EP0987350A2 - Procédé et dipositif pour l'application d'une couche en phosphate sur des pièces - Google Patents

Procédé et dipositif pour l'application d'une couche en phosphate sur des pièces Download PDF

Info

Publication number: EP0987350A2
Authority: EP; European Patent Office
Prior art keywords: workpiece; phosphating; bath; unit; pickling
Prior art date: 1998-08-06
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.): Granted

Application number

EP99890263A

Other languages

German (de)

English (en)

Other versions

EP0987350B1 (fr

EP0987350A3 (fr

Inventor

Heinz Dipl.-Ing. Stockner

Heinz Fischer

Josef Hönecke

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Voestalpine Wire Rod Austria GmbH

Original Assignee

Voestalpine Wire Rod Austria GmbH

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

1998-08-06

Filing date

1999-08-05

Publication date

2000-03-22

1999-08-05 Application filed by Voestalpine Wire Rod Austria GmbH filed Critical Voestalpine Wire Rod Austria GmbH

1999-08-05 Priority to AT99890263T priority Critical patent/ATE331825T1/de

1999-08-05 Priority to SI9930917T priority patent/SI0987350T1/sl

2000-03-22 Publication of EP0987350A2 publication Critical patent/EP0987350A2/fr

2004-03-24 Publication of EP0987350A3 publication Critical patent/EP0987350A3/fr

2006-06-28 Application granted granted Critical

2006-06-28 Publication of EP0987350B1 publication Critical patent/EP0987350B1/fr

2019-08-05 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

Links

229910019142 PO4 Inorganic materials 0.000 title claims abstract description 31
NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 30
239000010452 phosphate Substances 0.000 title claims abstract description 30
238000000576 coating method Methods 0.000 title claims abstract description 24
239000011248 coating agent Substances 0.000 title claims abstract description 22
238000000034 method Methods 0.000 title claims abstract description 22
238000011282 treatment Methods 0.000 claims abstract description 28
XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
238000010438 heat treatment Methods 0.000 claims abstract description 14
229910045601 alloy Inorganic materials 0.000 claims abstract description 10
239000000956 alloy Substances 0.000 claims abstract description 10
229910052742 iron Inorganic materials 0.000 claims abstract description 7
238000011144 upstream manufacturing Methods 0.000 claims abstract description 6
238000005554 pickling Methods 0.000 claims description 29
229910000831 Steel Inorganic materials 0.000 claims description 11
238000005868 electrolysis reaction Methods 0.000 claims description 11
239000010959 steel Substances 0.000 claims description 11
238000001035 drying Methods 0.000 claims description 7
230000001105 regulatory effect Effects 0.000 claims description 7
238000002360 preparation method Methods 0.000 claims description 5
239000007788 liquid Substances 0.000 claims description 4
238000009835 boiling Methods 0.000 claims description 2
150000001768 cations Chemical class 0.000 claims description 2
230000006698 induction Effects 0.000 claims description 2
235000021317 phosphate Nutrition 0.000 description 26
LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 4
229910000165 zinc phosphate Inorganic materials 0.000 description 4
229910001069 Ti alloy Inorganic materials 0.000 description 3
239000000314 lubricant Substances 0.000 description 3
239000007800 oxidant agent Substances 0.000 description 3
238000012545 processing Methods 0.000 description 3
XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
230000002378 acidificating effect Effects 0.000 description 2
230000033228 biological regulation Effects 0.000 description 2
230000015572 biosynthetic process Effects 0.000 description 2
238000010924 continuous production Methods 0.000 description 2
230000002349 favourable effect Effects 0.000 description 2
238000003780 insertion Methods 0.000 description 2
230000037431 insertion Effects 0.000 description 2
230000001050 lubricating effect Effects 0.000 description 2
239000000463 material Substances 0.000 description 2
239000000243 solution Substances 0.000 description 2
239000010936 titanium Substances 0.000 description 2
229910000851 Alloy steel Inorganic materials 0.000 description 1
229910002651 NO3 Inorganic materials 0.000 description 1
NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
238000005299 abrasion Methods 0.000 description 1
239000013543 active substance Substances 0.000 description 1
239000000853 adhesive Substances 0.000 description 1
230000001070 adhesive effect Effects 0.000 description 1
230000002411 adverse Effects 0.000 description 1
239000003513 alkali Substances 0.000 description 1
238000000137 annealing Methods 0.000 description 1
239000007864 aqueous solution Substances 0.000 description 1
238000005452 bending Methods 0.000 description 1
239000013522 chelant Substances 0.000 description 1
238000006243 chemical reaction Methods 0.000 description 1
239000003153 chemical reaction reagent Substances 0.000 description 1
239000003795 chemical substances by application Substances 0.000 description 1
150000001875 compounds Chemical class 0.000 description 1
238000005260 corrosion Methods 0.000 description 1
230000007797 corrosion Effects 0.000 description 1
238000005520 cutting process Methods 0.000 description 1
230000008021 deposition Effects 0.000 description 1
238000013461 design Methods 0.000 description 1
238000001514 detection method Methods 0.000 description 1
230000009189 diving Effects 0.000 description 1
238000004049 embossing Methods 0.000 description 1
238000003306 harvesting Methods 0.000 description 1
238000007654 immersion Methods 0.000 description 1
150000002500 ions Chemical class 0.000 description 1
230000007257 malfunction Effects 0.000 description 1
238000004519 manufacturing process Methods 0.000 description 1
239000000203 mixture Substances 0.000 description 1
150000004767 nitrides Chemical class 0.000 description 1
150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
238000000275 quality assurance Methods 0.000 description 1
238000009991 scouring Methods 0.000 description 1
238000007493 shaping process Methods 0.000 description 1
239000010935 stainless steel Substances 0.000 description 1
229910001220 stainless steel Inorganic materials 0.000 description 1
238000013517 stratification Methods 0.000 description 1
239000000126 substance Substances 0.000 description 1
238000004381 surface treatment Methods 0.000 description 1
229910052719 titanium Inorganic materials 0.000 description 1
239000011701 zinc Substances 0.000 description 1
229910052725 zinc Inorganic materials 0.000 description 1

