CN109021636A - A kind of processing technology of the high emissivity coating for electrothermal alloy - Google Patents
A kind of processing technology of the high emissivity coating for electrothermal alloy Download PDFInfo
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- CN109021636A CN109021636A CN201811177076.6A CN201811177076A CN109021636A CN 109021636 A CN109021636 A CN 109021636A CN 201811177076 A CN201811177076 A CN 201811177076A CN 109021636 A CN109021636 A CN 109021636A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
- C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
Abstract
The invention discloses a kind of processing technologys of high emissivity coating for electrothermal alloy, the graphite in raw material is ground and sieved first, generate the powder having a size of 10um, and it is classified as two equal portions, it will be ground in radioactive waste and segment glass investment ball mill, and it is uniformly mixed with a copy of it powdered graphite, is granulated and is compacted into briquetting；Remaining powdered graphite is ground and is uniformly mixed with remaining glass, and is pressed into the embryo block with cavity at high temperature；Briquetting is placed in the cavity of embryo block, controlled at 1000 DEG C, compression moulding obtains radioactivity substrate.It is reasonable to match in the present invention, not only effectively increase the service life and prospect of production of high emissivity coating, coating has more excellent inoxidizability and higher emissivity simultaneously, coating granule is evenly distributed, practicability is larger, radioactive waste obtained in production can be effectively treated simultaneously, waste utilization reduces cost.
Description
Technical field
The present invention relates to coating preparation field, the processing work of specifically a kind of high emissivity coating for electrothermal alloy
Skill.
Background technique
Heat source can generally be propagated in a manner of convection current, radiation, conduction, more hot environment when infra-red radiation specific gravity can add
By force, the energy conservation of radiant heat is just quite important, and the approach for reducing infra-red radiation generally changes the infrared signature of target, i.e. mesh
The emissivity distribution for marking object perhaps reduces infrared intensity or adjusts infra-red radiation propagation path, therefore develops low radiation
Rate coating can change infrared signature and reduce infrared intensity and it is present in the market, we common one
Kind solution.
And in some cases, the use for electrothermal alloy, it would be desirable to which the emissivity for improve body surface changes
Become infrared signature and improves infrared intensity.
For above situation, we devise a kind of processing technology of high emissivity coating for electrothermal alloy, not only
Need to improve the emissivity of electrothermal alloy, it is also necessary to increase service life, this is our problem urgently to be resolved.
Summary of the invention
The purpose of the present invention is to provide a kind of processing technologys of high emissivity coating for electrothermal alloy, existing to solve
There is the problems in technology.
To achieve the above object, the invention provides the following technical scheme: a kind of high emissivity coating for electrothermal alloy
Processing technology, the high emissivity coating includes following raw material components, by weight: 2-15 parts of radioactivity substrate, first slurry
Expect 25-35 parts, 35-45 parts of the second slurry, 5-10 parts of high temperature resistant filler.
Optimally, the radioactivity substrate includes following raw material components, by weight: 0-5 parts of radioactive waste, graphite
60-90 parts, 20-50 parts of inorganic bond.
Optimally, the graphite is one of natural graphite, synthetic graphite or a variety of.
Optimally, first slurry includes following raw material components, by weight: 3-8 parts of silica solution, silicon powder 12-18
Part, 25-30 parts of ceramic powder, 35-45 parts of dispersing agent；The dispersing agent mainly includes water, the first solvent and the second solvent, the water
Quality: the quality of the first solvent be 90/1-1/90, the quality of second solvent: the quality of dispersing agent be 0-0.05.
Optimally, the ceramic powder is one of SiC powder, ZrC powder or a variety of mixtures；First solvent is penta
The mixed solution of alkane, heptane；Second solvent is the mixed solution of methanol, dimethyl ether.
Optimally, second slurry includes following raw material components, by weight: frit: 35-40 parts, zirconium oxide: 8-
18 parts, chromium oxide: 5-15 parts, 2-6 parts of clay, 5-10 parts of silicon carbide, 0-3 parts of manganese dioxide, 45-50 parts of colloid；The colloid
It mainly include water, waterglass and silica, wherein water: 65-85%, waterglass: 10-12%, silica: 3-25%, and
The sum of above-mentioned each component is 100%.
Optimally, the high temperature resistant filler includes alumina powder, any one or mixture in clay powder.
Optimally, comprising the following steps:
1) pretreatment of radioactivity substrate；
2) preparation of electrothermal alloy；
3) pretreatment of electrothermal alloy；
4) the first coat coats；
5) the second coat coats；
6) sample treatment.
Optimally, comprising the following steps:
1) pretreatment of radioactivity substrate:
A) graphite in raw material is ground and is sieved, generate the powder having a size of 10-50um, and be classified as two etc.
