CN1236969A

CN1236969A - Technology for manufacturing white dumet wire

Info

Publication number: CN1236969A
Application number: CN 99115420
Authority: CN
Inventors: 王继红
Original assignee: Individual
Current assignee: Individual
Priority date: 1999-06-10
Filing date: 1999-06-10
Publication date: 1999-12-01
Anticipated expiration: 2019-06-10
Also published as: CN1109133C

Abstract

A technology for manufacturing white dumet wire includes such technological steps as selecting Fe-Ni alloy rod with constant linear expansion coefficient as core material, washing its surface with ethylene trichloride, annealing, anode erosion in H2SO4 solution, electroplating copper, annealing, cold drawing, plating N1, annealing drawing and continuous annealing. Its advanteges are easily controlled thickness of Ni layer and high oxidation resistance. Said white dumet wire can be used in electric vacuum device or as electric leading wire for higher air tightness of vacuum and longer service life.

Description

The production method of white Dumet wire

The present invention relates to a kind of production method of electrovacuum seal, sealing materials white Dumet wire.

Dumet wire is mainly used in electron tube, semiconductor device and bulb equipment, and the lead-in wire that dispatch from foreign news agency is led in the video picture device etc.The production method of existing Dumet wire generally is to adopt the iron-nickel alloy rod with certain coefficient of expansion, becomes bimetallic through multiple copper, after drawing, is coated with the borate goods on its surface again, and it is orange red to wine-colored finished product obtaining surface color.Because of this product surface is cuprous oxide and borate mixture, the easy moisture absorption, easy blackout be cannot say for sure pipe, simultaneously, thickness of oxide layer is wayward in production technology, too thick, the too thin sealing property that all influences itself and glass.

Task of the present invention provides a kind of method of producing white Dumet wire, is core with multiple copper iron-nickel alloy wire, three metallic composites that multiple nickel, drawing form.Nickel dam substitutes cuprous oxide and borate mixture, and surface color is silvery white.Because nickel layer thickness is easy to control, and nickel has good oxidization resistance, with white Dumet wire make electron tube, electric guide wire can improve its vacuum-tightness, prolongs its useful life.

It is as follows to finish concrete grammar of the present invention:

One, the production of multiple copper iron-nickel alloy wire core

1. the iron-nickel alloy rod of choosing the alignment coefficient of expansion is core, and the alloy of the 4J43 trade mark is comparatively desirable.Its chemical composition following (%) meets the GBn104-81 standard:

C	P	S	Mn	Si	?Ni	Fe
C	P	S	Mn	Si	?Ni	Fe	≤0.05	≤0.02	≤0.02	≤0.4	≤0.3	?42.5～43.5	Surplus

2. before electroplating the iron-nickel alloy rod is carried out surface clean with trichloroethylene, in hydrogen-burning stove, anneal, 1100～1150 ℃ of annealing temperatures, temperature retention time 2～3 hours is then at 160-200 grams per liter H ₂SO ₄Carry out anodic souring in the solution, copper facing again, the parameter of electroplating copper-plating technique is as follows:

The copper electroplating solution prescription is that concentration is the CuSO of 210～260 grams per liters ₄5H ₂O, concentration is the H of 50～75 grams per liters ₂SO ₄Reagent is pure, and temperature is between 20～32 ℃, and voltage is 2～4 volts in the groove, and working current density is 10～11 amperes/decimeter ², the copper facing time is 4 hours 15 minutes-6 hours 15 minutes.

3. the drawing of dumet

Iron-nickel alloy rod after the copper facing is carried out annealing in process in hydrogen-burning stove, annealing temperature is that 800～850 ℃, temperature retention time were assigned to 2 hours in 1 hour 20, and then carries out cold drawn silk processing.Draw the dumet rod on chain drawbench, being drawn into diameter is the dumet silk of φ≤4mm, and lubricant is with artificial hard oil fat.And then on vertical cylinder wire drawing machine, draw the dumet silk, be drawn into the dumet silk of diameter phi≤2mm, lubricant ammonia soap solution.

Two, electroplate multiple nickel

1. nickel plating pre-treatment

Before electroplating multiple nickel, the dumet silk is carried out annealing in process at hydrogen-burning stove, 800～850 ℃ of annealing temperatures earlier.Temperature retention time is to assign to 2 hours in 1 hour 20, with the soda boiling pineization of deoiling, uses hot water wash, with 1～10 second of chloroazotic acid etch, chargedly immediately after the washing puts into nickel bath nickel plating.

2. nickel plating technology

The nickel plating solution prescription

NiSO ₄7H ₂O 135 grams per liter Na ₂SO410H ₂O 70-80 grams per liter

H ₃BO ₃20-30 grams per liter NaCl 5-7 grams per liter

Temperature adopts room temperature, and pH value is that 5～5.5 current densities are 0.2～2 ampere/decimeter ², time 2-3 hour.

Nickel plating mode: adopt dumet silk one circle circle is evenly hung over the rack plating method or the continuous electroplating method of electroplating electronickelling on the hook rack.

