CN107686344A - A kind of absorbing material of adjustable frequency and preparation method thereof - Google Patents
A kind of absorbing material of adjustable frequency and preparation method thereof Download PDFInfo
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- CN107686344A CN107686344A CN201710546674.5A CN201710546674A CN107686344A CN 107686344 A CN107686344 A CN 107686344A CN 201710546674 A CN201710546674 A CN 201710546674A CN 107686344 A CN107686344 A CN 107686344A
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- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses a kind of absorbing material of adjustable frequency and preparation method thereof, for the absorbing material using barium carbonate, iron oxide as major ingredient, cobalt oxide, titanium oxide, zirconium oxide are that ion doping regulates and controls auxiliary material, are prepared through ball milling, sintering；The chemical formula of the absorbing material is BaFe12‑2x(CoTi0.5Zr0.5)xO19, wherein x span is 0.3 1.2.Preparation method comprises the following steps：Feed proportioning, ball milling, pre-sintering, secondary ball milling, a sinter molding.The present invention regulates and controls the suction wave frequency rate of absorbing material, the electromagnetic protection for the electronic product equipment of different frequency in life by changing the ion concentration of material.
Description
Technical field
The present invention relates to a kind of absorbing material technology, more particularly to a kind of absorbing material of adjustable frequency and its preparation side
Method.
Background technology
As science and technology, industrial development and the progress of defense needs, increasing electromagnetic wave are present in our week
Enclose, various electromagnetic radiation have been gradually filled with people's life, from each class of electronic devices such as radio broadcasting, TV or even computer
Widely use, while bringing convenient and efficient for our work and life, we are also just getting in invisible electromagnetic radiation
To be full of more in our living space.The electromagnetism density increasingly strengthened, while in change, we live, also change
Electromagnetic environment around us, nowadays existing people, which describes, lives in people in city, seemingly place oneself in the midst of in " big micro-wave oven ", bear
The impact of various electromagnetic radiation.Effect of the electromagnetic radiation to people mainly has three kinds, i.e. " fuel factor ", " non-thermal effect ", " cause
Cancer, mutagenesis, teratogenesis ", except the first fuel factor can occur in the case where being acted on compared with intense radiation, latter two is all in weaker electricity
Cumulative effect under the long term of magnetic radiation produces harmful influence to human body, and electromagnetic radiance density is less than 1mW/cm2
When, though irradiation will not cause body temperature significantly to raise for a long time, scientist has revealed that：Multi-frequency height is different
Electromagnetic Field can cause a large amount of losses of institute's calcium ions in human body cell when human body, and the missing pair of this calcium ion
Nerve be effectively conducted, the influence of cardiovascular function it is of crucial importance；Electromagnetic wave can also cause substance in vivo to produce covibration, shadow
The motion of substance in vivo ion is rung, so as to be formed so-called " non-thermal effect ".Eventually make one irritated, dizzy, fatigue occur, lose
The symptom such as change of dormancy, failure of memory, alopecia, vegetative nervous disorder and electroencephalogram, electrocardiogram.In terms of remote effect, for a long time
Electromagnetic radiation may induce cancer, it is also possible to cause the distortion of chromosome, there is carcinogenic mutagenesis.Therefore, building
The frequent use of each electron-like, electric product and wireless telecommunications system in space, does not produce electromagnetic radiation all the time, and electromagnetism is dirty
Dye has caused people widely to pay close attention to.So-called absorbing material, i.e., when electromagnetic wave passes through material, electromagnetic energy is absorbed, so as to
Make the energy expenditure of incident electromagnetic wave, electromagnetic energy is actually converted into heat energy and lost.It is all that electromagnetic wave can be made to pass through it
Surface, and there is the material of high loss characteristics to the energy of electromagnetic wave, absorbing material is used such as in building space, is can absorb
Existing electromagnetic radiation in space, effectively mitigates radiation intensity, fundamentally improves influence of the harmful radiation to human body.
The content of the invention
For overcome the deficiencies in the prior art, an object of the present invention is the suction ripple material for providing a kind of adjustable frequency
Material.Ion concentration by changing material regulates and controls the suction wave frequency rate of absorbing material, the electronic product for different frequency in life
The electromagnetic protection of equipment.
The second object of the present invention is to provide a kind of preparation method of the absorbing material of adjustable frequency.
