CN102211270B - Process for manufacturing high-precision titanium and titanium alloy tube - Google Patents
Process for manufacturing high-precision titanium and titanium alloy tube Download PDFInfo
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- CN102211270B CN102211270B CN2011100840335A CN201110084033A CN102211270B CN 102211270 B CN102211270 B CN 102211270B CN 2011100840335 A CN2011100840335 A CN 2011100840335A CN 201110084033 A CN201110084033 A CN 201110084033A CN 102211270 B CN102211270 B CN 102211270B
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Abstract
The invention provides a process for manufacturing a high-precision titanium or titanium alloy tube. The process comprises the following steps: sorting, smelting, forging, rod processing, rolling a tube, mechanical grinding, electrolysis compound polishing, and the like. By using the process, the problem that a mirror surface cannot be realized because of the surface precision and roughness of the titanium and titanium alloy tube is solved, the surface average roughness of the titanium and titanium alloy tube can approximate 0.03 mu m, the corrosion resistance of the tube can be increased with the help of an oxidation film formed on the surface, and an excellent foundation is established for widely applying the titanium and titanium alloy tube to medical apparatus and instruments, cultural and sports products and decorative materials.
Description
Technical field
The invention belongs to the titanium or titanium alloy processing technique field, be specifically related to a kind of high precision titanium or titanium alloy tube and prepare technology.
Background technology
The surface treatment of titanium or titanium alloy pipe has three different technologies at present: the one, and annealing and pickling in cold rolling after-baking annealing, carries out hydrofluoric acid and nitric acid acidwashing again, lets its surface lose silvery white gloss; The 2nd, vacuum annealing is carried out the vacuum annealing processing, and after carrying out alignment, is made its surface have metallic luster after cold rolling; The 3rd, the decorative pattern extruding, on the basis of annealing and pickling, the mode of utilizing mechanical presses to be shaped forms various concavo-convex tangible decorative patterns in tube surfaces.Present so-called mirror finish has two kinds of polishing, electrobrightenings, and polishing is with the sand paper on the polishing wheel, on polishing mechanical, makes tube surfaces form minute surface at a high speed, and this method wastes time and energy, and surface roughness is very high, and greater than 8 μ m, minute surface is fuzzyyer; Electrobrightening is on the polishing basis, to carry out electrolytic treatments, can form glossy surface in the short time, and is single to the large tracts of land parts; Realize that even mirror finish is difficult to form; Because titanium is prone to oxidation, therefore must apply high pressure, electrolyte can form oxide-film in moment in addition; And dangerous, so generally seldom use in processing industry.
Summary of the invention
The technical problem that the present invention solves: provide a kind of high precision titanium or titanium alloy tube to prepare technology; Solved the difficult problem that titanium or titanium alloy tube-surface precision and roughness can't realize minute surface; Titanium or titanium alloy tube-surface mean roughness can reach about 0.02 μ m-0.05 μ m; And the oxide-film that forms of surface can improve the corrosion resistance of tubing, titanium or titanium alloy tubing extensively popularized at medicine equipment, cultural and sports facility and ornament materials had laid a good foundation.
The technical scheme that the present invention adopts: high precision titanium or titanium alloy tube prepare technology, are made up of following step:
1) selects materials: select for use technical pure titanium sponge or titanium alloy as raw material;
2) melting: raw material is put into consumable electrode vacuum furnace, guarantee to begin when vacuum is less than 0.7Mpa in the stove to heat up, temperature is controlled between 1660 ℃ ± 30 ℃, carry out three meltings after ingot casting become the titanium ingot;
3) forge: the titanium ingot is put into electric furnace heat, temperature is guaranteed between 850 ℃-900 ℃, is incubated also repeatedly pier and pulls out the excellent base of back formation;
4) excellent base processing:
A, excellent base handle: with excellent base surface car light and guarantee that can not there be any defective on its surface, the qualified back of ultrasonic examination centering is then with excellent base surface and the extruding perforation of centre bore parcel back;
B, extrusion molding: the excellent base after will handling is put into electric furnace or induction furnace heating, and temperature is controlled between 800 ℃-1000 ℃, and temperature retention time is 1.5 hours-3 hours, once is squeezed into pipe;
C, pickling: pipe is carried out pickling;
5) tube rolling: with pipe rolling be finished product tubing, the thickness of reservation+0.05mm carries out vacuum annealing and handles, annealing temperature is controlled between 500 ℃-550 ℃, temperature retention time is 2-3 hours;
6) mechanical lapping: utilizing milling apparatus that tube surfaces is ground to surface roughness is about 8 μ m;
7) electrolysis composite polishing:
A, preparing electrolyte: in industrial alcohol, adding percentage by weight is 15%-25% and propyl alcohol; Percentage by weight is a 2%-8% aluminium chloride; Percentage by weight is processed electrolyte for 2%-8% zinc oxide; Electrolyte is heated to fluidized state, is injected in the electrolytic cell when then electrolyte being cooled to 30 ℃-50 ℃;
B, inject the electrolyte into electrolytic cell after, adopt the 380V high voltage, and use the alternating current of 240A-300A to carry out electrolysis;
C, composite polishing: tubing speed with 1m/min in electrolyte is at the uniform velocity passed through in electrolyte; The oxide-film that utilizes electrolysis to generate suppresses the chemical bond between tubing and the Zinc oxide particles; Utilize the Zinc oxide particles in the electrolyte to remove the oxide-film of tube surfaces, the tube surfaces that electric current is concentrated in the electrolyte is carried out the short time polishing;
D, composite polishing carry out can making in 10 minutes the tube surfaces roughness to reach 0.02 μ m-0.05 μ m.
