CN107540353A - A kind of preparation method of reinforced alumina ceramic - Google Patents
A kind of preparation method of reinforced alumina ceramic Download PDFInfo
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Abstract
The invention belongs to ceramic materials preparation technology field, more particularly to a kind of preparation method of reinforced alumina ceramic, using the sludge of aluminium section bar plant as being used as silicon source, impurity in sludge is as the first additive, filtered after soda acid is handled and obtain the aluminum precipitation with additive impurity, then aluminum precipitation is added into ethanol water, and adds nanometer aluminium powder and obtain slurries as Second addition, aerated reaction and vacuum distillation；The mode of last microwave reaction carries out slip casting solidification, and sintering obtains reinforced alumina ceramic after solidification.The present invention using the impurity in sludge as flexibilizer additive and stabilizer, not only solves the environmental protection treatment problem of the sludge of aluminium section bar plant, while also reduce the production cost of aluminium oxide ceramics using the sludge of aluminium section bar plant as silicon source.
Description
Technical field
The invention belongs to ceramic materials preparation technology field, and in particular to a kind of preparation method of reinforced alumina ceramic.
Background technology
With the development of science and technology, computer, electronic information, laser, new energy, space flight, ocean and bioengineering etc.
The application in field is also more and more stricter to the performance requirement such as the high temperature resistant of material, corrosion-resistant, wear-resistant.Ceramic material has excellent
High intensity, high rigidity, high-wearing feature and corrosion resistance and the metal material such as low-expansion coefficient and light weight be difficult to the spy being equal to
Point, it is widely used in various materials science fields, also, the exploitation of various crystalline ceramics, cermet, conductivity ceramics etc. should
With so that ceramic material plays more and more important effect, has in fields such as space flight and aviation, electronics, building, biology, medical treatment
The prospect of being widely applied.
Advanced ceramics are the new materials to grow up in recent years on the basis of traditional ceramics.It is main with traditional ceramics
Difference is：Traditional ceramics directly uses natural mineral raw, and product is made by the technique such as cleaning, eluriating, crushing and sintering.
And the research of raw material, the artificial design of component process more of advanced ceramics, the more composition of attention material, microstructure, phasor etc..
Raw material need to carry out purification processing, to material composition, each Phase Proportion and distribution, granularity, purity and doping, additive and life
Production. art etc. has extremely strict requirements, the physical property of advanced ceramics and the phase composition of material point and distribution, microstructure
And preparation technology etc. is closely related.
The species of structural ceramics is various, typically can according to chemical composition be divided into oxide ceramics, carbide ceramics, nitride pottery
Porcelain and boride ceramics etc..Aluminium oxide ceramics category oxide ceramics, and be always ceramic material with its excellent physical and chemical performance
Expect the focus of research.Aluminium oxide ceramics has following fundamental characteristics：
(1) mechanical performance：Sintered alumina ceramics are polycrystalline ceramic materials, and its intensity is mainly influenceed by the Nomenclature Composition and Structure of Complexes.
When not adding special additive, the 94- for the sintered alumina ceramics volume density accessibility theory density that apparent porosity is zero
96%.After with the addition of appropriate sintering aid refinement alpha-alumina crystals, its mechanical strength also strengthens that alumina composition is purer, and intensity is got over
It is high.Intensity can maintain to 900 DEG C at high temperature.
(2) hot property：Linear expansion coefficient of the aluminium oxide ceramics in 20-1000 DEG C of temperature range is 8.5 × 10-6℃-1。
Because crystal transfer is not present in aluminum oxide at high temperature, so its thermal expansion is not raised and changed with temperature.
(3) electrical property：The specific insulation of aluminium oxide ceramics is about 10 under normal temperature14-1016Ω·cm.Specific insulation
Numerical value is relevant with material purity, also relevant with the composition and property of the glass phase in ceramic structure.
(4) chemical stability：The chemical stability of aluminium oxide ceramics is at a relatively high.With aluminum oxide chemistry does not occur for bronsted lowry acids and bases bronsted lowry
Reaction.At normal temperatures, it is exactly that HF acid can not work to aluminium oxide ceramics.Aluminium oxide ceramics shows superelevation to soda acid
Stability, it ensure that its extensive use in chemical industry.
Then there is weakness-fragility of general character in aluminium oxide ceramics, be limit its practical ranges continue extension and it is excellent
The main reason for performance plays.Shown according to research, ceramic material is brittle have its source in ceramic crystal lack 5 it is independent
Slip system, when material stress, crackle sharp corner produce stress concentration, it is difficult to occur sliding caused by plastic deformation and it is loose
Relaxation stress, crackle extend rapidly, finally result in ceramic material fracture.
