CN107022733A - A kind of fused salt heat diffusion treatment equipment and its application - Google Patents
A kind of fused salt heat diffusion treatment equipment and its application Download PDFInfo
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- CN107022733A CN107022733A CN201610074177.5A CN201610074177A CN107022733A CN 107022733 A CN107022733 A CN 107022733A CN 201610074177 A CN201610074177 A CN 201610074177A CN 107022733 A CN107022733 A CN 107022733A
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- support bar
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/52—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions more than one element being applied in one step
- C23C8/54—Carbo-nitriding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
- C23C8/44—Carburising
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/40—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions
- C23C8/42—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using liquids, e.g. salt baths, liquid suspensions only one element being applied
- C23C8/48—Nitriding
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
- Furnace Details (AREA)
Abstract
The invention discloses a kind of fused salt heat diffusion treatment equipment and its application.It includes an air supply system, a vacuum system, a body of heater, a circulation water coil, a sample room, a crucible and a support bar；Air supply system is connected by air inlet pipe with body of heater, and vacuum system is connected by the first escape pipe with body of heater；Circulation water coil is sheathed on the top of body of heater；Crucible is located at bottom of furnace body, and crucible includes being provided with first annular groove on the outside of crucible body and crucible cover plate, the upper end of crucible body, and Open Side Down encases mouth of pot for crucible cover plate, and stretches into first annular groove；Support bar sequentially passes through fire door, crucible cover plate on body of heater, and stretches into crucible；One end that support bar stretches into crucible is connected with sample room.Present device treatment effeciency is high, system is closed, the water oxygen content of energy control system, prevents fused salt steam or its catabolite to be diffused into crucible external enwergy and reduce the influence of fused salt smog, it is to avoid equipment is caused to corrode or is accumulated on the resistance wire of heating furnace and causes equipment short circuit.
Description
Technical field
The present invention relates to a kind of fused salt heat diffusion treatment equipment and its application.
Background technology
With the development of science and technology, production and technical field to the hardness of material, wearability, heat-resisting quantity,
The performance such as corrosion resistance and fatigue resistance proposes higher and higher requirement.Surface modification technologies lead to
Metal material surface is set to obtain the surface texture that performance is much better than metal material frequently with certain process means.
After the surface-modified processing of metal material, the mechanical property of matrix material can be played, material list can be made again
Face obtains many excellent properties.Due to surface modification technologies relative inexpensiveness, thus increasingly by
The favor of those skilled in the art.
Common surface modification technologies mainly have plating, ion deposition (including chemical vapor deposition and
Physical vapour deposition (PVD)), plasma spray technology, surface coloring and dyeing and the method such as thermo-chemical treatment.Change
It is a kind of surface strengthening technology for making infiltration layer element penetrate into metal surface using the diffusion of element to learn heat treatment,
Including carburizing, nitriding, boronising, carbo-nitriding and TD processing (Toyota Diffusion Coating
The method such as Process).Wherein TD treatment technologies are researched and developed by Toyota Motor center research institute
A kind of process for modifying surface (Toyota Diffusion), be fused salt immersion plating, electrolysis and powder
The processing of the general name of method, also commonly known as metallic cementation.Coating obtained by TD treatment technologies has excellent resistance to
Polishing machine and high hardness, form metallurgical binding between coating and matrix, its adhesion is much larger than it
His film plating process, and TD treatment technologies are compared with other technologies, with simple to operate, equipment cost is low
The advantages of.But TD treatment technologies there is problems in use：Because crucible is exposed to big
In gas, without protective atmosphere, the water oxygen in air is dissolved into fused salt, causes molten salt deposition, influence
Fused salt activity, while the increase of fused salt reclaimed water oxygen content, can aggravate the corrosivity of fused salt, reduction equipment
Life-span；Along with due to easily decomposing volatilization under fused salt high temperature itself, its catabolite or fused salt smog can be right
Equipment, which is caused to corrode or is accumulated on the resistance wire of heating furnace, causes equipment short circuit.Therefore it is badly in need of exploitation a kind of
With protective atmosphere control, avoid water or oxygen in air from being dissolved into fused salt and decomposition production can be reduced
Thing or the fused salt heat diffusion treatment equipment of smog influence.
