CN109020519A - A kind of complex phase ceramic roller stick and preparation method thereof - Google Patents
A kind of complex phase ceramic roller stick and preparation method thereof Download PDFInfo
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- CN109020519A CN109020519A CN201810820944.1A CN201810820944A CN109020519A CN 109020519 A CN109020519 A CN 109020519A CN 201810820944 A CN201810820944 A CN 201810820944A CN 109020519 A CN109020519 A CN 109020519A
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of complex phase ceramic roller sticks, its raw material includes aggregate and binder, and aggregate includes 25~35 parts of corundum material, 25~35 parts of clay, 18~24 parts of alumina powder, 3~6 parts of yttrium oxide, 4~11 parts of titanium dioxide, 3~10 parts of zirconium silicate, 3~6 parts of finely-powdered minerals；The corundum material includes 7~11 parts of the corundum that granularity is 60~100 mesh, 14~17 parts of the corundum that granularity is 100~200 mesh, 4~7 parts of corundum of 250 mesh accounting≤10% of granularity.Correspondingly, the invention also discloses the preparation methods of the complex phase ceramic roller stick.Complex phase ceramic roller stick of the invention have the characteristics that refractoriness is high, Properties of High Temperature Creep is good, low thermal coefficient of expansion, using temperature height, good thermal shock stability, long service life, solve the problems, such as roller stick in roller kilns due to bending deformation caused by when temperature gradient is larger.
Description
Technical field
The present invention relates to ceramic rod technical field, in particular to a kind of complex phase ceramic roller stick and preparation method thereof.
Background technique
Ceramic rod is a kind of refractory kiln, and the products such as support and transmission Ceramic Tiles are played in roller-way calcining kiln and dry kiln
Effect, be the core component of roller kilns, it has important shadow to the energy conservation of roller kilns, product firing period and automatic operation
It rings, is used widely in fields such as architectural pottery, domestic ceramics, electronic ceramics, magnetic material, glass heat treatments.
Currently, ceramic rod material used in Production of Ceramics enterprise roller kilns is mainly the ceramics of corundum-mullite material
Roller stick, existing major defect are that thermal expansion coefficient is higher, when in use, since there are clinkering zone higher temperatures areas for roller way kiln
Domain and chilling band temperature difference large area, ceramic rod are easy to produce bending deformation in use, to influence normal production.
Aluminium titanates is a kind of ceramic material haveing excellent performance, it have close to zero thermal expansion coefficient, low thermal conductivity,
High-melting-point, anti-thermal shock and the characteristics such as thermal shock resistance is excellent, can use under the conditions of violent rapid heat cycle, and to aluminium
Liquid, molten steel, copper liquid, copper ashes, steel slag resist anti-erosion and alkali corrosion resistance with excellent, due to the heat-resistant knocking stability of material
Related with thermal expansion coefficient and thermal conductivity, material of aluminum titanate is a kind of replacer of heat-resistant knocking stability energy elite clone.Simultaneously
Characteristic, reasonable formula and the technical process having using material itself prepare material, can give full play to the spy of material itself
Point prepares satisfactory high-performance ceramic roller stick.
Aluminium titanates also encounters two problems in a particular application, first is that it easily divides within the temperature range of 800~1200 DEG C
Solution is rutile and corundum, causes material internal stress to concentrate, to lose its low thermal expansion characteristics, cannot not only improve material
Thermal stability and also greatly shorten the materials'use service life；Second is that its each axial thermal expansion coefficient difference is very big, when cooling
Material internal makes the reduction of its mechanical strength since thermal stress easily forms a large amount of micro-cracks, and material is difficult to dense sintering.
In recent years, aluminium titanates decomposes in order to prevent, and material worker has done many work, introduced in material of aluminum titanate all
Such as mullite, corundum, SiC, Si3N4Its intensity is improved Deng the crystal and ceramic fibre or whisker with high intensity and inhibits it
It decomposes.Since the chemical stability of mullite is good, high temperature resistant, thermal expansion coefficient is greater than aluminium titanates, therefore in above-mentioned different materials
Number mullite is most widely used.Mullite mutually forms continuous structure, and aluminium titanates is distributed wherein, and aluminium titanates crystal is by mullite
It wraps up and is compressed, it is suppressed that the decomposition of aluminium titanates makes aluminium titanates remain excellent low expansion, by adding other materials
The ceramic particle of matter can play " nail is solid " effect to the crack tip in extension, it is made to be difficult to extend or can only detour expansion forward
It opens up or is biased to crackle, or make crackle branching, or be bent crackle, to increase the energy to failure of material, prevent lead crack from running through
Entire ceramic structure, while grain growth can be inhibited in high―temperature nuclei, significantly improve the strength of materials.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of intensity and heat-resistant knocking stability be superior to commonly aoxidize
Complex phase ceramic roller stick of aluminium roller stick and preparation method thereof overcomes and causes ceramic rod bending deformation since the temperature difference is big or high temperature
Disadvantage.
