CN101407418A - Pink yttrium-zirconium structural ceramic and preparation thereof - Google Patents
Pink yttrium-zirconium structural ceramic and preparation thereof Download PDFInfo
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Abstract
The invention relates to pink yttrium-zirconium structured ceramics and a preparation method thereof, which belongs to the technical field of structured ceramics. The pink yttrium-zirconium structured ceramics consists of 4.8-5.5 percent of Y2O3, 92-96 percent of ZrO2, 0.1-0.8 percent of Nd2O3, 0.5-4.0 percent of Er2O3, 0.05-0.50 percent of La2O3, and 0.1-0.30 percent of Sc2O3. The preparation method for the pink yttrium-zirconium structured ceramics comprises the steps of batching-precipitation-washing-pressing-pink yttrium-zirconium ceramic powder precursor-ignition-vibrational milling-air flow crashing-spray granulation-dry press molding (or injection molding).
Description
Technical field
The present invention relates to a kind of pink yttrium-zirconium structural ceramic and preparation method thereof, belong to the structural ceramics technical field.
Background technology
As everyone knows, the zirconia ceramic product color category is single both at home and abroad at present, and an adularescent and black, ceramics only are that surperficial glaze colours is pink, and idiosome is not a pink, is the pink yttrium-zirconium structural ceramic goods in domestic industry and the civilian table and does not appear in the newspapers.
Summary of the invention
In order to overcome present zirconia ceramic product deficiency black, white dichromatism is only arranged, the invention provides in a kind of table and be pink yttrium-zirconium structural ceramic and preparation method thereof.The technical solution adopted for the present invention to solve the technical problems is: a kind of pink yttrium-zirconium structural ceramic is by 4.0-5.5%Y
2O
3, 92-96%ZrO
2, 0.1-0.8%Nd
2O
3, 0.5-4.0%Er
2O
3, 0.05-0.50%La
2O
3, 0.1-0.30%Sc
2O
3Form.
A kind of method for preparing above-mentioned described pink yttrium-zirconium structural ceramic is characterized in that:
Step 1: water-soluble 80 grams per liters, the Y of being made into of zirconium oxychloride
2O
3, Nd
2O
3, Er
2O
3, La
2O
3Sc
2O
3Be made into 0.5mol/l respectively with nitric acid dissolve, the 100 kilograms of amounts that are metered into each oxide compound respectively according to partition of at every turn preparing burden are to batch tank, and stirring and evenly mixing is standby then;
Step 2: adopt chemical coprecipitation to precipitate, reaction process is: the deionized water and the dispersion agent (dispersion agent/material=1.2%) that add 500L in the reactor, slowly be warming up to 60 ℃, slowly add feed liquid (institute's proportion liquid in the step 1) and precipitation agent (ammoniacal liquor simultaneously, concentration is 3N), control reaction temperature is 60 ℃, reaction process pH is 8～9, reaction times is 2 hours, ageing was 1 hour after reaction finished, and filtered, again through 5 deionized water wash (S/L=1: 2), wash the back and press dry, obtain pink yttrium hydroxide zirconium precursor body burden about 20% with plate-and-frame filter press.Settling apparatus is 3m
3Enamel reaction still.
Step 3: adopt electric roller kiln to carry out calcination presoma described in the step 2, heat-up rate is 2 ℃/min, and calcination temperature is 900 ℃, and soaking time is 2 hours, obtains pink yttrium Zirconium oxide.
Step 4: comminution by gas stream obtains pink yttrium zirconium air-flow powder with pink yttrium Zirconium oxide described in the step 3 after the gentle stream pulverizer of vibratory milling crusher machine is pulverized.
Step 5: mist projection granulating; with pink yttrium zirconium air-flow powder described in the step 4; add deionized water (S/L=1: 1); mix with agitating ball mill; add PVA (add-on is 1%) and CMC additives such as (0.5%); treat to carry out mist projection granulating with sponging granulator behind the abundant mixing, obtain pink yttrium zirconium granulation powder.
Step 6:
(1) dry-pressing formed preparation pink yttrium-zirconium structural ceramic goods: adopt four-column hydraulic press to carry out a premolding (pressure is 100T) in the described pink yttrium zirconium granulation powder of step 5, again employing wait static pressure to carry out post forming (pressure is 180MPa, time is 15 minutes) obtain green compact, (temperature is 1450 ℃ to green sintering, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), product behind the sintering (as mills through machining, mill, polishings etc.) obtain the pink yttrium-zirconium structural ceramic goods after, machining apparatus has: milling machine, vertical shaft grinder, surface grinding machine, multi-purpose grinding machine, mirror polish machine etc.
