CN101532776A - Crucible with Y2O3 etching resistant coating and method for producing Y*O* etching resistant coating using slip casting moulding technique - Google Patents

Crucible with Y2O3 etching resistant coating and method for producing Y*O* etching resistant coating using slip casting moulding technique Download PDF

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Publication number
CN101532776A
CN101532776A CN200910079973A CN200910079973A CN101532776A CN 101532776 A CN101532776 A CN 101532776A CN 200910079973 A CN200910079973 A CN 200910079973A CN 200910079973 A CN200910079973 A CN 200910079973A CN 101532776 A CN101532776 A CN 101532776A
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crucible
resistant coatings
erosion resistant
slurry
base
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CN200910079973A
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CN101532776B (en
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唐晓霞
张花蕊
高明
张虎
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JIANGSU HANGTAI NEW MATERIAL CO., LTD.
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Beihang University
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Abstract

The invention discloses a crucible with Y2O3 etching resistant coating and a method for producing the Y2O3 etching resistant coating using slip casting moulding technique. Y2O3 etching resistant sizing agent is prepared at the inner wall of the crucible basal body by the slip casting moulding technique and a Y2O3 etching resistant coating with the thickness of 0.5mm-8mm is formed. The Y2O3 etching resistant sizing agent comprises multilevel Y2O3 raw material powder, dispersant, binder and de-ionized water. The highest smelting temperature of the crucible with Y2O3 etching resistant coating is 1600-2000 DEG C, thereby meeting the requirement of smelting of high activity melt alloy such as Ti alloy, Nb alloy and rare earth alloy and alloy containing high activity elements such as, Ti, Al, Nb, Hf, rare earth elements and the like.

Description

A kind of have a Y 2O 3Erosion resistant coatings crucible and employing rolling pulp moulding process Y processed thereof 2O 3The method of erosion resistant coatings
Technical field
The present invention relates to a kind of coating material that is produced on the crucible inwall.More particularly, refer to that a kind of employing rolling pulp moulding process is with Y 2O 3Be produced on existing crucible base inwall, obtain having Y through high temperature sintering then 2O 3The Novel crucible of erosion resistant coatings.
Background technology
High temperature alloy is a critical material of making turbogenerator, occupy an important position in the Aeronautics and Astronautics field, therefore the melting of high temperature alloy is one of emphasis of the research of materials processing direction in recent years, result of study shows that the impurity element and the field trash of sneaking in the high temperature alloy fusion process have significant impact to alloy property, thereby the ultrapure clean melting of high temperature alloy has crucial meaning, and the chemical stability and the corrosion resistance of crucible for smelting are had higher requirement.
Ceramic crucible plays more and more important effect, Y in the high temperature alloy melting in recent years 2O 3Crucible, Al 2O 3Crucible or ZrO 2Hear resistance and thermal shock resistance are applied in alloy melting the high temperature oxide crucibles such as crucible because having preferably.Yet the Y that molds at present 2O 3Crucible, Al 2O 3Crucible and ZrO 2Crucible is normally made by the coarse granule grating, the crucible base grain size is inhomogeneous, between coarse granule and fine grained in conjunction with loose even exist than macrovoid, in the process of high melt, make the material of crucible and easily sneak in the melted material, affect the performance of melted material.The anti-melt infiltration of the unlikely close crucible of this outer surface is poor, has a strong impact on the service life of crucible.Therefore be necessary to develop a kind of high anti-melt permeability and the rodent crucible that is coated with of high resistance.
Yittrium oxide (Y 2O 3) be a kind of refractory oxides, its fusing point is up to more than 2400 ℃, and the decomposition pressure under 1500 ℃ is 1.62 * 10 -2MPa.Y 2O 3Pottery not only has good hear resistance and high-temperature stability, and has preferably chemical stability, is to make the preferred material that alloy melting is used crucible coating layer.In addition, because Y 2O 3High chemical stability, at high temperature be difficult for reacting with active metals such as Ti, Al, so Y 2O 3The erosion resistant coatings crucible will significantly improve Al 2O 3Crucible, ZrO 2The chemical stability of crucible.
