CN107244905A - A kind of preparation method of face coat high-temperature crucible - Google Patents
A kind of preparation method of face coat high-temperature crucible Download PDFInfo
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- CN107244905A CN107244905A CN201710415275.5A CN201710415275A CN107244905A CN 107244905 A CN107244905 A CN 107244905A CN 201710415275 A CN201710415275 A CN 201710415275A CN 107244905 A CN107244905 A CN 107244905A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
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- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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Abstract
The present invention relates to crucible preparing technical field.The invention discloses a kind of preparation method of face coat high-temperature crucible, the steps such as it includes getting the raw materials ready, the shaping of raw material for crucible, mixed powder, crucible, crucible sintering, coating paste, coating and coating sintering, also need to carry out the high-temperature process of a period of time after the completion of coating sintering, remove unreacted raw material.In forming process of the present invention, high-temperature crucible yields more preferably, in forming process is difficult to crush because of powder unbalance stress；High-temperature crucible results in homogeneity more base substrate after being particularly molded, can promote the efficiency of follow-up sintering technique in preparation process；The high-temperature crucible being prepared has a higher consistency, the consistency of most samples up to 97% and more than；The present invention obtains a kind of high-temperature crucible with higher heat resisting temperature by way of coating on the premise of low cost is kept.
Description
Technical field
The present invention relates to crucible preparing technical field, more particularly, to a kind of preparation side of face coat high-temperature crucible
Method.
Background technology
Crucible is a kind of conventional experiment and production equipment, either in the growth preparation process of crystalline material, still
In the building-up process of powder body material, the participation of crucible is all be unable to do without, the quality of crucible often influences the preparation of these materials
Process and the performance for being prepared material.In the prior art, crucible is generally sintered and is prepared again using powder shaping, its
Middle shaping is an important ring in whole crucible preparation process, the uniformity and compactness of shaping can to the sintering process of crucible and
The performance of the final obtained crucible of sintering produces tremendous influence；Existing crucible shaping or even the shaping of all powder body materials are big
All using techniques such as pressure forming, isostatic pressings, wherein isostatic pressing is that uniform in shaping and shaping compactness are best
Molding mode, but it generally requires and carried out under oil pressure environment, it is more complicated to there is moulding process, and former cost is high, behaviour
Be required height, the shortcomings of molding time is also longer in addition, for need to improve shaping efficiency and reduce the crucible of shaping cost into
Type is relatively not suitable for；Mechanical pressing by the way of applying unilateral pressure to powder typically using being molded, because it is in forming process
There is provided unilateral pressure so that its base substrate unbalance stress in forming process, pressure side stress is larger, the side away from pressure
Stress is smaller, and unbalance stress causes compactness also heterogeneity, and stress side is more closely knit, and opposite side then has more skies
Gap, this uneven closely knit situation produces larger adverse effect when can be sintered to crucible, is needed for the more side in space
Control sintering rate and enable the movement of crystal boundary in base substrate more slowly so that gas and impurity be excluded outside crystal grain rather than by
Crystal grain is wrapped up, and closely knit side then needs to accelerate the rate travel of base substrate crystal boundary in sintering process, improves sintering efficiency；Mirror
In this situation, must control sintering rate during sintering is enough slow, improves the sintering effect of base substrate, but inevitably
It can influence to sinter efficiency, while there is also the sintering effect of the high side of influence compactness；Accordingly, it would be desirable to which one kind can be molded
The powder body material of base substrate compactness and the uniformity can be promoted in journey.
