CN1125794C - Process for synthesizing composite ceramic powder body - Google Patents
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- CN1125794C CN1125794C CN99100590A CN99100590A CN1125794C CN 1125794 C CN1125794 C CN 1125794C CN 99100590 A CN99100590 A CN 99100590A CN 99100590 A CN99100590 A CN 99100590A CN 1125794 C CN1125794 C CN 1125794C
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Abstract
The present invention relates to a novel method for synthesizing polycomponent ceramic composite powder, which comprises: an organic monomer and a crosslinking agent which can form hydrogel are added to quickly gelatinize water slurry evenly ball-milled under the action of an initiator in an in-situ mode so as to maintain the evenness of the polycomponent ingredients; the wet gelatin block is dewatered, dried and calcined to synthesize the desired ceramic composite powder. Compared with the traditional solid-phase reaction synthesizing method, the present invention has the advantages of high efficiency, low synthesis temperature, and good quality and easy crushing of the synthesized powder; compared with the polyacrylamide liquid-phase gelatin method, and the chemical coprecipitation method or the sol-gel method, the present invention has the advantages of convenient raw material source, low cost, convenient operation, strong applicability, small environmental pollution and convenient industrial production.
Description
The invention belongs to field of inorganic nonmetallic material, relate to the improvement of multicomponent ceramic composite powder solid state reaction synthetic technology.
Most function ceramics and the employed powder raw material of functional coating all are the multicomponent composite granules, and the suitability for industrialized production of these powders normally adopts wet ball grinding mixing, drying, briquetting synthetic through the solid reaction process calcining then.In the uniform slurry dewatering drying process of wet method mix grinding, the multicomponent powder is because of the difference of proportion, suspension, the constituent element sedimentation appears easily, generally need to reduce the uneven components that this process causes by press filtration, spraying or cold method drying, this must increase facility investment and improve the technology cost.When calcining is synthetic, if carry out with natural accumulation mode, between the multicomponent powder contact bad, efficient is low and make easily that muddy composition scatters and disappears; Can improve reaction efficiency if calcine again behind the compound stalk forming, but because the inhomogeneous local sintering caking that causes easily of briquetting density.In a word, shortcoming such as traditional synthesis by solid state reaction produces that composite granule exists that each constituent element composition is difficult to mix, synthesis temperature height, powder are thick, and usually can not get required phase composite.
The preparation that develops into the polycomponent superfine powder of the method for liquid phase powder process in recent years provides good novel method.Because each components contents can accurately be controlled in the liquid phase, and can realize the uniform mixing on molecule, the atomic level, the powder that obtains has good performance, thereby becomes present laboratory and the industrial method that comparatively extensively adopts.In the liquid phase production of polycomponent functional ceramic powder, coprecipitation method and sol-gel method are used morely.The coprecipitation method raw materials cost is low, is easy to prepare the multicomponent system powder, but its coagulation process and filtration water washing process repeatedly are quite time-consuming, loaded down with trivial details.And for the polycomponent compound system, because of different metal ion in the solution generates sedimentary condition difference, it almost is impossible allowing the different kinds of ions of composition material precipitate simultaneously.Simultaneously, different throw out solubility product differences, the loss that may generating unit in the water washing process divides constituent element causes the inaccurate of composition, influences the performance of synthetic powder.Sol-gel method is utilized good dispersed and suitable dehydration, the drying process of colloidal particle, can obtain the nanometer superfine powder body.But it is a raw material with the more expensive metal alkoxide of price all generally, and cost height, cycle are long, and the control of sol-gel process also has certain difficulty, if dewatering was not at that time, polycondensation, caking phenomenon occur, cause the particulate hard aggregation, so its suitability for industrialized production has been subjected to considerable restraint.