Images

Classifications

- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/36—Phosphatising

Definitions

the invention relates to a method for applying a Phosphate coating on workpieces with a large longitudinal extension Iron-based alloys, especially on low-alloy or unalloyed steels in Form of wires or rods using electrical current.
the invention further comprises a device for applying a Phosphate coating on workpieces of large longitudinal extent Iron based alloys, especially on low alloyed or unalloyed steels in Form of wires or rods, consisting of at least the components: electrolytically operable phosphating unit, drying device, Provisioning, feeding and discharge devices for the workpiece.
Optimal stratification conditions can be achieved through precise coordination of the Phosphate concentration, accelerating the type and amount of added active agents as well as the temperature and pH in the bath.
the phosphate layers formed usually consist of two layers, the the former adheres firmly to the workpiece and the upper layer part has little adhesion. In a practical application of phosphating are therefore Process conditions to choose in which the loose layer part is formed as low as possible. Furthermore, by the procedural conditions the structure of the phosphate layer determines which structure the Adhesion of a lubricant to the surface is affected.
a non-cutting deformation for example drawing steel wires with high Deformation degrees and low tool wear, for example the It is to achieve drawing dies with savings from intermediate annealing treatments important that the surface of the workpiece both over its circumference and along its length a high adhesive strength, uniform trained, required thickness and a fine crystalline surface structure of the Has phosphate layer.
the correct phosphate layer thickness is special Importance because too thick layers of friction, especially at the first Process step or when harvesting train, if necessary, increase significantly.
too thin or uneven across the circumference of the workpiece Phosphating to tear open the layer during the train, making worse Surface quality of the production result and less durability of the drawing dies of the last moves can be caused.
EP 288 853 describes a method for preparing workpieces known from titanium or titanium alloys, in which the workpieces in one aqueous, acidic zinc phosphate-containing phosphating solution appears and creates a zinc phosphate coating on the surface by cathodic electrolysis. Titanium and titanium alloys are chemically more resistant than steel, so that it is difficult to apply suitable lubricant carrier layers.
the invention has for its object the shortcomings of the previously known Eliminate phosphating treatments and an economical process specify with which a firmly adhering, fine crystalline phosphate coating with a constant and selectable thickness in cross-section and with length constant basis weight on workpieces made of iron-based alloys, in particular on low-alloy steel wires.
a firmly adhering, fine crystalline phosphate coating with a constant and selectable thickness in cross-section and with length constant basis weight on workpieces made of iron-based alloys, in particular on low-alloy steel wires One should Consistency of the coating even with different treatment times and different ion concentrations can be reached in the treatment bath.
the object is achieved in a generic method in that the Workpiece moved in the longitudinal direction relative to the device while doing so consecutively at least its near-surface area to an elevated one Brought to temperature, passed through at least one treatment bath and during the passage through a phosphating unit with a passage time between 1.5 and 19 seconds, preferably between 4 and 9 seconds, the surface of which when exposed to electrical current, preferably cathodic, and an adjustment of the electrical values depending on the Treatment parameters phosphated and the applied layer after drying the workpiece from the bath or left to dry becomes.
a relatively thick phosphate layer of 5 to 15 g / m 2 is required for further processing, for example for cold heading wires, it can be done in a simple manner these can be achieved by increasing the electrical cathode current.
it is important that at least the area near the surface is brought to an elevated temperature before the workpiece or the wire is introduced into the phosphating bath in order to form a fine-crystalline layer structure immediately after the introduction.
the advantageous phosphate layer formation on the workpiece can be supported when brought to a temperature between 45 ° C and 120 ° C and that Treatment bath on one between 45 ° C and the boiling point thereof is held, preferably with the proviso that the bath temperature is equal to or is set lower than the workpiece surface temperature.
the anode in the phosphating bath is advantageous is formed that their current density to a value of 0.1 to 0.6, in particular about 0.3 times the current density on the workpiece surface Electrolysis parameters can be controlled particularly effectively can be achieved.
the workpiece is moved through the treatment bath at a speed of 5 to 500 m / min, preferably from 30 to 100 m / min, and in the process has a phosphate coating on its surface 1 to 50 g / m 2 , preferably from 5 to 15 g / m 2 is applied.
a phosphate coating on its surface 1 to 50 g / m 2 , preferably from 5 to 15 g / m 2 is applied.
Higher deposition rates could bring further economic process advantages, but bring about a coarse structure of the phosphate layer, which can thereby have an adverse influence on the soaping and in particular on the first pull of the cold deformation of the wire.
Both the quality and the uniformity of the phosphating can be increased if the electrical values during cathodic electrolysis in Dependence on the cation concentration in and on the respective Processing time of the workpiece through the phosphating bath with the stipulation be regulated that the coating thickness over the workpiece length in is kept substantially constant and that if the Continuous movement lifted the workpiece out of the treatment bath or whose bath level is lowered below the workpiece level. So that's it too possible, in the event of system malfunctions, a negative impact on the To largely eliminate product quality.
