CN108046789A - A kind of preparation method of electromagnetic shielding composite material - Google Patents
A kind of preparation method of electromagnetic shielding composite material Download PDFInfo
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- CN108046789A CN108046789A CN201711332841.2A CN201711332841A CN108046789A CN 108046789 A CN108046789 A CN 108046789A CN 201711332841 A CN201711332841 A CN 201711332841A CN 108046789 A CN108046789 A CN 108046789A
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Abstract
The invention discloses a kind of preparation methods of electromagnetic shielding composite material, belong to the technical field for preparing shielding material, implement in accordance with the following steps:Dispensing, ball milling, pouring molding and sintering.The preparation method of electromagnetic shielding composite material disclosed by the invention, process conditions are simple and easy to control, production cost is low, and the electromagnetic shielding composite material produced not only has good effectiveness, also with high mechanical strength, good toughness, heat safe performance.
Description
Technical field
The present invention relates to the technical field for preparing shielding material, more particularly to a kind of preparation side of electromagnetic shielding composite material
Method
Background technology
With the rapid development of electronic technology, electromagnetic interference, the problems such as electromagnetic environmental pollution, also becomes increasingly severe.Electricity
Magnetic radiation can cause electromagnetic interference to various electronic equipments, and then cause data transmission fault, while user is set using electronics
It is standby, easily by electromagnetic radiation, and then influence health.Therefore, using which kind of electromagnetic shielding material solving electromagnetism
The problem of radiation, has received widespread attention.At present, traditional electromagnetic shielding material, universal production cost is high, than great, perishable
Erosion, poor processability and cumbersome, exist simultaneously the limitations such as lack of homogeneity.
The content of the invention
The defects of in order to overcome the prior art, the technical problems to be solved by the invention are to propose that a kind of electromagnetic shielding is multiple
The preparation method of condensation material, the process conditions of the preparation method are simple and easy to control, production cost is low, and the electromagnetic shielding produced is compound
Material not only has good effectiveness, also with high mechanical strength, good toughness, heat safe performance.
For this purpose, the present invention uses following technical scheme:
The present invention provides a kind of preparation methods of electromagnetic shielding composite material, implement in accordance with the following steps:
Anisotropy strontium ferrum magnetic powder that mass fraction is 100~150 parts, mass fraction are 10~15 parts by S1 dispensings
High-temp glue and the electromagnetic shielding auxiliary agent that mass fraction is 10~40 parts are added in the deionized water of 500~1000ml, and in
Ultrasonic disperse is carried out under 70~100Hz frequencies, obtains metal suspension;After the metal suspension is warming up to 30~40 DEG C,
The binding agent that mass fraction is 1~8 part is added in thereto, and constant temperature stirs 30~90min, obtains ingredients mixture;
The ingredients mixture is transferred in ball mill and carries out ball milling by S2 ball millings, adds in scattered help by several times in grinding
Agent obtains ball milling slurry;
The ball milling slurry is cast in mold, and is put into vacuum tank by S3 cast moldings, is taken out using 50~70 DEG C true
After 30~60min of sky, drying process simultaneously moves into hot press progress hot-press solidifying shaping, obtains cast molding sample;
S4 is sintered, and the cast molding sample is put into vacuum drying oven and is sintered, the sintering is as follows:
1) after sintering temperature is first warming up to 300~400 DEG C with the heating rate of 8~10 DEG C/min, when constant temperature 1~3 is small;
2) after being warming up to 600~800 DEG C with the heating rate of 3~5 DEG C/min, when constant temperature 1~2 is small;
3) after being warming up to 1400~1450 DEG C with the heating rate of 6~8 DEG C/min, when constant temperature is small not less than 1;
4) electromagnetic screen is made in cooled to room temperature after cooling to 200~300 DEG C with the rate of temperature fall of 3~5 DEG C/min
Cover composite material;
The high-temp glue is nano inorganic ceramic material and modified isocyanurate curing agent.
In preferably technical solution of the invention, the nano inorganic ceramic material cures with the modified isocyanuric acid ester
Agent mass ratio is 8~20:1.
In preferably technical solution of the invention, when a length of 15~120min of ultrasonic disperse in S1 steps.
In preferably technical solution of the invention, the anisotropy strontium ferrum magnetic powder is broken before deionized water is added in
Broken, sieving processing, the anisotropy strontium ferrum magnetic powder mean particle size range that treated are 1.5~2.5 μm.