The content of the invention
For the problems of the prior art, the present invention provides a kind of preparation method of reinforced alumina ceramic, with aluminium section bar
The sludge of factory, using the impurity in sludge as flexibilizer additive and stabilizer, not only solves the dirt of aluminium section bar plant as silicon source
The environmental protection treatment problem of mud, while also reduce the production cost of aluminium oxide ceramics.
To realize above technical purpose, the technical scheme is that：A kind of preparation method of reinforced alumina ceramic, its
It is characterised by：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 3-5, stood
1-3h, mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder being added into suspension, is aerated back flow reaction 2-4h, reaction adds curing agent after terminating,
Form mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2-4h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 30-60min in mould, then opens mould and replenish slurries, continue microwave
Reaction, operate 2-5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
Preferably, the mixing speed for being slowly stirred dropwise addition in the step 1 is 2000-3000r/min, rate of addition
For 3-7mL/min, the concentration of hydrochloric acid is 0.03-0.08mol/L, and the washing, which is adopted, to be washed with deionized.
Preferably, it is 10-15mL/min that the ammonia in the step 2, which is passed through speed, the mixing speed is 1500-
3500r/min, the precipitation mixture is put into baking oven is dried with 60-80 DEG C.
Preferably, the concentration of polyvinylpyrrolidone is 5-13g/L in the step 3, the second of the ethanol water
Determining alcohol is 60-80%.
Preferably, the rate of addition of precipitation mixture is 2-5g/min in the step 3.
Preferably, the particle diameter of the nanometer aluminium powder in the step 4 is 50-500nm, the addition of the nanometer aluminium powder is
0.05-0.15g/L, the curing agent addition are 0.2-0.4g/L, and the curing agent uses silica gel curing agent.
Preferably, the pressure of the vacuum distillation reaction in the step 5 is the 50-70% of atmospheric pressure, vapo(u)rizing temperature is
50-70 DEG C, the slurry volume is the 10-15% of mixing suspension volume.
Preferably, the temperature of the microwave reaction in the step 6 is 150-300 DEG C, the power bracket of microwave reaction is
50-150W。
As an improvement, the microwave reaction in the step 6 uses compartment microwave reaction, interval time 3-5min.
Preferably, the sintering temperature in the step 7 is 1300-1400 DEG C, sintering time 4-8h, the pressure is
0.11-0.15MPa。
The present invention is using the sludge of aluminium section bar plant as silicon source, and the impurity in sludge is as the first additive, through soda acid
Filtered after processing and obtain the aluminum precipitation with additive impurity, then add aluminum precipitation into ethanol water, and added and receive
Rice aluminium powder obtains slurries as Second addition, aerated reaction and vacuum distillation；The mode of last microwave reaction carries out slip casting and consolidated
Change, sintering obtains reinforced alumina ceramic after solidification.
For the sludge of aluminium section bar plant based on aluminum oxide, impurity contains silica, iron oxide, calcium oxide, magnesia, oxidation
The materials such as potassium, sodium oxide molybdena, wherein silica, iron oxide, calcium oxide, magnesia can be as the toughness reinforcings in aluminium oxide ceramics
Material, substantially increase its toughening effect.The derivant of silica, calcium oxide and iron oxide as self toughening, can increase
The different growth of aluminum oxide, the performance of high concentration aluminum oxide can be greatly improved, can not only ensure silica, calcium oxide and
Compatibility between iron oxide and aluminum oxide, while the high-temperature behavior of ceramic material can be improved, possess from reinforcing property；Oxidation
Content of magnesium is less, although playing inhibitory action to alumina grain different growth, aluminum oxide has stabilizing effect, can
Ensure the Stability Analysis of Structures in aluminum oxide phase transition process, while the volumetric expansion that sintering belt comes influences can be ignored.
Step 1 adds hydrochloric acid in sludge, and pH is adjusted to acidity, by soil impurity in sludge and big after standing sedimentation
Part of silica removes, and obtains filtrate mixture, while silica, iron oxide, calcium oxide, magnesia are main addition
Thing, wherein silica particle diameter is smaller, and iron, calcium and magnesium are respectively formed relatively stable ion, and the low particle diameter of silica can have
There is good compatibility, toughness reinforcing to aluminium oxide ceramics and play facilitation from reinforcement.
