oven, and drying time is 24～36h.
It is 80～100 ℃ that said polyimide PI of step 2 and the finely dispersed suspension-s of zinc oxide ZnO compound place the bake out temperature of baking oven, and drying time is 48～72h.
The said sectional of step 4 heats up and insulating process does, begins 30min by room temperature and rises to 260 ℃, rises to 320～340 ℃ with 30min again behind the insulation 30min, insulation 30～60min.
The present invention is through carrying out the blend moulding with Nano-class zinc oxide ZnO powder and special engineering plastics polymeric media polyimide PI; Therefore in zinc oxide ZnO powder adding matrix resin; Between matrix resin and additive, formed a large amount of interface traps, and because the less interface trap that causes of size of additive is darker, thereby carrier mobility in the medium fettered; Form higher volume specific resistance, the insulating property of the polymer composites of therefore processing are enhanced.Simultaneously, because additive zinc oxide ZnO is a kind of mineral filler, have high thermal, because be dispersed in the overall thermal conductivity ability that just can improve material in the matrix resin.Thereby use the power electronic equipment of this matrix material, and can be when reducing the insulation system size, the working life of insulating material when satisfying apparatus insulated design requirements and guaranteeing that working temperature is higher.
The matrix material high insulating property of research has two important index, i.e. direct current volume conductance (the direct current volume specific resistance is reciprocal) and non-linear conductance characteristic.Direct current volume conductivity table has been levied the insulation characterisitic of material under the low voltage effect; Volume current density is with the variation tendency of strength of electric field in the medium under high electric field action for non-linear conductance characteristic present material, and the non-linear conductance characteristic has two key parameters, and one is threshold field intensity, and another is a non-linearization trend.Threshold field intensity is that nonlinearized initial strength of electric field takes place the medium volume conductance, and non-linearization trend is meant when electric field surpasses threshold field, the intensity of variation of non-linear conductance characteristic.
The heat conductivility of the matrix material of research has a leading indicator, the i.e. thermal conductivity of material.Thermal conductivity characterizes the heat that unit temperature gradient (temperature reduces 1K in 1m length) is transmitted through the unit thermal conductive surface in the unit time.Thermal conductivity curve under the varying environment temperature is reflection material transmissibility to heat when the different operating temperature.
Prepared composite material of the present invention is compared with pure polyimide PI; The direct current volume conductance descends to some extent under normal environment; The threshold field of non-linear conductance characteristic obviously descends simultaneously; Non-linearization trend weakens, and these two kinds of conductivity characteristics insulation characterisitic that promptly shows material that descends simultaneously is enhanced.Simultaneously, the heat conductivility of matrix material is compared with straight polymer and is increased, and along with the rising of envrionment temperature, thermal conductivity is also higher.
Description of drawings
Fig. 1 is the process flow sheet of composite material and preparation method thereof of the present invention.
Fig. 29 kinds of different proportioning matrix material direct current volume conductance comparison diagrams that to be pure polyimide PI obtain with the inventive method.
Fig. 35 kinds of different proportioning matrix material non-linear conductance characteristic comparison diagrams that to be pure polyimide PI obtain with the inventive method.
Fig. 45 kinds of different proportioning matrix materials thermal conductivity comparison diagram under the varying environment temperature that to be pure polyimide PI obtain with the inventive method.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment the present invention is explained further details.
Embodiment one
As shown in Figure 1, the preparation method of the high insulating composite material of present embodiment enhancement type may further comprise the steps:
Step 1: zinc oxide ZnO disperses and surface treatment; Taking by weighing the powder diameter is the zinc oxide ZnO powder of the preset quality of 100nm; Adding volume is in the alcohol of 5 times of zinc oxide ZnO powder volumes, and the suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 30min then, in suspension-s, adds the coupling agent that accounts for zinc oxide ZnO quality 1% in the ultrasonic vibration process; The suspension-s that will add coupling agent subsequently places baking oven to dry 24h; Bake out temperature is 100 ℃, with disperseed after the alcohol oven dry and surface treatment after zinc oxide ZnO raw material, described coupling agent is silane coupling agent KH550;
The pre-treatment of polyimide PI moulding powder, taking by weighing the powder diameter is the polyimide PI moulding powder of the preset quality of 18 μ m, is placed on then and dries 12h in the baking oven, bake out temperature is 90 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 1% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 2 times of mixture volumes, utilizes whisking appliance to stir 30min fast and obtains finely dispersed suspension-s, puts into baking oven then and dries; Bake out temperature is 80 ℃, and drying time is 72h;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 8MPa, the time length is 15s, colds pressing repeatedly 5 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 8MPa; Mold temperature is that sectional heats up and insulation, and detailed process is to begin 30min by room temperature and rise to 260 ℃; Rise to 320 ℃ with 30min again behind the insulation 30min; Insulation 60min lowers the temperature with body of heater afterwards naturally, obtains finished product.
