CN107021785A - A kind of ultra-toughness layered polymer ceramic composite and preparation method thereof - Google Patents
A kind of ultra-toughness layered polymer ceramic composite and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of ultra-toughness layered polymer ceramic composite and preparation method thereof.This method includes：By Al2O3Ceramic slurry is made in ceramic powders, water mixing, ball milling；Vacuum degassing is carried out to ceramic slurry, ceramic slurry is oriented solidification, ceramic body is made；Ceramic body is freeze-dried, the ceramic green with stratiform hole is made；Ceramic green with stratiform hole is sintered in nitrogen, heated up, room temperature is down in insulation, and fine and close stratiform hole ceramic body is made；Methyl methacrylate and azodiisobutyronitrile are added into fine and close stratiform hole ceramic body, heats in a water bath, obtains polymer；Polymer cooling is reacted, layered polymer ceramic composite is obtained.Present invention also offers the ultra-toughness layered polymer ceramic composite that above-mentioned preparation method is obtained.
Description
Technical field
The present invention relates to a kind of composite and preparation method thereof, more particularly to a kind of stratiform polymerization with ultra-tough
Thing-ceramic composite and preparation method thereof, belongs to technical field of material.
Background technology
Ceramic material is as the engineering material that intensity is high, hardness is big, wearability is good, good corrosion resistance, performance are stable, in boat
The fields such as empty space flight, mechano-electronic, engineering in medicine play highly important role.But one protrude shortcoming be exactly be broken it is tough
Property is very low, i.e., very sensitive to micro-crack and microdefect, this seriously constrains its application in engineering field.
The preparation method of existing ceramic matric composite has：
1st, sluny impregnation and hot pressing sintering method, continuous fiber and sintered matrix material powder are made with impregnation technology
Base substrate, then heat-agglomerating at high temperature, make fiber and matrix material be combined into composite.But this method is in process operation mistake
Cheng Zhong, fiber easily sustains damage and destroyed, and sintering can cause ceramic matrix to shrink, so that agglomerated material is also easy to produce defect
Or internal stress.
2nd, direct oxidation sedimentation, directly occurs oxidation reaction with oxidant using molten metal and prepares ceramic base and be combined
The process of material.The shortcoming of this method is that residual metal is difficult completely oxidized or removed, and is difficult to complex component.
3rd, sol-gel process, i.e., the sol impregnation fiber preform being made of organic precursor method, then hydrolysis, polycondensation, shape
Into gel, gel forms composite after drying and pyrolysis.The composite compactness that this method is made is poor, is not suitable for part non-
The preparation of oxide ceramics based composites.
4th, polymer precursor pyrolysismethod, i.e., using high molecular polymer as pioneer it is body formed after make macromolecule precursor occur
Pyrolytic reaction is converted into inorganic substances, is then prepared into ceramic matric composite through high temperature sintering again.The shortcoming of this method is to burn
Larger contraction can be produced during knot, yield is relatively low.
The content of the invention
In order to solve the above-mentioned technical problem, the low problem of fracture toughness present in existing ceramic material is overcome, the present invention
Purpose be the preparation method of layered polymer-ceramic composite that ultra-tough is provided a kind of.
In order to realize above-mentioned technical purpose, the invention provides a kind of system of ultra-toughness layered polymer-ceramic composite
Preparation Method, the preparation method of the ultra-toughness layered polymer-ceramic composite comprises the following steps：
Step one：By Al2O3Ceramic slurry is made in ceramic powders, water mixing, ball milling 12h-16h (preferably 12h)；Wherein,
Al2O3The mixing quality ratio of ceramic powders and water is 15%-20%：80%-85% (preferably 20%：80%), with Al2O3Ceramics
The gross mass of powder is counted for 100wt%, the Al2O3Ceramic powders include the citric acid of 1wt%-2wt% (being preferably 1wt%)
The Al of sodium, 1wt%-2wt% (being preferably 1wt%) polyvinyl alcohol (PVA) and surplus2O3Nanometer powder；
Step 2：Vacuum degassing is carried out to ceramic slurry, ceramic slurry is oriented solidification, ceramic body is made；
Step 3：The ceramic body is freezed under 50 DEG C to -60 DEG C, 10Pa-50Pa (preferably -54 DEG C, 10Pa) and done
It is dry, the ceramic green with stratiform hole is made；
Step 4：Ceramic green with stratiform hole is sintered in nitrogen, with 5 DEG C/min-10 DEG C (preferably 5 DEG C/min)
Speed be warming up to 1600 DEG C -1700 DEG C (preferably 1600 DEG C), insulation 4h-6h (be preferably 4h), then with 5 DEG C/min-10 DEG C/
Min (being preferably 5 DEG C/min) speed is down to room temperature (25 DEG C), and fine and close stratiform hole ceramic body is made；
Step 5：Added and Al into fine and close stratiform hole ceramic body2O3The mixed-powder of the quality such as ceramic powders, with
The gross mass of the mixed-powder is counted for 100wt%, and the mixed-powder includes 1wt%-2wt% azodiisobutyronitrile
(AIBN) and surplus methyl methacrylate (MMA), in 75 DEG C -80 DEG C of water-bath heat 30min-40min (preferably
30min), polymer is obtained；Polymer is cooled to 40 DEG C -45 DEG C, performed polymer is made；Performed polymer reacts at 55 DEG C -60 DEG C
8h-10h (preferably 8h), obtains layered polymer-ceramic composite.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, the Al of use2O3Nano powder
End is industrial Al2O3Nanometer powder.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step one,
Ball milling is carried out in ball mill.
