CN109457202A - A kind of tantalum zirconium clad steel plate reaction kettle heat treatment method - Google Patents
A kind of tantalum zirconium clad steel plate reaction kettle heat treatment method Download PDFInfo
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- CN109457202A CN109457202A CN201811300925.2A CN201811300925A CN109457202A CN 109457202 A CN109457202 A CN 109457202A CN 201811300925 A CN201811300925 A CN 201811300925A CN 109457202 A CN109457202 A CN 109457202A
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- steel plate
- heat treatment
- clad steel
- tantalum
- reaction kettle
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Heat Treatment Of Articles (AREA)
- Furnace Details (AREA)
Abstract
The invention discloses a kind of tantalum zirconium clad steel plate reaction kettle heat treatment methods, tantalum zirconium clad steel plate reactor pressure container is placed in heat treatment electric furnace, by carrying out tooling sealing to tantalum zirconium clad steel plate reaction kettle container itself, by the argon gas for being passed through purity >=99.99% outside furnace body, using the slow row of buffering, pressure maintaining Diluted replacement, the tantalum material in tantalum zirconium clad steel plate reaction kettle is in completely inert gas shield atmosphere with zirconium material to be heat-treated, when heat treatment is warming up to 300 DEG C, it is heated using the heating rate of 55~110 DEG C/h, when temperature reaches 555 DEG C ± 10 DEG C, keep the temperature 240~270min, then 55~140 DEG C/h of cooling velocity is controlled, until temperature is down to 300 DEG C.A kind of heat treatment method of tantalum zirconium clad steel plate reaction kettle of the invention, it can effectively avoid the high-temperature oxydation situation of tantalum zirconium clad steel plate reaction kettle internal coated layer tantalum material, zirconium material, it prevents active metal coating in equipment heat treatment process from aoxidizing, improves equipment service performance, prolong the service life.
Description
Technical field
The present invention relates to tantalum zirconium clad steel plate reaction kettle technical field, at specially a kind of tantalum zirconium clad steel plate reaction kettle heat
Reason method.
Background technique
Tantalum is industrial important meals material, with fusing point is high, processing performance is good, corrosion-resistant, steam forces down, expansion is
A series of excellent performances such as small are counted, have important application in pressure vessel manufacturing field.But tantalum material is easy to during heat treatment
Occur high-temperature oxydation, generate one layer of white powder or sheet oxidation, cause tantalum coating thickness occur be thinned, and corrosion resistance or
The decline of other service performances.At present in tantalum composite plate pressing pressure container manufacturing operation, if groundwork thickness has reached heat treatment requirements,
General pressure vessel manufacturer man can paint high temperature-proof coating in tantalum coating and carry out heat treatment coating protection, at the method heat
After the completion of reason, the coating of clad surface is particularly difficult to remove, and the damage of coating is be easy to cause in removal process.Pressure also
Force container manufacturing firm can carry out rubbing down, pickling to remove oxide to the tantalum coating of oxidation after the completion using being directly heat-treated, this
It will cause being thinned for tantalum coating, influence the service life of equipment.It is hot when needing to carry out for this tantalum pressure container of composite board
When processing, there is presently no comparative maturity, effects preferably to prevent tantalum coating oxidizing thermal treatment method or technique.
Summary of the invention
It is the purpose of the present invention is to provide a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method, tantalum zirconium clad steel plate is anti-
Kettle pressure vessel is answered to be placed in heat treatment electric furnace, it is close by carrying out tooling to tantalum zirconium clad steel plate reaction kettle container itself
Envelope, using the slow row of buffering, pressure maintaining Diluted replacement, keeps tantalum zirconium steel compound by being passed through the argon gas of purity >=99.99% outside furnace body
Tantalum material in plate reaction kettle, which is in completely inert gas shield atmosphere, to be heat-treated, and when heat treatment is warming up to 300 DEG C, is adopted
It is heated with the heating rate of 55~110 DEG C/h, when temperature reaches 555 DEG C ± 10 DEG C, then 240~270min of heat preservation is controlled
55~140 DEG C/h of cooling velocity processed, until temperature is down to 300 DEG C.
Preferably, the tooling sealing includes all pipes being connected to active metal coating inside container in sealing container
Mouthful.The gas shield atmosphere is not limited to argon gas, other inert gases.