Existing conventional crucible is generally corundum, 95 porcelain, and 99 town of porcelains are conventional corundum crucibles, its mostly by purity compared with
High aluminum oxide is directly fired and formed, and the temperature that it can be acted on is also higher, up to 1700 DEG C or so, can meet most of materials
It is synthetically prepared；But wherein also have a problem often ignored, under nearly 1700 DEG C of hot environment, due to
It is fairly close to the fusing point of aluminum oxide, although corundum crucible is now also unlikely to fail or damage, but the aluminum oxide on its surface
Composition have high activity, these have high active aluminium ion, oxygen atom can enter crucible in react
In reactant, for structural material, the influence that the foreign ion of these micro contents is produced is relatively small, it might even be possible to neglect
Slightly disregard, but for some functional materials, the intrusion of some impurity, even the few impurity intrusion of content also can be big
Its corresponding performance is influenceed greatly；Turn into a feasible selection from the material with higher heat resisting temperature, but using has
The material of higher heat resisting temperature can then accordingly increase experiment/production cost.
The content of the invention
In order to solve the above problems, it can be prepared at low cost with more preferable high temperature resistant the invention provides one kind
Performance, and with higher-density, the preparation method of the face coat high-temperature crucible of homogeneity.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of preparation method of face coat high-temperature crucible, comprises the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content be 99~99.5wt% 100 parts of schmigel, 0.05~0.15 part of crystalline graphite powder, sericite 0.3~
0.8 part, 0.3~0.5 part of talcum powder, 1.5~2.0 parts of pelletizing additives；
Prepare coating material by the component of following parts by weight：20~35 parts of carbon source, 35~47 parts of silicon source, 5~8 parts of dispersant；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 20~40 minutes under medium, dry after wet-milling and mixed powder are made；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 2.5~30MPa, system
Obtain crucible green compact；
e）Crucible is sintered：Crucible green compact are risen to 550~600 DEG C and be incubated 1~1.5 hour dumping by room temperature and arrange carbon；Afterwards will
Temperature continues to rise to 1350~1450 DEG C, and insulation is sintered for 4~6 hours, is naturally cooling to room temperature after the completion of sintering, resistance to height is made
Warm crucible crude product；
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
200~600rpm rotating speeds are stirred 5~15 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：Face coat high-temperature crucible crude product is small to insulation 2~3 in 1400~1600 DEG C by room temperature
When, room temperature is subsequently cooled to, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment.
One purpose of technical solution of the present invention is in order to increase crucible green compact compactness and homogeneity, that is, to cause in powder
It during shaping, can also obtain that the uniform compactness of powder is uniform and the high base substrate of compactness in the case where briquetting pressure is uneven, protect
Demonstrate,prove the homogeneity of base substrate；Above-mentioned purpose is obtained by two methods, one is the particle diameter distribution of rational allocation powder；Second side
Method be added in powder it is a certain amount of can increase the additive of powder fluidity, these additives are with crystalline flake graphite and talcum
Based on powder.In order to obtain have higher heat-resisting ability crucible, from alumina content for 98~99wt% corundum powder compared with
Suitably, and the corundum of high alumina content is originally a kind of refractory material with fabulous resistance to elevated temperatures.
Graphite is a kind of inorganic material of stratiform, and it has good greasy property, by increasing capacitance it is possible to increase the mobility of powder, but
It is due to that its constitution element is carbon, its refractoriness under air ambient is simultaneously bad, therefore, can only add a small part,
And removing of being tried one's best when being sintered after powder shaping；Sericite is a kind of aluminium silicate mineral, is also a kind of laminar silicic acid salt mine
Thing, it also has good greasy property, and the mobility of powder can be increased by being added in powder, and aluminium silicate mineral is also
A kind of material with good fire resistance, its a small amount of addition will not produce on the refractoriness of powder and deteriorate influence；Talcum powder
It is a kind of hydrous magnesium silicate mineral, it has good greasy property, while it also has very outstanding anti-greasy performance, its energy
Prevent to reunite between fine powder material.
Carbofrax material is a kind of new refractory material with higher heat resisting temperature, and surface after its coating sintering
It is more fine and close and smooth.Presoma is mixed to prepare using carbon source and silicon source in the present invention, is sintered after coating afterwards and is made corresponding
Coat of silicon carbide, improve crucible surface heat resistance；Because the part in material preparation process, being in contact with raw material becomes
For the coat of silicon carbide with higher heat resisting temperature, because reaction temperature is far below the fusing point of carborundum, the activity of carborundum is still
It is old weaker, in the material that its more difficult entrance is being synthesized, thus also prevent the material correlated performance that influence is being synthesized
Possibility, using this kind have coat of silicon carbide corundum crucible the less material of impurity content can be made.