In order to solve the above-mentioned technical problems, the present invention provides a kind of complex phase ceramic roller stick, raw material includes aggregate and glues
Agent is tied, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals；
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh of granularity
4~7 parts of the corundum of accounting≤10%.
As an improvement of the above scheme, the granularity of the alumina powder is 1~5 μm；The granularity of the finely-powdered minerals is
10~30 μm.
As an improvement of the above scheme, the amount ratio of the alumina powder and yttrium oxide is 4-5:1-2.
As an improvement of the above scheme, alumina content >=99% in the corundum material；
The titanium dioxide is Rutile structure；
The finely-powdered minerals are kyanite, andalusite or sillimanite.
As an improvement of the above scheme, the binder is one in cellulose ether, resin or calcium lignosulfonate solution
Kind is a variety of.
As an improvement of the above scheme, the cellulose ether is carboxymethyl cellulose, the carboxymethyl cellulose
Na2O content < 10%, additional amount are 1wt%~3wt%；
The resin is thermosetting phenolic resin, and additional amount is 0.5wt%~1.5wt%；
The mass ratio of calcium lignosulfonate and water is 3-5:5-7 in the calcium lignosulfonate solution, and additional amount is
0.5wt%~1.5wt%.
Correspondingly, the present invention also provides a kind of preparation methods of complex phase ceramic roller stick, comprising:
(1) it is formulated ingredient by aggregate, through ball milling, spraying, homogenizing processing, obtains mixture；
(2) mixture is dry-mixed with binder, add water wet mixing；
(3) dry blended and wet mixing mixture is granulated, and the extrusion molding on descaling extrusion press, obtains blank；
(4) blank is dried, the blank moisture after drying is controlled 1.0~1.5%；
(5) blank after drying is subjected to cold isostatic compaction；
(6) blank after cold isostatic compaction is lifted to sintering in kiln, obtains roller stick finished product；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh of granularity
4~7 parts of the corundum of accounting≤10%；
The binder is cellulose ether.
As an improvement of the above scheme, the mixed mechanism in step (2) are as follows: by mixture and 1wt%~3wt% binder
Dry-mixed 4~6min, then plus the mixed 10~13min of 14wt%~16wt% water-wet；
In step (4), drying temperature is 80~100 DEG C, and drying time is 35~45h；
In step (5), the pressure of cold isostatic compaction is 150~250MPa；
In step (6), sintering temperature is 1640~1650 DEG C, and sintering time is 28~33h.
In addition, the present invention also provides the preparation methods of another complex phase ceramic roller stick, comprising:
(1) it is formulated ingredient by aggregate, is handled through ball milling, filters pressing, obtains mixture；
(2) mixture is mixed with binder, carries out vacuum pugging and prepares pug, vacuum extruding blank；
(3) blank is dried, blank moisture≤0.6% after drying；
(4) dry blank is lifted to sintering in kiln；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh of granularity
4~7 parts of the corundum of accounting≤10%；
The binder is one of resin or calcium lignosulfonate solution or a variety of.
As an improvement of the above scheme, the mixed mechanism in step (2) are as follows: by mixture with 0.5wt%~1.5wt%'s
Thermosetting phenolic resin or calcium lignosulfonate solution's mixing；
In step (3), drying temperature is 80~120 DEG C, and drying time is 13~18h；
In step (4), sintering temperature is 1650~1665 DEG C, and sintering time is 31~35h.
The invention has the following beneficial effects:
The present invention provides a kind of complex phase ceramic roller sticks, utilize the excellent properties of aluminium titanates, the corundum pair of variable grain degree
Crack tip in extension plays " nail is solid " effect, improves the intensity of material；Primary mullite that the physical and chemical reaction of clay generates and
The mullite phase for the secondary mullite composition whole system that the silica decomposited is generated with oxidation reactive aluminum, while utilizing and adding
The titanium dioxide added synthesizes the aluminium titanates of low bulk with alumina powder, generates one using the coefficient of thermal expansion mismatch between three
A residual internal stress field can resist extraneous partial pressure, improve the intensity of material；Utilize the aluminium oxide and yttrium oxide of addition
It can guarantee the agglutinating property and stability of aluminium titanates in the liquid phase that hot conditions generate, while a certain amount of mullite is in the material
The decomposition for inhibiting aluminium titanates, guarantees the stability of material.
