CN1112337C - Preparation of silicon nitride-based composite material with superhigh tenacity - Google Patents
Preparation of silicon nitride-based composite material with superhigh tenacity Download PDFInfo
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- CN1112337C CN1112337C CN99107783A CN99107783A CN1112337C CN 1112337 C CN1112337 C CN 1112337C CN 99107783 A CN99107783 A CN 99107783A CN 99107783 A CN99107783 A CN 99107783A CN 1112337 C CN1112337 C CN 1112337C
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Abstract
The present invention relates to a preparation method of silicon nitride basing composite materials with superhigh toughness. A used basal body comprises a basal body Si3N4, combustion improver and toughener; an interface layer is BN; materials matched with the basal body are weighed according to the recipe of the basal body; mixed powder materials are obtained after ball milling; a polyvinyl alcohol solution is prepared; a polyvinyl alcohol water solution as an adhesive is added in the mixed powder materials, liquid paraffin as a lubricant is added in the mixing powder materials, and glycerol as a plasticizing agent is added in the mixing powder material; the interface layer is formed; and then a ceramic blank body after being coated is put in a graphite mould for exhausting glue and sintering, namely that the silicon nitride basing composite material is obtained. The composite material has the advantages of high toughness, high temperature resistance, good mechanical shock resistance, etc.
Description
The present invention relates to a kind of preparation method of silicon nitride-based composite material with superhigh tenacity, belong to materials science field.
Plurality of advantages such as structural ceramic material is high-strength with it, height is hard, high temperature resistant, corrosion-resistant, light weight, be subjected to people's extensive attention and research in recent decades always, obtained certain application at aspects such as heat exchanger, cutting tool, wear parts, sealing elements, used more widely but the fragility of stupalith has but limited it.For this reason, people have proposed many toughness reinforcing methods, as macrofiber is toughness reinforcing, crystal whisker toughened, particle dispersion is toughness reinforcing and transformation toughening etc., though these method for toughening have all been obtained certain toughening effect to some extent, but the fragility of stupalith fundamentally is not resolved.
In recent years, Chinese scholars takes a hint from the structure of natural biomaterial (as pearl, shell, bamboo etc.).These natural biologic materials only pass through the accurate compound of simple component, just can obtain excellent specific properties such as compound complementation, functional adaptation and wound healing.For example bamboo wood is typical macrofiber reinforced composite, and it strengthens the distribution that the body fiber has different yardstick and lift angle, makes its stretch-proof, bending and compressive strength and modulus can bring into play maximum effect in the combination of materials of isodose.Same, in shell pearl layer, the content of aragonite is up to 99%, but by connecting by special laminate structure less than 1% the organic matter aragonite wafer with different size, formed the matrix material of laminate structure, its fracture toughness property but exceeds more than 3000 times than pure aragonite.If with reference to the constructional feature of these biomaterials, when material designed, scientifically the microtexture of control material was expected to prepare the biomimetic features material with good mechanical property.Reported that as people such as the U.S. W.J.Clegg people such as the ceramic layered material of SiC/C, H.Y.Liu have reported Si
3N
4The ceramic layered material of/BN, Baskaran etc. have prepared the stupalith of SiC/C fiber monolithic structure, by these biomimetic features designs, the fracture toughness property and the work of rupture of prepared stupalith all have increased significantly, fracture toughness property can improve several times, and work of rupture can improve tens of times and even hundreds of times.A common characteristic is exactly in the design and preparation of material, has introduced a kind of weak bonded interfacial phase, by the repeatedly deviation of interfacial phase to crackle, improves fracture toughness property and work of rupture.Yet in research in the past, because the introducing of weak interface phase, though improved the toughness and the work of rupture of stupalith significantly, decline has to a certain degree but appearred in its intensity.
The objective of the invention is to propose a kind of preparation method of silicon nitride-based composite material with superhigh tenacity, on the basis of former studies, except introducing the weak interface phase, the whisker and the matrix long column shape crystal grain of strengthening effect also in the matrix ceramic phase, have been introduced, and through technology controlling and process, make whisker and matrix long column shape crystal grain by the certain way oriented alignment, improved the fracture toughness property and the fracture function of material on the one hand significantly, also kept the intensity of matrix stupalith simultaneously.
