CN103964854B - A kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof - Google Patents

A kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof Download PDF

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CN103964854B
CN103964854B CN201410188144.4A CN201410188144A CN103964854B CN 103964854 B CN103964854 B CN 103964854B CN 201410188144 A CN201410188144 A CN 201410188144A CN 103964854 B CN103964854 B CN 103964854B
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thin layer
silicon carbide
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resistant material
sic ceramic
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CN103964854A (en
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张玉军
李其松
龚红宇
张炎
艾树鹤
赵新巧
赵佳星
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Shandong University
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Abstract

The present invention relates to a kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof.This SiC ceramic thin layer bullet resistant material is the gel injection thin slice prepared by following feed composition: silicon carbide micro-powder, boron carbide micro powder, acrylamide monomer, N ' N methylene-bisacrylamide, Tetramethylammonium hydroxide, tributyl phosphate, deionized water and ammonium persulphate.The present invention also provides the preparation method of described SiC ceramic thin layer bullet resistant material.SiC ceramic layer material of the present invention achieves large size, fine and close smooth silicon carbide ceramics preparation of sections, size adjustable, hardness and fracture toughness property good, good as layer-built armor bullet resistant material protective capacities.

Description

A kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof
Technical field
The present invention relates to a kind of layer-built armor protection SiC ceramic thin layer bullet resistant material and preparation method thereof, belong to armor facing field of material technology.
Background technology
In modern war, armour material is one of gordian technique of military weapon.High-performance armour material not only can improve the battlefield survival of fight weapon, and does not reduce maneuverability when it is attacked.The advantage that the density that silicon carbide ceramics has is low, hardness is large, shock resistance is good, ballisticperformances is good, become the ideal material making high performance ballistic harness, be widely used in and make flak jackets, vehicle armor plate armour, naval vessel bulletproof armour, vertiplane bulletproof armour etc.
But stupalith toughness is low, the shortcoming of poor reliability limits the application of silicon carbide ceramics as armor facing material to a certain extent.In recent years, along with bionic fast development, the plate armour that thin layers of ceramic material and macromolecule layer lamination compound prepare similar clam shell feature becomes the developing direction of high-performance plate armour.At present, the forming method that thin layers of ceramic material is conventional mainly contains rolling formation, flow casting molding, gel casting forming etc.
Gel-casting process is a kind of near-net-shape technology of the people such as O.O.Omatete and M.A.Jenny invention of U.S.'s Oak Ridge National Laboratory nineties in 20th century, has cost low, can prepare the advantages such as high, the complex-shaped ceramic component of reliability.But, when preparing large size (length of side Thickness Ratio > 100) thin layer (thickness < 2mm) stupalith with Gel-casting process, in drying, sintering process, easily produce the defect such as warpage, cracking.
Chinese patent document CN101948312A discloses a kind of silicon carbide bullet-proof ceramics, and the mass percent of feed composition is: silicon carbide powder accounts for 40% ~ 50%, nanometer carbon black accounts for 8% ~ 12%, resol accounts for 3% ~ 10%, silicon accounts for 38% ~ 45%.CN103508734A provides a kind of Preparation method of bulletproof boron carbide/silicon carbide composite ceramic, by silicon carbide powder, boron carbide powder, nanometer carbon black mixing in mortar, is dissolved by resol alcohol, join in mortar, ball milling mixes, and the powder of mixing is added plastic agent and makes granule, then compression molding, make green compact, dry again, solidify, siliconising reaction sintering, the bullet resistant material of preparation, there is density little, the advantages such as ballistic performance is good.Method disclosed in foregoing invention is applicable to the preparation of block bullet-resistant ceramic material, and is silicon carbide reaction-sintered base bulletproof ceramic, and the fragility that free silica contained in material is low and hardness are unfavorable for giving full play to of silicon carbide ceramics ballistic performance.And the bulletproof ability of block bullet-resistant ceramic material is compared with novel laminated composite ceramic material, protective capacities is lower.
Summary of the invention
For the deficiencies in the prior art, preparing to solve the low and Gel-casting process of existing ceramic armor material toughness the problem easily producing warpage, cracking in large size thin ceramic product drying, sintering process, the invention provides a kind of layer-built armor protection SiC ceramic large size thin layer bullet resistant material and preparation method thereof.