Summary of the invention
One of purpose of the present invention provides a kind of Y of having 2O 3The Novel crucible of erosion resistant coatings is to adopt the rolling pulp moulding process with Y 2O 3The preparation of erosion resistant coatings slurry is on existing crucible base inwall.Of the present invention have a Y 2O 3The erosion resistant coatings crucible can improve anti-melt permeability and the anti-melt aggressivity of crucible base.
Two of purpose of the present invention is to propose a kind of employing rolling pulp moulding process with Y 2O 3The preparation of erosion resistant coatings slurry is in the method for crucible base inwall, this coating production is the control that realizes molding thickness by control rolling pulp rotating speed and time, forming method is simply controlled, the Novel crucible that makes has higher chemical stability and lower porosity, has improved anti-melt permeability and the anti-melt aggressivity of former crucible.
A kind of Y that has of the present invention 2O 3The erosion resistant coatings crucible, this has Y 2O 3The erosion resistant coatings crucible is by crucible base and Y 2O 3Erosion resistant coatings consists of, and Y 2O 3The erosion resistant coatings preparation is on the inwall of crucible base.This crucible can be applicable under 1600 ℃～2000 ℃ hot environments and use.
A kind of employing rolling pulp moulding process fixture has Y 2O 3The method of erosion resistant coatings crucible, it has the following step:
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, dispersant, binding agent and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, adds the multistage Y of 125.00g～409.09g in the deionized water of 100ml 2O 3The dispersant of raw meal, 1.25g～5.00g and the binding agent of 0.80g～3.20g;
Described dispersant is ammonium polyacrylate or gum arabic;
Described binding agent is polyvinyl alcohol or carboxymethyl cellulose;
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 50g～80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g～30g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
Adopt hairbrush that the moulding crucible is cleared up, obtain crucible base 1 after cleaning out;
The 3rd step: Y processed 2O 3Erosion resistant coatings
Step (A) is installed in second crucible base 1 that obtain of step on the anchor clamps 3 that roll the slurry former, regulates the angle of established angle α, α=30 °～45 °;
Step (B), the Y that the first step is obtained 2O 3The anti-erosion slurry joins in the crucible base 1;
Step (C) is regulated rotating shaft 5 and is rolled slurry along clockwise direction, rotating shaft rotating speed v=1～5r/min;
Step (D) is rolled slurry according to the coating layer thickness d=0.5mm～8mm that sets, and rolls to obtain first base substrate after slurry is finished;
Step (E) behind hothouse inner drying 20～50h of 25 ℃, makes second base substrate with first base substrate again behind high temperature drying 10～30h in 120 ℃ baking oven;
Step (F) is put into the sintering furnace high temperature sintering with second base substrate, and the firing time is 30～100h, and sintering temperature is 1500 ℃～1800 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
A kind of Y that has of the present invention 2O 3The advantage of erosion resistant coatings crucible is:
(1) smelting temperature reaches 1600 ℃～2000 ℃.Be applicable to the melting of high activity metal alloy, as Ti alloy, Nb alloy, rare earth alloy and contain the melting of the alloy of Ti, Al, Nb, Hf, the contour active element of rare earth element.
(2) crucible of the present invention melting by the process of fusant in, crucible with contacted at the interface by the fusant melt, its raw material of making crucible does not participate in by the reaction of fusant melt, has improved effectively by the degree of purity of fusant melt, more helps preparing high performance alloy material (by fusant).
(3) crucible of the present invention is through sem analysis, its internal layer homogeneous grain size, the little and even pore distribution of porosity.Crucible of the present invention has significantly improved anti-melt erosion, the anti-melt permeability of existing crucible, has effectively stoped the inner surface of crucible particle to sneak into the pollution that causes in the melted material, is conducive to improve the melted material alloy property.Crucible of the present invention has effectively improved existing Y 2O 3Crucible, Al 2O 3Crucible and ZrO 2The crucible grain size is inhomogeneous, between coarse granule and fine grained in conjunction with loose even have a more macroporous state.
(4) crucible of the present invention does not ftracture in fusion process, but and repeated multiple times use the service life of effectively having improved crucible.
