Alumina ceramic manufacturing process

Alumina ceramics are divided into high purity type and ordinary type two. High purity alumina
ceramics department of Al2O3 content in more than 99.9% of the ceramic material, due to its
high sintering temperature of 1650 - 1990 DEG C, the transmission wavelength of 1 6 ~ m,
generally made of molten glass to replace platinum crucible: using its light transmittance and
alkali metal corrosion for sodium lamp; in the electronic industry can be used as the integrated
circuit substrate and the insulating materials. Common type of alumina ceramic by different
Al2O3 content is divided into 99 porcelain, 95 porcelain, 90 porcelain, 85 porcelain and other
varieties, sometimes Al2O3 content in 80% or 75% are classified as ordinary alumina ceramic
series. One of 99 alumina ceramic material used for the production of high temperature crucible,
refractory furnace tube and the special wear-resistant material, such as ceramic bearings, ceramic
seals and valve piece; 95 alumina ceramics is mainly used for corrosion resistance, wear-resistant
parts; 85 porcelain occurs frequently in doped portion of talc, and improving the electrical
performance and mechanical strength, and molybdenum, can be niobium, tantalum metal sealing,
some used as electric vacuum device.
Its production process is as follows:
A powder preparation:
The factory of alumina powder according to the different requirements of products with
different forming processes is prepared into powder material. Powder particle size in 1 u m? M?
The following, if manufacturing high pure alumina ceramic products in addition to alumina
purity in the 99.99%, still need to superfine grinding and make its particle size distribution. By
extrusion or injection molding, powder binder and plasticizer is introduced,? Generally with the
weight ratio of 10 - 30% of thermoplastic plastic or resin? Organic binder and alumina powder in
150 - 200 DEG C to facilitate mixing, molding operation. The use of hot forming process of
powder raw materials without binder. If using a semi-automatic or fully automatic dry pressing,
the powder has the special requirements of the process, needs to use the spray granulation
method for powder processing, make its present shape of a ball, which is beneficial to improve
the fluidity of the powder for molding automatic filling and die wall. In addition, in order to
reduce powder and die wall friction, also need to add 1 ~ 2% lubricant? Such as stearic acid and
binder PVA?. To dry pressing need for powder spray granulation, which introduce a polyvinyl
alcohol as a binder. In recent years, a research institute in Shanghai, the development of a water
soluble wax used for Al2O3 spray granulation binder, heated in a case with good fluidity. Spray
granulation powder after must have good fluidity, loose density, flow angle of friction
temperature less than 30 DEG c.. Particle size ratio ideal conditions, to achieve a large biscuit
density.
Two forming method:
Alumina ceramic products forming method with stem pressure, grouting, extrusion, cold
isostatic pressing, hot pressing and casting, injection, hot isostatic pressing forming methods. In
recent years at home and abroad and the development of press forming, direct coagulation
casting, gel injection molding, centrifugal casting and solid freeform fabrication and molding