Preferably, described to buffer slow row, the inflation of pressure maintaining Diluted replacement, deflation rate, dwell time and displacement number
Because the equipment size of heat treatment is not of uniform size can appropriate adjustment.
Preferably, the heat preservation duration of the heat treatment, temperature rate are according to the groundwork thickness size need of Equipment for Heating Processing
It is adjusted.
Compared with prior art, the beneficial effects of the present invention are: a kind of heat of tantalum zirconium clad steel plate reaction kettle of the invention
Processing method can effectively avoid the high-temperature oxydation situation of tantalum zirconium clad steel plate reaction kettle internal coated layer tantalum material, zirconium material, prevent equipment hot
Active metal coating aoxidizes in treatment process, improves equipment service performance, prolongs the service life.
Detailed description of the invention
Fig. 1 is tantalum zirconium clad steel plate reaction kettle heat treatment method schematic diagram；
Fig. 2 is tantalum zirconium clad steel plate reaction kettle heat treatment parameter curve graph；
Fig. 3 is tantalum zirconium clad steel plate reaction kettle equipment overview figure.
In figure: 1 air inlet pipe, 2 ferrule baffles, 3 nozzle sleeves, 4 tooling cylinders, 5 tooling cylinders, 6 escape pipes, 7 pressures
Strength valve, 8 relief valves, 9 tooling cylinder sealing baffles, 10 first supporting saddles, 11 second supporting saddles, 12 thirds support saddle
Seat, 13 upper covers, 14 upper shells, 15 lower shells, 16 lower heads.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
Embodiment 1
Tantalum zirconium clad steel plate reactor pressure container is placed in Re Chu by a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method
It manages in electric furnace, by carrying out tooling sealing to tantalum zirconium clad steel plate reaction kettle container itself, by being passed through purity outside furnace body
>=99.99% argon gas is in the tantalum material in tantalum zirconium clad steel plate reaction kettle using the slow row of buffering, pressure maintaining Diluted replacement
It is heat-treated in completely inert gas shield atmosphere, when heat treatment is warming up to 300 DEG C, using the heating of 55~110 DEG C/h
Speed is heated, and when temperature reaches 555 DEG C ± 10 DEG C, keeps the temperature 240~270min, then control 55~140 DEG C of cooling velocity/
H, until temperature is down to 300 DEG C.The tooling sealing is connected to including all in sealing container with active metal coating inside container
Nozzle.The gas shield atmosphere is not limited to argon gas, other inert gases.The buffering delays row, pressure maintaining
The inflation of Diluted replacement, deflation rate, dwell time and displacement number because the equipment size of heat treatment is not of uniform size can be appropriate
Adjustment.The heat preservation duration of the heat treatment, temperature rate need to be adjusted according to the groundwork thickness size of Equipment for Heating Processing
Example tantalum zirconium clad steel plate reaction kettle equipment in attached drawing mainly include upper cover 13, upper shell 14, lower shell 15,
Lower head 16 forms.Upper cover 13 is zirconium/titanium/steel composite board；Upper shell 14 is tantalum/zirconium/titanium steel composite board；Lower shell be tantalum/
Titanium/steel composite board；Lower head is tantalum/titanium/steel composite board.The application is to guarantee that active metal zirconium, tantalum coating are being set inside autoclave body
High-temperature oxydation does not occur in standby heat treatment process, spy invents following heat-treatment technology method and technological means, specific as follows:
Annealing device mainly includes air inlet pipe 1, ferrule baffle 2, nozzle sleeve 3, tooling cylinder 4, tooling cylinder
5, escape pipe 6, pressure air valve 7, relief valve 8, tooling cylinder sealing baffle 9 and the first supporting saddle 10, the second supporting saddle
11, third supporting saddle 12.