Step 2 is passed through ammonia as alkaline gas in filtrate, and the hydrogen-oxygen to form flocculence can be reacted with metal ion
Change aluminium, magnesium hydroxide and ferric hydroxide precipitate, while calcium hydroxide can separate out white precipitate under low solubility；Flocculence
Aluminum hydroxide precipitation can be in adsorbent solution low particle diameter silica, iron hydroxide, magnesium hydroxide and calcium hydroxide, reach equal
Even mixing.
Dissolubility of the step 3 using polyvinylpyrrolidone in ethanol water, can be formed with certain viscosity
Dispersion liquid, precipitation mixture is being dispersed in ethanol water during being slowly added to, is obtaining uniform suspension.
Step 4 can play bridge linking effect, using aeration using nanometer aluminium powder as continuity toughness reinforcing particle to underbead crack
Nanometer aluminium powder is dispersed in sediment by the mode of backflow, forms homogeneous system, and reaction is put into curing agent after terminating, can formed
More micro- consistence suspension.
Micro- consistence suspension is put into be evaporated under reduced pressure in vacuum distillation apparatus by step 5 to react, by the second in ethanol water
Alcohol evaporative removal, thick water solution is formed, under the interaction of polyvinylpyrrolidone and curing agent, formation substantially increases viscous
Denseness.
Step 6 by slurry inject mould in, by microwave reaction by water evaporation, at the same using microwave band come heat power work
The intermolecular gap formed after water evaporation is diminished with lower, mould can be filled up by way of filling up slurries, ensures crude green body
Compact structure and fixed effect it is good；Microwave reaction can remove the hydrone in internal additive simultaneously, be formed more
Aluminum oxide, silica, iron oxide, the calcium oxide particle of stabilization, while ensure structural stability and compactness.
Thick embryo progress vacuum heating-press sintering can be ensured that thick embryo surface forms pressure by step 7, ensure the cause of internal structure
Close property, quickly filled up when forming framework hole, ensure that ceramic structure compactness structure, while also ensure that additive to ceramics
Toughening effect, stabilization of the magnesia to phase transformation.
From the above, it can be seen that the present invention possesses advantages below：
1. the present invention is using the sludge of aluminium section bar plant as silicon source, using the impurity in sludge as flexibilizer additive and stably
Agent, not only solves the environmental protection treatment problem of the sludge of aluminium section bar plant, while also reduces the production cost of aluminium oxide ceramics.
2. the present invention is using nanometer aluminium powder as continuity toughness reinforcing particle, using the good advantage of the compatibility of aluminium and aluminum oxide,
The energy of Crack Extension is absorbed using plastic deformation, alleviates the stress concentration of crack tip, while deformation makes the extension side of crackle
To changing, the energy for the Crack Extension that dissipated, so as to reach the purpose of ceramic toughening.
3. the present invention farthest ensures the mixed effect of silicon source and additive by the way of pickling successively and alkali cleaning,
Silica is played a role in filtering simultaneously, low particle diameter silica is obtained, improves silica on the whole in self toughening body
Inducing effect in system.
4. the present invention is dissolved in ethanol water using polyvinylpyrrolidone as dispersant, sediment can be formed
Good suspended dispersion effect, the addition of curing agent can form micro- thick suspended system with polyvinylpyrrolidone, curing agent
Coagulation and the peptizaiton of polyvinylpyrrolidone reach balance；The mode of microwave reaction breaks the balance, promotes solid
The coagulation of agent, while induce the bond effect of polyvinylpyrrolidone high polymer material itself.
5. the present invention, by pulp mould, can not only be removed solvent molecule in slurry by the way of microwave reaction,
The hydroxide precipitation in sediment is converted into oxide simultaneously, and is densified in the presence of microwave reaction, is obtained
Dense form idiosome.
6. the present invention, as toughness reinforcing reactive mode, can not only utilize the mode of sintering to protect using vacuum heating-press sintering mode
Self toughening and metal continuity particulate reinforcement inside card, reach the purpose of dual toughness reinforcing, while hot pressing can be in ceramic watch
Face forms relatively stable pressure, ensures the densified structure of aluminium oxide ceramics.
Embodiment
Describe the present invention in detail with the following Examples, but any restriction is not done to the claim of the present invention.
Embodiment 1
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 3, stand 1h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 2h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 30min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 2 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2000r/min, rate of addition 3mL/min, described
Concentration of hydrochloric acid is 0.03mol/L, and the washing, which is adopted, to be washed with deionized.
