CN1256393C - Prepn of nanometer aggregated zirconia powder for hot spraying - Google Patents

Prepn of nanometer aggregated zirconia powder for hot spraying Download PDF

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CN1256393C
CN1256393C CN 200410061306 CN200410061306A CN1256393C CN 1256393 C CN1256393 C CN 1256393C CN 200410061306 CN200410061306 CN 200410061306 CN 200410061306 A CN200410061306 A CN 200410061306A CN 1256393 C CN1256393 C CN 1256393C
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powder
drying
preparation
slip
nanometer
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CN1637080A (en
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程旭东
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Wuhan University of Technology WUT
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Abstract

The present invention relates to a preparation method for nanometer agglomeration type zirconia powder for hot spraying. In the preparation method, nanometer zirconia powder stabilized by yttrium oxide with the granularity from 20 to 60 nm and an adhesive are mixed at the quality ratio of 95:5 to 98:2; purified water whose weight is 1 to 1.3 times of that of mixed materials is added, and the mixture is prepared into slurry; then a spray-drying technology is adopted, micrometer agglomeration powder is prepared between 110 and 300DEGC, and the agglomeration powder bears plasma spheroidizing treatment or sintering densification treatment to be prepared into compact powder with the granularity from 40 to 90 mum in an unchanged nanometer crystal structure; the obtained powder can meet the requirements of a plasma spraying technology or a flame spraying technology. The preparation method has the advantages of few processes, simple operation, large production quantity, safety, reliability and low manufacture cost and is suitable for continuous industrial scale production.

Description

The preparation method of used for hot spraying nanoclusters aggressiveness Zirconium oxide powder
Technical field
The present invention relates to a kind of Surface Engineering preparation methods that is used for thermospray, particularly be used for the nanocrystalline Conglobation type Zirconium oxide powder preparation methods of plasma spraying or flame plating technology.
Background technology
Zirconium white belongs to the slant acidity oxide compound, and fusing point reaches 2760 ℃, and thermal conductivity is low, and chemical stability is good, and all stable in high temperature oxidation and weak reducing atmosphere, ability contains SO 2, CO and CO 2Corrosion Deng the high temperature combustion gas.But pure ZrO 2Material does not generally make as high-temperaure coating, and this is to degrade phenomenon because its crystal formation conversion can produce.Along with variation of temperature, different crystal formations can appear in crystal of zirconium oxide: normal temperature to 1000 ℃ is monoclinic crystal β-ZrO 2Surpass 1000 ℃, be converted into tetragonal structure α-ZrO 2, follow about 7% volume change take place.When cooling off, recover the monoclinic form structure again, volume then can not return to original state again, produces irreversible conversion, and this crystal conversion and volume change under coating suffers thermal cycle conditions, can produce big thermal stresses, make coating cracking and spalling failure.
At ZrO 2Mix yttrium oxide (Y in the crystal 2O 3) used as stabilizers, can make ZrO 2At high temperature obtain the crystalline structure of stabilization (YSZ) or partially stabilizedization (PYSZ).Think at present: partially stabilized ZrO 2/ Y 2O 3Crystalline structure is promptly mixed with cubic system by monoclinic crystal and forms.This crystalline structure at high temperature, the volumetric shrinkage phase transformation takes place in monocline mutually, cube phase then raises with temperature the volumetric expansion phase transformation takes place, two-phase suppresses mutually, thereby makes partially stabilized ZrO 2/ Y 2O 3Crystalline structure is than completely stable ZrO 2/ Y 2O 3Crystalline structure has lower mean thermal expansion coefficients, thereby has better thermal shock resistance.In addition, under 1650 ℃ of ultrahigh-temperature during life-time service, Y 2O 3Can not resemble other stablizers to the crystal external diffusion, be the highest heat barrier coat material of present use temperature.If at ZrO 2/ Y 2O 3Add a spot of cerium oxide (CeO) in the crystalline structure, can further improve the performance of this coating.
In recent years, further studies show that: the zirconium white that the partial oxidation yttrium is stable, when grain fineness number is controlled at less than 100nm, the sudden change that can bring material property, the strength of materials and fracture toughness property improve significantly, have superplasticity under the normal temperature.Utilize nanometer ZrO 2/ Y 2O 3Feature performance benefit, research and develop its application aspect high-temp heat barrier coating, be final purpose of the present invention.