Part, it will then be ground in radioactive waste and segment glass investment ball mill, and mixed with a copy of it powdered graphite
It is even, it is granulated and is compacted into briquetting；
B) remaining powdered graphite is ground and is uniformly mixed with remaining glass, and be pressed into have at high temperature
The embryo block of cavity；
C) briquetting is placed in the cavity of embryo block, controlled at 1000-1050 DEG C, compression moulding obtains radioactivity
Substrate；
2) preparation of electrothermal alloy:
A) raw material components are weighed by a certain percentage, and carry out raw material preparation；
B) prepared raw material is fitted into vacuum refining furnace and is smelted, and put into the radioactivity base being prepared in step 1)
Material and high temperature resistant filler, smelting temperature are 1450-1500 DEG C, refining time 0.5-1h, 1500-1520 DEG C of tapping temperature；
C) electroslag refining；
D) it forges；
E) gren rod: the ingot bar after forging is subjected to gren rod, hot-rolled temperature is 1150 DEG C -1300 DEG C, open rolling temperature
Degree: 1250 DEG C, finishing temperature: 1200 DEG C；
F) it anneals, 950-1150 DEG C of annealing temperature, annealing heat preservation 1.5-2h；
G) blank after annealing is subjected to pickling, washing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
3) pretreatment of electrothermal alloy:
A) sanding and polishing: the sand paper that 240#, 400#, 800# and 1500# is respectively adopted in the surface of electrothermal alloy is polished, then
It is polished with flannelette；
B) it cleans: being cleaned by ultrasonic 15-60min in acetone, then be cleaned by ultrasonic 10-30min in dehydrated alcohol, finally exist
Air drying is placed for 24 hours；
4) the first coat coats:
A) prepared by the first slurry: ratio weighs a certain amount of silica solution, silicon powder and ceramic powder by weight, is uniformly mixed, obtains
To the first mixed-powder, dispersing agent then is prepared by certain material rate, and dispersing agent and the first mixed-powder are placed in ball milling
Ball milling mixing is uniform in machine, the first slurry needed for obtaining；
B) it coats for the first time: the first obtained slurry is coated in the material surface of step 3) treated electrothermal alloy,
The first coat is obtained in alloy surface after drying, obtains being put into after sample being heat-treated in a vacuum furnace, treatment temperature 900-
1000℃；
5) the second coat coats:
A) prepared by powder: the raw material of the second coat of preparation is weighed by certain weight percent, be added ball mill ball milling,
And be uniformly mixed, and the powder body material after ball milling is heat-treated 8-10h under 1200-1300 DEG C of high temperature, by the powder after heat treatment
Body material ball milling, ultra fine again, until the particle size of obtained powder body material is in 1um hereinafter, obtaining the second mixing
Powder；
B) prepared by colloidal materials: the raw material of production colloidal materials are weighed by certain weight percent, and blender is added,
It is evenly stirred until the colloidal materials with certain viscosity；
C) prepared by the second slurry: the second mixed-powder being prepared in colloidal materials and step a) being sufficiently stirred, is mixed
It closes uniformly, handles 15-30min under ultrasonic wave effect, can be prepared by the second slurry；
D) it second coats: the second obtained slurry being coated in step 4) treated electrothermal alloy surface, after drying
The second coat is obtained in alloy surface, is put into a vacuum furnace after obtaining sample, 800-950 DEG C of heat treatment temperature；
6) sample treatment: treated electrothermal alloy is placed in vacuum sintering furnace, is (1.0 × 10 in vacuum degree- 3Pa)-(5.0×10-3Pa high-temperature melting, furnace cooling are carried out under conditions of), the height being prepared with a thickness of 30 μm -500 μm is put
Penetrate rate coating.
It optimally, is first 10 DEG C/min-30 DEG C/min's in heating rate when high-temperature melting in the step 6)
Under the conditions of be warming up to 450 DEG C -700 DEG C, 0.5-1.5h is kept the temperature, then in the condition that heating rate is 10 DEG C/min-15 DEG C/min
Under be warming up to 1100 DEG C -1550 DEG C, keep the temperature 0.4-1h.
Compared with prior art, the beneficial effects of the present invention are: the radioactive waste in the present invention includes coming from nuclear fuel
The radioactive substance generated in the waste of the nuclear fuel element of post-processing and some medical applications, the present invention in inorganic bond
Silicate glass powder is selected, because it is with good corrosion resistance and chemical-resistance；Pass through graphite in the present invention first
Radioactive waste is handled with silicate glass powder, select graphite for substrate be because graphite has high-termal conductivity, it is high
Hardness and relatively low thermal expansion and extremely low tearing tendency, for the processing of radioactive waste, we generally selected gold in the past
Belong to container, but known all metal materials all have 10,000 year expected maximum corrosion resistance so far, therefore cannot
Realize the safety clamp band of radioactive waste, and the half-life period of fission product is more much longer than the physical life of hitherto known material,
The influence of such as pH value fluctuation is existed simultaneously, this may cause the corrosion of canister material, so as to cause the leaching of waste packaging
Out, there are the great risks of radioactive waste leakage；Selected in the present invention nonmetallic materials graphite and silicate glass powder into
The placement and pretreatment of row radioactive waste can not only efficiently use the radioactivity of radioactive waste, while can also improve
The storage safety of radioactive waste.
The present invention is in the pretreatment of radioactivity substrate, by radioactive waste and part powdered graphite and part inorganic bond
Agent carries out mixing briquetting, while remaining powdered graphite and inorganic bond are pressed into the embryo block with cavity, will have and put
The briquetting of injectivity waste places the placement safety and leakage that can not only ensure that radioactive waste in the cavities, while can
The radioactivity of radioactive waste is efficiently used, convenient for the preparation of subsequent electrothermal alloy and the utilization of coating.