Dumping process in step e is in order to exclude the graphite added in base substrate in pelletizing additives and raw material, due to making
Grain additive is organic compound, its resistance to elevated temperatures extreme difference, and can decompose under hot environment generation gas or incomplete
The particle of burning, if the sintering character of crucible can be influenceed by before sintering not removing these additives, produces substantial amounts of gas
Also presence is the risk that crucible base substrate is burst, even if the reasons why excluding graphite is also to be endangered in this way, not produced in sintering stage,
Can be in the raw materials for sintering in pollution crucible during subsequent use.
In step h, it can not be obtained because the coat of silicon carbide such as carbon source and silicon source raw material carries out high temperature sintering under oxidizing atmosphere
Obtain carborundum, it is therefore desirable to be sintered under the inert gases such as nitrogen or reducing atmosphere.
Preferably, in raw material for crucible, 15~20wt% is coarse grain footpath schmigel in schmigel, 45~55wt% is middle particle diameter
Schmigel, surplus is fine grain schmigel；Pelletizing additives are the polyvinyl alcohol water solution that percetage by weight is 5%.
Preferably, in raw material for crucible, the particle diameter of coarse grain footpath schmigel is 250~350 mesh, the particle diameter of middle particle diameter schmigel
For 700~1000 mesh, the particle diameter of fine grain schmigel is 1200~1500 mesh；The median particle diameter D of coarse grain footpath schmigel50For 290
~300 mesh, the median particle diameter D of middle particle diameter schmigel50For 800~900 mesh, the median particle diameter D of fine grain schmigel50For 1350
~1400 mesh.
To make the base substrate of acquisition that there is the higher uniformity and compactness, it is ensured that the homogeneity of base substrate, also in crucible
Gas during sintering between powder granule can be excluded preferably, it is necessary to which the particle diameter distribution of rational allocation powder is so that medium grain size
Powder accounts for major part, so can both fill up compared with the space between coarse granule, reduces the gas content in base substrate after shaping, also may be used
With avoid when fine grain particle be in the great majority brought powder particles reunite the problem of, through test medium grain size powder account for
45wt% or so, then the minimum allocative decision of minimum thicker particles, which can try one's best, make the space between powder minimum, carefully
Agglomeration between particle is also minimum
The particle diameter of coarse grain footpath powder is in the range of 250~350 mesh, about 42~60 microns, the particle diameter of middle particle diameter powder
In the range of 700~1000 mesh, about 15~21 microns, the particle diameter of fine grain powder is 1200~1500 mesh scopes
It is interior, about 10~12 microns；Such particle diameter distribution can cause, fine grain powder can just fill up coarse grain footpath and
The space formed after middle particle diameter powder mixing, enables to powder to reach most compact state in theory；It is aided with mobility simultaneously
Additive, being distributed each several part in powder can be close to such ideal distribution state.
Preferably, in coating material, carbon source is one kind in lignin, starch, sucrose or sodium alginate, and silicon source is two
Silica percetage by weight is 60~70% Ludox, and dispersant is odium stearate or sodium carboxymethylcellulose.
Lignin, starch, sucrose and sodium alginate etc. are all common carbon containing organic polymers, and its phosphorus content is higher,
And it is added in the aqueous solution（As in Ludox）The viscosity of solution can also be increased, coating so can be more easily prepared
Layer.
Preferably, in step b mixing process, the weight of absolute ethyl alcohol is schmigel, graphite powder, land plaster, muscovite
1~1.5 times of powder and talcum powder gross weight；The rotating speed of wet-milling is 400~600rpm.
Preferably, molding process is completed on a vibration table in step d, shake table amplitude is 4.5~5.5mm, vibration frequency
Rate is 80~90 times/min.
