CN107021785B - 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 present invention provides a kind of ultra-toughness layered polymer-ceramic composites and preparation method thereof.This method comprises: 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, is heated up, room temperature is down in heat preservation, 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.The present invention also provides ultra-toughness layered polymer-ceramic composites that above-mentioned preparation method obtains.
Description
Technical field
The present invention relates to a kind of composite material and preparation method more particularly to a kind of stratiform polymerizations with ultra-tough
Object-ceramic composite and preparation method thereof, belongs to technical field of material.
Background technique
The engineering material that ceramic material is high as intensity, hardness is big, wearability is good, good corrosion resistance, performance are stable, is navigating
The fields such as empty space flight, mechano-electronic, engineering in medicine play highly important role.But the prominent disadvantage of one be exactly be broken it is tough
Property is very low, i.e., very sensitive to micro-crack and microdefect, this seriously constrains it in the application of engineering field.
The preparation method of existing ceramic matric composite has:
1, continuous fiber and sintered matrix material powder are made with impregnation technology for sluny impregnation and hot pressing sintering method
Green body, then heat-agglomerating at high temperature, make fiber and basis material be combined into composite material.But this method is in process operation mistake
Cheng Zhong, fiber are easy to be damaged and destroy, and sintering will lead to ceramic matrix contraction, so that agglomerated material is also easy to produce defect
Or internal stress.
2, direct oxidation sedimentation, directly occurs oxidation reaction with oxidant using molten metal and to prepare ceramic base compound
The process of material.The shortcomings that this method is that residual metal is difficult to be oxidized or remove completely, and is difficult to complex component.
3, sol-gel method, i.e., the sol impregnation fiber preform being made of organic precursor method, then hydrolysis, polycondensation, shape
At gel, gel forms composite material after drying and pyrolysis.Composite material compactness made of this method is poor, and it is non-to be not suitable for part
The preparation of oxide ceramics based composites.
4, polymer precursor pyrolysismethod is that macromolecule precursor occurs after pioneer is body formed with high molecular polymer
Pyrolytic reaction is converted into inorganic substances, is then prepared into ceramic matric composite through high temperature sintering again.The shortcomings that this method is to burn
Biggish contraction can be generated when knot, yield is lower.
Summary of the invention
In order to solve the above-mentioned technical problem, the problems such as overcoming fracture toughness present in existing ceramic material low, the present invention
The layered polymer-ceramic composite preparation method for being designed to provide a kind of ultra-tough.
In order to achieve the above technical purposes, the present invention provides a kind of systems of ultra-toughness layered polymer-ceramic composite
Preparation Method, ultra-toughness layered polymer-ceramic composite preparation method the following steps are included:
Step 1: by Al2O3Ceramic slurry is made in ceramic powders, water mixing, ball milling 12h-16h (preferably 12h)；Wherein,
Al2O3The mixing mass ratio of ceramic powders and water is 15%-20%:80%-85% (preferably 20%:80%), with Al2O3Ceramics
The gross mass of powder is 100wt% meter, the Al2O3Ceramic powders include the citric acid of 1wt%-2wt% (preferably 1wt%)
Sodium, 1wt%-2wt% (preferably 1wt%) polyvinyl alcohol (PVA) and surplus Al2O3Nanometer 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 at 50 DEG C to -60 DEG C, 10Pa-50Pa (preferably -54 DEG C, 10Pa) and is done
It is dry, the ceramic green with stratiform hole is made；
Step 4: the 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), keep the temperature 4h-6h (preferably 4h), then with 5 DEG C/min-10 DEG C/
The speed of min (preferably 5 DEG C/min) is down to room temperature (25 DEG C), and fine and close stratiform hole ceramic body is made；
Step 5: being added in the stratiform hole ceramic body of Xiang Zhimi and Al2O3The mixed-powder of the quality such as ceramic powders, with
The gross mass of the mixed-powder is 100wt% meter, and the mixed-powder includes the azodiisobutyronitrile of 1wt%-2wt%
(AIBN) and the methyl methacrylate of surplus (MMA), 30min-40min is heated (preferably in 75 DEG C -80 DEG C of water-bath
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 of ultra-toughness layered polymer-ceramic composite provided by the invention, the Al of use2O3Nano powder
End is industrial Al2O3Nanometer powder.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 1,
Ball milling carries out in the ball mill.
