CN109942289A - A kind of preparation method of transparent armor alumino-silicate crystalline ceramics - Google Patents
A kind of preparation method of transparent armor alumino-silicate crystalline ceramics Download PDFInfo
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- CN109942289A CN109942289A CN201910255744.0A CN201910255744A CN109942289A CN 109942289 A CN109942289 A CN 109942289A CN 201910255744 A CN201910255744 A CN 201910255744A CN 109942289 A CN109942289 A CN 109942289A
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Abstract
The present invention relates to a kind of transparent armor preparation methods of alumino-silicate crystalline ceramics, which is characterized in that the materials chemistry composition formula of the ceramics are as follows: Al57Ca28O384Si135, use high temperature solid-state method to prepare, reached by rationally controlling calcining system and material rate and be burnt into stable cube phase structure, i.e. Al57Ca28O384Si135The features such as crystalline structure, this ceramic material have excellent translucency, and intensity is big, and hardness is high, short preparation period, production cost is low.
Description
Technical field
The present invention relates to crystalline ceramics preparation technical field, in particular to a kind of transparent armor alumino-silicate crystalline ceramics
Preparation method.
Background technique
Large scale, lightweight, high intensity crystalline ceramics have the function of ceramic material and structural ceramic material concurrently: both had
For high-intensitive protective performance, and multiband can be penetrated, improve the observation of system, scout recognition capability, enhance the master of system
Dynamic property, is the development trend of current transparent armor.The result of study of past few years shows because transparent ceramic material has hardness
It is the advantages of height, light weight, all very strong to the defence capability of kinetic energy weapon and ammunition fragmentation, it has also become one kind is widely used in shellproof
The Protective armor of the equipments such as clothing, vehicle and aircraft.
Currently, the crystalline ceramics of cube phase structure accounts for always very big ratio in the application, the glass and high score with amorphous
Sub- material is compared, and polycrystalline ceramics has the characteristics that high mechanical strength, fusing point are high, physicochemical properties are stable；With monocrystal material phase
Than the manufacture craft of polycrystalline ceramic is more simple, can be easily made the component of large scale Multiple Shape, meets high power laser
The needs of equal devices, and can be used as excellent mechanics material and optical material and be used in in corrosive harsh environment.
More than a traditional cube phase ceramics have many advantages, such as, but various aspects always could be improved by the doping of orientation
Performance, and preparation temperature is high, and difficulty is big, it is also contemplated that the problems such as doping, addition amount of auxiliary, uniformity.
Summary of the invention
The main purpose of the present invention is to provide a kind of transparent armor preparation method of alumino-silicate crystalline ceramics, production
Temperature is low, and does not have to doping, and the crystal structure with excellent translucent effect, spacing of lattice is larger, and electron cloud arrangement is intensive, gathers around
There is wider band gap, through the electromagnetic wave of more multi-wavelength, especially in visible-range, and raw material stable phase easily generated, from
And the temperature of crystal generation is reduced, the cost of manufacture of reduction does not include heavy metal or rare earth ion, more naturally environmentally friendly.
In order to solve the above technical problems, the technical scheme adopted by the invention is as follows:
A kind of preparation method of transparent armor alumino-silicate crystalline ceramics, which is characterized in that it is described ceramics it is materialized
Learn composition formula are as follows: Al57Ca28O384Si135, use high temperature solid-state method to prepare, by rationally controlling calcining system and material rate
Stable cube phase structure, i.e. Al are burnt into reach57Ca28O384Si135Crystalline structure.