French A.Douy in 1989 and P.Odier have proposed a kind of method (Mat Res Bull. of polyacrylamide liquid phase gel method synthesize ceramic oxide compound superfine powder, Vol.24, pp.11191126,1989, Printed in the USA, Pergamon Press plc.), it is raw material that this method adopts water miscible inorganic salt (being generally nitrate, villaumite etc.), dissolve in and contain in the part lemon aqueous acid, adjust the pH value of solution value with ammoniacal liquor, add organic monomer and linking agent simultaneously, obtain liquid gel under certain condition.Dehydration then, dry, calcining synthesizing ceramic powder.Domestic Lee leap [functional materials, 1992, Vol.23 (3), P.157], people such as Li Qiang [first whole nation nano material utilisation technology exchanging meeting data compilation, 1997, P.130] Mount Putuo has also prepared multiple superfine powder with this kind liquid phase gel method.But it is raw material that this technology must adopt water-soluble salt, makes its range of application be subjected to certain limitation.Simultaneously, part is to add in the ratio of each valency of metal ionic in conjunction with a part citric acid, and consumption is very big, and is that maintenance solution is neutrality or weakly alkaline, also need add a large amount of ammoniacal liquor.This has not only increased cost greatly, and calcining can decomposite a large amount of corrodibility obnoxious flavour such as NH when synthetic
4Cl, HCl, HNO
3, Cl
2, NO, NO
2Deng, badly damaged body of heater, heating member, and cause environmental pollution, be difficult to be applied to suitability for industrialized production.
The objective of the invention is: propose a kind of multicomponent composite granule synthetic novel method---gel synthesis by solid state reaction, to overcome shortcoming such as the loaded down with trivial details and cost height of washing, filter operation that multicomponent that traditional solid reaction process exists disperses uneven problem of bringing and conventional liquid phase method to exist, simultaneously, harmful etchant gas damage equipment and the problem of environment pollution caused of avoiding above-mentioned liquid phase gel method to bring.
Technical scheme of the present invention is: a kind of process for synthesizing composite ceramic powder body is characterized in that adopting following processing step:
1, employing and traditional essentially identical starting material of synthesis by solid state reaction, wherein trace additives adopts water soluble salt, with the starting material of desiring synthetic powder in accordance with regulations proportioning be prepared into the water slip and carry out ball milling, ratio of grinding media to material is 1: 1～5: 1, amount of water is 20～200% of a raw material weight, and the ball milling time is 1～10O hour;
2, in 0.5～15 hour before the ball milling discharging, in slip, add organic monomer and linking agent, organic monomer be acrylamide or Methacrylamide one of them, linking agent be methylene-bisacrylamide or many ethyleneglycol dimethacrylates one of them, total add-on of organic monomer and linking agent is 1～10% of a raw material weight, and the weight ratio of organic monomer and linking agent is 3: 1～30: 1;
3, the slip behind the ball milling is placed container, add initiator, add-on is 0.1～0.5% of an organic monomer weight, stirs, initiator is one of following material: ammonium persulphate or tetrazo [ether propane] hydrochloric acid is mixed with 5～20% the aqueous solution during use;
4, one of them makes slurry gelization to adopt two kinds of methods of following first, second:
Party A's method: add Tetramethyl Ethylene Diamine in slip, add-on is 0.05～0.3% of an acrylamide weight, and place the back that stirs, and makes its natural gelation;
Party B's method: slip is heated to 40～80 ℃, makes its gelation;
5, the wet gel base substrate is taken out drying and dehydrating in container;
6, dried gel piece is placed calcining furnace be heated to the synthesis temperature of regulation, the insulation certain hour obtains required synthetic powder agglomates.
Compare with traditional synthesis by solid state reaction, the present invention has many advantages.At first, the present invention is by adding organic monomer and linking agent, makes slip generation home position polymerization reaction form gelinite, speed of response can be very fast, thereby makes gelinite keep the uniformly dispersed of each component in the mixed slurry substantially, is not easy to occur density gradient.Simultaneously, because gelation realizes by organic monomer and linking agent polymerization reaction take place formation macromolecule network structure, irrelevant with the synthetic powder raw material, both can use the water-soluble metal salt, also can use non-water-soluble metal oxide, metal-salt or contain the acids that needs constituent element, particularly the homodisperse of trace element and low temperature are synthetic is very favorable for polycomponent for this.In addition, gelation process is very easy to control, and the organism that is added is general only to be about 3% of solid material, gets final product complete burn off at 600 ℃, and left space helps to hinder the sintering alligatoring of raw material powder behind the macromolecule network structure burn off, and the powder agglomates that obtains after the calcining is loose easily to be pulverized.And compare with chemical coprecipitation, sol-gel method and polyacrylamide liquid phase gel method, raw material sources of the present invention are convenient, cost is low, easy and simple to handle, universality is strong, environmental pollution is little, is applicable to industrialized production.
