CN109928781A - It is a kind of for controlling the graphene ceramic film preparation method in Jinsui River mouthful - Google Patents
It is a kind of for controlling the graphene ceramic film preparation method in Jinsui River mouthful Download PDFInfo
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Abstract
The present invention provides a kind of for controlling the preparation method of the graphene ceramic membrane in Jinsui River mouthful, the following steps are included: (1) prepares heat-conducting layer first: graphite composite powder, graphene powder, binder being mixed, are evenly applied on the working surface of long nozzle or submersed nozzle；(2) then ceramic film protection layer is prepared: by Al2O3、SiN4, TiC, WC, binder, lubricant, dispersing agent, water is applied to after mixing on the heat-conducting layer that step (1) is prepared；(3) low temperature calcination；(4) high-temperature calcination.The present invention utilizes the high thermal conductivity ability of graphite and graphene, by the thermal shock rapid dispersion of molten steel in entire long nozzle or submersed nozzle ontology, avoid the heat accumulation of mouth of a river regional area, so that each position in the mouth of a river is able to maintain the stable and firm of internal structure, no weakness zone occurs, to improve the working time at the mouth of a river on the whole.
Description
Technical field
The present invention relates to functional refractory technical fields, more particularly, to a kind of graphene ceramics for controlling Jinsui River mouthful
The preparation method of film.
Background technique
The functionality such as integral column of sagger, long nozzle (big packet long nozzle), submersed nozzle (middle packet institute water nozzle), middle water-coating port
Refractory component is referred to as continuous-casting three-main-product.Its material mainly has aluminium carbonaceous, aluminium zirconium carbonaceous, magnesium carbonaceous or magnesium aluminate spinel carbonaceous,
Forming method uses isostatic pressing.
Wherein, long nozzle refers to when molten steel is from ladle to when basket pouring, in order to avoid aoxidizing and splashing, in Ladle Bottom
Long nozzle is installed in the lower end of the slide gate nozzle in portion, and one end is connected with collector nozzle, and it is close that the other end is inserted into progress in the molten steel of tundish
Seal molding casting.Its effect of long nozzle is as follows: (1) preventing secondary oxidation of steel, improve the quality of steel；(2) easy oxygen in steel is reduced
The oxidation product for changing element is deposited in mouth of a river inner wall, is prolonged its service life；(3) long nozzle is used multiple times, and reduces fire proofed wood
Material consumption.
Long nozzle should have following performance: (1) excellent thermal shock resistance；(2) energy of good mechanical performance and anti-vibration
Power；(3) aggressivity of anti-molten steel and slag is good；(4) side, which meets place, must have air seal set.The material of long nozzle generally has melting
Quartziferous and aluminium carbonaceous two major classes.
In continuous casting technology, to improve slab quality, submersed nozzle is equipped between tundish and crystallizer, it is main
Effect is: (1) preventing the splashing of secondary oxidation of steel nitridation and molten steel；(2) MOLTEN STEEL FLOW state and injection rate are adjusted；(3)
It prevents covering slag non-metallic inclusion to be involved in molten steel, plays an important role to the floating for promoting inclusion content in melting steel；(4) opposite side is cast
Throwing lumber recovery and slab quality have decisive influence.
From foregoing description, it can be seen that, long nozzle and submersed nozzle require to be subjected to high temperature impact, this high temperature impact
And it is non-generic be immersed in high-temperature molten steel, but molten steel in flow process can to the mouth of a river generate impact force, so the mouth of a river only
It is also far from enough with high temperature resistance, it is also necessary to which that there is thermal shock resistance.Since working environment is severe, longevity of long nozzle at present
Life generally 10 hours, the service life of submersed nozzle was generally 8~10 hours.Domestic price be long nozzle 1.8~2.9 ten thousand/only,
Submersed nozzle 2.2~2.3 ten thousand/only；The price of imported product be long nozzle 3.0~3.5 ten thousand/only, submersed nozzle 2.5~
2.6 ten thousand/only.High cost and it is of short duration use the time that researcher is made to be continuously improved mouth of a river material, used with improving
Performance reduces cost.
