CN108751956A - A kind of method that alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic micron powder mixture - Google Patents

A kind of method that alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic micron powder mixture Download PDF

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CN108751956A
CN108751956A CN201810751719.7A CN201810751719A CN108751956A CN 108751956 A CN108751956 A CN 108751956A CN 201810751719 A CN201810751719 A CN 201810751719A CN 108751956 A CN108751956 A CN 108751956A
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oxide
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solid solution
alumina
amorphous
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郑永挺
于永东
蒋劲松
栢跃磊
赫晓东
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Harbin Institute of Technology
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Abstract

A kind of method that alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic micron powder mixture, the present invention relates to a kind of preparation method fields of composite ceramic material, and in particular to a kind of method of alumina conbustion synthesis high-temperature fusant combination rotating metallic disk or roller equipment chilling.The invention solves existing preparation methods there are of high cost, efficiency is low, the time is long, low output, can only small lot production the technical issues of.Method：One, mixed powder is prepared；Two, cause synthetic reaction, heat preservation is cooling in the two pairs of rollers of rotating metallic disk or roller equipment, then crushes, ball milling.The technical process of this method is simple, is swift in response, and short preparation period, yield is big, and purity is high, can control, and is the process of preparing of a kind of low cost, high efficiency, high performance metastable state powder and micron.The present invention is used to prepare Al2O3Base amorphous and solid solution ceramic micron powder mixture.

Description

A kind of alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture
Technical field
The present invention relates to a kind of preparation method fields of composite ceramic material, and in particular to a kind of alumina conbustion synthesis high temperature The method of melt combination rotating metallic disk or roller equipment chilling.
Background technology
Conbustion synthesis (combustion synthesis), also known as self-propagating high-temperature synthesis (abbreviation SHS).This method Without external heat source, the heat released when being by raw material autoreactivity carries out the technology of inorganic refractory synthesis.The party The advantages of method is：It is at low cost, energy consumption is low, reaction temperature is high, production efficiency is high.
The preparation for concentrating on amorphous metal is mainly studied in non-crystalline material preparation field, and realizes industrialized production；Have Introducing of closing prepared by ceramic amorphous is fewer, the preparation of refractory ceramics amorphous does not have substantially, and there is currently ceramic amorphous Ceramic conversion rate is relatively low in preparation method, and of high cost, is unsuitable for industrialized production.
Non-crystalline material (amorphous metal+amorphous ceramic) is commonly used preparation method and is mainly the following：Melt supercooled method, chemistry Reduction method, mechanical alloying method, sol-gal process, precursor pyrolysismethod, arc discharge method.Wherein chilling method is earliest preparation The method of amorphous, principle are to make every effort to increase alloy sample specific surface area, and try the interface heat for reducing melt with cooling medium It hinders to reach high cooling rate.Atomization and single-roller method are the most commonly used two methods.Atomization is mainly used to produce Amorphous state and crystalline state powder.Its principle is to impact metal liquid stream by high velocity gas stream it is made to be separated into fine droplet, to real Now quickly solidification.This method equipment is simple, easy to operate, is easy to industrialization production.Single-roller method is to utilize atwirl copper The liquid metal of sprayed coating thereon is thrown away roll surface by roller after quickly solidification, is formed thickness and is about the amorphous of a few to tens of microns and micro- Crystal zone material.The method can obtain 106The cooling rate of K/s, is one of common method, and this method is mainly used for the system of amorphous metal It is standby.
For arc discharge method, it is mainly used in the preparation of amorphous metal；And prepared by amorphous ceramic, this method is also fitted It closes.The report that arc discharge prepares non-crystalline material at present is about A12O3-Y2O3-ZrO2It is prepared by amorphous.A12O3, Y2O3, ZrO2, Three kinds of raw materials weigh by a certain percentage, and club-shaped material is made after ball milling mixing, so that top is melted by arc discharge, and drip small liquid It drops on roll, amorphous board-like material is become by roll pressed.Using this kind of method, the melt of composite ceramics system is obtained, into And with the method quickly solidified, the amorphous of nonequilibrium state is obtained, nanocrystalline precipitation is realized in material after sintering or heat treatment, it can Obtain highdensity fine and closely woven, uniform nanostructure.But research focuses primarily upon mechanism study at present, is suitble to large-scale production Practical technique still has shortcoming.
In short, in the common preparation method of amorphous metal material, chemical reduction method cannot be used for preparing amorphous ceramic；Machine The powder sphericity of tool alloying production is poor, is easily mixed into impurity in crushing process and efficiency is low.And amorphous ceramic material is normal Preparation method, sol-gal process required time is long, and there are a large amount of micropores, will escape many gases again in the drying process And organic matter, and generate contraction；A large amount of hole and crackle are will produce during polymer cracking in precursor pyrolysismethod, is destroyed The globality of material, and finally influence the performance of material；Large-scale production is not implemented in arc discharge method.
Invention content
The present invention is to solve existing method prepare the of high cost of amorphous metal material, purity are low, efficiency is low, the time is long, Low output can only small lot production the technical issues of, and a kind of alumina conbustion synthesis chilling method is provided and prepares Al2O3Base amorphous and solid The method of solution ceramics micron powder mixture.
A kind of alumina conbustion synthesis chilling method preparation Al2O3The method of base amorphous and solid solution ceramic micron powder mixture, should Method specifically carries out according to the following steps：
One, aluminium powder and diluent are dried, are uniformly mixed, obtain mixed powder；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, is passed through oxidisability gas Body lights mixed powder and causes synthetic reaction, and heat preservation is then turned on voltage-resistant reactor nozzle, compounding flux in voltage-resistant reactor It is sprayed onto cooling in the two pairs of rollers of rotating metallic disk or roller equipment, is then crushed, ball milling, Al is obtained2O3Base amorphous and solid solution ceramic Micron powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method.
If compounding flux is sprayed onto in rotating metallic disk, rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/ min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water For 20~30L/min, hydraulic pressure is 0.1~0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution Film；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, roller Rotor speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter Two pairs of rollers, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
The present invention reacts (see chemical equation (1)) using alumina combustion heat release, and there is no use metal Al and various gold Genus nitrobacter combustion heat release reacts, and further increases A12O3The purity of powder eliminates remaining metal salt and generates impurity The influence of compound.It is reacted simultaneously using alumina combustion heat release, generates high temperature and pressure using system heat release, make the raw material of molten state High speed is ejected on atwirl iron, copper, steel disk (see attached drawing 1) or roller equipment (see attached drawing 2), and auxiliary water cooling, is accelerated Melt cooling velocity, obtains Al2O3/ZrO2Amorphous and solid solution hybrid films or strip material.This method belongs to far from equilibrium state Rapid solidification, it is possible to obtain the amorphous for being difficult to obtain under equilibrium state and high solid solubility powder；This micron of later stage When powder prepares eutectic ceramic, can be precipitated it is nanocrystalline, play it is nano combined enhancing ceramics effect, substantially increase ceramics Performance.