The content of the invention
The technical problems to be solved by the invention are to overcome crucible in the prior art to be exposed in air, are not had
Water oxygen in protective atmosphere, air is dissolved into fused salt, causes molten salt deposition, and influence fused salt is active,
And because fused salt high temperature itself easily decomposes volatilization, its catabolite or fused salt smog can cause corruption to equipment
Lose or be accumulated in caused on the resistance wire of heating furnace equipment short circuit defect there is provided a kind of fused salt thermal diffusion
Processing equipment and its application.Present device is cheap, and whole system is closed, can not only effectively control
The water oxygen content of system, and can also effectively prevent fused salt steam or its catabolite to be diffused into outside crucible,
Control climate is good, can reduce the influence of fused salt smog, be prevented effectively from and heating is caused to corrode or be accumulated in equipment
Equipment short circuit is caused on the resistance wire of stove；Present device is easy to operate during practical application, place
Efficiency high is managed, upper cavity operating space temperature is low, and system opens convenient, and sampling can be realized at high temperature
And sample-adding；In processing procedure can to fused salt sampling analysis or charging, by keeping fused salt steady quality,
And then the stabilization of the product quality after guarantee processing.
To overcome to above mentioned problem, present inventor is at the initial stage of research and development, it is contemplated that by weldering on crucible
Technique connection air supply system and vacuum system are connect, so that fused salt is isolated with the water oxygen in air.But the party
The problem of method is present is to carry out being required for being welded on crucible during TD processing every time, TD processing
After complete, again need remove welding, and if processing metal it is of different sizes, need change crucible, again need
Re-start welding operation.Thus bring cumbersome, and treatment effeciency is compared with low defect.On overcoming
Problem is stated, present inventor attempts to be designed body of heater again, newly increases the top of body of heater.In stove
The upper weld air supply system and vacuum system of body, effectively avoid Rewelding, remove the numerous of welding
Trivial operation, makes TD processing easy to operate, treatment effeciency height.Moreover, body of heater upper cavity operating space temperature
Low, system opens convenient, and sampling can be realized at high temperature and is loaded；Can be to fused salt in processing procedure
Sampling analysis or charging, by keeping the steady of the product quality after fused salt steady quality, and then guarantee processing
It is fixed.
The present invention solves above-mentioned technical problem by the following technical programs.
The invention provides a kind of fused salt heat diffusion treatment equipment, it includes an air supply system, a vacuum system
System, a body of heater, a circulation water coil, a sample room, a crucible and a support bar；
The air supply system is connected by air inlet pipe with the body of heater, and the vacuum system passes through the first outlet
Pipe is connected with the body of heater；The circulation water coil is sheathed on the top of the body of heater；
The crucible is located at the bottom of the body of heater, and the crucible includes crucible body and crucible cover plate, institute
State and first annular groove is provided with the outside of the upper end of crucible body, Open Side Down encases crucible for the crucible cover plate
Mouthful, and stretch into the first annular groove；
The support bar sequentially passes through fire door, the crucible cover plate on the body of heater, and stretches into the earthenware
In crucible；One end that the support bar stretches into the crucible is connected with the sample room.
In the present invention, the air supply system is preferably with gas purification apparatus.The gas purification apparatus
For preferably can by the water Control for Oxygen Content of air inlet below 1ppm gas purification apparatus.Specifically exist
During use, the air supply system and the vacuum system by inflation repeatedly and can vacuumize control
Water oxygen content in system.
In the present invention, the air supply system preferably also includes the device for being loaded with inert gas.The inertia
Gas refers to that during equipment use the gas that will not be reacted with material is not limited to conventionally referred
Rare gas, for example can be nitrogen.The rare gas is preferably argon gas.
In the present invention, the vacuum system is the conventional vacuum system in this area, preferably vavuum pump.
