CN100581335C - Zinc oxide wave-absorbing material and preparing process - Google Patents
Zinc oxide wave-absorbing material and preparing process Download PDFInfo
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- CN100581335C CN100581335C CN200610018278A CN200610018278A CN100581335C CN 100581335 C CN100581335 C CN 100581335C CN 200610018278 A CN200610018278 A CN 200610018278A CN 200610018278 A CN200610018278 A CN 200610018278A CN 100581335 C CN100581335 C CN 100581335C
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Abstract
The present invention relates to a wave absorbing material and a preparation technique thereof, particularly to a zinc oxide wave absorbing material and a preparing process thereof. The preparation technique of the zinc oxide wave absorbing material is characterized in that the preparation technique is operated according to the following steps that zinc powder and a carbonaceous reducing agent are proportioned and uniformly mixed, and the air is filled in a mixture of the zinc powder and the carbonaceous reducing agent under the condition that the air pressure is maintained from 0.1 to 0.2Pa; next, the mixture is heated to reach the temperature of 900 to 1200DEG C and react for 5 to 200 minutes; finally, the zinc oxide wave absorbing material is obtained, wherein the granularity of the zinc powder is from 60 to 200 meshes, and the particle diameter of the carbonaceous reducing agent is from 0.1 to 5mm; the weight ratio of the zinc powder to the carbonaceous reducing agent is 1: 0.1 to 5. The bulk density of the zinc oxide wave absorbing material is from 0.02 to 0.20 gram / cubic centimeter, and the specific surface area is from 80 to 100 square meters/ gram. Experiments show that the zinc oxide wave absorbing material provided by the present invention has the advantages of specific structure, high heat conversion efficiency and high speed. The zinc oxide wave absorbing material has good application prospects in the industrial field, particularly in ceramic industry. The invention relates to a zinc oxide wave -absorption material and preparing process therefor. Said process includes: uniformly mixing zinc powder and carbon reductant, feeding air under 0.1-0.2 Pa condition, heating to 900-1200C degree, reacting for 60-200 minutes, in which the granular size of the zinc powder is 60-200 mesh, the grain size of the carbon redundant is 0.1-5mm, the weight ratio the two is 1:1.0-5. Bulk density of the zinc oxide is 0.02-0.20 g/cm3, and the specific surface area thereof is 80-100m2/g. Advantages: high heat conversion efficiency and speed.
Description
Technical field
The present invention relates to a kind of absorbing material and preparation technology thereof.Particularly Zinc oxide wave-absorbing material and preparation technology thereof.
Background technology
Absorbing material is to absorb by the electromagnetic wave energy that is transmitted into its surface, and dielectric loss or magnetic loss by the material class material that changes heat energy into.Two major types can be divided into by its moulding process and carrying: structure-type wave-absorption material and application type absorbing material, i.e. antiradar coatings.Technology is simple because the application type absorbing material has, easy construction, be not subjected to plurality of advantages such as work shape restriction, so be widely used; The structure-type wave-absorption material has carrying and reduces the reflection of electromagnetic wave dual-use function, so receive much concern in military affairs.
In modern war, along with the fast development of high-tech such as electronic countermeasures, stealth technology has become one of important means of obtaining triumph.Stealth technology is subjected to the great attention of multinational military authority as the survival ability that improves the weaponry system and the effective means of penetration ability, and the application of absorbing material is one of key factor of stealth technology development.Applying absorbing material requires it to have bandwidth, in light weight, performance such as density is little, and is high temperature resistant and anticorrosive on using.Good absorbing material has been widely used in the military equipments such as Aeronautics and Astronautics, rocket, guided missile, aircraft, naval vessels, and for example the stealthy attack plane of the F-117A of the U.S., B-2 strategic bomber and the stealthy fighter plane of Muscovite S-37 etc. have all adopted good absorbing material.Along with the high speed development of hyundai electronics industry and information industry, the electronic equipment of the interference (EMI) that generates electromagnetic waves sharply increases, and makes that these new social effects of pollution of EMI are serious day by day, and the shielding electromagnetic waves problem also seems very important for this reason.Developed country has issued the rules of control Electromagnetic Interference in succession.According to laws and regulations requirement, the substandard electronic product of every shielding EMI is forbidden to dispatch from the factory and import without exception.We carry out suppressing electromagnetic electromagnetic compatibility standard from 1998.And from compulsory execution in 2000.Thereby the research and development of the shielding EMI material that uses attract people's attention, so absorbing material also has good prospects for application in electronics industry.