Preparation has ZrO 2/ Y 2O 3The thermal barrier coating of nanocrystalline structure must adopt Technologies such as plasma spraying or HVOF (High Velocity Oxygen Fuel) to be deposited as coating by nano raw material being made Conglobation type micron spraying powder then.So ZrO 2/ Y 2O 3The agglomeration technique key of nano material is keeping making the fine and close conglobation hot spray powder of being satisfied with plasma spraying or HVOF (High Velocity Oxygen Fuel) processing requirement under the constant prerequisite of nanocrystalline structure.
The Zirconium oxide powder of used for hot spraying generally adopts coprecipitation method and the preparation of electric smelting crush method at present; It is the reverse micelle method preparation that the Zirconium oxide powder of nanometer Conglobation type then adopts spray-drying process, sol-gel processing, microemulsion method.These methods respectively have its characteristics, but also have many weak points.As spray-drying process is that nano level zirconium white micro mist is mixed with binding agent, adds entry or other solvents are mixed with slip.It is ejected in the drying tower, and the surface tension by self in drying process is agglomerated into sphere, and the report of this respect is arranged in Journal of Inorganic Materials 2002,17 (4) plasma spray zirconia (PSZ) nano coating Research of microstructure one literary composition.Shrink because reunion powder is a nature, the loose density of powder only is 0.8～1.1 gram per centimeter 3, mobile poor, be 80～160 seconds/50 grams.Powder seems in the hot-spraying techniques process, and some " wafts ", can not obtain enough kinetic energy, so its coating density is not too high, can't obtain higher binding strength.China's powder technology 2002,8 (1) colloidal sols-emulsion-gel method prepares in zirconium dioxide plasma spraying powder one literary composition has reported the nano zirconium oxide powder for preparing used for plasma spraying with sol-gel processing, the powder particle of this method preparation is spherical, and particle size distribution is narrow.And, be difficult to realize mass-producing because the adding of organic reagents such as complexing agent causes the raising of production cost.Microemulsion method also claims reverse micelle method, is a kind of milling method that developed recently gets up.The nanometer powder that makes is spherical in shape, the globule size unanimity.But also there is the cost height, the problem that is difficult to accomplish scale production.In addition, research and the discussion that above-mentioned preparation method is combined with plasma spraying pyrolyzing method, supercritical drying that have, but also too wide in the gap apart from production practical application and mass-producing.
Summary of the invention
The objective of the invention is to overcome the method deficiency that above-mentioned preparation is suitable for the nanometer crystal zirconium powdered material that hot-spraying techniques uses, provide a kind of built-up type to prepare the method for nanocrystalline Conglobation type zirconia powder powder material, this method technical process is few, simple to operate, safe and reliable, low cost of manufacture is suitable for large-scale industrial production.
Reaching the goal of the invention technical scheme is: a kind of preparation method of used for hot spraying nanometer Conglobation type Zirconium oxide powder, and its preparation process is:
1st, batching: with granularity is that the partially stabilized nano zirconium oxide powder of yttrium oxide and the caking agent of 20～60nm particle diameter closes than compounding by 95: 5～98: 2 quality, and the water purification of 1～1.3 times of compound weight of adding is deployed into slip;
2nd, atomization drying: with the resulting slip of step 1 atomization drying in spray-drying tower, the drying tower temperature is controlled in 110～300 ℃ of scopes, makes reunion powder;
3rd, screening: the resulting reunion powder of step 2 is sieved, get the size range of required usefulness, the present invention gets particle between 180～325 mesh sieves, i.e. 40～90 μ m particles, and all the other powder are as foundry returns;
4th, densification: with the resulting granularity of step 3 is that the powder of 40～90 μ m places the sintering oven sintering, make densification, its temperature is 700～1000 ℃, sintering time is 10～30 minutes, then the dense powder that sinters is sieved, get dense powder between 180～325 mesh sieves, promptly get product; Perhaps resulting 40～90 μ m powder of step 3 are delivered to the plasma flame flow center by powder feeder, fine and close nodularization sprays into moulding in the water subsequently, then with after the moulding powder oven dry, adds residual organic binder bond of heat extraction and moisture content in≤300 ℃, promptly gets product;
ZrO in the partially stabilized nano zirconium oxide powder of described yttrium oxide 2With Y 2O 3Mass ratio be 94: 6～92: 8;
Described caking agent is one or more the mixture in dextrin, polyvinyl alcohol, carboxymethyl cellulose, the polystyrene.
