CN107723663A - A kind of apparatus and method in high strength steel surface continuous vacuum evaporation metal antimony - Google Patents

A kind of apparatus and method in high strength steel surface continuous vacuum evaporation metal antimony Download PDF

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Publication number
CN107723663A
CN107723663A CN201710881086.7A CN201710881086A CN107723663A CN 107723663 A CN107723663 A CN 107723663A CN 201710881086 A CN201710881086 A CN 201710881086A CN 107723663 A CN107723663 A CN 107723663A
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antimony
strength steel
evaporation
heater
adsorbent
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CN107723663B (en
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苏旭平
卓鑫池
刘亚
王建华
吴长军
涂浩
彭浩平
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Changzhou University
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Changzhou University
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/26Vacuum evaporation by resistance or inductive heating of the source
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/26Methods of annealing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING 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
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/68Temporary coatings or embedding materials applied before or during heat treatment
    • C21D1/70Temporary coatings or embedding materials applied before or during heat treatment while heating or quenching
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14Metallic material, boron or silicon
    • C23C14/16Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The present invention relates to a kind of apparatus and method in high strength steel surface continuous vacuum evaporation metal antimony.By being heated at high temperature metallic antimony; it is allowed to gasification and antimony molecule deposition is to the relatively low surface of steel plate of temperature; form fine and close solid diaphragm; the problem of making platability be deteriorated because of surface generation selective oxidation when fundamentally improving continuous zinc coating; guarantee is provided to provide high hot dip plated steel quality, there is considerable Social benefit and economic benefit.