The more general absorbing material of our uses is a ferrite at present, it has the frequency characteristic of broad, its relative permeability is higher, performances such as relative dielectric constant is less, but it is big that shortcoming is a density, poor heat stability only is suitable for making matching layer, and for example Chinese patent 200410099156 has proposed a kind of SIC electromagnetic-wave absorbent of coated with barium ferrite film.200,510,011,177 1 kinds of carbon nano-tube composite coating layer type wave absorption materials of Chinese patent and preparation method thereof, it is divided into matrix partly, is made up of polymer and carbon nano-tube, and coating layer portion is made up of coating and nano-ZnO, and they all are composite coating layer types.
Domestic not seeing as yet can the invention provides this good absorbing material efficiently apace with the high-quality absorbing material of electromagnetic wave conversion thermal energy at present.
Summary of the invention:
One of purpose of the present invention is to provide a kind of Zinc oxide wave-absorbing material.
Two of purpose of the present invention is to provide a kind of and has that density is little, light specific gravity, can be efficiently the Zinc oxide wave-absorbing material of absorbing property fast.
Three of purpose of the present invention is to provide the preparation technology of Zinc oxide wave-absorbing material.
The present invention is achieved by the following technical solutions:
Zinc oxide wave-absorbing material, wherein: the bulk density 0.02-0.20 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area are the 80-200 meters squared per gram.
Zinc oxide wave-absorbing material, wherein: the heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material is 1000-1500 ℃, bulk density 0.08-0.12 gram/cubic centimetre, specific area is the 80-100 meters squared per gram.
The preparation technology of Zinc oxide wave-absorbing material, wherein: follow these steps to operation: with zinc powder and carbonaceous reducing agent, through batching and mixing, keep at air pressure feeding gas under the condition of 0.1-0.2Pa, be heated to 900-1200 ℃, reaction and can obtain Zinc oxide wave-absorbing material in 5-200 minute; Wherein the granularity of zinc powder is the 60-200 order, and the particle diameter of carbonaceous reducing agent is 0.1-5mm; The weight ratio of zinc powder and carbonaceous reducing agent is 1: 0.1-5; Gas is air or oxygen.
The preparation technology of Zinc oxide wave-absorbing material, wherein: carbonaceous reducing agent comprises: any one in charcoal, walnut shell charcoal, the tea seed shell charcoal planted in active carbon, coke, charcoal, bamboo charcoal, corruption.
The preparation technology of Zinc oxide wave-absorbing material, wherein: being shaped as of carbonaceous reducing agent: any one in the particle shape of elongated cylindrical, short cylindrical shape, six shapes, oblateness, prismatic, triangle, bar-shaped, grain of rice shape, plate-like and none setting attitude.
The preparation technology of Zinc oxide wave-absorbing material, wherein: the flow that feeds gas the 30-60 liter/hour.
The preparation technology of Zinc oxide wave-absorbing material, wherein: the weight ratio of zinc powder and carbonaceous reducing agent is 1: 0.5-2.0.
Principle:
The present invention adopts the metallic zinc micro mist of certain particle size and the charcoal of certain shape; and the air of feeding trace; help the formation of zinc oxide crystallite; when the metallic zinc particulate is heated to 900 ℃; the zinc fume that generates forms zinc oxide nucleus particulate along with the thermal current rising combines with airborne oxygen; owing between the bigger charcoal particle of particle diameter bigger hole is arranged, guaranteed that the zinc fume particulate can move up along hole, unlikely being stopped and sinter duricrust into.Zinc oxide nucleus particulate rises to the surface of material and deposits, because zinc fume constantly generates, the zinc oxide nucleus constantly deposits, and nucleus is progressively grown up form the zinc oxide of certain pattern at last.It is regular that process having thus described the invention can make pattern, density is very little, outward appearance is white in color loose coccoid zinc oxide material, and its appearance features is as follows:
The heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material can reach 1200 ℃, bulk density 0.08-0.12 gram/cubic centimetre, and specific area is greater than the 80-90 meters squared per gram.