In the method for the present invention, most important is exactly Al-O2Between combustion heat release reaction (see chemical equation (1)), Moment generates high temperature and pressure, melts Al2O3、ZrO2Diluent and high temperature Al2O3/ZrO2Melt rapid solidification.Conbustion synthesis Basic principle is, with O2Or O2And N2The Al powder of mixed gas and high reproducibility is raw material, with ZrO2Powder and Al2O3Powder is diluent (or the other oxide diluents of addition), and phase transformation stabilizer (yttrium oxide, cerium oxide, magnesia, calcium oxide, titanium oxide is added Equal oxides) control tetragonal phase ZrO in product2Content.N is wherein added2Purpose be exactly, in Al-O2After preferential reaction, It is reacted with Al powder and generates a small amount of ZrN (square formula (2)), increase the conductivity and hardness of ceramics.Other gas are added simultaneously Body improves the safety coefficient of production also for the concentration for reducing oxidizing gas to reduce reaction rate.
4Al+3O2→2Al2O3 (1)
8Al+3N2+6ZrO2→4Al2O3+6ZrN (2)
The reaction has high theoretical temperatures (2100~4000 DEG C), and inert aluminium oxide and zirconium oxide is added as dilute Agent is released, the stability of conbustion synthesis on the one hand can be improved, is on the other hand conducive to regulate and control product ZrO2/Al2O3Ratio, obtain Obtain the ZrO of different proportion2/Al2O3Compound micron powder.When combustion reaction container inner pressure is sprayed with temperature joint effect melt Temperature, speed, when pressure is larger, spouting velocity is very fast, and melt cooling velocity is relatively fast；When pressure is low, express delivery is sprayed Relatively low, cooling velocity is relatively slow.Spouting velocity is not only related with pressure, also related with nozzle diameter, when spout is smaller, spray It is larger to go out speed, when spout is larger, spouting velocity is relatively low.Therefore to control high temperature (2100~4000 DEG C), high pressure (5~ 50MPa), melt heat preservation (1~60s) is sprayed afterwards.
The present invention can by design reactant ratio, come adjust combustion synthesis reaction theoretical adiabatic temperature and reaction Pressure.Wherein the control of pressure mainly passes through three kinds of approach：1) container after reacting is adjusted by feed change proportioning, atmosphere pressures Interior gas pressure；2) pressure is adjusted by reacting the temperature generated；3) system is made to drop to formulation pressure by decompression after reacting Power.Finally the pressure limit in system is controlled in 0.5~50MPa.
In reactor electric heating tube in drier body, raw material powder is heated to 25~300 DEG C, ZrO can be improved2Content, reduce Al2O3Content, to improve, regulate and control the performance of prepared nano combined enhancing ceramics.
Above method diluent has wide applicability, and diluent includes but not limited to barium monoxide, iron oxide, oxidation Vanadium, molybdenum oxide, aluminium oxide, zirconium oxide, magnesia, calcium oxide, strontium oxide strontia, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, oxidation Nickel, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, oxidation Gadolinium, terbium oxide, dysprosia, holimium oxide, erbium oxide, thulium oxide, ytterbium oxide, luteium oxide and silica etc. are a kind of and combine.Such as system Standby Al2O3/MgO、Al2O3/TiO2、Al2O3/Y2O3、Al2O3/ZrO2/Y2O3Equal oxides.
For cooling technique, the present invention is using the iron, copper, steel disk rotated (temperature, the pressure sprayed according to melt determines) Or roller equipment is to Al2O3/ZrO2Melt supercooled obtains Al2O3/ZrO2The mixture of amorphous and solid solution film or band.For height Warm Al2O3/ZrO2Melt is quickly cooled down, must be requested that rotating circular disk or roller equipment heat conductivility are superior；The metals such as Ag, Al are led It is hot good, but fusing point is low, Al2O3/ZrO2Melt temperature is excessively high to cause prodigious corrosion function to cooling metal, so choosing Rotating circular disk or roller equipment be that heat safe iron, copper, steel and auxiliary water cooling accelerate cooling rate.Wherein for pivoting rail, Copper, steel disk equipment, one side spray high temperature Al of disk2O3/ZrO2Melt, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter simultaneously drop The temperature of low pivoting rail, copper, steel disk (see attached drawing 1).And for roller equipment, two pairs of rollers centre spray high temperature Al2O3/ZrO2Melt, two Side spray high pressure, high-velocity flow supplement heat rejecter two pairs of rollers (see attached drawing 2).In general, metal dish and two pairs of rollers rotating speed are faster, Al2O3/ ZrO2Melt temperature is lower, Al2O3/ZrO2Lower (the different mol ratio Al of melt solidification point2O3、ZrO2Solidification point it is different), it is cold But rate is higher.
Since using pivoting rail, copper, steel disk cooling, melt is fast close to disk side cooling rate, is amorphous structure；Due to Ceramic coefficient is smaller, and in the outer layer far from metal dish cooling surface, melt cooling velocity is relatively slow to form supersaturation admittedly Solution.Similarly, for roller equipment, the band close to two round rollers is amorphous structure, is supersaturated solid solution among band.
The pressure-resistant reaction vessel includes reactor 1, tabletting 4, nozzle 5, nozzle holder 6, sealing preload piece 8, upper slide 10, lower skateboard 11 and actuator 9 are provided with two-stage ladder circular hole, the first ladder circular hole 2 along the device bottom thickness direction of reactor 1 It is more than the diameter of the second ladder circular hole 3 positioned at the diameter of the top of the second ladder circular hole 3 and the first ladder circular hole 2；
The nozzle holder 6 forms coaxial integral structure by circular plate type frame body portion 6-1 and cylindrical portion 6-2, along nozzle branch The central axes of frame 6 are provided with jack 6-3, and the end face of cylindrical portion 6-2 is provided with ring groove 6-4, and nozzle holder 6 inserts embedded two-stage ladder In circular hole, cylindrical portion 6-2 and the second ladder circular hole 3 coordinate, and circular plate type frame body portion 6-1 and the first ladder circular hole 2 coordinate, circular plate type The lower surface of frame body portion 6-1 is overlapped on the step surface of two-stage ladder circular hole, and ring groove 6-4 is embedded with sealing preload piece 8；
The tabletting 4 is arranged in the upper surface of circular plate type frame body portion 6-1, and tabletting 4 and 2 screw thread of the first ladder circular hole connect It connects, the center of tabletting 4 is provided with tabletting through-hole；
Nozzle 5 is arranged in the tabletting through-hole of tabletting 4 and the jack 14 of nozzle holder 6, and nozzle 5 is built-in with graphite core, spray The bottom surface of mouth 5 is against the upper surface of sealing preload piece 8, and the upper face of upper slide 10 is in contact with the device bottom outer surface of reactor 1, The contact of lower skateboard 11, which is arranged on the lower section of upper slide 10, upper slide 10 and lower skateboard 11, has slide plate through-hole, and slide plate is logical The aperture in hole ensures that sealing preload piece 8 passes through, and the slide plate through-hole face on lower skateboard 11 seals preload piece 8, and upper slide 10 is by dragging The dynamic driving of device 9 moves horizontally, and the jet size of the nozzle is Φ 1-20mm.