In general, present coating on the market is coated on the surface of electrothermal alloy mostly, but needs in the present invention
The emissivity for improving electrothermal alloy, if radioactive waste is coated by coating, over time, coating can be with
Fall off, not only to the placement of radioactive waste, there are security risks, while the emissivity of electrothermal alloy cannot also ensure, because
We pre-process radioactive waste for this, then in the radioactivity substrate investment vacuum refining furnace that pretreatment is obtained, then with
The raw material of electrothermal alloy carry out the preparation of electrothermal alloy together so that the emissivity of electrothermal alloy will not be because of surface covering
Variation changes.
Sanding and polishing processing is carried out to the electrothermal alloy being prepared in the present invention, is convenient for subsequent progress coating preparation and painting
The electrothermal alloy for covering operation, while being prepared is individually positioned in acetone, is cleaned by ultrasonic in dehydrated alcohol, effectively removes electric heating and closes
Gold surface impurity, so that the smoothness of the coating of coating greatly promotes, stability is higher.
Raw material zirconium oxide, the chromium oxide of floating coat of the present invention all have good infrared radiation property, and alkali resistance is strong, together
When clay binding force and adhesive force between raw material can be improved, coating surface is bright and clean after sintering, and adhesive force is strong, not easily to fall off.
Not only radioactive waste is placed in the raw material of electrothermal alloy in the present invention and is performed physical exercise, and makes radioactive waste
It is present in inside electrothermal alloy, while the surface layer of electrothermal alloy is coated with coating, coating is high IR emissivity coating, specific to wrap
The first coat and the second coat are included, wherein the first coat improves coating by controlling accurate raw material proportioning and selection
Inoxidizability, the second coat improves the emissivity of coating by reasonably designing, and passes through the first coat and second and applies
Fitting closely between coating and melting have finally obtained high emissivity coating required for us.
The preparation of dispersing agent has been carried out when preparing the first coat in the present invention, has wherein been selected in dispersing agent first molten
Agent, water and the second solvent, the first solvent selected in invention is pentane, the mixed solution of heptane, also can choose pentane, heptan
One or more kinds of mixing of alkane, dodecane, benzene, toluene, the first solvent belong to organic liquid not soluble in water, can be with water shape
At liquid-liquid interface, and wettable polymer powders；Second solvent is the mixed solution of methanol, dimethyl ether, also can choose first
The mixing of one or more of alcohol, the tert-butyl alcohol, dimethyl ether, the second solvent is water-soluble, and can infiltrate polymer powder
Material, by the proportion of the first solvent of control, the second solvent and water, we can effectively control the big of the first slurry powder diameter
It is small.
The present invention provides a kind of processing technology of high emissivity coating for electrothermal alloy, matches and close in the present invention
Reason, not only effectively increases the service life and prospect of production of high emissivity coating, at the same coating have it is more excellent anti-oxidant
Property and higher emissivity, coating granule are evenly distributed, and practicability is larger, at the same can to radioactive waste obtained in production into
Row is effectively treated, and waste utilization reduces cost.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1:
First carry out radioactivity substrate pretreatment, the graphite in raw material is ground and is sieved, generate having a size of
The powder of 10um, and two equal portions are classified as, it will then be ground in radioactive waste and segment glass investment ball mill, and
It is uniformly mixed with a copy of it powdered graphite, is granulated and is compacted into briquetting；Again by remaining powdered graphite and remaining glass into
Row grinds and is uniformly mixed, and is pressed into the embryo block with cavity at high temperature；With briquetting is placed in the cavity of embryo block,
Controlled at 1000 DEG C, compression moulding obtains radioactivity substrate；
The preparation for carrying out electrothermal alloy again weighs raw material components by a certain percentage first, and carries out raw material preparation；It will match again
The raw material made, which is fitted into vacuum refining furnace, to be smelted, and puts into the radioactivity substrate and high temperature resistant filler being prepared, and smelts temperature
Degree is 1450 DEG C, refining time 0.5h, 1500 DEG C of tapping temperature；Electroslag refining；Forging；Then the ingot bar after forging is subjected to heat
Wire rod is rolled, hot-rolled temperature is 1150 DEG C, start rolling temperature: 1250 DEG C, finishing temperature: 1200 DEG C；Annealing, is moved back by 950 DEG C of annealing temperature
Fire heat preservation 1.5h；Pickling, washing are carried out with the blank after will annealing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
Then carry out electrothermal alloy pretreatment, by the surface of electrothermal alloy be respectively adopted 240#, 400#, 800# and
The sand paper of 1500# polishes, then is polished with flannelette；It is cleaned by ultrasonic 15min in acetone, then is cleaned by ultrasonic in dehydrated alcohol
10min is finally dried in air, is placed for 24 hours；
The preparation of the first slurry is carried out again, and ratio by weight weighs a certain amount of silica solution, silicon powder and ceramic powder, and mixing is equal
It is even, the first mixed-powder is obtained, then prepares dispersing agent by certain material rate, and dispersing agent and the first mixed-powder are placed in
Ball milling mixing is uniform in ball mill, the first slurry needed for obtaining；The first obtained slurry is coated in treated electrothermal alloy
Material surface, obtain the first coat in alloy surface after drying, obtain being put into after sample being heat-treated in a vacuum furnace, handle
900 DEG C of temperature；
The coating of the second coat is carried out immediately, weighs the original of the second coat of preparation by certain weight percent first
Material is added ball mill ball milling and is uniformly mixed, and the powder body material after ball milling is heat-treated 8h under 1200 DEG C of high temperature, will be hot