At present for long nozzle and submersed nozzle improvement there are two direction, one of them is to improve two kinds of mouths of a river itself
Material, make it have higher intensity, preferable thermal shock resistance, high corrosion resistance and long-life, another direction be
Anti-oxidant, heat-resisting paint is coated outside two kinds of mouths of a river, so that it is formed fine and close glaze layer in hot operation, to protect mouth of a river sheet
Body.
CN106631053A provides a kind of converter taphole refractory material and preparation method thereof, in magnesia carbon brick body surface
One layer of glaze slip is sprayed, the coating layer thickness of the glaze slip is 1~2mm, it is 12~24 hours dry under the conditions of 110 DEG C, it is warming up to 240
DEG C, 24 hours are kept the temperature, converter taphole refractory material is made.The raw material and its content of the glaze slip are: glass powder be 40~
65wt%, spodumene be 5~25wt%, potassium feldspar be 10~20wt%, silicon powder be 2~8wt%, potassium carbonate be 1~
3wt%, SiC fine powder are 3~10wt%, and chrome green is 1~3wt%, and aluminium dihydrogen phosphate is 1~3wt%.
The glaze slip coating starts to soften and seal magnesia carbon brick body surface major part stomata at 900 DEG C or so, can be substantially
Reduce oxidation of the magnesia carbon brick ontology before tapping；As the temperature rises, the liquid phase in glaze slip coating is toward magnesia carbon brick body interior
Infiltration continues to protect the carbon in magnesia carbon brick ontology not oxidized；SiO in glaze slip coating at the same time2、Cr2O3Etc. components and magnesium
Sand fine powder reacts, and increases the surface strength of magnesia carbon brick ontology, not only increases the globality of magnesia carbon brick ontology, and promoted
The anti-molten steel scouring capability of magnesia carbon brick ontology.
CN102424593A provides a kind of oxidation resistance coating material for continuous casting function fire resistance material, with potassium feldspar for basic object
Material；Potassium feldspar melting temperature section is wider, is suitble to firing glaze；Acidic fluxing agent B is introduced using borax2O3And alkali flux
Na2O；Al is deployed with pyrophyllite, silica2O3And SiO2Content；Dispersing agent is done using sodium tripolyphosphate, coating material can be stablized
Slurry, and can generate micro- stomata during heat treatment, avoid drawing volatilizing with resinoid bond in refractory material sintering process
The phenomenon that playing peeling, being bubbled.
For the technology after carbon containing refractory molding, coating antioxidizing paint is put into drying after natural drying 2 hours
In 80 DEG C~110 DEG C slowly drying in room, it is reloaded into firing in kiln, is burnt into 4 hours in 1050 DEG C~1300 DEG C air atmospheres,
Inoxidzable coating is obtained on carbon containing refractory surface；Provided antioxidizing paint is in loose porous knot after coating drying
Structure, the cold stage of sintering process, bonding agent volatile matter can be distributed by coating porosity；The glaze viscosity that high temperature is formed at the glaze stage
It is low, be conducive to the volatilization of refractory material internal gas, it is good at glaze spreadability., non-scale, no good with green body caking property after coating drying
It cracks, is not bubbled in sintering process, it is flat and smooth at glaze.
Above two scheme is all to lay one layer of smooth, closely knit glaze layer in mouth of a river body surface, is equivalent to and strengthens water
Mouth ontology, extends the heat shock resistance time of ontology, there is no the innovations in terms of heat shock resistance principle, therefore also can not be to the mouth of a river
Working life carry out significant effective improve.
Summary of the invention
In view of the above-mentioned problems existing in the prior art, this application provides a kind of for controlling the graphene ceramic membrane in Jinsui River mouthful
Preparation method.The present invention utilizes the high thermal conductivity ability of graphite and graphene, by the thermal shock rapid dispersion of molten steel in entire long water
Mouth or submersed nozzle ontology, avoid the heat accumulation of mouth of a river regional area, so that each position in the mouth of a river is able to maintain internal junction
Stable and firm, the no weakness zone appearance, to improve the working time at the mouth of a river on the whole of structure.