The beneficial effects of the invention are as follows：
The technical process of this method is simple, and be swift in response (several seconds to a few minutes), short preparation period, and yield is big, and (1-30 is public Jin), purity is high, can control, and is the preparation process side of a kind of novel low cost, high efficiency, high performance metastable state powder and micron Method.
Mainly by Al in the present invention2O3/ZrO2The quick chilling of melt obtains Al2O3/ZrO2Amorphous and solid-solution powder are mixed Object is closed, it is high to cooling requirements.In general cooling rate is higher than 106K/s just has the presence of amorphous, must be requested that rotational circle Disk or roller equipment good heat conductivity, the metal heat-conductings such as Ag, Al are good, but fusing point is low, Al2O3/ZrO2Melt temperature is excessively high right Cooling metal causes prodigious corrosion function, so the rotating circular disk or roller equipment chosen are heat safe iron, copper, steel and auxiliary Water cooling is helped to accelerate cooling rate.Increase melt spouting velocity simultaneously, reduces melt temperature, subzero Al2O3/ZrO2Mole Than cooling velocity can be improved, and the cooling velocity the fast more is conducive to the formation of amorphous structure.
In general, obtained amorphous and solid solution membrane thickness are 5 μm~30 μm.Powder prepared by crushing ball mill, leads to The sintering of high temperature densification process is crossed, uniformly fine and closely woven nano composite oxides aluminium/zirconia ceramics can be obtained.At present using we Method hot pressed sintering can obtain nano composite oxides aluminium/zirconium oxide eutectic ceramic.
As zirconia content relatively low (20wt%-40wt%), intensity may be up to 1000MPa, and toughness may be up to 12MPa m1/2；As zirconia content medium (40wt%-60wt%), intensity may be up to 1100MPa, and toughness may be up to 13MPam1/2； As zirconia content higher (60wt%-80wt%), intensity may be up to 1200MPa, and toughness may be up to 15MPam1/2。
The diluent of the method for the present invention has wide applicability, and diluent includes but not limited to barium monoxide, iron oxide, oxygen Change vanadium, molybdenum oxide, aluminium oxide, zirconium oxide, magnesia, calcium oxide, strontium oxide strontia, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, oxygen Change nickel, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, oxygen Change the one kind such as gadolinium, terbium oxide, dysprosia, holimium oxide, erbium oxide, thulium oxide, ytterbium oxide, luteium oxide and silica and combination.Such as Prepare Al2O3/MgO、Al2O3/TiO2、Al2O3/Y2O3、Al2O3/ZrO2/Y2O3Equal oxides.
Description of the drawings
Fig. 1 is rotating metallic disk cooling schematic diagram of the present invention；
Fig. 2 is two pairs of rollers cooling schematic diagram of the present invention；
Fig. 3 is the structural schematic diagram of voltage-resistant reactor in invention；
Fig. 4 is the structural schematic diagram of nozzle holder in voltage-resistant reactor in invention；
Fig. 5 is the surface microscopic SEM pictures of powder and micron after the crushing of embodiment one, ball milling.
Specific implementation mode
Technical solution of the present invention is not limited to the specific implementation mode of act set forth below, further include each specific implementation mode it Between arbitrary combination.
Specific implementation mode one：A kind of alumina conbustion synthesis chilling method of present embodiment prepares Al2O3Base amorphous and solid solution The method of ceramic micron powder mixture, this method specifically carry out according to the following steps：
One, aluminium powder and diluent are dried, are uniformly mixed, obtain mixed powder；It is 10 according to mass fraction aluminium powder ~40 parts, diluent be 60~90 parts；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, is passed through oxidisability gas Body lights mixed powder and causes synthetic reaction, and heat preservation is then turned on voltage-resistant reactor nozzle, compounding flux in voltage-resistant reactor It is sprayed onto cooling in the two pairs of rollers of rotating metallic disk or roller equipment, is then crushed, ball milling, Al is obtained2O3Base amorphous and solid solution ceramic Micron powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method.
Specific implementation mode two：The present embodiment is different from the first embodiment in that：Diluent in the step 1 For barium monoxide, iron oxide, vanadium oxide, molybdenum oxide, aluminium oxide, zirconium oxide, magnesia, calcium oxide, strontium oxide strontia, scandium oxide, oxidation Titanium, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, tantalum oxide, lanthana, cerium oxide, praseodymium oxide, oxidation Neodymium, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosia, holimium oxide, erbium oxide, thulium oxide, ytterbium oxide, luteium oxide and oxygen One kind in SiClx or in which several mixing.It is other same as the specific embodiment one.
Specific implementation mode three：The present embodiment is different from the first and the second embodiment in that：Work as Al2O3Base amorphous and When containing zirconium oxide in solid solution ceramic micron powder mixture, Y2O3With ZrO2Molar ratio be (0~15): 100；CeO2With ZrO2's Molar ratio is (0~30): 100；MgO and ZrO2Molar ratio be (0~28): 100；CaO and ZrO2Molar ratio be (0~ 33.45):100；TiO2With ZrO2Molar ratio be (0~44.41): 100；Sc2O3With ZrO2Molar ratio be (0~20): 100. It is other the same as one or two specific embodiments.
Y in present embodiment2O3, CeO2, MgO, CaO, TiO2, Sc2O3Act as phase transformation stabilizer.
Specific implementation mode four：Unlike one of present embodiment and specific implementation mode one to three：Lead in step 2 It is O to enter oxidizing gas2Or oxidizing gas is O2Mixing or oxidizing gas with air are O2And N2Mixing or oxygen The property changed gas is O2, air and N2Mixing.It is other identical as one of specific implementation mode one to three.
The air pressure of oxidizing gas is 5~50MPa, wherein O in present embodiment2Partial pressure >=5MPa.
Specific implementation mode five：Unlike one of present embodiment and specific implementation mode one to four：If in step 2 Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/min；Rotation gold Belong to one side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water are 20~30L/ Min, hydraulic pressure are 0.1~0.5MPa, solidify to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, roller Rotor speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter Two pairs of rollers, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
Specific implementation mode six：Unlike one of present embodiment and specific implementation mode one to five：A kind of alumina combustion Burnt together prepares Al at chilling method2O3The method of base amorphous and solid solution ceramic micron powder mixture, specifically according to the following steps into Row：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 60~120 DEG C, is done The dry time is 8~16h, and vacuum degree is 0.05~0.09MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, Ball-milling Time is 2~8h, then crosses 40~200 mesh sieve, is uniformly mixed, obtains mixed powder；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little oxidizing gas for being 1~20mm of Φ, being passed through that pressure is 5~50MPa, oxidizing gas O2Or O2Mixed gas, then Voltage-resistant reactor is attached in water-circulating cooling device, sets theoretical temperatures as 2100~4000 DEG C, reaction pressure is 5~50MPa, Resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 1~60s, is then turned on voltage-resistant reactor nozzle, voltage-resistant reactor Interior Al2O3/ZrO2Compounding flux is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, is then used Planetary ball mill carries out ball milling, and control ball material mass ratio is 3: 1, and Ball-milling Time is 3~6h, and sieving obtains Al2O3/ZrO2Amorphous With solid solution ceramic micron powder mixture, a kind of alumina conbustion synthesis chilling method preparation Al is completed2O3Base amorphous and solid solution ceramic The method of micron powder mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/ min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water For 20~30L/min, hydraulic pressure is 0.1~0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution Film.