Real part of permittivity 4.5-30, dielectric constant imaginary part 35-140, wave absorbtion matter: inhale ripple dielectric loss type.
The zinc oxide of the present invention's preparation is a kind of good absorbing material, under irradiation of electromagnetic waves, can quickly and efficiently the electromagnetism wave energy be converted into heat energy, its feature is that efficient height, speed are fast, under certain power and efficient, can make heated object reach fervid, be 2.45GHz for example in the microwave oven frequency, power 700W, the Zinc oxide wave-absorbing material that 1-2g is heavy is put in the crucible of heavy 30g, just crucible can be heated to 800-900 ℃ high temperature in tens seconds, its microwave and heat energy conversion efficient are high.
Be that frequency is under the 2.45GHz electromagnetic wave condition below, during different capacity, the thermal conversion of Zinc oxide wave-absorbing material is table as a result:
Microwave and heat energy conversion usefulness form:
| Frequency | Power | Time (second) | Crucible temperature | |
| 2.45 | 700W | 30 | 800-900℃ | |
| 2.45 | 800W | 20 | 800-900℃ | |
| 2.45GHz | 1000W | 10 | 800-900℃ |
Show that according to above-mentioned test the thermal conversion efficiency that the invention provides Zinc oxide wave-absorbing material is high, speed is fast, industrial circle particularly ceramic industry good application prospects is arranged.
The excellent characteristic of the Zinc oxide wave-absorbing material of the present invention's preparation can also illustrate by following test:
Zinc oxide wave-absorbing material mixed with the acrylic resin modified compounds of epoxy-ester in 3: 1000 ratio add the small diluted amount agent, adopt stirring and hyperacoustic method fully to mix thoroughly, be sprayed at then on paper or the plastic sheet, the about 0.05mm of thick coating is in 50 ℃ of oven dry, carry out again spraying thick about 0.1mm the second time, paper is cut into 5cm, wide little of long 2cm, reveal instrument with HI-2790B type microwave and test 0.05mm and the former little paper slip of 0.10mm coating respectively, its microwave attenuation is respectively 41% and 85%.
The zinc oxide material of proof the present invention preparation has the effect of inhaling ripple.
Zinc oxide wave-absorbing material of the present invention militarily can be used as the micro-wave screening material, in communications industry, can be used as the breadboard outer overcoat layer in research center, and the signal that shielding is divulged a secret easily prevents that the adversary from monitoring.
The appearance white that Zinc oxide wave-absorbing material of the present invention has is bulk, and its crystallite is four needle-likes, crystal grain profile rule, and structure is intact, smooth surface, big or small homogeneous.
The particle diameter 6-8 μ m of the zinc oxide crystallite that Zinc oxide wave-absorbing material of the present invention has, pin is short and thick, about 3-5 μ m, crown portion is by three or four semilunes synthetic nodular that closes that hardens, the about 1 μ m of root thickness.
Zinc oxide wave-absorbing material of the present invention has has that light specific gravity, density are little, density is at 0.02-0.2 gram/cubic centimetre, specific area is big, and specific area is 80 meters squared per gram, the thermal endurance height, do not decompose under 1000 ℃ of high temperature, efficiently the performance of fast Absorption microwave property.
Description of drawings:
Dress Zinc oxide wave-absorbing material in the crucible.
Fig. 1,2,3, the 4th, the PHILIP sem photograph of a kind of Zinc oxide wave-absorbing material of the present invention.It belongs to four acicular textures, big or small homogeneous, and structural integrity, crystal grain 6-8 μ m, the long 3-5 μ of pin m constitutes the pass nodular by three or four meniscuss between two pins of root, the about 1 μ m of root diameter (RD) thickness, pin footpath pin is long than being 1: 3-5.