method. Products of different shape, size, complex shape and precision products require different
forming methods. Abstract the common shaping introduction:
1 pressing: alumina ceramic dry press forming technology is limited to the shape of herpes and
the inner wall thickness to exceed 1mm, the length and diameter ratio greater than 4 : 1. Method
of forming a uniaxial or biaxial. Compressor having hydraulic, mechanical type two, a semiautomatic or fully automatic molding method. Compressor maximum pressure for 200Mpa. The
yield can reach 15 to 50 pieces per minute. As the hydraulic press stroke uniform pressure, so the
powder filling there are differences when pressing different height. Mechanical press for powder
filling pressure size and how much change, easily lead to sintering shrinkage difference, affect
the quality of the product. So dry pressing process of powder particles are evenly distributed on
the mold filling is very important. Filling amount is accurate or not for the manufacture of
alumina ceramic parts size precision control influence. The powder particles with a greater than
60 m, ranging from 60 to 200 between the head may be the biggest free flow effect, to achieve
the best effect of forming pressure.
2 casting method: Casting alumina ceramic using earliest forming method. Due to the adoption
of the gypsum mold, low cost and easy forming of large size, the shape of complex parts.
Injection molding is the key of alumina slurry preparation. Usually in water flux as medium,
adding solution of glue and adhesive after grinding, fully exhaust, then pour into the gypsum
mould. As a result of plaster mold capillary on moisture sorption, slurry and solidification in
mould. Hollow grouting, in the mold wall adsorption slurry of required thickness, also needs to
be poured out excess slurry. In order to reduce body shrinkage, should try to use a high
concentration slurry. Alumina ceramic slurry is needed in the organic additives added to make
the slurry particles formed on the surface of electrical double layer so that the slurry stable
suspension of precipitation. In addition to adding vinyl alcohol, methyl cellulose, alginate amines
such as binder and polypropylene amine, Arabia gum as dispersing agent, goal is to make the
slurry for grouting forming operation.
Three burning technology:
Granular ceramic densification and the formation of solid materials technology method called
sintering. Sintering is inner particles in hollow out, a small amount of gas and impurity removal
so that the particles of organic matter, combined with mutual growth, formation of new material
for. Burning heating device used most widely used in electric furnace. In addition to normal
pressure sintering? I.e. pressureless sintering?, and hot pressing sintering and hot isostatic
pressing sintering. Continuous Hot-pressing Sintering while improving yield, but the equipment
and tooling costs are too high, moreover because of the axial heat, products length is restricted.
Hot isostatic pressing sintering with high temperature and high pressure gas as pressure transfer
medium, has the advantages of uniform heating, very suitable for the shape of complex products
sintering. Due to the structure of uniform, material properties than cold pressing sinter is
improved about 30 ~ 50%. Than the average increase 10 ~ 15% sintering. Therefore, the high
additional value of alumina ceramic products or national defense needs of special parts, such as
ceramic bearing, mirror, nuclear fuel and the barrel and other products, field using a hot isostatic

pressing sintering method. In addition, microwave sintering, arc plasma sintering method, since
the spread node technique is also in development studies. Four fine processing and packaging
process: Some alumina ceramic material in sintering, still need to undertake finishing. If used as
artificial bone products requirements have high surface smoothness, such as a mirror, to increase
the lubricity. As a result of alumina ceramic materials with high hardness, needs to be more hard
abrasive polishing brick material for finishing. Such as SiC, B4C or diamond. Usually a coarse to
fine abrasive level grinding, the end surface polishing. The general use of < 1 u m? M? Al2O3
powder or diamond abrasive polishing paste. In addition to laser processing and ultrasonic
grinding and polishing method can also be used. Some alumina ceramic parts and other materials
for packaging processing.

Alumina ceramic injection molding technology

Alumina ceramic is a kind of Al2O3 as the main raw materials, with corundum (a - Al2O3 ) as
main crystalline phase ceramic material. Because of its high mechanical strength, high hardness,
high frequency dielectric loss of small, high temperature and high insulation resistance, chemical
corrosion resistance and good thermal conductivity, excellent comprehensive performance, and
wide source of raw materials, the price is relatively cheap, manufacturing technology is mature
advantages, alumina ceramics have been widely used in electronics, electrical appliances,
machinery, chemical, textile, automobile, metallurgy, aerospace and other industries, has become
the world 's largest amount of oxide ceramic material. However, due to the high melting point of
2050 DEG C of alumina, alumina ceramic sintering temperature leads to higher (see Table 1 in
the standard, so that the sintering temperature ) alumina ceramic manufacture require the use of
high-temperature heating body or a high quality fuel and high-level refractory material for
furnace and kiln, which to some extent, it limits the production and the more widespread
application. Therefore, lower alumina ceramic sintering temperature, reduce energy
consumption, shortening the firing cycle, reduce the loss of furnace and kiln, thereby reducing
the production cost, has been a business concern and important issues need to be resolved. At
present, on alumina ceramics low temperature sintering technology research work has very
extensive and in-depth, from 75 to 99 porcelain of systematic research, has achieved remarkable
results. The watch is realized all kinds of alumina ceramics sintered at low temperature
condition. Table of low temperature sintering of alumina ceramics of the mechanical and
electrical properties have reached the corresponding national standards or porcelain, alumina
porcelain in some technical standards more than high aluminum porcelain GB, such as the CAS
Shanghai Institute of silicate of 1360 DEG C firing 85 porcelain, the bending strength of more
than 99%Al2O3 ceramic GB, the electric property is better than 95%Al2O3 porcelain GB;
Al2O3 content are respectively 90% and 95% of the low-temperature sintered ceramics, its
mechanical properties are better than the 95 porcelain and porcelain 99 gb. Looking at the
current all kinds of alumina ceramics low temperature sintering technology, Baconian rise,
mainly from the processing of raw materials, formulation design and firing technology from
three aspects to take measures respectively, are summarized below.