Preferably, in step e, the heating rate control before dumping row's carbon stage is in 1~3 DEG C/min, dumping row's carbon rank
Heating rate after section is controlled in 3~5 DEG C/min.
Preferably, after the completion of step h, obtained face coat high-temperature crucible at 550~600 DEG C and is incubated 1~
1.5 hour.
The problem of due to there is reaction efficiency, fail completely and silicon source there is part carbon source material through coating sintering successor
Material carries out reaction generation carborundum, and these carbon source materials can produce harmful effect in pyroreaction again, such as produce
Some gases impact/situations such as pollute reactant, it is therefore desirable in advance by these unreacted carbon sources after the completion of coating sintering
Material is removed, in order to avoid influence subsequent use.
Therefore, the invention has the advantages that：
（1）High-temperature crucible of the present invention is in forming process, and yields more preferably, in forming process is difficult because of powder unbalance stress
It is broken；
（2）High-temperature crucible results in homogeneity more base substrate, energy in preparation process after being particularly molded in the present invention
Enough promote the efficiency of follow-up sintering technique；
（3）The high-temperature crucible being prepared in the present invention has a higher consistency, and the consistency of most samples is up to 97%
And more than；
（4）The present invention obtains a kind of resistance to higher heat resisting temperature by way of coating on the premise of low cost is kept
High-temperature crucibles.
Embodiment
Technical scheme is further described with reference to embodiment.
Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on this
Embodiment in invention, all other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example is applied, the scope of protection of the invention is belonged to.
Embodiment 1
A kind of preparation method of face coat high-temperature crucible, comprises the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content be 99wt% 100 parts of schmigel, 0.05 part of crystalline graphite powder, 0.3 part of sericite, 0.3 part of talcum powder,
1.5 parts of pelletizing additives；15wt% is coarse grain footpath schmigel in schmigel, and 45wt% is middle particle diameter schmigel, and 40wt% is fine grain
Schmigel；The particle diameter of coarse grain footpath schmigel is 250~350 mesh, and the particle diameter of middle particle diameter schmigel is 700~1000 mesh, fine grain
The particle diameter of schmigel is 1200~1500 mesh；The median particle diameter D of coarse grain footpath schmigel50For 290 mesh, the intermediate value of middle particle diameter schmigel
Particle diameter D50For 800 mesh, the median particle diameter D of fine grain schmigel50For 1350 mesh；Pelletizing additives are that percetage by weight is 5%
Polyvinyl alcohol water solution；
Prepare coating material by the component of following parts by weight：20 parts of carbon source, 35 parts of silicon source, 5 parts of dispersant；Carbon source is lignin,
Silicon source is the Ludox that silica weight percentage is 60%, and dispersant is odium stearate；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 20 minutes under medium, dry after wet-milling and mixed powder are made；The weight of absolute ethyl alcohol be schmigel, graphite powder, land plaster,
1 times of white mica powder and talcum powder gross weight；The rotating speed of wet-milling is 400rpm；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 2.5MPa, earthenware is made
Crucible green compact；Compression molding is completed on a vibration table, and shake table amplitude is 4.5mm, and vibration frequency is 80 times/min；
e）Crucible is sintered：Crucible green compact are risen to 55 DEG C and be incubated 1 hour dumping by room temperature and arrange carbon；Temperature is continued afterwards to rise to
1350 DEG C, and be incubated 4 hours and sinter, room temperature is naturally cooling to after the completion of sintering, and high-temperature crucible crude product is made；Dumping arranges carbon rank
Heating rate of the heating rate control after 1 DEG C/min, dumping row's carbon stage before section is controlled in 3 DEG C/min
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
200rpm rotating speeds are stirred 5 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：Then face coat high-temperature crucible crude product was cooled down by room temperature to insulation in 1400 DEG C 2 hours
To room temperature, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment；
After the completion of above-mentioned steps, by obtained face coat high-temperature crucible at 550 DEG C and be incubated 1 hour.