Wherein Fig. 1 is that ESEM amplifies 5000 times zinc oxide crystallite absorbing material.
Wherein Fig. 2 is that ESEM amplifies 10000 times zinc oxide crystallite absorbing material.
Wherein Fig. 3 is that ESEM amplifies 10000 times zinc oxide crystallite absorbing material.
Wherein Fig. 4 is the figure of root that ESEM amplifies 20000 times zinc oxide crystallite absorbing material.
Fig. 5 is zinc oxide crystallite absorbing material X-ray diffraction analysis figure of the present invention.
Fig. 6 is common zinc oxide material X-ray diffraction analysis figure.
Nine corresponding successively lattice constants of crest line among Fig. 5 there is no the diffraction maximum of zinc simple substance or other impurity element, are the zinc oxide of the hexagonal structure of based on very high purity.
Among Fig. 5 nine crest lines corresponding successively (100), (002), (101), (102), (110), (103), (200), (112) and (201) crystal face of hexagonal crystal system zinc oxide of lattice constant a=0.325nm, c=0.521nm of zinc oxide of hexagonal crystal system of the present invention.
Need be illustrated especially that (100) crystal face intensity is higher than (101) crystal face among the figure, it is distinguishing that (101) crystal face intensity of the zinc oxide of this and traditional general hexagonal crystal system is higher than (100) crystal face.
Variation has taken place in certification structure.
Fig. 7,8, the 9th, Zinc oxide wave-absorbing material of the present invention are at microwave oven frequency 2.45HZ, and under the power 700W condition, 25 seconds crucibles reach the live telecast shooting figure of 800-900 ℃ crimson state.Fig. 7 is the shooting figure of heating when fire door was closed in 25 seconds, and Fig. 8 is heating shooting figure when door opened after 25 seconds.Fig. 9 heats the shooting figure of door opened back cooling in the time of 20 seconds after 25 seconds.
Embodiment
Getting 10 gram particle degree is 80 purpose zinc powders, itself and unformed charcoal 12 grams of particle diameter 1mm are made into compound, are laid in the high-temperature resistant container, place high temperature furnace to be heated to 940 ℃ in the container that compound is housed, be incubated 20 minutes, feeding air pressure simultaneously is 0.1Pa, and flow is 40 liters/hour a air, cools to room temperature naturally with the furnace, get the purity height, the good outward appearance of absorbing property is the white accumulation body of loose cotton-wool shape, and bulk density is 0.1 gram/cubic centimetre, and electron microscope is the regular zinc oxide of form down.Get the loose zinc oxide of 2g in the 30ml crucible, and to place frequency be 2.45GHz, in the microwave oven of power 800W, starts back 15-20 and be heated to 800-900 ℃ of state second immediately, the crucible appearance presents crimson pellucidity, and its electromagnetic wave and thermal energy conversion efficiency are very high.
The heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material is higher than 1200 ℃, bulk density 0.105 gram/cubic centimetre, and specific area is greater than 80 meters squared per gram.
Getting 20 gram particle degree is 60 purpose zinc powders, with itself and particle diameter is that 0.5mm active carbon 20 grams are made into compound and are laid in the high-temperature resistant container, place high temperature furnace to be heated to 960 ℃ in the container that compound is housed, be incubated 15 minutes, feeding air pressure simultaneously is 0.2Pa, flow is 40 liters/hour a air, naturally cool to room temperature with the furnace and get the purity height, the outward appearance of absorbing property excellence be the white accumulation body of loose cotton-wool shape, bulk density is 0.08 gram/cubic centimetre, and electron microscope is the zinc oxide of complete form down.Get the loose zinc oxide of 2g in the 30ml crucible, be built in frequency for for 2.45GHz, in the microwave oven of power 1000W, start back 10-15 and be heated to 800-900 ℃ of state second second immediately, the crucible appearance presents crimson pellucidity, and its electromagnetic wave and thermal energy conversion efficiency are very high.