In the present invention, the body of heater is preferably the body of heater provided with cooling structure.The cooling structure is this
The conventional cooling structure in field, preferably double-deck recirculated water cooling structure.The double-deck recirculated water cooling structure
Inside it is typically provided a cooling water interlayer.When specifically used, by the cooling of the double-deck recirculated water cooling structure
Effect, the external temperature of described sidewall of the furnace body is smaller than 50 DEG C.
In the present invention, the inwall of the body of heater is typically provided a heating furnace.The burner hearth of the body of heater is preferably
Solidify burner hearth for polycrystalline alumina fiber.It is reachable that the polycrystalline alumina fiber solidification burner hearth bears the highest temperature
1100℃。
In the present invention, the inside of the body of heater, to avoid temperature measuring equipment is out of control from causing heating out of control, preferably
Ground includes a temperature measuring equipment and a temperature control device.Wherein, the temperature measuring equipment is used for measurement temperature, described
Temperature control device is used to control temperature.The temperature measuring equipment and the temperature control device are that this area is conventional, compared with
It is thermocouple goodly.
In the present invention, the fire door on the body of heater, which is preferably centre, the half cover plates in aperture.The hole
Footpath is preferably greater than the diameter of the support bar.It can be seen from common sense in the field, the half cover plates refer to
The fire door being made up of two semicircular cover plates.During specifically used, the fire door on the body of heater is used for
The top of the inside heating system of the body of heater and the body of heater is separated.
In the present invention, covered it is preferred that the top of the body of heater is additionally provided with one.The upper lid is preferably
Upper lid provided with glove box transition hatch door.During specifically used, the closed and unlatching of the upper lid is adopted
With the glove box transition hatch door, it not only can guarantee that vacuum-packed requirement, and can be easy to open and
Close.
In the present invention, the side wall of the body of heater is sequentially provided with an outer wall, a cooling knot from outside to inside, typically
Structure, a heat-insulation layer, a high temperature resistant interlayer and a heating furnace.The cooling structure is preferably double-deck circulation
Cooling water pipe.The material of the heat-insulation layer is that this area is conventional.The high temperature resistant interlayer bears the highest temperature
Up to 1100 DEG C.
In the present invention, the top of the body of heater is preferably also provided with a pressure gauge.The pressure gauge be used for
When detect furnace interior pressure.
In the present invention, the circulation water coil refers to plate-like knot for refrigerating function, being made up of water pipe
Structure.When specifically used, by the cooling effect of the circulation water coil, the outside on described body of heater top
Temperature is smaller than 40 DEG C.During the continuous use of the equipment, body of heater tip temperature is relatively low, is easy to operation,
Fused salt quality can be followed the trail of in time, production efficiency height is improved, and be conducive to keeping product quality stable.
In the present invention, the sample room is preferably the basket of stainless steel.
In the present invention, the outside of the crucible and the inner side spacing of the body of heater are preferably greater than 20mm.
The spacing is used to avoid the crucible in high temperature caused by expanded by heating contact furnace body inside heater strip
Short circuit.
In the present invention, one first positioning knot and/or one second positioning knot are preferably also provided with the support bar.
After the fused salt in the crucible is melted, the first positioning knot, can located at the top of the crucible cover plate
Height for adjusting the sample room according to the amount of fused salt, it is ensured that sample room energy in processing procedure
Cross and be totally immersed into fused salt, and the bottom with the crucible is not contacted.The second positioning knot is located at institute
The lower end of crucible cover plate is stated, the crucible cover plate is blocked when the support bar is extracted, is taken during such high temperature
Just without first removing the crucible cover plate when going out the sample room.
In the present invention, the top of the support bar preferably is provided with dismountable handle, so as to the sample
The taking-up of room.
In the present invention, the material of the crucible, the sample room and the support bar can be according to actual fused salt
Specific species, carry out this area conventional selection, may generally be the metal material of resistance to fused salt corrosion used,
It is preferably stainless steel or nickel, is more preferably 316L stainless steels, conventional metal material can be prevented in height
It is corroded under temperature molten salt system and pollutes fused salt.