In preferably technical solution of the invention, the dispersant is methanol, ethyl alcohol, acetone, two n-butanols, cyclohexanone
Any one of or several combinations;
3~5 additions of the dispersant point;
The volume ratio that the dispersant accounts for the ingredients mixture is 20%~50%.
In preferably technical solution of the invention, in the S3 steps, hot pressing temperature is 125~250 DEG C, pressure for 5~
15MPa, hot pressing time are 15~25min.
In preferably technical solution of the invention, using rotating speed as 30~50r/min in S2 mechanical milling processes, Ball-milling Time 2
~4h;It needs that operation is exhausted in mechanical milling process, the bleeding frequency is 1~3 time/h.
In preferably technical solution of the invention, the binding agent is nylon resin.
In preferably technical solution of the invention, the temperature of drying process is 100~120 DEG C in S3 steps, dry duration
For 1~3 it is small when.
In preferably technical solution of the invention, the mean particle size range of the electromagnetic shielding auxiliary agent is 2~3 μm.
In preferably technical solution of the invention, the electromagnetic shielding auxiliary agent is graphene, nanometer ferrite base, zinc oxide
Any one of whisker, nanometer silicon carbide, nano metal nickel powder or several combinations.
Beneficial effects of the present invention are:
The preparation method of electromagnetic shielding composite material provided by the invention, first by anisotropy strontium ferrum magnetic powder, high-temp glue
And electromagnetic shielding auxiliary agent is added in deionized water and carries out ultrasonic disperse, is allowed to uniformly mix, while the electromagnetic shielding added in
Auxiliary agent has good effectiveness, and the ceramic material containing nano inorganic added in and modified isocyanurate curing agent are high
Warm glue makes composite material machinery intensity height, good toughness.Then pouring molding will be carried out after ingredients mixture ball milling obtained, and then
Structure is promoted more to stablize.It is sintered finally by segmented, further improves the electromagnetic shielding of composite material and heat safe
Performance.
The preparation method of electromagnetic shielding composite material provided by the invention, after testing prepared electromagnetic shielding composite material
Granule size is uniform, and optimal to can reach 1.4~1.6 μm, density is no more than 1.85g/cm3, the porosity is up to 25%, bending resistance
Intensity is 5.63MPa, and compression strength is not less than 8MPa.This method preparation is measured in the frequency range of 500MHz~1.5GHz
The electromagnet shield effect of composite material is more than 65dB.
Specific embodiment
Technical solution to further illustrate the present invention With reference to embodiment.It is it should be noted that right
It is used to help understand the present invention in the explanation of these embodiments, but does not form limitation of the invention.In addition, it is retouched below
Involved technical characteristic can be combined with each other as long as they do not conflict with each other in each embodiment of the present invention stated.
Embodiment one, the present invention provide a kind of preparation method of electromagnetic shielding composite material, implement in accordance with the following steps:
S1 dispensings:The anisotropy strontium ferrum magnetic powder that mass fraction is 100 parts is first crushed, sieving processing, put down
Equal particle size range is 1.5~2.5 μm of anisotropy strontium ferrum magnetic powder, then with the high-temp glue (height that mass fraction is 10 parts
Warm glue is nano inorganic ceramic material and modified isocyanurate curing agent, and the nano inorganic ceramic material and the modification are different
Cyanurate curing agent mass ratio is 8:1, wherein nano inorganic ceramic material and modified isocyanurate curing agent are market
Purchase.) and electromagnetic shielding auxiliary agent that mass fraction is 10 parts (electromagnetic shielding auxiliary agent is graphene and nano metal nickel powder, than
Weight is 4:1, and the mean particle size range bought is 2~3 μm) be added in the deionized water of 800ml, and under 100Hz frequencies
Ultrasonic disperse 30min is carried out, obtains metal suspension;After metal suspension is warming up to 30 DEG C, mass fraction is added in thereto
For 5 parts of nylon resin, constant temperature stirring 60min obtains ingredients mixture;
Ingredients mixture is transferred in ball mill and carries out ball milling 2h by 35r/min of rotating speed by S2 ball millings, and in grinding
Cyclohexanone is added three times, obtains ball milling slurry, while generated in mechanical milling process with the bleeding frequency discharge of 1~3 time/h
Excessive gas;
Ball milling slurry is cast in mold, and is put into vacuum tank by S3 cast moldings, and 60min is vacuumized using 65 DEG C
Afterwards, with 120 DEG C of drying process 1 it is small when after, move into hot press and be 150 DEG C, pressure 10MPa with hot pressing temperature, during hot pressing
Between for 20min carry out hot-press solidifying shaping, obtain cast molding sample;
S4 is sintered, and cast molding sample is put into vacuum drying oven, initial temperature is room temperature, with the heating rate of 8 DEG C/min
After being warming up to 380 DEG C, when constant temperature 1.5 is small, then after being warming up to 600 DEG C with the heating rate of 3 DEG C/min, when constant temperature 1.5 is small, then
After being warming up to 1400 DEG C with the heating rate of 6 DEG C/min, when constant temperature 2 is small, finally 220 are cooled to the rate of temperature fall of 3 DEG C/min
Electromagnetic shielding composite material is made in cooled to room temperature after DEG C.