Wherein, Above-mentioned steps two; After one time ingot casting is come out of the stove, must ingot casting two ends and surface scale be removed, and then an ingot casting adopted carry out melting after the butt welding of vacuum plasma technology and cast the secondary ingot casting; Detect a flaw after the secondary ingot casting is come out of the stove and the descale processing, carry out three melting ingot castings again and become the titanium ingot.
Wherein, above-mentioned steps three, titanium ingot temperature be between 850 ℃-900 ℃ the time, is incubated 3.5 hours and carries out first time pier and pull out, and secondary melts down and is heated between 850 ℃-900 ℃ again then, is incubated 1.5 hours and carries out pier again to pull out, and pulls out until pier so repeatedly and form excellent base.
Further, above-mentioned steps seven adds percentage by weight and is 20% and propyl alcohol in industrial alcohol, and percentage by weight is 5% aluminium chloride, and percentage by weight is that 5% zinc oxide is processed electrolyte.
The present invention's advantage compared with prior art:
1, both guarantees material metallographic and material internal ion queueing discipline, guaranteed the various physical properties and the chemical property of material again;
2, with the tubing specification, length can reach 3000mm-6000mm, and diameter can reach between Φ 10mm-Φ 108mm, the thinnest 1mm that reaches of thickness;
3, the surface roughness of mirror effect can reach 0.02 μ m-0.05 μ m, and roughness is minimum for both at home and abroad;
4, processing technology is simpler, and processing charges is lower, yield rate is higher;
5, can both be up to standard in medicine equipment, jewellery, cultural and sports facility and decoration material field;
6, can material be done etched surfaces, minute surface and pattern pipe;
7, the oxide-film that in electrolytic process, forms can improve the tubing corrosion resistance.
The specific embodiment
A kind of embodiment of the present invention is described below.
High precision titanium or titanium alloy tube prepare technology, are made up of following step:
1) selects materials: select for use technical pure titanium sponge or titanium alloy as raw material.High precision titanium and the titanium alloy tube initial stage of producing at first will be strict with on batching; Because of considering that this material will relate to medical equipment and human part; Preferential (ELI) technical pure titanium sponge that adopts is to guarantee inherent quality and the gap between metal ion and the security harmless to human non-toxic of specular material.
2) melting: raw material for guaranteeing metallographic and physicochemical property, must adopt during melting to become ingot more than three times or three times, i.e. during melting in fusion process; Do the melting of twice secondary ingot casting; The vacuum plasma welding procedure is adopted in welding, guarantees that face of weld is pollution-free, free from admixture.When melting, must guarantee that titanium sponge carries out in health, clean environment and in the dosage bunker, and guarantee dry in the environment; Raw material must not be in atmosphere surpasses 12 hours, can be squeezed into piece after will particle being stirred during spice, and pressure must not 2500Mpa when squeezing; Must carry out assembly welding (and avoiding assembly welding otherwise) with vacuum plasma, assembly welding carries out melting after accomplishing immediately, and the electrode group must not be put in atmosphere above 6 hours; During melting, must use consumable electrode vacuum furnace, vacuum is less than 0.7Mpa the time in the stove; Can heat up, melting must be controlled between 1660 ℃ ± 30 ℃, after one time ingot casting is come out of the stove; Must ingot casting two ends and surface scale be removed; And then ingot casting adopted carry out melting after the butt welding of vacuum plasma technology and cast the secondary ingot casting, after coming out of the stove, the secondary ingot casting detects a flaw and descale is handled, and carry out three melting ingot castings again and become the titanium ingot.