In the present invention, one second annular groove preferably is provided with the inside of the upper end of the crucible body.It is described
Preferably contain carbon particle and/or metallic copper in second annular groove.The carbon particle and/or metallic copper can be with
In high temperature with the oxygen reaction remained in crucible, the oxygen of residual is to molten salt system effectively in control crucible
Influence.
In the present invention, in the first annular groove, preferably contain sand.Sand can be used for will be described
Sand seal is carried out between crucible and the crucible cover plate.The sand seal on the one hand can effectively prevent fused salt steam or
Its catabolite is diffused into outside the crucible, and control climate is good, can be reduced the influence of fused salt smog, effectively be kept away
Exempt from that equipment is caused to corrode or be accumulated on the resistance wire of heating furnace and cause equipment short circuit；Another further aspect,
The water oxygen of outside atmosphere can effectively be controlled to the influence of molten salt system.
In the present invention, the fused salt heat diffusion treatment equipment preferably also includes a relief valve, the pressure release
Valve is connected by the second escape pipe with the body of heater.During fused salt heating treatment, if system pressure is high
In 0.2MPa, pressure release is carried out to system preferably by the relief valve.
In the present invention, the fused salt heat diffusion treatment equipment is before use, preferably first check the close of equipment
Feng Xing.The detection method of the sealing is this area routine operation, is preferably carried out in the steps below：
Equipment is inflated to 0.2~0.5MPa, is kept for more than 20 hours, if pressure drop is less than 5%, the sealing of equipment
Property is good.
During specifically used, the operation, the operation of sampling and the operation of sample-adding for tracking fused salt quality are equal
Need to open the upper lid of the body of heater；In addition to aforesaid operations, by the air supply system, the body of heater it is upper
Lid, the vacuum system, the body of heater and relief valve composition sealing system.
Set present invention also offers a kind of fused salt heat diffusion treatment equipment as metallochemistry heat treatment
Standby application.
In the present invention, the metallochemistry heat treatment is infiltration layer element is penetrated into metal using the diffusion of element
A kind of surface strengthening technology on top layer, including carburizing, nitriding, boronising, carbo-nitriding and TD processing
Methods such as (Toyota Diffusion Coating Process).
In the present invention, the thermo-chemical treatment is preferably TD processing.
On the basis of common sense in the field is met, above-mentioned each optimum condition can be combined, produce this hair
Bright each preferred embodiments.
The positive effect of the present invention is：
Present device is cheap, and whole system is closed, can not only effective control system water oxygen content,
And can also effectively prevent fused salt steam or its catabolite to be diffused into outside crucible, control climate is good, can subtract
Few fused salt smog influence, is prevented effectively from that equipment is caused to corrode or is accumulated on the resistance wire of heating furnace and causes
Equipment short circuit；Present device is easy to operate during practical application, and treatment effeciency is high, upper cavity
Operating space temperature is low, and system opens convenient, and sampling can be realized at high temperature and is loaded；Processing procedure
In can be to fused salt sampling analysis or charging, by keeping after fused salt steady quality, and then guarantee processing
The stabilization of product quality.
Brief description of the drawings
Fig. 1 is heat diffusion treatment equipment drawing of the invention；Wherein, 101 be air supply system, and 102 be true
Empty pump, 2 be support bar, and 201 be the first positioning knot, and 202 be the second positioning knot, and 3 be crucible, 301
It is the second annular groove for first annular groove, 302,303 be crucible cover plate, and 4 be sample room, 501
It is heater strip for thermocouple, 502,6 be body of heater, and 601 be high temperature resistant interlayer, and 602 be heat-insulation layer, 603
It is upper lid for cooling water interlayer, 604,605 be fire door, and 701 be dual-layer cycle cooling water pipe, and 702 follow
Ring water coil, 801,802,804 be valve, and 803 be relief valve, and 9 be pressure gauge, and 10 be sand
Son, 11 be carbon particle and/or metallic copper, and 12 be fused salt.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but is not therefore limited the present invention to
Among described scope of embodiments.The experimental method of unreceipted actual conditions in the following example, according to normal
Rule method and condition, or selected according to catalogue.