Therefore, the present invention is mentioned using corundum and mullite and the thermal mismatching with aluminium titanates, the residual internal stress field of generation
The intensity and thermal shock resistance of high material react generation three-phase matched coefficients of thermal expansion by solid-phase sintering and crystal development are preferable
Microstructure, to prepare excellent corundum-mullite-aluminium titanates complex phase ceramic roller stick, performance is as follows:
Resistance to thermal shocks (1350 DEG C~room temperature) >=6 times is not split, room temperature bending strength >=55MPa, high temperature bend strength
(1350 DEG C) >=40MPa, thermal expansion coefficient (1000 DEG C)≤5.5 × 10-6/℃.The roller stick has refractoriness height, high temperature creep-resisting
Performance is good, low thermal coefficient of expansion, using temperature height, good thermal shock stability, long service life the features such as, efficiently solve roller stick and exist
Due to that the problem of bending deformation, can be widely applied in each region of roller kilns caused by when temperature gradient is larger in roller kilns.
Detailed description of the invention
Fig. 1 is a kind of one embodiment flow chart of manufacturing method of complex phase ceramic roller stick of the present invention.
Fig. 2 is a kind of another embodiment flow chart of manufacturing method of complex phase ceramic roller stick of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention is made into one below in conjunction with attached drawing
Step ground detailed description.
The present invention provides a kind of complex phase ceramic roller stick, raw material includes aggregate and binder, and the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals；
Wherein, it is that 100~200 purposes are rigid that the corundum material, which includes: 7~11 parts of corundum, granularity that granularity is 60~100 mesh,
It is 4~7 parts of corundum 14~17 parts beautiful, 250 mesh accounting≤10% of granularity.
The parts by weight of above-mentioned corundum material, clay, alumina powder, yttrium oxide, titanium dioxide, zirconium silicate and finely-powdered minerals
Summation is 100 parts.
Preferably, the aggregate includes:
27~33 parts of corundum material
27~33 parts of clay
19~22 parts of alumina powder
4~5 parts of yttrium oxide
5~10 parts of titanium dioxide
4~8 parts of zirconium silicate
4~5 parts of finely-powdered minerals；
Wherein, it is that 100~200 purposes are rigid that the corundum material, which includes: 8~10 parts of corundum, granularity that granularity is 60~100 mesh,
It is 5~6 parts of corundum 15~16 parts beautiful, 250 mesh accounting≤10% of granularity.
More preferably, the aggregate includes:
28~32 parts of corundum material
28~32 parts of clay
20~22 parts of alumina powder
4~5 parts of yttrium oxide
6~9 parts of titanium dioxide
5~7 parts of zirconium silicate
4~5 parts of finely-powdered minerals；
Wherein, it is that 100~200 purposes are rigid that the corundum material, which includes: 8~10 parts of corundum, granularity that granularity is 60~100 mesh,
It is 5~6 parts of corundum 15~16 parts beautiful, 250 mesh accounting≤10% of granularity.
Corundum is one kind by aluminium oxide (Al2O3) the jewel that is formed of crystallization, the aluminium oxide in corundum material of the present invention contains
Amount >=99%.Corundum ranks the 9th grade in Mohs scale, be so far found in nature, hardness is only second to bore
No. second high rigidity substance of stone.The corundum of variable grain degree of the present invention plays " nail is solid " effect to the crack tip in extension, makes
It is difficult to extend forward or can only detour to extend or crackle is made to be biased to or make crackle branching or be bent crackle, to increase
The energy to failure of material prevents lead crack through entire ceramic structure, guarantees composite diphase material high refractoriness and refractoriness under load,
Improve the intensity of material.
Granularity is that the dosage of the corundum of 60~100 mesh is 7~11 parts, and granularity is that the dosage of the corundum of 100~200 mesh is 14
~17 parts, the dosage of the corundum of 250 mesh accounting≤10% of granularity is 4~7 parts, and aggregate of the invention uses these three variable grains
The corundum material of rank, may be implemented maximum bulk density, simultaneously as void among particles are small, the roller stick burnt be can reach
Stomata is small and the good result that is evenly distributed.