Technical scheme of the present invention is as follows:
A kind of layer-built armor protection SiC ceramic thin layer bullet resistant material, be that the gel injection thin slice prepared by the feed composition of following mass parts sinters, described sheet thickness is 0.3-2.5mm:
Silicon carbide micro-powder 100 parts, boron carbide micro powder 0.5-2 part, acrylamide monomer 20-35 part, N ' N methylene-bisacrylamide 1-3 part, Tetramethylammonium hydroxide 0.5-1.5 part, tributyl phosphate 0.2-0.8 part, deionized water 30-45 part, initiator ammonium persulfate solution 2-5 part.
Described silicon carbide micro-powder median size is 0.45 μm, purity >=98.5%;
Described boron carbide micro powder median size is 1.5-3.5 μm, purity >=93.5%;
Described ammonium persulfate solution is the ammonium persulfate aqueous solution of 2-4wt.%;
Preferred according to the present invention, feed composition mass parts is as follows: silicon carbide micro-powder 100 parts, boron carbide micro powder 0.5-1.5 part, acrylamide monomer 15-30 part, N ' N methylene-bisacrylamide 1.5-2.5 part, Tetramethylammonium hydroxide 0.8-1.2 part, tributyl phosphate 0.4-0.6 part, deionized water 35-42 part, initiator ammonium persulfate solution 2-3 part.
Preferred according to the present invention, the thickness 0.5-2mm of described SiC ceramic thin layer bullet resistant material; Length and width size selects die size as required, can realize the preparation of SiC ceramic sheet product of long 100 ~ 1000mm, wide 100 ~ 1000mm.Belong to large size thin ceramic product.
The present invention's silicon carbide micro-powder used, boron carbide micro powder, acrylamide monomer, N ' N methylene-bisacrylamide, Tetramethylammonium hydroxide, tributyl phosphate, ammonium persulphate are commercially available industrial pure material.
A preparation method for layer-built armor protection SiC ceramic thin layer bullet resistant material, comprises step as follows:
(1) ceramic size is prepared
Take silicon carbide micro-powder, boron carbide micro powder, acrylamide monomer, N ' N methylene-bisacrylamide, Tetramethylammonium hydroxide, tributyl phosphate by proportioning, add deionized water, ball milling mixes; Vacuum stirring de-bubble; Then add ammonium persulfate solution initiator, in vacuum mixer, be evacuated to-0.08MPa while stirring, keep 3-7 minute, make slurry Homogeneous phase mixing, and remove bubble.
(2) casting
Slurry obtained for step (1) is injected silica glass mould, at 25-35 DEG C of temperature, solidifies 10-18 hour, the demoulding, obtained regular thin layer silicon carbide green body;
(3) body drying
Thin layer silicon carbide green body obtained for step (2) is moved in the kiln of 40-50 DEG C, smooth drying between the gypsum thin plate being placed in surface smoothing, obtain injection moulding blank;
(4) sinter
A. low-temperature primary smooths sizing
Thin layer silicon carbide green body obtained for step (3) is loaded in vacuum oven, under being placed in the graphite cake of surface smoothing, is slowly warming up to 200-300 DEG C with the speed of 2-5 DEG C/min, is incubated 1-3 hour under protective atmosphere, sizing is smoothed to base substrate;
B. high temperature secondary smooths sintering
The thin layer silicon carbide green body smoothing sizing obtained by step a is inserted in graphite vacuum high temperature furnace, the graphite cake of upper pressure surface smoothing, and at graphite cake corner advance expenditure pad, spacer thickness is 1.05-1.15 times of thin layer silicon carbide green body thickness; Under protective atmosphere, at 2050-2180 DEG C of temperature, be incubated 1-3 hour, obtained fine and close smooth silicon carbide ceramics layer material.
Gained thin layer silicon carbide ceramics layer material can realize the large size specification of long 100 ~ 1000mm, wide 100 ~ 1000mm, and can keep smooth, not warpage, do not ftracture; Volume density is 3.02 ~ 3.12g/cm 3, vickers microhardness > 25GPa, fracture toughness property > 4.5MPam 1/2, protective capacities reaches IV grade of requirement of shelter of NIJ0101.06 standard regulation.
Preferred according to the present invention, the vacuum stirring de-bubble described in step (1), is add in vacuum mixer by the slurry that ball milling mixes, is evacuated to-0.08MPa while stirring, keep 10-30 minute, bubble residual in removing slurry.
Preferred according to the present invention, the ammonium persulfate aqueous solution of to be concentration the be 2-4wt% of the ammonium persulfate solution initiator described in step (1), wherein ammonium persulfate aqueous solution add-on accounts for silicon carbide mass ratio 2.0-3.0wt%.