It is 10mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 1500r/min, the precipitation
Mixture is put into baking oven is dried with 60 DEG C.
The concentration of polyvinylpyrrolidone is 5g/L in the step 3, and the concentration of alcohol of the ethanol water is 60%；
The rate of addition of precipitation mixture is 2g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 50nm, and the addition of the nanometer aluminium powder is 0.05g/L, described
Curing agent addition is 0.2g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 50% of atmospheric pressure, and vapo(u)rizing temperature is 50 DEG C.
The temperature of microwave reaction in the step 6 is 150 DEG C, and the power bracket of microwave reaction is 50W.
Sintering temperature in the step 7 is 1300 DEG C, sintering time 4h, and the pressure is 0.11MPa.
Embodiment 2
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 5, stand 3h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 4h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 60min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 3000r/min, rate of addition 7mL/min, described
Concentration of hydrochloric acid is 0.08mol/L, and the washing, which is adopted, to be washed with deionized.
It is 15mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3500r/min, the precipitation
Mixture is put into baking oven is dried with 80 DEG C.
The concentration of polyvinylpyrrolidone is 13g/L in the step 3, and the concentration of alcohol of the ethanol water is
80%；The rate of addition of precipitation mixture is 5g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 500nm, and the addition of the nanometer aluminium powder is 0.15g/L, described
Curing agent addition is 0.4g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 70% of atmospheric pressure, and vapo(u)rizing temperature is 70 DEG C.
The temperature of microwave reaction in the step 6 is 300 DEG C, and the power bracket of microwave reaction is 150W.
Sintering temperature in the step 7 is 1400 DEG C, sintering time 8h, and the pressure is 0.15MPa.
Embodiment 3
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 4, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 3h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 3h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 45min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 3 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 5mL/min, described
Concentration of hydrochloric acid is 0.05mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 2500r/min, the precipitation
Mixture is put into baking oven is dried with 70 DEG C.
The concentration of polyvinylpyrrolidone is 9g/L in the step 3, and the concentration of alcohol of the ethanol water is 70%；
The rate of addition of precipitation mixture is 3g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 250nm, and the addition of the nanometer aluminium powder is 0.1g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 60% of atmospheric pressure, and vapo(u)rizing temperature is 60 DEG C.
The temperature of microwave reaction in the step 6 is 250 DEG C, and the power bracket of microwave reaction is 100W.
Sintering temperature in the step 7 is 1350 DEG C, sintering time 6h, and the pressure is 0.13MPa.
Embodiment 4
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 3, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 3h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 3h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 45min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 4mL/min, described
Concentration of hydrochloric acid is 0.05mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 2500r/min, the precipitation
Mixture is put into baking oven is dried with 65 DEG C.
The concentration of polyvinylpyrrolidone is 7g/L in the step 3, and the concentration of alcohol of the ethanol water is 65%,
The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 450nm, and the addition of the nanometer aluminium powder is 0.08g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 55% of atmospheric pressure, and vapo(u)rizing temperature is 55 DEG C.
The temperature of microwave reaction in the step 6 is 200 DEG C, and the power bracket of microwave reaction is 50-150W, and microwave is anti-
Compartment microwave reaction, interval time 3min should be used, its microwave reaction sets such as following table：
| Number | Power W | Temperature DEG C |
| For the first time | 50 | 200 |
| Second | 100 | 200 |
| For the third time | 100 | 200 |
| 4th time | 150 | 200 |
| 5th time | 150 | 200 |
Sintering temperature in the step 7 is 1330 DEG C, sintering time 5h, and the pressure is 0.12MPa.
Embodiment 5
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 3, stand 3h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 50min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 4 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2800r/min, rate of addition 4mL/min, described
Concentration of hydrochloric acid is 0.07mol/L, and the washing, which is adopted, to be washed with deionized.
It is 14mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 2000r/min, the precipitation
Mixture is put into baking oven is dried with 65 DEG C.
The concentration 10g/L of polyvinylpyrrolidone in the step 3, the concentration of alcohol of the ethanol water is 75%；
The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 450nm, and the addition of the nanometer aluminium powder is 0.12g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 55% of atmospheric pressure, and vapo(u)rizing temperature is 70 DEG C.
The temperature of microwave reaction in the step 6 is 250 DEG C, and the power bracket of microwave reaction is 50-150W；Microwave is anti-
Compartment microwave reaction should be used, interval time 5min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C |
| For the first time | 50 | 250 |
| Second | 100 | 250 |
| For the third time | 150 | 250 |
| 4th time | 150 | 250 |
Sintering temperature in the step 7 is 1370 DEG C, sintering time 7h, and the pressure is 0.14MPa.