One, by raising the Al2O3 powder fineness and activity decreased porcelain sintering
temperature. Compared with the lump, powder has a large specific surface area, which is outside
of the powder work results. Using mechanical or chemical action preparation powder when
consumed by mechanical or chemical energy, part of the surface energy and stored as a powder,
in addition, in powder preparation process, can cause the powder surface and internal appear all
sorts of lattice defects, so that the lattice activation. For these reasons, the powder has high
surface free energy. The surface of powder which can be sintered intrinsic motivation. Therefore,
Al2O3 powder particles finer and finer, the higher the degree of activation, powder more easily
sintering, sintering temperature is low. In the alumina sintering technology, the use of highly
active easily sintered Al2O3 powder as raw materials is one of important steps, so the powder
preparation technology of low temperature sintering of ceramics technology become a basic link.
At present, the preparation of ultrafine activated easily sintered Al2O3 powder method is divided
into two categories, one category is mechanical method, another kind is the chemical method.
Mechanical method is to use external mechanical force to make Al2O3 powder particle
refinement, commonly used grinding process with milling and crushing, vibration mill, sand
mill, airflow grinding etc.. Through the mechanical crushing method to improve powder specific
surface area, though it is effective, but it has some limits, usually only the powder average
particle size as small as 1 m or more detailed, and the particle size distribution range is wide,
easy to impurities. In recent years, wet chemical method of manufacturing ultrafine high purity
Al2O3 powder development is rapidder, is one of the more mature is the sol - gel method. The
sol is highly stable, and can be a variety of metal ions is uniform, stable distribution in the
colloid, by further dehydration to form homogeneous gel (amorphous), after appropriate
treatment can obtain extremely active ultrafine powder mixed oxides or uniform solid solution.
At present it has roughly the following 3 kinds of technological process. (1) formed of metal
oxygen organic complexes, hydrolysis and condensation synthesis sol hydroxy containing three
dimensional structure of polymer and sol gel - low temperature evaporation and dehydration is
calcined into active oxide powder. (2) containing different metal ions and organic acid salt
solution glue mixing into solution, sol gel, evaporation and dehydration of calcined into powder.
(3) containing different metal ions by direct quenching, deposition or heated into a gel, low
temperature calcined into powder. Wet chemical synthesis of Al2O3 powder particle size can be
achieved nanometer particle size, narrow distribution range, high chemical purity, crystal defects.
Therefore chemical powder surface energy and activity than mechanical powder is much higher.
The ultrafine Al2O3 powder as raw materials not only can reduce alumina sintering temperature
(150 degrees - 300 degrees C can be reduced, but also can obtain microcrystalline) high strength
high aluminum porcelain materials. Table two is the Japanese Sumitomo Chemical Company
Limited production of sintered Al2O3 powder food chemical index. In addition, some experts
recommend the following three kinds of ultrafine Al2O3 powder preparation method, for
reference purposes only:
(1) the (NH4) SO4Al2 (SO4)3 2H2O (MgCO3) and 4Mg (OH)2 5H2O mixed, heated to 1200
DEG C decomposition, can be obtained with MgO 99% purity, particle size of 0. From 2 to 0.5 u
m alpha Al2O3 superfine powder.
(2) two acetic acid anhydrous aluminum heating to 1200 deg.c for 3 hours or more, can obtain
a particle size of less than 0 . 5 u m alpha Al2O3 superfine powder.