Technical scheme is as follows:
It is a kind of for controlling the preparation method of the graphene ceramic membrane in Jinsui River mouthful, comprising the following steps:
(1) prepare heat-conducting layer first: by graphite composite powder, graphene powder, binder according to mass ratio be 1:0.03~
0.08:0.1~0.2 is mixed, and 1.5~3 times of the water that quality is the sum of three is then added, will be owned using ultrasonic disperser
Raw material is dispersed in water, is then evenly applied on the working surface of long nozzle or submersed nozzle, coating thickness 20
~50 microns；It is dried after coating at 150~180 DEG C；
(2) then ceramic film protection layer is prepared: by Al2O3: 40~50 parts；SiN4: 7~10 parts；TiC:3~5 part；WC:3
~5 parts；Binder: 5~10 parts；Lubricant: 1~3 part；Dispersing agent: 1~3 part；Water: 25~30 parts are applied to after mixing
On the heat-conducting layer that step (1) is prepared；Above-mentioned number is mass fraction；
(3) low temperature calcination: the mouth of a river for being coated with heat-conducting layer and ceramic film protection layer is forged under conditions of vacuumizing
It burns, excludes two layers of additive and impurity；520~580 DEG C of calcination temperature, calcination time 30~50 minutes；
(4) high-temperature calcination: after low temperature calcination, continue to be heated to 1150~1180 DEG C, kept for 10~20 minutes, make to make pottery
Porcelain film protective layer is tentatively changed into air-locked glaze layer, then cooled to room temperature.
Preferably, the graphite composite powder, graphene powder cross 200~400 meshes respectively before mixing.
Preferably, the partial size of each solid material of the ceramic film protection layer is 3~8 microns.
Preferably, the binder is methylcellulose or hydroxypropyl methyl cellulose.
Preferably, the lubricant is atoleine or corn oil.
Preferably, the dispersing agent includes triethanolamine, tbp, terpinol, stearic acid, polyethylene glycol or poly-
Propylene.
The present invention is beneficial to be had the technical effect that
The applicant has found that molten steel is an impact to long nozzle and washing away for submersed nozzle in long-term practice, rather than
Face impact.Some position for all putting forth effort on the mouth of a river, such as slag lining are washed away in point impact every time, rather than the entire mouth of a river is rushed
Brush.This allows for that mouth of a river uneven heating is even, and the number that some positions are washed away is more frequent, and the internal structure at the position is easier
Occur to destroy and be broken, is scrapped so as to cause the entire mouth of a river.
Therefore, the present invention got around it is conventional lay one layer of smooth, closely knit glaze layer in mouth of a river body surface, thus plus
Gu, thicken mouth of a river ontology thinking, but use mouth of a river ontology coat one layer of graphene composite material, it is strong by graphene
It is whole to be quickly transmitted to the mouth of a river by the big capacity of heat transmission (thermal coefficient is up to 5300W/mK) for the thermal shock that some position of the mouth of a river is subject to
On body, disperse the heat accumulation of the part.This thinking, which is equivalent to, alleviates the thermal shock that the position is subject to, and keeps its internal structure long
Time keeps firm orderly, and so the service life of mouth of a river entirety also can significantly extend.
Since oxidizing temperature of the graphene in oxygen only has 500 DEG C, also there was only 1000 DEG C in argon gas, is far below molten steel
Temperature, it is therefore desirable to coat layer of ceramic film protective layer outside graphene layer, for completely cutting off gas, maintain graphene itself
Architectural characteristic.Graphene is easy denaturation at high temperature, generates a large amount of active groups, so with the extension of working time, graphite
The heating conduction of alkene can be gradually reduced.It, can be by the mouth of a river after the present invention is coated with graphene layer and protective film on mouth of a river surface
Working time extends 6~7 hours.
The price of graphene is very expensive, in order to reduce cost, it is necessary to use graphite as the basic material of thermally conductive film layer.Stone
The fusing point of ink is 3850 ± 50 DEG C, and boiling point is 4250 DEG C, though through superhigh temperature electric arc calcination, the loss very little of weight, thermal expansion
Coefficient also very little.And the electric conductivity of graphite is 100 times higher than general nonmetallic ore, and thermal conductivity is more than the metal materials such as steel, iron, lead
Material, is the ideal material of heat-conducting layer.