Described atomization drying is with the centrifugal atomizing nozzle slip to be sprayed into drying in the drying tower, and the rotating speed of its centrifugal atomizer is 800～2000r/min.
Described atomization drying is to be carrier with dried compressed air, adopts two streaming nozzles that slurry is sprayed into the drying tower inner drying.
Characteristics of the present invention are:
1, the whole process of Conglobation type nano zircite preparation adopts physical agglomeration to combine with relative low-temperature sintering processing, thereby has controlled the factor that nanocrystal is grown up.Guaranteed that in whole granulation process nanometer protocrystal structure is not grown up, for the realization of follow-up plasma spraying nano coating is laid a good foundation.
2, added caking agent in the spray drying granulation process in follow-up granulation process, will all burnt or vapored away below 300 ℃, can not become the impurity in the hot spray coating.
3, the whole preparation process flow process is few, and equipment is simple, and processing parameter is easy to control, is suitable for serialization scale operation.
4, it is relatively low that nano raw material prepares the reunion powder cost, is easy to promote.
5, can on same production line, adjust the solid and hollow bead shape of reunion powder flexibly according to product requirement, and guarantee high purity, high-specific surface area and certain surfactivity of aggregate powder of AI/Yt.
Nano zircite reunion powder of the present invention mainly utilizes the characteristics that its heat-conduction coefficient is low, high-temperature stability is good, be applied to plasma spraying and prepare high-temp heat barrier coating or high-temperature abrasive coating, and, can adopt solid reunion powder to be prepared into different coatings respectively with the hollow bead shape according to the performance requriements of coating.
Embodiment
Embodiment 1:
Get the partially stabilized nano zirconium oxide powder of yttrium oxide (its ZrO of 9.8 kilograms of 20～40nm particle diameters 2With Y 2O 3Mass ratio is 93: 7), add 0.2 kilogram polyvinyl alcohol caking agent, behind the thorough mixing, adding 10 kilograms water purification again, to stir into the slip that homodisperse suspends stand-by.
Carry gas with the purified pressurized air of drying, gaseous tension is controlled at 0.8Mpa, take two streaming nozzles that slip is sprayed in the drying tower, the slip of atomizing relies on the surface tension of self to be shrunk to the reunion hollow ball shape, dry in hot blast, the heating and temperature control of drying tower well heater is between 150～280 ℃, and the height of temperature is regulated and exceeded with the powder thorough drying.To collect in the exsiccant reunion powder suction cyclonic separator by vacuum fan subsequently.The powder of collecting is sieved with mechanical sub-sieve, get the powder between 180～325 mesh sieves, its size range is 40～90 μ m (being called pelletizing finished product one time).Granularity greater than 90 μ m and less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip and use.
With a pelletizing finished product powder of 40～90 μ m granularities charging tray of packing into, after 10 minutes, obtain densification finished product (being called the secondary granulation finished product) at van-type heat treatment furnace internal heating to 700～1000 ℃ of sintering.Powder content of effective behind the sintering is greater than 99.9%, and remaining additive foreign matter content is less than 0.1%.With the loose density and the flowability of Hall under meter mensuration powder, scanning electron microscope is measured the pattern of powder, and X ray powder crystal diffraction is measured the crystalline structure of powder, measures the specific surface area of powder with the BET method.The results are shown in table 1.
The test data of the reunion shape nano zirconium oxide powder that table 1 embodiment 1 obtains
Technology Powder morphology Loose density g/cm 3 Mobile S/50g Specific surface area (BET) m 2/g
A granulation secondary granulation The hollow ball shape that loose hollow ball shape is fine and close 0.92 1.78 135 71 32.55 13.27
Embodiment 2:
Get the partially stabilized nano zirconium oxide powder of yttrium oxide (its ZrO of 9.5 kilograms of 20～60nm particle diameters 2With Y 2O 3Mass ratio is 94: 6), add each 0.2 kilogram of 0.1 kilogram in dextrin, polystyrene and polyvinyl alcohol caking agent, be made into 10 kilograms solid mixture through thorough mixing, adding 10 kilograms water purification again, to stir into the slip that homodisperse suspends stand-by.