Description of drawings.
Fig. 1 is that the XRD spectrum of the synthetic magnesium titanate powder of different process compares.
Below the present invention is described in detail.Salt and acid that the present invention uses metal oxide, oxyhydroxide and do not produce or produce less obnoxious flavour are raw material, be mixed with earlier corresponding water slip by a certain percentage, add gel organic monomer and linking agent, carry out the quick in situ polyreaction under certain condition, form the gel piece that contains multicomponent solid phase raw material.Cross the ceramic powder that calcining generation solid state reaction obtains requiring after dehydrate the traffic of burn off organism.The main points of technology of the present invention are:
The first, employing and traditional essentially identical starting material of synthesis by solid state reaction.But for trace additives, should use water soluble salt, so that guarantee that batch mixing is even.On the other hand, under the condition that does not increase material cost, with the metal oxide that does not produce or produce less in oxyhydroxide obnoxious flavour, that contain required metallic element, oxalate, carbonate, metatitanic acid, the boric acid material replacement raw material, make the solid state reaction building-up process be easy to carry out to utilize oxide compound newly-generated in its calcination process to have greater activity as far as possible.These raw materials only produce H when decomposing
2O, CO
2Deng gas, and do not produce NH
4Cl, HCl, HNO
3, Cl
2, NO, NO
2Etc. the corrodibility obnoxious flavour, can reduce pollution to environment.
The second, with water be medium, make various raw material refinements and mix by abundant ball milling.Can between 1: 1～5: 1, choose ratio of grinding media to material according to levigate and principle mixing, the add-on of water can be material heavy 20～200%, the time of ball milling is 1～100 hour.For reducing water consumption and improving grinding efficiency, can add raw material weight 0.1～0.5%, can not introduce impurity and at when calcining all kinds of dispersion agents of burn off fully, as organic electrolyte dispersion agents such as polyacrylate, poly-methyl acrylate, carbonyl hydrochlorate, Citrate trianions.
Three, before discharging, add the organic monomer to form hydrogel under certain condition such as acrylamide, Methacrylamide etc. and linking agent such as methylene radical acrylamide, many ethyleneglycol dimethacrylates etc. again in 0.5～15 hour.Both ratios can be chosen between 3: 1～30: 1.Total add-on for material heavy 1～10%., mix grinding time thin in the material powder granularity less than 15 hours situation under, organic monomer and linking agent also can add ball milling simultaneously with raw material.
Four, ball milling is the good slip that has organic monomer and linking agent is poured in the container, adds the initiator such as the aqueous solution such as ammonium persulphate, tetrazo [ether propane] hydrochloric acid, stirs, and any in available then following two kinds of methods makes slurry gelization:
First, adding catalyzer Tetramethyl Ethylene Diamine, the nature gelation is placed in the back that stirs.
Second, slip is heated to 40～80 ℃ makes its gelation.Type of heating can adopt electrically heated, water-bath heat, microwave heating etc.
The add-on of above-mentioned initiator is generally 0.1～1.0% of organic monomer weight, and the add-on of catalyzer is 0.05～0.5% of an organic monomer weight.
Five, the wet gel base substrate is taken out drying and dehydrating in container, drying mode can adopt seasoning, blowing drying or heat drying.For accelerating to dehydrate process, gel piece can be cut into or break off with the fingers and thumb into plurality of small blocks.