Embodiment 6
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 5, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 3h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 3h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 35min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2800r/min, rate of addition 5mL/min, described
Concentration of hydrochloric acid is 0.07mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 70 DEG C.
The concentration of polyvinylpyrrolidone is 11g/L in the step 3, and the concentration of alcohol of the ethanol water is
75%；The rate of addition of precipitation mixture is 3g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 400nm, and the addition of the nanometer aluminium powder is 0.12g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 50% of atmospheric pressure, and vapo(u)rizing temperature is 55 DEG C.
The temperature of microwave reaction in the step 6 is 150 DEG C, and the power bracket of microwave reaction is 50-150W；The step
Microwave reaction in rapid 6 uses compartment microwave reaction, and interval time 3min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C |
| For the first time | 50 | 150 |
| Second | 50 | 150 |
| For the third time | 100 | 150 |
| 4th time | 100 | 150 |
| 5th time | 150 | 150 |
Sintering temperature in the step 7 is 1400 DEG C, sintering time 4h, and the pressure is 0.13MPa.
Embodiment 7
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 5, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 3h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 3h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 35min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2800r/min, rate of addition 5mL/min, described
Concentration of hydrochloric acid is 0.07mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 70 DEG C.
The concentration of polyvinylpyrrolidone is 11g/L in the step 3, and the concentration of alcohol of the ethanol water is
75%；The rate of addition of precipitation mixture is 3g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 400nm, and the addition of the nanometer aluminium powder is 0.12g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 50% of atmospheric pressure, and vapo(u)rizing temperature is 55 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；Institute
The microwave reaction stated in step 6 uses compartment microwave reaction, interval time 3-5min, the reactions steps of the microwave reaction
It is as follows：
Sintering temperature in the step 7 is 1300 DEG C, sintering time 7h, and the pressure is 0.14MPa.
Embodiment 8
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 5, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 3h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 3h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 35min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2800r/min, rate of addition 5mL/min, described
Concentration of hydrochloric acid is 0.07mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 70 DEG C.
The concentration of polyvinylpyrrolidone is 11g/L in the step 3, and the concentration of alcohol of the ethanol water is
75%；The rate of addition of precipitation mixture is 3g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 400nm, and the addition of the nanometer aluminium powder is 0.12g/L, described
Curing agent addition is 0.3g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 50% of atmospheric pressure, and vapo(u)rizing temperature is 55 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；Institute
The microwave reaction stated in step 6 uses compartment microwave reaction, interval time 3-5min, the reactions steps of the microwave reaction
It is as follows：
| Number | Power W | Temperature DEG C | Interval time |
| For the first time | 50 | 150 | 3min |
| Second | 100 | 150 | 3min |
| For the third time | 150 | 200 | 4min |
| 4th time | 150 | 250 | 5min |
| 5th time | 150 | 300 | 5min |
Sintering temperature in the step 7 is 1350 DEG C, sintering time 8h, and the pressure is 0.12MPa.
Embodiment 9
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 4, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 50min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 6mL/min, described
Concentration of hydrochloric acid is 0.06mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 75 DEG C.
The concentration of polyvinylpyrrolidone is 10g/L in the step 3, and the concentration of alcohol of the ethanol water is
70%；The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 300nm, and the addition of the nanometer aluminium powder is 0.1g/L, described
Curing agent addition is 0.4g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 65% of atmospheric pressure, and vapo(u)rizing temperature is 50-70 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；It is micro-
Ripple reaction uses compartment microwave reaction, and interval time 3-5min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C | Interval time |
| For the first time | 50 | 150 | 3min |
| Second | 100 | 200 | 3min |
| For the third time | 100 | 200 | 4min |
| 4th time | 100 | 250 | 5min |
| 5th time | 150 | 300 | 5min |
Sintering temperature in the step 7 is 1350 DEG C, sintering time 5h, and the pressure is 0.13MPa, the sintering
Heating mode it is as follows：
| Sintering time | Sintering temperature | Programming rate |
| 30min | - 300 DEG C of room temperature | 10℃/min |
| 20min | 300℃ | - |
| 25min | 300-800℃ | 20℃/min |
| 110min | 800-1350℃ | 5℃/min |
| Remaining time | 1350℃ | - |
Embodiment 10
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 4, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 50min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 6mL/min, described
Concentration of hydrochloric acid is 0.06mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 75 DEG C.