Specific implementation mode seven：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron The method of mixture, specifically follows the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 60~120 DEG C, is done The dry time is 8~16h, and vacuum degree is 0.05~0.09MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, Ball-milling Time is 2~8h, then crosses 40~200 mesh sieve, is uniformly mixed, obtains mixed powder；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little oxidizing gas for being 1~20mm of Φ, being passed through that pressure is 5~50MPa, oxidizing gas O2Or O2Mixed gas, then Voltage-resistant reactor is attached in water-circulating cooling device, sets theoretical temperatures as 2100~4000 DEG C, reaction pressure is 5~50MPa, Reaction time is 10~600s, and resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 1~60s, is then turned on pressure-resistant anti- Answer device nozzle, Al in voltage-resistant reactor2O3/ZrO2Compounding flux is sprayed onto cooling in the two pairs of rollers of roller equipment, then cleans, dry, It is crushed, ball milling, is sieved using crusher, obtain Al2O3/ZrO2Amorphous and solid solution ceramic micron powder mixture, complete a kind of aluminium Oxygen conbustion synthesis chilling method prepares Al2O3The method of base amorphous and solid solution ceramic micron powder mixture；
Compounding flux is sprayed onto in the two pairs of rollers of roller equipment, and using double roller equipments, roller pressure is 30~70MPa, and roller turns Speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter two pairs of rollers, Water is 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
Specific implementation mode eight：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron The method of mixture, specifically follows the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 60~120 DEG C, is done The dry time is 8~16h, and vacuum degree is 0.05~0.09MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, Ball-milling Time is 2~8h, then crosses 40~200 mesh sieve, is uniformly mixed, obtains mixed powder；Wherein press mass parts The dosage of number Al is 10~40 parts, diluent Al2O3And ZrO2Total dosage be 60~90 parts；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little oxidizing gas for being 1~20mm of Φ, being passed through that pressure is 5~50MPa, oxidizing gas is the O of 5~30MPa2With 0~ The N of 20MPa2Mixed gas, then voltage-resistant reactor is attached in water-circulating cooling device, set theoretical temperatures as 2100~ 4000 DEG C, it lights mixed powder and causes synthetic reaction, then keep the temperature 1~60s, be then turned on voltage-resistant reactor nozzle, pressure resistance reaction Al in device2O3/ZrO2Compounding flux is sprayed onto cooling in the two pairs of rollers of rotating metallic disk or roller equipment, then cleans, dry, uses Crusher crushes, ball milling, and sieving obtains Al2O3/ZrO2Amorphous and solid solution ceramic micron powder mixture complete a kind of alumina combustion Burnt together prepares Al at chilling method2O3The method of base amorphous and solid solution ceramic micron powder mixture；Wherein rotating metallic disk is iron Disk, copper dish or steel disk；
If compounding flux is sprayed onto in rotating metallic disk, rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/ min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water For 20~30L/min, hydraulic pressure is 0.1~0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution Film；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, roller Rotor speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter Two pairs of rollers, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
Specific implementation mode nine：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron The method of mixture, specifically follows the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 60~120 DEG C, is done The dry time is 8~16h, and vacuum degree is 0.05~0.09MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, Ball-milling Time is 2~8h, then crosses 40~200 mesh sieve, is uniformly mixed, obtains mixed powder；Wherein press mass parts The dosage of number Al is 10~40 parts, diluent Al2O3And ZrO2Total dosage be 60~90 parts；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little oxidizing gas for being 1~20mm of Φ, being passed through that pressure is 5~50MPa, oxidizing gas is the O of 5~30MPa2With 0~ The N of 20MPa2Mixed gas, then voltage-resistant reactor is attached in water-circulating cooling device, mixed powder is heated to 25~ 300 DEG C, theoretical temperatures are set as 2100~4000 DEG C, reaction pressure is 5~50MPa, and resistance wire lights mixed powder and causes conjunction At reaction, 1~60s is then kept the temperature, is then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2Compounding flux is sprayed onto It is cooling in the two pairs of rollers of rotating metallic disk or roller equipment, then clean, it is dry, it is crushed, ball milling, is sieved using crusher, obtained Al2O3/ZrO2Amorphous and solid solution ceramic micron powder mixture complete a kind of alumina conbustion synthesis chilling method preparation Al2O3Base is non- Brilliant and solid solution ceramic micron powder mixture method；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
If compounding flux is sprayed onto in rotating metallic disk, rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/ min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water For 20~30L/min, hydraulic pressure is 0.1~0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution Film；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, roller Rotor speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter Two pairs of rollers, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
Specific implementation mode ten：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron The method of mixture, specifically follows the steps below：
One, Al and diluent are put into vacuum drying chamber and are dried, control drying temperature is 60~120 DEG C, dry Time is 8~16h, and vacuum degree is 0.05~0.09MPa, and planetary ball mill is then used to carry out ball milling, and control Ball-milling Time is 2 Then~8h crosses 40~200 mesh sieve, is uniformly mixed, obtains mixed powder；The dosage for wherein pressing mass fraction Al is 10~40 Part, the dosage of diluent is 60~90 parts；Diluent be barium monoxide, iron oxide, vanadium oxide, molybdenum oxide, aluminium oxide, zirconium oxide, Magnesia, calcium oxide, strontium oxide strontia, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, niobium oxide, hafnium oxide, Tantalum oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosia, holimium oxide, One or more of erbium oxide, thulium oxide, ytterbium oxide, luteium oxide and silica mix；Work as Al2O3Base amorphous and solid solution pottery When containing zirconium oxide in porcelain micron powder mixture, Y2O3With ZrO2Molar ratio be (0~15): 100；CeO2With ZrO2Molar ratio be (0~30): 100；MgO and ZrO2Molar ratio be (0~28): 100；CaO and ZrO2Molar ratio be (0~33.45): 100； TiO2With ZrO2Molar ratio be (0~44.41): 100；Sc2O3With ZrO2Molar ratio be (0~20): 100；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little oxidizing gas for being 1~20mm of Φ, being passed through that pressure is 5~50MPa, oxidizing gas is the O of 5~30MPa2With 0~ The N of 20MPa2Mixed gas, then voltage-resistant reactor is attached in water-circulating cooling device, set theoretical temperatures as 2100~ 4000 DEG C, reaction pressure is 5~50MPa, and resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 1~60s, then open Open voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2Compounding flux is sprayed onto the two pairs of rollers of rotating metallic disk or roller equipment Middle cooling, is then cleaned, dry, is crushed using crusher, ball milling, is sieved, and Al is obtained2O3/ZrO2Amorphous and solid solution ceramic are micro- Rice flour mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
If compounding flux is sprayed onto in rotating metallic disk, rotating metallic disk radius is 50~200cm, and rotating speed is 60~150r/ min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water For 20~30L/min, hydraulic pressure is 0.1~0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution Film；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, roller Rotor speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter Two pairs of rollers, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