With the centrifugal atomizing nozzle slip is sprayed in the drying tower, the rotating speed of centrifugal atomizer is 800～2000r/min, the slip particulate of atomizing relies on the surface tension of self to be shrunk to the solid sphere of reuniting, dry in hot blast, the heating and temperature control of drying tower well heater is between 150～280 ℃, and the height of temperature is regulated and exceeded with the powder thorough drying.To collect in the exsiccant reunion powder suction cyclonic separator by vacuum fan subsequently.The powder of collecting is sieved with mechanical sub-sieve, get the powder between 180～325 mesh sieves, its size range is 40～90 μ m (being called pelletizing finished product one time).Granularity greater than 90 μ m and less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip and use.
A pelletizing finished product powder of 40～90 μ m granularities charging tray of packing into after 30 minutes, is obtained densification finished product (being called the secondary granulation finished product) at van-type heat treatment furnace internal heating to 700～1000 ℃ of sintering.Powder content of effective behind the sintering is greater than 99.9%, and remaining additive foreign matter content is less than 0.1%.With the loose density and the flowability of Hall under meter mensuration powder, scanning electron microscope is measured the pattern of powder, and X ray powder crystal diffraction is measured the crystalline structure of powder, measures the specific surface area of powder with the BET method.The results are shown in table 2.
The test data of the reunion shape nano zirconium oxide powder that table 2 embodiment 2 obtains
Technology Powder morphology Loose density g/cm 3 Mobile S/50g Specific surface area (BET) m 2/g
A granulation secondary granulation The solid sphere that loose solid sphere is fine and close 0.94 1.86 83 44 29.58 9.42
Embodiment 3:
Get the partially stabilized nano zirconium oxide powder of yttrium oxide (its ZrO of 9.8 kilograms of 20～40nm particle diameters 2With Y 2O 3Mass ratio is 94: 6), each 0.1 kilogram of the carboxymethyl cellulose of adding and polyvinyl alcohol caking agent are made into 10 kilograms solid mixture through thorough mixing, and adding 10 kilograms water purification again, to stir into the slip that homodisperse suspends stand-by.
Carry gas with the purified pressurized air of drying, gaseous tension is controlled at 0.8Mpa, take two streaming nozzles that slip is sprayed in the drying tower, the slip of atomizing relies on the surface tension of self to be shrunk to the reunion hollow ball shape, dry in hot blast, the heating and temperature control of drying tower well heater is between 150～280 ℃, and the height of temperature is regulated and exceeded with the powder thorough drying.To collect in the exsiccant reunion powder suction cyclonic separator by vacuum fan subsequently.The powder of collecting is sieved with mechanical sub-sieve, get the powder between 180～325 mesh sieves, its size range is 40～90 μ m (being called pelletizing finished product one time).Granularity greater than 90 μ m and less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip and use.Adopt the plasma spheroidization technology to carry out secondary granulation in a pelletizing finished product powder of 40～90 μ m granularities, the finished product powder of a granulation is delivered to the plasma flame flow center, in the extremely short time, reach fine and close nodularization, spray moulding in the entry subsequently by powder feeder.Inserting after the oven dry of the secondary granulation powder collected in the water≤heating in 300 ℃ baking oven or the stove, remove organic additive composition residual in the powder, powder content of effective after the baking is greater than 99.9%, and remaining additive foreign matter content is less than 0.1% (being called the secondary granulation finished product).With the loose density and the flowability of Hall under meter mensuration powder, scanning electron microscope is measured the pattern of powder, and X ray powder crystal diffraction is measured the crystalline structure of powder, measures the specific surface area of powder with the BET method.The results are shown in table 3.
The test data of the reunion shape nano zirconium oxide powder that table 3 embodiment 3 obtains
Technology Powder morphology Loose density g/cm 3 Mobile S/50g Specific surface area (BET) m 2/g
A granulation secondary granulation The hollow ball shape of loose hollow ball shape densification 0.92 1.84 135 54 32.28 12.91
Embodiment 4:
Get the partially stabilized nano zirconium oxide powder of yttrium oxide (its ZrO of 9.8 kilograms of 20～40nm particle diameters 2With Y 2O 3Mass ratio is 92: 8), add 0.2 kilogram of polystyrene caking agent, be made into 10 kilograms solid mixture through thorough mixing, adding 10 kilograms water purification again, to stir into the slip that homodisperse suspends stand-by.