The present invention adopts the rolling pulp moulding process at existing Y 2O 3Crucible, Al 2O 3Crucible and ZrO 2The inwall of crucible Y processed 2O 3The method of erosion resistant coatings, the advantage of its preparation method is:
(1) by regulating established angle α between rotating shaft and the processing platform=30 °～45° angle degree, and the velocity of rotation v=1 of control crucible base～5r/min, obtains Y on the crucible inwall by simple rolling pulp technology 2O 3Erosion resistant coatings thickness d=0.5mm～8mm.
(2) make fine and close Y at existing crucible inwall 2O 3Coating can remedy the existing Y that is made by coarse granule grating powder 2O 3Crucible, Al 2O 3Crucible and ZrO 2The weakness that the crucible density is inadequate makes the crucible function admirable of the present invention that obtains, and is safe and reliable.
Description of drawings
Fig. 1 is that the present invention adopts rolling pulp moulding process fixture that Y is arranged 2O 3The flow chart of erosion resistant coatings crucible.
Fig. 2 is that the present invention has Y 2O 3The structure chart of erosion resistant coatings crucible.
Fig. 3 is the assembling schematic diagram that the present invention rolls slurry moulding and crucible base.
The specific embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
The present invention is a kind of Y of having 2O 3Erosion resistant coatings crucible, this crucible are to adopt the rolling pulp moulding process with Y 2O 3The preparation of anti-erosion slurry is on the inwall of crucible base 1.Referring to shown in Figure 2, the inwall of crucible base 1 is formed with the Y that a layer thickness is changed to d=0.5mm～8mm 2O 3Erosion resistant coatings 2, because what adopt in the present invention is the rolling pulp moulding of tilting to have certain angle (rolling pulp angle β) to carry out, so 11 coating layer thickness is thicker than the coating layer thickness of crucible base openend 12 in crucible base bottom, for the thickness of coating as long as the rotating speed when control rolling pulp time, rolling pulp can obtain required thickness.
In the present invention, Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, dispersant, binding agent and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, adds the multistage Y of 125.00g～409.09g in the deionized water of 100ml 2O 3The dispersant of raw meal, 1.25g～5.00g and the binding agent of 0.80g～3.20g; Described dispersant can be ammonium polyacrylate or gum arabic; Described binding agent can be polyvinyl alcohol (PVA) or carboxymethyl cellulose; In the present invention, the Y of different-grain diameter 2O 3Powder mixes and obtains multistage Y 2O 3Raw meal.This multistage Y 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder, particle diameter are the secondary Y of 25 μ m 2O 3Powder and particle diameter are three grades of Y of 45 μ m 2O 3Powder.The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 50g～80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g～30g and surplus is three grades of Y of 45 μ m 2O 3Powder.
In the present invention, crucible base 1 refers in type such as Y 2O 3Crucible, Al 2O 3Crucible, ZrO 2Crucible.The present invention be with the existing crucible that is made by coarse granule grating powder after cleaning namely as crucible base 1, adopt then the rolling pulp moulding process to roll on the Y that thickness is d=0.5mm～8mm at the inwall of crucible base 1 2O 3Erosion resistant coatings 2 forms and a kind ofly can be applicable to the Novel crucible that uses under 1600 ℃～2000 ℃ hot environments.
The present invention adopts rolling pulp Y processed 2O 3Erosion resistant coatings technology is to having cheaply Al now 2O 3Crucible, ZrO 2Crucible improves, and obtains to have the melting Novel crucible of high chemical stability, and this kind technology has been saved whole employing Y 2O 3Powder is made the cost of crucible.
The present invention adopts rolling pulp Y processed 2O 3Erosion resistant coatings technology is to existing Y 2O 3Crucible improves, and has remedied existing Y 2O 3The defective that the crucible density is inadequate.