Specific implementation mode 11：Unlike one of present embodiment and specific implementation mode one to ten：The pressure resistance Reaction vessel includes reactor 1, tabletting 4, nozzle 5, nozzle holder 6, sealing preload piece 8, upper slide 10,11 and of lower skateboard Actuator 9 is provided with two-stage ladder circular hole along the device bottom thickness direction of reactor 1, and the first ladder circular hole 2 is located at the second ladder circle The diameter of the top in hole 3 and the first ladder circular hole 2 is more than the diameter of the second ladder circular hole 3；
The nozzle holder 6 forms coaxial integral structure by circular plate type frame body portion 6-1 and cylindrical portion 6-2, along nozzle branch The central axes of frame 6 are provided with jack 6-3, and the end face of cylindrical portion 6-2 is provided with ring groove 6-4, and nozzle holder 6 inserts embedded two-stage ladder In circular hole, cylindrical portion 6-2 and the second ladder circular hole 3 coordinate, and circular plate type frame body portion 6-1 and the first ladder circular hole 2 coordinate, circular plate type The lower surface of frame body portion 6-1 is overlapped on the step surface of two-stage ladder circular hole, and ring groove 6-4 is embedded with sealing preload piece 8；
The tabletting 4 is arranged in the upper surface of circular plate type frame body portion 6-1, and tabletting 4 and 2 screw thread of the first ladder circular hole connect It connects, the center of tabletting 4 is provided with tabletting through-hole；
Nozzle 5 is arranged in the tabletting through-hole of tabletting 4 and the jack 14 of nozzle holder 6, and nozzle 5 is built-in with graphite core, spray The bottom surface of mouth 5 is against the upper surface of sealing preload piece 8, and the upper face of upper slide 10 is in contact with the device bottom outer surface of reactor 1, The contact of lower skateboard 11, which is arranged on the lower section of upper slide 10, upper slide 10 and lower skateboard 11, has slide plate through-hole, and slide plate is logical The aperture in hole ensures that sealing preload piece 8 passes through, and the slide plate through-hole face on lower skateboard 11 seals preload piece 8, and upper slide 10 is by dragging The dynamic driving of device 9 moves horizontally.
The content of present invention is not limited only to the content of the respective embodiments described above, the group of one of them or several specific implementation modes Contract sample can also realize the purpose of invention.
Effect of the present invention is verified using following embodiments
Following embodiment be all made of pressure-resistant reaction vessel progress, the pressure-resistant reaction vessel include reactor 1, resistance wire 2, The upper cover inside of nozzle 5, sealing preload piece 8, upper slide 10, lower skateboard 11 and actuator 9, reactor 1 is equipped with resistance wire 2, Device bottom thickness direction along reactor 1 is provided with vertical through-hole 20, and nozzle 5 is screwed in vertical through-hole 20 and is connected through a screw thread, perpendicular The circumferential direction of 20 times spouts of clear opening is provided with preload piece slot, and sealing preload piece 8 is inserted in embedded preload piece slot, and sealing preload piece 8 is vertical to be cut Face takes the shape of the letter U, and the upper face of upper slide 10 is in contact with the device bottom outer surface of reactor 1, and the contact of lower skateboard 11 is arranged in upper slide Slide plate through-hole is had on 10 lower section, upper slide 10 and lower skateboard 11, the aperture of slide plate through-hole ensures that sealing preload piece 8 is logical It crosses, the slide plate through-hole face on lower skateboard 11 seals preload piece 8, and upper slide 10 is moved horizontally by the driving of actuator 9.
Embodiment one：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 80 DEG C, when dry Between be 10h, vacuum degree 0.06MPa, then use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, when ball milling Between be 3h, then sieve with 100 mesh sieve, be uniformly mixed, obtain mixed powder；Al is 131.79g, Al in mixed powder2O3For 399.22g、ZrO2For 468.98g,
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 8mm, being passed through that pressure is 13MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 10s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2It is compound Melt is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, then planetary ball mill is used to carry out Ball milling, control ball material mass ratio are 3: 1, Ball-milling Time 4h, and sieving obtains Al2O3/ZrO2Amorphous and solid solution ceramic micron Powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3The side of base amorphous and solid solution ceramic micron powder mixture Method；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 100r/min；Rotating metallic One side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 30L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane.
The surface microscopic SEM pictures of powder and micron are as shown in figure 5, from Fig. 5 superfines after the crushing of embodiment one, ball milling SEM pictures can be seen that powder size in sub-micron between several microns, granularity is more uniform.These results further illustrate： By high-temperature heating device by Al2O3/ZrO2Composite granule melts, then is cooled down by pivoting rail, copper, steel disk, can prepare height The micron powder of purity；And it is at low cost, environmentally protective, be suitable for large-scale industrial production.
To amorphous and solid solution micro-powder through hot pressed sintering densification, the material of preparation is subjected to three-point bending examination Test tries, and performance is：Fracture toughness 8.35MPam1/2, bending strength 710MPa.
Embodiment two：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 80 DEG C, when dry Between be 10h, vacuum degree 0.06MPa, then use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, when ball milling Between be 3h, then cross 40 mesh sieve, be uniformly mixed, obtain mixed powder；Al is 207.69g, Al in mixed powder2O3For 554.08g、ZrO2For 238.24g,
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 3mm, being passed through that pressure is 22MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 20s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2It is compound Melt is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, then planetary ball mill is used to carry out Ball milling, control ball material mass ratio are 3: 1, Ball-milling Time 3h, and sieving obtains Al2O3/ZrO2Amorphous and solid solution ceramic micron Powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3The side of base amorphous and solid solution ceramic micron powder mixture Method；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane.
Embodiment three：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2And stabilizer Y2O3It is put into vacuum drying chamber and is dried, control drying temperature It is 100 DEG C, drying time 8h, vacuum degree 0.05MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, then Ball-milling Time 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Al is in mixed powder 154.76g、Al2O3For 367.14g, ZrO2For 478.10g, Y2O3For 175.79g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 4mm, being passed through that pressure is 15MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 10s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2 (Y2O3) compounding flux is sprayed onto in the two pairs of rollers of roller equipment cooling, then cleans, it is dry, it is crushed, ball milling, is sieved using crusher, Obtain Al2O3/ZrO2(Y2O3) amorphous and solid solution ceramic micron powder mixture, it completes a kind of alumina conbustion synthesis chilling method and prepares Al2O3The method of base amorphous and solid solution ceramic micron powder mixture；
Compounding flux is sprayed onto in the two pairs of rollers of roller equipment, and using double roller equipments, roller pressure 50MPa, roller rotating speed is 2000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2(Y2O3) compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter two pairs of rollers, water For 25L/min, hydraulic pressure 0.3MPa, extruding forms Al2O3/ZrO2(Y2O3) amorphous and solid solution strip.
