CN108892489A - Easy fired high alumina ceramic and preparation method thereof - Google Patents

Easy fired high alumina ceramic and preparation method thereof Download PDF

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CN108892489A
CN108892489A CN201810663748.8A CN201810663748A CN108892489A CN 108892489 A CN108892489 A CN 108892489A CN 201810663748 A CN201810663748 A CN 201810663748A CN 108892489 A CN108892489 A CN 108892489A
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alumina ceramic
high alumina
raw material
oxide
slurry
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任国兴
马冬冬
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Hejin Jinhao Special Ceramics Co Ltd
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Hejin Jinhao Special Ceramics Co Ltd
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Abstract

Easy fired high alumina ceramic of the present invention and preparation method thereof belongs to aluminium oxide ceramics technical field;The technical issues of solution is:A kind of easy fired high alumina ceramic and preparation method thereof is provided, while keeping mechanical high alumina ceramic, electrical and biological property, and easy fired is able to achieve, reduces technology difficulty and energy loss;The technical solution used for:Easy fired high alumina ceramic, the raw material including following weight:0.2 ~ 1 part of bismuth oxide, 0.2 ~ 1 part of antimony oxide, 0.4 ~ 1 part of titanium dioxide, 0.1 ~ 0.5 part of magnesia, 0.5 ~ 1.5 part of silica, 0.5 ~ 2 part of kaolin, 2 ~ 8 parts of calcium oxide, 100 parts of aluminium oxide;Present invention process is simple, and on the basis of not changing existing equipment, effect is prominent, while keeping mechanical high alumina ceramic, electrical and biological property, 120 DEG C lower than nominal sintering temperatures of firing temperature or more, extends the service life of kiln, alms bowl tool and molybdenum bar.

