CN117682880A - Repairing agent and repairing method for graphite crucible - Google Patents

Repairing agent and repairing method for graphite crucible Download PDF

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Publication number
CN117682880A
CN117682880A CN202311718685.9A CN202311718685A CN117682880A CN 117682880 A CN117682880 A CN 117682880A CN 202311718685 A CN202311718685 A CN 202311718685A CN 117682880 A CN117682880 A CN 117682880A
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China
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graphite crucible
repairing
repairing agent
parts
damaged
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CN202311718685.9A
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Chinese (zh)
Inventor
杨九福
古波涛
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Miluo Fuyuan New Material Co ltd
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Miluo Fuyuan New Material Co ltd
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Priority to CN202311718685.9A priority Critical patent/CN117682880A/en
Publication of CN117682880A publication Critical patent/CN117682880A/en
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Abstract

The invention discloses a repairing agent and a repairing method for a graphite crucible, wherein the repairing agent is a two-component repairing agent and comprises an interface repairing agent and a surface layer repairing agent; the interface repairing agent is prepared from graphite powder, paraffin oil, asphalt powder, pyridine and SiC-Y 2 O 3 Preparing slurry as a raw material; the surface layer repairing agent is prepared from petroleum coke powder, graphite powder, asphalt powder and resin materials; the corresponding graphite crucible repairing method uses the repairing agent as a tool to repair the damaged area of the damaged graphite crucible, and when repairing, the damaged area of the damaged graphite crucible is coated by the interface repairing agent, after coating, the damaged area is covered by aluminum foil and wrapped by glass fiber mesh cloth for pre-curing treatment, and then the repairing operation of the graphite crucible is finally completed by using surface layer repairing paste. The repairing agent and the repairing method of the invention repair damaged graphiteThe crucible has a better repairing effect, and can be used for prolonging the service life of the damaged graphite crucible.

