CN101122025B - Titanium alloying milling solution and milling technique used for the same - Google Patents
Titanium alloying milling solution and milling technique used for the same Download PDFInfo
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Abstract
The invention discloses a titanium alloying milling solution and an application million technology of the milling solution, which essentially contains a mixed acid corrosive solution with nitrate acid and fluohydric acid as the main components and sodium laurylsulfate, glycol n-butyl ether and/or urea additive. The invention maintains the surface tension of the solution within a stable value. Absorption of the glycol n-butyl ether can reduce the interfacial tension and improve the milling rate. The sodium laurylsulfate capable of improving the fluidity of the solution can remove the over corrosion of the metal at the root of a milling circle, so as to prevent deficiencies of corrosion groove, slope and wave. The sodium nitrate prevents scale produced by the alloy elements on the surface of a milling groove, improves the smoothness of the milling surface and convenient maintenance of equipments. The urea can effectively absorb the nitrogen mixture gases, reduce vaporization of acid solution and prevents environmental pollution. The invention does not need any warming equipment, the hydrogen increase is less than 9ppm, the service life of the solution is long, the hydrogen brittleness phenomenon will not appear, and the technology has little impact on the fatigue performance of the material.
Description
Technical field
The present invention relates to a kind of titanium alloy milling solution and use the milling processing method of this milling solution.
Background technology
Chemistry milling is a kind of accurate micro-milling processing that is specially adapted to dimensional precision height, complex-shaped part.The chemistry milling moulding is that the metal stock part is immersed in the chemical corrosion solution, utilizes the processing method of the corrosive nature removal surface metal of solution.Chemistry milling technological process of the prior art is: metal parts is cleaned oil removing, apply from the teeth outwards and can resist the protective strip coating of etchant solution effect, carve shape behind room temperature or hot setting.Need the protective cover of milling working position to peel off with being coated on, then part is immersed in the etchant solution, corrosion processing is carried out on exposed surface.Working depth, speed and surface quality were controlled by composition, concentration, working temperature and the part buried time of adjusting etchant solution.The limitation of this technology is: the rib root that chemistry milling is come out always has a radius and corrosion processing degree of depth fillet about the same, has increased the useless weight of part; The smooth finish on milling surface is poorer than raw-material smooth finish.。
Applied chemistry milling technology can the machining shape complexity multiple metal and alloy part such as aluminium, magnesium, titanium, nickel, copper, iron and steel.To use different etchant solutions and protective cover for different metal needs.Adopt with sodium hydroxide for aluminium alloy is the alkaline corrosion solution of main ingredient more, contains the acid attack solution that multiple mixing acid such as sulfuric acid, nitric acid, hydrochloric acid, hydrofluoric acid, phosphoric acid is formed for adopt such as iron and steel, titanium alloy more.Protective strip coating is used materials such as chloroprene rubber, isoprene-isobutylene rubber, styrene-butadiene rubber(SBR), polyacrylonitrile, polyvinyl chloride more.Such as the disclosed application number of Chinese patent is 200510044852.1, and it is exactly the titanium or titanium alloy etchant solution of being formed with hydrofluoric acid, nitric acid and water that name is called " chemical etching liquor that is used for titanium or titanium alloy ".The percent by volume scope that it adopts is hydrofluoric acid 5%-15%, nitric acid 8%-35%, water 50%-85%.
U.S. Patent number in September, 4116755,1978, Coggins, et al.Chem-milling oftitanium and refractory metals also discloses the etchant solution that contains hydrofluoric acid, nitric acid, carboxylic acid derivative and Sodium Benzoate in its solution.Its advantage be this etchant solution milling rate evenly, to increase hydrogen few.
U.S. Patent number 4900398, February nineteen ninety, Chen.Chemical milling of titanium.Also containing in its solution with hydrofluoric acid, sodium chlorate is the mixed type chemical milling solution of main component, and contains a kind of in sulfuric acid, hydrochloric acid or the nitric acid.Its advantage be after the milling to increase hydrogen few.
The main drawback of above-mentioned patent is: owing to lack tensio-active agent in the solution, the surface tension of solution can not be maintained in the stable numerical value, make that the flowability of solution is poor, be prone to " etched groove " after the milling, " slope " reaches " ripple " defective, the milling rate in same milling zone is inhomogeneous, is difficult to guarantee the depth accuracy of milling.Along with the carrying out of milling, the alloying element in the titanium alloy can slowly form the incrustation scale that one deck is unfavorable for maintenance of the equipment at the milling rooved face.Can produce in the milling process and be discharged into the nitrogenous obnoxious flavour of the xanchromatic that is unfavorable for environment protection in the air, the solution working temperature need maintain between 44 ℃-54 ℃, easily causes the acid solution volatilization and polluted air.