(2) injection molding prepares the pink yttrium-zirconium structural ceramic goods: with the described pink yttrium zirconium air-flow powder of step 4, add PP, PE and initiator (massfraction is 53% ammonium persulfate aqueous solution), by weight ratio preparation in 40: 40: 20, preparing the back, to be made into content with pink yttrium zirconium air-flow powder be slurry about 50wt%, stir, inject mold cavity, pressurize 2 minutes, make and have the wet base substrate that ultimate compression strength surpasses 1MPa, wet base substrate adopts the solvent pairs defatting technology to remove PP again, PE and initiator, (sintering temperature is 1450 ℃ to carry out sintering then, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), the product behind the sintering obtains the pink yttrium-zirconium structural ceramic goods after polishing.
The invention has the beneficial effects as follows: for domestic and international yttrium zircon-structure pottery has increased a kind of goods of color and luster novelty, pink yttrium-zirconium structural ceramic goods of the present invention have been filled up external blank, its goods pink the same outside and inside.
The present invention is further described below in conjunction with drawings and Examples.
Description of drawings:
Fig. 1 is a process route chart of the present invention.
Embodiment
Embodiment one,
Referring to Fig. 1, step 1: water-soluble 80 grams per liters, the Y of being made into of zirconium oxychloride
2O
3, Nd
2O
3, Er
2O
3, La
2O
3, Sc
2O
3Be made into 0.5mol/l respectively with nitric acid dissolve, prepare burden 100 kilograms (being converted to oxide compound): ZrO2=93.6 kilogram, Y
2O
3=5.2 kilograms, Nd
2O
3=0.4 kilogram, Er
2O
3=0.6 kilogram, La
2O
3=0.1 kilogram, Sc
2O
3=0.1 kilogram, get the volume number of above-mentioned material respectively: 1170 liters, 92.12 liters, 4.76 liters, 6.28 liters, 1.23 liters, 2.90 liters, successively join in 2000 liters the stirred pot, stirring and evenly mixing is standby;
Step 2: adopt chemical coprecipitation to precipitate, reaction process is: add the deionized water of 500L and dispersion agent (dispersion agent/material heavy=1.2%) in the reactor, slowly be warming up to 60 ℃, slowly add feed liquid (institute's proportion liquid in the step 1) and precipitation agent (ammoniacal liquor simultaneously, concentration is 3N), control reaction temperature is 60 ℃, the reaction process pH value is 8～9, reaction times is 2 hours, ageing was 1 hour after reaction finished, and filtered, again through 5 deionized water wash (S/L=1: 2), wash the back and press dry, obtain pink yttrium hydroxide zirconium precursor body burden about 20% with plate-and-frame filter press.Settling apparatus is 3m
3Enamel reaction still.
Step 3: adopt electric roller kiln to carry out calcination presoma described in the step 2, heat-up rate is 2 ℃/min, and calcination temperature is 900 ℃, and soaking time is 2 hours, obtains pink yttrium Zirconium oxide.
Step 4: comminution by gas stream, pink yttrium Zirconium oxide described in the step 3 is obtained pink yttrium zirconium air-flow powder after the gentle stream pulverizer of vibratory milling crusher machine is pulverized (leading indicator is: D50=0.70 μ m, SBET=24.6m
2/ g).
Step 5: mist projection granulating; with 90 kilograms in pink yttrium zirconium air-flow powder described in the step 4; join agitating ball mill; add 90 kilograms of (S/L=1: 1) of deionized water; stir and add PVA 0.9 kilogram of (add-on is 1wt%) and 0.45 kilogram of additives such as (0.5wt%) of CMC after 30 minutes respectively; stirring ball-milling was put into storage tank for standby use after 5 hours; carry out mist projection granulating with sponging granulator then; 265 ℃ of control inlet temperature; 110 ℃ of air outlet temperatures obtain pink yttrium zirconium granulation powder (granulation powder degree is 50-80 μ m).