Description

A kind of apparatus and method in high strength steel surface continuous vacuum evaporation metal antimony
Technical field
The present invention relates to galvanizing by dipping technical field, it is related to before a kind of annealing in the method for high strength steel surface preparation, Specifically, a kind of method in the hole continuous vacuum evaporation metal antimony of high strength steel surface three is referred to.
Background technology
Vacuum vapor plating (evaporation) is that under vacuum, heating evaporation material is allowed to the substrate surface that gasifies and be deposited on Solid film is formed, is a kind of physical phenomenon.It is widely used in machinery, electrovacuum, radio, optics, atomic energy, space skill The fields such as art.Its oxidation potential of metallic antimony is less than iron, and oxidation reaction during annealing is not related to the element substantially.Meanwhile the steam of antimony Pressure is higher, and in vacuum environment, antimony is 10 in the vapour pressure corresponding to 677 DEG C-2Torr。
Galvanizing by dipping, it is that steel component immerses in the zinc liquid of melting a kind of method for obtaining metal cladding.With high pressure Transmission of electricity, traffic, communication career develop rapidly, to the quality requirement of galvanizing by dipping also more and more higher.At present, applied to industrial production Continuous zinc coating method have a many kinds, such as Sendzimir methods, U.S. steel connection method, Wheeling methods, Selas methods.
But current most of galvanizing production is produced by Sendzimir methods.Typical Sendzimir methods, steel plate are necessary Through over cleaning, to remove the cold rolling on surface, oil, carbon and ferrous powder granules.The solution of cleaning is usually 1.5%~2.5% NaOH Solution.Next steel plate is dried up with low-pressure gas.Then enter back into heating and heat preservation zone carries out recrystallization annealing.From annealing furnace After out, steel plate is cooled to the temperature of slightly above zinc pond (460 DEG C), is then immersed in zinc pond.
It is well known that in the annealing stage of continuous zinc coating line, because temperature is too high, steel and active gases can occur very So-called selective oxidation will occur for complicated reaction, the wherein alloying element of surface of steel plate;" selective oxidation " refers in steel Behavior of the stronger alloying element prior to matrix Fe Element generation oxides with oxygen affinity.And in DP steel, due to Si, The selective oxidation of the alloying elements such as Mn, surface of steel plate cover the oxide of these alloying elements, and its platability can be deteriorated.Institute With the problem of variation for DP steel platability, it is necessary to find and reduce the effective way that selective oxidation occurs for its surface.
The content of the invention
The present invention is intended to provide one kind is simple to operate, economical and practical and is adapted to industrial quantity-produced high strength steel annealing Preceding preprocess method, by being heated at high temperature metallic antimony, it is allowed to gasification and antimony molecule deposition is to the relatively low surface of steel plate of temperature, shape Into the solid diaphragm of densification, as shown in Figure 1, 2, the selective oxygen of surface of steel plate can be effectively reduced by the implementation of the present invention Change, make oxide on surface SiO2, MnO and Mn-Si composite oxides significantly reduce, enhancing later stage zinc-plated platability.
The present invention implement its purpose technical scheme be:
A kind of apparatus and method in the hole continuous vacuum evaporation metal antimony of high strength steel surface three, it is technically characterized in that: Vacuum vapor plating pre-processes to high strength steel, and oxide when making the high strength steel anneal significantly reduces, and specific steps are such as Under:
1. whole evaporation process is carried out in a vacuum chamber, vacuum is 1 × 10-2Pa。
2. the matrix of high strength steel is iron, trace additives include carbon, silicon, manganese, chromium.
3. evaporation described device includes:Vacuum chamber, detection contact pilotage and three hole antimony regulus vaporization chambers;Three hole antimony regulus vaporization chambers are located at In vacuum chamber wall body, along high-strength steel sheet specular, face centered on occuping the high-strength steel sheet in whole vacuum chamber center The two-sided both sides of high strength steel, are divided into left side vaporization chamber and right side vaporization chamber, structure are identical:Left side vaporization chamber includes vaporization chamber wall Body, around resistive band, adsorbent, adsorbent heater, temperature measurer, evaporation source antimony regulus, evaporation heater, cooling circulating water, absolutely Edge substrate.Vaporization chamber wall bottom is provided with dielectric base, and dielectric base is provided with evaporation source antimony regulus, and evaporation source antimony regulus is surrounded by Evaporation heater, is provided with cooling circulating water between evaporation source antimony regulus and dielectric base, evaporation heater is provided with temperature measurer, steamed Wall outer side is placed equidistant three tongues with holes on the right side of hair room, and tongue is provided with tongue mouth, nestles up wall on the right side of vaporization chamber The scattered placement adsorbent in outside and adsorbent heater, adsorbent and adsorbent heater abut, and substrate heater is against high-strength Steel plate is spent, detection contact pilotage contacts detection below steel plate with steel plate.The evaporation heater is frequency spiral coil;The absorption Agent heater is electromagnetic heater;The substrate heater is around resistive band.
Tongue uses square structure, is highly 50~70 ㎝, width is bigger 5~10 ㎝ than the high-strength steel sheet width of required evaporation.
Tongue mouth uses square structure, highly consistent with tongue for 5~10 ㎝, width.
The distance of high-strength steel sheet and tongue with holes is 15 ㎝.
