CN109467416A - A kind of corundum with low porosity and preparation method thereof - Google Patents
A kind of corundum with low porosity and preparation method thereof Download PDFInfo
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Abstract
本发明公开了一种低气孔率刚玉及其制备方法，低气孔率刚玉按原料总重量的百分含量计，由如下各原料组成：氧化铝90％‑98％、氧化钇1.5％‑5％、氧化镧0.5％‑5％。制备方法为按上述重量百分比称量各原料，将氧化铝、氧化钇和氧化镧混合均匀，然后转入电熔炉进行电熔；待氧化铝、氧化钇和氧化镧完全熔解；继续保持熔体温度并进行精炼，精炼完成后自然冷却结晶获得球状结晶体，即所述低气孔率刚玉。本发明的低气孔率刚玉中含α‑氧化铝相为95％以上，低气孔率刚玉的气孔率可达1％以下；故低气孔率刚玉具有气孔率低、耐热性好、韧性好、稳定性强的优点。The invention discloses a low-porosity corundum and a preparation method thereof. The low-porosity corundum is composed of the following raw materials according to the percentage content of the total weight of the raw materials: aluminum oxide 90%-98%, yttrium oxide 1.5%-5% , Lanthanum oxide 0.5%-5%. The preparation method is to weigh each raw material according to the above-mentioned weight percentage, mix the alumina, yttrium oxide and lanthanum oxide evenly, and then transfer to an electric melting furnace for electric melting; wait for the alumina, yttrium oxide and lanthanum oxide to be completely melted; continue to maintain the melt temperature And refining, after refining is completed, natural cooling and crystallization obtain spherical crystals, that is, the low porosity corundum. The α-alumina phase contained in the low porosity corundum of the present invention is more than 95%, and the porosity of the low porosity corundum can reach below 1%; therefore, the low porosity corundum has the advantages of low porosity, good heat resistance, good toughness, The advantage of strong stability.
Description
Technical field
The present invention relates to technical field of refractory materials more particularly to a kind of low-porosity corundum and preparation method thereof.
Background technique
The resistance to acid and alkali of corundum is strong, good stability of the dimension, forming, and crystal phase is stablized, and hardness is high, is widely used in various modelings
The strengthening and toughening of the products such as material, rubber, ceramics, refractory material；But currently, the porosity of existing general corundum is up to 30%-
45%, crystal be in tip-like structure or plate structure, thus plant corundum made of product, heat resistance, intensity, toughness and
Structural stability certainly will be affected.The porosity of corundum is reduced as a result, and changes the crystal structure of corundum to improvement corundum
Characteristic has actual significance.
Summary of the invention
Therefore, in view of the above problems, it is an object of the invention to overcome above-mentioned the deficiencies in the prior art, providing one kind has
The low-porosity corundum that the porosity is low, heat-resist, good toughness, stability are high；In addition, the present invention also provides a kind of low-porosities
The preparation method of corundum.
The technical scheme to solve the above technical problems is that a kind of low-porosity corundum, by raw material gross weight
Percentage composition meter is made of: aluminium oxide 90%-98%, yttrium oxide 1.5%-5%, lanthana 0.5%-5% following each raw material.
The beneficial effects of the present invention are: aluminium oxide, can at 1500 DEG C or more mainly with the presence of gama-alumina crystal form under room temperature
It is completely converted into Alpha-alumina.Therefore, at a temperature of 2300 DEG C or more of electric smelting, gama-alumina crystal is completely transformed into α-oxygen
Change aluminium.In addition, the yttrium oxide in raw material of the present invention, generates yttrium aluminate with oxidation reactive aluminum in electric melting process, yttrium aluminate can promote
Make alpha-alumina crystals spherical structure during from gama-alumina crystal form to Alpha-alumina crystal transfer, avoids alpha-oxidation
Aluminium crystal is to the exhibition of binding up one's hair of tip-like crystal structure or platelike crystal.After electric smelting and refining, natural cooling crystallization obtains spherical
Crystalline solid, the chondritic of crystal effectively reduce the spacing between each crystal grain of crystals.In addition, the lanthana in raw material has
There is compact crystallizationization effect, can further improve the structural compactness of product.Furthermore containing being mutually deformed into low-porosity corundum
Alpha-alumina is mutually up to 95% or more.The porosity of the corundum formed as a result, is low, and the porosity is up to 1% or less.The extremely low porosity
It is greatly improved the heat resistance, intensity, toughness and structural stability of corundum with high Alpha-alumina phase content, so that being carried out with it
The product of the manufacturing has good quality.