Referring to shown in Figure 1, the present invention adopts the rolling pulp moulding process with Y 2O 3The preparation of anti-erosion slurry is on the inwall of crucible base 1, and it includes following steps:
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, dispersant, binding agent and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, adds the multistage Y of 125.00g～409.09g in the deionized water of 100ml 2O 3The dispersant of raw meal, 1.25g～5.00g and the binding agent of 0.80g～3.20g;
Described dispersant can be ammonium polyacrylate or gum arabic;
Described binding agent can be polyvinyl alcohol (PVA) or carboxymethyl cellulose;
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 50g～80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g～30g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
Adopt hairbrush that the moulding crucible is cleared up, obtain crucible base 1 after cleaning out; The moulding crucible refers to Y 2O 3Crucible, Al 2O 3Crucible or ZrO 2Crucible;
Moulding crucible in this step refers to Y 2O 3Crucible, Al 2O 3Crucible or ZrO 2Crucible, these crucibles can be inventor's making of controlling oneself in the present invention, also can buy from businessman.
The 3rd step: Y processed 2O 3Erosion resistant coatings
Step (A) is installed in second crucible base 1 that obtain of step on the anchor clamps 3 that roll the slurry former, regulates the angle of established angle α, α=30 °～45 °;
Step (B), the Y that the first step is obtained 2O 3The anti-erosion slurry joins in the crucible base 1;
Step (C) is regulated rotating shaft 5 and is rolled slurry along clockwise direction, rotating shaft rotating speed v=1～5r/min;
Step (D) is rolled slurry according to the coating layer thickness d=0.5mm～8mm that sets, and rolls to obtain first base substrate after slurry is finished;
Step (E) behind hothouse inner drying 20～50h of 25 ℃, makes second base substrate with first base substrate again behind high temperature drying 10～30h in 120 ℃ baking oven;
Step (F) is put into the sintering furnace high temperature sintering with second base substrate, and the firing time is 30～100h, and sintering temperature is 1500 ℃～1800 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
In the present invention, rolls on the processing platform 4 of starching former a rotating shaft 5 is installed at least, and the end of rotating shaft 5 is anchor clamps 3 that these anchor clamps 3 are used for placing crucible base 1.Can obtain being added on Y in the crucible base 1 by the established angle α angle of regulating rotating shaft 5 and processing platform 4 2O 3The slurry liquid level of anti-erosion slurry, the angle of this slurry liquid level and shaft centerline is designated as rolling pulp angle β, then has rolling pulp angle β to equal established angle α.Choose suitable rolling pulp angle β and can save Y 2O 3The consumption of anti-erosion slurry.
Embodiment 1At Al 2O 3Be coated with Y on the crucible 2O 3Erosion resistant coatings
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, ammonium polyacrylate, polyvinyl alcohol (PVA) and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, add the multistage Y of 214.00g in the deionized water of 100ml 2O 3The ammonium polyacrylate of raw meal, 1.50g and the polyvinyl alcohol of 2.00g (PVA);
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 65g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 30g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
The employing hairbrush will be from the Al of the prosperous Science and Technology Ltd. of Beijing Orient ancient cooking vessel production 2O 3Crucible is cleared up, and obtains crucible base after cleaning out;
The 3rd step: Y processed 2O 3Erosion resistant coatings
The crucible base 1 that second step was obtained is installed on the anchor clamps 3 that roll the slurry former, regulates established angle α=30 ° of angles, regulates rotating shaft rotating speed v=3r/min;
The Y that the first step is obtained 2O 3The anti-erosion slurry adds in the crucible base 1, and the rolling pulp time is 2min, obtains first base substrate of coating layer thickness d=1～3.5mm (crucible bottom is 3.5mm, and the crucible openend is 1mm, and thickness changes continuously);
First base substrate behind 25 ℃ hothouse inner drying 45h, is made second base substrate again behind the high temperature drying 24h in 120 ℃ baking oven;
Second base substrate is put into the sintering furnace high temperature sintering, and the firing time is 80h, and the highest sintering temperature is 1650 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
Has a Y to what embodiment 1 obtained 2O 3The erosion resistant coatings crucible adopts sem analysis, Y 2O 3The erosion resistant coatings homogeneous grain size, the little and even pore distribution of porosity.