Preferred according to the present invention, in step (2), silica glass mould is clean, smooth silica glass mould, cuts the corner of irregularity after the demoulding, obtained regular thin layer silicon carbide green body.
Preferred according to the present invention, described in step (3), gypsum sheet gauge is 3.0-6.5mm.Gypsum sheet size used can be determined according to needing the size of dry silicon carbide green body thin slice.Smooth drying between gypsum thin plate thin layer silicon carbide green body being placed in surface smoothing, prepare to solve Gel-casting process the warpage, the problems of crack that produce in large size thin ceramic product drying process.
Preferred according to the present invention, graphite cake described in step (4) is the graphitic sheet of thickness 2.5-7.5mm, and graphitic sheet size used can be determined according to the thin layer silicon carbide green body lamina dimensions at sintering.
Preferred according to the present invention, the protective atmosphere described in step (4) a, b is argon gas or nitrogen.
Preferred according to the present invention, the pad of the graphite cake corner advance expenditure described in step (4) b is that the injection moulding blank of the step (3) identical with thin layer silicon carbide green body material to be sintered is cut into slices; The shim size of graphite cake corner advance expenditure according to the Mass adjust-ment of graphitic sheet, can be preferably the square pad of length of side 5-20mm.
Beneficial effect
1, the present invention is that carbon source substitutes direct carbon source with acrylamide monomer, both ensure that the dispersed of carbon, turn improve blank strength, be especially applicable to Gel-casting process and prepare large size silicon-carbide thin layers of ceramic material, solve the problem of easy warpage, cracking in body drying, sintering process.
2, the present invention adopts graphitic sheet to smooth sintering process, and at the gel injection thin slice that the advance expenditure of graphitic sheet corner is filled a prescription equally and prepared by same process, utilize the principle that its equal proportion is shunk, ensure that graphitic sheet is adjacent to all the time and don't is pressed in completely on gel injection thin slice, the base substrate buckling deformation problem produced in sintering process can be solved, laminar green tape under graphitic sheet weight can be avoided again cannot to move the problem of Cracking shrinking and cause, simultaneously can also laminated multi-layer, improve batch.
3, the thickness of SiC ceramic layer material thin slice of the present invention is 0.3-2.5mm, and product length and width size adjusts as required, can realize the preparation of large size SiC ceramic sheet product of long 100 ~ 1000mm, wide 100 ~ 1000mm.
4, the hardness of SiC ceramic layer material thin slice of the present invention and fracture toughness property good, be a kind of novel laminated composite ceramic material, good as layer-built armor bullet resistant material protective capacities.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but institute of the present invention protection domain is not limited thereto.
Described silicon carbide micro-powder median size is 0.45 μm, purity >=98.5%; Described boron carbide micro powder median size is 1.5-3.5 μm, purity >=93.5%; Commercial products.
Embodiment 1: a kind of preparation method of layer-built armor SiC ceramic thin layer bullet resistant material, step is as follows:
1) ball milling mixing
By mass parts, take the silicon carbide micro-powder 100 parts that median size is 0.45 μm respectively, median size is the boron carbide micro powder 1 part of 1.5 μm, acrylamide monomer 20 parts, N ' N methylene-bisacrylamide 1.5 parts, Tetramethylammonium hydroxide 1 part, tributyl phosphate 0.5 part, adds in the deionized water of 38 parts, and in tumbling ball mill, ball milling obtains gel injection silicon carbide slurry in 10 hours.
2) vacuum stirring de-bubble
By through step 1) slurry after process adds in vacuum mixer, and be evacuated to-0.08MPa while stirring, keep 20 minutes, the bubble remained in removing slurry.
3) initiator is added
Configuration 2.5wt.% ammonium persulfate aqueous solution as initiator, take 3 parts of described initiator solutions by mass parts and add through step 2) process after slurry in, in vacuum mixer, be evacuated to-0.08MPa while stirring, keep 4 minutes.
4) casting
Will through through step 3) slurry after process injects clean, smooth silica glass mould, glass size is 420mm × 420mm, between glass, gap is 1mm, solidify 12 hours at 25 DEG C of temperature, the demoulding, cut the corner of irregularity, obtain regular, that specification is 400mm × 400mm × 1mm large size thin layer silicon carbide green body.