Embodiment 3, Zinc oxide wave-absorbing material, wherein: the bulk density 0.02 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 200 meters squared per gram.All the other are with embodiment 1.
Embodiment 4, Zinc oxide wave-absorbing material, wherein: the bulk density 0.20 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 80 meters squared per gram.All the other are with embodiment 2.
Embodiment 5, Zinc oxide wave-absorbing material, wherein: the bulk density 0.11 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 143 meters squared per gram.All the other are with embodiment 1.
Embodiment 6, Zinc oxide wave-absorbing material, wherein: the heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material is 1000 ℃, bulk density 0.12 gram/cubic centimetre, specific area is greater than 80 meters squared per gram.All the other are with embodiment 2.
Embodiment 7, Zinc oxide wave-absorbing material, wherein: the heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material is 1500 ℃, bulk density 0.08 gram/cubic centimetre, specific area is greater than 160 meters squared per gram.All the other are with embodiment 1.
Embodiment 8, embodiment 6, Zinc oxide wave-absorbing material, wherein: the heat-resisting decomposition temperature of this Zinc oxide wave-absorbing material is 1236 ℃, bulk density 0.09 gram/cubic centimetre, specific area is greater than 137 meters squared per gram.All the other are with embodiment 1.
The preparation technology of embodiment 9, Zinc oxide wave-absorbing material, wherein: follow these steps to operation: with zinc powder and carbonaceous reducing agent, through batching and mixing, keep bubbling air under the condition of 0.2Pa at air pressure, be heated to 900 ℃, reaction and can obtain Zinc oxide wave-absorbing material in 5 minutes; Wherein the granularity of zinc powder is 200 orders, and the particle diameter of carbonaceous reducing agent is 0.1mm; The weight ratio of zinc powder and carbonaceous reducing agent is 1: 0.1.The air mass flow of bubbling air is at 60 liters/hour.
The preparation technology of embodiment 10, Zinc oxide wave-absorbing material, wherein: follow these steps to operation: with zinc powder and carbonaceous reducing agent, through batching and mixing, keep bubbling air under the condition of 0.1Pa at air pressure, be heated to 1200 ℃, reaction and can obtain Zinc oxide wave-absorbing material in 200 minutes; Wherein the granularity of zinc powder is 60 orders, and the particle diameter of carbonaceous reducing agent is 5mm; The weight ratio of zinc powder and carbonaceous reducing agent is 1: 5.The air mass flow of bubbling air is at 30 liters/hour.
The preparation technology of embodiment 11, Zinc oxide wave-absorbing material, wherein: follow these steps to operation: with zinc powder and carbonaceous reducing agent, through batching and mixing, keep bubbling air under the condition of 0.16Pa at air pressure, be heated to 980 ℃, reaction and can obtain Zinc oxide wave-absorbing material in 25 minutes; Wherein the granularity of zinc powder is 105 orders, and the particle diameter of carbonaceous reducing agent is 0.3mm; The weight ratio of zinc powder and carbonaceous reducing agent is 1: 0.4.The air mass flow of bubbling air is at 45 liters/hour.
The weight ratio of embodiment 12, zinc powder and carbonaceous reducing agent is 1: 0.5.All the other are with embodiment 9.
The weight ratio of embodiment 13, zinc powder and carbonaceous reducing agent is 1: 2.0.All the other are with embodiment 10.
The weight ratio of embodiment 14, zinc powder and carbonaceous reducing agent is 1: 1.4.All the other are with embodiment 11.
Embodiment 15, carbonaceous also original reagent are active carbon.All the other are with embodiment 9.
Embodiment 16, carbonaceous also original reagent are coke.All the other are with embodiment 10.
Embodiment 17, carbonaceous also original reagent are charcoal.All the other are with embodiment 11.
Embodiment 18, carbonaceous also original reagent are bamboo charcoal.All the other are with embodiment 9.
Embodiment 19, carbonaceous also original reagent are that charcoal is planted in corruption.All the other are with embodiment 10.