The used raw material of the present invention is:
Matrix:
Si
3N
4(50～80)％
Sintering agent (10～25) %[(0～10) %La
2O
3+ (0～10) %Y
2O
3+ (0～5) %Al
2O
3+ (0～5) %MgO]
Toughner (0～25) %SiC whisker+(0～10) % β-Si
3N
4Crystal seed
Interfacial layer:
BN(60～90)％
Interface conditioning agent (0～40) %Al
2O
3+ (0～20) %Si
3N
4
The preparation method of silicon nitride-based composite material with superhigh tenacity of the present invention comprises following each step:
(1) by matrix formulation weighing ligand material, putting into ball grinder, is abrading-ball with the agate ball, is medium with alcohol, 24 hours (material: ball: alcohol=1: (1～2): (1.2～2)) of ball mill mixing.Discharging after oven dry about 80 ℃, is crossed 50～100 mesh sieves, obtains the blended powder.
(2) compound concentration is 10～25% polyvinyl alcohol solution: get the polymerization degree and be 10～25 parts of 1400～2000 polyvinyl alcohol, be dissolved in 75～85 parts 80 ℃ the distilled water, and add 4～10% calcium chloride (CaCl
2) as stablizer, after stirring, constant temperature is 8～15 hours in 80 ℃ water-bath.
(3) moulding process: comprise the moulding of matrix lamella and the formation of interfacial layer, the matrix lamella is divided into the base substrate of fiber born of the same parents shape base substrate and laminate structure again.
For the base substrate with fiber cell structure, fibrous green compact obtain by extrusion forming.
The polyvinyl alcohol water solution that adds preparation in (3) in the mixed powder that in (2), obtains as binding agent, add whiteruss as lubricant, add glycerine as softening agent.Add-on is pressed mixed powder: binding agent: lubricant: softening agent=100: (25～75): (1～5): (1～5).Carry out the batch mixing pugging with roll forming machine or vacuum mixer, until obtaining the good plastic walk of plasticity, the walk water ratio is 10～25%.And with walk under sealed state old 12～24 hours.Then plastic walk is put into forcing machine, extrusion moulding, extrusion pressure is 15～50MPa, extrusion diameter 0.3～1.5mm.Hang the thread base substrate of extruding up seasoning.
For the base substrate of rhythmo structure, synusia shape base substrate can obtain by methods such as rolling or curtain coatings, and thickness is 0.03～1mm.
If adopt rolling method, the polyvinyl alcohol water solution that then adds preparation in (3) in the mixed powder that in (2), obtains as binding agent, add whiteruss as lubricant, adding glycerine as softening agent.Add-on is pressed mixed powder: binding agent: lubricant: softening agent=100: (25～75): (1～5): (1～5).Carry out repeat-rolling with roll forming machine, obtain the green compact thin slice of thickness by roughing earlier, pass through finish rolling again, roll into the thin slice of thickness less than 0.08～1mm less than 2mm.
If adopt casting method, then in mixed powder: polyvinyl alcohol solution: dispersion agent: lubricant: softening agent: distilled water=100: (40～75): (1～2): (1～5): (1～5): the ratio of (30～120), the mixed powder that obtains in (2) is put into ball grinder with poly (vinyl alcohol) binder and dispersion agent, lubricant, softening agent and distilled water, ball mill mixing, obtain slurry even, good fluidity, the viscosity controller of slurry is at 1～100Pas.Curtain coating speed is 0.1～1m/min, and thickness is 0.03～1mm.
By the above method of moulding moulding process, the SiC whisker and the β-Si that in raw material, add in advance
3N
4The column crystal seed forms has aligning of certain orientation degree.
(4) interfacial layer moulding
By (60～90) %BN+ (0～40) %Al
2O
3+ (0～20) %Si
3N
4Ratio, put into ball grinder, in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: (150～200): (20～50): (20～100): the ratio of (10～40), BN is mixed with the interfacial layer conditioning agent, obtain uniform interfacial layer slurry.Adopt the BN interfacial layer of methods such as spraying, dip-coating or silk screen printing at fiber born of the same parents shape or lamellated ceramic body surface-coated (0.01～0.1) mm thickness.