Embodiment 1
Fig. 1 is heat diffusion treatment equipment drawing of the invention；Wherein, 101 be air supply system, and 102 be true
Empty pump, 2 be support bar, and 201 be the first positioning knot, and 202 be the second positioning knot, and 3 be crucible, 301
It is the second annular groove for first annular groove, 302,303 be crucible cover plate, and 4 be sample room, 501
It is heater strip for thermocouple, 502,6 be body of heater, and 601 be high temperature resistant interlayer, and 602 be heat-insulation layer, 603
It is upper lid for cooling water interlayer, 604,605 be fire door, and 701 be dual-layer cycle cooling water pipe, and 702 follow
Ring water coil, 801,802,804 be valve, and 803 be relief valve, and 9 be pressure gauge, and 10 be sand
Son, 11 be carbon particle and/or metallic copper, and 12 be fused salt.
Wherein, air supply system 101 is connected by air inlet pipe with body of heater 6；Air supply system 101 carries gas
Purification devices, the device for being loaded with inert gas；Specifically in use, air supply system 101 and vacuum
Pump 102 by inflation repeatedly and can vacuumize the water oxygen content in control system；Inert gas refers to
During equipment use, the gas that will not be reacted with material is not limited to conventionally referred rare gas,
For example can be nitrogen.
Vacuum system is vavuum pump 102, is connected by the first escape pipe with body of heater 6.
Support bar 2 sequentially passes through fire door 605, crucible cover plate 303 on body of heater 6, and stretches into crucible 3
In, one end that support bar 2 stretches into crucible 3 is connected with sample room 4, and sample room 4 is the net of stainless steel
Basket；The first positioning knot 201 and one second positioning knot 202 are additionally provided with support bar 2；The top of support bar 2
End is provided with handle, so as to the taking-up of sample room 4；After the fused salt in crucible 3 is melted, the first positioning 201
Knot, available for the height that sample room 4 is adjusted according to the amount of fused salt, is protected located at the top of crucible cover plate 303
Card sample room 4 can be crossed in processing procedure to be totally immersed into fused salt, and is not contacted with crucible bottom；The
Two positioning knots 202 are located at the lower end of crucible cover plate 303, and crucible cover plate 303 is blocked when support bar 2 is extracted,
So high temperature when take out sample room 4 when just without first removing crucible cover plate 303.
Crucible 3 is located at the bottom of body of heater 6, and crucible 3 includes a crucible body and a crucible cover plate 303, earthenware
The inside of crucible body is to be provided with first annular groove 301, crucible on the outside of fused salt 12, the upper end of crucible body
Open Side Down encases mouth of pot for cover plate 303, and stretches into first annular groove 301；Crucible body it is upper
End inner side, which is provided with one second annular groove 302, the second annular groove 302, contains carbon particle and/or metallic copper
11；The oxygen reaction that carbon particle or metallic copper 11 can be remained in high temperature and in crucible 3, effectively control
Influence of the oxygen of residual to molten salt system in crucible processed.Contain sand 10 in first annular groove 301；
Sand 10 can be used for that sand seal will be carried out between crucible 3 and crucible cover plate 303.
The inside of body of heater 6, for avoid temperature measuring equipment it is out of control cause heating it is out of control, including a temperature measuring equipment and
One temperature control device；Wherein temperature measuring equipment is used for measurement temperature, and temperature control device is used to control temperature, thermometric dress
It is thermocouple 501 to put with temperature control device；The inwall of body of heater 6 is provided with heater strip 502, the stove of body of heater 6
Thorax is to bear the highest temperature to solidify burner hearth up to 1100 DEG C of polycrystalline alumina fiber；
Fire door 605 on body of heater 6 is half cover plates, and there is aperture centre, and aperture is more than support bar 2
Diameter.It can be seen from common sense in the field, half cover plates refer to the fire door being made up of two semicircular cover plates.