An object of the present invention adopts the following technical scheme that realization：A kind of absorbing material of adjustable frequency, the suction ripple material
For material using barium carbonate, iron oxide as major ingredient, cobalt oxide, titanium oxide, zirconium oxide are that ion doping regulates and controls auxiliary material, are made through ball milling, sintering
It is standby to form；The chemical formula of the absorbing material is BaFe12-2x(CoTi0.5Zr0.5)xO19, wherein x span is 0.3-1.2.
The second object of the present invention adopts the following technical scheme that realization：A kind of preparation side of the absorbing material of adjustable frequency
Method, including：
Feed proportioning step：According to the absorbing material component dispensing of following molal weight percentage：10-18mol% carbon
Sour barium, 57-85mol% iron oxide, 0-5mol% cobalt oxide, 0-5mol% titanium oxide and 0-5mol% zirconium oxide；
Said components molal weight percentage sum is 100%；
Ball milling step：After dispensing is complete, adds deionized water and ball milling iron ball carries out a ball milling, Ball-milling Time is
12-18 hours, rotational speed of ball-mill 220-250r/min, after ball milling terminates, abrasive material is taken out, is dried in 80-120 DEG C of baking oven；
Pre-sintering step：After drying, 60 mesh sub-sieves are crossed, is put into sintering furnace and is sintered, then with stove Temperature fall
To room temperature, barium ferrite pre-sintered powder is obtained；
Secondary ball milling step：Barium ferrite pre-sintered powder is added into deionized water and ball milling iron ball carries out secondary ball milling, ball
Consume time 10-12h, rotational speed of ball-mill 250r/min；
Sinter molding step：Secondary ball abrasive material is taken out and dried, adhesive granulating and forming is added and is pressed into blank, then
Blank is put into sintering furnace, 4-6h is sintered at a temperature of 1150-1280 DEG C, being cooled to room temperature with stove obtains the Frequency Adjustable
The absorbing material of rate.
Further, in the step of feed proportioning, all absorbing material components are that chemical analysis is pure.
Further, in the step of ball milling, the quality summation of absorbing material, deionized water, the weight of ball milling iron ball
Amount is than being 1：(1.2-1.4)：4.
Further, in the step of pre-sintering, after being put into sintering furnace, with 2 DEG C/min heating rate by room temperature liter
Temperature is to 1000-1100 DEG C and is incubated 2-6h.
Further, in the step of secondary ball milling, barium ferrite pre-sintered powder, deionized water, the weight of ball milling iron ball
Than for 1:1:3.5.
Further, in the step of sinter molding, described adhesive is polyvinyl alcohol, vinyl acetate, acrylic acid etc.
In one kind；The addition of described adhesive is the 5-20% of secondary ball abrasive material gross weight.
Further, in the step of sinter molding, described to be pressed into pressure in the process of blank be 8-10Mpa.
Further, in the step of first and second ball milling, the ball milling iron ball includes a diameter of 1mm bead and diameter
For 3mm big ball, the quantitative proportion of bead and big ball is 3:1, ball milling direction is per hour alternately once during ball milling.
Compared with prior art, the beneficial effects of the present invention are：
The absorbing material of adjustable frequency as made from preparation method of the present invention, have and inhale that wave frequency bandwidth, function be strong, adjustable model
The features such as enclosing width, and ferrite ceramic material is used as, wave-absorbing and camouflage function, the complicated portion of and can forming shape can be played
Part, certain carrying effect is played, this material is also the critical material that China's national defense modernization is badly in need of, to the military thunder in China
In terms of stealth technology, there is good impetus, be of great significance for the military capability of the country tool for improving China.
Brief description of the drawings
Fig. 1 is absorbing material preparation technology flow chart prepared by the present invention；
Fig. 2 is the reflectance test result figure of absorbing material prepared by embodiment 1；
Fig. 3 is the reflectance test result figure of absorbing material prepared by embodiment 2；
Fig. 4 is the reflectance test result figure of absorbing material prepared by embodiment 3.
Embodiment
Below, with reference to accompanying drawing and embodiment, the present invention is described further, it is necessary to which explanation is, not
Under the premise of afoul, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
In the present invention, if not refering in particular to, all parts, percentage are unit of weight, used equipment and raw material etc.
It is commercially available or commonly used in the art.Method in following embodiments, it is the normal of this area unless otherwise instructed
Rule method.
The present invention provides a kind of absorbing material of adjustable frequency, and the absorbing material is using barium carbonate, iron oxide as major ingredient, oxidation
Cobalt, titanium oxide, zirconium oxide are that ion doping regulates and controls auxiliary material, are prepared through ball milling, sintering；The chemical formula of the absorbing material is
BaFe12-2x(CoTi0.5Zr0.5)xO19, wherein x span is 0.3-1.2.