Embodiment two, the present invention provide a kind of preparation method of electromagnetic shielding composite material, implement in accordance with the following steps:
S1 dispensings:The anisotropy strontium ferrum magnetic powder that mass fraction is 150 parts is first crushed, sieving processing, put down
Equal particle size range is 1.5~2.5 μm of anisotropy strontium ferrum magnetic powder, then with the high-temp glue (height that mass fraction is 12 parts
Warm glue is nano inorganic ceramic material and modified isocyanurate curing agent, and the nano inorganic ceramic material and the modification are different
Cyanurate curing agent mass ratio is 15:1, wherein nano inorganic ceramic material and modified isocyanurate curing agent are market
Purchase.) and nanometer ferrite base (mean particle size range of purchase is 2~3 μm) that mass fraction is 20 parts be added to
In the deionized water of 1000ml, and ultrasonic disperse 30min is carried out under 100Hz frequencies, obtain metal suspension;Metal is suspended
After liquid is warming up to 35 DEG C, the nylon resin that mass fraction is 4 parts is added in thereto, and constant temperature stirring 60min obtains dispensing mixing
Object;
Ingredients mixture is transferred in ball mill and carries out ball milling 2h by 35r/min of rotating speed by S2 ball millings, and in grinding
Add in acetone and cyclohexanone points for 5 times, and acetone and cyclohexanone account for the volume ratio of ingredients mixture as 50%, obtain ball milling slurry,
The excessive gas generated simultaneously in mechanical milling process with the bleeding frequency discharge of 1~3 time/h;
Ball milling slurry is cast in mold, and is put into vacuum tank by S3 cast moldings, and 60min is vacuumized using 65 DEG C
Afterwards, with 100 DEG C of drying process 1 it is small when after, move into hot press and be 125 DEG C, pressure 10MPa with hot pressing temperature, during hot pressing
Between for 20min carry out hot-press solidifying shaping, obtain cast molding sample;
S4 is sintered, and cast molding sample is put into vacuum drying oven, initial temperature is room temperature, with the heating rate of 8 DEG C/min
After being warming up to 400 DEG C, when constant temperature 1.5 is small, then after being warming up to 700 DEG C with the heating rate of 4 DEG C/min, when constant temperature 1.5 is small, then
After being warming up to 1400 DEG C with the heating rate of 8 DEG C/min, when constant temperature 2 is small, finally 220 are cooled to the rate of temperature fall of 5 DEG C/min
Electromagnetic shielding composite material is made in cooled to room temperature after DEG C.