Treated powder body material ball milling, ultra fine again, until the particle size of obtained powder body material in 1um hereinafter,
To the second mixed-powder；The raw material for weighing production colloidal materials by certain weight percent again, are added blender, and stirring is equal
The even colloidal materials extremely with certain viscosity；The second mixed-powder that colloidal materials are prepared in is sufficiently stirred, mixing
Uniformly, 15min is handled under ultrasonic wave effect, can be prepared by the second slurry；Then the second obtained slurry is coated in processing
Electrothermal alloy surface afterwards obtains the second coat in alloy surface after drying, is put into a vacuum furnace after obtaining sample, at heat
800 DEG C of temperature of reason；
Finally carry out sample treatment, treated electrothermal alloy be placed in vacuum sintering furnace, vacuum degree be 1.0 ×
10-3It carries out high-temperature melting under conditions of Pa, when high-temperature melting, is warming up under conditions of heating rate is 10 DEG C/min first
450 DEG C, 0.5h is kept the temperature, 1100 DEG C are then warming up under conditions of heating rate is 10 DEG C/min, keeps the temperature 0.4h；It is cold with furnace
But, the high emissivity coating with a thickness of 30 μm is prepared.
2 parts of 1 selective emission substrate of embodiment, 25 parts of the first slurry, 35 parts of the second slurry, 5 parts of high temperature resistant filler；Wherein
Radioactivity substrate includes following raw material components: 5 parts of radioactive waste, 60 parts of graphite, 35 parts of inorganic bond；
First slurry includes following raw material components: 3 parts of silica solution, 12 parts of silicon powder, 25 parts of ceramic powder, 35 parts of dispersing agent；Point
Powder mainly includes water, the first solvent and the second solvent, and the quality of the water: the quality of the first solvent is 90: 1, described second
The quality of solvent: the quality of dispersing agent is 0.01；
Second slurry includes following raw material components: frit: 35 parts, zirconium oxide: 8 parts, chromium oxide: 5 parts, 2 parts of clay, carbonization
5 parts of silicon, 45 parts of colloid；Colloid mainly includes water 65%, waterglass 10% and silica 25%.
Ceramic powder is SiC powder；High temperature resistant filler is alumina powder, the mixture in clay powder；First solvent is
The mixed solution of pentane, heptane；Second solvent is the mixed solution of methanol, dimethyl ether.
Embodiment 2:
First carry out radioactivity substrate pretreatment, the graphite in raw material is ground and is sieved, generate having a size of
The powder of 30um, and two equal portions are classified as, it will then be ground in radioactive waste and segment glass investment ball mill, and
It is uniformly mixed with a copy of it powdered graphite, is granulated and is compacted into briquetting；Again by remaining powdered graphite and remaining glass into
Row grinds and is uniformly mixed, and is pressed into the embryo block with cavity at high temperature；With briquetting is placed in the cavity of embryo block,
Controlled at 1050 DEG C, compression moulding obtains radioactivity substrate；
The preparation for carrying out electrothermal alloy again weighs raw material components by a certain percentage first, and carries out raw material preparation；It will match again
The raw material made, which is fitted into vacuum refining furnace, to be smelted, and puts into the radioactivity substrate and high temperature resistant filler being prepared, and smelts temperature
Degree is 1450 DEG C, refining time 1h, 1500 DEG C of tapping temperature；Electroslag refining；Forging；Then the ingot bar after forging is subjected to hot rolling
Wire rod, hot-rolled temperature are 1200 DEG C, start rolling temperature: 1250 DEG C, finishing temperature: 1200 DEG C；Annealing, is moved back by 1050 DEG C of annealing temperature
Fire heat preservation 2h；Pickling, washing are carried out with the blank after will annealing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
Then carry out electrothermal alloy pretreatment, by the surface of electrothermal alloy be respectively adopted 240#, 400#, 800# and
The sand paper of 1500# polishes, then is polished with flannelette；It is cleaned by ultrasonic 45min in acetone, then is cleaned by ultrasonic in dehydrated alcohol
20min is finally dried in air, is placed for 24 hours；
The preparation of the first slurry is carried out again, and ratio by weight weighs a certain amount of silica solution, silicon powder and ceramic powder, and mixing is equal
It is even, the first mixed-powder is obtained, then prepares dispersing agent by certain material rate, and dispersing agent and the first mixed-powder are placed in
Ball milling mixing is uniform in ball mill, the first slurry needed for obtaining；The first obtained slurry is coated in treated electrothermal alloy
Material surface, obtain the first coat in alloy surface after drying, obtain being put into after sample being heat-treated in a vacuum furnace, handle
950 DEG C of temperature；
The coating of the second coat is carried out immediately, weighs the original of the second coat of preparation by certain weight percent first
Material is added ball mill ball milling and is uniformly mixed, and the powder body material after ball milling is heat-treated 9h under 1250 DEG C of high temperature, will be hot
Treated powder body material ball milling, ultra fine again, until the particle size of obtained powder body material in 1um hereinafter,
To the second mixed-powder；The raw material for weighing production colloidal materials by certain weight percent again, are added blender, and stirring is equal
The even colloidal materials extremely with certain viscosity；Colloidal materials are sufficiently stirred with the second mixed-powder being prepared, mixing is equal
It is even, 20min is handled under ultrasonic wave effect, can be prepared by the second slurry；Then after treatment by the second obtained slurry coating
Electrothermal alloy surface, obtain the second coat in alloy surface after drying, obtain being put into after sample in a vacuum furnace, heat treatment
900 DEG C of temperature；
Finally carry out sample treatment, treated electrothermal alloy be placed in vacuum sintering furnace, vacuum degree be 1.0 ×
10-3It carries out high-temperature melting under conditions of Pa, when high-temperature melting, is warming up under conditions of heating rate is 30 DEG C/min first
600 DEG C, 1h is kept the temperature, 1350 DEG C are then warming up under conditions of heating rate is 15 DEG C/min, keeps the temperature 0.8h；Furnace cooling,
The high emissivity coating with a thickness of 100 μm is prepared.