(3) the iron tube ball, wet grinding hundreds of hours, slurry heating pickling iron removal,
flotation, repeated several times, can be prepared from a size 0.3 - 0.5 u m alpha Al2O3 superfine
powder. Two, through the ceramic composition design dopant lowers porcelain sintering
temperature Alumina ceramic sintering temperature mainly by its chemical composition and the
content of Al2O3 in the decision, the higher Al2O3 content, the ceramic sintering temperature is
high, in addition, also with porcelain composition system, the composition and additives on the
type. For example, in the Al2O3 content is very, CaOAl2O3SiO2 Al2O3 porcelain than
MgOAl2O3SiO2 system ceramic materials low sintering temperature, the mass production of
CaOMgOAl2O3SiO2 system porcelain, for it has the advantages of low sintering temperature
and good performance, should control its SiO2 / CaO is 1. 6 ~ 0. 6., MgO content does not
exceed the flux oxide total 1 / 3, at the same time, introduced in the formula of small amounts of
La2O3, Y2O3, Cr2O3, MnO, TiO2, ZrO2, Ta2O3 oxide can further reduce the sintering
temperature, improve the porcelain body of the microstructure and properties of. Therefore, in
ensuring the porcelain body meet product use and technical requirements under the premise, we
can through the formulation design, reasonable choice of porcelain system, adding proper
sintering additives, so that the sintering temperature of alumina is reduced as much as possible.
At present in the formulation design of adding various additives, according to its promotion of
alumina ceramics sintering mechanism is different, they can be divided to form new phase or
solid solution additive and produces liquid additives two categories. In 1, and Al2O3 to form a
new phase or solid solution additive. The additives are alumina lattice constant phase near the
oxide, such as TiO2, Cr2O3, Fe2O3, MnO2 etc, during sintering, these additives can with Al2O3
to form solid solution, the solid solution or for mixing solid solution (such as Ti4 replacement
when Al3 ), or as a limited solid solution body, or as a continuous solid solution ( such as Cr2O3
and Al2O3 formed ), they can activate the lattice (TI4, Al3 ionic radius difference caused by
forming a hole or migration of atoms), (3TiO2, AbO3 3Tia1Va160) and so that the lattice
distortion, the action of the Al2O3 easy crystallization and sintering of ceramics. For example,
adding 0.5 ~ 1.0% TiO2, can make the ceramic sintering temperature decreased from 150 to 200
DEG c.. With solid phase sintering based high alumina porcelain often uses this kind of
additives, such as a black alumina ceramic formula follows (wt% ): Al2O3 91, CoO 0 . 5, MnO2
3 . 7, Cr2O3 2 . 1, SiO2 0 . 4, TiO2 2 . 0, V2O3 0 . 3, the porcelain in the 1350 temperature
insulation 2 hours firing. This kind of additive to promote the role of alumina ceramic sintering
has certain regularity: 1 can be formed between Al2O3 limited solid solution additive is formed
of continuous solid solution of the cooling effect of the additive is greater; the variable valency
ion additives than changeless value of additive effect; the cationic charge much, electrovalency is
tall the cooling effect of the additives of greater. Note that, because this kind of additives is in
lack of liquid phase sintering conditions (heavy crystallization sintering), so the intracrystalline
porosity is difficult to fill, poor air tightness, and electrical performance to drop more, to be
considered in formulation design.2, the formation of liquid phase sintering additives. This kind
of additive chemical composition are mainly SiO2, CaO, MgO, SrO, BaO, they can with other
components in the firing process of the formation of two yuan, three yuan or a plurality of
eutectic. As a result of liquid phase formation temperature is low, thus greatly reducing the
alumina ceramic sintering temperature. When there is a considerable amount (about 12% ) of the
liquid, solid particles in liquid phase and solid phase particles have certain solubility can be