Three, the drawing of white Dumet wire:

1. three metal composite wires after the nickel plating are carried out annealing in process at hydrogen-burning stove earlier, 800～880 ℃ of annealing temperatures, temperature retention time 1 hour to 1 hour 40 minutes is carried out cold drawn silk processing then.

2. three metal composite wires are drawn, intermediate annealing, 800～880 ℃ of annealing temperatures, temperature retention time 1 hour to 1 hour 40 minutes is drawn into the finished product of all size then.

3. the finished products of white Dumet wire adopts the continuous annealing furnace of hydrogen shield to carry out continuous annealing, 800～880 ℃ of annealing temperatures, 18～25 meters/minute of speed.

The iron-nickel alloy rod that embodiment chooses φ 8.0 * 1600mm is core, alloy designations 4J43

1. earlier 4J43 iron-nickel alloy rod is carried out surface clean with trichloroethylene, in hydrogen-burning stove, anneal, 1100 ℃ of annealing temperatures, temperature retention time 2 hours is then at 180 grams per liter H ₂SO ₄Carry out anodic souring in the solution.Electroplating the copper plating solution prescription is CuSO ₄5H ₂O 220 grams per liters, H ₂SO ₄(reagent is pure), 59 grams per liters, 30 ℃ of temperature, voltage is 4 volts in the groove, 10 amperes/decimeter of working current density ², 5-6 hour copper facing time.

2. the drawing of dumet

Iron-nickel alloy rod after the copper facing is carried out annealing in process in hydrogen-burning stove, annealing temperature is 800～850 ℃, temperature retention time was assigned to 2 hours in 1 hour 20, and then carry out cold drawn silk and process, on chain drawbench, draw the dumet rod, be drawn into the iron-nickel alloy wire that diameter phi is 3.8mm, lubricant: artificial hard oil fat.

On vertical cylinder wire drawing machine, draw the dumet silk, be drawn into the copper-beryllium silk of diameter phi 1.5mm.

3, electroplate multiple nickel

Before electroplating multiple nickel, the dumet silk is carried out annealing in process at hydrogen-burning stove, 800～850 ℃ of annealing temperatures earlier, temperature retention time is to assign to 2 hours in 1 hour 20, with the soda boiling pineization of deoiling, uses hot water wash, with 1～10 second of chloroazotic acid etch, chargedly immediately after the washing put into nickel bath nickel plating.The nickel plating technology parameter is as follows: the nickel plating solution prescription

NiSO ₄7H ₂O 135 grams per liter Na ₂SO ₄10H ₂O 70-80 grams per liter

H ₃BO ₃20-30 grams per liter NaCl 5-7 grams per liter

Temperature adopts room temperature, and pH value is 5～5.5, and current density is 0.2～2 ampere/decimeter ², time 2-3 hour.

Nickel plating mode: adopt rack plating method or continuous electroplating method.

4, the drawing of white Dumet wire:

Claims

1. method of producing Dumet wire is characterized in that may further comprise the steps:

(1) produces multiple copper iron-nickel alloy wire core

1. the iron-nickel alloy rod of choosing the alignment coefficient of expansion is core, and chemical composition is (%): C≤0.05, P≤0.02, and S≤0.02, Mn≤0.4, Si≤0.3, Ni:42.5～4 3.5, surplus is Fe, meets the GBn104-81 standard;

2. the iron-nickel alloy rod is carried out surface clean with trichloroethylene, annealing then is again at 160-200 grams per liter H ₂SO ₄Carry out anodic souring in the solution, electroplate copper facing then;

3. the iron-nickel alloy rod after the copper facing is carried out annealing in process, annealing temperature is 800～850 ℃, and temperature retention time was assigned to 2 hours in 1 hour 20, and then carries out cold drawn silk processing;

(2) electroplate multiple nickel

1. earlier with the annealing of dumet silk, annealing temperature is 800～850 ℃, is incubated 1 hour 20 and assigns to 2 hours, with the soda boiling pineization of deoiling, uses hot water wash, uses the chloroazotic acid etch, chargedly immediately after the washing puts into nickel bath nickel plating, and the nickel plating technology parameter is as follows:

The nickel plating solution prescription

NiSO ₄7H ₂O 135 grams per liter Na ₂SO ₄10H ₂O 70-80 grams per liter

H ₃BO ₃20-30 grams per liter NaCl 5-7 grams per liter

Temperature adopts that room temperature, pH value are 5～5.5, current density is 0.2～2 ampere/decimeter ², time 2-3 hour;

2. use rack plating method or the nickel plating of continuous electroplating method;

(3) drawing of white Dumet wire:

1. with the annealing earlier of three metal composite wires after the nickel plating, 800～880 ℃ of annealing temperatures, temperature retention time 1 hour to 1 hour 40 minutes;

2. three metal composite wires are drawn, intermediate annealing, 800～880 ℃ of annealing temperatures, temperature retention time 1 hour to 1 hour 40 minutes is drawn into the finished product of all size then;

3. finished products adopts the continuous annealing furnace of hydrogen shield to carry out continuous annealing, 800～880 ℃ of annealing temperatures, 18～25 meters/minute of speed.

2. the method for a production Dumet wire according to claim 1 is characterized in that: the time with the chloroazotic acid etch before the nickel plating was 1～10 second.