Clay after silicate mineral at the earth's surface weathering generally by forming.General in situ weathering, particle is larger to be formed
Tap nearly original stone, referred to as primary clay or primary clay.The ingredient of this clay is mainly silica and aluminium oxide,
Color is white and fire resisting, for the main aggregate for preparing china clay.And clay is further continued for weathering, migrates through flowing water and wind-force, and in downstream shape
At a thick layer clay, referred to as secondary clay or secondary clay.For this clay because contaminated, containing metal oxide is more, color
It is deep and refractoriness is lower.Because stickiness and plasticity are good, for the main aggregate for preparing clay.Before clay of the present invention is usually
Primary clay described in person or primary clay.
Clay of the invention by physical and chemical reaction generate primary mullite, in addition, clay through decompose generate silica with
Aluminium oxide, silica and oxidation reactive aluminum generate secondary mullite, and primary mullite and secondary mullite form whole system
Mullite phase.
The titanium dioxide is Rutile structure.Rutile titanium dioxide refractive index height, thermal stability and chemistry are steady
It is qualitative strong, it is thermodynamically stable phase.
The present invention synthesizes the aluminum titanate powder of low bulk using the titanium dioxide of addition with alumina powder, wherein described
The granularity of alumina powder is 1~5 μm, and the material of aluminum titanate crystal grain of synthesis is tiny, and densification degree is high, and defect is few, mechanical strong
Degree is high.
The weight ratio of aluminium oxide and yttrium oxide of the present invention is 4-5:1-2, preferably 5:1.The aluminium oxide and oxidation
Yttrium can guarantee the agglutinating property and stability of aluminium titanates in the liquid phase that hot conditions generate.Aluminium oxide and oxidation under the ratio
Yttrium, the optimal stability of the aluminium titanates of generation；When yttria levels are too low, the agglutinating property and stabilization of aluminium titanates can not be improved
Property；When the content of yttrium oxide is too high, it will appear fluxing effect instead, can be melt away after aluminium titanates synthesis, reduce aluminium titanates
Stability.
The granularity of finely-powdered minerals of the present invention is 10~30 μm, and the finely-powdered minerals can be kyanite, andalusite or silicon line
Stone, but not limited to this.
It should be noted that kyanite, andalusite and sillimanite are high aluminium silicate mineral, and also referred to as kyanite mineral, three
Person is polymorph, and chemical composition is identical, is Al2O3·SiO2, wherein Al2O3Account for 63.1%, SiO2Account for 36.9%.?
Under different physical and chemical conditions, the crystal of a variety of different structures is crystallized into, the existing general character of physicochemical property, and it is variant.Three
Stone has many advantages, such as that resist chemical performance is strong, thermal shock mechanical strength is big, refractoriness is high, expanded by heating is irreversible, is indefinite form
The good swelling agent of refractory material.At a certain temperature, mullite and the free SiO of molten will be resolved into2, there is product resistance to
Fiery degree is high, and resistance to chemical corrosion is good, the low feature of thermal expansivity.These three mineral when heated generate volume expansion, especially with
The expansion of kyanite is maximum, and sillimanite takes second place, and andalusite is minimum.
Binder of the present invention is one or more of cellulose ether, resin or calcium lignosulfonate solution, the fiber
Plain ether includes carboxymethyl cellulose, hydroxypropyl methyl cellulose or methylcellulose etc..Preferably, the binder is cellulose
One of ether, resin, calcium lignosulfonate solution.
When binder selects cellulose ether, preferably carboxymethyl cellulose, wherein the Na of the carboxymethyl cellulose2O
Content < 10%, additional amount are 1wt%~3wt% of aggregate.
When binder selects resin, preferably thermosetting phenolic resin, additional amount be aggregate 0.5wt%~
1.5wt%.
When binder selects calcium lignosulfonate solution, the mass ratio of calcium lignosulfonate and water is 3-5:5-7, preferably
For 4:6, additional amount is 0.5wt%~1.5wt% of aggregate.Solution under the ratio can guarantee that calcium lignosulfonate is all molten
Solution, and certain concentration is maintained, it prevents that the subsequent pugging technique of excessive water influence is added.
It should be noted that part of the invention refers to parts by weight, % refers to weight percent.
Since aluminium titanates deposits two large problems stated in the background in the application, i.e., in 800~1200 DEG C of temperature
It is easily decomposed in range, loses low thermal expansion characteristics；Each axial thermal expansion coefficient difference is very big, is easily formed when cooling in material internal
A large amount of micro-cracks；The present invention is to solve the above-mentioned problems, swollen using the heat between mullite phase, corundum phase and aluminium titanates phase three
The residual internal stress field that swollen CTE mismatch generates resists extraneous partial pressure, improves the intensity of material.Work of the invention is former
It manages as follows:
(1) present invention synthesizes the aluminium titanates phase of low bulk using the titanium dioxide of addition with alumina powder.