During specifically used, fire door 605 on stove 6 is used for the heating system inside body of heater 6 and body of heater
Top is separated；The top of body of heater 6 is additionally provided with lid 604 on one.The closed and unlatching of upper lid uses gloves
The design of case transition cabin door；During specifically used, glove box transition hatch door not only can guarantee that vacuum
Sealedly require, and can be easy to open and close.
Body of heater 6 is the body of heater provided with pair of lamina recirculated water cooling structure 701, dual-layer cycle cooling water pipe 701
Inside be provided with a cooling water interlayer 603；When specifically used, by double-deck recirculated water cooling structure 701
Cooling effect, the external temperature of sidewall of the furnace body is smaller than 50 DEG C.Circulate the pipe sleeve of water pond 702 and be located at body of heater 6
Top；Circulation water coil 702 refers to disk-like structure for refrigerating function, being made up of water pipe.Tool
Body is in use, by the cooling effect of circulation water coil 702, the external temperature on body of heater top is smaller than
40℃。
The side wall of body of heater 6 from outside to inside, be sequentially provided with dual-layer cycle cooling water pipe 701, heat-insulation layer 602,
High temperature resistant interlayer 601 and heater strip 502.The top of body of heater 6 also includes a pressure gauge 9.
The spacing of crucible 3 and the inner side of body of heater 6 is more than 20mm；The spacing is used to avoid crucible 3 in height
Short circuit caused by the expanded by heating contact inner side heater strip 502 of body of heater 6 when warm.
Fused salt heat diffusion treatment equipment also includes a relief valve 803, and relief valve 803 passes through the second escape pipe
Connected with body of heater 6；During fused salt heating treatment, if the pressure of pressure gauge 9 is higher than 0.2MPa,
Pressure release is carried out to system.
During specifically used, the operation, the operation of sampling and the operation of sample-adding for tracking fused salt quality are equal
Need the upper lid 604 of opening body of heater 6；In addition to aforesaid operations, by air supply system 101, the upper lid of body of heater
604th, vavuum pump 102, body of heater 6 and the composition sealing system of relief valve 803.
The specifically used method of the heat diffusion treatment equipment such as following step of the present invention：
(1) such as Fig. 1 connected modes are attached, and tighten lid 604, the sealing of inspection system, tool
Gymnastics is made as follows：0.2MPa is inflated to, is kept for 24 hours, pressure drop is as qualified less than 5%；
(2) after pressurize is qualified, first system is carried out to take out true using air supply system 101 and vavuum pump 102
Empty and inflation processing, to remove substantial amounts of adsorption moisture, is then passed through purifier by air supply system 101
Nitrogen after processing carries out baker, to remove the moisture of the absorption such as stove inner thermal insulating layer, improves insulating properties；
After baker, the water oxygen adsorbed in heat-insulation layer 602 can be evaporate into nitrogen, then anti-to being carried out in system
Multiple inflated with nitrogen (by air supply system 101) vacuumizes (by vavuum pump 102) processing, to reduce
Water oxygen content in system；After the water oxygen content in system is reduced to below 10ppm, inflated with nitrogen malleation
Protection system；
(3) cooling-water machine is opened, whether test cooling water recirculation system work is normal, if normally, carrying out
Next step；
(4) fused salt is prepared as needed, fused salt consumption is high according to the size of crucible 3 and required fused salt
Degree is calculated, and in glove box (if the fused salt and Qi Nei into being placed in air, small is influenceed on it,
Can directly be operated under air atmosphere) fused salt is crushed and weighed；Then according to formula, it is weighed
Its component, these components and fused salt is added in crucible 3, rocks uniform；
Carbon particle and/or metallic copper 11 are added in the second annular groove 302.Sample is put into sample room 4
Interior, sample room 4 hangs over the bottom of support bar 2.Support bar 2 passes through crucible cover plate 303, and according to crucible
Height and fused salt height, position knot 201, lower end positioning knot 202 by upper end and are fixedly mounted (it is required that molten
When salt is melted, sample room is immersed in fused salt, and is not contacted with crucible bottom, it is to avoid electric between dissimilar materials
Chemical reaction, influences result)；Put into again in the crucible 3 for installing fused salt, crucible cover plate 303 is covered
On crucible 3；
Now because fused salt is solid, sample room 4 can only be placed on fused salt top, not contained by fused salt.