Further, the high temperature solid-state method preparation, specifically comprises the following steps:
(1) to the raw material calcium oxide CaO of 99.99% purity, the raw alumina Al of 99.9999% purity2O3, 99.99%
The raw material silicon oxide sio of purity2It is calcined, removes the impurity and moisture in raw material；
(2) according to chemical formula Al57Ca28O384Si135The molar ratio of middle each element, by calcined aluminium oxide, calcium oxide and
Silica is put into ball grinder with the cation mole ratio of 57:28:135, and abrading-ball is added, and suitable dehydrated alcohol work is added and disperses
Agent carries out ball milling；
(3) slurry after ball milling is put into baking oven drying, until being completely dried, and with the sieve of 200 mesh to powder
Sieving three times；
(4) powder after drying is fitted into mold, then plastic packaging in blocks with the pressure dry-pressing of 10MPa, carry out it is cold etc.,
Pressure maintaining 5 minutes, obtain potsherd under the pressure of 200MPa；
(5) potsherd is put into precalcining in Muffle furnace；
(6) potsherd after precalcining is put into high temperature Muffle furnace and is sintered, temperature is 1600-1700 DEG C, soaking time
6-8 hours；
(7) sintered potsherd is put into Muffle furnace and is made annealing treatment, temperature is 1350-1450 DEG C, when heat preservation
Between 4-6 hours；
(8) potsherd after annealing is subjected to polishing grinding, twin polishing to 1-3mm to get showing under visible light
The ceramic material of high transmittance.
Further, in the step (2), abrading-ball is alumina balls, rotational speed of ball-mill 160-240r/min, time 8-
10 hours.
Further, in the step (3), drying temperature is 60-80 DEG C, is at least dried 24 hours.
Further, in the step (5), precalcining temperature is 500-700 DEG C, and the time is 6-8 hours, and in precalcining
Before, it needs to open ventilation equipment, to guarantee that exhaust gas excludes, prevents the trend of heating air-flow in sample pollution and adjustment furnace.
Further, in the step (6), heating rate is 5-6 DEG C/min.
Compared with prior art, the invention has the advantages that being:
(1) production temperature is low, and does not have to doping, the crystal structure with excellent translucent effect, i.e.,
Al57Ca28O384Si135, which is in cubic, and space group is F d-3m (227), and silicon ion regularly interaction arrangement is brilliant
For compartment away from larger, electron cloud arrangement is intensive, possesses wider band gap, through the electromagnetic wave of more multi-wavelength, especially in visible light
Range, and raw material stable phase easily generated, to reduce the temperature of crystal generation, the cost of manufacture of reduction does not include a huge sum of money
Category or rare earth ion, more naturally environmentally friendly, the phase of the current transparent ceramic material without the alumino-silicate cubic structure both at home and abroad
Close report；
(2) transparent ceramic material prepared by the present invention, prepares that simple controllability is strong, and crystal feature can carry out secondary
It is processing, various focal needs is such as met by adulterating.
Detailed description of the invention
It in order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, below will be to needed for embodiment
Attached drawing to be used is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention,
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings
Other attached drawings.
Fig. 1 is sample Al of the present invention57Ca28O384Si135X-ray powder diffraction pattern；
Fig. 2 is sample Al of the present invention57Ca28O384Si135SEM figure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with attached drawing to the present invention
Technical solution in embodiment is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented
Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of labour.
Embodiment 1
According to chemical formula Al57Ca28O384Si135The molar ratio of middle each element takes raw material calcium oxide CaO (99.99%) 15.70
Gram, aluminium oxide Al2O3(99.9999%) 29.07g, silicon oxide sio2(99.99%) 81.14g is calcined, and is removed in raw material
Impurity and moisture.Raw material is put into ball grinder, abrading-ball is added, suitable dehydrated alcohol is added and makees dispersing agent, carries out ball milling.It will
Slurry after ball milling is put into baking oven and dries 24 hours, until being completely dried, and with the sieve of 200 mesh to powder sieving three
Time.Powder is fitted into mold, then plastic packaging in blocks with the pressure dry-pressing of 10MPa, carry out it is cold etc., under the pressure of 200MPa
Pressure maintaining 5 minutes.Potsherd is put into precalcining in Muffle furnace, 500 DEG C of 8 hours of heat preservation.Potsherd is put into high temperature Muffle furnace
Middle sintering, temperature are 1700 DEG C, soaking time 8 hours.Potsherd is put into Muffle furnace and is made annealing treatment, temperature 1350
DEG C, soaking time 6 hours.Obtained potsherd is subjected to polishing grinding, twin polishing 1mm to get showing under visible light
The ceramic material of high transmittance.