Step 6: the pink Stupalox goods of dry-pressing formed preparation: adopt four-column hydraulic press to carry out a premolding (pressure is 100T) in the described pink yttrium zirconium granulation powder of step 5, again employing wait static pressure to carry out post forming (pressure is 180MPa, time is 15 minutes) obtain green compact, (temperature is 1450 ℃ to green sintering, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), Stupalox blank behind the sintering is through the vertical shaft grinder face machined flat, floor stand grinder is repaiied knife-edge, open the casket mouth with two-sided tool sharpening machine, open cutting edge of a knife or a sword with blade grinding machine at last, load onto and be the pink Stupalox that is used for market sale after hilt is packed.Table 1 is the product detected result of this examples preparation.
Embodiment two,
Referring to Fig. 1, step 1: water-soluble 80 grams per liters, the Y of being made into of zirconium oxychloride
2O
3, Nd
2O
3, Er
2O
3, La
2O
3, Sc
2O
3Be made into 0.5mol/l respectively with nitric acid dissolve, prepare burden 100 kilograms (being converted to oxide compound): ZrO2=92.1 kilogram, Y
2O
3=5.0 kilograms, Nd
2O
3=0.7 kilogram, Er
2O
3=1.5 kilograms, La
2O
3=0.4 kilogram, Sc
2O
3=0.3 kilogram, get the volume number of above-mentioned material respectively: 1151 liters, 88.57 liters, 8.32 liters, 15.69 liters, 4.91 liters, 8.71 liters, successively join in 2000 liters the stirred pot, stirring and evenly mixing is standby.
Step 2: adopt chemical coprecipitation to precipitate, reaction process is: add the deionized water of 500L and dispersion agent (dispersion agent/material heavy=1.2%) in the reactor, slowly be warming up to 60 ℃, slowly add feed liquid (institute's proportion liquid in the step 1) and precipitation agent (ammoniacal liquor simultaneously, concentration is 3N), control reaction temperature is 60 ℃, the reaction process pH value is 8～9, reaction times is 2 hours, ageing was 1 hour after reaction finished, and filtered, again through 5 deionized water wash (S/L=1: 2), wash the back and press dry, obtain pink yttrium hydroxide zirconium precursor body burden about 20% with plate-and-frame filter press.Settling apparatus is 3m
3Enamel reaction still.
Step 3: adopt electric roller kiln to carry out calcination presoma described in the step 2, heat-up rate is 2 ℃/min, and calcination temperature is 900 ℃, and soaking time is 2 hours, obtains pink yttrium Zirconium oxide.
Step 4: comminution by gas stream, pink yttrium Zirconium oxide described in the step 3 is obtained pink yttrium zirconium air-flow powder after the gentle stream pulverizer of vibratory milling crusher machine is pulverized (leading indicator is: D50=0.76 μ m, SBET=23.9m
2/ g).
Step 5: injection molding prepares the pink yttrium-zirconium structural ceramic goods: with the described pink yttrium zirconium air-flow powder of step 4, add PP, PE and initiator (massfraction is 53% ammonium persulfate aqueous solution), in ratio preparation in 40: 40: 20, preparing the back, to be made into content with pink yttrium zirconium air-flow powder be slurry about 50wt%, stir, inject mold cavity, pressurize 2 minutes, make and have the wet base substrate that ultimate compression strength surpasses 1MPa, wet base substrate adopts the solvent pairs defatting technology to remove PP again, PE and initiator, (sintering temperature is 1450 ℃ to carry out sintering then, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), the product behind the sintering obtains the pink yttrium-zirconium structural ceramic goods after polishing.At present the goods through the injection molding preparation mainly contain: ceramic clock and watch accessory, inner and outer rings of ceramic bearing, have jewel glossy ceramic ornament etc.
The pink ceramic main performance index that this example is produced is as shown in table 2.
Embodiment three,
Referring to Fig. 1, step 1: water-soluble 80 grams per liters, the Y of being made into of zirconium oxychloride
2O
3, Nd
2O
3, Er
2O
3, La
2O
3, Sc
2O
3Be made into 0.5mol/l respectively with nitric acid dissolve, prepare burden 100 kilograms (being converted to oxide compound): ZrO2=92.0 kilogram, Y
2O
3=4.0 kilograms, Nd
2O
3=0.3 kilogram, Er
2O
3=3.5 kilograms, La
2O
3=0.1 kilogram, Sc
2O
3=0.1 kilogram, get the volume number of above-mentioned material respectively: 1150 liters, 70.86 liters, 3.56 liters, 36.61 liters, 1.23 liters, 2.90 liters, successively join in 2000 liters the stirred pot, stirring and evenly mixing is standby;
Step 2: adopt chemical coprecipitation to precipitate, reaction process is: add the deionized water of 500L and dispersion agent (dispersion agent/material heavy=1.2%) in the reactor, slowly be warming up to 60 ℃, slowly add feed liquid (institute's proportion liquid in the step 1) and precipitation agent (ammoniacal liquor simultaneously, concentration is 3N), control reaction temperature is 60 ℃, the reaction process pH value is 8～9, reaction times is 2 hours, ageing was 1 hour after reaction finished, and filtered, again through 5 deionized water wash (S/L=1: 2), wash the back and press dry, obtain pink yttrium hydroxide zirconium precursor body burden about 20% with plate-and-frame filter press.Settling apparatus is 3m
3Enamel reaction still.