The thickness of graphene layer (i.e. heat-conducting layer) and ceramic film protection layer is restricted；Theoretically, the bigger guarantor of thickness
Shield ability is stronger, it is contemplated that molten steel can generate when impacting the mouth of a river is parallel to mouth of a river surface and the mechanics perpendicular to mouth of a river surface
Vector, there is the effect of removing mouth of a river superficial film, and thickness gets over great Rong and is easy to be stripped；And protective film layer is ceramic membrane, is led
Hot coefficient is small, heat transfer that is more thick more stopping graphene；So must be by thickness control in most reasonable range.In addition, raw material
Selection and dosage allotment need to optimize by many experiments；Such as protective film layer raw material selection also to consider it is thermally conductive
Property, leakproofness and permeability.Leakproofness is stronger, and the working time of graphene is more long；The strong raw material of permeability can then destroy stone
The thermal conductivity of black alkene.
Specific embodiment
Below with reference to embodiment and comparative example, the present invention is specifically described.Following long nozzle ontologies are safe using Jiangsu
The big packet long nozzle of auspicious fire resisting Co., Ltd, using raw materials such as high-quality crystalline flake graphite, electrofused mullites through super-pressure isostatic cool pressing
Molding is 10 hours or so using the time；Submersed nozzle ontology use the said firm using aluminium oxide as primary raw material, through super-pressure
The submersed nozzle of cold isostatic compaction is 8 hours using the time.
Embodiment 1
The preparation method of graphene ceramic membrane provided in this embodiment for long nozzle the following steps are included:
(1) heat-conducting layer is prepared first: being according to mass ratio by graphite composite powder, graphene powder, binder methylcellulose
Then 1.5 times of the water that quality is the sum of three is added in 1:0.03:0.1 mixing, using ultrasonic disperser that all raw materials are equal
It is even to be dispersed in water, it is then evenly applied on the working surface of long nozzle, coating thickness is 50 microns；At 180 DEG C after coating
Drying；The graphite composite powder, graphene powder are commercially available technical grade product, cross 200 meshes respectively before mixing.
(2) then ceramic film protection layer is prepared: by Al2O3: 40 parts；SiN4: 7 parts；TiC:3 parts；WC:3 parts；Binder first
Base cellulose: 5 parts；Lubricant corn oil: 1 part；Dispersing agent triethanolamine: 1 part；Water: 25 parts are applied to step after mixing
(1) on the heat-conducting layer being prepared；Each raw material of the ceramic film protection layer is commercially available technical grade product, wherein each solid is former
The partial size of material is 3~8 microns.
(3) low temperature calcination: the mouth of a river for being coated with heat-conducting layer and ceramic film protection layer is forged under conditions of vacuumizing
It burns, excludes two layers of additive and impurity；520 DEG C of calcination temperature, calcination time 50 minutes；
(4) high-temperature calcination: after low temperature calcination, continue to be heated to 1150 DEG C, kept for 20 minutes, make ceramic film protection layer
Tentatively it is changed into air-locked glaze layer, then cooled to room temperature.
Embodiment 2
The preparation method of graphene ceramic membrane provided in this embodiment for long nozzle the following steps are included:
(1) heat-conducting layer is prepared first: by graphite composite powder, graphene powder, binder hydroxypropyl methyl cellulose according to matter
Then amount is added 2 times of the water that quality is the sum of three, will be owned using ultrasonic disperser than being that 1:0.05:0.15 is mixed
Raw material is dispersed in water, is then evenly applied on the working surface of long nozzle, and coating thickness is 20 microns；After coating
150 DEG C of drying；The graphite composite powder, graphene powder are commercially available technical grade product, cross 400 meshes respectively before mixing.