Embodiment 2
A kind of preparation method of face coat high-temperature crucible, comprises the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content is 99~99.5wt% 100 parts of schmigel, 0.05 part of crystalline graphite powder, 0.8 part of sericite, talcum powder
0.5 part, 1.5 parts of pelletizing additives；15wt% is coarse grain footpath schmigel in schmigel, and 55wt% is middle particle diameter schmigel, and 30wt% is
Fine grain schmigel；The particle diameter of coarse grain footpath schmigel is 250~350 mesh, and the particle diameter of middle particle diameter schmigel is 800~1000 mesh,
The particle diameter of fine grain schmigel is 1300~1400 mesh；The median particle diameter D of coarse grain footpath schmigel50For 300 mesh, middle particle diameter schmigel
Median particle diameter D50For 900 mesh, the median particle diameter D of fine grain schmigel50For 1350 mesh；Pelletizing additives are percetage by weight
For 5% polyvinyl alcohol water solution；
Prepare coating material by the component of following parts by weight：25 parts of carbon source, 40 parts of silicon source, 6 parts of dispersant；Carbon source is starch, silicon
Source is the Ludox that silica weight percentage is 65%, and dispersant is odium stearate；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 25 minutes under medium, dry after wet-milling and mixed powder are made；The weight of absolute ethyl alcohol be schmigel, graphite powder, land plaster,
1.2 times of white mica powder and talcum powder gross weight；The rotating speed of wet-milling is 450rpm；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 10MPa, earthenware is made
Crucible green compact；Compression molding is completed on a vibration table, and shake table amplitude is 5mm, and vibration frequency is 85 times/min；
e）Crucible is sintered：Crucible green compact are risen to 550 DEG C and be incubated 1 hour dumping by room temperature and arrange carbon；Temperature is continued afterwards to rise
To 1400 DEG C, and insulation is sintered for 5 hours, is naturally cooling to room temperature after the completion of sintering, high-temperature crucible crude product is made；Dumping arranges carbon
Heating rate of the heating rate control after 2 DEG C/min, dumping row's carbon stage before stage is controlled in 4 DEG C/min
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
300rpm rotating speeds are stirred 10 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：By face coat high-temperature crucible crude product by room temperature to insulation in 1450 DEG C 2.5 hours, Ran Houleng
But to room temperature, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment；
After the completion of above-mentioned steps, by obtained face coat high-temperature crucible at 550 DEG C and be incubated 1.5 hours.
Embodiment 3
A kind of preparation method of face coat high-temperature crucible, comprises the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content is 99~99.5wt% 100 parts of schmigel, 0.10 part of crystalline graphite powder, 0.3 part of sericite, talcum powder
0.5 part, 1.8 parts of pelletizing additives；18wt% is coarse grain footpath schmigel in schmigel, and 52wt% is middle particle diameter schmigel, and 30wt% is
Fine grain schmigel；The particle diameter of coarse grain footpath schmigel is 250~350 mesh, and the particle diameter of middle particle diameter schmigel is 700~900 mesh, carefully
The particle diameter of particle diameter schmigel is 1300~1400 mesh；The median particle diameter D of coarse grain footpath schmigel50For 300 mesh, middle particle diameter schmigel
Median particle diameter D50For 800 mesh, the median particle diameter D of fine grain schmigel50For 1350 mesh；Pelletizing additives are that percetage by weight is
5% polyvinyl alcohol water solution；
Prepare coating material by the component of following parts by weight：30 parts of carbon source, 45 parts of silicon source, 7 parts of dispersant；Carbon source is sucrose, silicon
Source is the Ludox that silica weight percentage is 65%, and dispersant is sodium carboxymethylcellulose；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 35 minutes under medium, dry after wet-milling and mixed powder are made；The weight of absolute ethyl alcohol be schmigel, graphite powder, land plaster,
1.3 times of white mica powder and talcum powder gross weight；The rotating speed of wet-milling is 550rpm；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 20MPa, earthenware is made
Crucible green compact；Compression molding is completed on a vibration table, and shake table amplitude is 5mm, and vibration frequency is 85 times/min；
e）Crucible is sintered：Crucible green compact are risen to 600 DEG C and be incubated 1.5 hours dumpings by room temperature and arrange carbon；Temperature is continued afterwards
1400 DEG C are risen to, and is incubated 5 hours and is sintered, room temperature is naturally cooling to after the completion of sintering, high-temperature crucible crude product is made；Dumping is arranged
Heating rate of the heating rate control after 2 DEG C/min, dumping row's carbon stage before the carbon stage is controlled in 4 DEG C/min
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
500rpm rotating speeds are stirred 10 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：By face coat high-temperature crucible crude product by room temperature to insulation in 1550 DEG C 2.5 hours, Ran Houleng
But to room temperature, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment；
After the completion of above-mentioned steps, by obtained face coat high-temperature crucible at 600 DEG C and be incubated 1.5 hours.