(2) to prevent aluminium titanates from decomposing, primary mullite and decomposite that the present invention is generated using the physical and chemical reaction of clay
Silica and oxidation reactive aluminum generate secondary mullite composition whole system mullite phase.Mullite can not only mutually mention
High composite diphase material high temperature creep resistance and elevated temperature strength, and the decomposition of aluminium titanates phase can be inhibited, guarantee the stability of material, makes titanium
The low expansion of sour aluminium phase plays a role in complex phase ceramic.
(3) present invention also utilizes varigrained corundum material, and the corundum of variable grain degree plays the crack tip in extension
" nail is solid " effect, guarantees composite diphase material high refractoriness and refractoriness under load, improves the intensity of material.
In addition, the agglutinating property of the liquid phase guarantee aluminium titanates generated in hot conditions using the aluminium oxide and yttrium oxide of addition and
Stability.
The present invention further reacts generation three-phase matched coefficients of thermal expansion by solid-phase sintering and crystal development is preferably micro-
Structure is seen, to prepare excellent corundum-mullite-aluminium titanates complex phase ceramic roller stick.Its performance is as follows:
Resistance to thermal shocks (1350 DEG C~room temperature) >=6 times is not split, room temperature bending strength >=55MPa, high temperature bend strength
(1350 DEG C) >=40MPa, thermal expansion coefficient (1000 DEG C)≤5.5 × 10-6/℃.The roller stick has refractoriness height, high temperature creep-resisting
Performance is good, low thermal coefficient of expansion, using temperature height, the features such as good thermal shock stability and long service life, efficiently solve roller stick
Due to that the problem of bending deformation, can be widely applied in each region of roller kilns caused by when temperature gradient is larger in roller kilns.
Correspondingly, as shown in Figure 1, the present invention also proposes an a kind of embodiment of the preparation method of complex phase ceramic roller stick, packet
It includes:
S101, it is formulated ingredient by aggregate, through ball milling, spraying, homogenizing processing, obtains mixture；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh of granularity
4~7 parts of the corundum of accounting≤10%；
The binder is cellulose ether.
It should be noted that the technical detail of the aggregate is same as above, details are not described herein.
It is S102, mixture and binder is dry-mixed, add water wet mixing；
Specifically, the mixed mechanism are as follows: by mixture and the dry-mixed 4~6min of 1wt%~3wt% binder, then plus
14wt%~16wt% water-wet mixes 10~13min.
S103, dry blended and wet mixing mixture is granulated, and the extrusion molding on descaling extrusion press, obtains base
Part；
S104, the blank is dried, the blank moisture after drying is controlled 1.0~1.5%；
The drying temperature is 80~100 DEG C, and drying time is 35~45h；
S105, the blank after drying is subjected to cold isostatic compaction；
The pressure of the cold isostatic compaction is 150~250MPa；
S106, the blank after cold isostatic compaction is lifted in kiln to sintering, obtains roller stick finished product；
The sintering temperature is 1640~1650 DEG C, and sintering time is 28~33h.
In addition, the present invention also proposes a kind of another embodiment of the preparation method of complex phase ceramic roller stick, comprising:
S201, it is formulated ingredient by aggregate, is handled through ball milling, filters pressing, obtains mixture；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh of granularity
4~7 parts of the corundum of accounting≤10%；
The binder is one of resin or calcium lignosulfonate solution or a variety of.
It should be noted that the technical detail of the aggregate is same as above, details are not described herein.
S202, mixture is mixed with binder, carries out vacuum pugging and prepares pug, vacuum extruding blank；
The mixed mechanism are as follows: by the thermosetting phenolic resin or lignin sulfonic acid of mixture and 0.5wt%~1.5wt%
Calcium solution mixing；
S203, the blank is dried, blank moisture≤0.6% after drying；
The drying temperature is 80~120 DEG C, and drying time is 13~18h；
S204, dry blank is lifted in kiln to sintering, obtains roller stick finished product；
The sintering temperature is 1650~1665 DEG C, and sintering time is 31~35h.
With specific embodiment, the present invention is further explained below
Embodiment 1
(1) it is formulated:
(1) aggregate
Granularity is the corundum 7.5kg of 60~100 mesh
Granularity is the corundum 15.5kg of 100~200 mesh
The corundum 5kg of 250 mesh accounting≤10% of granularity
Clay 30kg
Alumina powder 21kg
Yttrium oxide 4kg
Titanium dioxide 7kg
Zirconium silicate 6kg
Finely-powdered minerals 4kg.