(2) then ceramic film protection layer is prepared: by Al2O3: 45 parts；SiN4: 8 parts；TiC:4 parts；WC:4 parts；Binder hydroxyl
Propyl methocel: 7 parts；Lubricating fluid paraffin: 2 parts；Dispersing agent polypropylene: 2 parts；Water: 28 parts are smeared after mixing
In on the heat-conducting layer that step (1) is prepared；Each raw material of the ceramic film protection layer is commercially available technical grade product, wherein respectively
The partial size of solid material is 3~8 microns.
(3) low temperature calcination: the mouth of a river for being coated with heat-conducting layer and ceramic film protection layer is forged under conditions of vacuumizing
It burns, excludes two layers of additive and impurity；560 DEG C of calcination temperature, calcination time 50 minutes；
(4) high-temperature calcination: after low temperature calcination, continue to be heated to 1160 DEG C, kept for 10 minutes, make ceramic film protection layer
Tentatively it is changed into air-locked glaze layer, then cooled to room temperature.
Embodiment 3
The preparation method of graphene ceramic membrane provided in this embodiment for submersed nozzle the following steps are included:
(1) heat-conducting layer is prepared first: by graphite composite powder, graphene powder, binder hydroxypropyl methyl cellulose according to matter
Then 3 times of the water that quality is the sum of three is added than being that 1:0.08:0.2 is mixed in amount, using ultrasonic disperser by all originals
Material is dispersed in water, is then evenly applied on the working surface of submersed nozzle, and coating thickness is 30 microns；After coating
It is dried at 160 DEG C；The graphite composite powder, graphene powder are commercially available technical grade product, cross 300 meshes respectively before mixing.
(2) then ceramic film protection layer is prepared: by Al2O3: 50 parts；SiN4: 10 parts；TiC:5 parts；WC:5 parts；Binder hydroxyl
Propyl methocel: 10 parts；Lubricating fluid paraffin: 3 parts；Dispersing agent polyethylene glycol: 3 parts；Water: 30 parts apply after mixing
It smears on the heat-conducting layer that step (1) is prepared；Each raw material of the ceramic film protection layer is commercially available technical grade product, wherein
The partial size of each solid material is 3~8 microns.
(3) low temperature calcination: the mouth of a river for being coated with heat-conducting layer and ceramic film protection layer is forged under conditions of vacuumizing
It burns, excludes two layers of additive and impurity；580 DEG C of calcination temperature, calcination time 40 minutes；
(4) high-temperature calcination: after low temperature calcination, continue to be heated to 1180 DEG C, kept for 15 minutes, make ceramic film protection layer
Tentatively it is changed into air-locked glaze layer, then cooled to room temperature.
Comparative example 1: the TiC in embodiment 1 is changed to ZrO2, other raw materials and preparation method are constant.
Comparative example 2: the WC in embodiment 2 is changed to TiC, that is, the dosage of TiC is 8 parts, does not use WC, other raw materials
It is constant with preparation method.
Comparative example 3: by the SiN in embodiment 34It is changed to Al2O3, that is, Al2O3Dosage be 60 parts, do not use SiN4,
Other raw materials and preparation method are constant.
Comparative example 4: according to 3 step of embodiment (2)~(4) method only on the mouth of a river coated ceramic film, do not apply heat-conducting layer.
The product that embodiment and comparative example is prepared carries out working time test, and the results are shown in Table 1.
Table 1 (unit: hour)
As can be seen from Table 1, the dosage of graphene is higher, and heating conduction is better, longer to the guard time at the mouth of a river；But
It is expensive in view of graphene, it is therefore necessary to take into account performance and cost, dosage is selected according to company actual situation.From comparison
From the point of view of the data of example, the strong TiC of thermal conductivity is changed to the ZrO of high rigidity2, the thermal conductivity of protective layer can be reduced, graphene is influenced
The effect of uniform mouth of a river temperature；Although TiC and WC are highly heat-conductive materials, respective performance is had any different, and cannot be substituted mutually；
Service life of ceramic membrane can be significantly reduced by lacking high-hardness ceramic raw material；If being not coated by heat-conducting layer, coated ceramic film protective layer,
The protecting effect at the mouth of a river can be also greatly reduced.