Example IV：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2And stabilizer CeO2It is put into vacuum drying chamber and is dried, control drying temperature It is 100 DEG C, drying time 8h, vacuum degree 0.05MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, then Ball-milling Time 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Al is in mixed powder 178.62g、Al2O3For 334.37g, ZrO2For 487.01g, CeO2For 204.42g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 8mm, being passed through that pressure is 20MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 10s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2 (CeO2) compounding flux is sprayed onto in rotating metallic disk cooling, then cleans, it is dry, it is crushed using crusher, then uses planet Ball mill carries out ball milling, and control ball material mass ratio is 3: 1, Ball-milling Time 3h, and sieving obtains Al2O3/ZrO2(CeO2) amorphous With solid solution ceramic micron powder mixture, a kind of alumina conbustion synthesis chilling method preparation Al is completed2O3Base amorphous and solid solution ceramic The method of micron powder mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2(CeO2) compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/ Min, hydraulic pressure 0.5MPa solidify to form Al in rotating metallic panel surface2O3/ZrO2(CeO2) amorphous and solid solution membrane.
Embodiment five：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 100 DEG C, when dry Between be 8h, vacuum degree 0.05MPa, then use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, when ball milling Between be 3h, then cross 60 mesh sieve, be uniformly mixed, obtain mixed powder；It is Al 168.97g, ZrO wherein in mixed powder2For 483.41g、Al2O3For 347.62g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 4mm, being passed through that pressure is 15MPa2With the N of 3MPa2Mixed gas, voltage-resistant reactor is then attached to recirculated water cooling In device, resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 10s, is then turned on voltage-resistant reactor nozzle, and pressure resistance is anti- Answer Al in device2O3/ZrO2Compounding flux is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, uses Planetary ball mill carries out ball milling, and control ball material mass ratio is 3: 1, Ball-milling Time 3h, ball milling, and sieving obtains Al2O3/ZrO2It is non- Brilliant and solid solution ceramic micron powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution pottery The method of porcelain micron powder mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane.
Embodiment six：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 100 DEG C, when dry Between be 8h, vacuum degree 0.05MPa, then use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, when ball milling Between be 3h, then cross 60 mesh sieve, be uniformly mixed, obtain mixed powder；Be wherein Al in mixed powder it is 1317.3g, ZrO2For 4697.8g、Al2O3For 3984.9g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 6mm, being passed through that pressure is 13MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, by mixed powder plus Heat to 300 DEG C, light mixed powder and cause synthetic reaction, then keeps the temperature 10s, is then turned on voltage-resistant reactor nozzle, resistance to by resistance wire Press Al in reactor2O3/ZrO2Compounding flux is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, Ball milling is carried out using planetary ball mill, control ball material mass ratio is 3: 1, Ball-milling Time 3h, ball milling, and sieving obtains Al2O3/ ZrO2Amorphous and solid solution ceramic micron powder mixture complete a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid The method of solution ceramics micron powder mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane.
Embodiment seven：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, MgO and HfO2It is put into vacuum drying chamber and is dried, control drying temperature is 80 DEG C, drying time For 12h, vacuum degree 0.07MPa, planetary ball mill is then used to carry out ball milling, control ball material mass ratio is 3: 1, Ball-milling Time For 3h, 60 mesh sieve is then crossed, is uniformly mixed, obtains mixed powder；Wherein be Al in mixed powder it is that 145.20g, MgO are 429.56g、HfO2For 425.23g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 4mm, being passed through that pressure is 15MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 10s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/MgO/HfO2 Compounding flux is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, is carried out using planetary ball mill Ball milling, control ball material mass ratio are 3: 1, Ball-milling Time 3h, ball milling, and sieving obtains Al2O3/MgO/HfO2Amorphous and solid solution Ceramic micron powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron are mixed The method for closing object；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/MgO/HfO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/ Min, hydraulic pressure 0.5MPa solidify to form Al in rotating metallic panel surface2O3/MgO/HfO2Amorphous and solid solution membrane.
Embodiment eight：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al and TiO2It is put into vacuum drying chamber and is dried, control drying temperature is 80 DEG C, and drying time is Then 12h, vacuum degree 0.07MPa use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, and Ball-milling Time is Then 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Be wherein Al in mixed powder it is 114.2g, TiO2For 885.8g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 8mm, being passed through that pressure is 10MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, lights mixed powder Cause synthetic reaction, then keep the temperature 10s, is then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/TiO2Compounding flux sprays To cooling in rotating metallic disk, then clean, it is dry, it is crushed using crusher, ball milling, control ball is carried out using planetary ball mill Expect that mass ratio is 3: 1, Ball-milling Time 3h, ball milling, sieving, acquisition Al2O3/TiO2Amorphous and the mixing of solid solution ceramic powder and micron Object completes a kind of alumina conbustion synthesis chilling method preparation Al2O3The method of base amorphous and solid solution ceramic micron powder mixture；Its Middle rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/TiO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/TiO2Amorphous and solid solution membrane.
Embodiment nine：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al and Al2O3It is put into vacuum drying chamber and is dried, control drying temperature is 100 DEG C, and drying time is Then 8h, vacuum degree 0.05MPa use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, and Ball-milling Time is Then 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；It is Al 136g, Al wherein in mixed powder2O3For 864g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 6mm, being passed through that pressure is 13MPa2With the mixed gas of the air of 3MPa, voltage-resistant reactor is then attached to cycle In water cooling plant, resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 15s, is then turned on voltage-resistant reactor nozzle, resistance to Press Al in reactor2O3Melt is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, using planet Ball mill carries out ball milling, and control ball material mass ratio is 3: 1, Ball-milling Time 3h, ball milling, and sieving obtains Al2O3Amorphous and solid solution Body ceramics micron powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic powder and micron The method of mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, hydraulic pressure are 0.5MPa solidifies to form Al in rotating metallic panel surface2O3Amorphous and solid solution membrane.
Embodiment ten：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and solid solution ceramic micron powder mixture Method, specifically follow the steps below：
One, by Al, Al2O3And ZrO2And stabilizer Y2O3It is put into vacuum drying chamber and is dried, control drying temperature It is 100 DEG C, drying time 8h, vacuum degree 0.05MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, then Ball-milling Time 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Al is in mixed powder 179.39g、Al2O3For 587.43g, ZrO2For 233.18g, Y2O3For 34.25g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 10mm, being passed through that pressure is 20MPa2With the N of 2MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, electricity Resistance silk lights mixed powder and causes synthetic reaction, then keeps the temperature 10s, is then turned on voltage-resistant reactor nozzle, in voltage-resistant reactor Al2O3/ZrO2(Y2O3) compounding flux is sprayed onto in the two pairs of rollers of roller equipment cooling, then cleans, it is dry, it is crushed using crusher, Ball milling, sieving obtain Al2O3/ZrO2(Y2O3) amorphous and solid solution ceramic micron powder mixture, complete a kind of alumina conbustion synthesis Chilling method prepares Al2O3The method of base amorphous and solid solution ceramic micron powder mixture；
Compounding flux is sprayed onto in the two pairs of rollers of roller equipment, and using double roller equipments, roller pressure 50MPa, roller rotating speed is 2000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2(Y2O3) compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter two pairs of rollers, water For 25L/min, hydraulic pressure 0.3MPa, extruding forms Al2O3/ZrO2(Y2O3) amorphous and solid solution strip.