4. the adsorbent Zr-16Al of vaporization chamber wall outer side is preheated 3 hours at 800 DEG C using adsorbent heater, Active gases in vacuum chamber is removed, now steel plate is in room temperature with antimony regulus, after the completion of absorption, stops the heating of adsorbent.
5. evaporation source antimony regulus is incubated substrate steel disc by utilization evaporation heater in 677 DEG C of continuous heatings, circular resistive band At low temperature (230~300 DEG C).
6. high-strength steel sheet slow transits through left and right sides tongue spray antimony mouth in three times from top to bottom, right at 677 DEG C using antimony It is 10 to answer vapour pressure-2Torr, evaporation effect is optimal and high temperature atomic can be covered high strength steel is two-sided to the characteristic that low temperature face is moved Cover uniform antimony diaphragm.
7. film thickness is deposited using contact pilotage detection is detected in the steel plate after the completion of cooling.
The specific implementation step of described device is:
The adsorbent Zr-16Al of vaporization chamber wall outer side is preheated 3 hours at 800 DEG C using adsorbent heater, gone Except active gases in vacuum chamber, now steel plate is in room temperature with antimony regulus, after the completion of absorption, stops the heating of adsorbent.
Using evaporation heater by evaporation source antimony regulus in 677 DEG C of continuous heatings, while utilize cooling circulating water regulation and control mutation Temperature, make the insulation of substrate steel disc in low temperature (230~300 DEG C), the registration change of observation temperature measurer around resistive band.
Drive device, which produces driving force, makes high-strength steel sheet slow transit through left and right sides tongue spray antimony in three times from top to bottom Mouthful, it is 10 using saturated vapour pressure-2Torr evaporation effects are optimal and high temperature atomic can be to the characteristic that low temperature face is moved, by high intensity The uniform antimony diaphragm of the two-sided covering of steel.
Film thickness is deposited using contact pilotage detection is detected in steel plate after the completion of cooling.
When changing antimony regulus, it need to stop heating, after the completion of replacing, restart from step 1.
The method of the hole continuous vacuum evaporation metal antimony of high strength steel surface three of the present invention, one is provided for continuous hot-dipping galvanizing The method of kind pretreatment, the oxide on surface, preprocessing process are completed in a vacuum chamber when reducing zinc-plated.Fundamentally improve The problem of making platability be deteriorated because of surface generation selective oxidation during continuous zinc coating, provided to provide high hot dip plated steel quality Ensure, there is considerable Social benefit and economic benefit.
Brief description of the drawings
Accompanying drawing described herein as is used for being further explained the present invention, forms the part of the application, of the invention shows Meaning property is illustrated for explaining the present invention, does not form inappropriate limitation of the present invention, protection scope of the present invention is not limited to following Schematic diagram.
Fig. 1 is the high strength steel surface FE-SEM figures of 1000 times of completion evaporation metal antimony.
Fig. 2 is the high strength steel surface FE-SEM figures of 10000 times of completion evaporation metal antimony.
Fig. 3 is internal vacuum chamber schematic device.
Drawing reference numeral
[1] dielectric base [2] cooling circulating water [3] evaporation source antimony regulus
[4] frequency spiral coil [5] temperature measurer [6] electromagnetic heater
[7] adsorbent [8] is around resistive band [9] high-strength steel sheet
[10] tongue spray antimony mouth [11] tongue [12] vacuum chamber wall
[13] vaporization chamber wall [14] detection contact pilotage
Embodiment
Specifically the present embodiment is introduced below in conjunction with the accompanying drawings to elaborate:The present embodiment using technical solution of the present invention as Under the premise of implemented, give detailed embodiment and process, but protection scope of the present invention is not limited to following embodiments.
The adsorbent 7 of vaporization chamber wall outer side is preheated 3 hours at 800 DEG C using electromagnetic heater 6, removes vacuum chamber Interior active gases, now steel plate 9 and antimony regulus 3 be in room temperature, after the completion of absorption, stop the heating of adsorbent.
Using frequency spiral coil 4 by evaporation source antimony regulus 3 in 677 DEG C of continuous heatings, while regulated and controled using cooling circulating water 2 Abrupt temp, substrate steel disc 9 is set to be incubated in low temperature (230~300 DEG C), the registration change of observation temperature measurer 5 around resistive band 8.
Drive device, which produces driving force, makes high-strength steel sheet 9 slow transit through left and right sides tongue 11 in three times from top to bottom Tongue spray antimony mouth 10, is 10 using saturated vapour pressure-2Torr evaporation effects are optimal and high temperature atomic can be to the spy that low temperature face is moved Property, by the uniform antimony diaphragm of the two-sided covering of high strength steel.
Film thickness is deposited using the detection of contact pilotage 14 is detected in steel plate 9 after the completion of cooling.
The method of the hole continuous vacuum evaporation metal antimony of high strength steel surface three of the present invention, one is provided for continuous hot-dipping galvanizing The method of kind pretreatment, the oxide on surface, preprocessing process are completed in a vacuum chamber when reducing zinc-plated.Fundamentally improve The problem of making platability be deteriorated because of surface generation selective oxidation during continuous zinc coating, provided to provide high hot dip plated steel quality Ensure, there is considerable Social benefit and economic benefit.

