CN100334037C - Nanostructured yttrium stable zirconium oxide agglomerate type powder and its production method - Google Patents
Nanostructured yttrium stable zirconium oxide agglomerate type powder and its production method Download PDFInfo
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
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Abstract
The present invention relates to Yt stabilized zirconia aggregate powder with a nanometer structure, and the inner part of which is composed of nanometer crystal particles which are less than 100 nm; the powder has a spherical aggregate structure, the particle size is from 40 to 90 mum, nanometer zirconium dioxide particles in the aggregate powder are in body surface contact, and a nonexposed place is a pure cavity. The present invention has the method that water is added into the nanometer zirconium dioxide particles containing yttrium oxide, and aqueous suspended colloid is obtained; the present invention is prepared by spray drying, sieving, heat treatment and plasma densification. The present invention has the advantages of less production technological flow, simple operation, low cost and continuous industrial production in a large scale. The product meets the requirements of the hot spraying technologies of plasma spraying, flame spraying, electric arc spraying, etc. and is used for preparing various thermal barrier coatings with high temperature resistance or coatings with high temperature resistance, wear resistance and corrosion resistance. The product is applied to the industry of spaceflight, large-sized gas turbine engines, ships, automobiles, machinery, chemical engineering, etc.
Description
Technical field
The present invention relates to a kind of yttrium stable zirconium oxide agglomerate type powder material and production method thereof of nanostructure, this powdered material is specially adapted to thermospray (plasma spraying or flame plating) prepared thermal barrier coating or high-sintering process prepares structural ceramics.
Background technology
Zirconium white (ZrO
2) have excellent physics and chemical property, be a kind of important 26S Proteasome Structure and Function stupalith.Common zirconium white ℃ exists with monocline mutually at normal temperature to 1170, changes cubic phase when being heated to 1170～2370 ℃ into, becomes cube phase (2700 ℃ of left and right sides fusions) by tetragonal phase converting in the time of more than 2370 ℃.Because the high temperature phase (cube phase or cubic phase) of pure zirconia be along with the reduction of temperature can be transformed into low temperature phase (monocline phase), and be attended by the volumetric expansion about 5～7%.If this crystal transition and the volume change of pure zirconia as structural ceramics and function ceramics coated material, being subjected to can causing excessive thermal stress under the thermal cycle conditions, make ceramic product or coating cracking and spalling failure.Obtain high temperature phase zircite stable under the room temperature, some other oxide compound that just need mix in zirconium white as yttrium oxide, calcium oxide, magnesium oxide, cerium oxide, aluminum oxide etc., forms zirconic composite oxides.Other oxide-doped zirconium white composite oxides have application widely at structural ceramic material and ceramic material field.
Zirconium white is applied to the research of thermal barrier coating, and after succeeing on the whirlpool steam turbine of the seventies in 20th century, the research to zirconia coating both at home and abroad reaches a peak in the eighties in 20th century, and a large amount of studies show that, with yttrium oxide (Y
2O
3) (massfraction is 6～8%) stable ZrO
2Its thermal shock resistance of material is superior.
Yttrium stable zirconium oxide is compared with other ceramic coating material as the heat barrier coat material of widespread use, has high temperature resistant, corrosion-resistant, wear-resistant, high intensity and fracture toughness property, high coefficient of linear expansion (near metal matrix, is about 10 * 10
-6/ K) and low thermal conductivity excellent properties such as (1W/mK), especially when 1000 ℃ of high temperature, its thermal conductivity numerical value is minimum in all dense ceramic material, it is mutually compound with metallic matrix with coating form, and makes it can stand higher use temperature when improving metal fever end pieces opposing high temperature corrosion ability.
Since 20 end of the centurys, along with the maturation of nanosecond science and technology and nano powder preparation technology, nanometer ZrO
2The preparation of coating has become the emphasis of research gradually, utilizes the nanostructure ceramic heat-barrier coating of nanotechnology exploitation to be meant the microstructure of ceramic coating such as the nanometer level (2～100nm) that crystal grain, hole etc. are in ultra-fine size.Thereby mechanics and physicals to coating produce material impact, obtain the performance more excellent than ordinary hot barrier coating.