a particular advantage with regard to continuous, highly economical phosphating can be achieved if the workpiece is pickled in the direction of its passage before being supported by the action of electrical current, in particular cathodic phosphating. It has proven to be useful if anodic pickling is carried out in one pass with a current density on the workpiece between 20 and 100 A / dm 2 , preferably between 40 and 80 A / dm 2 , and the pickling bath at a temperature between 45 ° C and 95 ° C is maintained.
the electrical power supply to the device can be simplified and its Regulations can be obtained effectively if the electrolytic pickling as well the same phosphating bath electrically connected in series and with regulated DC voltage can be supplied.
the material flow can be improved and the quality assurance of the coating can be increased if the workpiece with a cross-sectional area of 0.003 to 700 mm 2 is descaled and / or straightened linearly after removal from the stock.
the further aim of the invention is in a device of the type mentioned Art achieved in that the individual components of the device each one have such embodiment and arrangement that the workpiece in Longitudinal direction is movable through this and editable in this and that the phosphating unit at least one heating device for a is arranged upstream moving workpiece, the one with electric current supplyable unit, in particular an electrolysis unit for phosphating at least one, essentially tubular, surrounding the workpiece Has electrode and a feed and an inlet and outlet side Has overflow device for the phosphate bath.
the phosphating unit which can be supplied with electrical current in the Phosphating bath area and / or in the feed or discharge area Device for quickly lowering the bath level below the level of the Has workpiece.
the electrolytically operable phosphating unit has at least one, preferably essentially identical pickling unit, preferably is a particularly economical and safe one Phosphating with high product quality achievable.
the course of the coating can with regard to the structure and design of the Phosphate support on the workpiece are conveyed when the phosphating unit and the pickling unit and / or the preparation means for the liquid phosphating and Pickling media have adjustable heating devices for them.
the tube electrode of the pickling unit and Tubular electrode of the phosphating unit with the minus and plus pole of an adjustable one DC voltage source can be connected and that the workpiece is connectionless can be formed as an anode and a cathode.
Both for easy insertion of the workpiece and for improved Service conditions can be provided that are essentially concentric tubular electrode of the phosphating and / or arranged around the workpiece the pickling unit, viewed in the axial direction by at least two each Shell segments are formed and at least some of the shell segments can be lifted off or swung out.
Electrolysis bath Particularly effective in preventing short circuits in the Electrolysis bath has been found to be at least the bottom of the tubular electrode or a shell segment arranged in this way Provided holes or is designed in grid form.
the heating device as induction or as conductive acting system is formed and at least after the heating device, preferably in each case before and / or after the pickling unit of the phosphating unit and optionally the drying device, a temperature measuring device is arranged to determine and / or regulate the workpiece temperature, and if all measuring devices of the device with a central measuring and / or A control and / or documentation unit can be connected fully automatic operation of the device for applying a Phosphate coating and the highest quality of the coating can be achieved.
a pickled wire rod 11 is axially directed from a drum or a bundle 1, for example by a bending straightening system, and is introduced into a controllable heating device 3.
a regulation of the heating system which in particular acts inductively or conductively on the wire, can be carried out by a downstream temperature measuring device T 1 .
a phosphating unit 5 arranged downstream in the direction Z of passage of the wire 11 has a container for a phosphating medium 50 and has at least one feed 52 for this. On the inlet and outlet sides, the container has an overflow device 53, 54, through which the wire 11 can be brought through the phosphating bath largely without friction. In the event of faults or for insertion of the wire 11, the phosphating bath level can be lowered by means of a device 55.
a tubular electrode 51 in the container which can be designed in segment form, can be positioned essentially concentrically around the wire 11 and has a connection to the PLUS pole of a controllable direct current source 8, the MINUS pole of which is connected to a contact roller 51 '.
a heating device (not shown) for the phosphating medium 50 can be arranged in the container or in a preparation vessel.
the surface temperatures of the wire and those of the bath can be determined by means of temperature detection means T 3 T 4 T 5 , the measured values of which are preferably supplied to the control device.
the phosphating unit 5 are rinsing agents for the wire, not shown in FIG 11 downstream, which wire in the sequence a drying device 6 and optionally passes through a soaping device and in a drawing bench 7 is deformed.
FIG. 2 shows a device 5 for applying a Phosphate coating is shown schematically with an upstream pickling unit 4.
the pickling unit 4 in Fig.2 has in principle the same structure as that Phosphating unit 5, but can be constructed differently. Important here is that because pickling takes place in the same line as applying one Phosphating coating, the pickling parameters with concentration of the pickling liquid, Temperature of the pickling medium and the wire, electrolysis conditions as well Pickling time and the like are matched to the wire speed. It is particularly advantageous to conduct current via the tubular electrode 51 in the Phosphating medium 50 over the wire 11 and over the tube electrode 41 in the Pickling liquid 40 when the electrodes are connected to a controllable one DC power source 8.