Six, dried gel piece places calcining furnace to be heated to the synthesis temperature insulation down of regulation, just obtains required synthetic powder agglomates.Synthesis temperature is decided on the requirement of different ceramic powders with soaking time.When the gel piece size is big, cause the danger of bursting apart for preventing that organism from volatilizing rapidly, can adopt one of following two kinds of methods with the organism burn off in the gel piece during calcining: the one, the gel piece of bulk is broken into fritter after, in 220～600 ℃, slowly heat up the burn off organism; Perhaps gel piece is heated to 450～600 ℃, is incubated 0.5～5 hour, the organism burn off.Behind above-mentioned steps burn off organism, again furnace temperature is brought up to specified temperature calcining synthetic powder.
Embodiment 1, synthetic magnesium titanate MgTiO
3Powder.
In order to confirm advantage of the present invention, adopt A, B, three kinds of processing condition of C to compare.
A technology: starting material adopt metatitanic acid H
2TiO
3With magnesium basic carbonate Mg (OH)
24MgCO
36H
2O, Mg: Ti=1: 1, add organic monomer acrylamide and linking agent methylene-bisacrylamide simultaneously, add-on is that 8% both ratios of raw-material weight are 20: 1.And add deionized water and be made into ball milling behind the slip, ball: material=2: 1, water: material=1.5: 1, ball milling time 4h.Discharging is to Glass Containers and add the initiator ammonium persulfate of organic monomer weight 0.5% and 0.3% catalyzer Tetramethyl Ethylene Diamine, and the back that stirs is placed gelation was taken place in about 10 minutes.Take out the wet gel piece and place 80 ℃ of baking ovens to be dried to constant weight, put into retort furnace then and be warming up to 800 ℃ of insulation 2h, numbering A8 with stove.
B technology: starting material adopt titanium dioxide TiO
2With magnesium basic carbonate Mg (OH)
24MgCO
36H
2O, Mg: Ti=1: 1, processing condition and A technology are identical, numbering B8.
C technology: starting material are identical with B technology, do not add organic monomer and linking agent, and ball milling condition is identical with A technology.Directly in 80 ℃ of baking ovens, be dried to constant weight after the discharging, put into retort furnace then and be warming up to 800 ℃ of insulation 2h, promptly adopt traditional solid phase reaction process, numbering C8 with stove.
Three kinds of technology synthetic powders are carried out X-ray diffraction analysis, and its XPD spectrum is seen accompanying drawing 1.As can be seen, A8 is single magnesium titanate structure substantially, and B8 and C8 are all not synthetic.This and A process using metatitanic acid are raw material, and it is relevant that the newly-generated titanium dioxide of calcining and decomposing has higher surface activity.Though and B technology is identical with the starting material that C technology adopts, the synthetic magnesium titanate is obviously more than C8 among the B8, and residual titanium dioxide then is less than C8, and the synthetic effect of this explanation gel solid state reaction is better than traditional solid reaction process.
Embodiment 2, synthetic W type ferrite BaZn
0.5Co
1.5Fe
16O
27Powder.
Starting material adopt non-water-soluble Fe
2O
3, BaSO
4With water miscible ZnCl
2, CoCl
2, its proportioning is Ba: Zn: Co: Fe=1: 0.5: 1.5: 7.8, add organic monomer acrylamide and linking agent methylene-bisacrylamide simultaneously, and add-on is a raw material weight 5%, both ratios are 15: 1.Add deionized water and be made into slip, with ball milling behind the ammoniacal liquor adjustment slip pH=8, ball: material=3: 1, water: material=0.5: 1, ball milling time 5h.The initiator ammonium persulfate that adds organic monomer weight 0.3% after the discharging, put into glass beaker after stirring, in microwave oven, heat, gelation behind about 3Os, take out the wet gel piece, break fritter into about 2cm3 off with the fingers and thumb and place under the ventilation condition and be dried to constant weight, place retort furnace to be warming up to 1200 ℃ of insulation 2h then with stove.The synthetic ferrite powder is carried out the X-ray diffraction structural analysis, prove to obtain good W type plane hexad ferrite structure.Through with the same temperature of chemical coprecipitation under the synthetic powder relatively, both XRD spectrum is identical.But gel solid state reaction skill obviously is better than chemical coprecipitation process from aspects such as material cost, technological operations.