The key of preparation nanostructure thermal barrier coating is a hot-spraying nano structure agglomerate type powder, and it must keep nanostructure, and satisfies the requirement of spraying coating process, as granular size and distribution thereof, particle shape, flowability etc.Because the mobile extreme difference of nano-powder can not satisfy the powder feeding requirement of spraying coating process.During thermospray, have only particle just can possess the required quality of plasma thermal sprayed when a certain size and density, granular mass is too little, can not obtain enough kinetic energy, and spray is less than workpiece surface.Prepare Y
2O
3Stable ZrO
2The nanocrystalline structure thermal barrier coating, used nano-powder must pass through mist projection granulating and densification process, and nano raw material is made Conglobation type micron spraying powder, adopts plasma spraying or HVOF (High Velocity Oxygen Fuel) Technology to be deposited as coating again.So Y
2O
3Stabilized nanoscale structure ZrO
2The exploitation of agglomerate type powder and production technique thereof, it is the prerequisite of preparation nanostructure thermal barrier coating, its key is to keep nanocrystalline structure constant, is satisfied with plasma spraying or HVOF (High Velocity Oxygen Fuel) processing requirement again, and obtains the due high-performance of nanostructure thermal barrier coating.
The powder of the nano zircite Conglobation type of used for hot spraying mainly adopts spray-drying process and microemulsion method (reverse micelle method) preparation at present.These methods respectively have its characteristics, but also have many deficiencies.As spray-drying process is that nano level zirconium white micro mist is mixed with a certain amount of binding agent, adds an amount of water or other solvents and is mixed with certain density slip.Adopt certain pressure that it is ejected in the drying tower, the surface tension by self is agglomerated into sphere when dry in hot blast.Shrink because this agglomerate type powder is a nature, the loose density of powder is little, and is mobile poor.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.Because the various organic additives that add in this method, it is clean all to volatilize under the hot conditions of thermal spray process utmost point short period of time again, is present in the coating with the form of tiny carbon granules, and the performance of coating is had a negative impact.Microemulsion method is a kind of milling method that development in recent years is got up.The powder that makes is spherical in shape, and globule size unanimity, weak point are the raisings of production cost, is difficult to realize mass-producing.In addition, what have is used in combination aforementioned production method with plasma spraying pyrolyzing method, supercritical drying etc., only carried out some limited research and discussions, then too wide in the gap apart from production practical application and mass-producing.
Summary of the invention
Purpose of the present invention just provides a kind of yttrium stable zirconium oxide agglomerate type powder with nanostructure, it does not contain harmful impurity, aggregate density height, good fluidity, the needs of nanostructure hot-spraying techniques can be satisfied, higher coating density and higher binding strength can be obtained.
Another object of the present invention provides the production method of the yttrium stable zirconium oxide agglomerate type powder with nanostructure, and this technical matters flow process is few, working method is simple, turnout is big, and is safe and reliable, and low cost of manufacture is suitable for suitability for industrialized production.
The yttrium stable zirconium oxide agglomerate type powder of the nanostructure that the present invention proposes is characterized in that this agglomerate type powder is by containing 3～9wt%Y
2O
3Nanometer ZrO
2Powder granule constitutes, and the particulate average mean crystal size is 5～60nm, is the body surface contact between the nano zircite particle in the agglomerate type powder, and Jie Chu place is not pure cavity.
The yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure is characterized in that crystalline structure is respectively monocline phase+cubic phase (cube phase) or pure cubic phase (cube phase).
The production method of the yttrium stable zirconium oxide agglomerate type powder of nanostructure is characterized in that comprising the steps:
With yttrium stabilized nano level ZrO
2Powder granule mixes with water, is prepared into the water nano suspensoid;
Adopt drying process with atomizing that the water nano suspensoid is made the micron order agglomerate type powder;
Agglomerate type powder is heat-treated;
Powder after adopting plasma technology to thermal treatment carries out densification, obtains the yttrium stable zirconium oxide agglomerate type powder of nanostructure.