10 parts of selective emission substrate, 35 parts of the first slurry, 45 parts of the second slurry, 10 parts of high temperature resistant filler in embodiment 2；
Wherein radioactivity substrate includes following raw material components: 5 parts of radioactive waste, 70 parts of graphite, 25 parts of inorganic bond；
First slurry includes following raw material components: 5 parts of silica solution, 15 parts of silicon powder, 28 parts of ceramic powder, 45 parts of dispersing agent；Point
Powder mainly includes water, the first solvent and the second solvent, and the quality of the water: the quality of the first solvent is 1: 90, described second
The quality of solvent: the quality of dispersing agent is 0.03；
Second slurry includes following raw material components: frit: 38 parts, zirconium oxide: 15 parts, chromium oxide: 10 parts, 4 parts of clay, carbon
5 parts of SiClx, 2 parts of manganese dioxide, 45 parts of colloid；Colloid mainly includes water 65%, waterglass 10% and silica 25%.
Ceramic powder is SiC powder；High temperature resistant filler is alumina powder, the mixture in clay powder；First solvent is
The mixed solution of pentane, heptane；Second solvent is the mixed solution of methanol, dimethyl ether.
Embodiment 3:
First carry out radioactivity substrate pretreatment, the graphite in raw material is ground and is sieved, generate having a size of
The powder of 30um, and two equal portions are classified as, it will then be ground in radioactive waste and segment glass investment ball mill, and
It is uniformly mixed with a copy of it powdered graphite, is granulated and is compacted into briquetting；Again by remaining powdered graphite and remaining glass into
Row grinds and is uniformly mixed, and is pressed into the embryo block with cavity at high temperature；With briquetting is placed in the cavity of embryo block,
Controlled at 1050 DEG C, compression moulding obtains radioactivity substrate；
The preparation for carrying out electrothermal alloy again weighs raw material components by a certain percentage first, and carries out raw material preparation；It will match again
The raw material made, which is fitted into vacuum refining furnace, to be smelted, and puts into the radioactivity substrate and high temperature resistant filler being prepared, and smelts temperature
Degree is 1500 DEG C, refining time 1h, 1520 DEG C of tapping temperature；Electroslag refining；Forging；Then the ingot bar after forging is subjected to hot rolling
Wire rod, hot-rolled temperature are 1300 DEG C, start rolling temperature: 1250 DEG C, finishing temperature: 1200 DEG C；Annealing, is moved back by 1150 DEG C of annealing temperature
Fire heat preservation 2h；Pickling, washing are carried out with the blank after will annealing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
Then carry out electrothermal alloy pretreatment, by the surface of electrothermal alloy be respectively adopted 240#, 400#, 800# and
The sand paper of 1500# polishes, then is polished with flannelette；It is cleaned by ultrasonic 60min in acetone, then is cleaned by ultrasonic in dehydrated alcohol
30min is finally dried in air, is placed for 24 hours；
The preparation of the first slurry is carried out again, and ratio by weight weighs a certain amount of silica solution, silicon powder and ceramic powder, and mixing is equal
It is even, the first mixed-powder is obtained, then prepares dispersing agent by certain material rate, and dispersing agent and the first mixed-powder are placed in
Ball milling mixing is uniform in ball mill, the first slurry needed for obtaining；The first obtained slurry is coated in treated electrothermal alloy
Material surface, obtain the first coat in alloy surface after drying, obtain being put into after sample being heat-treated in a vacuum furnace, handle
1000 DEG C of temperature；
The coating of the second coat is carried out immediately, weighs the original of the second coat of preparation by certain weight percent first
Material is added ball mill ball milling and is uniformly mixed, and the powder body material after ball milling is heat-treated 10h under 1300 DEG C of high temperature, will be hot
Treated powder body material ball milling, ultra fine again, until the particle size of obtained powder body material in 1um hereinafter,
To the second mixed-powder；The raw material for weighing production colloidal materials by certain weight percent again, are added blender, and stirring is equal
The even colloidal materials extremely with certain viscosity；Colloidal materials are sufficiently stirred with the second mixed-powder being prepared, mixing is equal
It is even, 30min is handled under ultrasonic wave effect, can be prepared by the second slurry；Then after treatment by the second obtained slurry coating
Electrothermal alloy surface, obtain the second coat in alloy surface after drying, obtain being put into after sample in a vacuum furnace, heat treatment
950 DEG C of temperature；
Finally carry out sample treatment, treated electrothermal alloy be placed in vacuum sintering furnace, vacuum degree be 5.0 ×
10-3It carries out high-temperature melting under conditions of Pa, when high-temperature melting, is warming up under conditions of heating rate is 30 DEG C/min first
700 DEG C, 1.5h is kept the temperature, 1550 DEG C are then warming up under conditions of heating rate is 15 DEG C/min, keeps the temperature 1h；Furnace cooling,
The high emissivity coating with a thickness of 30 μm is prepared.