In ultra-toughness layered polymer-ceramic composite preparation method of the invention, sodium citrate as dispersing agent,
Polyvinyl alcohol (PVA) is used as binder.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, in step 2, ceramic slurry
Material carries out vacuum degassing in vacuum degassing instrument.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 2
In, is carried out for 30min-60min the vacuum degassed time to ceramic slurry；It is highly preferred that carrying out vacuum degassing to ceramic slurry
Time be 30min.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 2
In, the compulsive means of directional solidification are as follows:
The ceramic slurry after vacuum degassing is cooled to -20 DEG C from room temperature (20 DEG C -30 DEG C) with the rate of 6-10 DEG C/min
To -30 DEG C (more preferably -30 DEG C), 5min-10min is kept the temperature.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, in step 2, use is cold
Freeze foundry engieering and is oriented solidification.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 3
In, it is freeze-dried after ceramic body is demoulded.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, in step 3, by ceramic blank
It is freeze-dried in freeze drier after body demoulding.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 3
In, the time of freeze-drying is -36h for 24 hours；It is highly preferred that the time of freeze-drying is for 24 hours.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, in step 4, there is layer
The ceramic green in shape hole is sintered in Muffle furnace.
In the preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, it is preferable that in step 5
In, 5min-10min is placed after polymer is cooled to 40 DEG C -45 DEG C carries out next step again.
It the present invention also provides a kind of ultra-toughness layered polymer-ceramic composite, is gathered by above-mentioned ultra-toughness stratiform
Close what object-ceramic composite preparation method was prepared.
The preparation method of ultra-toughness layered polymer-ceramic composite provided by the invention, specific preparation step include:
Mixing: by Al2O3Nanometer powder, sodium citrate, PVA and water mixing, ball milling 12h-16h, is made pottery in the ball mill
Porcelain slurry；Al2O3The mixing mass ratio of ceramic powders and water is 15%-20%:80%-85%, with Al2O3Ceramic powders it is total
Quality is 100wt% meter, the Al2O3Ceramic powders include the polyethylene of the sodium citrate of 1wt%-2wt%, 1wt%-2wt%
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 the rate of 6-10 DEG C/min-
20 DEG C to -30 DEG C, keep the temperature 5min-10min), ceramic body is made；
Distillation: after ceramic body is demoulded, being put into freeze drier, -50 DEG C to -60 DEG C, it is (under 10Pa-50Pa cold
Dry -36h for 24 hours is lyophilized, the ceramic green with stratiform hole is made；
Sintering: the ceramic green with stratiform hole is put into Muffle furnace, is sintered in nitrogen, with 5 DEG C/min-10 DEG C/
The speed of min is warming up to 1600 DEG C -1700 DEG C, keeps the temperature 4h-6h, then with the speed of 5 DEG C/min-10 DEG C/min, be 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, addition and Al2O3Ceramic powders
Etc. quality mixed-powder, by the gross mass of mixed-powder for 100wt% in terms of, mixed-powder includes the azo of 1wt%-2wt%
Bis-isobutyronitrile (AIBN) and the methyl methacrylate (MMA) of surplus are uniformly mixed, and are then sealed with rubber band and preservative film, are used
The bottleneck of the fixed conical flask of test tube clamp, is put into water-bath, heats in 75 DEG C -80 DEG C of water-bath, while being shaked gently 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: uses 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, removes conical flask finally to get ultra-toughness layered polymer-ceramics (Al2O3/ PMMA) composite material.
It ultra-toughness layered polymer-ceramic composite preparation method of the invention and is prepared by this method super
Tough layered polymer-ceramic composite has the advantage that
Ultra-toughness layered polymer-ceramic composite of the invention has high tenacity；
In ultra-toughness layered polymer-ceramic composite preparation method of the invention, the ceramic slurry that is prepared
The distillation of solvent can be shunk and stress and potential fracture when normal dry due to dry to avoid green compact；
Ultra-toughness layered polymer-ceramic composite preparation method environmental sound of the 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 has more excellent
Mechanical performance；
Ultra-toughness layered polymer-ceramic composite of the invention has good shock resistance and wear resistance,
Improve the brittleness of ceramic matrix.
Detailed description of the invention
Fig. 1 is the SEM figure under ultra-toughness layered polymer -200 μm of ceramic composite of embodiment 1.
Fig. 2 is the SEM figure under ultra-toughness layered polymer -20 μm of ceramic composite that Fig. 1 is embodiment 1.