The production method of the yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure is characterized in that used yttrium stabilized nanoscale Zirconium powder feed particles granularity is between 5～60nm.
The production method of the yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure is characterized in that water nano particle suspension colloidal medium is a water, and the weight ratio of nano particle and water is 1: 1～3.
The production method of the yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure is characterized in that spray drying process can be one of two fluid-types or centrifugal spray-drying process.
The production method of the yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure, the thermal treatment temp that it is characterized in that spray-dried powders is between 200～600 ℃
The production method of the yttrium stable zirconium oxide agglomerate type powder of aforesaid nanostructure, the plasma body densificationization that it is characterized in that agglomerate type powder can be direct-current plasma or high-frequency induction plasma body.
The production method of the yttrium stable zirconium oxide agglomerate type powder of nanostructure, concrete steps are as follows:
(1) the stable dispersion suspension colloid of preparation nano-powder: will add an amount of pure water in the yttrium stabilized nanoscale Zirconium powder, the consumption of water is 1～3 times of powder quality by weight, back injection colloidal mill stirs, handled 5～30 minutes continuously, be prepared into nano-powder suspension aqueous colloidal with proper concn and certain viscosity;
(2) aqueous colloidal of nano zirconium oxide powder is made the micron order agglomerate type powder with certain particle size distribution by drying process with atomizing, an i.e. granulation: spray pattern is centrifugal or two fluid-types, the slip of atomizing relies on the surface tension of self to be shrunk to sphere, by warm air the water in the slip is volatilized fast, the dry spherical powder that forms of droplet; Spray-dired inlet temperature is 180～350 ℃, and air outlet temperature is controlled at 80～180 ℃, and the height of temperature is regulated and exceeded with the powder thorough drying; To collect in the exsiccant agglomerate type powder suction cyclonic separator by exhausting subsequently.This process agglomerate type powder still is a nanostructure, and granularity is 5～100 μ m, is shaped as sphere;
(3) screening; Because spray-dired spherical agglomerated type powder has certain particle distribution (5～100 μ m), pass through mechanical grading, choose the powder (40～100 μ m) that meets the finished product size range that the plasma spraying thermal barrier coating uses, other powder can be made colloid, mist projection granulating once more more again;
The thermal treatment of (4) prilling powders: with a prilling powder of 40～100 μ m granularities pack into charging tray in the van-type High Temperature Furnaces Heating Apparatus in 300～600 ℃ of thermal treatments of carrying out 5～30 minutes; Remove the residual water-content in the powder, eliminate the relaxation phenomena and the internal stress at nano particle interface in the powder, reduce the grain breakage rate in the plasma body densificationization powder feeding process, improve product quality and productive rate;
(5) densification of agglomerate type powder; Because the agglomerate type powder structure of a granulation is looser, broken easily, in thermal spray process, easily float, sedimentation effect is not high, and the coating of formation is not fine and close, need carry out densification (the fine and close nodularization of plasma body) to the agglomerate type powder of a granulation.The plasma body that adopts can be high-frequency induction plasma body or direct-current plasma, and temperature is 5000～10000 ℃, and gases used is air, argon gas, hydrogen and nitrogen.Adopt the mode of quenching (water-cooled or air cooling) to collect powder, crystalline is grown up in the control powder.Strictly control the power parameter and the operational throughput of grain agglomerate type powder once, manufacture not only fine and close but also keep the constant hot spray powder of nanocrystalline structure.
(6) nanostructure Conglobation type yttrium stable zirconium oxide powder finished product.With collect through the agglomerate type powder of plasma body densificationization in 100～300 ℃ of oven dry, sieve again, obtain the powder-product of finished product powder index request.
The gordian technique and the craft feature of product of the present invention are:
(1) do not use any additives (caking agent, suspension agent, dispersion agent, wetting agent, tensio-active agent) in the aqueous colloidal preparation process, but directly utilize the natural characteristics (particle surface unsaturation chemical bond is many, surfactivity big, be easy to the absorption bonding) of nano-powder and the key bridge reactive force of water, in spray process, form agglomerate type powder.All technological process can not introduced any impurity, has avoided pollution, has guaranteed high purity, high-specific surface area and certain surfactivity of product.