Step 3: adopt electric roller kiln to carry out calcination presoma described in the step 2, heat-up rate is 2 ℃/min, and calcination temperature is 900 ℃, and soaking time is 2 hours, obtains pink yttrium Zirconium oxide.
Step 4: comminution by gas stream, pink yttrium Zirconium oxide described in the step 3 is obtained pink yttrium zirconium air-flow powder after the gentle stream pulverizer of vibratory milling crusher machine is pulverized (leading indicator is: D50=0.70 μ m, SBET=24.6m
2/ g).
Step 5: mist projection granulating; with 90 kilograms in pink yttrium zirconium air-flow powder described in the step 4; join agitating ball mill; add 90 kilograms of (S/L=1: 1) of deionized water; stir and add PVA 0.9 kilogram of (add-on is 1wt%) and 0.45 kilogram of additives such as (0.5wt%) of CMC after 30 minutes respectively; stirring ball-milling was put into storage tank for standby use after 5 hours; carry out mist projection granulating with sponging granulator then; 265 ℃ of control inlet temperature; 110 ℃ of air outlet temperatures obtain pink yttrium zirconium granulation powder (granulation powder degree is 50-80 μ m).
Step 6: dry-pressing formed preparation pink yttrium-zirconium structural ceramic goods: adopt four-column hydraulic press to carry out a premolding (pressure is 100T) in the described pink yttrium zirconium granulation powder of step 5, again employing wait static pressure to carry out post forming (pressure is 180MPa, time is 15 minutes) obtain green compact, (temperature is 1450 ℃ to green sintering, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), product behind the sintering (as mills through machining, mill, polishings etc.) obtain the pink yttrium-zirconium structural ceramic goods after, machining apparatus has: milling machine, vertical shaft grinder, surface grinding machine, multi-purpose grinding machine, mirror polish machine etc.The goods of this examples preparation mainly contain: sieve circle, cutter cup ring etc. and the pink yttrium-zirconium structural ceramic goods main performance index of being produced is as shown in table 3.
The product detected result of table 1 example one preparation
| Title | Index request | Detected result |
| Total length mm | 185±1 | 184.6 |
| Width mm | 40±0.2 | 39.7 |
| The wide mm of handle | 15.6 | 15.6 |
| Thickness mm | 2.6-2.8 | 2.8 |
| The long mm of sword | 157±1 | 156 |
| Degree of deformation mm | ＜0.30 | 0.20 |
| Density g/cm 3 | ≥6.0 | 6.096 |
| Intensity and toughness | 2 meters are highly freely landed intact | 2 meters are highly freely landed, and blade is intact |
| Outward appearance | Nothing collapses scarce, flawless | Nothing collapses scarce, flawless |
The pink ceramic main performance index that this example of table 2 two is produced
| Performance | The Unit of unit | The product detected result |
| Composition | Wt％ | Y 2O 3＝5.06％；ZrO 2＝92.20％；Nd 2O 3＝0.65％； Er 2O 3＝1.56％；La 2O 3＝0.32％；Sc 2O 3＝0.21％ |
| Density | g/cm 3 | 6.06 |
| Hardness | Gpa | 13.6 |
| Bending strength | Mpa | 1370 |
| Fracture toughness property | MPam 1/ 2 | 13 |
| Grain size | μm | 0.4 |
The pink yttrium-zirconium structural ceramic goods main performance index that table 3 example three is produced
| Performance | The Unit of unit | The product detected result |
| Composition | Wt％ | Y 2O 3＝5.06％；ZrO 2＝92.20％；Nd 2O 3＝0.65％； Er 2O 3＝1.56％；La 2O 3＝0.32％；Sc 2O 3＝0.21％ |
| Density | g/cm 3 | 6.02 |
| Hardness | Gpa | 13.3 |
| Bending strength | Mpa | 1386 |
| Fracture toughness property | MPam 1/ 2 | 12.6 |
| Grain size | μm | 0.46 |
Claims (2)
1, a kind of pink yttrium-zirconium structural ceramic is characterized in that: by 4.8-5.5%Y
2O
3, 92-96% ZrO
2, 0.1-0.8%Nd
2O
3, 0.5-4.0%Er
2O
3, 0.05-0.50%La
2O
3, 0.1-0.30%Sc
2O
3Form;
2, the preparation method of a kind of pink yttrium-zirconium structural ceramic according to claim 1 is characterized in that:
Step 1: water-soluble 80 grams per liters, the Y of being made into of zirconium oxychloride