Embodiment three, the present invention provide a kind of preparation method of electromagnetic shielding composite material, implement in accordance with the following steps:
S1 dispensings:The anisotropy strontium ferrum magnetic powder that mass fraction is 100 parts is first crushed, sieving processing, put down
Equal particle size range is 1.5~2.5 μm of anisotropy strontium ferrum magnetic powder, then with the high-temp glue (height that mass fraction is 15 parts
Warm glue is nano inorganic ceramic material and modified isocyanurate curing agent, and the nano inorganic ceramic material and the modification are different
Cyanurate curing agent mass ratio is 20:1, wherein nano inorganic ceramic material and modified isocyanurate curing agent are market
Purchase.) and electromagnetic shielding auxiliary agent that mass fraction is 10 parts (electromagnetic shielding auxiliary agent be ZnOw, nanometer silicon carbide and
Nano metal nickel powder, proportion 2:1:1, and the mean particle size range bought is 2~3 μm) it is added to the deionized water of 1000ml
In, and ultrasonic disperse 30min is carried out under 100Hz frequencies, obtain metal suspension;After metal suspension is warming up to 30 DEG C,
The binding agent that mass fraction is 5 parts is added in thereto, and constant temperature stirring 60min obtains ingredients mixture;
Ingredients mixture is transferred in ball mill and carries out ball milling 2h by 45r/min of rotating speed by S2 ball millings, and in grinding
Divide 5 times and add in methanol and two n-butanols, obtain ball milling slurry, while arranged in mechanical milling process with the bleeding frequency of 1~3 time/h
Go out the excessive gas of generation;
Ball milling slurry is cast in mold, and is put into vacuum tank by S3 cast moldings, and 60min is vacuumized using 65 DEG C
Afterwards, with 120 DEG C of drying process 1 it is small when after, move into hot press and be 150 DEG C, pressure 10MPa with hot pressing temperature, during hot pressing
Between for 20min carry out hot-press solidifying shaping, obtain cast molding sample;
S4 is sintered, and cast molding sample is put into vacuum drying oven, initial temperature is room temperature, with the heating rate of 8 DEG C/min
After being warming up to 380 DEG C, when constant temperature 1.5 is small, then after being warming up to 600 DEG C with the heating rate of 3 DEG C/min, when constant temperature 1.5 is small, then
After being warming up to 1400 DEG C with the heating rate of 6 DEG C/min, when constant temperature 2 is small, finally 220 are cooled to the rate of temperature fall of 3 DEG C/min
Electromagnetic shielding composite material is made in cooled to room temperature after DEG C.
Comparative example:Mass fraction is directly taken to be placed in for 100 parts of anisotropy strontium ferrum magnetic powder and deionized water in ball mill
Ball milling 4h is carried out, subsequent pouring molding and sintering step are identical with embodiment one.
Respectively the powder after Example one to three and comparative example ball milling or slurry its granularity is tested and
Electromagnetic shielding composite material made from Example one to three and comparative example is tested for the property respectively, and test event includes
Granularity, density, bending strength and the shield effectiveness of these materials.It should be noted that density is weighing the matter of composite material
Amount, bending strength bend not broken energy to weigh to resist, and shield effectiveness is weighing the effect of shielding or electromagnetism of decaying.
Specific test result such as following table:
Note:The test method of particle size range in upper table after ball milling is tested using GB/T 19077.1-2008, density
Test method tested using GB/T 1423-1996, adopted in 500MHz~1.5GHz frequency inner shield effect test methods
It is tested with GB/T 12190-2006.
The present invention is described with reference to the preferred embodiments, and those skilled in the art know, is not departing from the present invention's
In the case of spirit and scope, various changes or equivalence replacement can be carried out to these features and embodiment.The present invention is from this
The limitation of specific embodiment disclosed in place, other embodiments fallen into claims hereof belong to protection of the present invention
Scope.
Claims (10)
1. a kind of preparation of electromagnetic shielding composite material, which is characterized in that implement in accordance with the following steps:
S1 dispensings, by anisotropy strontium ferrum magnetic powder that mass fraction is 100~150 parts, the high temperature that mass fraction is 10~15 parts
Glue and mass fraction are that 10~40 parts of electromagnetic shielding auxiliary agent is added in the deionized water of 500~1000ml, and in 70~
Ultrasonic disperse is carried out under 100Hz frequencies, obtains metal suspension;After the metal suspension is warming up to 30~40 DEG C, Xiang Qi
Middle to add in the binding agent that mass fraction is 1~8 part, constant temperature stirs 30~90min, obtains ingredients mixture;
The ingredients mixture is transferred in ball mill and carries out ball milling by S2 ball millings, adds in dispersing aid by several times in grinding, obtains
To ball milling slurry;
The ball milling slurry is cast in mold, and is put into vacuum tank by S3 cast moldings, and 30 are vacuumized using 50~70 DEG C
After~60min, drying process simultaneously moves into hot press progress hot-press solidifying shaping, obtains cast molding sample;
S4 is sintered, and the cast molding sample is put into vacuum drying oven and is sintered, the sintering is as follows:
1) after sintering temperature is first warming up to 300~400 DEG C with the heating rate of 8~10 DEG C/min, when constant temperature 1~3 is small;
2) after being warming up to 600~800 DEG C with the heating rate of 3~5 DEG C/min, when constant temperature 1~2 is small;
3) after being warming up to 1400~1450 DEG C with the heating rate of 6~8 DEG C/min, when constant temperature is small not less than 1;
4) it is multiple that electromagnetic shielding is made in cooled to room temperature after cooling to 200~300 DEG C with the rate of temperature fall of 3~5 DEG C/min
Condensation material;
The high-temp glue is nano inorganic ceramic material and modified isocyanurate curing agent.
2. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The nano inorganic ceramic material is 8~20 with the modified isocyanurate curing agent mass ratio:1.
3. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
When a length of 15~120min of ultrasonic disperse in S1 steps.
4. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The anisotropy strontium ferrum magnetic powder is crushed before deionized water is added in, sieving processing, and it is described respectively to different that treated
Property strontium ferrum magnetic powder mean particle size range be 1.5~2.5 μm.
5. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The dispersant is any one of methanol, ethyl alcohol, acetone, two n-butanols, cyclohexanone or several combinations;
3~5 additions of the dispersant point;
The volume ratio that the dispersant accounts for the ingredients mixture is 20%~50%.
6. the preparation of electromagnetic shielding composite material according to claim 4, it is characterised in that:
In the S3 steps, hot pressing temperature is 125~250 DEG C, and pressure is 5~15MPa, and hot pressing time is 15~25min.
7. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
Using rotating speed as 30~50r/min in S2 mechanical milling processes, Ball-milling Time is 2~4h;
It needs that operation is exhausted in mechanical milling process, the bleeding frequency is 1~3 time/h.
8. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The binding agent is nylon resin.
9. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The temperature of drying process is 100~120 DEG C in S3 steps, when dry it is a length of 1~3 it is small when.
10. the preparation of electromagnetic shielding composite material according to claim 1, it is characterised in that:
The electromagnetic shielding auxiliary agent is graphene, nanometer ferrite base, ZnOw, nanometer silicon carbide, nano metal nickel powder
Any one of or several combinations.
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CN201711332841.2A CN108046789B (en) | 2017-12-13 | 2017-12-13 | Preparation method of electromagnetic shielding composite material |
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CN108046789B CN108046789B (en) | 2020-10-02 |
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Cited By (7)
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CN108585908A (en) * | 2018-06-12 | 2018-09-28 | 佛山市华强协兴陶瓷有限公司 | A kind of preparation method of the high tenacity without electromagnetic shielding ceramic composite |
CN109879635A (en) * | 2019-04-15 | 2019-06-14 | 苏州安洁新材料有限公司 | A kind of ultra-thin high magnetic permeability inhales wave plate and its casting slurry and preparation method |
CN110494030A (en) * | 2019-08-28 | 2019-11-22 | 合肥工业大学 | A kind of preparation method for the ferrite solid waste sound stage width band electromagnetic wave absorber that resin is strengthened |
CN110835269A (en) * | 2019-10-30 | 2020-02-25 | 安徽朗基新材料科技有限公司 | Production process of high-strength high-performance soft magnetic ferrite material |
CN111592743A (en) * | 2020-06-29 | 2020-08-28 | 江西伟普科技有限公司 | Electromagnetic shielding composite material and preparation method thereof |
CN111621139A (en) * | 2020-06-29 | 2020-09-04 | 江西伟普科技有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
CN113488330A (en) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | Preparation method of functional magnetic slurry and magnetic device |
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CN108585908A (en) * | 2018-06-12 | 2018-09-28 | 佛山市华强协兴陶瓷有限公司 | A kind of preparation method of the high tenacity without electromagnetic shielding ceramic composite |
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CN110835269A (en) * | 2019-10-30 | 2020-02-25 | 安徽朗基新材料科技有限公司 | Production process of high-strength high-performance soft magnetic ferrite material |
CN111592743A (en) * | 2020-06-29 | 2020-08-28 | 江西伟普科技有限公司 | Electromagnetic shielding composite material and preparation method thereof |
CN111621139A (en) * | 2020-06-29 | 2020-09-04 | 江西伟普科技有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
CN111621139B (en) * | 2020-06-29 | 2022-04-08 | 江西伟普科技有限公司 | Wave-absorbing heat-conducting flexible composite material and preparation method thereof |
CN113488330A (en) * | 2021-07-15 | 2021-10-08 | 无锡蓝沛新材料科技股份有限公司 | Preparation method of functional magnetic slurry and magnetic device |
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