3) forge: the titanium ingot removes the cap mouth after must using x-ray inspection qualified, adopts electric furnace to forge; Forbid coal stove to forge, forging temperature guarantees that temperature retention time is 3.5 hours between 850 ℃-900 ℃; Strict this technology of carrying out can be forged into 250mm * 250mm * L, after in multiple length, forging; Secondary melts down and is heated between 850 ℃-900 ℃, is incubated 1.5 hours, forges finished product φ 80 ~ 100mm * L rod blank once more.The alloy type material will take different modes to forge according to different materials and standard, and individual material must adopt 3-7 piers to pull out could form excellent base.
Base heating of titanium or titanium alloy rod and temperature retention time
4) excellent base processing:
A, excellent base handle: excellent base surface machined into must guarantee more than the 3mm, otherwise be regarded as defective, and the no any defective in excellent base surface of Che Guanghou; Qualified through ultrasonic examination; Can centering, centre bore off-centre can not surpass 3mm, pushes perforation with Copper Foil again after with surface, centre bore parcel then; The rod blank must wrap up does not have the base of leakage, the welding of smooth back.
B, extrusion molding: after excellent base is finished dealing with, carry out extrusion molding, extruding must be adopted electric furnace heating or induction furnace heating dual mode.Extrusion temperature is controlled between 800 ℃-1000 ℃, and temperature retention time is 1.5 hours-3 hours, strict control temperature and temperature retention time, and the necessary once-forming of extruding, otherwise be regarded as substandard products, the pipe of extrusion molding must carry out alignment.
C, pickling: the pipe of extrusion molding must thoroughly be washed inside and outside surperficial copper sheet off through overpickling.The pickle proportioning is (percentage by weight): water 50%, and nitric acid 45%, hydrofluoric acid 5%, the pipe after the pickling is inside and outside clean towards Xian, changes next process over to after cutting away the cap head.
5) tube rolling: before pipe was rolling, the pipe endoporus must be processed it with boring machine, made pipe endoporus zero defect, and outer surface of tube blank makes its outer surface zero defect, no foreign matter with machined into or pickling, through being rolled after the assay was approved.After being rolling to finished product tubing, the thickness of reservation+0.05mm is annealed again.Before the annealing titanium or titanium alloy pipe is carried out oil removing, pickling, guarantee inside and outside do not have oil, no foreign matter.Annealing temperature is controlled between 500 ℃-550 ℃, and temperature retention time is 2-3 hours, and must adopt vacuum annealing, and the higher meeting of annealing temperature makes mirror effect fuzzy not good.
6) mechanical lapping: before forming minute surface, must carry out mechanical lapping.The large-scale milling apparatus of Japanese import is adopted in mechanical lapping, and tubing carries out the spiral rotation earlier with milling apparatus and progressively grinds.Abrasive wheel adopts the circular abrasive wheel of 620 orders, four groups of comprehensive grindings of abrasive wheel.For guaranteeing the shape in the tubing process of lapping, the abrasive wheel dynamics adopts computer to adjust the abrasive wheel spacing automatically, and with surface grinding to half mirror status, promptly surface roughness is about 8 μ m, and the back gets into next road program.
7) electrolysis composite polishing: adopt this technology to carry out large-area mirror finish at short notice, the electrolysis composite polishing must adopt the 380V high voltage, and uses the 240A-300A alternating current; In industrial alcohol, adding percentage by weight is 15%-25% and propyl alcohol, and preferred weight percent is 20% and propyl alcohol, and percentage by weight is a 2%-8% aluminium chloride; Preferred weight percent is 5% aluminium chloride; Percentage by weight is a 2%-8% zinc oxide, and preferred weight percent is 5% zinc oxide, processes electrolyte.Electrolyte is heated to fluidized state, is injected in the electrolytic cell when then electrolyte being cooled to 30 ℃-50 ℃; Utilize electrolysis to generate oxide-film and suppress the chemical bond between tubing and the zinc oxide; Utilize plant equipment that tubing speed with 1m/min in electrolyte is at the uniform velocity passed through in electrolyte; Utilize the zinc oxide in the electrolyte to remove oxide-film; Electric current is concentrated on carry out on the tubing in the electrolyte short time polishing, each only can form surface roughness with ten minutes and reaches 0.02 μ m-0.05 μ m tubing in the electrolysis recombination process.