Embodiment 4
A kind of preparation method of face coat high-temperature crucible, comprises the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content is 99.5wt% 100 parts of schmigel, 0.15 part of crystalline graphite powder, 0.8 part of sericite, talcum powder 0.5
Part, 2.0 parts of pelletizing additives；20wt% is coarse grain footpath schmigel in schmigel, and 55wt% is middle particle diameter schmigel, and 25wt% is thin
Particle diameter schmigel；The particle diameter of coarse grain footpath schmigel is 250~350 mesh, and the particle diameter of middle particle diameter schmigel is 700~1000 mesh, carefully
The particle diameter of particle diameter schmigel is 1200~1500 mesh；The median particle diameter D of coarse grain footpath schmigel50For 300 mesh, middle particle diameter schmigel
Median particle diameter D50For 900 mesh, the median particle diameter D of fine grain schmigel50For 1400 mesh；Pelletizing additives are that percetage by weight is
5% polyvinyl alcohol water solution；
Prepare coating material by the component of following parts by weight：35 parts of carbon source, 47 parts of silicon source, 8 parts of dispersant；Carbon source is alginic acid
Sodium, silicon source is the Ludox that silica weight percentage is 70%, and dispersant is sodium carboxymethylcellulose；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 40 minutes under medium, dry after wet-milling and mixed powder are made；The weight of absolute ethyl alcohol be schmigel, graphite powder, land plaster,
1.5 times of white mica powder and talcum powder gross weight；The rotating speed of wet-milling is 600rpm；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 30MPa, earthenware is made
Crucible green compact；Compression molding is completed on a vibration table, and shake table amplitude is 5.5mm, and vibration frequency is 90 times/min；
e）Crucible is sintered：Crucible green compact are risen to 600 DEG C and be incubated 1.5 hours dumpings by room temperature and arrange carbon；Temperature is continued afterwards
1450 DEG C are risen to, and is incubated 6 hours and is sintered, room temperature is naturally cooling to after the completion of sintering, high-temperature crucible crude product is made；Dumping is arranged
Heating rate of the heating rate control after 3 DEG C/min, dumping row's carbon stage before the carbon stage is controlled in 5 DEG C/min
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
600rpm rotating speeds are stirred 15 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：Then face coat high-temperature crucible crude product was cooled down by room temperature to insulation in 1600 DEG C 3 hours
To room temperature, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment；
After the completion of above-mentioned steps, by obtained face coat high-temperature crucible at 600 DEG C and be incubated 1.5 hours.
Performance test：
1. compression molding yields：
After the completion of shaping count molding blank yields, wherein base substrate rupture, it is imperfect be considered as unqualified base substrate, through statistics
Be molded yields 96% and more than, and in the existing powder forming process of identical size, yields can barely reach that 90% is left
It is right；
2. the consistency of high-temperature crucible after sintering：
The bulk density of finished product is calculated by the dry weight, weightlessness, buoyant weight of testing finished product respectively, and obtained with raw material weighted average calculation
To solid density compare acquisition consistency, after tested the consistency of the finished product in above-described embodiment be 97% and more than, and show
The consistency for having structural ceramics in technology is 95% or so；
3. the refractoriness under load test of finished product：
The high temperature resistant being prepared according to the load softening point method of testing described in GB/T 5989-2008 to above-described embodiment
Crucible carries out load softening point test, after testing under the conditions of 0.2MPa, the high-temperature crucible that the various embodiments described above are prepared
Refractoriness under load be not less than 1800 DEG C.