The concentration of polyvinylpyrrolidone is 10g/L in the step 3, and the concentration of alcohol of the ethanol water is
70%；The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 300nm, and the addition of the nanometer aluminium powder is 0.1g/L, described
Curing agent addition is 0.4g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 65% of atmospheric pressure, and vapo(u)rizing temperature is 50-70 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；It is micro-
Ripple reaction uses compartment microwave reaction, and interval time 3-5min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C | Interval time |
| For the first time | 50 | 150 | 3min |
| Second | 100 | 200 | 3min |
| For the third time | 100 | 250 | 5min |
| 4th time | 150 | 250 | 5min |
| 5th time | 150 | 300 | 5min |
Sintering temperature in the step 7 is 1400 DEG C, sintering time 4h, and the pressure is 0.15MPa, the sintering
Heating mode it is as follows：
| Sintering time | Sintering temperature | Programming rate |
| 25min | - 500 DEG C of room temperature | 20℃/min |
| 50min | 500-1000℃ | 10℃/min |
| 25min | 1000℃ | - |
| 40min | 1000-1400℃ | 10℃/min |
| Remaining time | 1400℃ | - |
Embodiment 11
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 4, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 50min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 6mL/min, described
Concentration of hydrochloric acid is 0.06mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 75 DEG C.
The concentration of polyvinylpyrrolidone is 10g/L in the step 3, and the concentration of alcohol of the ethanol water is
70%；The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 300nm, and the addition of the nanometer aluminium powder is 0.1g/L, described
Curing agent addition is 0.4g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 65% of atmospheric pressure, and vapo(u)rizing temperature is 50-70 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；It is micro-
Ripple reaction uses compartment microwave reaction, and interval time 3-5min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C | Interval time |
| For the first time | 50 | 150 | 3min |
| Second | 100 | 200 | 3min |
| For the third time | 150 | 250 | 4min |
| 4th time | 150 | 300 | 5min |
| 5th time | 150 | 300 | 5min |
Sintering temperature in the step 7 is 1380 DEG C, sintering time 8h, and the pressure is 0.15MPa, the sintering
Heating mode it is as follows：
| Sintering time | Sintering temperature | Programming rate |
| 40min | - 600 DEG C of room temperature | 15℃/min |
| 10min | 600℃ | - |
| 30min | 600-900℃ | 10℃/min |
| 30min | 900℃ | - |
| 96min | 900-1380℃ | 5℃/min |
| Remaining time | 1380℃ | - |
Embodiment 12
A kind of preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：
Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 4, stand 2h,
Mixing filtrate is collected after filtration washing；
Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitated after suction filtration
Mixture；
Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtained
Stable suspension；
Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 4h, reaction adds curing agent, shape after terminating
Into mixing suspension；
Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2h, obtain thick slurries；
Step 6, slurries are injected into microwave reaction 50min in mould, then opens mould and replenish slurries, it is anti-to continue microwave
Should, operate 5 times repeatedly, obtain drying the crude green body of densification；
Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
The mixing speed for being slowly stirred dropwise addition in the step 1 is 2500r/min, rate of addition 6mL/min, described
Concentration of hydrochloric acid is 0.06mol/L, and the washing, which is adopted, to be washed with deionized.
It is 13mL/min that ammonia in the step 2, which is passed through speed, and the mixing speed is 3000r/min, the precipitation
Mixture is put into baking oven is dried with 75 DEG C.
The concentration of polyvinylpyrrolidone is 10g/L in the step 3, and the concentration of alcohol of the ethanol water is
70%；The rate of addition of precipitation mixture is 4g/min in the step 3.
The particle diameter of nanometer aluminium powder in the step 4 is 300nm, and the addition of the nanometer aluminium powder is 0.1g/L, described
Curing agent addition is 0.4g/L, and the curing agent uses silica gel curing agent.
The pressure of vacuum distillation reaction in the step 5 is the 65% of atmospheric pressure, and vapo(u)rizing temperature is 50-70 DEG C.
The temperature of microwave reaction in the step 6 is 150-300 DEG C, and the power bracket of microwave reaction is 50-150W；It is micro-
Ripple reaction uses compartment microwave reaction, and interval time 3-5min, the reactions steps of the microwave reaction are as follows：
| Number | Power W | Temperature DEG C | Interval time |
| For the first time | 50 | 150 | 4min |
| Second | 50 | 200 | 4min |
| For the third time | 50 | 250 | 3min |
| 4th time | 150 | 250 | 3min |
| 5th time | 150 | 300 | 5min |
Sintering temperature in the step 7 is 1400 DEG C, sintering time 6h, and the pressure is 0.11MPa, the sintering
Heating mode it is as follows：
Performance test：
1. fracture toughness：Fracture toughness is to weigh an important materials constant of material resistance Crack Extension ability, in AG-
Fracture on IC20KN type electronic universal testers using SENB (single edge notched beam) method measure sample is tough
Property.