5) drying is smoothed
By step 4) the large size thin layer silicon carbide green body that obtains moves in the kiln of 40 DEG C, drying is smoothed between the gypsum thin plate being placed in surface smoothing, plasterboard is of a size of 420mm × 420mm × 5mm, 20 hours time of drying, obtain the large size thin layer silicon carbide green body that specification is 372mm × 372mm × 0.92mm.
6) low-temperature primary smooths sizing
By step 5) the large size thin layer silicon carbide green body that obtains loads in vacuum oven, and under being placed in the graphitic sheet of surface smoothing, graphite cake is of a size of 400mm × 400mm × 5mm.Slowly be warming up to 270 DEG C with the speed of 3 DEG C/min, be incubated 2 hours under argon gas atmosphere, sizing is smoothed to base substrate.
7) high temperature secondary smooths sintering
By step 6) the large size thin layer silicon carbide green body that obtains inserts in graphite vacuum high temperature furnace, and furnace bottom is the level and smooth thick graphite cake of load-bearing.Base substrate is pressed the graphitic sheet of surface smoothing, graphitic sheet is of a size of 390mm × 390mm × 4mm, and be 1mm, length of side 12mm square injection molding blank at thickness prepared by the same Recipe of graphitic sheet corner advance expenditure, under an argon atmosphere, be incubated 1.5 hours at 2160 DEG C of temperature, obtaining specification is 298mm × 298mm × 0.75mm, fine and close smooth large size thin layer silicon carbide ceramics layer material.
After testing, the volume density of gained thin layer thyrite is 3.10g/cm 3, vickers microhardness 26.7Gpa, fracture toughness property 5.57MPam 1/2.
Embodiment 2: a kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof, step is as follows:
1) ball milling mixing
By mass parts, take the silicon carbide micro-powder 100 parts that median size is 0.45 μm respectively, median size is the boron carbide micro powder 1.5 parts of 3.5 μm, acrylamide monomer 22 parts, N ' N methylene-bisacrylamide 1.6 parts, Tetramethylammonium hydroxide 1 part, tributyl phosphate 0.5 part, adds in the deionized water of 41 parts, and in tumbling ball mill, ball milling obtains gel injection silicon carbide slurry in 12 hours.
2) vacuum stirring de-bubble
By through step 1) slurry after process adds in vacuum mixer, and be evacuated to-0.08MPa while stirring, keep 20 minutes, the bubble remained in removing slurry.
3) initiator is added
Configuration 2.5wt.% ammonium persulfate aqueous solution as initiator, take 3 parts of described initiators by mass parts and add through step 2) process after slurry in, in vacuum mixer, be evacuated to-0.08MPa while stirring, keep 4 minutes.
4) casting
Will through through step 3) slurry after process injects clean, smooth silica glass mould, glass size is 320mm × 320mm, between glass, gap is 0.8mm, solidify 15 hours at 25 DEG C of temperature, the demoulding, cut the corner of irregularity, obtain regular, that specification is 300mm × 300mm × 0.8mm large size thin layer silicon carbide green body.
5) drying is smoothed
By step 4) the large size thin layer silicon carbide green body that obtains moves in the kiln of 40 DEG C, drying is smoothed between the gypsum thin plate being placed in surface smoothing, plasterboard is of a size of 320mm × 320mm × 5mm, 25 hours time of drying, obtain the large size thin layer silicon carbide green body that specification is 282mm × 282mm × 0.74mm.
6) low-temperature primary smooths sizing
By step 5) the large size thin layer silicon carbide green body that obtains loads in vacuum oven, and under being placed in the graphitic sheet of surface smoothing, graphite cake is of a size of 300mm × 300mm × 4mm.Slowly be warming up to 250 DEG C with the speed of 2.5 DEG C/min, be incubated 2.5 hours under argon gas atmosphere, sizing is smoothed to base substrate.
7) high temperature secondary smooths sintering
By step 6) the large size thin layer silicon carbide green body that obtains inserts in graphite vacuum high temperature furnace, and furnace bottom is the level and smooth thick graphite cake of load-bearing.Base substrate is pressed the graphitic sheet of surface smoothing, graphitic sheet is of a size of 300mm × 300mm × 4mm, and fill a prescription equally in the advance expenditure of graphitic sheet corner, to prepare thickness be 0.8mm, length of side 10mm square gel injection blank to technique, under an argon atmosphere, be incubated 2 hours at 2140 DEG C of temperature, obtaining specification is the fine and close smooth large size thin layer silicon carbide ceramics layer material of 228mm × 228mm × 0.59mm.