(2) the nanocrystal granularity in spray drying technology of Cai Yonging (prilling process) and transient plasma densification technology (secondary granulation method) the restriction agglomerate type powder grows up, keep its grain-size constant substantially, for the realization of follow-up plasma spraying nano coating is laid a good foundation.
(3) it is relatively low that nano raw material prepares the agglomerate type powder cost, is easy to promote.
(4) because spray drying technology (prilling process) and plasma body densificationization technology (secondary granulation method) all belong to sophisticated industrial agglomeration technique, by the control of technical parameter and the transformation of critical process process, the whole preparation process flow process is few, equipment is simple, processing parameter is easy to control, is suitable for serialization scale operation.
Description of drawings:
Fig. 1, embodiment of the invention agglomerate type powder internal structure synoptic diagram.Wherein, 1 agglomerate type powder, 2 nano particles, 3 body surface contact surfaces, 4 pure cavitys.
Fig. 2, granulation stereoscan photograph of embodiment of the invention agglomerate type powder.
Fig. 3, embodiment of the invention agglomerate type powder secondary granulation stereoscan photograph.
Concrete embodiment
In order to be illustrated more clearly in the present invention, enumerate following specific embodiment.
Embodiment 1:
Get 10 kilograms and contain 6wt%Y
2O
3Nanometer ZrO
2(yttrium oxide is partially stabilized) powder, average crystalline particle diameter 20nm adds 15 kilograms ultra-pure water, stirs, and with colloidal mill homodisperse 10 minutes, it was stand-by to be prepared into stable suspension slip.
With carrying gas through the pressurized air that purifies, gaseous tension is controlled at 0.3～0.8MPa, take two fluid-type 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 Conglobation type sphere, the intake air temperature of drying tower is controlled at 200 ℃, the air outlet temperature is controlled at 120 ℃, makes aerosol mist drop in thorough drying in the hot blast.To collect in the exsiccant agglomerate type powder suction cyclonic separator by exhausting subsequently.
The powder of collecting is sieved with mechanical sub-sieve, present embodiment finished powder size range is between 40～100 μ m (i.e. 150～350 orders), granularity greater than 100 μ m, less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip again.
With the charging tray 300 ℃ of thermal treatment 20 minutes in the van-type High Temperature Furnaces Heating Apparatus of packing into of a prilling powder of 40～100 μ m granularities.Remove the residual water-content in the powder, eliminate the relaxation phenomena and the internal stress at nano particle interface in the powder, reduce the grain breakage rate in the plasma body densificationization powder feeding process, improve product quality and productive rate.
The using plasma technology is to the heat treated prilling powder densification of process, and plasma power 30kW, argon gas, hydrogen and nitrogen are working gas, by powder feeder the powder of a granulation are delivered to the plasma flame flow center, powder feed rate 60g/ minute.Make powder in the extremely short time, reach fine and close nodularization, spray quenching collection in the entry.The secondary granulation powder of the collecting oven dry of in 100～300 ℃ baking oven or High Temperature Furnaces Heating Apparatus, heating, remove moisture content.Obtain the yttrium stable zirconium oxide agglomerate type powder of nanostructure.This process agglomerated type powder further shrinks on original particulate basis, has improved the loose density and the flowability of powder greatly, obtains to satisfy the agglomerate type powder of plasma spray coating process requirement.At 40～90 μ m, crystal size remains unchanged or only has small growing up, agglomerate type powder pattern to have tangible globosity feature the grain of secondary granulation powder through scope, and powder flowbility is good, and the prolonged preservation and the back that makes moist are difficult for broken.
The content of effective of agglomerate type powder is greater than 99.9%, and the content that is present in the trace impurity in the nano zircite particle 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 and the primary particle crystalline mean particle size of powder.The result is as shown in table 1.