Application Example 1 obtains has Y 2O 3The erosion resistant coatings crucible is at vacuum induction melting Ni-44Ti-6Al-3Nb (atomic percent) alloy 15Kg, and being evacuated to furnace pressure is 5 * 10 -3Pa begins to send electricity, and sending electrical power is 35KW, and after waiting liquid phase to occur, charging into argon gas to furnace pressure is 0.5 * 10 5Pa all moltenly is warming up to 1600 ℃ of melting 10min after clear, is cooled to 1500 ℃ and is poured into and makes the Ni-44Ti-6Al-3Nb alloy pig in the graphite casting mould.
Has a Y with what embodiment 1 obtained 2O 3Behind erosion resistant coatings crucible continuous smelting 30 stoves, the visual inspection crucible is not found crackle, illustrates that this crucible has good anti-melt erosion, thermal shock resistance.
Ni-44Ti-6Al-3Nb alloy pig to cast carries out electron probing analysis, does not find Y element, illustrates that the crucible that embodiment 1 makes has good anti-melt infiltration, corrosion resistance and chemical stability.
Embodiment 2At Y 2O 3Be coated with Y on the crucible 2O 3Erosion resistant coatings
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, gum arabic, polyvinyl alcohol (PVA) and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, add the multistage Y of 125.00g in the deionized water of 100ml 2O 3The gum arabic of raw meal, 1.25g and the polyvinyl alcohol of 3.20g (PVA);
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
The Y that adopts hairbrush that BJ University of Aeronautics ﹠ Astronautics is developed voluntarily 2O 3Crucible is cleared up, and obtains crucible base 1 after cleaning out; This Y 2O 3Crucible is the crucible of embodiment 1 component in the number of patent application 200810115856.8.
The 3rd step: Y processed 2O 3Erosion resistant coatings
The crucible base 1 that second step was obtained is installed on the anchor clamps 3 that roll the slurry former, regulates established angle α=45 degree, regulates rotating shaft rotating speed v=1r/min;
The Y that the first step is obtained 2O 3The anti-erosion slurry adds in the crucible base 1, and the rolling pulp time is 2min, makes first base substrate of coating layer thickness d=0.5～3mm (crucible bottom is 3mm, and the crucible openend is 0.5mm, and thickness changes continuously);
First base substrate behind 25 ℃ hothouse inner drying 24h, is made second base substrate again behind the high temperature drying 10h in 120 ℃ baking oven;
Second base substrate is put into the sintering furnace high temperature sintering, and the firing time is 30h, and the highest sintering temperature is 1750 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
Has a Y to what embodiment 2 obtained 2O 3The erosion resistant coatings crucible adopts sem analysis, Y 2O 3The erosion resistant coatings homogeneous grain size, the little and even pore distribution of porosity.
Application Example 2 obtains has Y 2O 3The erosion resistant coatings crucible is at vacuum induction melting Nb-14Si-22Ti-2Cr-2Al-8Hf (atomic percent) alloy 10Kg, and being evacuated to furnace pressure is 5 * 10 -3Pa begins to send electricity, and sending electrical power is 25KW, and after waiting liquid phase to occur, charging into argon gas to furnace pressure is 0.5 * 10 5Pa all moltenly is warming up to 2000 ℃ of melting 10min after clear, is cooled to 1900 ℃ and is poured into and makes the Nb-14Si-22Ti-2Cr-2Al-8Hf alloy pig in the graphite casting mould.
Has a Y with what embodiment 2 obtained 2O 3Behind erosion resistant coatings crucible continuous smelting 30 stoves, the visual inspection crucible is not found crackle, illustrates that this crucible has good anti-melt erosion, thermal shock resistance.
Nb-14Si-22Ti-2Cr-2Al-8Hf alloy pig to cast carries out electron probing analysis, does not find Y element, illustrates that the crucible that embodiment 2 makes has good anti-melt infiltration, corrosion resistance and chemical stability.