Fig. 3 is the SEM figure under ultra-toughness layered polymer -8 μm of ceramic composite that Fig. 1 is embodiment 1.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
Embodiment 1
A kind of ultra-toughness layered polymer-ceramic composite is present embodiments provided, through the following steps that being prepared into
It arrives:
Mixing: by Al2O3Nanometer powder, sodium citrate, PVA and water mixing, by Al2O3Ceramic powders, water mixing, ball milling
Ceramic slurry is made in 12h；Wherein, Al2O3The mixing mass ratio of ceramic powders and water is 15%-20%:80%-85%, with
Al2O3The gross mass of ceramic powders is 100wt% meter, the Al2O3Ceramic powders include 1wt%-2wt% sodium citrate,
The polyvinyl alcohol of 1wt%-2wt% and the Al of surplus2O3Nanometer powder；Freezing: by mixed ceramic slurry in vacuum degassing instrument
Vacuum degassing 30min, using freezing casting technology, by ceramic slurry -30 DEG C at a temperature of be oriented solidification, ceramics are made
Green body；
Distillation: after ceramic body is moved back mould, being put into freeze drier, is freeze-dried for 24 hours, is made at -54 DEG C, 10Pa
Ceramic green with stratiform hole；
Sintering: the ceramic green with stratiform hole is put into Muffle furnace, is sintered in nitrogen, with the speed of 5 DEG C/min
1600 DEG C are warming up to, keeps the temperature 4h, then room temperature is down to the speed of 5 DEG C/min, fine and close stratiform hole ceramic body is made；
Polymerization:
(1) prepolymerization: fine and close stratiform hole ceramic body is put into conical flask, is added and Al2O3The matter such as ceramic powders
The mixed-powder of amount, wherein by the gross mass of the mixed-powder for 100wt% in terms of, the mixed-powder includes 1wt%-
The azodiisobutyronitrile of 2wt% and the methyl methacrylate of surplus are uniformly mixed, and are then sealed, are used with rubber band and preservative film
The bottleneck of the fixed conical flask of test tube clamp, is put into water-bath, heats in 75 DEG C -80 DEG C of water-bath, while being shaked gently 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 completely, completes polymerization, removes conical flask finally to get layered polymer-ceramics
(Al2O3/ PMMA) composite material.
Ultra-toughness layered polymer-ceramics (Al that the present embodiment is obtained2O3/ PMMA) composite material carry out SEM scanning
(as shown in Figure 1, Figure 2 and Figure 3, wherein the scale of Fig. 1 is 200 μm, and the scale of Fig. 2 is 20 μm, and the scale of Fig. 3 is 8 μm) is from figure
1, 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
Phase-polymerization object PMMA interface cohesion is good.
Ultra-toughness layered polymer-ceramics (Al that the present embodiment is obtained2O3/ PMMA) composite material progress fracture toughness survey
Examination, test result are as shown in table 1.
It reads up the literature it is found that Al2O3The fracture toughness of ceramics is 3-5MPam1/2, the fracture toughness of polymer P MMA is 0.7-
1.6MPa·m1/2, and the fracture toughness of metal Al is 14-28MPam1/2.The layered polymer of acquisition-ceramics (Al2O3/
PMMA) fracture toughness of composite material and metal Al are close, about matrix Al2O34 times, 16 times of reinforced phase PMMA of ceramics.Therefore
Stratiform Al obtained2O3/ PMMA composite material has excellent fracture toughness, significantly improves the brittleness of ceramic material.
The different initial solid concentration stratiform Al of table 12O3The fracture toughness of/PMMA composite material
Above embodiments illustrate what the layered polymer of ultra-toughness through the invention-ceramic composite preparation method obtained
Layered polymer-ceramic composite has high tenacity, and morphology controllable, has excellent fracture toughness, significantly improves
The brittleness of ceramic material.