liquid wetting, its promote sintering effect is obvious. The mechanism is relatively solid liquid
surface wettability and surface tension of the solid particles, both close to and fill the pores. In
addition, the sintering process by small defective crystal surface activity, therefore in the liquid
phase solubility than larger crystals of the much larger. Thus, sintering process and crystal
growing, porosity decreases, appeared heavy crystallization. In order to prevent recrystallization
grain too grown up, affect the mechanical properties of ceramics, in the formula design should be
considered in selection of some of the grain increase without influence or even can inhibit grain
increased additives, such as MgO, CuO and NiO etc..At present, in the liquid phase sintering of
Al2O3 ceramic composition, sintering additives can adopt the following 3 materials form to join.
The natural mineral form join. This kind of mineral raw materials mainly include: kaolin,
bentonite clay mine. Quartz, talc, magnesite, dolomite, calcite and so on, they are the
introduction of SiO2, MgO, CaO and other chemical constituents. Formula of kaolin and other
clay minerals are used, in addition to meeting the porcelain body chemical composition
requirements, more can improve the blank forming performance. This form of adding additives
for Al2O3 content below 90% of aluminous porcelain ingredients, such as a low temperature
sintering of 75 porcelain formula as follows ( wt% ): Al2O3 65, 24, calcined kaolin bentonite 2,
BaCO3 4, 3, 2 talc calcite. The synthetic additives, to form join. It is in the CaOAl2O3SiO2,
MgOAl2O3SiO2 CaOMgOAl2O3SiO2, three yuan, four yuan or other phase diagram in to find
the lowest eutectic composition, advance in points CaO, MgO, SiO2 component, Al2O3 desired
compounds were first ingredients, through ball milling, calcined made eutectic, namely" artificial
synthesis additive", then according to a certain ratio of artificial synthetic additives and Al2O3
powder second ingredients, to meet the requirements of chemical composition and properties of
alumina ceramics. The method has high purity, mainly used to reduce the chemical composition
of accurate, high performance requirements of high aluminum porcelain sintering temperature,
disadvantage is the complicated process, high energy consumption, product cost is high, only in
exceptional cases by. The chemical raw material to form join. In the ingredients, directly to the
various chemical raw materials as additive and Al2O3 powder with a complete ingredients,
various sintering additives composition ratio remains the reference professional phase diagram in
lowest eutectic point composition to set. Production practice proves, this method not only with
artificial synthetic additive method has the same cooling effect, but also greatly simplifies the
process, regardless of formulation design, ingredients and process are better than synthetic
additive method is simple, but also more easily than the natural mineral form of porcelain, stable
performance, energy-saving benefit. In practical production, from reduce cost and blank forming
performance reasons, natural mineral raw materials and chemical raw materials are often used at
the same time. For example, a sintered at low temperature (1500 degrees C x 2 ) high aluminum
porcelain formula follows (wt%); alpha 93, Suzhou 3, Al2O3 soil burned bone stone 2, CaCO3 1
. 5, BaCO3 0.5, and ZrO2, CeO2, La2O3 2%.Three, using a special firing process to reduce
porcelain sintering temperature Sintered by hot pressing process, in the billet heating and
pressurizing sintering, so only by diffusion mass transfer to complete, the plastic flow plays an
important role, blank sintering temperature than normal pressure sintering is much lower, thus
reducing Al2O3 sintering is one of the important techniques of ceramic sintering temperature.
The hot pressing sintering method with pressure sintering and hot isostatic pressing sintering
method (HIP) two. The HIP method can make the body be isotropic pressure, the microstructure

of ceramics sintering method is more uniform than pressure. Alumina porcelain, if under
ordinary sinter must burn to high temperature more than 1800 DEG C, pressing 20MPa sintering,
at about 1000 DEG C lower temperature has been densified. Hot pressing sintering technology
not only reduce alumina sintering temperature, but also can restrain the grain growth, to obtain
high strength dense microcrystalline alumina ceramic, especially for transparent alumina ceramic
and porcelain sintered corundum ceramics .In addition, because the alumina sintering process
with anion diffusion rate, and reducing atmosphere in favor of anion vacancies increases, can
promote the sintering. Therefore, vacuum sintering, a hydrogen atmosphere sintering alumina
porcelain sintered at low temperature is an effective auxiliary method. In production practice, in
order to obtain the best comprehensive economic benefits, the fever techniques often used in
conjunction, adding sintering additive method compared with other methods, has the advantages
of low cost, good effect, simple process and practical characteristics. In the aluminum porcelain,
high-alumina corundum porcelain production is widely used. In addition, from the material point
of view, by doping modification technology, greatly improve the mechanical properties of
alumina ceramic, porcelain body with low Al2O3 content instead of high content of Al2O3 of
porcelain body, also is the enterprise commonly used to reduce the sintering temperature of
alumina ceramic products is an effective technical means. For example, in the material properties
to meet the product requirements, use 85 instead of 90 or 95 porcelain, 90 porcelain, 95
porcelain, 99 porcelain instead is feasible. Although the alumina ceramic fever technology has
achieved good economic benefit, but still has the potential to be excavated, at present there are
still some products, from the special properties of materials requirements and under the condition
of high temperature device size stability considerations, still using high temperature sintering,
how will this kind of product sintering temperature also falls, is the future of porcelain body
doping such low fever technical direction.