Embodiment 21, carbonaceous also original reagent are tea seed shell charcoal.All the other are with embodiment 11.
Embodiment 22, employing oxygen replaces air, all the other repeat above-mentioned all embodiment.
Embodiment 23, Zinc oxide wave-absorbing material, wherein: the bulk density 0.06 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 120 meters squared per gram.All the other repeat above-mentioned all embodiment.
Embodiment 24, Zinc oxide wave-absorbing material, wherein: the bulk density 0.07 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 168 meters squared per gram.All the other repeat above-mentioned all embodiment.
Embodiment 25, Zinc oxide wave-absorbing material, wherein: the bulk density 0.12 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 100 meters squared per gram.All the other repeat above-mentioned all embodiment.
Embodiment 26, Zinc oxide wave-absorbing material, wherein: the bulk density 0.13 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 84 meters squared per gram.All the other repeat above-mentioned all embodiment.
Embodiment 27, Zinc oxide wave-absorbing material, wherein: the bulk density 0.15 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 106 meters squared per gram.All the other repeat above-mentioned all embodiment.
Embodiment 28, Zinc oxide wave-absorbing material, wherein: the bulk density 0.04 gram/cubic centimetre of this Zinc oxide wave-absorbing material, specific area is 92 meters squared per gram.All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 29, Zinc oxide wave-absorbing material, wherein: react and can obtain Zinc oxide wave-absorbing material in 10 minutes; All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 30, Zinc oxide wave-absorbing material, wherein: react and can obtain Zinc oxide wave-absorbing material in 60 minutes; All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 31, Zinc oxide wave-absorbing material, wherein: react and can obtain Zinc oxide wave-absorbing material in 45 minutes; All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 32, Zinc oxide wave-absorbing material, wherein: the flow that feeds gas is at 100 liters/hour.All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 33, Zinc oxide wave-absorbing material, wherein: the flow that feeds gas is at 85 liters/hour.All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 34, Zinc oxide wave-absorbing material, wherein: the flow that feeds gas is at 75 liters/hour.All the other repeat above-mentioned all embodiment.
The preparation technology of embodiment 35, Zinc oxide wave-absorbing material, wherein: the flow that feeds gas is at 52 liters/hour.All the other repeat above-mentioned all embodiment.
Claims (1)
1, a kind of preparation technology of Zinc oxide wave-absorbing material, it is characterized in that: getting 10 gram particle degree is 80 purpose zinc powders, itself and unformed charcoal 12 grams of particle diameter 1mm are made into compound, be laid in the high-temperature resistant container, place high temperature furnace to be heated to 940 ℃ in the container that compound is housed, be incubated 20 minutes, feeding air pressure simultaneously is 0.1Pa, flow is 40 liters/hour a air, cools to room temperature naturally with the furnace, promptly.
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| CN102502780B (en) * | 2011-10-11 | 2013-08-28 | 浙江大学宁波理工学院 | Preparation method of lanthanum-doped zinc oxide microsphere with wave absorbing performance |
| CN102628214A (en) * | 2012-04-09 | 2012-08-08 | 天津大学 | Carbon fiber composite material with ZnO layer electrolytically deposited on surface as well as preparation method and application thereof |
| WO2019157805A1 (en) * | 2018-02-13 | 2019-08-22 | 陈志勇 | Midsole material and method for manufacturing same, outsole material, hot-melt adhesive film, laminating apparatus and sole |
| CN110876493B (en) * | 2019-11-26 | 2021-11-09 | 深圳麦克韦尔科技有限公司 | Aerosol generating product, electronic atomization device and wave-absorbing phase change body preparation method |
| CN116004184B (en) * | 2023-02-07 | 2024-04-16 | 西南石油大学 | Nano metal oxide/carbon composite wave-absorbing material and preparation method thereof |
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| A NEW METHOD FOR PREPARATION OF ZINCOXIDEWHISKERS. Zuowan Zhou,Hai Deng,Jing Yi,and Shikai Liu.Materials Research Bulletin,Vol.34 No.10/11. 1999 |
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