Embodiment 3At ZrO 2Be coated with Y on the crucible 2O 3Erosion resistant coatings
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, gum arabic, carboxymethyl cellulose and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, add the multistage Y of 409.09g in the deionized water of 100ml 2O 3The gum arabic of raw meal, 5.00g and the carboxymethyl cellulose of 0.80g;
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 50g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 15g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
The employing hairbrush will be from the ZrO of the prosperous Science and Technology Ltd. of Beijing Orient ancient cooking vessel production 2Crucible is cleared up, and obtains crucible base 1 after cleaning out;
The 3rd step: Y processed 2O 3Erosion resistant coatings
The crucible base 1 that second step was obtained is installed on the anchor clamps 3 that roll the slurry former, regulates established angle α=35 ° of angles, regulates rotating shaft rotating speed v=5r/min;
The Y that the first step is obtained 2O 3The anti-erosion slurry adds in the crucible base 1, and the rolling pulp time is 4min, makes first base substrate of coating layer thickness d=5～8mm (crucible bottom is 8mm, and the crucible openend is 5mm, and thickness changes continuously);
First base substrate behind 25 ℃ hothouse inner drying 36h, is made second base substrate again behind the high temperature drying 30h in 120 ℃ baking oven;
Second base substrate is put into the sintering furnace high temperature sintering, and the firing time is 100h, and the highest sintering temperature is 1800 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
Has a Y to what embodiment 3 obtained 2O 3The erosion resistant coatings crucible adopts sem analysis, Y 2O 3The erosion resistant coatings homogeneous grain size, the little and even pore distribution of porosity.
Application Example 3 obtains has Y 2O 3The erosion resistant coatings crucible is at vacuum induction melting Tb 0.3Dy 0.7Fe 2(Terfenol-D) alloy 12Kg, being evacuated to furnace pressure is 5 * 10 -3Pa begins to send electricity, and sending electrical power is 30KW, and after waiting liquid phase to occur, charging into argon gas to furnace pressure is 0.5 * 10 5Pa all moltenly is warming up to 1700 ℃ of melting 5min after clear, is cooled to 1550 ℃ and is poured into and makes Tb in the graphite casting mould 0.3Dy 0.7Fe 2Alloy pig.
Has a Y with what embodiment 3 obtained 2O 3Behind erosion resistant coatings crucible continuous smelting 30 stoves, the visual inspection crucible is not found crackle, illustrates that this crucible has good anti-melt erosion, thermal shock resistance.
Tb to cast 0.3Dy 0.7Fe 2Alloy pig carries out electron probing analysis, does not find Y element, illustrates that the crucible that embodiment 3 makes has good anti-melt infiltration, corrosion resistance and chemical stability.

Claims (6)

1, a kind of have a Y 2O 3The erosion resistant coatings crucible is characterized in that: be in the preparation of the inwall of crucible base (1) Y to be arranged 2O 3Erosion resistant coatings.
2, according to claim 1 have a Y 2O 3The erosion resistant coatings crucible is characterized in that: this has Y 2O 3The erosion resistant coatings crucible is by crucible base (1) and Y 2O 3Erosion resistant coatings (2) consists of, and Y 2O 3Erosion resistant coatings (2) preparation is on the inwall of crucible base (1);
Y 2O 3The thickness of erosion resistant coatings (2) from thick to thin order be crucible base bottom (11) to crucible base openend (12), thickness range is d=0.5mm～8mm;
Described Y 2O 3The raw material of erosion resistant coatings (2) is multistage Y 2O 3Powder, the multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the powder 2O 3Powder 50g～80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g～30g and surplus is three grades of Y of 45 μ m 2O 3Powder.
3, according to claim 1 and 2 have a Y 2O 3The erosion resistant coatings crucible is characterized in that: crucible base (1) refers in type such as Y 2O 3Crucible, Al 2O 3Crucible or ZrO 2Crucible.
4, according to claim 1 and 2 have a Y 2O 3The erosion resistant coatings crucible is characterized in that: this crucible can be applicable under 1600 ℃～2000 ℃ hot environments and use.