Summary of the invention
The purpose of this invention is to provide a kind of titanium alloy milling solution, to solve the above-mentioned problems in the prior art.Can reduce interfacial tension with this titanium alloy milling solution of the present invention, prevent " etched groove ", " slope " and " ripple ", obnoxious flavour separates out the minimizing environmental pollution in the inhibition milling process.
Another object of the present invention provides a kind of processing method of using the milling of above-mentioned milling solution, to avoid deficiency that existing milling complete processing exists and the problem that the hydrogen embrittlement phenomenon occurs, reaches the purpose of accurate milling.
In order to achieve the above object, a kind of titanium alloy milling solution provided by the invention, a kind of titanium alloy milling solution, comprise, mainly contain with nitric acid, hydrofluoric acid is the mixing acid acid attack solution that main component is formed, sodium lauryl sulphate, ethylene glycol n-butyl ether and/or urea addn contain SODIUMNITRATE and/or resolvability titanium ion, wherein, hydrofluoric acid 35-65 grams per liter, nitric acid 100-180 grams per liter, ethylene glycol n-butyl ether 5-8 grams per liter, SODIUMNITRATE 10-12 grams per liter, urea 10-15 grams per liter, sodium lauryl sulphate 0.3-0.5 grams per liter, resolvability titanic ion 0-30 grams per liter, water 730-850 grams per liter.
Use milling solution milling titanium alloy technology of the present invention, comprise the steps:
(a) anneal titanium alloy workpiece, and to workpiece surface oil removing degreasing;
(b) soak workpiece with hot alkaline solution, use hot water, cold water cleaning workpiece then respectively; Adopt sodium hydroxide 250～300 grams per liters, sodium dichromate 99 11～14 grams per liters, SODIUMNITRATE 11～14 grams per liters to form alkaline solution, preferred temperature is that 95～110 ℃, time are that 5～10 minutes processing parameter soaks workpiece
(c) pickling workpiece;
(d) cold water cleans and dry workpiece;
(e) dip-coating strippability protection glue;
(f) at room temperature thorough solidified glue film;
(g) delineation milling figure;
(h) peel off the protection glue in milling zone;
(i) with containing the above-mentioned milling solubilisate miller part of sodium lauryl sulphate and/or SODIUMNITRATE, and in the milling process, every 4-5 minute to solution stirring one time 30 seconds;
(j) clean and remove the protection glue in non-milling zone.
Above steps is all carried out at normal temperatures and pressures.
The present invention has following beneficial effect than prior art:
In above-mentioned milling solution, sodium lauryl sulphate is a stabilized surfactant, and the surface tension of solution is maintained in the stable numerical value.Sodium lauryl sulphate can also be improved the flowability of solution, eliminates the excessive corrosion of milling fillet root metal, thereby prevents that " etched groove ", " slope " from reaching the appearance of " ripple " defective, helps carrying out the high precision milling.The ethylene glycol n-butyl ether contains hydrophilic group ehter bond-O-and non-dissociated hydroxyl-OH, can produce adsorption at titanium alloy surface, reduce interfacial tension, improve the wetting action of solution to the milling surface, the useful area of augmenting response, thereby the raising milling rate makes that its milling rate just can reach 10-22 μ m/min/ single face in the room temperature range of working temperature between 26-32 ℃.The SODIUMNITRATE of adding can prevent the deposition of incrustation scale in the solution, prevents that the alloying element in the titanium alloy from forming incrustation scale at the milling rooved face, helps to improve the surface smoothness on milling surface and make things convenient for the maintenance of equipment, and can improve milling rate.Urea can produce the fine and close persistent foam of one deck in solution surface in the milling process, effectively absorb the nitrogenous obnoxious flavour of the xanchromatic that produces in the milling process.Working temperature maintains in the room temperature range between 26-32 ℃, can reduce the volatilization of acid solution, avoids the pollution to environment.And can save the expense of heating; The milling solution life-span is long, and resolvability titanic ion can reach 30 grams per liters; The milling etch is 0.45 than only, and therefore, the fillet radius of the rib root after the chemistry milling is 0.45 times of the corrosion processing degree of depth, and the useless of part heavily reduces 55%; The milling amount is even, and milling depth limit deviation can reach ± 0.04mm; Increase the hydrogen amount seldom, only 9ppm of the hydrogen amount that heightens most after the milling; Milling surface roughness Ra＜0.55 μ m, its milling surface smoothness obviously is better than raw-material surface smoothness.