Embodiment two
As shown in Figure 1, the preparation method of the high insulating composite material of present embodiment enhancement type may further comprise the steps:
Step 1: zinc oxide ZnO disperses and surface treatment; Taking by weighing the powder diameter is the zinc oxide ZnO powder of the preset quality of 80nm; Adding volume is in the alcohol of 10 times of zinc oxide ZnO powder volumes, and the suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 60min then, in suspension-s, adds the coupling agent that accounts for zinc oxide ZnO quality 5% in the ultrasonic vibration process; The suspension-s that will add coupling agent subsequently places baking oven to dry 36h; Bake out temperature is 80 ℃, with disperseed after the alcohol oven dry and surface treatment after zinc oxide ZnO raw material, described coupling agent is silane coupling agent KH550;
The pre-treatment of polyimide PI moulding powder, taking by weighing the powder diameter is the polyimide PI moulding powder of the preset quality of 10 μ m, is placed on then and dries 24h in the baking oven, bake out temperature is 70 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 10% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 4 times of mixture volumes, utilizes whisking appliance to stir 60min fast and obtains finely dispersed suspension-s, puts into baking oven then and dries; Bake out temperature is 100 ℃, and drying time is 48h;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 12MPa, the time length is 15s, colds pressing repeatedly 3 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 12MPa; Mold temperature is that sectional heats up and insulation, and detailed process is to begin 30min by room temperature and rise to 260 ℃; Rise to 340 ℃ with 30min again behind the insulation 30min; Insulation 30min lowers the temperature with body of heater afterwards naturally, obtains finished product.
Embodiment three
As shown in Figure 1, the preparation method of the high insulating composite material of present embodiment enhancement type may further comprise the steps:
Step 1: zinc oxide ZnO disperses and surface treatment; Take by weighing the ZnO powder that the powder diameter is the preset quality of 60nm; Adding volume is in the alcohol of 7 times of zinc oxide ZnO powder volumes, and the suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 40min then, in suspension-s, adds the coupling agent that accounts for zinc oxide ZnO quality 2% in the ultrasonic vibration process; The suspension-s that will add coupling agent subsequently places baking oven to dry 30h; Bake out temperature is 90 ℃, with disperseed after the alcohol oven dry and surface treatment after zinc oxide ZnO raw material, described coupling agent is silane coupling agent KH550;
The pre-treatment of polyimide PI moulding powder, taking by weighing the powder diameter is the polyimide PI moulding powder of the preset quality of 8 μ m, is placed on then and dries 18h in the baking oven, bake out temperature is 80 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 2% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 3 times of mixture volumes, utilizes whisking appliance to stir 45min fast the suspension-s of compound is uniformly dispersed, and puts into baking oven after the end and dries; Bake out temperature is 90 ℃, and drying time is 60h;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 10MPa, the time length is 15s, colds pressing repeatedly 4 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 10MPa; Mold temperature is that sectional heats up and insulation, and detailed process is to begin 30min by room temperature and rise to 260 ℃; Rise to 330 ℃ with 30min again behind the insulation 30min; Insulation 45min lowers the temperature with body of heater afterwards naturally, obtains finished product.
Embodiment four
As shown in Figure 1, the preparation method of the high insulating composite material of present embodiment enhancement type may further comprise the steps:
Step 1: zinc oxide ZnO disperses and surface treatment; Take by weighing the ZnO powder that the powder diameter is the preset quality of 60nm; Adding volume is in the alcohol of 7 times of zinc oxide ZnO powder volumes, and the suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 50min then, in suspension-s, adds the coupling agent that accounts for zinc oxide ZnO quality 4% in the ultrasonic vibration process; The suspension-s that will add coupling agent subsequently places baking oven to dry 30h; Bake out temperature is 90 ℃, with disperseed after the alcohol oven dry and surface treatment after zinc oxide ZnO raw material, described coupling agent is silane coupling agent KH550;
The pre-treatment of polyimide PI moulding powder, taking by weighing the powder diameter is the polyimide PI moulding powder of the preset quality of 8 μ m, is placed on then and dries 18h in the baking oven, bake out temperature is 80 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 8% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 3 times of mixture volumes, utilizes whisking appliance to stir 45min fast the suspension-s of compound is uniformly dispersed, and puts into baking oven after the end and dries; Bake out temperature is 90 ℃, and drying time is 60h;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 10MPa, the time length is 15s, colds pressing repeatedly 4 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 10MPa; Mold temperature is that sectional heats up and insulation, and detailed process is to begin 30min by room temperature and rise to 260 ℃; Rise to 330 ℃ with 30min again behind the insulation 30min; Insulation 45min lowers the temperature with body of heater afterwards naturally, obtains finished product.