The test data of the yttrium stabilized nanoscale structural zirconia agglomerate type powder that table 1 embodiment 1 obtains
| Technology | Powder morphology | Loose density g/cm 3 | Mobile S/50g | Crystal mean particle size nm |
| A granulation secondary granulation | Spherical compacted sphere | 0.92 1.75 | 102 50 | 20 48 |
Embodiment 2:
Get 10 kilograms and contain 6wt%Y
2O
3Nanometer ZrO
2(yttrium oxide is partially stabilized) powder, average crystalline particle diameter 20nm adds 15 kilograms ultra-pure water, stirs, and with colloidal mill homodisperse 10 minutes, it was stand-by to be prepared into stable suspension slip.
With the centrifugal atomizing dish slip is sprayed in the drying tower, the rotating speed of centrifugal atomizer is 10000r/min, the slip particle of atomizing relies on the surface tension of self to be shrunk to the Conglobation type sphere, hot blast in dry, the heating and temperature control of drying tower well heater is at 200 ℃, make the moisture rapid evaporation in the droplet, collect the exsiccant agglomerate type powder with cyclonic separator.The powder of collecting is sieved with mechanical sub-sieve, and size range is continuing to employ between 40～100 μ m (i.e. 150～350 orders), granularity greater than 100 μ m, less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip again.
With the charging tray 500 ℃ of thermal treatment 10 minutes in the van-type heat treatment furnace of packing into of the dried powder of 40～100 μ m granularities.Remove the residual water-content in the powder, eliminate the relaxation phenomena and the internal stress at nano particle interface in the powder, reduce the grain breakage rate in the plasma body densificationization powder feeding process, improve product quality and productive rate.
The using plasma technology is to carrying out densification through heat treated prilling powder, and plasma power 30kW, argon gas, hydrogen and nitrogen are working gas, by powder feeder the powder of a granulation are delivered to the plasma flame flow center, powder feed rate 60g/ minute.Make powder in the extremely short time, reach fine and close nodularization, spray quenching collection in the entry.The secondary granulation powder of the collecting oven dry of in 100～300 ℃ baking oven or High Temperature Furnaces Heating Apparatus, heating, remove moisture content.Obtain the yttrium stable zirconium oxide agglomerate type powder of nanostructure.
The powder content of effective is greater than 99.9%, and the content that is present in the trace impurity in the nano zircite particle 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 and the primary particle crystalline mean particle size of powder.The result is as shown in table 2.
The test data of the Conglobation type shape nano zirconium oxide powder that table 2 embodiment 2 obtains
| Technology | Powder morphology | Loose density g/cm 3 | Mobile S/50g | Average mean crystal size/nm |
| A granulation secondary granulation | Spherical compacted solid sphere | 0.90 2.06 | 98 40 | 20 45 |
Embodiment 3:
Get 10 kilograms and contain 8wt%Y
2O
3Nanometer ZrO
2(yttrium oxide is partially stabilized) powder, average crystalline particle diameter 10nm adds 20 kilograms ultra-pure water, stirs, and with colloidal mill homodisperse 10 minutes, it was stand-by to be prepared into stable suspension slip.
With carrying gas through the pressurized air that purifies, gaseous tension is controlled at 0.3～0.8MPa, take two fluid-type 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 Conglobation type sphere, the intake air temperature of drying tower is controlled at 240 ℃, the air outlet temperature is controlled at 150 ℃, makes aerosol mist drop in thorough drying in the hot blast.To collect in the exsiccant agglomerate type powder suction cyclonic separator by exhausting subsequently.
The powder of collecting is sieved with mechanical sub-sieve, present embodiment finished powder size range is between 40～100 μ m (i.e. 150～350 orders), granularity greater than 100 μ m, less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip again.
With the charging tray 300 ℃ of thermal treatment 20 minutes in the van-type High Temperature Furnaces Heating Apparatus of packing into of a prilling powder of 40～100 μ m granularities.Remove the residual water-content in the powder, eliminate the relaxation phenomena and the internal stress at nano particle interface in the powder, reduce the grain breakage rate in the plasma body densificationization powder feeding process, improve product quality and productive rate.