Then that the ceramic body after the coating is parallel, lamination or arrange by certain mode is put into graphite jig.
(5) binder removal and sintering
To arrange good ceramic body under air atmosphere, heat up at a slow speed earlier (＜5 ℃/minute) be incubateds 2～4 hours and carry out the binder removal processing to 300～400 ℃, treat that organism drains fully after, the pressure that applies 5～10MPa is colded pressing.Place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is (5～20) ℃/min, and sintering temperature is 1600～1850 ℃, soaking time 1～2 hour, and in sintering process, apply the pressure of 15～40MPa, be nitride silicon based composite material of the present invention.
By the reality of biomimetic features and above-mentioned preparation technology, prepare SiCw-Si respectively with fiber cell structure
3N
4/ BN matrix material and SiCw-Si with laminate structure
3N
4/ BN matrix material in this two classes material, includes the ceramic matrix phase and the low intensive interfacial phase of high-intensity densification.Wherein low intensive interfacial phase forms a large amount of mechanics weak interfaces in stupalith, can carry out repeatedly deviation, make the crack tip passivation, cause the bridge joint of the fine and close relative crackle of ceramic matrix and extract etc. crackle in stupalith stressed when cracking, thereby reduce stupalith greatly to the susceptibility of crackle and improve toughness.Simultaneously the high strength matrix mutually in introducing whisker, bridge joint that long column shape crystal grain plays whisker again, extract, the bridge joint of long column shape crystal grain, extract, pinning and to the multiple toughening mechanisms such as deflection of crackle, thereby formed the coordination plasticizing effect of the multistage toughening mechanisms of different scale, thereby improved the mechanical property of described stupalith significantly.Prepared this two class matrix materials all have mechanical property preferably: fracture toughness property＞20MPa.m
1/2, intensity is 500～700MPa, work of rupture＞4000J/m
2, and the load-displacement curve of material demonstrates non-brittle destructive characteristic.
The prepared biomimetic features matrix material of the present invention has high tenacity, high temperature resistant, good advantages such as mechanical shock resistance, can be used for the surfacing of parts such as space shuttle, plate armour, transport pipe and the material of some structure component, have boundless application prospect.
Introduce embodiments of the invention below:
Embodiment one:
The body material formulation selection is 85%Si
3N
4+ 8%Y
2O
3+ 2.5%Al
2O
3+ 1.5%MgO+3% β-Si
3N
4Crystal seed.The interfacial layer formulation selection is 80%BN+20%Al
2O
3With the matrix material weighing, putting into ball grinder earlier, is abrading-ball with the agate ball, is medium with alcohol, 24 hours (material: ball: alcohol=1: 2: 1.5) of ball mill mixing.Discharging after oven dry about 80 ℃, is crossed 100 mesh sieves, obtains the blended powder.Get the polymerization degree and be 20 parts of 1788 polyvinyl alcohol, be dissolved in 80 parts 80 ℃ the distilled water, and add 7% calcium chloride (CaCl
2) as stablizer, after stirring, constant temperature is 10 hours in 80 ℃ water-bath.In mixed powder: binding agent: lubricant: softening agent=100: 40: 3: 3 ratio joins binding agent, lubricant and softening agent in the mixed powder, carry out the batch mixing pugging with roll forming machine, until obtaining the good plastic walk of plasticity, the walk water ratio is 20%.And with walk under sealed state old 24 hours.Then plastic walk is put into forcing machine, extrusion moulding, extrusion pressure is 20MPa, extrusion diameter 0.3mm.Hang the thread base substrate of extruding up seasoning.The interfacial layer raw material is put into ball grinder by above-mentioned prescription, and in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: 150: 30: 80: 20 ratio is carried out batch mixing, obtains uniform interfacial layer slurry.Adopt the BN interfacial layer of the method for dip-coating at base substrate fiber surface coating 0.03mm thickness.Then the ceramic body after the coating is arranged in parallel, puts into graphite jig.To arrange good ceramic body under air atmosphere, the speed with 2 ℃/min is warming up to 320 ℃ at a slow speed earlier, be incubated 4 hours and carry out binder removal to handle, treat that organism drains fully after, the pressure that applies 8MPa is colded pressing.Place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is 10 ℃/min, and sintering temperature is 1800 ℃, soaking time 1.5 hours, and in sintering process, apply the pressure of 22MPa.Contain β-Si thereby prepare
3N
4The Si of crystal seed
3N
4The matrix material of/BN fiber cell structure presents to a certain degree oriented alignment by the formed long column shape crystal grain of crystal seed along fiber direction.Through measuring, its bending strength is 530MPa, and fracture toughness property is 17.2MPam
1/2, work of rupture is 4000J/m
2, its load one inflection curves presents non-linear destructive characteristic.