Claims (7)

  1. A kind of 1. device in high strength steel surface continuous vacuum evaporation metal antimony, it is characterised in that:Described device includes:Vacuum Room, detection contact pilotage and three hole antimony regulus vaporization chambers;Three hole antimony regulus vaporization chambers are located in vacuum chamber wall body, to occupy in whole vacuum chamber Along high-strength steel sheet specular centered on the high-strength steel sheet of centre, the two-sided both sides of face high strength steel, it is divided into left side vaporization chamber It is identical with right side vaporization chamber, structure:Left side vaporization chamber includes vaporization chamber wall, around resistive band, adsorbent, adsorbent heating Device, temperature measurer, evaporation source antimony regulus, evaporation heater, cooling circulating water, dielectric base;Vaporization chamber wall bottom is provided with insulation base Bottom, dielectric base are provided with evaporation source antimony regulus, and evaporation source antimony regulus is surrounded by evaporation heater, evaporation source antimony regulus and dielectric base Between be provided with cooling circulating water, evaporation heater is provided with temperature measurer, and wall outer side is placed equidistant three bands on the right side of vaporization chamber Hole tongue, tongue are provided with tongue mouth, nestle up the scattered placement adsorbent in outside and the adsorbent heating of wall on the right side of vaporization chamber Device, adsorbent and adsorbent heater abut, and substrate heater abuts high-strength steel sheet, detection contact pilotage below steel plate with steel plate Contact detection.
  2. A kind of 2. device in high strength steel surface continuous vacuum evaporation metal antimony as claimed in claim 1, it is characterised in that: The evaporation heater is frequency spiral coil;The adsorbent heater is electromagnetic heater;The substrate heater is ring Around resistive band.
  3. A kind of 3. device in high strength steel surface continuous vacuum evaporation metal antimony as claimed in claim 1, it is characterised in that: Whole evaporation process is carried out in a vacuum chamber, and vacuum is 1 × 10-2Pa。
  4. A kind of 4. device in high strength steel surface continuous vacuum evaporation metal antimony as claimed in claim 1, it is characterised in that: Tongue uses square structure, is highly 50~70 ㎝, width is bigger 5~10 ㎝ than the high-strength steel sheet width of required evaporation.
  5. A kind of 5. device in high strength steel surface continuous vacuum evaporation metal antimony as claimed in claim 1, it is characterised in that: Tongue mouth uses square structure, highly consistent with tongue for 5~10 ㎝, width.
  6. A kind of 6. device in high strength steel surface continuous vacuum evaporation metal antimony as claimed in claim 1, it is characterised in that: The distance of high-strength steel sheet and tongue with holes is 15 ㎝.
  7. 7. device as claimed in claim 1 is utilized to exist in the method for high strength steel surface continuous vacuum evaporation metal antimony, its feature In:
    (1) the adsorbent Zr-16Al of vaporization chamber wall outer side is preheated 3 hours at 800 DEG C using adsorbent heater, removed Active gases in vacuum chamber, now steel plate and antimony regulus be in room temperature, after the completion of absorption, stop the heating of adsorbent;
    (2) insulation of substrate steel disc is made to exist in 677 DEG C of continuous heatings, circular resistive band evaporation source antimony regulus using evaporation heater 230~300 DEG C;
    (3) high-strength steel sheet slow transits through left and right sides tongue spray antimony mouth in three times from top to bottom, using antimony in 677 DEG C of corresponding steamings Air pressure is 10-2Torr, evaporation effect is optimal and high temperature atomic can be equal by the two-sided covering of high strength steel to the characteristic that low temperature face is moved Even antimony diaphragm;
    (4) film thickness is deposited using contact pilotage detection is detected in the steel plate after the completion of cooling down.
CN201710881086.7A 2017-09-26 2017-09-26 A kind of device and method in high strength steel surface continuous vacuum evaporation metal antimony Active CN107723663B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112262226A (en) * 2018-06-13 2021-01-22 安赛乐米塔尔公司 Vacuum deposition apparatus and method for coating a substrate
CN112505286A (en) * 2019-09-16 2021-03-16 中国科学院上海光学精密机械研究所 Detection device and method for zinc-induced liquid metal crack formation condition
WO2023072184A1 (en) * 2021-10-27 2023-05-04 宝山钢铁股份有限公司 Production method and production line for galvanized plate

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CN2632980Y (en) * 2003-07-16 2004-08-11 上海大学 Vacuum evaporating heater for producing organic electroluminescent thin membrane
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CN102732842A (en) * 2011-04-13 2012-10-17 韩商Snu精密股份有限公司 Depositing apparatus for forming thin film
CN103628025A (en) * 2012-08-21 2014-03-12 深圳富泰宏精密工业有限公司 Alloy coevaporation material and evaporation coating method employing alloy coevaporation material
CN105112914A (en) * 2015-08-31 2015-12-02 中国钢研科技集团有限公司 Continuous hot-dip galvanizing device and continuous hot-dip galvanizing method

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Publication number Priority date Publication date Assignee Title
CN2632980Y (en) * 2003-07-16 2004-08-11 上海大学 Vacuum evaporating heater for producing organic electroluminescent thin membrane
US20100252849A1 (en) * 2009-04-07 2010-10-07 Hitachi Cable, Ltd. Light-emitting element
CN102732841A (en) * 2011-04-13 2012-10-17 韩商Snu精密股份有限公司 Device for supplying materials
CN102732842A (en) * 2011-04-13 2012-10-17 韩商Snu精密股份有限公司 Depositing apparatus for forming thin film
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112262226A (en) * 2018-06-13 2021-01-22 安赛乐米塔尔公司 Vacuum deposition apparatus and method for coating a substrate
CN112262226B (en) * 2018-06-13 2023-03-21 安赛乐米塔尔公司 Vacuum deposition apparatus and method for coating a substrate
CN112505286A (en) * 2019-09-16 2021-03-16 中国科学院上海光学精密机械研究所 Detection device and method for zinc-induced liquid metal crack formation condition
CN112505286B (en) * 2019-09-16 2023-08-11 中国科学院上海光学精密机械研究所 Detection device and method for zinc-induced liquid metal crack formation condition
WO2023072184A1 (en) * 2021-10-27 2023-05-04 宝山钢铁股份有限公司 Production method and production line for galvanized plate

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