(2) binder
Carboxymethyl cellulose, additional amount 2.6kg.
(2) preparation method:
(1) by corundum 7.5kg that granularity is 60~100 mesh, the corundum 15.5kg that granularity is 100~200 mesh, granularity 250
Corundum 5kg, clay 30kg, alumina powder 21kg, yttrium oxide 4kg, the titanium dioxide 7kg, zirconium silicate of mesh accounting≤10%
6kg, finely-powdered minerals 4kg mix obtain mixture through ball milling, spraying, homogenizing processing；
(2) will be added the dry-mixed 4.5min of carboxymethyl cellulose of 2.6kg in mixture, then plus 14.5kg water-wet it is mixed
10.5min；
(3) dry blended and wet mixing mixture is granulated twice, extrusion molding obtains blank on descaling extrusion press；
(4) blank is dried, drying condition is 40h at 84~97 DEG C, the blank moisture control after drying
System is 1.2%；
(5) by the blank after drying through 155MPa cold isostatic compaction；
(6) blank after cold isostatic compaction is lifted to sintering in kiln, sintering condition is 31h at 1645 DEG C, is obtained
Roller stick finished product.
Embodiment 2
(1) it is formulated:
(1) aggregate
Granularity is the corundum 7kg of 60~100 mesh
Granularity is the corundum 15kg of 100~200 mesh
The corundum 5kg of 250 mesh accounting≤10% of granularity
Clay 29.5kg
Alumina powder 21.5kg
Yttrium oxide 3kg
Titanium dioxide 10kg
Zirconium silicate 6kg
Finely-powdered minerals 3kg.
(2) binder
Carboxymethyl cellulose, additional amount 2.7kg.
(2) preparation method:
(1) corundum 7kg, the corundum 15kg that granularity is 100~200 mesh, 250 mesh of granularity that granularity is 60~100 mesh are accounted for
Corundum 5kg, clay 29.5kg, alumina powder 21.5kg, yttrium oxide 3kg, titanium dioxide 10kg, zirconium silicate than≤10%
6kg, finely-powdered minerals 3kg mix obtain mixture through ball milling, spraying, homogenizing processing；
(2) by the dry-mixed 5.5min of the carboxymethyl cellulose of mixture and 2.7kg, then plus 16kg water-wet mix 12min；
(3) dry blended and wet mixing mixture is granulated twice, extrusion molding obtains blank on descaling extrusion press；
(4) blank is dried, drying condition is 40h at 88~92 DEG C, the blank moisture control after drying
System is 1.3%；
(5) by the blank after drying through 180MPa cold isostatic compaction；
(6) blank after cold isostatic compaction is lifted to sintering in kiln, sintering condition is 32h at 1645 DEG C, is obtained
Roller stick finished product.
Embodiment 3
(1) it is formulated:
(1) aggregate
Granularity is the corundum 11kg of 60~100 mesh
Granularity is the corundum 17kg of 100~200 mesh
The corundum 7kg of 250 mesh accounting≤10% of granularity
Clay 25kg
Alumina powder 18kg
Yttrium oxide 3kg
Titanium dioxide 4kg
Zirconium silicate 9kg
Finely-powdered minerals 6kg.
(2) binder
Thermosetting phenolic resin, additional amount 0.7kg.
(2) preparation method:
(1) corundum 11kg, the corundum 17kg that granularity is 100~200 mesh, 250 mesh of granularity that granularity is 60~100 mesh are accounted for
Corundum 7kg, clay 25kg, alumina powder 18kg, yttrium oxide 3kg, titanium dioxide 4kg, zirconium silicate 9kg, mine than≤10%
Object fine powder 6kg mix is formulated ingredient by aggregate, handles through ball milling, filters pressing, prepares mixture；
(2) mixture is mixed with the resin of 0.7kg, carries out vacuum pugging and prepares pug, vacuum extruding blank；
(3) blank is dried, drying condition is 14h at 120 DEG C, so that blank moisture is 0.25%；
(4) dry blank is lifted to sintering in kiln, sintering condition is 32h at 1655 DEG C, obtains ceramic rod.
Embodiment 4
(1) it is formulated:
(1) aggregate
Granularity is the corundum 8kg of 60~100 mesh
Granularity is the corundum 14kg of 100~200 mesh
The corundum 4kg of 250 mesh accounting≤10% of granularity
Clay 35kg
Alumina powder 24kg
Yttrium oxide 3kg
Titanium dioxide 4kg
Zirconium silicate 4kg
Finely-powdered minerals 4kg.