In addition, based on the above technical solution, the present invention can also be improved as follows, can also have following additional
Technical characteristic.
Further, the low-porosity corundum of the present embodiment, based on the percentage composition of raw material gross weight, by following each raw material group
At: aluminium oxide 95%, yttrium oxide 3.5%, lanthana 1.5%.The porosity of the low-porosity corundum of formation is low, and the porosity is reachable
1% or less.
Further, the purity of the aluminium oxide is 95% or more；The purity is high of aluminium oxide, it is few containing objectionable impurities, it can reduce
Destruction when impurity is transformed into gas evolution in electric melting process to corundum structure, avoids the increase of the corundum porosity, can also subtract
Few influence of the impurity to corundum performance.
In addition, a kind of preparation method of low-porosity corundum provided by the invention, includes the following steps:
(1) based on the percentage composition of raw material gross weight, the following raw material is weighed: aluminium oxide 90%-98%, yttrium oxide 1.5%-
5%, lanthana 0.5%-5%；
(2) then aluminium oxide, yttrium oxide and lanthana are uniformly mixed, are transferred in electric smelter and carry out electric smelting, aluminium to be oxidized,
Yttrium oxide and lanthana melt；
(3) electric smelting melts completely to raw material；Continue to keep melt temperature and be refined, crystallisation by cooling obtains after the completion of refining
Obtain spheroidal cementite body, i.e., the described low-porosity corundum.
The preparation method of low-porosity corundum through the invention, at a temperature of 2300 DEG C or more of electric smelting, gama-alumina
Crystal is completely transformed into Alpha-alumina.In addition, the yttrium oxide in the present embodiment raw material, raw with oxidation reactive aluminum in electric melting process
At yttrium aluminate, yttrium aluminate can promote alpha-alumina crystals ball during from gama-alumina crystal form to Alpha-alumina crystal transfer
Shape structuring avoids alpha-alumina crystal to the exhibition of binding up one's hair of tip-like crystal structure or platelike crystal.After electric smelting and refining, from
Right crystallisation by cooling obtains spheroidal cementite body, and the chondritic of crystal effectively reduces the spacing between each crystal grain of crystals.Separately
Outside, the lanthana in raw material has compact crystallizationization effect, can further improve the structural compactness of product.Furthermore low stomata
Containing the Alpha-alumina being mutually deformed into mutually up to 95% or more in rate corundum.The porosity of the corundum formed as a result, is low, and the porosity is reachable
1% or less.The extremely low porosity and high Alpha-alumina phase content are greatly improved the heat resistance, intensity, toughness and knot of corundum
Structure stability, so that there is good quality with the product that it is manufactured.
Further, the preparation method of low-porosity corundum of the invention the step of in (2), electric smelting temperature is 2300 DEG C-
2700℃；Temperature is high, and gama-alumina crystal form is made sufficiently to be changed into Alpha-alumina crystal form.
Further, the preparation method of low-porosity corundum of the invention the step of in (3), the type of cooling is that nature is cold
But；It prevents from destroying crystallographic tissue due to the too fast biggish shrinkage stress of generation of cooling.
Further, the stomata of the low-porosity corundum made from the preparation method of low-porosity corundum through the invention
Rate is 1% or less；The porosity of low-porosity corundum is low, with high density, high intensity, obdurability excellent performance.
Further, α-oxygen in the low-porosity corundum made from the preparation method of low-porosity corundum through the invention
Change aluminium mutually up to 95% or more；The Alpha-alumina phase content of low-porosity corundum is high, and heat resistance and anti-phase change structure stability are good.
Further, the aluminium oxide, yttrium oxide and lanthana are powder；Aluminium oxide, yttrium oxide and lanthana are processed
At powder, is conducive to shorten the electric smelting time, reduces the chemical reaction temperature between oxide, increase the contact between each reactant
Area is accelerated reaction and is carried out, reduces power consumption.
Further, the partial size of the aluminium oxide, yttrium oxide and lanthana is 30-70 μm；Aluminium oxide, yttrium oxide and oxidation
The moderate in grain size of lanthanum, difficulty of processing is low, is conducive to processing and obtains.
Specific embodiment
Principles and features of the present invention are described below in conjunction with specific embodiment, example is served only for explaining this hair
Bright, still, the present invention can also be implemented using other different from other way described herein, therefore, protection of the invention
Range is not limited by the specific embodiments disclosed below.