Embodiment five
As shown in Figure 1, the preparation method of the high insulating composite material of present embodiment enhancement type may further comprise the steps:
Step 1: zinc oxide ZnO disperses and surface treatment; Take by weighing the ZnO powder that the powder diameter is the preset quality of 50nm; Adding volume is in the alcohol of 7 times of zinc oxide ZnO powder volumes, and the suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 45min then, in suspension-s, adds the coupling agent that accounts for zinc oxide ZnO quality 3% in the ultrasonic vibration process; The suspension-s that will add coupling agent subsequently places baking oven to dry 30h; Bake out temperature is 90 ℃, with disperseed after the alcohol oven dry and surface treatment after zinc oxide ZnO raw material, described coupling agent is silane coupling agent KH550;
The pre-treatment of polyimide PI moulding powder, taking by weighing the powder diameter is the polyimide PI moulding powder of the preset quality of 5 μ m, is placed on then and dries 18h in the baking oven, bake out temperature is 80 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 4% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 3 times of mixture volumes, utilizes whisking appliance to stir 45min fast the suspension-s of compound is uniformly dispersed, and puts into baking oven after the end and dries; Bake out temperature is 90 ℃, and drying time is 60h;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 10MPa, the time length is 15s, colds pressing repeatedly 4 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 10MPa; Mold temperature is that sectional heats up and insulation, and detailed process is to begin 30min by room temperature and rise to 260 ℃; Rise to 330 ℃ with 30min again behind the insulation 30min; Insulation 45min lowers the temperature with body of heater afterwards naturally, obtains finished product.
9 kinds of different proportioning matrix material direct current volume conductance comparison diagrams that Fig. 2 obtains for pure polyimide and the prepared method of the present invention; Can find out when additive level hour (less than 10%) by Fig. 2; Matrix material direct current volume conductance descends to some extent, and promptly insulating property are enhanced.Particularly when additive level was 4%, minimum value appearred in matrix material direct current volume conductance.
Fig. 3 is pure polyimide and the resulting 5 kinds of different proportioning matrix material non-linear conductance characteristic comparison diagrams of embodiment of the invention preparation method; As can beappreciated from fig. 3; The non-linear conductance characteristic threshold field of 5 kinds of different proportioning matrix materials all descends; Non-linearization trend obviously weakens, and this non-linear conductance characteristic that shows matrix material is weakened, and the insulation characterisitic under high electric field increases.Particularly when additive level was 4%, the non-linearization trend of matrix material became very faint, had effectively suppressed the Leakage Current in the complex media under the High-Field.
Fig. 4 is pure polyimide and the resulting 5 kinds of different proportioning matrix material heat conductivility comparison diagrams of embodiment of the invention preparation method; As can beappreciated from fig. 4; The heat conductivility of 5 kinds of different proportioning matrix materials all increases, and along with the rising of envrionment temperature, the thermal conductivity of material slightly increases.Particularly when additive level is 4%, the heat conductivility most excellent of matrix material.
Therefore; Take all factors into consideration direct current volume conductance, non-linear conductance characteristic and three factors of thermal conductivity; Zinc oxide ZnO accounts for matrix material total mass per-cent should be 1～10%, and best proportioning is 96% for polyimide PI accounts for total mass per-cent, and zinc oxide ZnO accounts for total mass per-cent 4%.
The best proportioning polyimide/zinc oxide composite that adopts preparation method according to the invention to obtain; Be that to account for the total mass mark be 4% sample to zinc oxide ZnO; The direct current volume conductance descends more than 50% than the pure polyimide that falls; The non-linear conductance characteristic obtains obvious suppression, and the matrix material overall thermal conductivity can obviously improve.Therefore adopt PI/ZnO matrix material that the inventive method obtains in normal environment, high electric field applied environment and under, have high insulating property and the working life more excellent than pure polyimide for a long time than the elevated operating temperature applied environment.
Claims (9)
1. high insulating composite material of enhancement type; It is characterized in that: said matrix material comprises matrix resin and additive; Said matrix resin is polyimide PI; Said additive is zinc oxide ZnO, and the mass percent of each component is in this matrix material: polyimide PI is 90～99%, zinc oxide ZnO is 1%～10%.
2. matrix material according to claim 1 is characterized in that: said matrix resin is micron order polyimide PI, and said additive is Nano-class zinc oxide ZnO.
3. matrix material according to claim 1 is characterized in that: the mass percent of each component is in the said matrix material: polyimide PI is 92～98%, zinc oxide ZnO is 2%～8%.
4. matrix material according to claim 3 is characterized in that: the mass percent of each component is in the said matrix material: polyimide PI is 96%, zinc oxide ZnO is 4%.