It should be appreciated that to those skilled in the art, can according to the above description be improved or be become
Change, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (8)
1. a kind of preparation method of face coat high-temperature crucible, it is characterised in that comprise the following steps：
a）Get the raw materials ready：
Prepare raw material for crucible by the component of following parts by weight：
Alumina content be 99~99.5wt% 100 parts of schmigel, 0.05~0.15 part of crystalline graphite powder, sericite 0.3~
0.8 part, 0.3~0.5 part of talcum powder, 1.5~2.0 parts of pelletizing additives；
Prepare coating material by the component of following parts by weight：20~35 parts of carbon source, 35~47 parts of silicon source, 5~8 parts of dispersant；
b）Raw material for crucible batch mixing：Schmigel, graphite powder, land plaster, white mica powder and talcum powder are mixed and are in absolute ethyl alcohol
Wet-milling 20~40 minutes under medium, dry after wet-milling and mixed powder are made；
c）Mixed powder is granulated：Pelletizing additives are added into mixed powder and are well mixed；
d）Crucible is molded：The mixed powder granulated is added to compression molding in mould, briquetting pressure is 2.5~30MPa, system
Obtain crucible green compact；
e）Crucible is sintered：Crucible green compact are risen to 550~600 DEG C and be incubated 1~1.5 hour dumping by room temperature and arrange carbon；Afterwards will
Temperature continues to rise to 1350~1450 DEG C, and insulation is sintered for 4~6 hours, is naturally cooling to room temperature after the completion of sintering, resistance to height is made
Warm crucible crude product；
f）It is prepared by coating paste：Dispersant is added in silicon source and stirred, carbon source is then added thereto again, and with
200~600rpm rotating speeds are stirred 5~15 minutes, and coating paste is made；
g）Coating：By in high-temperature crucible crude product immersion coating slurry, after slurry is completely covered after high-temperature crucible crude product surface
Take out and dry, face coat high-temperature crucible crude product is made；
h）Coating is sintered：Face coat high-temperature crucible crude product is small to insulation 2~3 in 1400~1600 DEG C by room temperature
When, room temperature is subsequently cooled to, face coat high-temperature crucible is made；Coating sintering process is carried out in a nitrogen environment.
2. a kind of preparation method of face coat high-temperature crucible according to claim 1, it is characterised in that：
In the raw material for crucible, 15~20wt% is coarse grain footpath schmigel in schmigel, and 45~55wt% is middle particle diameter schmigel, remaining
Measure as fine grain schmigel；Pelletizing additives are the polyvinyl alcohol water solution that percetage by weight is 5%.
3. a kind of preparation method of face coat high-temperature crucible according to claim 2, it is characterised in that：
In the raw material for crucible, the particle diameter of coarse grain footpath schmigel is 250~350 mesh, the particle diameter of middle particle diameter schmigel for 700~
1000 mesh, the particle diameter of fine grain schmigel is 1200~1500 mesh；The median particle diameter D of coarse grain footpath schmigel50For 290~300 mesh,
The median particle diameter D of middle particle diameter schmigel50For 800~900 mesh, the median particle diameter D of fine grain schmigel50For 1350~1400 mesh.
4. a kind of preparation method of face coat high-temperature crucible according to claim 1, it is characterised in that：
In the coating material, carbon source is one kind in lignin, starch, sucrose or sodium alginate, and silicon source is silica weight
The Ludox that percentage is 60~70% is measured, dispersant is odium stearate or sodium carboxymethylcellulose.