Use the workpiece of milling solution milling titanium alloy of the present invention, do not need warming-up device, no xanchromatic nitrogenous gas is discharged in the solution, can reduce separating out of obnoxious flavour in the chemistry milling process; The no any defective in milling zone, the milling amount is even, surface quality good, hydrogen is little, chemistry milling speed is moderate, can significantly improve the smooth finish on milling surface.The hydrogen embrittlement phenomenon can not occur in the milling, its technology is very little to the fatigue property influence of material.
Embodiment
Further specify the present invention below by embodiment.In following examples, can contain with prior art nitric acid, hydrofluoric acid is the mixing acid acid attack mother liquor that main component is formed.Its mixing acid acid attack mother liquor is not got rid of the etchant solution that contains hydrofluoric acid, nitric acid, carboxylic acid derivative and Sodium Benzoate, comprise contain hydrofluoric acid, sodium chlorate is the mixed type chemical milling solution of main component, and a kind of in sulfuric acid, hydrochloric acid or the nitric acid.The per-cent of milling solution (weight) is hydrofluoric acid 3.5%-6.5%, nitric acid 10%-18%, water 72%-83%, all the other are sodium lauryl sulphate, ethylene glycol n-butyl ether and/or SODIUMNITRATE, urea, the resolvability titanic ion of certain amount, above chemical ingredients is chemical pure.
Embodiment 1
Prepare 20 liters solution:
Hydrofluoric acid 35 grams per liters
Nitric acid 100 grams per liters
SODIUMNITRATE 10 grams per liters
Urea 10 grams per liters
Ethylene glycol n-butyl ether 5 grams per liters
Sodium lauryl sulphate 0.3 grams per liter
Resolvability titanic ion 0 grams per liter
29 ± 1 ℃ of temperature
Embodiment 2
Prepare 20 liters solution:
Hydrofluoric acid 65 grams per liters
Nitric acid 180 grams per liters
SODIUMNITRATE 12 grams per liters
Urea 15 grams per liters
Ethylene glycol n-butyl ether 8 grams per liters
Sodium lauryl sulphate 0.5 grams per liter
Resolvability titanic ion 30 grams per liters
31 ± 1 ℃ of temperature
Embodiment 3
Prepare 20 liters solution:
Hydrofluoric acid 45 grams per liters
Nitric acid 140 grams per liters
SODIUMNITRATE 11 grams per liters
Urea 12 grams per liters
Ethylene glycol n-butyl ether 7 grams per liters
Sodium lauryl sulphate 0.4 grams per liter
Resolvability titanic ion 15 grams per liters
27 ± 1 ℃ of temperature
Use milling solution milling titanium alloy technology of the present invention, as follows:
(a) oil removing degreasing;
Workpiece surface cleans with organic solvents such as butanone, removes degreasing, grease etc.The purpose of this operation is: 1. clean workpiece surface, guarantee that protection glue is good with combining of workpiece surface; 2. prevent greasy dirt, grease contamination milling solution.These 2 is the key that guarantees to obtain qualified workpiece.
(b) hot alkali dipping;
It is that 95-110 ℃, naoh concentration are that 250-300 grams per liter, sodium dichromate 99 concentration are that 11-14 grams per liter, sodium nitrate concentration are in the solution of 11-14 grams per liter 5-10 minute that workpiece is immersed in temperature, its objective is the thermal treatment oxide skin of softening loosening workpiece surface, under room temperature state, just can remove the oxide skin of workpiece surface for step (e) and get ready.
(c) hot water cleaning workpiece;
(d) cold water cleaning workpiece;
(e) pickling;
Workpiece was immersed in the solution of hydrofluoric acid 15-25 grams per liter, nitric acid 350-450 grams per liter of room temperature state 5-8 minute, its objective is and remove the oxide skin of titanium alloy surface became uneven clean, because this layer oxide skin can make the milling rate inequality of titanium alloy surface, thereby influence the homogeneity of milling.
(f) cold water cleans and dry workpiece;
(g) dip-coating strippability protection glue;
Strippability protection glue used in the present invention is by Turco Products, the AC-850 protection glue that Inc provides.Workpiece is repeated to be immersed in for 4-5 time in the protection sol solution, workpiece should be inverted 180 degree during each impregnation, and seasoning 10-15 minute, final film thickness is 0.2-0.4mm
(h) glued membrane solidifies;
Glued membrane was at room temperature placed more than 24 hours the finish-drying glued membrane.