2. bending strength：Bending strength test equipment used is AG-IC20KN type electronic universal testers, curved with 3 points
The bending strength of bent method test compound material sample.
3. Vickers hardness：The microhardness of composite is determined on HV-1000 microhardness testers, loads 9.8N,
Dwell time 15s.
Comparative example is using common commercially available aluminium oxide ceramics
The performance test results such as following table：
Drawn through performance test, reinforced alumina ceramic prepared by preparation method provided by the invention is made pottery with commercial alumina
Porcelain is compared, and Vickers hardness, bending strength and fracture toughness are steadily improved, wherein, improve during Vickers hardness maximum
8.6%, improve 28% during bending strength maximum, improve 86% during fracture toughness maximum.
In summary, the present invention has advantages below：
1. the present invention is using the sludge of aluminium section bar plant as silicon source, using the impurity in sludge as flexibilizer additive and stably
Agent, not only solves the environmental protection treatment problem of the sludge of aluminium section bar plant, while also reduces the production cost of aluminium oxide ceramics.
2. the present invention is using nanometer aluminium powder as continuity toughness reinforcing particle, using the good advantage of the compatibility of aluminium and aluminum oxide,
The energy of Crack Extension is absorbed using plastic deformation, alleviates the stress concentration of crack tip, while deformation makes the extension side of crackle
To changing, the energy for the Crack Extension that dissipated, so as to reach the purpose of ceramic toughening.
3. the present invention farthest ensures the mixed effect of silicon source and additive by the way of pickling successively and alkali cleaning,
Silica is played a role in filtering simultaneously, low particle diameter silica is obtained, improves silica on the whole in self toughening body
Inducing effect in system.
4. the present invention is dissolved in ethanol water using polyvinylpyrrolidone as dispersant, sediment can be formed
Good suspended dispersion effect, the addition of curing agent can form micro- thick suspended system with polyvinylpyrrolidone, curing agent
Coagulation and the peptizaiton of polyvinylpyrrolidone reach balance；The mode of microwave reaction breaks the balance, promotes solid
The coagulation of agent, while induce the bond effect of polyvinylpyrrolidone high polymer material itself.
5. the present invention, by pulp mould, can not only be removed solvent molecule in slurry by the way of microwave reaction,
The hydroxide precipitation in sediment is converted into oxide simultaneously, and is densified in the presence of microwave reaction, is obtained
Dense form idiosome.
6. the present invention, as toughness reinforcing reactive mode, can not only utilize the mode of sintering to protect using vacuum heating-press sintering mode
Self toughening and metal continuity particulate reinforcement inside card, reach the purpose of dual toughness reinforcing, while hot pressing can be in ceramic watch
Face forms relatively stable pressure, ensures the densified structure of aluminium oxide ceramics.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical scheme described by inventive embodiments.It will be understood by those within the art that still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
- A kind of 1. preparation method of reinforced alumina ceramic, it is characterised in that：Its preparation process is as follows：Step 1, the sludge of aluminium section bar plant is put into reactor, is slowly stirred dropwise addition hydrochloric acid, until pH is 3-5, stand 1-3h, Mixing filtrate is collected after filtration washing；Step 2, ammonia is passed through in mixing filtrate, stirs and produced up to without flocculation sediment, precipitation mixing is obtained after suction filtration Thing；Step 3, polyvinylpyrrolidone is added into ethanol water, is then slowly added into precipitation mixture, obtain stabilization Suspension；Step 4, nanometer aluminium powder is added into suspension, is aerated back flow reaction 2-4h, reaction adds curing agent after terminating, and is formed Mixing suspension；Step 5, mixing suspension is put into vacuum distillation apparatus and is evaporated under reduced pressure reaction 2-4h, obtain thick slurries；Step 6, slurries are injected into microwave reaction 30-60min in mould, then open mould and replenish slurries, continue microwave reaction, Operate 2-5 times repeatedly, obtain drying the crude green body of densification；Step 7, crude green body is put into vacuum sintering funace and be sintered, obtain reinforced alumina ceramic.