Description

Repairing agent and repairing method for graphite crucible
Technical Field
The invention relates to the technical field of graphite crucibles, in particular to a repairing agent and a repairing method for a graphite crucible.
Background
The graphite material has the excellent performances of small thermal expansion coefficient, high temperature resistance, electric conduction and heat conduction, stable chemical property, excellent high-temperature mechanical property and the like, and is widely applied to the high-temperature fields of aerospace, electronics, machinery and the like. The graphite crucible is a crucible which is fired based on graphite materials, has good thermal conductivity and high temperature resistance, has small thermal expansion coefficient in the high-temperature use process, has good resistance to rapid heating, quenching and acid-base environments, and is suitable for casting and molding of various different dies. Therefore, graphite crucibles are widely used for the smelting of alloy tool steels and the smelting of nonferrous metals and alloys thereof.
The graphite crucible is mainly two kinds in the actual use process, one kind is a knocked wound caused by external force knocks in the processes of charging, discharging, transferring and storing; in addition, graphite materials also have the own material defects that oxidation is easy to occur under the environment of high temperature and oxidizing atmosphere, and the higher the temperature is, the faster the oxidation rate is, and continuous use under the high temperature environment can lead to the strength reduction caused by oxidation inside the graphite materials, loose internal structures and further lead to the generation of cracks or breakage of the graphite crucible. Under the traditional technical conditions, the graphite crucible with cracks or breakage cannot be used continuously, is generally scrapped and is replenished with a new crucible, so that the use cost of the graphite crucible is high, and the graphite crucible has a considerable proportion in the production cost.
For the reasons mentioned above, to increase the number of times of use of the graphite crucible, repairing the crack or damage portion of the graphite crucible to recycle the graphite piece is an important means for increasing the life of the graphite crucible, and has a very important meaning for reducing the production cost. At present, a special graphite crucible repairing paste is mainly adopted for repairing a graphite crucible, is used as a special paste adhesive, is mainly prepared by taking graphite powder as a matrix and adding modified resin and other additives, has excellent high temperature resistance, binding force and chemical stability, and can provide effective repairing protection for the damaged part of the graphite crucible in high temperature, high pressure or corrosive environments, however, the existing graphite crucible repairing paste has the defect of low repairing strength generally, and the bonding property of the graphite crucible repairing paste and the graphite crucible is poor, collapse easily occurs on the surface after forming, so that the repairing effect is not ideal, the structural stability of the repairing position also has certain strength defect, and the repairing paste is easy to cause secondary damage very quickly after being used and influence the reuse.
Disclosure of Invention
The technical problem solved by the invention is to provide a repairing agent and a repairing method for a graphite crucible, which can be used for solving the defects in the technical background.
The invention firstly provides a repairing agent for a graphite crucible, which is a two-component repairing agent and comprises an interface repairing agent and a surface layer repairing agent;
the interface repairing agent comprises the following components in parts by mass:
graphite powder: 45-55 parts of paraffin oil: 10-15 parts of asphalt powder: 10-15 parts of pyridine: 3 to 5 parts of SiC-Y 2 O 3 Slurry: 2-3 parts;
wherein SiC-Y 2 O 3 The slurry consists of 25 to 35 parts of SiC and 2 to 5 parts of Y 2 O 3 30-40 parts of resin material is dissolved in 40-70 parts of organic solvent, and is obtained after ultrasonic dispersion and magnetic stirring are carried out uniformly;
the surface layer repairing agent comprises the following components in parts by mass:
petroleum coke powder: 35-45 parts of graphite powder: 15-20 parts of asphalt powder: 8-10 parts of resin material and 20-30 parts of solvent; the particle size of the petroleum coke powder is below 1mm, the mass ratio of the petroleum coke powder with the particle size below 0.6mm is 70-80%, and the mass ratio of the petroleum coke powder with the particle size below 0.2mm is 30-40%.
By way of further limitation, the SiC-Y 2 O 3 The resin material adopted in the slurry is phenolic resin or epoxy resin.
As a further limitation, the resin material used in the surface layer repairing agent is one or a combination of polyethylene resin, polyvinyl alcohol resin, polypropylene resin, phenolic resin and epoxy resin.
As a further limitation, the asphalt powders used in the interfacial agent and the surface layer agent are the same kind and batch of asphalt powders.
The invention also provides a repairing method for the graphite crucible, which adopts the repairing agent for the graphite crucible to repair the damaged graphite crucible, and comprises the following operation steps:
s1, cleaning the surface of a damaged area of a damaged graphite crucible, and ensuring that the surface of the area to be repaired is free of greasy dirt, moisture and other impurities;
s2, mixing solid powder components in the interface repairing agent, mixing the mixture with an organic solvent after uniform mixing, preparing a medium-low viscosity pasty fluid with a viscosity value of 600-650 Pa.s, and then adding SiC-Y 2 O 3 Uniformly dispersing the slurry, paraffin oil and pyridine to obtain an interface repairing agent slurry;
s3, coating the interface repairing agent prepared in the step S2 on a damaged area of a damaged graphite crucible, trowelling and removing excessive materials after coating, covering the coated area with aluminum foil, wrapping and keeping close fit on the outer side of the aluminum foil by utilizing glass fiber mesh cloth, and then performing pre-curing treatment and keeping for 2-3 hours at the temperature of 300-500 ℃ of the graphite crucible after treatment;