Sand 10 is added in the first annular groove 303 of crucible 3, sand seal is carried out；The crucible cover that Open Side Down
Plate 303 and sand seal, which can effectively prevent fused salt volatile component in crucible 3, can cause body of heater heater strip 502
Fusing phenomenon；
(5) outlet valve 803 is opened to system decompression, is let out to normal pressure, lid 604 in unlatching, is opened
Fire door 605, the support bar 2 and crucible 3 that step (4) is fixed rapidly is put into furnace chamber center (to keep away
Exempt from body of heater short circuit, crucible should not be allowed to be contacted with the wall of heating furnace)；Cover and covered in heat-preservation furnace door 605, closing
604；Lid 604 in inflation processing, reduction is vacuumized repeatedly to system again to open to system water oxygen
The influence of content；
(6) heating schedule set by temperature control system is handled sample, in heating schedule setting,
It is recommended that more than fused salt melting temperature, below treatment temperature, constant temperature is more than half an hour, to ensure fused salt
Melting；
In temperature-rise period, as temperature of molten salt reaches more than melting temperature, fused salt starts dissolving, sample room
4 and sample can slowly be immersed in melting fused salt in by fused salt contain, eventually through upper end position knot 201
Hang on crucible cover plate 303；
In processing procedure, pressure in the system that is represented in pressure gauge 9 is noted, if during higher than 0.2MPa,
Outlet valve 803 is opened to system decompression.
(7) if after the completion of processing, at high temperature, opening outlet valve 803 to system decompression, opening
Upper lid 604, opens fire door 605, wears high temperature gloves, and the handle for extracting support bar 2 takes out support bar 2
With sample room 4, at high temperature, melting fused salt can from water clock on sample room 4 and sample, therefore when taking out,
Support bar can be held to stop 10 seconds or so on crucible top, fused salt is viscous on reduction sample and sample room 4
It is attached, the processing of sample can be somewhat completed after cooling with distilled water cleaning sample.
If the processing being equally formulated, sample room 4 and support bar 2 can not be cleaned, directly make again
With.It is analyzable after three times are handled, it is proposed that take molten salt sample to be analyzed with being glued under nickel rod high temperature
Project includes, oxygen content and main component element.Supplement fused salt or other components to ensure according to analysis result
Product quality is stable.
Claims (10)
1. a kind of fused salt heat diffusion treatment equipment, it is characterised in that it includes an air supply system, one true
Empty set system, a body of heater, a circulation water coil, a sample room, a crucible and a support bar；
The air supply system is connected by air inlet pipe with the body of heater, and the vacuum system passes through the first outlet
Pipe is connected with the body of heater；The circulation water coil is sheathed on the top of the body of heater；
The crucible is located at the bottom of the body of heater, and the crucible includes crucible body and crucible cover plate, institute
State and first annular groove is provided with the outside of the upper end of crucible body, Open Side Down encases crucible for the crucible cover plate
Mouthful, and stretch into the first annular groove；
The support bar sequentially passes through fire door, the crucible cover plate on the body of heater, and stretches into the earthenware
In crucible；One end that the support bar stretches into the crucible is connected with the sample room.
2. equipment as claimed in claim 1, it is characterised in that the air supply system is pure with gas
Makeup is put；The gas purification apparatus be preferably can by the water Control for Oxygen Content of air inlet 1ppm with
Under gas purification apparatus；
The air supply system also includes the device for being loaded with inert gas；
The vacuum system is vavuum pump.
3. equipment as claimed in claim 1, it is characterised in that the burner hearth of the body of heater is polycrystalline oxygen
Change aluminum fiber solidification burner hearth；
The top of the body of heater is additionally provided with a pressure gauge.
4. equipment as claimed in claim 1, it is characterised in that the body of heater is provided with cooling structure
Body of heater；
The inside of the body of heater includes a temperature measuring equipment and a temperature control device；
Fire door on the body of heater has the half cover plates in aperture for centre；
The top of the body of heater is additionally provided with one and covered.