Description

Easy fired high alumina ceramic and preparation method thereof
Technical field
Easy fired high alumina ceramic of the present invention and preparation method thereof belongs to aluminium oxide ceramics technical field, and in particular to a kind of The preparation of easy fired aluminium oxide ceramics.
Background technique
Aluminium oxide ceramics is one kind with Alpha AL2O3For the ceramic material of principal crystalline phase, alumina content generally 75 ~ Between 99%.Traditionally classified with alumina content in ingredient, alumina content is " 75 " magnetic, aluminium oxide 75% or so Content is " 99 " magnetic 99% or so.Since alumina raw material is from a wealth of sources, relative low price, so that it is in electronics, machine Tool, weaving, automobile, chemical industry, field of metallurgy are used widely.
High alumina ceramic refers to aluminium oxide ceramics of the alumina content 90 ~ 99%, calcination temperature generally 1600 DEG C with On, the sintering temperature of 99 magnetic is more up to 1800 DEG C or so.It is generally necessary to which CaO-MgO-SiO is added in aluminium oxide2Etc. appraising at the current rate Oxide is as sintering aid, and to reduce firing temperature, but typical temperature is also up to 1650 DEG C or more.The oxidation of sintering aid is added Aluminium is after high temperature firing, and volume is fine and close, and high mechanical strength, heating conduction is good, and dielectric strength is high, and dielectric loss is low, bio-compatible Property is good, commonly known as corundum magnetic, is widely used in each field.
In order to reduce the firing temperature of high alumina magnetic, the alumina raw material of smaller particle can be used, it can also be using such as Hot pressed sintering, HIP sintering, vacuum-sintering, atmosphere sintering, microwave sintering, etc. the sintering methods such as particles sinterings, but these The odd high or equipment of method or cost of material costly or is difficult to produce in enormous quantities, all limits answering for these methods With.Therefore, suitable sintering aid is found, is at this stage being still the method for the reduction sintering temperature of economical rationality.
Summary of the invention
The present invention overcomes the shortcomings of the prior art, and technical problem to be solved is:It is high to provide a kind of easy fired Aluminium ceramics and preparation method thereof while keeping mechanical high alumina ceramic, electrical and biological property, and are able to achieve easy fired, Reduce technology difficulty and energy loss.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is:Easy fired high alumina ceramic, including it is as follows The raw material of weight:
0.2 ~ 1 part of bismuth oxide,
0.2 ~ 1 part of antimony oxide,
0.4 ~ 1 part of titanium dioxide,
0.1 ~ 0.5 part of magnesia,
0.5 ~ 1.5 part of silica,
0.5 ~ 2 part of kaolin,
2 ~ 8 parts of calcium oxide,
100 parts of aluminium oxide.
Preferably, easy fired high alumina ceramic, the raw material including following weight:
0.3 ~ 0.5 part of bismuth oxide,
0.3 ~ 0.5 part of antimony oxide,
0.4 ~ 0.8 part of titanium dioxide,
0.2 ~ 0.4 part of magnesia,
0.5 ~ 1 part of silica,
1 ~ 2 part of kaolin,
2 ~ 4 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry, the weight of the raw material and water by the first step For:300 parts of raw material, 150-180 parts of water;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling, mixing speed 90-120 to slurry for second step R/min, mixing time is 140-160 min, when the fineness through laser particle size detector test slurry reaches D50≤2.2 micron Stop wet-milling;
Third step is added PVA solution and is uniformly mixed in slurry, and the weight of the PVA solution is the 10-12% of slurry gross weight;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2-2.5 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
PVA solution in the third step is the PVA solution of concentration 10%.
The present invention has the advantages that compared with prior art:
Present invention process is simple, and on the basis of not changing existing equipment, effect is prominent, is keeping high alumina ceramic mechanical, electrical While with biological property, 120 DEG C lower than nominal sintering temperatures of firing temperature or more, it can be burnt completely at 1490 ~ 1520 DEG C or less At the service life of extension kiln, alms bowl tool and molybdenum bar reduces electricity charge consumption;
The effect of bismuth oxide and antimony oxide in ceramic raw material is to generate low temperature liquid phase, promotes alumina sintering, adds Fast dissolution, precipitation effect and evaporation, condensation effects, wherein bismuth oxide fusing point is 825 DEG C, and antimony oxide fusing point is 655 DEG C, sintering velocity can be greatly speeded up;
Titanium dioxide in ceramic raw material can be formed continuous solid due to close with alumina atom radius and lattice with aluminium oxide Solution, increases aluminium oxide distortion of lattice, and activated alumina lattice energy reduces sintering temperature;
Magnesia effect in ceramic raw material is to form aluminum-spinel, hinders growing up for alumina grain, forms fine grained texture, Improve mechanical performance.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention, Technical solution of the present invention is clearly and completely described, it is clear that described embodiment is that a part of the invention is implemented Example, instead of all the embodiments;Based on the embodiments of the present invention, those of ordinary skill in the art are not making creativeness Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of labour.
In the present invention PVA solution be polyvinyl alcohol resin solution, the present invention used in PVA solution be in advance allotment and it is molten The PVA solution of the concentration 10% solved.
Embodiment one
Easy fired high alumina ceramic, the raw material including following weight:
0.2 part of bismuth oxide,
0.2 part of antimony oxide,
0.4 part of titanium dioxide,
0.1 part of magnesia,
0.5 part of silica,
0.5 part of kaolin,
2 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by said ratio plus water is mixed into slurry, 300 kg of raw material gross weight by the first step, and water weighs 150 kg;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling to slurry for second step, and mixing speed is 90 r/ Min, mixing time are 140 min, and the fineness through laser particle size detector test slurry stops wet when reaching D50≤2.2 micron Mill;
Third step is added the PVA solution of 45 kg and is uniformly mixed in slurry;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
Embodiment two
Easy fired high alumina ceramic, the raw material including following weight:
0.3 part of bismuth oxide,
0.3 part of antimony oxide,
0.4 part of titanium dioxide,
0.2 part of magnesia,
0.5 part of silica,
1 part of kaolin,
2 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry by the first step, and raw material gross weight is 300 kg, and water weighs 160 kg;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling to slurry for second step, and mixing speed is 100 r/ Min, mixing time are 150 min, and the fineness through laser particle size detector test slurry stops wet when reaching D50≤2.2 micron Mill;
Third step is added the PVA solution of 50 kg and is uniformly mixed in slurry;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
Embodiment three
Easy fired high alumina ceramic, the raw material including following weight:
0.4 part of bismuth oxide,
0.4 part of antimony oxide,
0.6 part of titanium dioxide,
0.3 part of magnesia,
0.8 part of silica,
1.5 parts of kaolin,
3 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry by the first step, and raw material gross weight is 300 kg, and water weighs 160 kg;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling to slurry for second step, and mixing speed is 100 r/ Min, mixing time are 150 min, and the fineness through laser particle size detector test slurry stops wet when reaching D50≤2.2 micron Mill;
Third step is added the PVA solution of 50kg and is uniformly mixed in slurry;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2.3 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
Example IV
Easy fired high alumina ceramic, the raw material including following weight:
0.5 part of bismuth oxide,
0.5 part of antimony oxide,
0.8 part of titanium dioxide,
0.4 part of magnesia,
Silica 1 part,
2 parts of kaolin,
4 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry by the first step, and raw material gross weight is 300 kg, and water weighs 170 kg;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling to slurry for second step, and mixing speed is 110 r/ Min, mixing time are 150 min, and the fineness through laser particle size detector test slurry stops wet when reaching D50≤2.2 micron Mill;
Third step is added the PVA solution of 50kg and is uniformly mixed in slurry;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2.5 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
Embodiment five
Easy fired high alumina ceramic, the raw material including following weight:
1 part of bismuth oxide,
1 part of antimony oxide,
1 part of titanium dioxide,
0.5 part of magnesia,
.5 parts of silica 1,
2 parts of kaolin,
8 parts of calcium oxide,
100 parts of aluminium oxide.
It is thin that the bismuth oxide, antimony oxide, titanium dioxide are all made of the high-purity that fineness is D50≤4 micron, height Spend raw material.
It is the high-purity of D50≤4 micron that the magnesia, silica, kaolin, calcium oxide and aluminium oxide, which are all made of fineness, Degree, high fineness raw material.
The preparation method of easy fired high alumina ceramic, includes the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry by the first step, and raw material gross weight is 300 kg, and water weighs 180 kg;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling to slurry for second step, and mixing speed is 120 r/ Min, mixing time are 160 min, and the fineness through laser particle size detector test slurry stops wet when reaching D50≤2.2 micron Mill;
Third step is added the PVA solution of 55 kg and is uniformly mixed in slurry;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2.5 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
Finally it should be noted that:The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Present invention has been described in detail with reference to the aforementioned embodiments for pipe, those skilled in the art should understand that:Its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (6)