Embodiment 1:
The low-porosity corundum of the present embodiment is made of: oxidation based on the percentage composition of raw material gross weight following each raw material
Aluminium 90%, yttrium oxide 5%, lanthana 5%.
Specifically, the aluminium oxide of the present embodiment is preferably the aluminium oxide of purity is high, to reduce Impurities In Alumina element pair
The influence of product.For example, the amount of impure elements of Na is larger in aluminium oxide, at high temperature, i.e., in gama-alumina crystal form to α-oxygen
During changing aluminium transformation, sodium is reacted with another impurity element boron in aluminium oxide generates gaseous sodium tetraborate, gaseous state object
Matter is constantly escaped between aluminium oxide lattice to bath surface under the promotion of chemical potential, to destroy the crystal structure of aluminium oxide.
In addition, for the oxidation aluminum product of different demands, the requirement to aluminium oxide purity is also different；The purity shadow of aluminium oxide
Ring physics, mechanical performance and its service life that molding product is made by it.Specifically, in the present embodiment " aluminium oxide is pure
Degree is high " refer to that the impurity that is inevitable or being difficult to remove contained in aluminium oxide is few, the essence of " corundum " in the present embodiment
For the product based on alpha alumina-based crystal formed by aluminium oxide, lanthana, yttrium oxide through pyroreaction and crystallisation by cooling.
It, can also be with specifically, aluminium oxide, yttrium oxide, the lanthana in the raw material of the present embodiment can be blocky or particle
It is by processing powder obtained.
Specifically, having yttrium oxide in the raw material of the present embodiment, under electric smelting, for temperature at 2300 DEG C or more, gama-alumina is brilliant
Body is completely transformed into Alpha-alumina.In addition, the yttrium oxide in the present embodiment raw material, generates in electric melting process with oxidation reactive aluminum
Yttrium aluminate, yttrium aluminate can promote alpha-alumina crystals spherical during from gama-alumina crystal form to Alpha-alumina crystal transfer
Structuring avoids alpha-alumina crystal to the exhibition of binding up one's hair of tip-like crystal structure or platelike crystal.It is natural after electric smelting and refining
Crystallisation by cooling obtains spheroidal cementite body, and the chondritic of crystal effectively reduces the spacing between each crystal grain of crystals.In addition,
Lanthana in raw material has compact crystallizationization effect, can further improve the structural compactness of product.Furthermore low-porosity is rigid
The Alpha-alumina that Yu Zhonghan phase is deformed into is mutually up to 95% or more.The porosity of the corundum formed as a result, is low, and the porosity is up to 1%
Below.The heat resistance, intensity, toughness and structure that the extremely low porosity and high Alpha-alumina phase content are greatly improved corundum are steady
It is qualitative, so that there is good quality with the product that it is manufactured.
In one embodiment of the invention, the low-porosity corundum of the present embodiment, by the percentage composition of raw material gross weight
Meter is made of: aluminium oxide 90%, yttrium oxide 5%, lanthana 5% following each raw material.The low-porosity corundum that the present embodiment is formed
The porosity it is low, the porosity is up to 0.7%.
In one embodiment of the invention, the purity of the aluminium oxide is 95% or more；Specifically, the purity of aluminium oxide
Height, it is few containing objectionable impurities, destruction when impurity in electric melting process is transformed into gas evolution to corundum structure can be reduced, corundum is avoided
The increase of the porosity can also reduce the purity is high of influence aluminium oxide of the impurity to corundum performance, contain inevitably miscellaneous
Matter is few, reduces and destroys the structure of corundum since impurity forms gas overflowing in electric melting process, increases the porosity of corundum；
And it is possible to reduce influence of the impurity to corundum.And it carries out making molding product using the aluminium oxide that purity is 95% or more
Heat-resist, good toughness, stability it is high；The aluminium oxide for the use of purity being 95% or more, heat resistance, toughness, the stabilization of product
Property is more preferable.In addition, the lanthana and yttrium oxide raw material of the embodiment of the present invention are high-purity original of the impurity quality less than 0.5%
Material.
In addition, including the following steps: the present embodiment provides a kind of preparation method of low-porosity corundum
(1) based on the percentage composition of raw material gross weight, the following raw material is weighed: aluminium oxide 90%, yttrium oxide 5%, lanthana
5%；
(2) then aluminium oxide, yttrium oxide and lanthana are added in electric smelter and are mixed evenly, then carry out electricity
Molten, aluminium, yttrium oxide and lanthana to be oxidized melt；
(3) electric smelting causes raw material to melt completely；Continue to keep melt temperature and be refined, crystallisation by cooling shape after the completion of refining
Glomeration crystalline solid can obtain the low-porosity corundum.