2O
3, Nd
2O
3, Er
2O
3, La
2O
3Sc
2O
3Be made into 0.5mol/l respectively with nitric acid dissolve, the 100 kilograms of amounts that are metered into each oxide compound respectively according to partition of at every turn preparing burden are to batch tank, and stirring and evenly mixing is standby then;
Step 2: adopt chemical coprecipitation to precipitate, reaction process is: add the deionized water of 500L and dispersion agent (dispersion agent/material heavy=1.2%) in the reactor, slowly be warming up to 60 ℃, slowly add feed liquid (institute's proportion liquid in the step 1) and precipitation agent (ammoniacal liquor simultaneously, concentration is 3N), control reaction temperature is 60 ℃, reaction process pH value is 8～9, reaction times is 2 hours, ageing was 1 hour after reaction finished, and filtered, again through 5 deionized water countercurrent washing (S/L=1: 2), wash the back and press dry, obtain pink yttrium hydroxide zirconium precursor body burden about 20% with plate-and-frame filter press.Settling apparatus is 3m
3Enamel reaction still.
Step 3: adopt electric roller kiln to carry out calcination presoma described in the step 2, heat-up rate is 2 ℃/min, and calcination temperature is 900 ℃, and soaking time is 2 hours, obtains pink yttrium Zirconium oxide.
Step 4: comminution by gas stream, pink yttrium Zirconium oxide described in the step 3 is obtained pink yttrium zirconium air-flow powder after the gentle stream pulverizer of vibratory milling crusher machine is pulverized (leading indicator is: D50=0.70 μ m, SBET=24.6m
2/ g).
Step 5: mist projection granulating; with pink yttrium zirconium air-flow powder described in the step 4; add deionized water (S/L=1: 1); mix with agitating ball mill; add PVA (add-on is 1%) and CMC additives such as (0.5%); treat to carry out mist projection granulating with sponging granulator behind the abundant mixing, obtain pink yttrium zirconium granulation powder.
Step 6:
(1) dry-pressing formed preparation pink yttrium-zirconium structural ceramic goods: adopt four-column hydraulic press to carry out a premolding (pressure is 100T) in the described pink yttrium zirconium granulation powder of step 5, again employing wait static pressure to carry out post forming (pressure is 180MPa, time is 15 minutes) obtain green compact, (temperature is 1450 ℃ to green sintering, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), product behind the sintering (as mills through machining, mill, polishings etc.) obtain the pink yttrium-zirconium structural ceramic goods after, machining apparatus has: milling machine, vertical shaft grinder, surface grinding machine, multi-purpose grinding machine, mirror polish machine etc.
(2) injection molding prepares the pink yttrium-zirconium structural ceramic goods: with the described pink yttrium zirconium air-flow powder of step 4, add PP, PE and initiator (massfraction is 53% ammonium persulfate aqueous solution), by weight ratio preparation in 40: 40: 20, preparing the back, to be made into content with pink yttrium zirconium air-flow powder be slurry about 50wt%, stir, inject mold cavity, pressurize 2 minutes, make and have the wet base substrate that ultimate compression strength surpasses 1MPa, wet base substrate adopts the solvent pairs defatting technology to remove PP again, PE and initiator, (sintering temperature is 1450 ℃ to carry out sintering then, temperature rise rate is 1～2 ℃/min, soaking time is 4 hours), the product behind the sintering obtains the pink yttrium-zirconium structural ceramic goods after polishing.
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Address after: 341000 289 piety Road, Zhanggong District, Ganzhou, Jiangxi Patentee after: Qian Dong lanthanide group limited company Address before: 341000 Shuidong Town, Zhanggong District, Jiangxi Province Patentee before: Ganzhou Qiandong Rare Earth Group Co., Ltd. |