The present invention ultra-toughness layered polymer-ceramic composite preparation method in, sodium citrate as dispersant,
Polyvinyl alcohol (PVA) is used as binding agent.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, in step 2, ceramic slurry
Material carries out vacuum degassing in vacuum degassing instrument.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step 2
In, it is 30min-60min that the vacuum degassed time is carried out to ceramic slurry；It is highly preferred that carrying out vacuum degassing to ceramic slurry
Time be 30min.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step 2
In, the compulsive means of directional solidification are：
The ceramic slurry after vacuum degassing is cooled to -20 DEG C from room temperature (20 DEG C -30 DEG C) with 6-10 DEG C/min speed
To -30 DEG C (more preferably -30 DEG C), 5min-10min is incubated.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, in step 2, using cold
Freeze foundry engieering and be oriented solidification.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step 3
In, it is freeze-dried after ceramic body is stripped.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, in step 3, by ceramic blank
It is freeze-dried after the body demoulding in freeze drier.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step 3
In, the time of freeze-drying is 24h-36h；It is highly preferred that the time of freeze-drying is 24h.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, in step 4, with layer
The ceramic green in shape hole is sintered in Muffle furnace.
In the preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, it is preferable that in step 5
In, polymer is cooled to placement 5min-10min after 40 DEG C -45 DEG C and carries out next step again.
Present invention also offers a kind of ultra-toughness layered polymer-ceramic composite, it is gathered by above-mentioned ultra-toughness stratiform
What the preparation method of compound-ceramic composite was prepared.
The preparation method for ultra-toughness layered polymer-ceramic composite that the present invention is provided, specific preparation process includes：
Batch mixing：By Al2O3Nanometer powder, sodium citrate, PVA and water mixing, the ball milling 12h-16h in ball mill, are made pottery
Porcelain slurry；Al2O3The mixing quality ratio of ceramic powders and water is 15%-20%：80%-85%, with Al2O3Ceramic powders it is total
Quality is counted for 100wt%, the Al2O3Ceramic powders include 1wt%-2wt% sodium citrate, 1wt%-2wt% polyethylene
The Al of alcohol (PVA) and surplus2O3Nanometer powder；
Freezing：By the ceramic slurry mixed in vacuum degassing instrument vacuum degassing 30min-60min, using freezing casting
Technology, by ceramic slurry be oriented solidification (ceramic slurry after vacuum degassing is cooled to 6-10 DEG C/min speed-
20 DEG C to -30 DEG C, it is incubated 5min-10min), ceramic body is made；
Distillation：After ceramic body is stripped, be put into freeze drier, -50 DEG C to -60 DEG C, it is (under 10Pa-50Pa cold
Dry 24h-36h is freezed, the ceramic green with stratiform hole is made；
Sintering：Ceramic green with stratiform hole is put into Muffle furnace, in nitrogen sinter, with 5 DEG C/min-10 DEG C/
Min speed, is warming up to 1600 DEG C -1700 DEG C, is incubated 4h-6h, then with 5 DEG C/min-10 DEG C/min speed, is down to room temperature,
Fine and close stratiform hole ceramic body is made；
Polymerization：(1) prepolymerization：Fine and close stratiform hole ceramic body is put into conical flask, added and Al2O3Ceramic powders
Etc. the mixed-powder of quality, counted by 100wt% of the gross mass of mixed-powder, mixed-powder includes 1wt%-2wt% azo
Bis-isobutyronitrile (AIBN) and the methyl methacrylate (MMA) of surplus are well mixed, are then sealed, used with rubber band and preservative film
Test tube clamp fixes the bottleneck of conical flask, is put into water-bath, is heated in 75 DEG C -80 DEG C of water-bath, while gently rocked with hand,
Pre-polymerization and about 30min-40min are carried out, conical flask is further taken out, takes down rubber band and preservative film, polymer is cooled to 40 DEG C -45
DEG C, it is disposed vertically 5min-10min and drives bubble out of, the performed polymer of ceramic/polymer is made；(2) it polymerize afterwards：With rubber band and guarantor
Conical flask is sealed mouth by fresh film, and then performed polymer is put into baking oven, is reacted 8h-10h at 55 DEG C -60 DEG C, is converted monomer
Completely, polymerization is completed, conical flask is finally removed, produces ultra-toughness layered polymer-ceramics (Al2O3/ PMMA) composite.