Embodiment 11：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and the mixing of solid solution ceramic powder and micron The method of object, specifically follows the steps below：
One, by Al, Al2O3And ZrO2And stabilizer Y2O3It is put into vacuum drying chamber and is dried, control drying temperature It is 100 DEG C, drying time 8h, vacuum degree 0.05MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, then Ball-milling Time 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Al is in mixed powder 142.89g、Al2O3For 518.54g, ZrO2For 338.56g, Y2O3For 18.66g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 3mm, being passed through that pressure is 14MPa2With 2MPa air, then voltage-resistant reactor is attached in water-circulating cooling device, it will Mixed powder is heated to 200 DEG C, and resistance wire lights mixed powder and causes synthetic reaction, then keeps the temperature 15s, is then turned on pressure-resistant reaction Device nozzle, Al in voltage-resistant reactor2O3/ZrO2(Y2O3) compounding flux is sprayed onto in the two pairs of rollers of roller equipment cooling, it then cleans, does It is dry, it is crushed, ball milling, is sieved using crusher, obtain Al2O3/ZrO2(Y2O3) amorphous and solid solution ceramic micron powder mixture, it is complete Al is prepared at a kind of alumina conbustion synthesis chilling method2O3The method of base amorphous and solid solution ceramic micron powder mixture；
Compounding flux is sprayed onto in the two pairs of rollers of roller equipment, and using double roller equipments, roller pressure 50MPa, roller rotating speed is 2000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2(Y2O3) compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter two pairs of rollers, water For 30L/min, hydraulic pressure 0.3MPa, extruding forms Al2O3/ZrO2(Y2O3) amorphous and solid solution strip.
To amorphous and solid solution micron powder through hot pressed sintering densification, the material of preparation is subjected to three-point bending examination Test tries, and performance is：Fracture toughness 9.25MPam1/2, bending strength 920MPa.
Embodiment 12：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and the mixing of solid solution ceramic powder and micron The method of object, specifically follows the steps below：
One, by Al, Al2O3And ZrO2And stabilizer CeO2It is put into vacuum drying chamber and is dried, control drying temperature It is 100 DEG C, drying time 8h, vacuum degree 0.05MPa, then planetary ball mill is used to carry out ball milling, control ball material quality Than being 3: 1, then Ball-milling Time 3h crosses 60 mesh sieve, is uniformly mixed, obtains mixed powder；Al is in mixed powder 114.11g、Al2O3For 3.56g, ZrO2For 882.32g, CeO2For 129.54g.
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 6mm, being passed through that pressure is 12MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 10s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2 (CeO2) compounding flux is sprayed onto in rotating metallic disk cooling, then cleans, it is dry, it is crushed using crusher, then uses planet Ball mill carries out ball milling, and control ball material mass ratio is 3: 1, Ball-milling Time 3h, and sieving obtains Al2O3/ZrO2(CeO2) amorphous With solid solution ceramic micron powder mixture, a kind of alumina conbustion synthesis chilling method preparation Al is completed2O3Base amorphous and solid solution ceramic The method of micron powder mixture；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2(CeO2) compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/ Min, hydraulic pressure 0.5MPa solidify to form Al in rotating metallic panel surface2O3/ZrO2(CeO2) amorphous and solid solution membrane.
To amorphous and solid solution micron powder through hot pressed sintering densification, the material of preparation is subjected to three-point bending examination Test tries, and performance is：Fracture toughness 13.15MPam1/2, bending strength 1020MPa.
Embodiment 13：A kind of alumina conbustion synthesis chilling method preparation Al2O3Base amorphous and the mixing of solid solution ceramic powder and micron The method of object, specifically follows the steps below：
One, by Al, Al2O3And ZrO2It is put into vacuum drying chamber and is dried, control drying temperature is 100 DEG C, when dry Between be 8h, vacuum degree 0.05MPa, then use planetary ball mill to carry out ball milling, control ball material mass ratio is 3: 1, when ball milling Between be 3h, then cross 60 mesh sieve, be uniformly mixed, obtain mixed powder；It is Al 147.26g, ZrO wherein in mixed powder2For 680.39g、Al2O3For 172.35g；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, the spout ruler of nozzle The very little O for being Φ 3mm, being passed through that pressure is 15MPa2, then voltage-resistant reactor is attached in water-circulating cooling device, resistance wire is lighted mixed It closes powder and causes synthetic reaction, then keep the temperature 20s, be then turned on voltage-resistant reactor nozzle, Al in voltage-resistant reactor2O3/ZrO2It is compound Melt is sprayed onto cooling in rotating metallic disk, then cleans, dry, is crushed using crusher, and ball milling is carried out using planetary ball mill, Control ball material mass ratio is 3:1, Ball-milling Time 3h, ball milling, sieving obtain Al2O3/ZrO2Amorphous and solid solution ceramic micron Powder mixture completes a kind of alumina conbustion synthesis chilling method preparation Al2O3The side of base amorphous and solid solution ceramic micron powder mixture Method；Wherein rotating metallic disk is iron pan, copper dish or steel disk；
Compounding flux is sprayed onto in rotating metallic disk, and rotating metallic disk radius is 80cm, rotating speed 90r/min；Rotating metallic One side spray Al of disk2O3/ZrO2Compounding flux, corresponding another side spray high pressure, high-velocity flow supplement heat rejecter, water 20L/min, water Pressure is 0.5MPa, solidifies to form Al in rotating metallic panel surface2O3/ZrO2Amorphous and solid solution membrane.

Claims (6)

1. a kind of method that alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic micron powder mixture, It is characterized in that this method specifically carries out according to the following steps：
One, aluminium powder and diluent are dried, are uniformly mixed, obtain mixed powder；It is 10~40 according to mass fraction aluminium powder Part, diluent are 60~90 parts；
Two, the mixed powder that step 1 obtains is fitted into voltage-resistant reactor of the lower end equipped with nozzle, is passed through oxidizing gas, point It fires mixed powder and causes synthetic reaction, heat preservation is then turned on voltage-resistant reactor nozzle, compounding flux is sprayed onto rotation in voltage-resistant reactor Turn cooling in the two pairs of rollers of metal dish or roller equipment, then crushes, ball milling, obtain Al2O3Base amorphous and solid solution ceramic powder and micron Mixture completes the side that a kind of alumina conbustion synthesis chilling method prepares alumina base amorphous and solid solution ceramic micron powder mixture Method.
2. a kind of alumina conbustion synthesis chilling method according to claim 1 prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture, it is characterised in that diluent described in step 1 is barium monoxide, iron oxide, vanadium oxide, molybdenum oxide, oxidation Aluminium, zirconium oxide, magnesia, calcium oxide, strontium oxide strontia, scandium oxide, titanium oxide, chromium oxide, cobalt oxide, nickel oxide, yttrium oxide, oxidation Niobium, hafnium oxide, tantalum oxide, lanthana, cerium oxide, praseodymium oxide, neodymia, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, oxidation One kind in dysprosium, holimium oxide, erbium oxide, thulium oxide, ytterbium oxide, luteium oxide and silica or in which several mixing.