The present invention also provides a kind of preparation method of the absorbing material of adjustable frequency, including：
Feed proportioning step：According to the absorbing material component dispensing of following molal weight percentage：10-18mol% carbon
Sour barium, 57-85mol% iron oxide, 0-5mol% cobalt oxide, 0-5mol% titanium oxide and 0-5mol% zirconium oxide；
Said components molal weight percentage sum is 100%；
Ball milling step：After dispensing is complete, adds deionized water and ball milling iron ball carries out a ball milling, Ball-milling Time is
12-18 hours, rotational speed of ball-mill 220-250r/min, after ball milling terminates, abrasive material is taken out, is dried in 80-120 DEG C of baking oven；
Pre-sintering step：After drying, 60 mesh sub-sieves are crossed, is put into sintering furnace and is sintered, then with stove Temperature fall
To room temperature, barium ferrite pre-sintered powder is obtained；
Secondary ball milling step：Barium ferrite pre-sintered powder is added into deionized water and ball milling iron ball carries out secondary ball milling, ball
Consume time 10-12h, rotational speed of ball-mill 250r/min；
Sinter molding step：Secondary ball abrasive material is taken out and dried, adhesive granulating and forming is added and is pressed into blank, then
Blank is put into sintering furnace, 4-6h is sintered at a temperature of 1150-1280 DEG C, being cooled to room temperature with stove obtains the Frequency Adjustable
The absorbing material of rate.
As the preferred scheme of the present invention, in the step of feed proportioning, all absorbing material components are chemistry point
Analyse pure.
As the preferred scheme of the present invention, in the step of ball milling, the quality summation of absorbing material, deionized water,
The weight ratio of ball milling iron ball is 1：(1.2-1.4)：4.
As the preferred scheme of the present invention, in the step of pre-sintering, after being put into sintering furnace, with 2 DEG C/min heating
Speed to 1000-1100 DEG C and is incubated 2-6h by room temperature.
As the preferred scheme of the present invention, in the step of secondary ball milling, barium ferrite pre-sintered powder, deionized water, ball
The weight ratio for grinding iron ball is 1:1:3.5.
As the preferred scheme of the present invention, in the step of sinter molding, described adhesive is polyvinyl alcohol, vinyl acetate
One kind in ester, acrylic acid etc.；The addition of described adhesive is the 5-20% of secondary ball abrasive material gross weight.
It is described to be pressed into pressure in the process of blank and be in the step of sinter molding as the preferred scheme of the present invention
8-10Mpa。
As the preferred scheme of the present invention, in the step of first and second ball milling, the ball milling iron ball includes a diameter of 1mm
Bead and a diameter of 3mm big ball, the quantitative proportion of bead and big ball is 3:1, ball milling direction replaces per hour during ball milling
Once.
Embodiment 1
The absorbing material of adjustable frequency, is prepared by following steps：
(1) according to x=0.3, BaFe11.4Co0.3(Ti0.15Zr0.15)O19Stoichiometric proportion, weighing 7.69mol% barium carbonates,
87.69mol% iron oxide, 2.32mol% cobalt oxides, 1.15mol% titanium oxide and 1.15mol% zirconium oxides；
(2) mill is made with deionized water to be situated between；With absorbing material powder gross mass：Deionized water：Ball milling iron ball=1：1.2：4
Ratio carries out a ball milling, and mixing and ball milling is carried out in planetary ball mill, wherein, 220 revs/min of drum's speed of rotation, every 1 is small
When alternating direction once, 18 hours altogether, be well mixed；Powder after ball milling is dried, keeps air dry oven temperature
For 90 DEG C, moisture is evaporated, obtains dry powder.
(3) pre-sintering is carried out to the powder in step (2) using high temperature sintering furnace, crosses 60 mesh sub-sieves, be put into sintering furnace
It is interior, 4h to 1100 DEG C and is incubated by room temperature with 2 DEG C/min heating rate, then room temperature is naturally cooling to stove, obtains
Barium ferrite pre-sintered powder.
(4) powder after sintering is added and carries out secondary ball milling, barium ferrite pre-sintered powder gross mass：Deionized water：Ball
The weight ratio for grinding iron ball is 1：1：3.5, Ball-milling Time 12 hours, 220 revs/min of drum's speed of rotation, alternating direction one per hour
It is secondary；After ball milling, the powder after ball milling is dried using the drying means of step (2).