s4, preparing each component of the surface layer repairing agent into surface layer repairing paste by using an organic solvent, then taking out the damaged graphite crucible, removing the glass fiber mesh cloth and the aluminum foil, coating the surface layer repairing paste on the surface of the surface layer repairing paste, trowelling after coating is finished, removing the residual materials, and then curing and maintaining the surface layer repairing paste to complete the repairing operation of the graphite crucible after the surface layer repairing paste is completely solidified.
As a further limitation, the damaged graphite crucible repairable by the repair method is a graphite crucible having no through-hole and no surface damage, and the width of the damaged crack on the corresponding graphite crucible is not more than 10mm.
As a further limitation, when the pre-curing treatment is performed in the step S3, the damaged graphite crucible wrapped by the glass fiber mesh cloth may be placed in a vacuum container for the pre-curing treatment, where the set vacuum degree in the vacuum container is-0.12 to-0.09 MPa, and the treatment duration is 30 to 45min.
By way of further limitation, the curing and maintaining in step S4 is performed at a temperature of 90 to 120 ℃ for a curing period of 24 to 48 hours.
By way of further limitation, the maintenance is performed at room temperature in the maintenance in step S4, and the maintenance period is 5 to 7 days.
The beneficial effects are that: the invention provides a repairing agent for a graphite crucible, which is used for repairing a local damaged part of the damaged graphite crucible through a two-component structure, wherein the repairing agent is used as an interface repairing agent and a surface layer repairing agent of the two-component structure, both the interface repairing agent and the surface layer repairing agent are used as a matrix with graphite powder, the affinity between components is improved through the same type of asphalt powder and other additives, a stable interface structure is built through the interface repairing agent, and then the surface layer repairing is carried out by using the surface layer repairing agent with better affinity on the basis of the interface structure, so that a stable external interface structure is obtained;
the repairing agent is matched with a specific repairing method to obtain a stable repairing structure body at the damaged position of the graphite crucible, and the repairing structure body has good heat conductivity and high temperature resistance, good structural stability at high temperature and small thermal expansion coefficient; and is especially suitable for the graphite crucible in the burning state, ensures the use form of the graphite crucible in high temperature, high pressure or corrosive environment, and prolongs the service life of the graphite crucible.
Detailed Description
In order to better understand the solution of the present invention and make the technical means, creation characteristics, achievement purposes and effects achieved by the present invention easy to understand, the technical solution in the embodiments of the present invention will be clearly and completely described below in conjunction with the specific embodiments.
This embodiment is only a part of the embodiments of the present invention and represents all the embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention. It should be noted that terms like "comprising" and "having" and any variations thereof are used in the description of the invention, the claims and the following embodiments to distinguish similar objects, and furthermore, are intended to cover a non-exclusive inclusion, such as a process, method, system, article or apparatus that comprises a list of steps or elements not necessarily limited to those listed or explicitly listed.
The repairing agent for graphite crucible of the embodiment can be used for repairing the damaged graphite crucible which is a graphite crucible with surface damage and no through hole, has better repairing effect on damage with surface damage crack width not exceeding 10mm, and is especially suitable for graphite crucible in burning loss state.
The repairing agent is a two-component repairing agent, and comprises an interface repairing agent and a surface layer repairing agent, wherein the interface repairing agent and the surface layer repairing agent are prepared independently and are packaged independently according to parts;
the interface repairing agent comprises, by mass, 50 parts of graphite powder, 12 parts of paraffin oil, 13 parts of asphalt powder, 4 parts of pyridine and 2 parts of SiC-Y 2 O 3 And (3) slurry.
Wherein SiC-Y 2 O 3 The slurry consists of 30 parts of SiC and 3 parts of Y 2 O 3 Dissolving 35 parts of resin material in 60 parts of organic solvent, and uniformly stirring by ultrasonic dispersion and magnetic force to obtain SiC-Y 2 O 3 The mass part relation of the components in the slurry component is independent and is irrelevant to the mass part relation of the interface repairing agent, siC-Y 2 O 3 The resin material adopted in the slurry is phenolic resin, and the organic solvent correspondingly used is petroleum ether.
The surface layer repairing agent comprises 35-45 parts of petroleum coke powder, 15-20 parts of graphite powder, 8-10 parts of asphalt powder and 20-30 parts of resin materials according to the mass part ratio.
The petroleum coke powder is obtained after ball milling and screening and has a finer particle size, the particle size of the corresponding particles is below 1mm, the mass ratio of the petroleum coke powder with the particle size of below 0.6mm is 68%, and the mass ratio of the petroleum coke powder with the particle size of below 0.2mm is 36%; the resin material adopted in the surface layer repairing agent is phenolic resin.
In this example, the asphalt powders used as the raw materials in the interfacial agent and the surface layer agent were the same type and batch of asphalt powders.
When the repairing agent is used for repairing the damaged graphite crucible, the following steps are carried out:
firstly, cleaning the surface of a damaged area of the damaged graphite crucible by using a cleaning agent, ensuring that the surface of the area to be repaired is free of greasy dirt, moisture and other impurities, and also integrally cleaning the damaged graphite crucible if necessary. And after the cleaning is finished, the damaged area of the damaged graphite crucible is circled by using the sticker and is used as the boundary of the area to be coated.
Dry-mixing graphite powder and asphalt powder in the interface repairing agent, uniformly mixing, using proper amount of solvent oil as an organic solvent, adding the dry-mixed graphite powder and asphalt powder into the mixture, mixing the mixture, preparing a medium-low viscosity pasty fluid with a viscosity value of 630 Pa.s, obtaining the pasty fluid with stable form, and then adding SiC-Y into the pasty fluid 2 O 3 Adding the slurry, paraffin oil and pyridine into the slurry and uniformly dispersing the slurry to obtain the interface repairing agent slurry.
And (3) carrying out surface coating on the area to be coated by taking the area circled by the adhesive paper as a boundary, wherein the coating is carried out continuously for a plurality of times until the surface defect corresponding to the area to be coated is completely covered and a flush surface is obtained, then trowelling the coated surface, sticking an aluminum foil on the trowelled surface, tearing off the adhesive paper for positioning, wrapping and keeping close sticking on the aluminum foil surface outside the aluminum foil by utilizing glass fiber mesh cloth, and adopting high-melting-point glass fiber to the glass fiber mesh cloth corresponding to the glass fiber mesh cloth so as to avoid softening and denaturation of the glass fiber mesh cloth in the subsequent pre-curing process.
And (3) feeding the graphite crucible treated by the glass fiber mesh cloth and the aluminum foil into a heat treatment furnace, and performing pre-curing treatment for 150min at a set temperature of 400 ℃ by using the heat treatment furnace. And (5) naturally cooling along with the furnace after the treatment is completed, keeping for 60min, taking out the graphite crucible, removing the glass fiber mesh cloth, and scraping off the aluminum foil.
Preparing each component of the surface layer repairing agent into surface layer repairing paste by using solvent oil, then taking out the damaged graphite crucible subjected to the treatment, coating the surface of the surface layer repairing paste on the surface of the corresponding interface repairing agent treatment area, trowelling after coating is finished, removing excessive materials, then moving to a closed indoor space for standing maintenance, and obtaining the repaired graphite crucible after 7 days of maintenance treatment.
When the graphite crucible repairing agent is used for repairing the graphite crucible, the interface repairing agent is used for repairing the damaged surface, and the damaged surface is repairedWhen the graphite crucible is used, graphite powder is used as a filler and asphalt is used as a binder to fill and repair the damaged area, paraffin oil and pyridine are used to modify the surface of the filled area, and a layer of SiC-Y is built 2 O 3 A transition layer composed of slurry, the transition layer structure can reinforce the defect position, and meanwhile, siC-Y 2 O 3 The resin material in the slurry system can undergo volume shrinkage during high-temperature pyrolysis, so that surface micro-holes are formed on the surface of the repairing area of the interface repairing agent; the micro-holes are favorable for anchoring in the surface layer repairing agent attaching process, and are stable and fully solidified in the curing process under static conditions, so that the structural stability of the interface repairing agent is improved.
The repaired graphite crucible can be directly used after the interface repairing agent is fully solidified, when the using temperature reaches the softening point of the added asphalt powder, the asphalt further bonds the graphite powder and the petroleum coke powder together, volatile matters continuously overflow along with the increase of the using temperature, the asphalt is converted into amorphous carbon with strong adhesiveness and toughness, and paraffin oil and pyridine form an affinity interface in a composite system of the interface repairing agent and the surface layer repairing agent in the process, so that a crosslinked system with an interpenetrating polymer network structure is formed, and the strength and stability requirements of the graphite crucible under the high-temperature operation condition can be met.
The repairing agent is matched with the repairing method, so that the service life of the damaged graphite crucible can be prolonged by 30-50%, repeated repairing can be carried out for many times, and the use cost of the graphite crucible can be effectively reduced.
In addition, based on the optional technical path, in other embodiments, the damaged graphite crucible wrapped by the glass fiber mesh cloth can be placed in the vacuum container for pre-curing treatment in the pre-curing treatment stage, so that the duration of the pre-curing treatment can be effectively reduced, and the interface repairing agent can be deeper into the damaged position of the graphite crucible to further improve the reinforcing effect; when the damaged graphite crucible is correspondingly subjected to pre-curing treatment, the set vacuum degree in the vacuum container is minus 0.12 to minus 0.09MPa, and the treatment time is 30 to 45 minutes.
In the curing stage, the curing can be performed at the temperature of 90-120 ℃ during the maintenance, so that the curing market can be effectively reduced, the curing time is shortened to 24-48 hours, the efficiency is higher, but the stability of the repaired graphite crucible is slightly worse than that of the repaired graphite crucible obtained by the static natural curing mode mentioned in the previous embodiment.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be appreciated by those skilled in the art that the present invention is not limited to the above examples and that the skilled person can suitably modify the process parameters to achieve this in view of the present disclosure. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that the invention can be practiced and practiced with modification and alteration and combination of the methods and applications herein without departing from the spirit and scope of the invention.