10 parts of selective emission substrate, 35 parts of the first slurry, 45 parts of the second slurry, 10 parts of high temperature resistant filler in embodiment 3；
Wherein radioactivity substrate includes following raw material components: 5 parts of radioactive waste, 75 parts of graphite, 20 parts of inorganic bond；
First slurry includes following raw material components: 5 parts of silica solution, 15 parts of silicon powder, 28 parts of ceramic powder, 45 parts of dispersing agent；Point
Powder mainly includes water, the first solvent and the second solvent, and the quality of the water: the quality of the first solvent is 90: 1, described second
The quality of solvent: the quality of dispersing agent is 0.05；
Second slurry includes following raw material components: frit: 38 parts, zirconium oxide: 15 parts, chromium oxide: 10 parts, 4 parts of clay, carbon
5 parts of SiClx, 3 parts of manganese dioxide, 50 parts of colloid；Colloid mainly includes water 65%, waterglass 10% and silica 25%.
Ceramic powder is SiC powder；High temperature resistant filler is alumina powder；First solvent is pentane, the mixing of heptane is molten
Liquid；Second solvent is the mixed solution of methanol, dimethyl ether.
Embodiment 4:
The preparation for carrying out electrothermal alloy first, weighs raw material components, and carry out raw material preparation by a certain percentage；It will prepare again
Good raw material, which is fitted into vacuum refining furnace, to be smelted, and puts into high temperature resistant filler, and smelting temperature is 1500 DEG C, refining time 1h, out
1520 DEG C of steel temperature；Electroslag refining；Forging；Then the ingot bar after forging is subjected to gren rod, hot-rolled temperature is 1300 DEG C, is opened
Roll temperature: 1250 DEG C, finishing temperature: 1200 DEG C；Annealing, 1150 DEG C of annealing temperature, annealing heat preservation 2h；With the base after will annealing
Part carries out pickling, washing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
Then carry out electrothermal alloy pretreatment, by the surface of electrothermal alloy be respectively adopted 240#, 400#, 800# and
The sand paper of 1500# polishes, then is polished with flannelette；It is cleaned by ultrasonic 60min in acetone, then is cleaned by ultrasonic in dehydrated alcohol
30min is finally dried in air, is placed for 24 hours；
The preparation of the first slurry is carried out again, and ratio by weight weighs a certain amount of silica solution, silicon powder and ceramic powder, and mixing is equal
It is even, the first mixed-powder is obtained, then prepares dispersing agent by certain material rate, and dispersing agent and the first mixed-powder are placed in
Ball milling mixing is uniform in ball mill, the first slurry needed for obtaining；The first obtained slurry is coated in treated electrothermal alloy
Material surface, obtain the first coat in alloy surface after drying, obtain being put into after sample being heat-treated in a vacuum furnace, handle
1000 DEG C of temperature；
The coating of the second coat is carried out immediately, weighs the original of the second coat of preparation by certain weight percent first
Material is added ball mill ball milling and is uniformly mixed, and the powder body material after ball milling is heat-treated 10h under 1300 DEG C of high temperature, will be hot
Treated powder body material ball milling, ultra fine again, until the particle size of obtained powder body material in 1um hereinafter,
To the second mixed-powder；The raw material for weighing production colloidal materials by certain weight percent again, are added blender, and stirring is equal
The even colloidal materials extremely with certain viscosity；Colloidal materials are sufficiently stirred with the second mixed-powder being prepared, mixing is equal
It is even, 30min is handled under ultrasonic wave effect, can be prepared by the second slurry；Then after treatment by the second obtained slurry coating
Electrothermal alloy surface, obtain the second coat in alloy surface after drying, obtain being put into after sample in a vacuum furnace, heat treatment
950 DEG C of temperature；
Finally carry out sample treatment, treated electrothermal alloy be placed in vacuum sintering furnace, vacuum degree be 5.0 ×
10-3It carries out high-temperature melting under conditions of Pa, when high-temperature melting, is warming up under conditions of heating rate is 30 DEG C/min first
700 DEG C, 1.5h is kept the temperature, 1550 DEG C are then warming up under conditions of heating rate is 15 DEG C/min, keeps the temperature 1h；Furnace cooling,
The high emissivity coating with a thickness of 30 μm is prepared.