It is super that the preparation method of ultra-toughness layered polymer-ceramic composite of the invention and this method that passes through are prepared
Tough layered polymer-ceramic composite has advantages below：
Ultra-toughness layered polymer-ceramic composite of the present invention has high tenacity；
In the preparation method of ultra-toughness layered polymer-ceramic composite of the present invention, the ceramic slurry prepared
The distillation of solvent can avoid green compact potential fracture due to dry contraction and stress in normal dry；
The preparation method environmental sound of ultra-toughness layered polymer-ceramic composite of the present invention, applicable material bodies
System is wide, and additive capacity is few, and the degreasing time of ceramic body is few, the hole morphology controllable of the ceramic body of preparation, and with more excellent
Mechanical performance；
Ultra-toughness layered polymer-ceramic composite of the present invention has good shock resistance and wear resistance,
Improve the fragility of ceramic matrix.
Brief description of the drawings
Fig. 1 is the SEM figures under ultra-toughness layered polymer -200 μm of ceramic composite of embodiment 1.
Fig. 2 is the SEM figures under ultra-toughness layered polymer -20 μm of ceramic composite that Fig. 1 is embodiment 1.
Fig. 3 is the SEM figures under ultra-toughness layered polymer -8 μm of ceramic composite that Fig. 1 is embodiment 1.
Embodiment
In order to which technical characteristic, purpose and beneficial effect to the present invention are more clearly understood from, now to the skill of the present invention
Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of ultra-toughness layered polymer-ceramic composite is present embodiments provided, it is through the following steps that be prepared into
Arrive：
Batch mixing：By Al2O3Nanometer powder, sodium citrate, PVA and water mixing, by Al2O3Ceramic powders, water mixing, ball milling
12h, is made ceramic slurry；Wherein, Al2O3The mixing quality ratio of ceramic powders and water is 15%-20%：80%-85%, with
Al2O3The gross mass of ceramic powders is counted for 100wt%, the Al2O3Sodium citrate of the ceramic powders including 1wt%-2wt%,
1wt%-2wt% polyvinyl alcohol and the Al of surplus2O3Nanometer powder；Freezing：By mixed ceramic slurry in vacuum degassing instrument
Vacuum degassing 30min, using freezing casting technology, ceramic slurry is oriented at a temperature of -30 DEG C solidification, and ceramics are made
Base substrate；
Distillation：Ceramic body is moved back after mould, is put into freeze drier, 24h is freeze-dried under -54 DEG C, 10Pa, is made
Ceramic green with stratiform hole；
Sintering：Ceramic green with stratiform hole is put into Muffle furnace, sintered in nitrogen, with 5 DEG C/min speed
1600 DEG C are warming up to, 4h is incubated, then room temperature is down to 5 DEG C/min speed, fine and close stratiform hole ceramic body is made；
Polymerization：
(1) prepolymerization：Fine and close stratiform hole ceramic body is put into conical flask, added and Al2O3The matter such as ceramic powders
The mixed-powder of amount, wherein, counted using the gross mass of the mixed-powder as 100wt%, the mixed-powder includes 1wt%-
2wt% azodiisobutyronitrile and the methyl methacrylate of surplus are well mixed, are then sealed, used with rubber band and preservative film
Test tube clamp fixes the bottleneck of conical flask, is put into water-bath, is heated in 75 DEG C -80 DEG C of water-bath, while gently rocked with hand,
Pre-polymerization and about 30min are carried out, conical flask is further taken out, takes down rubber band and preservative film, polymer is cooled to 40 DEG C -45 DEG C, is hung down
The straight 5min-10min that places drives bubble out of, and the performed polymer of ceramic/polymer is made；
(2) it polymerize afterwards：Conical flask is sealed into mouth with rubber band and preservative film, then performed polymer is put into baking oven, 55
8h is reacted at DEG C -60 DEG C, makes monomer conversion complete, completes polymerization, finally remove conical flask, produce layered polymer-ceramics
(Al2O3/ PMMA) composite.
Ultra-toughness layered polymer-ceramics (the Al obtained to the present embodiment2O3/ PMMA) composite carry out SEM scanning
(as shown in Figure 1, Figure 2 and Figure 3, wherein, Fig. 1 scale is 200 μm, and Fig. 2 scale is 20 μm, and Fig. 3 scale is 8 μm) is from figure
1st, Fig. 2 and Fig. 3 can be seen that ceramic layer and polymeric layer distributes alternately, and lamellar structure is obvious, matrix alumina interface and enhancing
Gathering compound PMMA interface cohesions are good.