Embodiment 3, synthesis of barium titanate BaTiO
3Powder.
Starting material adopt BaCO
3And TiO
2, its proportioning is Ba: Ti=1: 1, add organic monomer acrylamide and linking agent methylene-bisacrylamide simultaneously, and add-on is 3% of a raw material weight, both ratios are 25: 1.Add deionized water and be made into slip, add pan feeding simultaneously and weigh 1% commercially available JA-281 dispersion agent (a kind of vinylformic acid and Sipacril 2739OF ammonium salt aqueous solution, concentration are 30%), and adjust slip pH value to 9 ball milling afterwards with ammoniacal liquor, ball: material=2: 1, water: material=0.3: 1, ball milling time 5h.Discharging adds the initiator ammonium persulfate of organic monomer weight 1% and 0.5% catalyzer Tetramethyl Ethylene Diamine to Glass Containers.Gelation took place in about 5 minutes in the back placement that stirs.Take out the dice of gel piece cutting into about 2cm * 2cm * 2cm, blowing dehydrates to constant weight.Put into retort furnace then and be heated to 600 ℃ of insulation 1h burn off organism, further be warming up to 1100 ℃ of insulation 2h calcining again and synthesize.Synthetic powder is carried out the X-ray diffraction structural analysis, prove and finish the synthesis of barium titanate structure, the same with traditional synthesis by solid state reaction 1150 ℃ of calcining synthetic effects.But the process that dehydrates is more remarkable than traditional solid reaction process energy-saving effect, 50 ℃ of the also corresponding reductions of synthesis temperature.
Embodiment 4, synthetic multicomponent piezoelectric ceramics PZT powder.
Starting material adopt Pb
3O
4, ZrO
2, TiO
2, La
2O
3, Nb
2O
5, MnO
2, its proportioning is Pb: Zn: Ti=1: 0.53: 0.47, add 0.01La, 0.012Nb, 0.002Mn.Add organic monomer Methacrylamide and linking agent methylene-bisacrylamide simultaneously, add-on is 2.4% of a raw material weight, and both ratios are 6: 1.Add deionized water and be made into slip, add the JA-281 dispersion agent of raw material weight 0.8% simultaneously, and adjust ball milling behind the slip pH=9, ball: material=1.5: 1, water: material=0.2: 1, ball milling time 8h with ammoniacal liquor.Discharging adds dinitrogen [ether propane] the hydrochloric acid initiator of organic monomer weight 1% to Glass Containers, after stirring container is immersed gelation in about 5 minutes in 60 ℃ of hot water baths.Taking out the wet gel piece breaks off with the fingers and thumb into about 1cm
3Fritter places in the crucible, dehydrates to constant weight in 100 ℃ of baking ovens earlier.Place the spacious lid of retort furnace to be warming up to 600 ℃ of insulation 1h burn off organism then, add a cover again that to be warming up to 850 ℃ of insulation 2h calcining synthetic.Synthetic powder is got three samples in position, upper, middle and lower carry out X-ray diffraction structural analysis and chemical composition analysis, show that each position sample structure and composition are in full accord.Compare with traditional solid reaction process, avoided Pb in the slurry dewatering drying process
3O
4The uneven components that sedimentation causes, the synthetic powder quality obviously improves.
Embodiment 5, synthetic multicomponent thermal sensitive ceramics PTC powder.