After testing, the volume density of gained silicon carbide ceramics layer material is 3.08g/cm 3, vickers microhardness 25.9GPa, fracture toughness property 5.48MPam 1/2.
The silicon carbide ceramics layer material that embodiment 1-2 obtains carries out trajectory test, uses 53 formula 7.62mm armour piercing incendiary shelies, and during bullet velocity 840m/s, its protective capacities reaches IV grade of requirement of shelter of NIJ0101.06 standard regulation.

Claims (7)

1. a layer-built armor protection preparation method for SiC ceramic thin layer bullet resistant material, this material is that the gel injection thin slice prepared by the feed composition of following mass parts sinters, and described sheet thickness is 0.3-2.5mm:
Silicon carbide micro-powder 100 parts, boron carbide micro powder 0.5-2 part, acrylamide monomer 20-35 part, N ' N methylene-bisacrylamide 1-3 part, Tetramethylammonium hydroxide 0.5-1.5 part, tributyl phosphate 0.2-0.8 part, deionized water 30-45 part, initiator ammonium persulfate solution 2-5 part;
Described silicon carbide micro-powder median size is 0.45 μm, purity >=98.5%;
Described boron carbide micro powder median size is 1.5-3.5 μm, purity >=93.5%;
Preparation process is as follows:
(1) ceramic size is prepared
Take silicon carbide micro-powder, boron carbide micro powder, acrylamide monomer, N ' N methylene-bisacrylamide, Tetramethylammonium hydroxide, tributyl phosphate by proportioning, add deionized water, ball milling mixes; Vacuum stirring de-bubble; Then add ammonium persulfate solution initiator, in vacuum mixer, be evacuated to-0.08MPa while stirring, keep 3-7 minute, make slurry Homogeneous phase mixing, and remove bubble;
(2) casting
Slurry obtained for step (1) is injected silica glass mould, at 25-35 DEG C of temperature, solidifies 10-18 hour, the demoulding, obtained regular thin layer silicon carbide green body;
(3) body drying
Thin layer silicon carbide green body obtained for step (2) is moved in the kiln of 40-50 DEG C, smooth drying between the gypsum thin plate being placed in surface smoothing, obtain injection moulding blank;
(4) sinter
A. low-temperature primary smooths sizing
Thin layer silicon carbide green body obtained for step (3) is loaded in vacuum oven, under being placed in the graphite cake of surface smoothing, is slowly warming up to 200-300 DEG C with the speed of 2-5 DEG C/min, is incubated 1-3 hour under protective atmosphere, sizing is smoothed to base substrate;
B. high temperature secondary smooths sintering
The thin layer silicon carbide green body smoothing sizing obtained by step a is inserted in graphite vacuum high temperature furnace, the graphite cake of upper pressure surface smoothing, and at graphite cake corner advance expenditure pad, the pad of described graphite cake corner advance expenditure, be that the injection moulding blank identical with thin layer silicon carbide green body material to be sintered is cut into slices, spacer thickness is 1.05-1.15 times of thin layer silicon carbide green body thickness; Under protective atmosphere, at 2050-2180 DEG C of temperature, be incubated 1-3 hour, obtained smooth silicon carbide ceramics layer material.
2. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, it is characterized in that the vacuum stirring de-bubble described in step (1), that the slurry that ball milling mixes is added in vacuum mixer, be evacuated to-0.08MPa while stirring, keep 10-30 minute, bubble residual in removing slurry.
3. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, it is characterized in that the ammonium persulfate initiator described in step (1) to be concentration be the ammonium persulfate aqueous solution of 2-4wt%, wherein ammonium persulfate aqueous solution add-on accounts for silicon carbide mass ratio 2.0-3.0wt%.
4. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, is characterized in that described in step (3), gypsum sheet gauge is 3.0-6.5mm.
5. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, is characterized in that graphite cake described in step (4) is the graphitic sheet of thickness 2.5-7.5mm.
6. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, is characterized in that the protective atmosphere described in step (4) a, b is argon gas or nitrogen.
7. the preparation method of SiC ceramic thin layer bullet resistant material according to claim 1, is characterized in that the pad of the graphite cake corner advance expenditure described in step (4) b is the square of length of side 5-20mm.
CN201410188144.4A 2014-05-06 2014-05-06 A kind of layer-built armor SiC ceramic thin layer bullet resistant material and preparation method thereof Expired - Fee Related CN103964854B (en)

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