With the centrifugal atomizing nozzle slip is sprayed in the drying tower, the rotating speed of centrifugal atomizer is 800～2000r/min, the slip particulate of atomizing relies on the surface tension of self to be shrunk to the solid sphere of reuniting, dry in hot blast, the heating and temperature control of drying tower well heater is between 150～280 ℃, and the height of temperature is regulated and exceeded with the powder thorough drying.To collect in the exsiccant reunion powder suction cyclonic separator by vacuum fan subsequently.The powder of collecting is sieved with mechanical sub-sieve, get the powder between 180～325 mesh sieves, its size range is 40～90 μ m (being called pelletizing finished product one time).Granularity greater than 90 μ m and less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip and use.
Adopt the plasma spheroidization technology to carry out secondary granulation in a pelletizing finished product powder of 40～90 μ m granularities, the finished product powder of a granulation is delivered to the plasma flame flow center, in the extremely short time, reach fine and close nodularization, spray moulding in the entry subsequently by powder feeder.Inserting after the oven dry of the secondary granulation powder collected in the water≤heating in 300 ℃ baking oven or the stove, remove organic additive composition residual in the powder, powder content of effective after the baking is greater than 99.9%, and remaining additive foreign matter content is less than 0.1% (being called the secondary granulation finished product).With the loose density and the flowability of Hall under meter mensuration powder, scanning electron microscope is measured the pattern of powder, and X ray powder crystal diffraction is measured the crystalline structure of powder, measures the specific surface area of powder with the BET method.The result is as shown in table 2.
The test data of the reunion shape nano zirconium oxide powder that table 4 embodiment 4 obtains
Technology Powder morphology Loose density g/cm 3 Mobile S/50g Specific surface area (BET) m 2/g
A granulation secondary granulation Loose solid spherical compacted solid sphere 0.94 2.2 83 38 28.98 9.59

Claims (3)

1, a kind of preparation method of used for hot spraying nanometer Conglobation type Zirconium oxide powder is characterized in that preparation process is:
1st, batching: with granularity is that partially stabilized nano zirconium oxide powder of 20～60nm yttrium oxide and caking agent close than compounding by 95: 5～98: 2 quality, adds the water purification of 1～1.3 times of compound weight, is deployed into slip;
2nd, atomization drying: with the resulting slip of step 1 atomization drying in spray-drying tower, the drying tower temperature is controlled in 110～300 ℃ of scopes, makes reunion powder;
3rd, screening: the resulting reunion powder of step 2 is sieved, get particle between 180～325 mesh sieves, i.e. 40～90 μ m particles, all the other powder are as foundry returns;
4th, densification: with the resulting granularity of step 3 is that the powder of 40～90 μ m places the sintering oven sintering, make densification, its temperature is 700～1000 ℃, sintering time is 10～30 minutes, then the dense powder that sinters is sieved, get dense powder between 180～325 mesh sieves, promptly get product; Perhaps resulting 40～90 μ m powder of step 3 are delivered to the plasma flame flow center by powder feeder, fine and close nodularization sprays into moulding in the water subsequently, then with after the moulding powder oven dry, adds residual organic binder bond of heat extraction and moisture content in≤300 ℃, promptly gets product;
ZrO in the partially stabilized nano zirconium oxide powder of described yttrium oxide 2With Y 2O 3Mass ratio be 94: 6～92: 8; Described caking agent is one or more the mixture in dextrin, polyvinyl alcohol, carboxymethyl cellulose, the polystyrene.
2, preparation method as claimed in claim 1 is characterized in that described atomization drying is with the centrifugal atomizing nozzle slip to be sprayed into drying in the drying tower, and the rotating speed of its centrifugal atomizer is 800～2000r/min.
3, preparation method as claimed in claim 1 is characterized in that described atomization drying is is carrier with dried compressed air, adopts two streaming nozzles that slurry is sprayed into the drying tower inner drying.
CN 200410061306 2004-12-09 2004-12-09 Prepn of nanometer aggregated zirconia powder for hot spraying Expired - Fee Related CN1256393C (en)

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