Claims (12)
1. a kind of preparation method of ultra-toughness layered polymer-ceramic composite, which is characterized in that the ultra-toughness layered polymer-
The preparation method of ceramic composite the following steps are included:
Step 1: by Al2O3Ceramic slurry is made in ceramic powders, water mixing, ball milling 12h-16h；Wherein, Al2O3Ceramic powders and
The mixing mass ratio of water is 15%-20%:80%-85%, with Al2O3The gross mass of ceramic powders is 100wt% meter, described
Al2O3Ceramic powders include the Al of the sodium citrate of 1wt%-2wt%, the polyvinyl alcohol of 1wt%-2wt% and surplus2O3Nanometer
Powder；
Step 2: vacuum degassing is carried out to the ceramic slurry, is oriented solidification, ceramic body is made；
The ceramic body: being freeze-dried by step 3 at -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 kept the temperature, then room temperature is down to the speed of 5 DEG C/min-10 DEG C/min, fine and close stratiform hole pottery is made
Porcelain billet body；
Step 5: being added in the stratiform hole ceramic body of Xiang Zhimi and Al2O3The mixed-powder of the quality such as ceramic powders, 75 DEG C-
30min-40min is heated in 80 DEG C of water-bath, obtains polymer；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% meter, and the mixed-powder includes the azodiisobutyronitrile of 1wt%-2wt% and remaining
The methyl methacrylate of amount.
2. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that institute
It states in step 1, ball milling carries out in the ball mill.
3. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that institute
It states in step 1, Al2O3The mixing mass ratio of ceramic powders and water is 20%:80%.
4. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that with
Al2O3The gross mass of ceramic powders is 100wt% meter, the Al2O3Ceramic powders include 1wt% sodium citrate, 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, which is characterized in that
In the step 2, is carried out for 30min-60min the vacuum degassed time to the ceramic slurry.
6. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 5, which is characterized in that
In the step 2, is carried out for 30min the vacuum degassed time to the ceramic slurry.
7. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that
In the step 2, the compulsive means of directional solidification are as follows:
The ceramic slurry after vacuum degassing is cooled to -20 DEG C to -30 DEG C with the rate of 6-10 DEG C/min, keeps the temperature 5min-
10min。
8. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that
In the step 3, it will be freeze-dried after ceramic body demoulding.
9. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1 or claim 7, which is characterized in that
In the step 3, the time of freeze-drying is -36h for 24 hours.
10. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 9, which is characterized in that
In the step 3, the time of freeze-drying is for 24 hours.
11. the preparation method of ultra-toughness layered polymer-ceramic composite according to claim 1, which is characterized in that
In the step 5,5min-10min is placed after the polymer is cooled to 40 DEG C -45 DEG C.
12. a kind of ultra-toughness layered polymer-ceramic composite, which is characterized in that the ultra-toughness layered polymer-Ceramic Composite material
Material is prepared by the preparation method of the described in any item ultra-toughness layered polymer-ceramic composites of claim 1-11
's.
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| CN108329044A (en) * | 2018-03-22 | 2018-07-27 | 佛山市熙华科技有限公司 | A kind of preparation method of light-weight environment-friendly composite bionic material |
| CN108409350A (en) * | 2018-03-28 | 2018-08-17 | 苏州凌科特新材料有限公司 | A kind of preparation method of light high performance laminar composite |
| CN108585910A (en) * | 2018-04-03 | 2018-09-28 | 苏州凌科特新材料有限公司 | A kind of preparation method of toughening cutter material |
| CN108642316A (en) * | 2018-05-22 | 2018-10-12 | 新沂市中诺新材料科技有限公司 | A kind of Al-Mg/SiC composite materials |
| CN108743405B (en) * | 2018-06-14 | 2021-03-26 | 中国科学院金属研究所 | Zirconia/resin bionic composite material for false tooth and preparation method thereof |
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| CN108994300B (en) * | 2018-07-03 | 2021-03-26 | 中国科学院金属研究所 | Carbon/metal composite material with micro-oriented structure for electric contact and preparation method thereof |
| CN108994301B (en) * | 2018-07-03 | 2021-03-26 | 中国科学院金属研究所 | Metal-based bionic composite material reinforced by nano carbon material and preparation method thereof |
| CN109482885B (en) * | 2018-10-22 | 2021-05-18 | 中国科学院金属研究所 | Copper-based contact material with micro-oriented structure and preparation method thereof |
-
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Non-Patent Citations (3)
| Title |
|---|
| Designing highly toughened hybrid composites through nature-inspired hierarchical complexity;M.E. Launey等;《Acta Materialia》;20090406;第57卷;第2919–2932页 |
| Thermal conductivity of tunable lamellar aluminum oxide/polymethyl methacrylate hybrid composites;Ran Chen等;《J. Mater. Res.》;20120728;第27卷(第14期);第1869-1876页 |
| Tough, Bio-Inspired Hybrid Materials;E. Munch等;《Science》;20081205;第322卷;第1516-1520页 |
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