Embodiment two:
The body material formulation selection is 60%Si
3N
4+ 11.3%La
2O
3+ 7.8%Y
2O
3+ 0.9%Al
2O
3+ 20%SiC whisker.The interfacial layer formulation selection is 85%BN+15%Si
3N
4With the matrix material weighing, putting into ball grinder earlier, is abrading-ball with the agate ball, is medium with alcohol, 24 hours (material: ball: alcohol=1: 2: 1.8) of ball mill mixing.Discharging after oven dry about 80 ℃, is crossed 60 mesh sieves, obtains the blended powder.Get the polymerization degree and be 18 parts of 1650 polyvinyl alcohol, be dissolved in 82 parts 80 ℃ the distilled water, and add 6% calcium chloride (CaCl
2) as stablizer, after stirring, constant temperature is 12 hours in 80 ℃ water-bath, obtains concentration and be 18% polyvinyl alcohol solution.In mixed powder: binding agent: lubricant: softening agent=100: 45: 3: 3 ratio joins binding agent, lubricant and softening agent in the mixed powder, carry out the batch mixing pugging with roll forming machine, until obtaining the good plastic walk of plasticity, the walk water ratio is 21.5%.And with walk under sealed state old 12 hours.Then plastic walk is put into forcing machine, extrusion moulding, extrusion pressure is 14MPa, extrusion diameter 0.5mm.Hang the thread base substrate of extruding up seasoning.The interfacial layer raw material is put into ball grinder by above-mentioned prescription, and in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: 120: 30: 90: 30 ratio is carried out batch mixing, obtains uniform interfacial layer slurry.Adopt the BN interfacial layer of the method for dip-coating at base substrate fiber surface coating 0.025mm thickness.Then the ceramic body after the coating is arranged in parallel, puts into graphite jig.To arrange good ceramic body under air atmosphere, the speed with 3 ℃/min is warming up to 350 ℃ at a slow speed earlier, be incubated 2 hours and carry out binder removal to handle, treat that organism drains fully after, the pressure that applies 10MPa is colded pressing.Place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is 10 ℃/min, and sintering temperature is 1820 ℃, soaking time 1.5 hours, and in sintering process, apply the pressure of 20MPa.Thereby prepare the Si that contains the SiC whisker
3N
4The matrix material of-SiCw/BN fiber cell structure, and whisker presents oriented alignment preferably along fiber direction.Through measuring, its bending strength is 705MPa, and fracture toughness property is 20MPam
1/2, work of rupture is 4400J/m
2, its load one inflection curves presents non-linear destructive characteristic.