5. equipment as claimed in claim 4, it is characterised in that the cooling structure circulates to be double-deck
Water-cooling structure；
The temperature measuring equipment and the temperature control device are thermocouple；
The aperture is more than the diameter of the support bar；
The upper lid is the upper lid provided with glove box transition cabin door.
6. equipment as claimed in claim 1, it is characterised in that the sample room is stainless steel
Basket；
The outside of the crucible and the inner side spacing of the body of heater are more than 20mm；
One second annular groove is provided with the inside of the upper end of the crucible body；In second annular groove preferably
Contain carbon particle and/or metallic copper in ground；
Contain sand in the first annular groove.
7. equipment as claimed in claim 1, it is characterised in that one is additionally provided with the support bar
One positioning knot and/or one second positioning knot, the first positioning knot is located at the top of the crucible cover plate, institute
State the lower end that the second positioning knot is located at the crucible cover plate；
The top of the support bar is provided with dismountable handle；
The material of the crucible, the sample room and the support bar is stainless steel or nickel.
8. equipment as claimed in claim 1, it is characterised in that the fused salt heat diffusion treatment equipment
Also include a relief valve, the relief valve is connected by the second escape pipe with the body of heater.
9. a kind of fused salt heat diffusion treatment equipment as described in any one of claim 1~8 is used as metallochemistry
The application of Equipment for Heating Processing.
10. application as claimed in claim 9, it is characterised in that the thermo-chemical treatment is at TD
Reason.
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| CN201610074177.5A CN107022733B (en) | 2016-02-02 | 2016-02-02 | Molten salt thermal diffusion treatment equipment and application thereof |
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| CN201610074177.5A CN107022733B (en) | 2016-02-02 | 2016-02-02 | Molten salt thermal diffusion treatment equipment and application thereof |
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| CN109536880A (en) * | 2019-01-29 | 2019-03-29 | 东北大学 | A kind of method of melten salt electriochemistry method to stainless steel surface nitriding or carbo-nitriding |
| CN110042434A (en) * | 2018-01-15 | 2019-07-23 | 中国科学院上海应用物理研究所 | Reaction unit and its operation method for molten salt system uranium fluorination reaction |
| CN110333180A (en) * | 2019-07-02 | 2019-10-15 | 中国科学院上海硅酸盐研究所 | High-temperature molten salt environment simulator and method |
| CN112725725A (en) * | 2020-12-07 | 2021-04-30 | 江苏省镔鑫钢铁集团有限公司 | Deformed steel bar thermal diffusion treatment method and treatment equipment |
| CN114440477A (en) * | 2020-11-03 | 2022-05-06 | 中国科学院上海应用物理研究所 | Fused salt temperature difference control device |
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| CN110042434A (en) * | 2018-01-15 | 2019-07-23 | 中国科学院上海应用物理研究所 | Reaction unit and its operation method for molten salt system uranium fluorination reaction |
| CN110042434B (en) * | 2018-01-15 | 2024-04-12 | 中国科学院上海应用物理研究所 | Reaction device for uranium fluorination reaction of molten salt system and operation method thereof |
| CN109536880A (en) * | 2019-01-29 | 2019-03-29 | 东北大学 | A kind of method of melten salt electriochemistry method to stainless steel surface nitriding or carbo-nitriding |
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| CN114440477A (en) * | 2020-11-03 | 2022-05-06 | 中国科学院上海应用物理研究所 | Fused salt temperature difference control device |
| CN114440477B (en) * | 2020-11-03 | 2024-03-26 | 中国科学院上海应用物理研究所 | Fused salt temperature difference control device |
| CN112725725A (en) * | 2020-12-07 | 2021-04-30 | 江苏省镔鑫钢铁集团有限公司 | Deformed steel bar thermal diffusion treatment method and treatment equipment |
| CN112725725B (en) * | 2020-12-07 | 2021-12-24 | 江苏省镔鑫钢铁集团有限公司 | Deformed steel bar thermal diffusion treatment method and treatment equipment |
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