It cleans specifically, " refining " of the present embodiment refers to the melt after melting, refining techniques is in the art
It is usually used in cleaning to melt, refining time can be 30-60min.Specifically, electric smelting is carried out in electric smelter, need to continue
The time of electric smelting is also related with the primary amount of electric smelting raw material that carries out, can be according to the needs being added when specifically carrying out electric smelting
The electric smelting time is appropriately configured in the raw material for carrying out electric smelting.The present embodiment in step (3), electric smelting temperature be 2500 DEG C, make
Gama-alumina crystal is sufficiently changed into Alpha-alumina.
Specifically, the cooling technique of the present embodiment is natural cooling；Prevent due to cooling it is too fast generate it is biggish contraction and
To destruction crystallographic tissue.
Specifically, the porosity of the low-porosity corundum obtained of the present embodiment is 0.7%, density 4.05g/
cm3；The quality of low-porosity corundum is good, and density is high.
The preparation method of low-porosity corundum through this embodiment, under electric smelting, temperature is at 2300 DEG C or more, γ-oxygen
Change aluminium crystal and is completely converted into Alpha-alumina；Yttrium oxide in raw material of the invention, it is raw with oxidation reactive aluminum in electric melting process
At yttrium aluminate, yttrium aluminate can promote alpha-alumina crystals ball during from gama-alumina crystal form to Alpha-alumina crystal transfer
Shape structuring avoids alpha-alumina crystal to the exhibition of binding up one's hair of tip-like crystal structure or platelike crystal.After electric smelting and refining, from
Right crystallisation by cooling obtains spheroidal cementite body, and the chondritic of crystal effectively reduces the spacing between each crystal grain of crystals.Separately
Outside, the lanthana in raw material has compact crystallizationization effect, can further improve the structural compactness of product.Furthermore low stomata
Containing the Alpha-alumina being mutually deformed into mutually up to 95% or more in rate corundum.The porosity of the corundum formed as a result, is low, and the porosity is reachable
0.7%, density 4.05g/cm3；Corundum has preferable heat resistance, toughness and stability, so that carrying out production formation with it
Product has good quality.
In one embodiment of the invention, the aluminium oxide, yttrium oxide, lanthana are powder；Aluminium oxide, oxygen
The partial size for changing yttrium and lanthana is 30-70 μm.Specifically, the partial size of aluminium oxide is smaller, more has and carry out quick electric smelting using it；
But the smaller then difficulty of processing of partial size is bigger, and processing cost is high.The partial size of the aluminium oxide of the present embodiment is 30-70 μm, is easily worked
It obtains.
Embodiment 2:
The present embodiment 2 is similar to Example 1, and unlike the first embodiment, the low-porosity corundum of the present embodiment is pressed
The percentage composition meter of raw material gross weight is made of: aluminium oxide 95%, yttrium oxide 3.5%, lanthana 1.5% following each raw material.
The present embodiment is by upper component proportionally feeding, and the preparation method is the same as that of Example 1 for the present embodiment；It is obtained described low
The porosity of porosity corundum is 0.6%, and the density of the low-porosity corundum obtained is 4.10g/cm3。
Embodiment 3:
The present embodiment 3 is similar to Example 1, and unlike the first embodiment, the low-porosity corundum of the present embodiment is pressed
The percentage composition meter of raw material gross weight is made of: aluminium oxide 98%, yttrium oxide 1.5%, lanthana 0.5% following each raw material.
The present embodiment is by upper component proportionally feeding, and the preparation method is the same as that of Example 1 for the present embodiment；It is obtained described low
The porosity of porosity corundum is 0.9%, and the density of the low-porosity corundum obtained is 4.0g/cm3。
It is obtained by many experiments, to the functional of low-porosity corundum obtained by the present embodiment 1-3；The corundum of formation
The porosity is 1% hereinafter, density is 4.0g/cm3More than；To improve the heat resistance, toughness and stability of corundum, so that using it
The product for carrying out production formation has good quality.
These are only the preferred embodiment of the present invention, is not intended to restrict the invention, in the bound value of raw material
And interval value can realize the present invention, just be not listed one by one herein, for those skilled in the art, the present invention can be with
There are various modifications and variations.All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on,
It should be included within protection scope of the present invention.
Claims (10)
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