Embodiment three:
The body material formulation selection is 75%Si
3N
4+ 11.3%La
2O
3+ 7.8%Y
2O
3+ 0.9%Al
2O
3+ 15%SiC whisker.The interfacial layer formulation selection is 75%BN+25%Al
2O
3With the matrix material weighing, putting into ball grinder earlier, is abrading-ball with the agate ball, is medium with alcohol, 24 hours (material: ball: alcohol=1: 2: 1.5) of ball mill mixing.Discharging after oven dry about 80 ℃, is crossed 80 mesh sieves, obtains the blended powder.Get the polymerization degree and be 20 parts of 1800 polyvinyl alcohol, be dissolved in 80 parts 80 ℃ the distilled water, and add 9% calcium chloride (CaCl
2) as stablizer, after stirring, constant temperature is 8 hours in 80 ℃ water-bath, obtains concentration and be 20% polyvinyl alcohol solution.In mixed powder: binding agent: lubricant: softening agent=100: 35: 3: 1 ratio joins binding agent, lubricant and softening agent in the mixed powder, carry out repeat-rolling with roll forming machine, earlier obtain the green compact thin slice that thickness is 0.8mm by roughing, pass through finish rolling again, roll into the thin slice of thickness, seasoning less than 0.15mm.The interfacial layer raw material is put into ball grinder by above-mentioned prescription, and in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: 120: 40: 80: 25 ratio is carried out batch mixing, obtains uniform interfacial layer slurry.Adopt the BN interfacial layer of the method for spraying at base substrate fiber surface coating 0.04mm thickness.With the ceramic body stacked arrangement after the coating, put into graphite jig then.To arrange good ceramic body under air atmosphere, the speed with 3 ℃/min is warming up to 380 ℃ at a slow speed earlier, be incubated 2.5 hours and carry out binder removal to handle, treat that organism drains fully after, the pressure that applies 12MPa is colded pressing.Place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is 10 ℃/min, and sintering temperature is 1780 ℃, soaking time 1 hour, and in sintering process, apply the pressure of 25MPa.Thereby prepare the Si that contains the SiC whisker
3N
4The matrix material of-SiCw/BN laminate structure, whisker presents one dimension oriented alignment preferably in the synusia direction.Through measuring, its bending strength is 740MPa, and fracture toughness property is 28.4 MPa.m
1/2, work of rupture is 5700J/m
2, its load-deformation curve presents non-linear destructive characteristic.
Embodiment four:
The body material formulation selection is 67%Si
3N
4+ 10%Y
20
3+ 3%MgO+20%SiC whisker.The interfacial layer formulation selection is 90%BN+10%Si
3N
4With the matrix material weighing, putting into ball grinder earlier, is abrading-ball with the agate ball, is medium with alcohol, 24 hours (material: ball: alcohol=1: 1.5: 1.2) of ball mill mixing.Discharging after oven dry about 80 ℃, is crossed 60 mesh sieves, obtains the blended powder.Get the polymerization degree and be 15 parts of 1700 polyvinyl alcohol, be dissolved in 85 parts 80 ℃ the distilled water, and add 6% calcium chloride (CaCl
2) as stablizer, after stirring, constant temperature is 15 hours in 80 ℃ water-bath, obtains concentration and be 15% polyvinyl alcohol solution.In mixed powder: polyvinyl alcohol solution: dispersion agent: lubricant: softening agent: distilled water=100: 55: 1: 3: 2: 80 ratio, mixed powder is put into ball grinder with tackiness agent, dispersion agent, lubricant, softening agent and distilled water, ball mill mixing, obtain even, mobile slurry, the viscosity controller of slurry is at 0.5Pas.Under the curtain coating speed of 1m/min, curtain coating goes out the matrix lamella that thickness is 0.09mm, seasoning.The interfacial layer raw material is put into ball grinder by above-mentioned prescription, and in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: 150: 30: 75: 30 ratio is carried out batch mixing, obtains uniform interfacial layer slurry.Adopt the BN interfacial layer of the method for dip-coating at base substrate fiber surface coating 0.03mm thickness.With the ceramic body stacked arrangement after the coating, put into graphite jig then.To arrange good ceramic body under air atmosphere, the speed with 2 ℃/min is warming up to 350 ℃ at a slow speed earlier, be incubated 3 hours and carry out binder removal to handle, treat that organism drains fully after, the pressure that applies 15MPa is colded pressing.Place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is l0 ℃/min, and sintering temperature is 1800 ℃, soaking time 1.5 hours, and in sintering process, apply the pressure of 25MPa.Thereby prepare the Si that contains the SiC whisker
3N
4The matrix material of-SiCw/BN laminate structure, whisker presents one dimension oriented alignment preferably in the synusia direction.Through measuring, its bending strength is 710MPa, and fracture toughness property is 29MPam
1/2, work of rupture is 6500J/m
2, its load-deformation curve presents non-linear destructive characteristic.