5, a kind of employing rolling pulp moulding process system is as claimed in claim 1 has a Y 2O 3The method of erosion resistant coatings crucible is characterized in that the following step is arranged:
The first step: Y processed 2O 3The anti-erosion slurry
Y 2O 3The anti-erosion slurry is by multistage Y 2O 3Raw meal, dispersant, binding agent and deionized water form, and each component obtains the slurry of good fluidity after sufficiently mixing, wherein, adds the multistage Y of 125.00g～409.09g in the deionized water of 100ml 2O 3The dispersant of raw meal, 1.25g～5.00g and the binding agent of 0.80g～3.20g;
Described dispersant is ammonium polyacrylate or gum arabic;
Described binding agent is polyvinyl alcohol or carboxymethyl cellulose;
The multistage Y of described 100g 2O 3Include the one-level Y that particle diameter is 5 μ m in the raw meal 2O 3Powder 50g～80g, particle diameter are the secondary Y of 25 μ m 2O 3The particle diameter of powder 5g～30g and surplus is three grades of Y of 45 μ m 2O 3Powder;
Second step: choose crucible base
Adopt hairbrush that the moulding crucible is cleared up, obtain crucible base (1) after cleaning out;
The 3rd step: Y processed 2O 3Erosion resistant coatings
Step (A) is installed in second crucible base (1) that obtain of step on the anchor clamps (3) that roll the slurry former, regulates the angle of established angle α, α=30 °～45 °;
Step (B), the Y that the first step is obtained 2O 3The anti-erosion slurry joins in the crucible base (1);
Step (C) is regulated rotating shaft (5) and is rolled slurry along clockwise direction, rotating shaft rotating speed v=1～5r/min;
Step (D) is rolled slurry according to the coating layer thickness d=0.5mm～8mm that sets, and rolls to obtain first base substrate after slurry is finished;
Step (E) behind hothouse inner drying 20～50h of 25 ℃, makes second base substrate with first base substrate again behind high temperature drying 10～30h in 120 ℃ baking oven;
Step (F) is put into the sintering furnace high temperature sintering with second base substrate, and the firing time is 30～100h, and sintering temperature is 1500 ℃～1800 ℃, makes to have Y 2O 3The crucible of erosion resistant coatings.
6, employing rolling pulp moulding process fixture according to claim 4 has Y 2O 3The method of erosion resistant coatings crucible is characterized in that: rolling pulp angle β equates with the angle of established angle α.
CN2009100799738A 2009-03-16 2009-03-16 Method for producing Y2O3 etching resistant coating using slip casting moulding technique Expired - Fee Related CN101532776B (en)

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CN103827048A (en) * 2011-08-05 2014-05-28 科卢斯博知识产权有限公司 Crucible materials
CN104744055A (en) * 2013-12-30 2015-07-01 比亚迪股份有限公司 Preparation method of sol for preparing coating, coating and preparation method of coating
CN113165083A (en) * 2018-11-29 2021-07-23 京瓷株式会社 Coated cutting tool and cutting tool provided with same
CN113620694A (en) * 2021-09-03 2021-11-09 湖南昕昱科技有限公司 Crucible for smelting alloy containing active elements and preparation method thereof
CN115368779A (en) * 2022-08-23 2022-11-22 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) Coating slurry, coating preparation method and application thereof

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CN103827048A (en) * 2011-08-05 2014-05-28 科卢斯博知识产权有限公司 Crucible materials
CN103827048B (en) * 2011-08-05 2017-05-10 科卢斯博知识产权有限公司 Crucible materials
CN104744055A (en) * 2013-12-30 2015-07-01 比亚迪股份有限公司 Preparation method of sol for preparing coating, coating and preparation method of coating
CN103771886A (en) * 2014-01-24 2014-05-07 南京理工大学 Method for preparing yttrium oxide coating of corundum crucible
CN113165083A (en) * 2018-11-29 2021-07-23 京瓷株式会社 Coated cutting tool and cutting tool provided with same
CN113165083B (en) * 2018-11-29 2024-01-26 京瓷株式会社 Coated cutting tool and cutting tool provided with same
CN113620694A (en) * 2021-09-03 2021-11-09 湖南昕昱科技有限公司 Crucible for smelting alloy containing active elements and preparation method thereof
CN115368779A (en) * 2022-08-23 2022-11-22 北京理工大学深圳汽车研究院(电动车辆国家工程实验室深圳研究院) Coating slurry, coating preparation method and application thereof

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