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Chemical & Material Sciences (AREA)
Engineering & Computer Science (AREA)
Chemical Kinetics & Catalysis (AREA)
Electrochemistry (AREA)
Materials Engineering (AREA)
Metallurgy (AREA)
Organic Chemistry (AREA)
Chemical Treatment Of Metals (AREA)
Metal Extraction Processes (AREA)
Electroplating Methods And Accessories (AREA)

EP99890263A 1998-08-06 1999-08-05 Procédé et dipositif pour appliquer sur des pièces une couche de phosphate Expired - Lifetime EP0987350B1 (fr)

Priority Applications (2)

Application Number	Priority Date	Filing Date	Title
AT99890263T ATE331825T1 (de)	1998-08-06	1999-08-05	Verfahren und vorrichtung zum aufbringen eines phosphatüberzuges auf werkstücke
SI9930917T SI0987350T1 (sl)	1998-08-06	1999-08-05	Postopek in naprava za nanasanje fosfatne prevleke na obdelovance

Applications Claiming Priority (2)

Application Number	Priority Date	Filing Date	Title
AT0136398A AT405947B (de)	1998-08-06	1998-08-06	Verfahren und vorrichtung zum aufbringen eines phosphatüberzuges auf werkstücke
AT136398		1998-08-06

Publications (3)

Publication Number	Publication Date
EP0987350A2 true EP0987350A2 (fr)	2000-03-22
EP0987350A3 EP0987350A3 (fr)	2004-03-24
EP0987350B1 EP0987350B1 (fr)	2006-06-28