Ultra-toughness layered polymer-ceramics (the Al obtained to the present embodiment2O3/ PMMA) composite progress fracture toughness survey
Examination, test result is as shown in table 1.
Read up the literature and understand, Al2O3The fracture toughness of ceramics is 3-5MPam1/2, polymer P MMA fracture toughness is 0.7-
1.6MPa·m1/2, and metal Al fracture toughness is 14-28MPam1/2.The layered polymer of acquisition-ceramics (Al2O3/
PMMA) fracture toughness of composite and metal Al is approached, about matrix Al2O34 times of ceramics, 16 times of enhancing phase PMMA.Therefore
The stratiform Al obtained2O3/ PMMA composites have excellent fracture toughness, significantly improve the fragility of ceramic material.
The different initial solid concentration stratiform Al of table 12O3The fracture toughness of/PMMA composites
Above example illustrates what is obtained by the preparation method of ultra-toughness layered polymer-ceramic composite of the present invention
Layered polymer-ceramic composite has high tenacity, and morphology controllable, with excellent fracture toughness, significantly improves
The fragility of ceramic material.
Claims (10)
1. a kind of preparation method of ultra-toughness layered polymer-ceramic composite, it is characterised in that the ultra-toughness layered polymer-
The preparation method of ceramic composite comprises the following steps：
Step one：By Al2O3Ceramic slurry is made in ceramic powders, water mixing, ball milling 12h-16h；Wherein, Al2O3Ceramic powders and
The mixing quality ratio of water is 15%-20%：80%-85%, with Al2O3The gross mass of ceramic powders is counted for 100wt%, described
Al2O3Ceramic powders include the Al of 1wt%-2wt% sodium citrate, 1wt%-2wt% polyvinyl alcohol and surplus2O3Nanometer
Powder；
Step 2：Vacuum degassing is carried out to the ceramic slurry, solidification is oriented, ceramic body is made；
Step 3：The ceramic body is freeze-dried under -50 DEG C to -60 DEG C, 10Pa-50Pa, is made with stratiform hole
Ceramic green；
Step 4：The ceramic green with stratiform hole is sintered in nitrogen, is warming up to 5 DEG C/min-10 DEG C of speed
1600 DEG C -1700 DEG C, 4h-6h is incubated, then room temperature is down to 5 DEG C/min-10 DEG C/min speed, fine and close stratiform hole pottery is made
Porcelain base substrate；
Step 5：Added and Al into fine and close stratiform hole ceramic body2O3The mixed-powder of the quality such as ceramic powders, 75 DEG C-
30min-40min is heated in 80 DEG C of water-bath, polymer is obtained；The polymer is cooled to 40 DEG C -45 DEG C, pre-polymerization is made
Body；The performed polymer reacts 8h-10h at 55 DEG C -60 DEG C, obtains layered polymer-ceramic composites；Wherein, with
The gross mass of the mixed-powder is 100wt% meters, the azodiisobutyronitrile of the mixed-powder including 1wt%-2wt% and remaining
The methyl methacrylate of amount.
2. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that institute
State in step one, ball milling is carried out in ball mill.
3. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that institute
State in step one, Al2O3The mixing quality ratio of ceramic powders and water is 20%：80%.
4. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that with
Al2O3The gross mass of ceramic powders is counted for 100wt%, the Al2O3Ceramic powders include 1wt% sodium citrates, 1wt% it is poly-
The Al of vinyl alcohol and surplus2O3Nanometer powder.
5. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that
In the step 2, it is 30min-60min that the vacuum degassed time is carried out to the ceramic slurry；Preferably, to the ceramics
Slurry carries out the vacuum degassed time for 30min.
6. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that
In the step 2, the compulsive means of directional solidification are：
The ceramic slurry after vacuum degassing is cooled to -20 DEG C to -30 DEG C with 6-10 DEG C/min speed, 5min- is incubated
10min。
7. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that
In the step 3, it is freeze-dried after the ceramic body is stripped.
8. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1 or 7, it is characterised in that
In the step 3, the time of freeze-drying is 24h-36h；Preferably, the time of freeze-drying is 24h.
9. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, it is characterised in that
In the step 5,5min-10min is placed after the polymer is cooled into 40 DEG C -45 DEG C.
10. a kind of ultra-toughness layered polymer-ceramic composite, it is characterised in that the ultra-toughness layered polymer-Ceramic Composite material
Material is prepared as the preparation method of ultra-toughness layered polymer-ceramic composite described in claim any one of 1-9.
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