Air inlet pipe 1 uses carbon steel pipe, specification and length by equipment it is whole into after furnace at furnace body ventilation distance carry out it is real
Match, and wants and supply end interface matching；In one end insertion nozzle sealing baffle 2 of air inlet pipe 1, the other end, which leads to outside furnace body, to be connect
Supply port；It is welded on the outside of blind plate between air inlet pipe 1 and ferrule baffle 2 using manual welding；Ferrule baffle 2 and pipe
The first centering group of port sleeve 3 is soldered into, is welded inside and outside using manual welding；Nozzle sleeve 3 covers the equipment on lower head 16
It is welded using manual welding from outside between nozzle, with lower head base；Coaxial group to point solid welding between 4 lower head 16 of tooling cylinder
After fixed, manual welding can be used and be intermittently welded；After coaxial group to point solid welding is fixed between tooling cylinder 5 and upper cover 13, use
Manual welding continuously welds；It is welded between tooling cylinder sealing baffle 9 and tooling cylinder 5 using manual welding sealing, it is continuous to weld；Out
Tracheae 6 uses carbon steel pipe, specification product length by equipment it is whole into after furnace at furnace body ventilation distance carry out it is real match, and in furnace body
The matched pressure air valve 7 of outside size for connection and relief valve 8；5 top of one end insertion tooling cylinder of escape pipe 6, the other end are logical
To the outside of furnace body；It is welded on the outside of baffle between escape pipe 6 and tooling cylinder sealing baffle 9 using manual welding；By with top
Method completes autoclave body inner sealing using apparatus body.
First supporting saddle 10, the second supporting saddle 11, third supporting saddle 12 are placed into suitable position by attached drawing 1, prevent
Only autoclave body occurrence of equipment deformation or the problems such as shift in position during heat treatment.
After the completion of inner sealing, into the inert gas replacement stage.
First the relief valve 8 on the outside of furnace body is closed, applying argon gas (Ar.) is carried out to autoclave body inside using air inlet pipe 1 and is operated, is filled
It is inflated during argon gas using compared with slug flow amount, autoclave body internal pressure can be gradually increased at this time, and pressure is shown on pressure air valve 7
Force value closes argon filling when the pressure value on pressure air valve 7 reaches 0.1MPa, carries out pressure maintaining processing at this time, and pressure maintaining stands 5-
After 10min, relief valve 8 is opened, and be vented using slower flow, until showing that pressure value is 0 on pressure air valve 7, closing is let out
Pressure valve 8；Then second of applying argon gas, pressure maintaining, exhaust process are carried out in the same way；This process is carried out 3-5 times,
During this, the intracorporal air of kettle largely can all be replaced dry by continuous dilution displacement, the final intracorporal air of kettle
Only, remaining inert argon and extremely least a portion of air in autoclave body, will not during heat treatment aoxidize active metal coating
Generate damaging oxidation.The buffering proposed here it is the application delays row, pressure maintaining Diluted replacement.
Whether the air inside detection autoclave body is replaced completely, the application proposes that Mars inspection gas method is verified.
Because the outlet side of relief valve 8 is there are airflow influence, gas displacement can not sentence the atmosphere of outlet side using open fire in the process
It is disconnected, so being extended in the atmosphere of outlet side using a charcoal with Mars, if Mars extinguishes immediately, illustrate in autoclave body
Air with clean by basic conversion, examined using the method fast and convenient, and be more suitable for the environment of plant.It can certainly
It is detected using the opposed gas to change gear out of other atmosphere detection means.
After the completion of ventilation and detection, into heat treatment stages.
To electric furnace electrified regulation, equipment is heat-treated using the heat treatment process mode that guarantor is prolonged in cooling.Equipment
Room temperature heats up into stove heating, when temperature rises to the heating rate of 300 DEG C of control heating, in the heating rate model of 55~110 DEG C/h
As far as possible using quickly heating in enclosing, until temperature reaches 555 DEG C ± 10 DEG C, into holding stage, 240~270min is kept the temperature.Herein
In the heating process that heats up, because of autoclave body inner sealing, it is filled with inert gas, temperature, which increases gas expansion, increases autoclave body internal pressure
Greatly, during this when the pressure value on pressure air valve 7 is more than 0.1MPa, manual exhaust pressure release is carried out to relief valve 8.It can also be with
Using one-way pressure valve, instead of relief valve 8, when the pressure value on pressure air valve 7 is more than 0.1MPa, one-way pressure valve is arranged automatically
Gas pressure release.Cool down after heat preservation by the cooling velocity of 55~140 DEG C/h, until temperature is down to 300 DEG C, heat treatment process
Curve is as shown in Fig. 2.In cool down, gas volume reduces in autoclave body, will form negative pressure, so in cooling down
In the process, it is indicated according to the pressure value on pressure air valve 7, needs to compensate heating to pouring appropriate inert gas inside autoclave body again
The gas being discharged in the process prevents from generating negative pressure inside autoclave body.