Claims (1)
1, a kind of preparation method of silicon nitride-based composite material with superhigh tenacity is characterized in that, this preparation method comprises following each step:
(1) by matrix formulation weighing ligand material, the proportioning of matrix is:
Si
3N
4(50～80)％
Sintering agent (10～25) %[(0～10) %La
2O
3+ (0～10) %Y
2O
3+ (0～5) %Al
2O
3+ (0～5) %MgO]
Toughner (0～25) %SiC whisker+(0～10) % β-Si
3N
4Crystal seed
Putting into ball grinder, is abrading-ball with the agate ball, is medium with alcohol, ball mill mixing 20～26 hours, and its ratio is: material: ball: alcohol=1: (1～2): (1.2～2), discharging after oven dry about 80 ℃, is crossed 50～100 mesh sieves, obtains the blended powder;
(2) preparation 10～25% polyvinyl alcohol solution: get the polymerization degree and be 10～25 parts of 1400～2000 polyvinyl alcohol, be dissolved in 75～85 parts 80 ℃ the distilled water, and add 4～10% calcium chloride as stablizer, after stirring, constant temperature is 8～15 hours in 80 ℃ water-bath;
(3) in the mixed powder that the above-mentioned the first step obtains, add the polyvinyl alcohol water solution of above-mentioned second step preparation as binding agent, add whiteruss as lubricant, add glycerine as softening agent, add-on is pressed mixed powder: binding agent: lubricant: softening agent=100: (25～75): (1～5): (1～5), carry out the batch mixing pugging with roll forming machine or vacuum mixer, until obtaining the good plastic walk of plasticity, the walk water ratio is 10～25%, and with walk under sealed state old 12～24 hours, then plastic walk is put into forcing machine, extrusion moulding, extrusion pressure is 15～50MPa, extrusion diameter 0.3～1.5mm, hang the thread base substrate of extruding up seasoning;
Or adopt rolling method adds above-mentioned second step preparation in the mixed powder that the above-mentioned the first step obtains polyvinyl alcohol water solution as binding agent, add whiteruss as lubricant, add glycerine as softening agent.Add-on is pressed mixed powder: binding agent: lubricant: softening agent=100: (25～75): (1～5): (1～5), carry out repeat-rolling with roll forming machine, earlier obtain the green compact thin slice of thickness, pass through finish rolling again, roll into the thin slice of thickness less than 0.08～1mm less than 2mm by roughing;
(4) interfacial layer moulding
By (60～90) %BN+ (0～40) %Al
2O
3+ (0～20) %Si
3N
4Ratio, put into ball grinder, in expecting: ball: alcohol: distilled water: polyvinyl alcohol solution=100: (150～200): (20～50): (20～100): the ratio of (10～40), BN is mixed with the interfacial layer conditioning agent, obtain uniform interfacial layer slurry, adopt spraying, dip-coating or method for printing screen at the fiber born of the same parents shape of above-mentioned the 3rd step acquisition or the BN interfacial layer of lamellated ceramic body surface-coated (0.01～0.1) mm thickness; Then the ceramic body after the coating is put into graphite jig;
(5) binder removal and sintering
To arrange good ceramic body under air atmosphere, speed with 2～5 ℃ of per minutes is warming up to 300～400 ℃ earlier, be incubated 2～4 hours and carry out the binder removal processing, after treating that organism drains fully, the pressure that applies 5～10MPa is colded pressing, place the hot-pressed sintering furnace hot pressed sintering of nitrogen atmosphere afterwards, temperature rise rate is 5～20 ℃/minute, sintering temperature is 1600～1850 ℃, soaking time 1～2 hour, and in sintering process, apply the pressure of 15～40MPa, be silicon nitride-based composite material with superhigh tenacity of the present invention.
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| CN99107783A CN1112337C (en) | 1999-05-28 | 1999-05-28 | Preparation of silicon nitride-based composite material with superhigh tenacity |
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|---|---|---|---|
| CN99107783A CN1112337C (en) | 1999-05-28 | 1999-05-28 | Preparation of silicon nitride-based composite material with superhigh tenacity |
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| CN1232805A (en) | 1999-10-27 |
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