1. easy fired high alumina ceramic, it is characterised in that the raw material including following weight:
0.2 ~ 1 part of bismuth oxide,
0.2 ~ 1 part of antimony oxide,
0.4 ~ 1 part of titanium dioxide,
0.1 ~ 0.5 part of magnesia,
0.5 ~ 1.5 part of silica,
0.5 ~ 2 part of kaolin,
2 ~ 8 parts of calcium oxide,
100 parts of aluminium oxide.
2. easy fired high alumina ceramic according to claim 1, it is characterised in that the raw material including following weight:
0.3 ~ 0.5 part of bismuth oxide,
0.3 ~ 0.5 part of antimony oxide,
0.4 ~ 0.8 part of titanium dioxide,
0.2 ~ 0.4 part of magnesia,
0.5 ~ 1 part of silica,
1 ~ 2 part of kaolin,
2 ~ 4 parts of calcium oxide,
100 parts of aluminium oxide.
3. easy fired high alumina ceramic according to claim 1, it is characterised in that:The bismuth oxide, three oxidations two It is the high-purity of D50≤4 micron, high fineness raw material that antimony, titanium dioxide, which are all made of fineness,.
4. easy fired high alumina ceramic according to claim 1, it is characterised in that:The magnesia, silica, kaolinite It is the high-purity of D50≤4 micron, high fineness raw material that soil, calcium oxide and aluminium oxide, which are all made of fineness,.
5. the preparation method of easy fired high alumina ceramic as described in claim 1, it is characterised in that include the following steps:
Raw material is poured into container by the proportion plus water is mixed into slurry, the weight of the raw material and water by the first step For:300 parts of raw material, 150-180 parts of water;
Dispersing agent and plasticiser are added in slurry, and is stirred wet-milling, mixing speed 90-120 to slurry for second step R/min, mixing time is 140-160 min, when the fineness through laser particle size detector test slurry reaches D50≤2.2 micron Stop wet-milling;
Third step is added PVA solution and is uniformly mixed in slurry, and the weight of the PVA solution is the 10-12% of slurry gross weight;
Slurry is granulated, then dry-pressing or isostatic pressing by the 4th step by mist projection granulating tower;
Powder is made ceramic blank and is fired molding in tunnel oven by the 5th step, and the firing temperature in tunnel oven is 1490 ~ 1520 DEG C, and ceramic blank must keep the temperature 2-2.5 h in firing at 1520 DEG C;
6th step, will be cooling after the high alumina ceramic formed by a firing removal tunnel oven.
6. the preparation method of easy fired high alumina ceramic according to claim 5, it is characterised in that:In the third step PVA solution is the PVA solution of concentration 10%.
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