Earlier synthetic PTC original washing powder, starting material adopt BaCO
3, Pb
3O
4, CaCO
3, TiO
2With water miscible YCl
3, its proportioning is Ba: Pb: Ca: Ti: Y=0.93: 0.03: 0.04: 1.01: 0.0011, and add deionized water and be made into the water slip, the JA-281 dispersion agent that adds raw material weight 1% simultaneously, and adjust ball milling behind the slip pH=9, ball: material=2: 1, water: material=0.25: 1 with ammoniacal liquor.Behind the ball milling time 18h, add organic monomer Methacrylamide and linking agent polyoxyethylene glycol (1000) dimethacrylate, add-on is 3% of a raw material weight, and both ratios are 3: 1.Discharging adds initiator tetrazo [ether propane] hydrochloric acid of organic monomer weight 0.8% after continuing ball milling 0.5h to plastic containers, after stirring container is immersed gelation in about 5 minutes in 60 ℃ of hot water baths.Taking out the wet gel piece breaks off with the fingers and thumb into about 1cm
3Fritter places in the crucible, dehydrates to constant weight in 100 ℃ of baking ovens earlier.Place the spacious lid of retort furnace to be warming up to 600 ℃ of insulation 1h burn off organism then, add a cover again and be warming up to 1180 ℃ of insulation 2h, the synthetic PTC original washing powder that obtains.
The original washing powder coarse crushing by the 0.5mm hole sizer, is carried out secondary doping.The secondary doping starting material adopt Sb
2O
3, MnO
2, SiO
2, Al
2O
3, Li
2CO
3, consumption mixes with original washing powder in accordance with regulations, adds organic monomer Methacrylamide and linking agent polyoxyethylene glycol (1000) dimethacrylate simultaneously, and add-on is 3% of a raw material weight, and both ratios are 3: 1.Add deionized water and be made into slip, add the JA-281 dispersion agent of raw material weight 0.8% simultaneously, and adjust ball milling behind the slip pH=9, ball: material=2: 1, water: material=0.25: 1 with ammoniacal liquor.Discharging behind the ball milling time 4h.With as hereinbefore method gelation, dehydrate, spacious lid is warming up to 600 ℃ of insulation 1h burn off organism in retort furnace at last, promptly obtains through overdoping and the uniform PTC powder of composition.
Claims (3)
1, a kind of process for synthesizing composite ceramic powder body is characterized in that adopting following processing step,
(1) starting material that will desire synthetic powder in accordance with regulations proportioning be prepared into the water slip and carry out ball milling, ratio of grinding media to material is 1: 1～5: 1, amount of water is 20～200% of a raw material weight, the ball milling time is 1～100 hour;
(2) in 0.5～15 hour before the ball milling discharging, in slip, add organic monomer and linking agent, organic monomer be acrylamide or Methacrylamide one of them, linking agent be methylene-bisacrylamide or many ethyleneglycol dimethacrylates one of them, total add-on of organic monomer and linking agent is 1～10% of a raw material weight, and the weight ratio of organic monomer and linking agent is 3: 1～30: 1;
(3) slip behind the ball milling is placed container, add initiator, add-on is 0.1～0.5% of an organic monomer weight, stirs, initiator is one of following material: ammonium persulphate or tetrazo [ether propane] hydrochloric acid is mixed with 5%～20% the aqueous solution during use;
(4) one of them makes slurry gelization to adopt two kinds of methods of following first, second:
Party A's method: add Tetramethyl Ethylene Diamine in slip, add-on is 0.05～0.3% of an acrylamide weight, and place the back that stirs, and makes its natural gelation;
Party B's method: slip is heated to 40～80 ℃, makes its gelation;
(5) the wet gel base substrate is taken out drying and dehydrating in container;
(6) dried gel piece is placed calcining furnace be heated to the synthesis temperature of regulation, the insulation certain hour obtains required synthetic powder agglomates.
2, process for synthesizing composite ceramic powder body according to claim 1 and 2, it is characterized in that, when desiring to contain metal oxide in the starting material of synthetic powder, should selecting not produce or seldom produce oxyhydroxide obnoxious flavour, this metal or acid or carbonate, oxalate, to replace original metal oxide be raw material.
3, process for synthesizing composite ceramic powder body according to claim 1 and 2 is characterized in that, during said calcining gel piece, is heated to 500～800 ℃ earlier, is incubated 30 minutes～4 hours, and the burn off organism is brought up to specified temperature then.
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| CN1263878A (en) | 2000-08-23 |
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