(5) add adhesive polyethylene alcohol (PVA) granulating and forming and blank is pressed under 8-10MPa, then blank is put
Enter in sintering furnace, ceramic powder is sintered using high temperature sintering furnace, 1200 DEG C of sintering temperature, be incubated 6 hours, obtain inhaling ripple
Material.
As shown in Fig. 2 the reflectivity for the absorbing material that embodiment 1 is prepared is shown, the centre frequency of absorbing material exists
4.45GHz。
Embodiment 2
The absorbing material of adjustable frequency, is prepared by following steps：
(1) according to x=0.6, BaFe10.8Co0.3(Ti0.15Zr0.15)O19Stoichiometric proportion, weighing 7.69mol% barium carbonates,
83.08mol% iron oxide, 4.61mol% cobalt oxides, 2.31mol% titanium oxide and 2.31mol% zirconium oxides；
(2) mill is made with deionized water to be situated between；With absorbing material powder gross mass：Deionized water：Ball milling iron ball=1：1.3：4
Ratio carries out a ball milling, and mixing and ball milling is carried out in planetary ball mill, wherein, 220 revs/min of drum's speed of rotation, every 1 is small
When alternating direction once, 18 hours altogether, be well mixed；Powder after ball milling is dried, keeps air dry oven temperature
For 90 DEG C, moisture is evaporated, obtains dry powder.
(3) pre-sintering is carried out to the powder in step (2) using high temperature sintering furnace, crosses 60 mesh sub-sieves, be put into sintering furnace
It is interior, 4h to 1100 DEG C and is incubated by room temperature with 2 DEG C/min heating rate, then room temperature is naturally cooling to stove, obtains
Barium ferrite pre-sintered powder.
(4) powder after sintering is added and carries out secondary ball milling, barium ferrite pre-sintered powder gross mass：Deionized water：Ball
The weight ratio for grinding iron ball is 1：1：3.5, Ball-milling Time 12 hours, 220 revs/min of drum's speed of rotation, alternating direction one per hour
It is secondary；After ball milling, the powder after ball milling is dried using the drying means of step (2).
(5) add adhesive polyethylene alcohol (PVA) granulating and forming and blank is pressed under 8-10MPa, then blank is put
Enter in sintering furnace, ceramic powder is sintered using high temperature sintering furnace, 1200 DEG C of sintering temperature, be incubated 6 hours, obtain inhaling ripple
Material.
As shown in figure 3, the reflectivity for the absorbing material that embodiment 2 is prepared is shown, the centre frequency of absorbing material exists
6.00GHz。
Embodiment 3
The absorbing material of adjustable frequency, is prepared by following steps：
(1) according to x=1.2, BaFe9.6Co1.2(Ti0.6Zr0.6)O19Stoichiometric proportion, weighing 7.69mol% barium carbonates,
73.84mol% iron oxide, 9.23mol% cobalt oxides, 4.62mol% titanium oxide and 4.62mol% zirconium oxides；
(2) mill is made with deionized water to be situated between；With absorbing material powder gross mass：Deionized water：Ball milling iron ball=1：1.4：4
Ratio carries out a ball milling, and mixing and ball milling is carried out in planetary ball mill, wherein, 220 revs/min of drum's speed of rotation, every 1 is small
When alternating direction once, 18 hours altogether, be well mixed；Powder after ball milling is dried, keeps air dry oven temperature
For 90 DEG C, moisture is evaporated, obtains dry powder.
(3) pre-sintering is carried out to the powder in step (2) using high temperature sintering furnace, crosses 60 mesh sub-sieves, be put into sintering furnace
It is interior, 4h to 1100 DEG C and is incubated by room temperature with 2 DEG C/min heating rate, then room temperature is naturally cooling to stove, obtains
Barium ferrite pre-sintered powder.
(4) powder after sintering is added and carries out secondary ball milling, barium ferrite pre-sintered powder gross mass：Deionized water：Ball
The weight ratio for grinding iron ball is 1：1：3.5, Ball-milling Time 12 hours, 220 revs/min of drum's speed of rotation, alternating direction one per hour
It is secondary；After ball milling, the powder after ball milling is dried using the drying means of step (2).
(5) add adhesive polyethylene alcohol (PVA) granulating and forming and blank is pressed under 8-10MPa, then blank is put
Enter in sintering furnace, ceramic powder is sintered using high temperature sintering furnace, 1200 DEG C of sintering temperature, be incubated 6 hours, obtain inhaling ripple
Material.