The using plasma technology is to the heat treated prilling powder densification of process, and plasma power 50kW, argon gas, hydrogen and nitrogen are working gas, by powder feeder the powder of a granulation are delivered to the plasma flame flow center, powder feed rate 100g/ minute.Make powder in the extremely short time, reach fine and close nodularization, spray quenching collection in the entry.The secondary granulation powder of the collecting oven dry of in 100～300 ℃ baking oven or High Temperature Furnaces Heating Apparatus, heating, remove moisture content.Obtain the yttrium stable zirconium oxide agglomerate type powder of nanostructure.
The content of effective of agglomerate type powder is greater than 99.9%, and the content that is present in the trace impurity in the nano zircite particle 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 and the primary particle crystalline mean particle size of powder.The result is as shown in table 3.
The test data of the yttrium stabilized nanoscale structural zirconia agglomerate type powder that table 3 embodiment 3 obtains
| Technology | Powder morphology | Loose density g/cm 3 | Mobile S/50g | Crystal mean particle size nm |
| A granulation secondary granulation | Spherical compacted sphere | 0.85 1.94 | 105 48 | 12 46 |
Embodiment 4:
Get 10 kilograms and contain 8wt%Y
2O
3Nanometer ZrO
2(yttrium oxide is partially stabilized) powder, average crystalline particle diameter 10nm adds 20 kilograms ultra-pure water, stirs, and with colloidal mill homodisperse 10 minutes, it was stand-by to be prepared into stable suspension slip.
With the centrifugal atomizing dish slip is sprayed in the drying tower, the rotating speed of centrifugal atomizer is 15000r/min, the slip particulate of atomizing relies on the surface tension of self to be shrunk to the Conglobation type sphere, hot blast in dry, the heating and temperature control of drying tower well heater is at 200 ℃, make the moisture rapid evaporation in the droplet, collect the exsiccant agglomerate type powder with cyclonic separator.The powder of collecting is sieved with mechanical sub-sieve, and size range is continuing to employ between 40～100 μ m (i.e. 150～350 orders), granularity greater than 100 μ m, less than the powder of 40 μ m as foundry returns, when carrying out a granulation next time, make slip again.
With the charging tray 400 ℃ of thermal treatment 20 minutes in the van-type High Temperature Furnaces Heating Apparatus of packing into of a prilling powder of 40～100 μ m granularities.Remove the residual water-content in the powder, eliminate the relaxation phenomena and the internal stress at nano particle interface in the powder, reduce the grain breakage rate in the plasma body densificationization powder feeding process, improve product quality and productive rate.
The using plasma technology is to the heat treated prilling powder densification of process, and plasma power 30kW, argon gas, hydrogen and nitrogen are working gas, by powder feeder the powder of a granulation are delivered to the plasma flame flow center, powder feed rate 80g/ minute.Make powder in the extremely short time, reach fine and close nodularization, spray quenching collection in the entry.The secondary granulation powder of the collecting oven dry of in 100～300 ℃ baking oven or High Temperature Furnaces Heating Apparatus, heating, remove moisture content.Obtain the yttrium stable zirconium oxide agglomerate type powder of nanostructure.
The content of effective of agglomerate type powder is greater than 99.9%, and the content that is present in the trace impurity in the nano zircite particle 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, the results are shown in accompanying drawing; X ray powder crystal diffraction is measured the crystalline structure and the primary particle crystalline mean particle size of powder.The result is as shown in table 4.
The test data of the Conglobation type shape nano zirconium oxide powder that table 4 embodiment 4 obtains
| Technology | Powder morphology | Loose density g/cm 3 | Mobile S/50g | Crystal mean particle size nm |
| A granulation secondary granulation | Loose solid spherical compacted solid sphere | 0.94 2.1 | 83 38 | 10 52 |
The protection domain of present patent application is not subjected to above-mentioned restriction of giving an example.Yttrium stable zirconium oxide agglomerate type powder by the disclosed nanostructure of present patent application, mainly utilize characteristics such as its heat-conduction coefficient is low, coefficient of linear expansion is big, high-temperature stability is good, can be widely used in hot-spraying techniques and prepare various high temperature resistance thermal barrier coatings or high temperature resistance abrasion performance, corrosion-resistant finishes.