Claims (9)

1. The repairing agent for the graphite crucible is characterized by being a two-component repairing agent, and comprising an interface repairing agent and a surface layer repairing agent;
the interface repairing agent comprises the following components in parts by mass:
graphite powder: 45-55 parts of paraffin oil: 10-15 parts of asphalt powder: 10-15 parts of pyridine: 3 to 5 parts of SiC-Y 2 O 3 Slurry: 2-3 parts;
wherein SiC-Y 2 O 3 The slurry consists of 25 to 35 parts of SiC and 2 to 5 parts of Y 2 O 3 30-40 parts of resin material is dissolved in 40-70 parts of organic solvent, and is obtained after ultrasonic dispersion and magnetic stirring are carried out uniformly;
the surface layer repairing agent comprises the following components in parts by mass:
petroleum coke powder: 35-45 parts of graphite powder: 15-20 parts of asphalt powder: 8-10 parts of resin material and 20-30 parts of solvent; the particle size of the petroleum coke powder is below 1mm, the mass ratio of the petroleum coke powder with the particle size below 0.6mm is 70-80%, and the mass ratio of the petroleum coke powder with the particle size below 0.2mm is 30-40%.
2. The repairing agent for a graphite crucible according to claim 1, wherein the SiC-Y 2 O 3 The resin material adopted in the slurry is phenolic resin or epoxy resin.
3. The repairing agent for graphite crucible according to claim 1, wherein the resin material used in the surface layer repairing agent is one or a combination of polyethylene resin, polyvinyl alcohol resin, polypropylene resin, phenolic resin and epoxy resin.
4. The repairing agent for graphite crucible according to claim 1, wherein the asphalt powders used in the interfacial repairing agent and the surface layer repairing agent are the same kind and batch of asphalt powders.
5. A repair method for a graphite crucible, characterized in that a repair operation for a damaged graphite crucible is performed using the repair agent for a graphite crucible as set forth in any one of claims 1 to 4, comprising the steps of:
s1, cleaning the surface of a damaged area of a damaged graphite crucible, and ensuring that the surface of the area to be repaired is free of greasy dirt, moisture and other impurities;
s2, mixing solid powder components in the interface repairing agent, mixing the mixture with an organic solvent after uniform mixing, preparing a medium-low viscosity pasty fluid with a viscosity value of 600-650 Pa.s, and then adding SiC-Y 2 O 3 Uniformly dispersing the slurry, paraffin oil and pyridine to obtain an interface repairing agent slurry;
s3, coating the interface repairing agent prepared in the step S2 on a damaged area of a damaged graphite crucible, trowelling and removing excessive materials after coating, covering the coated area with aluminum foil, wrapping and keeping close fit on the outer side of the aluminum foil by utilizing glass fiber mesh cloth, and then performing pre-curing treatment and keeping for 2-3 hours at the temperature of 300-500 ℃ of the graphite crucible after treatment;
s4, preparing each component of the surface layer repairing agent into surface layer repairing paste by using an organic solvent, then taking out the damaged graphite crucible, removing the glass fiber mesh cloth and the aluminum foil, coating the surface layer repairing paste on the surface of the surface layer repairing paste, trowelling after coating is finished, removing the residual materials, and then curing and maintaining the surface layer repairing paste to complete the repairing operation of the graphite crucible after the surface layer repairing paste is completely solidified.
6. The repairing agent for a graphite crucible according to claim 5, wherein the damaged graphite crucible is a graphite crucible having no through-holes and the width of damaged cracks on the corresponding graphite crucible is not more than 10mm.
7. The repairing agent for graphite crucible according to claim 5, wherein in the pre-curing treatment in step S3, the damaged graphite crucible covered with the glass fiber mesh cloth is placed in a vacuum container for the pre-curing treatment, wherein the set vacuum degree in the vacuum container is-0.12 to-0.09 MPa, and the treatment time is 30 to 45min.
8. The repairing agent for graphite crucible according to claim 5, wherein the maintenance is performed at a temperature of 90 to 120 ℃ for a maintenance period of 24 to 48 hours when the maintenance is performed in step S4.
9. The repairing agent for graphite crucible according to claim 5, wherein the maintenance is performed at room temperature for a period of 5 to 7 days while the maintenance is performed in step S4.
CN202311718685.9A 2023-12-14 2023-12-14 Repairing agent and repairing method for graphite crucible Pending CN117682880A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311718685.9A CN117682880A (en) 2023-12-14 2023-12-14 Repairing agent and repairing method for graphite crucible

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311718685.9A CN117682880A (en) 2023-12-14 2023-12-14 Repairing agent and repairing method for graphite crucible

Publications (1)

Publication Number Publication Date
CN117682880A true CN117682880A (en) 2024-03-12

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311718685.9A Pending CN117682880A (en) 2023-12-14 2023-12-14 Repairing agent and repairing method for graphite crucible

Country Status (1)

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