As shown in figure 4, the reflectivity for the absorbing material that embodiment 3 is prepared is shown, the centre frequency of absorbing material exists
10.2GHz。
Embodiment 1-3 is prepared below absorbing material is measured using reflectivity instrument, as a result table 1 with
And shown in accompanying drawing 1-3.
The centre frequency of embodiment 1-3 absorbing material
| Centre frequency/GHz of absorbing material | |
| Embodiment 1 | 4.45 |
| Embodiment 2 | 6.0 |
| Embodiment 3 | 10.2 |
Above-mentioned embodiment is only the preferred embodiment of the present invention, it is impossible to the scope of protection of the invention is limited with this,
The change and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed scope.
Claims (9)
1. a kind of absorbing material of adjustable frequency, it is characterised in that the absorbing material is using barium carbonate, iron oxide as major ingredient, oxidation
Cobalt, titanium oxide, zirconium oxide are that ion doping regulates and controls auxiliary material, are prepared through ball milling, sintering；The chemical formula of the absorbing material is
BaFe12-2x(CoTi0.5Zr0.5)xO19, wherein x span is 0.3-1.2.
A kind of 2. preparation method of the absorbing material of adjustable frequency, it is characterised in that including：
Feed proportioning step：According to the absorbing material component dispensing of following molal weight percentage：10-18mol% barium carbonate,
57-85mol% iron oxide, 0-5mol% cobalt oxide, 0-5mol% titanium oxide and 0-5mol% zirconium oxide；Above-mentioned group
Centimorgan your mass percent sum is 100%；
Ball milling step：After dispensing is complete, adds deionized water and ball milling iron ball carries out a ball milling, Ball-milling Time 12-18
Hour, rotational speed of ball-mill 220-250r/min, after ball milling terminates, abrasive material is taken out, is dried in 80-120 DEG C of baking oven；
Pre-sintering step：After drying, 60 mesh sub-sieves are crossed, is put into sintering furnace and is sintered, be then naturally cooling to room with stove
Temperature, obtain barium ferrite pre-sintered powder；
Secondary ball milling step：Barium ferrite pre-sintered powder is added into deionized water and ball milling iron ball and carries out secondary ball milling, during ball milling
Between 10-12h, rotational speed of ball-mill 250r/min；
Sinter molding step：Secondary ball abrasive material is taken out and dried, adhesive granulating and forming is added and is simultaneously pressed into blank, then by base
Part is put into sintering furnace, and 4-6h is sintered at a temperature of 1150-1280 DEG C, and being cooled to room temperature with stove obtains the adjustable frequency
Absorbing material.
3. preparation method as claimed in claim 2, it is characterised in that in the step of feed proportioning, all absorbing materials
Component is that chemical analysis is pure.
4. preparation method as claimed in claim 2, it is characterised in that in the step of ball milling, the quality of absorbing material
Summation, deionized water, the weight ratio of ball milling iron ball are 1：(1.2-1.4)：4.
5. preparation method as claimed in claim 2, it is characterised in that in the step of pre-sintering, after being put into sintering furnace, with
2 DEG C/min heating rate to 1000-1100 DEG C and is incubated 2-6h by room temperature.
6. preparation method as claimed in claim 2, it is characterised in that in the step of secondary ball milling, barium ferrite pre-sintered powder
Material, deionized water, the weight ratio of ball milling iron ball are 1:1:3.5.
7. preparation method as claimed in claim 2, it is characterised in that in the step of sinter molding, described adhesive is poly-
One kind in vinyl alcohol, vinyl acetate, acrylic acid etc.；The addition of described adhesive is the 5- of secondary ball abrasive material gross weight
20%.
8. preparation method as claimed in claim 2, it is characterised in that described to be pressed into blank in the step of sinter molding
Process in pressure be 8-10Mpa.
9. preparation method as claimed in claim 2, it is characterised in that in the step of first and second ball milling, the ball milling iron ball
The quantitative proportion of the big ball of bead and a diameter of 3mm including a diameter of 1mm, bead and big ball is 3:1, ball milling side during ball milling
To per hour alternately once.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710546674.5A CN107686344A (en) | 2017-07-06 | 2017-07-06 | A kind of absorbing material of adjustable frequency and preparation method thereof |
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| CN109879270A (en) * | 2019-04-24 | 2019-06-14 | 哈尔滨工业大学 | A kind of preparation method of lightweight ultra-wideband carbonization red bayberry absorbing material |
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