5. a kind of preparation method of face coat high-temperature crucible according to claim 1, it is characterised in that：
In the step b mixing process, the weight of absolute ethyl alcohol is schmigel, graphite powder, land plaster, white mica powder and talcum powder
1~1.5 times of gross weight；The rotating speed of wet-milling is 400~600rpm.
6. a kind of preparation method of face coat high-temperature crucible according to claim 1, it is characterised in that：
Molding process is completed on a vibration table in the step d, and shake table amplitude is 4.5~5.5mm, and vibration frequency is 80~90
Secondary/min.
7. a kind of preparation method of face coat high-temperature crucible according to claim 1, it is characterised in that：
In the step e, heating of the heating rate control after 1~3 DEG C/min, dumping row's carbon stage before dumping row's carbon stage
Speed control is in 3~5 DEG C/min.
8. a kind of preparation method of face coat high-temperature crucible according to claim 1 or 7, it is characterised in that：
After the completion of the step h, by obtained face coat high-temperature crucible at 550~600 DEG C and be incubated 1~1.5 hour.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997000A (en) * | 2018-08-31 | 2018-12-14 | 青岛中冶坩埚有限公司 | A kind of high-temperature crucible and its manufacturing method |
| CN109183147A (en) * | 2018-11-16 | 2019-01-11 | 晶科能源有限公司 | A kind of preparation method and crucible of polycrystalline cast ingot crucible coating layer |
| CN112176289A (en) * | 2020-09-22 | 2021-01-05 | 中国建材国际工程集团有限公司 | Crucible boat for cadmium telluride/cadmium sulfide/cadmium selenide film deposition and preparation method thereof |
| CN112694347A (en) * | 2020-12-28 | 2021-04-23 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11292615A (en) * | 1998-04-16 | 1999-10-26 | Nippon Crucible Co Ltd | Crucible for melted metal and its production |
| CN102490253A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Forming method and forming mold for alumina ceramic crucible |
| CN202643896U (en) * | 2012-05-26 | 2013-01-02 | 保定顺天新材料股份有限公司 | Crucible made of carbon/carbon composite material |
-
2017
- 2017-06-05 CN CN201710415275.5A patent/CN107244905A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11292615A (en) * | 1998-04-16 | 1999-10-26 | Nippon Crucible Co Ltd | Crucible for melted metal and its production |
| CN102490253A (en) * | 2011-11-22 | 2012-06-13 | 中国铝业股份有限公司 | Forming method and forming mold for alumina ceramic crucible |
| CN202643896U (en) * | 2012-05-26 | 2013-01-02 | 保定顺天新材料股份有限公司 | Crucible made of carbon/carbon composite material |
Non-Patent Citations (2)
| Title |
|---|
| 林宗寿主编: "《无机非金属材料工学 第4版》", 31 December 2013, 武汉理工大学出版社 * |
| 王成彪等: "《摩擦学材料及表面工程》", 29 February 2012, 国防工业出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997000A (en) * | 2018-08-31 | 2018-12-14 | 青岛中冶坩埚有限公司 | A kind of high-temperature crucible and its manufacturing method |
| CN109183147A (en) * | 2018-11-16 | 2019-01-11 | 晶科能源有限公司 | A kind of preparation method and crucible of polycrystalline cast ingot crucible coating layer |
| CN109183147B (en) * | 2018-11-16 | 2021-01-08 | 晶科能源有限公司 | Preparation method of crucible coating for polycrystalline ingot casting and crucible |
| CN112176289A (en) * | 2020-09-22 | 2021-01-05 | 中国建材国际工程集团有限公司 | Crucible boat for cadmium telluride/cadmium sulfide/cadmium selenide film deposition and preparation method thereof |
| CN112694347A (en) * | 2020-12-28 | 2021-04-23 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
| CN112694347B (en) * | 2020-12-28 | 2022-06-07 | 湖南世鑫新材料有限公司 | Carbon-carbon composite material crucible with silicon carbide coating and preparation method |
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