The above is only the specific embodiment that the present invention is directed to 3 equipment of attached drawing, and other features, titanium are multiple
It is anti-that method progress active metal coating described herein can be used in plywood and the coloured pressure vessel product of other structures etc.
High-temperature oxydation heat treatment, and obtain good effect.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method, which is characterized in that hold tantalum zirconium clad steel plate reactor pressure
Device be placed in heat treatment electric furnace in, by carrying out tooling sealing to tantalum zirconium clad steel plate reaction kettle container itself, by furnace body outside
Portion is passed through the argon gas of purity >=99.99%, using the slow row of buffering, pressure maintaining Diluted replacement, makes in tantalum zirconium clad steel plate reaction kettle
Tantalum material be in completely inert gas shield atmosphere and be heat-treated, when heat treatment is warming up to 300 DEG C, using 55~110
DEG C/heating rate of h heated, when temperature reaches 555 DEG C ± 10 DEG C, 240~270min is kept the temperature, cooling velocity is then controlled
55~140 DEG C/h, until temperature is down to 300 DEG C.
2. a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method according to claim 1, which is characterized in that the tooling
Sealing includes all nozzles being connected to active metal coating inside container in sealing container.
3. a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method according to claim 1, which is characterized in that the gas
Protection atmosphere is not limited to argon gas, other inert gases.
4. a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method according to claim 1, which is characterized in that the buffering
Slow row, the inflation of pressure maintaining Diluted replacement, deflation rate, the dwell time and replace number because heat treatment equipment size size not
One can appropriate adjustment.
5. a kind of tantalum zirconium clad steel plate reaction kettle heat treatment method according to claim 1, which is characterized in that at the heat
The heat preservation duration of reason, temperature rate need to be adjusted according to the groundwork thickness size of Equipment for Heating Processing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811300925.2A CN109457202B (en) | 2018-11-02 | 2018-11-02 | Tantalum-zirconium steel composite plate reaction kettle heat treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811300925.2A CN109457202B (en) | 2018-11-02 | 2018-11-02 | Tantalum-zirconium steel composite plate reaction kettle heat treatment method |
Publications (2)
| Publication Number | Publication Date |
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| CN109457202A true CN109457202A (en) | 2019-03-12 |
| CN109457202B CN109457202B (en) | 2020-12-01 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2663471B2 (en) * | 1988-01-08 | 1997-10-15 | 日本電気株式会社 | Manufacturing method of insulating thin film |
| CN1934465A (en) * | 2004-02-26 | 2007-03-21 | 富士胶片株式会社 | Optical compensation sheet, polarizing plate and liquid crystal display device |
| CN101493284A (en) * | 2009-02-24 | 2009-07-29 | 上海大学 | Crucible for fusing titan and method of preparation thereof |
| CN107379683A (en) * | 2017-07-31 | 2017-11-24 | 河南永威教育发展有限公司 | A kind of wood substrate high pressure decorative door-plate and preparation method thereof |
| CN108453403A (en) * | 2017-02-20 | 2018-08-28 | 中国石油天然气股份有限公司 | The welding method of Pressure container manhole flange anticorrosion sieve plate |
-
2018
- 2018-11-02 CN CN201811300925.2A patent/CN109457202B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2663471B2 (en) * | 1988-01-08 | 1997-10-15 | 日本電気株式会社 | Manufacturing method of insulating thin film |
| CN1934465A (en) * | 2004-02-26 | 2007-03-21 | 富士胶片株式会社 | Optical compensation sheet, polarizing plate and liquid crystal display device |
| CN101493284A (en) * | 2009-02-24 | 2009-07-29 | 上海大学 | Crucible for fusing titan and method of preparation thereof |
| CN108453403A (en) * | 2017-02-20 | 2018-08-28 | 中国石油天然气股份有限公司 | The welding method of Pressure container manhole flange anticorrosion sieve plate |
| CN107379683A (en) * | 2017-07-31 | 2017-11-24 | 河南永威教育发展有限公司 | A kind of wood substrate high pressure decorative door-plate and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN109457202B (en) | 2020-12-01 |
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