(2) binder
Calcium lignosulfonate solution, additional amount 0.5kg.
(2) preparation method:
(1) corundum 8kg, the corundum 14kg that granularity is 100~200 mesh, 250 mesh of granularity that granularity is 60~100 mesh are accounted for
Corundum 4kg, clay 35kg, alumina powder 24kg, yttrium oxide 3kg, titanium dioxide 4kg, zirconium silicate 4kg, mine than≤10%
Object fine powder 4kg mix handles through ball milling, filters pressing, prepares mixture；
(2) mixture is mixed with the calcium lignosulfonate solution of 0.5kg, carries out vacuum pugging and prepare pug, vacuum is squeezed
Blank out；
(3) blank is dried, drying condition is 15h at 80 DEG C, so that the control of blank moisture exists
0.2%；
(4) dry blank is lifted to sintering in kiln, sintering condition is 33h at 1665 DEG C, obtains roller stick finished product.
Embodiment 5
(1) it is formulated:
(1) aggregate
Granularity is the corundum 7kg of 60~100 mesh
Granularity is the corundum 15kg of 100~200 mesh
The corundum 5kg of 250 mesh accounting≤10% of granularity
Clay 25kg
Alumina powder 18kg
Yttrium oxide 6kg
Titanium dioxide 11kg
Zirconium silicate 10kg
Finely-powdered minerals 3kg.
(3) binder
Calcium lignosulfonate solution, additional amount 0.7kg.
(2) preparation method:
(1) corundum 7kg, the corundum 15kg that granularity is 100~200 mesh, 250 mesh of granularity that granularity is 60~100 mesh are accounted for
Corundum 5kg, clay 25kg, alumina powder 18kg, yttrium oxide 6kg, titanium dioxide 11kg, zirconium silicate 10kg than≤10%,
Finely-powdered minerals 3kg mix handles through ball milling, filters pressing, prepares mixture；
(2) mixture is mixed with the calcium lignosulfonate solution of 1.5kg, carries out vacuum pugging and prepare pug, vacuum is squeezed
Blank out；
(3) blank is dried, drying condition is 18h at 120 DEG C, so that the control of blank moisture exists
0.1%；
(4) dry blank is lifted to sintering in kiln, sintering condition is 31h at 1650 DEG C, obtains roller stick finished product.
The resulting ceramic rod of embodiment 1-5 is done into technology detection, as a result as follows:
To sum up, the present invention has the following technical effect that
The present invention provides a kind of complex phase ceramic roller stick, with its special formula and technique, in-situ preparation aluminium titanates phase
Method improves the thermal shock resistance of complex phase ceramic, effectively solve roller stick as the temperature difference it is big caused by Bending Deformation even be broken feelings
Condition；Mullite crystalline phase in complex phase can not only improve composite diphase material high temperature creep resistance and elevated temperature strength, and can inhibit aluminium titanates
The decomposition of phase makes the low expansion of aluminium titanates phase play a role in complex phase ceramic；Corundum in complex phase mutually guarantees composite diphase material
High refractoriness and refractoriness under load, performance: resistance to thermal shocks (1350 DEG C~room temperature) >=6 times is not split, room temperature bending
Intensity >=55MPa, high temperature bend strength (1350 DEG C) >=40MPa, thermal expansion coefficient (1000 DEG C)≤5.5 × 10-6/ DEG C.The roller
Stick have refractoriness is high, Properties of High Temperature Creep is good, low thermal coefficient of expansion, using temperature height, good thermal shock stability and use the longevity
Order the features such as long, solve the problems, such as roller stick in roller kilns due to bending deformation caused by when temperature gradient is larger, can
It is widely applied in each region of roller kilns.
Above disclosed is only a preferred embodiment of the present invention, cannot limit the power of the present invention with this certainly
Sharp range, therefore equivalent changes made in accordance with the claims of the present invention, are still within the scope of the present invention.
Claims (11)
1. a kind of complex phase ceramic roller stick, raw material include aggregate and binder, which is characterized in that the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals；
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh accounting of granularity
4~7 parts of≤10% corundum.
2. complex phase ceramic roller stick as described in claim 1, which is characterized in that the granularity of the alumina powder is 1~5 μm；
The granularity of the finely-powdered minerals is 10~30 μm.
3. complex phase ceramic roller stick as described in claim 1, which is characterized in that the amount ratio of the alumina powder and yttrium oxide
For 4-5:1-2.