Referring to attached drawing 1, X-ray powder diffraction pattern shows that the sample of preparation is Al57Ca28O384Si135Pure phase, peak type point
Differentiate clear, crystallinity is fine；
Referring to attached drawing 2, from scanning electron microscope diagram as can be seen that the crystalline ceramics structure stomata is less, compactness is good.
It should be pointed out that being above schematical by the detailed description that preferred embodiment carries out technical solution of the present invention
And not restrictive.Those skilled in the art can be to recorded in embodiment on the basis of reading description of the invention
Technical solution modify or equivalent replacement of some of the technical features, and these are modified or replaceed, not
The essence of corresponding technical solution is set to be detached from the range of technical solution of the embodiment of the present invention.
Claims (6)
1. a kind of transparent armor preparation method of alumino-silicate crystalline ceramics, which is characterized in that the materials chemistry of the ceramics
Composition formula are as follows: Al57Ca28O384Si135, use high temperature solid-state method to prepare, by rationally control calcining system and material rate come
Reach and is burnt into stable cube phase structure, i.e. Al57Ca28O384Si135Crystalline structure.
2. a kind of preparation method of transparent armor alumino-silicate crystalline ceramics according to claim 1, which is characterized in that
The high temperature solid-state method preparation, specifically comprises the following steps:
(1) to the raw material calcium oxide CaO of 99.99% purity, the raw alumina Al of 99.9999% purity2O3, 99.99% purity
Raw material silicon oxide sio2It is calcined, removes the impurity and moisture in raw material；
(2) according to chemical formula Al57Ca28O384Si135The molar ratio of middle each element, by calcined aluminium oxide, calcium oxide and oxidation
Silicon is put into ball grinder with the cation mole ratio of 57:28:135, and abrading-ball is added, suitable dehydrated alcohol is added and makees dispersing agent,
Carry out ball milling；
(3) slurry after ball milling is put into baking oven drying, be sieved until being completely dried, and with the sieve of 200 mesh to powder
Three times；
(4) powder after drying is fitted into mold, then plastic packaging in blocks with the pressure dry-pressing of 10MPa, carry out it is cold etc.,
Pressure maintaining 5 minutes, obtain potsherd under the pressure of 200MPa；
(5) potsherd is put into precalcining in Muffle furnace；
(6) potsherd after precalcining is put into high temperature Muffle furnace and is sintered, temperature is 1600-1700 DEG C, and soaking time 6-8 is small
When；
(7) sintered potsherd is put into Muffle furnace and is made annealing treatment, temperature is 1350-1450 DEG C, soaking time 4-6
Hour；
(8) potsherd after annealing is subjected to polishing grinding, twin polishing to 1-3mm is high saturating to get showing under visible light
Cross the ceramic material of rate.
3. a kind of preparation method of alumino-silicate crystalline ceramics according to claim 2, it is characterised in that: the step
(2) in, abrading-ball is alumina balls, and rotational speed of ball-mill 160-240r/min, the time is 8-10 hours.
4. a kind of preparation method of alumino-silicate crystalline ceramics according to claim 2, it is characterised in that: the step
(3) in, drying temperature is 60-80 DEG C, is at least dried 24 hours.
5. a kind of preparation method of alumino-silicate crystalline ceramics according to claim 2, it is characterised in that: the step
(5) in, precalcining temperature is 500-700 DEG C, and the time is 6-8 hours, and before precalcining, needs to open ventilation equipment, to protect
The trend that card exhaust gas excludes, prevents sample from polluting and adjusting heating air-flow in furnace.
6. a kind of preparation method of alumino-silicate crystalline ceramics according to claim 2, it is characterised in that: the step
(6) in, heating rate is 5-6 DEG C/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111634079A (en) * | 2020-04-28 | 2020-09-08 | 江苏华尚汽车玻璃工业有限公司 | Anti-splashing bulletproof glass and manufacturing method and application thereof |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111634079A (en) * | 2020-04-28 | 2020-09-08 | 江苏华尚汽车玻璃工业有限公司 | Anti-splashing bulletproof glass and manufacturing method and application thereof |
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