Nanostructure Conglobation type yttrium stable zirconium oxide powder of the present invention becomes thermal barrier coating through the plasma spraying prepared, coat-thickness 300～400 μ m.Through to its Performance Detection, to compare with the micrometer structure coating of routine, the microhardness of nano-structured coating is 1.5 times of conventional micron coating; Anti-thermal shock (thermal shocking) performance improves at least 2～3 times; Shock resistance (reflection coating toughness and cracking resistance line extended capability) obviously strengthens; Bond Strength of Coating has improved 1.5 times; Effect of heat insulation has improved 1.5～2 times.The nanostructure thermal barrier coating has important application prospects in industries such as aerospace, large-scale gas turbine, boats and ships, automobile, machinery, chemical industry.
Claims (7)
1, the yttrium stable zirconium oxide agglomerate type powder of nanostructure is characterized in that this agglomerate type powder is by containing 3～9wt%Y
2O
3Nanometer ZrO
2Particle constitutes, and the particulate crystal size is 5～60nm, is the body surface contact between the nano zircite particle in the agglomerate type powder, and Jie Chu place is not pure cavity.
2, the yttrium stable zirconium oxide agglomerate type powder of nanostructure as claimed in claim 1 is characterized in that crystalline structure is respectively monocline phase+four directions phase or pure cubic phase.
3, the production method of the yttrium stable zirconium oxide agglomerate type powder of the described nanostructure of claim 1 is characterized in that comprising the steps:
With yttrium stabilized nano level ZrO
2Powder granule mixes with water, is prepared into the water nano suspensoid;
Adopt drying process with atomizing that the water nano suspensoid is made the micron order agglomerate type powder;
Agglomerate type powder is heat-treated;
Powder after adopting plasma technology to thermal treatment carries out densification, obtains the yttrium stable zirconium oxide agglomerate type powder of nanostructure.
4, the production method of the yttrium stable zirconium oxide agglomerate type powder of nanostructure according to claim 3 is characterized in that water nano particle suspension colloidal medium is a water, and the weight ratio of nano particle and water is 1: 1～3.
5, according to the production method of the yttrium stable zirconium oxide agglomerate type powder of the described nanostructure of claim 3, it is characterized in that spray drying process is one of two fluid-types or centrifugal spray-drying process.
6, the production method of the yttrium stable zirconium oxide agglomerate type powder of nanostructure according to claim 3, the thermal treatment temp that it is characterized in that spray-dried powders is between 200～600 ℃
7, the production method of the yttrium stable zirconium oxide agglomerate type powder of nanostructure according to claim 3, the plasma body densificationization that it is characterized in that Conglobation type are direct-current plasma or high-frequency induction plasma body.
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| KR101323697B1 (en) * | 2006-08-17 | 2013-11-08 | 하.체. 스타르크 게엠베하 | Zirconium oxide and method for the production thereof |
| CN101550001B (en) * | 2009-04-09 | 2012-10-31 | 上海交通大学 | Yttrium zirconium composite nano-ceramic powder and preparation method thereof |
| CN108660403A (en) * | 2018-05-15 | 2018-10-16 | 北京金轮坤天特种机械有限公司 | A method of plasma physical vapor deposit thermal barrier coatings powder is prepared using oxide raw material |
| CN109173925B (en) * | 2018-07-28 | 2020-08-18 | 西安交通大学 | Hierarchical discrete high-efficiency evaporation multilevel structure powder material and preparation method thereof |
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| KR940006423A (en) * | 1992-06-01 | 1994-03-23 | 모리시타 요이찌 | Heating device |
| CN1382662A (en) * | 2002-02-20 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Low-temp sinter process for squar-phase zirconium oxide polycrystal with stabilized nano yttrium oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR940006423A (en) * | 1992-06-01 | 1994-03-23 | 모리시타 요이찌 | Heating device |
| CN1382662A (en) * | 2002-02-20 | 2002-12-04 | 中国科学院上海硅酸盐研究所 | Low-temp sinter process for squar-phase zirconium oxide polycrystal with stabilized nano yttrium oxide |
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