5. a method for preparing the said matrix material of claim 1 comprises the steps:
Step 1:ZnO disperses and surface treatment; Take by weighing the zinc oxide ZnO powder of powder diameter less than the preset quality of 100nm; Adding volume is in the alcohol of 5～10 times of zinc oxide ZnO powder volumes; Suspension-s with zinc oxide ZnO powder and alcohol places the ultrasonic vibration appearance to disperse 30～60min then; In suspension-s, add the coupling agent account for zinc oxide ZnO quality 1～5% in the ultrasonic vibration process, disperseed after the suspension-s that will add coupling agent subsequently places baking oven that alcohol is dried and surface treatment after zinc oxide ZnO raw material;
The pre-treatment of polyimide PI moulding powder takes by weighing the polyimide PI moulding powder of powder diameter less than the preset quality of 20 μ m, is placed on then and dries 12～24h in the baking oven, and bake out temperature is 70～90 ℃, obtains polyimide PI raw material after the pre-treatment;
Step 2: two kinds of raw materials of liquid-phase mixing also stir and dry processing fast; Take by weighing that the zinc oxide ZnO raw material behind the polyimide PI raw material and dispersion and surface treatment places beaker to form compound after the pre-treatment that step 1 obtains; Make the zinc oxide ZnO content account for 1%～10% of compound total mass; In beaker, adding volume is the alcohol formation suspension-s of 2～4 times of mixture volumes, stirs 30～60min and obtains finely dispersed suspension-s, puts into baking oven then and dries;
Step 3: coldmoulding, place grinding tool to carry out coldmoulding the finely dispersed suspension-s in step 2 oven dry back, forming pressure is 8～12MPa, the time length is 15s, colds pressing repeatedly 3～5 times, obtains sample after the coldmoulding;
Step 4: high-temperature molding, place moulding press to carry out high-temperature molding on the sample after step 3 coldmoulding, forming pressure is 8～12MPa; Mold temperature is that sectional heats up and insulation; The final molding temperature is 320～340 ℃, lowers the temperature naturally with body of heater afterwards, obtains finished product.
6. preparation method according to claim 5 is characterized in that: the described coupling agent of step 1 is silane coupling agent KH550.
7. preparation method according to claim 5 is characterized in that: it is 80～100 ℃ that the suspension-s of the said adding coupling agent of step 1 places the bake out temperature of baking oven, and drying time is 24～36h.
8. preparation method according to claim 5 is characterized in that: it is 80～100 ℃ that said polyimide PI of step 2 and the finely dispersed suspension-s of zinc oxide ZnO compound place the bake out temperature of baking oven, and drying time is 48～72h.
9. preparation method according to claim 5 is characterized in that: the said sectional of step 4 heats up and insulating process does, begins 30min by room temperature and rises to 260 ℃, rises to 320～340 ℃ with 30min again behind the insulation 30min, insulation 30～60min.
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| CN110494932A (en) * | 2017-04-05 | 2019-11-22 | Abb瑞士股份有限公司 | Insulating materials for DC electric component |
| CN110494932B (en) * | 2017-04-05 | 2021-06-18 | Abb电网瑞士股份公司 | Insulating material for DC electrical components |
| US11342095B2 (en) | 2017-04-05 | 2022-05-24 | Hitachi Energy Switzerland Ag | Insulation material for a DC electrical component |
| CN107043535A (en) * | 2017-04-25 | 2017-08-15 | 晶锋集团股份有限公司 | A kind of bismuth, manganese, cobalt, zinc oxide polyimide composite film of niobium doping and preparation method thereof |
| CN107123463A (en) * | 2017-04-25 | 2017-09-01 | 晶锋集团股份有限公司 | A kind of zinc oxide composite insulating material that can adaptively regulate and control conductance and dielectric and preparation method thereof |
| CN107123463B (en) * | 2017-04-25 | 2019-02-05 | 晶锋集团股份有限公司 | A kind of zinc oxide composite insulating material and preparation method thereof that can adaptively regulate and control conductance and dielectric |
| CN111334041A (en) * | 2020-03-26 | 2020-06-26 | 中国科学院兰州化学物理研究所 | Polyimide lubricating material filled with nano titanium nitride and preparation method thereof |
| CN111334041B (en) * | 2020-03-26 | 2021-07-23 | 中国科学院兰州化学物理研究所 | Polyimide lubricating material filled with nano titanium nitride and preparation method thereof |
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Effective date of registration: 20160413 Address after: 225800 Jiangsu County of Baoying Province Wang Zhi Hong Kong industrial zone. Patentee after: Jiangsu Adin New Materials Co., Ltd. Address before: 710049 Xianning Road, Shaanxi, China, No. 28, No. Patentee before: Xi'an Jiaotong University |