In addition, other raw materials of the invention and preparation technology parameter are modified or adjusted, it can be to last water
The mouth service life has an impact, and no longer enumerates one by one here, and through applicant, experimental results demonstrate raw material provided herein forms tool
There is optimal extension mouth of a river service life effect, and impurity will not be brought to molten steel.
Claims (7)
1. a kind of for controlling the preparation method of the graphene ceramic membrane in Jinsui River mouthful, it is characterised in that the following steps are included:
(1) prepare heat-conducting layer first: by graphite composite powder, graphene powder, binder according to mass ratio be 1:0.03~0.08:
Then 1.5~3 times of the water that quality is the sum of three is added in 0.1~0.2 mixing, using ultrasonic disperser by all raw materials
It is dispersed in water, is then evenly applied on the working surface of long nozzle or submersed nozzle, coating thickness is 20~50
Micron；It is dried after coating at 150~180 DEG C；
(2) then ceramic film protection layer is prepared: by Al2O3: 40~50 parts；SiN4: 7~10 parts；TiC:3~5 part；WC:3~5
Part；Binder: 5~10 parts；Lubricant: 1~3 part；Dispersing agent: 1~3 part；Water: 25~30 parts are applied to step after mixing
(1) on the heat-conducting layer being prepared；
(3) low temperature calcination: calcining the mouth of a river for being coated with heat-conducting layer and ceramic film protection layer under conditions of vacuumizing, row
Except two layers of additive and impurity；520~580 DEG C of calcination temperature, calcination time 30~50 minutes；
(4) high-temperature calcination: after low temperature calcination, continue to be heated to 1150~1180 DEG C, kept for 10~20 minutes, make ceramic membrane
Protective layer is tentatively changed into air-locked glaze layer, then cooled to room temperature.
2. preparation method according to claim 1, it is characterised in that the graphite composite powder, graphene powder divide before mixing
200~400 meshes are not crossed.
3. preparation method according to claim 1, it is characterised in that the grain of each solid material of the ceramic film protection layer
Diameter is respectively 3~8 microns.
4. preparation method according to claim 1, it is characterised in that the binder is methylcellulose or hydroxypropyl first
Base cellulose.
5. preparation method according to claim 1, it is characterised in that the lubricant is atoleine or corn oil.
6. preparation method according to claim 1, it is characterised in that the dispersing agent includes triethanolamine, tricresyl phosphate fourth
Rouge, terpinol, stearic acid, polyethylene glycol or polypropylene.
7. preparation method according to claim 1, it is characterised in that the number is mass fraction.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85109111A (en) * | 1984-10-23 | 1986-08-27 | 日本坩埚株式会社 | The refractory materials that contains aluminium oxynitride, slide gate nozzle refractory materials and the continuous casting steel machine mouth of a river |
| JPS62158561A (en) * | 1986-01-06 | 1987-07-14 | Harima Refract Co Ltd | Nozzle for low-temperature casting of molten steel |
| CN1084150A (en) * | 1993-09-03 | 1994-03-23 | 中国科学院上海硅酸盐研究所 | The middle water containing opening silicon nitride combined with silicon carbide refractory material |
| CN104387093A (en) * | 2014-10-13 | 2015-03-04 | 瑞泰科技股份有限公司 | Flow controlling water gap for production of mineral wool from blast furnace slag and production process thereof |
-
2019
- 2019-02-20 CN CN201910124917.5A patent/CN109928781B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85109111A (en) * | 1984-10-23 | 1986-08-27 | 日本坩埚株式会社 | The refractory materials that contains aluminium oxynitride, slide gate nozzle refractory materials and the continuous casting steel machine mouth of a river |
| JPS62158561A (en) * | 1986-01-06 | 1987-07-14 | Harima Refract Co Ltd | Nozzle for low-temperature casting of molten steel |
| CN1084150A (en) * | 1993-09-03 | 1994-03-23 | 中国科学院上海硅酸盐研究所 | The middle water containing opening silicon nitride combined with silicon carbide refractory material |
| CN104387093A (en) * | 2014-10-13 | 2015-03-04 | 瑞泰科技股份有限公司 | Flow controlling water gap for production of mineral wool from blast furnace slag and production process thereof |
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