4. complex phase ceramic roller stick as described in claim 1, which is characterized in that alumina content in the corundum material >=
99%；
The titanium dioxide is Rutile structure；
The finely-powdered minerals are kyanite, andalusite or sillimanite.
5. complex phase ceramic roller stick as described in claim 1, which is characterized in that the binder is cellulose ether, resin or wood
One of quality sulfonic acid calcium solution is a variety of.
6. complex phase ceramic roller stick as claimed in claim 5, which is characterized in that the cellulose ether is carboxymethyl cellulose, institute
State the Na of carboxymethyl cellulose2O content < 10%, additional amount are 1wt%~3wt% of aggregate；
The resin is thermosetting phenolic resin, and additional amount is 0.5wt%~1.5wt% of aggregate；
The mass ratio of calcium lignosulfonate and water is 3-5:5-7 in the calcium lignosulfonate solution, and additional amount is aggregate
0.5wt%~1.5wt%.
7. complex phase ceramic roller stick as described in claim 1, which is characterized in that the resistance to thermal shocks of the complex phase ceramic roller stick
(1350 DEG C~room temperature) >=6 times are not split, room temperature bending strength >=55MPa, high temperature bend strength (1350 DEG C) >=40MPa, and heat is swollen
Swollen coefficient≤5.5 × 10-6/℃。
8. a kind of method for preparing the described in any item complex phase ceramic roller sticks of claim 1-7 characterized by comprising
(1) it is formulated ingredient by aggregate, through ball milling, spraying, homogenizing processing, obtains mixture；
(2) mixture is dry-mixed with binder, add water wet mixing；
(3) dry blended and wet mixing mixture is granulated, and the extrusion molding on descaling extrusion press, obtains blank；
(4) blank is dried, the blank moisture after drying is controlled 1.0~1.5%；
(5) blank after drying is subjected to cold isostatic compaction；
(6) blank after cold isostatic compaction is lifted to sintering in kiln, obtains roller stick finished product；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh accounting of granularity
4~7 parts of≤10% corundum；
The binder is cellulose ether.
9. complex phase ceramic roller stick preparation method as claimed in claim 8, which is characterized in that the mixed mechanism in step (2) are as follows:
By mixture and the dry-mixed 4~6min of 1wt%~3wt% binder, then plus the mixed 10~13min of 14wt%~16wt% water-wet；
In step (4), drying temperature is 80~100 DEG C, and drying time is 35~45h；
In step (5), the pressure of cold isostatic compaction is 150~250MPa；
In step (6), sintering temperature is 1640~1650 DEG C, and sintering time is 28~33h.
10. a kind of method for preparing the described in any item complex phase ceramic roller sticks of claim 1-7 characterized by comprising
(1) it is formulated ingredient by aggregate, is handled through ball milling, filters pressing, obtains mixture；
(2) mixture is mixed with binder, carries out vacuum pugging and prepares pug, vacuum extruding blank；
(3) blank is dried, blank moisture≤0.6% after drying；
(4) dry blank is lifted to sintering in kiln, obtains roller stick finished product；
Wherein, the aggregate includes:
25~35 parts of corundum material
25~35 parts of clay
18~24 parts of alumina powder
3~6 parts of yttrium oxide
4~11 parts of titanium dioxide
3~10 parts of zirconium silicate
3~6 parts of finely-powdered minerals
Wherein, the corundum material includes:
Granularity is 7~11 parts of the corundum of 60~100 mesh, granularity is 100~200 mesh 14~17 parts of corundum, 250 mesh accounting of granularity
4~7 parts of≤10% corundum；
The binder is one of resin or calcium lignosulfonate solution or a variety of.
11. complex phase ceramic roller stick preparation method as claimed in claim 10, which is characterized in that the mixed mechanism in step (2)
Are as follows: mixture is mixed with the thermosetting phenolic resin of 0.5wt%~1.5wt% or calcium lignosulfonate solution；
In step (3), drying temperature is 80~120 DEG C, and drying time is 13~18h；
In step (4), sintering temperature is 1650~1665 DEG C, and sintering time is 31~35h.
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| CN117142843A (en) * | 2023-10-31 | 2023-12-01 | 淄博工陶新材料集团有限公司 | Rotary tube for molding medium borosilicate glass tube and preparation method thereof |
| CN117142843B (en) * | 2023-10-31 | 2024-01-26 | 淄博工陶新材料集团有限公司 | Rotary tube for molding medium borosilicate glass tube and preparation method thereof |
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Application publication date: 20181218 |