Family

ID=3512272

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP99890263A Expired - Lifetime EP0987350B1 (fr)	1998-08-06	1999-08-05	Procédé et dipositif pour appliquer sur des pièces une couche de phosphate

Country Status (5)

Country	Link
EP (1)	EP0987350B1 (fr)
AT (1)	AT405947B (fr)
CZ (1)	CZ295733B6 (fr)
DE (1)	DE59913624D1 (fr)
ES (1)	ES2268846T3 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
CN103741195A (zh) *	2013-12-23	2014-04-23	南通恒新金属工艺科技有限公司	钢丝电解磷化处理装置
CN112226755A (zh) *	2020-09-23	2021-01-15	山东大业股份有限公司	一种金属线材表面处理用磷化方法及装置

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* Cited by examiner, † Cited by third party
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DE102010028385A1 (de) *	2010-04-29	2011-11-03	Endress + Hauser Gmbh + Co. Kg	Verfahren und Vorrichtung zur Durchführung mindestens eines oberflächenmodifizierenden Prozesses an metallischen Werkstücken
CN102277612A (zh) *	2011-08-02	2011-12-14	威海银兴预应力线材有限公司	钢绞线拉丝在线磷化、皂化装置
CN102586839B (zh) *	2012-03-26	2014-12-10	南通高罕金属设备科技有限公司	折叠式开坯在线磷化处理装置
DE102015121349A1 (de) *	2015-12-08	2017-06-08	Staku Anlagenbau Gmbh	Vorrichtung zur Oberflächenbehandlung eines Endlosmaterials sowie deren Verwendung
CN108360042A (zh) *	2018-04-02	2018-08-03	江阴海瑞德机电科技有限公司	单丝过电轮装置
CN110863229A (zh) *	2019-12-09	2020-03-06	嘉兴东恒机械设备有限公司	新型金属材料无酸电解磷化工艺

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
FR1080914A (fr) *	1953-06-16	1954-12-14	United States Steel Corp	Procédé électrochimique de revêtement des surfaces en acier, produits destinés à sa mise en oeuvre et produits en résultant
GB1165014A (en) *	1966-08-22	1969-09-24	Herbert Kenmore	Apparatus for Treating Wire and Rods.
JPS5837391B2 (ja) *	1980-02-21	1983-08-16	新日本製鐵株式会社	燐酸塩処理性に優れた冷延鋼板の製造方法
JPS58100902A (ja) *	1981-12-09	1983-06-15	Hitachi Ltd	広幅鋼帯の分割処理法
US5087342A (en) *	1988-04-07	1992-02-11	Seneca Wire And Manufacturing Company	Continuous steel strand electrolytic processing
JPH0436498A (ja) *	1990-06-01	1992-02-06	Nippon Parkerizing Co Ltd	鉄鋼線材の表面処理方法

1998
- 1998-08-06 AT AT0136398A patent/AT405947B/de not_active IP Right Cessation
1999
- 1999-07-30 CZ CZ19992710A patent/CZ295733B6/cs not_active IP Right Cessation
- 1999-08-05 EP EP99890263A patent/EP0987350B1/fr not_active Expired - Lifetime
- 1999-08-05 ES ES99890263T patent/ES2268846T3/es not_active Expired - Lifetime
- 1999-08-05 DE DE59913624T patent/DE59913624D1/de not_active Expired - Fee Related

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number	Priority date	Publication date	Assignee	Title
CN103741195A (zh) *	2013-12-23	2014-04-23	南通恒新金属工艺科技有限公司	钢丝电解磷化处理装置
CN103741195B (zh) *	2013-12-23	2016-06-15	南通恒新金属工艺科技有限公司	钢丝电解磷化处理装置
CN112226755A (zh) *	2020-09-23	2021-01-15	山东大业股份有限公司	一种金属线材表面处理用磷化方法及装置
CN112226755B (zh) *	2020-09-23	2023-06-23	山东大业股份有限公司	一种金属线材表面处理用磷化方法及装置

Also Published As

Publication number	Publication date
CZ295733B6 (cs)	2005-10-12
ATA136398A (de)	1999-05-15
AT405947B (de)	1999-12-27
EP0987350B1 (fr)	2006-06-28
ES2268846T3 (es)	2007-03-16
EP0987350A3 (fr)	2004-03-24
CZ271099A3 (cs)	2000-03-15
DE59913624D1 (de)	2006-08-10

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