- A kind of 2. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 1 The mixing speed for being slowly stirred dropwise addition be 2000-3000r/min, rate of addition 3-7mL/min, the concentration of hydrochloric acid is 0.03-0.08mol/L, the washing, which is adopted, to be washed with deionized.
- A kind of 3. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 2 Ammonia to be passed through speed be 10-15mL/min, the mixing speed is 1500-3500r/min, and the precipitation mixture is put into baking Dried in case with 60-80 DEG C.
- A kind of 4. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 3 The concentration of polyvinylpyrrolidone is 5-13g/L, and the concentration of alcohol of the ethanol water is 60-80%.
- A kind of 5. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 3 The rate of addition of precipitation mixture is 2-5g/min.
- A kind of 6. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 4 The particle diameter of nanometer aluminium powder be 50-500nm, the addition of the nanometer aluminium powder is 0.05-0.15g/L, and the curing agent adds Measure and use silica gel curing agent for 0.2-0.4g/L, the curing agent.
- A kind of 7. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 5 Vacuum distillation reaction pressure be atmospheric pressure 50-70%, vapo(u)rizing temperature is 50-70 DEG C, and the slurry volume is that mixing is outstanding The 10-15% of turbid volume.
- A kind of 8. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 6 Microwave reaction temperature be 150-300 DEG C, the power bracket of microwave reaction is 50-150W.
- A kind of 9. preparation method of reinforced alumina ceramic according to claim 8, it is characterised in that：In the step 6 Microwave reaction use compartment microwave reaction, interval time 3-5min.
- A kind of 10. preparation method of reinforced alumina ceramic according to claim 1, it is characterised in that：In the step 7 Sintering temperature be 1300-1400 DEG C, sintering time 4-8h, the pressure is 0.11-0.15MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387141A (en) * | 2018-03-06 | 2018-08-10 | 绍兴文理学院 | A kind of preparation method of bulletproof composite ceramic plate |
| RU2730229C1 (en) * | 2019-07-17 | 2020-08-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Сибирский государственный университет путей сообщения" (СГУПС) | Mixture based on aluminium oxide and method of producing strong ceramics |
| CN114349485A (en) * | 2022-01-11 | 2022-04-15 | 无锡特科精细陶瓷有限公司 | Preparation method of high-strength alumina ceramic |
| RU2730229C9 (en) * | 2019-07-17 | 2023-10-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Сибирский государственный университет путей сообщения" (СГУПС) | Mixture based on aluminium oxide and method of producing strong ceramics |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0697241A1 (en) * | 1994-08-19 | 1996-02-21 | Toyota Jidosha Kabushiki Kaisha | A high heat-resistant copper-alumina composite oxide and a method for purifying exhaust gases |
| CN102690953A (en) * | 2011-03-19 | 2012-09-26 | 渤海大学 | Method for preparing compound powder of alumina and chrome oxide from chromium-containing aluminum sludge |
-
2017
- 2017-09-29 CN CN201710911382.7A patent/CN107540353B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0697241A1 (en) * | 1994-08-19 | 1996-02-21 | Toyota Jidosha Kabushiki Kaisha | A high heat-resistant copper-alumina composite oxide and a method for purifying exhaust gases |
| CN102690953A (en) * | 2011-03-19 | 2012-09-26 | 渤海大学 | Method for preparing compound powder of alumina and chrome oxide from chromium-containing aluminum sludge |
Non-Patent Citations (1)
| Title |
|---|
| 戴武斌等: ""煅烧温度对铝型材厂污泥晶相结构影响的研究"", 《中国陶瓷》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108387141A (en) * | 2018-03-06 | 2018-08-10 | 绍兴文理学院 | A kind of preparation method of bulletproof composite ceramic plate |
| CN108387141B (en) * | 2018-03-06 | 2020-08-18 | 绍兴文理学院 | A kind of preparation method of composite bulletproof ceramic plate |
| RU2730229C1 (en) * | 2019-07-17 | 2020-08-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Сибирский государственный университет путей сообщения" (СГУПС) | Mixture based on aluminium oxide and method of producing strong ceramics |
| RU2730229C9 (en) * | 2019-07-17 | 2023-10-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Сибирский государственный университет путей сообщения" (СГУПС) | Mixture based on aluminium oxide and method of producing strong ceramics |
| CN114349485A (en) * | 2022-01-11 | 2022-04-15 | 无锡特科精细陶瓷有限公司 | Preparation method of high-strength alumina ceramic |
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