The foregoing description is preferred embodiment of the present invention, is not to be used for limiting practical range of the present invention, so all equivalences of being done with the said content of claim of the present invention change, all should be included within the claim scope of the present invention.
Claims (2)
1. high precision titanium or titanium alloy tube prepare technology, it is characterized in that being made up of following step:
1) selects materials: select for use technical pure titanium sponge or titanium alloy as raw material;
2) melting: raw material is put into consumable electrode vacuum furnace, guarantee to begin when vacuum is less than 0.7Mpa in the stove to heat up, temperature is controlled between 1660 ℃ ± 30 ℃, carry out three meltings after ingot casting become the titanium ingot; After one time ingot casting is come out of the stove; Must ingot casting two ends and surface scale be removed; And then ingot casting adopted carry out melting after the butt welding of vacuum plasma technology and cast the secondary ingot casting, after coming out of the stove, the secondary ingot casting detects a flaw and descale is handled, and carry out three melting ingot castings again and become the titanium ingot;
3) forge: the titanium ingot is put into electric furnace heat, temperature is guaranteed between 850 ℃-900 ℃, is incubated also repeatedly pier and pulls out the excellent base of back formation; Titanium ingot temperature is between 850 ℃-900 ℃ the time, is incubated 3.5 hours and carries out first time pier and pull out, and secondary melts down and is heated between 850 ℃-900 ℃ again then, is incubated 1.5 hours and carries out pier again to pull out, and pulls out until pier so repeatedly and forms excellent base;
4) excellent base processing:
A, excellent base handle: with excellent base surface car light and guarantee that can not there be any defective on its surface, the qualified back of ultrasonic examination centering is then with excellent base surface and the extruding perforation of centre bore parcel back;
B, extrusion molding: the excellent base after will handling is put into electric furnace or induction furnace heating, and temperature is controlled between 800 ℃-1000 ℃, and temperature retention time is 1.5 hours-3 hours, once is squeezed into pipe;
C, pickling: pipe is carried out pickling;
5) tube rolling: with pipe rolling be finished product tubing, the thickness of reservation+0.05mm carries out vacuum annealing and handles, annealing temperature is controlled between 500 ℃-550 ℃, temperature retention time is 2-3 hours;
6) mechanical lapping: utilizing milling apparatus that tube surfaces is ground to surface roughness is about 8 μ m;
7) electrolysis composite polishing:
A, preparing electrolyte: in industrial alcohol, adding percentage by weight is 15%-25% and propyl alcohol; Percentage by weight is a 2%-8% aluminium chloride; Percentage by weight is processed electrolyte for 2%-8% zinc oxide; Electrolyte is heated to fluidized state, is injected in the electrolytic cell when then electrolyte being cooled to 30 ℃-50 ℃;
B, inject the electrolyte into electrolytic cell after, adopt the 380V high voltage, and use the alternating current of 240A-300A to carry out electrolysis;
C, composite polishing: tubing speed with 1m/min in electrolyte is at the uniform velocity passed through in electrolyte; The oxide-film that utilizes electrolysis to generate suppresses the chemical bond between tubing and the Zinc oxide particles; Utilize the Zinc oxide particles in the electrolyte to remove the oxide-film of tube surfaces, the tube surfaces that electric current is concentrated in the electrolyte is carried out the short time polishing;
D, composite polishing carry out can making in 10 minutes the tube surfaces roughness to reach 0.02 μ m-0.05 μ m.
2. high precision titanium according to claim 1 or titanium alloy tube prepare technology; It is characterized in that: above-mentioned steps 7); In industrial alcohol, add percentage by weight and be 20% and propyl alcohol, percentage by weight is 5% aluminium chloride, and percentage by weight is that 5% zinc oxide is processed electrolyte.
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| CN2011100840335A CN102211270B (en) | 2011-04-06 | 2011-04-06 | Process for manufacturing high-precision titanium and titanium alloy tube |
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| CN2011100840335A CN102211270B (en) | 2011-04-06 | 2011-04-06 | Process for manufacturing high-precision titanium and titanium alloy tube |
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| CN102211270B true CN102211270B (en) | 2012-11-07 |
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