35 parts of the first slurry, 45 parts of the second slurry, 10 parts of high temperature resistant filler are selected in embodiment 4；
First slurry includes following raw material components: 5 parts of silica solution, 15 parts of silicon powder, 28 parts of ceramic powder, 45 parts of dispersing agent；Point
Powder mainly includes water, the first solvent and the second solvent, and the quality of the water: the quality of the first solvent is 90: 1, described second
The quality of solvent: the quality of dispersing agent is 0.05；
Second slurry includes following raw material components: frit: 38 parts, zirconium oxide: 15 parts, chromium oxide: 10 parts, 4 parts of clay, carbon
5 parts of SiClx, 3 parts of manganese dioxide, 50 parts of colloid；Colloid mainly includes water 65%, waterglass 10% and silica 25%.
Ceramic powder is SiC powder；High temperature resistant filler is alumina powder；First solvent is pentane, the mixing of heptane is molten
Liquid；Second solvent is the mixed solution of methanol, dimethyl ether.
Embodiment 5:
The preparation for carrying out electrothermal alloy first, weighs raw material components, and carry out raw material preparation by a certain percentage；It will prepare again
Good raw material, which is fitted into vacuum refining furnace, to be smelted, and puts into high temperature resistant filler, and smelting temperature is 1500 DEG C, refining time 1h, out
1520 DEG C of steel temperature；Electroslag refining；Forging；Then the ingot bar after forging is subjected to gren rod, hot-rolled temperature is 1300 DEG C, is opened
Roll temperature: 1250 DEG C, finishing temperature: 1200 DEG C；Annealing, 1150 DEG C of annealing temperature, annealing heat preservation 2h；With the base after will annealing
Part carries out pickling, washing；Multiple drawing is carried out again, obtains electrothermal alloy finished product.
Experiment detection:
Every detection is carried out to high emissivity coating obtained as above,
Such as draw a conclusion by the way that above data is available:
Embodiment 3, embodiment 4, embodiment 5 are comparative experiments, wherein in the preparation process of the electrothermal alloy in embodiment 3
The radioactivity substrate that is added to that treated, and electrothermal alloy surface is covered with coating；In embodiment 4 and the radiation that is not added with that treated
Property substrate, electrothermal alloy surface is covered with coating, and the data in embodiment 5 are common electrothermal alloy, and in addition to this remaining is joined
Number is identical, by obtaining using data it is found that the emissivity of the electrothermal alloy that is prepared in embodiment 3 is whole higher, and
Antioxygenic property is good；Lower than in embodiment 3, alloy has good the emissivity for the electrothermal alloy being prepared in embodiment 4
Oxidation susceptibility, and oxidation susceptibility, emissivity data are below embodiment 3, embodiment 4 in embodiment 5, performance is poor.
Embodiment 1, embodiment 2, embodiment 3 are comparative experimentss, are prepared by embodiment 1, embodiment 2, embodiment 3
High emissivity coating when being coated on electrothermal alloy, oxidation resistant, while the infrared emissivity of 3-5 μm of normal direction is equal at room temperature
Reach the infrared emissivity of 0.85 or more, 8-14 μm of normal direction and reaches 0.90 or more；Electrothermal alloy surface forms one layer of densification
Protective layer, when doing ablation experiments at 1600 DEG C, the electrothermal alloy of matcoveredn does not occur ablation phenomen, and unprotected
Material is obviously ablated；Simultaneously by table it is found that addition high temperature resistant filler after electrothermal alloy high-temperature resistant result it is more preferable；Coating
Qualification rate respectively to 97% or more, coating using effect is good, have wide prospect of production.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
Claims (10)
1. a kind of processing technology of the high emissivity coating for electrothermal alloy, it is characterised in that: the high emissivity coating packet
Following raw material components are included, by weight: 2-15 parts of radioactivity substrate, 25-35 parts of the first slurry, 35-45 parts of the second slurry, resistance to height
Warm filler 5-10 parts.
2. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 1, it is characterised in that:
The radioactivity substrate includes following raw material components, by weight: 0-5 parts of radioactive waste, 60-90 parts of graphite, inorganic bond
20-50 parts of agent.
3. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 2, it is characterised in that:
The graphite is one of natural graphite, synthetic graphite or a variety of.
4. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 1, it is characterised in that:
First slurry includes following raw material components, by weight: 3-8 parts of silica solution, 12-18 parts of silicon powder, 25-30 parts of ceramic powder,
35-45 parts of dispersing agent；The dispersing agent mainly includes water, the first solvent and the second solvent, the quality of the water: the first solvent
Quality is 90/1-1/90, the quality of second solvent: the quality of dispersing agent is 0-0.05.
5. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 4, it is characterised in that:
The ceramic powder is one of SiC powder, ZrC powder or a variety of mixtures；First solvent is pentane, the mixing of heptane is molten
Liquid；Second solvent is the mixed solution of methanol, dimethyl ether.
6. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 1, it is characterised in that:
Second slurry includes following raw material components, by weight: frit: 35-40 parts, zirconium oxide: 8-18 parts, chromium oxide: 5-15
Part, 2-6 parts of clay, 5-10 parts of silicon carbide, 0-3 parts of manganese dioxide, 45-50 parts of colloid；The colloid mainly includes water, waterglass
And silica, wherein water: 65-85%, waterglass: 10-12%, silica: 3-25%, and the sum of above-mentioned each component is
100%.
7. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 1, it is characterised in that:
The high temperature resistant filler includes alumina powder, any one or mixture in clay powder.
8. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 1, it is characterised in that:
The following steps are included:
1) pretreatment of radioactivity substrate；
2) preparation of electrothermal alloy；
3) pretreatment of electrothermal alloy；
4) the first coat coats；
5) the second coat coats；
6) sample treatment.
9. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 7, it is characterised in that:
The following steps are included:
1) pretreatment of radioactivity substrate:
A) graphite in raw material is ground and is sieved, generate the powder having a size of 10-50um, and be classified as two equal portions,
It will then grind in radioactive waste and segment glass investment ball mill, and be uniformly mixed with a copy of it powdered graphite,
It is granulated and is compacted into briquetting；
B) remaining powdered graphite is ground and is uniformly mixed with remaining glass, and be pressed at high temperature with cavity
Embryo block；
C) briquetting is placed in the cavity of embryo block, controlled at 1000-1050 DEG C, compression moulding obtains radioactivity substrate；
2) preparation of electrothermal alloy:
A) raw material components are weighed by a certain percentage, and carry out raw material preparation；
B) prepared raw material is fitted into vacuum refining furnace and is smelted, and put into the radioactivity substrate that is prepared in step 1) and
High temperature resistant filler, smelting temperature are 1450-1500 DEG C, refining time 0.5-1h, 1500-1520 DEG C of tapping temperature；
C) electroslag refining；
D) it forges；
E) gren rod: the ingot bar after forging is subjected to gren rod, hot-rolled temperature is 1150 DEG C -1300 DEG C, start rolling temperature:
1250 DEG C, finishing temperature: 1200 DEG C；
F) it anneals, 950-1150 DEG C of annealing temperature, annealing heat preservation 1.5-2h；
G) blank after annealing is subjected to pickling, washing；Multiple drawing is carried out again, obtains electrothermal alloy finished product；
3) pretreatment of electrothermal alloy:
A) 240#, 400 sanding and polishing: is respectively adopted in the surface of electrothermal alloy；The sand paper of #, 800# and 1500# polish, then use
Flannelette polishing；
B) it cleans: being cleaned by ultrasonic 15-60min in acetone, then be cleaned by ultrasonic 10-30min in dehydrated alcohol, finally in air
Middle drying is placed for 24 hours；
4) the first coat coats:
A) prepared by the first slurry: ratio weighs a certain amount of silica solution, silicon powder and ceramic powder by weight, is uniformly mixed, and obtains the
Then one mixed-powder prepares dispersing agent by certain material rate, and dispersing agent and the first mixed-powder is placed in ball mill
Ball milling mixing is uniform, the first slurry needed for obtaining；
B) it coats for the first time: the first obtained slurry is coated in the material surface of step 3) treated electrothermal alloy, drying
The first coat is obtained in alloy surface afterwards, obtains being put into after sample being heat-treated in a vacuum furnace, 900-1000 DEG C for the treatment of temperature；
5) the second coat coats:
A) prepared by powder: weighing the raw material of the second coat of preparation by certain weight percent, ball mill ball milling is added and mixes
It closes uniformly, and the powder body material after ball milling is heat-treated 8-10h under 1200-1300 DEG C of high temperature, by the powder material after heat treatment
Ball milling, ultra fine again are expected, until the particle size of obtained powder body material is in 1um hereinafter, obtaining the second mixed-powder；
B) prepared by colloidal materials: weighing the raw material of production colloidal materials by certain weight percent, blender, stirring is added
Uniformly to the colloidal materials with certain viscosity；
C) prepared by the second slurry: the second mixed-powder being prepared in colloidal materials and step a) being sufficiently stirred, mixing is equal
It is even, 15-30min is handled under ultrasonic wave effect, can be prepared by the second slurry；
D) it second coats: the second obtained slurry being coated in step 4) treated electrothermal alloy surface, is being closed after drying
Gold surface obtains the second coat, is put into a vacuum furnace after obtaining sample, 800-950 DEG C of heat treatment temperature:
6) sample treatment: treated electrothermal alloy is placed in vacuum sintering furnace, is (1.0 × 10 in vacuum degree-3Pa)-
(5.0×10-3Pa high-temperature melting is carried out under conditions of), the high emissivity with a thickness of 30 μm -500 μm is prepared in furnace cooling
Coating.
10. a kind of processing technology of high emissivity coating for electrothermal alloy according to claim 8, feature exist
In: in the step 6), when high-temperature melting, 450 are warming up under conditions of heating rate is 10 DEG C/min-30 DEG C/min first
DEG C -700 DEG C, keep the temperature 0.5-1.5h, be then warming up under conditions of heating rate is 10 DEG C/min-15 DEG C/min 1100 DEG C -
1550 DEG C, keep the temperature 0.4-1h.
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