3. a kind of alumina conbustion synthesis chilling method according to claim 1 prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture, it is characterised in that work as Al2O3When containing zirconium oxide in base amorphous and solid solution ceramic micron powder mixture, Y2O3With ZrO2Molar ratio be (0~15): 100；CeO2With ZrO2Molar ratio be (0~30): 100；MgO and ZrO2Mole Than for (0~28): 100；CaO and ZrO2Molar ratio be (0~33.45): 100；TiO2With ZrO2Molar ratio be (0~ 44.41):100；Sc2O3With ZrO2Molar ratio be (0~20): 100.
4. a kind of alumina conbustion synthesis chilling method according to claim 1 prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture, it is characterised in that it is O to be passed through oxidizing gas2Or oxidizing gas is O2With the mixing of air, or Oxidizing gas is O2And N2Mixing or oxidizing gas be O2, air and N2Mixing.
5. a kind of alumina conbustion synthesis chilling method according to claim 1 prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture, it is characterised in that mixed powder in step 2 is heated to 25~300 DEG C, resistance wire lights mixed powder Body causes synthetic reaction, then keeps the temperature 1~60s.
6. a kind of alumina conbustion synthesis chilling method according to claim 1 prepares alumina base amorphous and solid solution ceramic is micro- The method of rice flour mixture, it is characterised in that if compounding flux is sprayed onto in rotating metallic disk in step 2, rotating metallic disk radius For 50~200cm, rotating speed is 60~150r/min；One side spray Al of rotating metallic disk2O3/ZrO2Compounding flux, corresponding another side spray High pressure, high-velocity flow supplement heat rejecter, water are 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, solidifying in rotating metallic panel surface Solid is at Al2O3/ZrO2Amorphous and solid solution membrane；
If compounding flux is sprayed onto in the two pairs of rollers of roller equipment, using double roller equipments, roller pressure is 30~70MPa, and roller turns Speed is 100~4000rpm；Al is sprayed among two pairs of rollers2O3/ZrO2Compounding flux, two side spray high pressures, high-velocity flow supplement heat rejecter two pairs of rollers, Water is 20~30L/min, and hydraulic pressure is 0.1~0.5MPa, and extruding forms Al2O3/ZrO2Amorphous and solid solution strip.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105647A (en) * 2021-10-26 2022-03-01 广州大学 Rapid preparation of multi-scale nano composite structure beta-FeSi by atomization and rapid freezing crystallization method2Method for producing thermoelectric material

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4491482A (en) * 1982-03-29 1985-01-01 Kureha Kagaku Kogyo Kabushiki Kaisha Powdery material of minute composite ceramic particles having a dual structure and a process and an apparatus producing thereof
JPH04359068A (en) * 1991-06-04 1992-12-11 Tokai Carbon Co Ltd Carbon black producing furnace
DE10061016A1 (en) * 2000-12-08 2002-07-04 Degussa New aluminum oxide-germanium dioxide-silicon dioxide mixed oxide is used as a catalyst support or precursor for e.g. green moldings for optical fiber or zero glass production
CN101351420A (en) * 2005-12-30 2009-01-21 3M创新有限公司 Ceramic materials and methods of making and using the same
CN101956119A (en) * 2010-09-19 2011-01-26 北京科技大学 Preparation method of prealloying powder for dispersion strengthening metal by low-temperature combustion synthesis method
CN103304222A (en) * 2013-05-31 2013-09-18 哈尔滨工业大学 Method for combustion-synthesis casting of Al2O3/ZrO2 eutectic ceramic
CN103787655A (en) * 2012-10-29 2014-05-14 河北联合大学 Method for preparing ZrN-Al2O3-ZrO2 multiphase ceramic material by Al-ZrO2-N2 reactive sintering
CN104193311A (en) * 2014-09-05 2014-12-10 哈尔滨工业大学 Reaction spraying preparation method of oxide eutectic ceramic amorphous powder
CN106629799A (en) * 2016-10-25 2017-05-10 乌鲁木齐市三锐科技有限公司 Method for synthesizing aluminium oxide powder by using combustion method
CN107601537A (en) * 2017-11-01 2018-01-19 乌鲁木齐市三锐科技有限公司 Rafifinal atomization explosion method prepares the method and special purpose device of high-purity alumina powder

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4491482A (en) * 1982-03-29 1985-01-01 Kureha Kagaku Kogyo Kabushiki Kaisha Powdery material of minute composite ceramic particles having a dual structure and a process and an apparatus producing thereof
JPH04359068A (en) * 1991-06-04 1992-12-11 Tokai Carbon Co Ltd Carbon black producing furnace
DE10061016A1 (en) * 2000-12-08 2002-07-04 Degussa New aluminum oxide-germanium dioxide-silicon dioxide mixed oxide is used as a catalyst support or precursor for e.g. green moldings for optical fiber or zero glass production
CN101351420A (en) * 2005-12-30 2009-01-21 3M创新有限公司 Ceramic materials and methods of making and using the same
CN101956119A (en) * 2010-09-19 2011-01-26 北京科技大学 Preparation method of prealloying powder for dispersion strengthening metal by low-temperature combustion synthesis method
CN103787655A (en) * 2012-10-29 2014-05-14 河北联合大学 Method for preparing ZrN-Al2O3-ZrO2 multiphase ceramic material by Al-ZrO2-N2 reactive sintering
CN103304222A (en) * 2013-05-31 2013-09-18 哈尔滨工业大学 Method for combustion-synthesis casting of Al2O3/ZrO2 eutectic ceramic
CN104193311A (en) * 2014-09-05 2014-12-10 哈尔滨工业大学 Reaction spraying preparation method of oxide eutectic ceramic amorphous powder
CN106629799A (en) * 2016-10-25 2017-05-10 乌鲁木齐市三锐科技有限公司 Method for synthesizing aluminium oxide powder by using combustion method
CN107601537A (en) * 2017-11-01 2018-01-19 乌鲁木齐市三锐科技有限公司 Rafifinal atomization explosion method prepares the method and special purpose device of high-purity alumina powder

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
JIAYU PAN等: "Solidification mechanism and microstructure evolution of Al2O3-ZrO2 ceramic coating prepared by combustion synthesis and thermal explosion spraying", 《CERAMICS INTERNATIONAL》 *
SEYED ALI TAYEBIFARD等: "Synthesis of Al2O3-ZrO2 Nanocomposite by Mechanical Activated Self-propagating High Temperature Synthesis(MASHS) and Ignited via Laser", 《TRANSACTIONS：A BASICS》 *
YONGTING ZHENG等: "Microstructure and mechanism of Al2O3–ZrO2 eutectic coating prepared by combustion-assisted thermal explosion spraying", 《APPLIED SURFACE SCIENCE》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105647A (en) * 2021-10-26 2022-03-01 广州大学 Rapid preparation of multi-scale nano composite structure beta-FeSi by atomization and rapid freezing crystallization method2Method for producing thermoelectric material

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