(i) delineation milling figure;
Milling model and workpiece are posted and fixed,, require groove to carve saturating protection glue just, but can not on workpiece, stay tangible indentation with carving the lines of shape cutter (as the No.11 scalpel) along milling model delineation milling pattern.
(j) peel off protection glue;
After the lines delineation of all milling patterns finishes, take the milling model away, peel off the protection glue in zone to be milled.
(k) milling
With acidproof plastic cord the workpiece level is suspended on and carries out milling in the solution.In the milling process, every 4-5 minute to solution stirring once, churning time is controlled at about 30 seconds usually.
(l) clean
With the thorough cleaning workpiece of cold water, to prevent residual acid liquid corrosion workpiece.
(m) remove protection glue.
Remove the protection glue in non-milling zone.
Case 1
With thickness is that 1.55mm, milling zone are that the TC1 of 75 * 55mm and each 1 of TC4 Ti alloy under annealing sheet material immersed in the milling solution milling 70 minutes, and wherein the surface roughness Ra of TC1 is 0.66 μ m, and the surface roughness Ra of TC4 is 0.57 μ m.
Measure the milling degree of depth with ultrasonic thickness indicator, TC1 is 0.86-0.88mm, and TC4 is 0.80-0.82mm, so its average milling rate is respectively 12.4 μ m/min/ single faces and 11.6 μ m/min/ single faces; Milling depth limit deviation is ± 0.01mm.
With the dimensional change in vernier caliper measurement milling zone, record the sideetching size in the milling process, TC1 is 0.39mm, TC4 is 0.37mm, so direction finding etch ratio is 0.45.
With luminosity instrumentation scale surface roughness, TC1 is 0.50 μ m, and TC4 is 0.42 μ m.
Measure hydrogen content before and after the milling with hydrogen determinator, what obtain titanium alloy in the milling process increases the hydrogen amount, and TC1 is 3ppm, and TC4 is 3ppm.
The no any defective in milling zone, no yellow gas is discharged in the solution.
Case 2
With thickness is that 1.54mm, milling zone are that the TC1 of 75 * 55mm and each 1 of TC4 Ti alloy under annealing sheet material immersed in the milling solution milling 70 minutes, and wherein the surface roughness Ra of TC1 is 0.63 μ m, and the surface roughness Ra of TC4 is 0.57 μ m.
Measure the milling degree of depth with ultrasonic thickness indicator, TC1 is 0.92-0.97mm, and TC4 is 0.89-0.97mm, so its milling rate is respectively 13.6 μ m/min/ single faces and 13.3 μ m/min/ single faces; Milling depth limit deviation is ± 0.04mm.
With the dimensional change in vernier caliper measurement milling zone, record the direction finding corrosion size in the milling process, TC1 is 0.43mm, TC4 is 0.41mm, so its direction finding etch ratio is 0.45.
With luminosity instrumentation scale surface roughness, TC1 is 0.40 μ m, and TC4 is 0.29 μ m.
Measure hydrogen content before and after the milling with hydrogen determinator, what obtain titanium alloy in the milling process increases the hydrogen amount, and TC1 is 6ppm, and TC4 is 7ppm.
The no any defective in milling zone, no yellow gas is discharged in the solution.
Case 3
With thickness is that 1.55mm, milling zone are that the TC1 of 75 * 55mm and each 1 of TC4 Ti alloy under annealing sheet material immersed in the milling solution milling 50 minutes, and wherein the surface roughness Ra of TC1 is 0.67 μ m, and the surface roughness Ra of TC4 is 0.55 μ m.
Measure the milling degree of depth with ultrasonic thickness indicator, TC1 is 0.99-1.02mm, and TC4 is 0.91-0.93mm, so its milling rate is respectively 20.0 μ m/min/ single faces and 18.4 μ m/min/ single faces; Milling depth limit deviation is ± 0.02mm.
With the dimensional change in vernier caliper measurement milling zone, record the direction finding corrosion size in the milling process, TC1 is 0.45mm, TC4 is 0.42mm, so its direction finding etch ratio is 0.45.
With luminosity instrumentation scale surface roughness, TC1 is 0.42 μ m, and TC4 is 0.33 μ m.
Measure hydrogen content before and after the milling with hydrogen determinator, what obtain titanium alloy in the milling process increases the hydrogen amount, and TC1 is 5ppm, and TC4 is 7ppm.The no any defective in milling zone, no yellow gas is discharged in the solution.
Claims (2)
1. titanium alloy milling solution, comprise, mainly containing with nitric acid, hydrofluoric acid is the mixing acid acid attack solution that main component is formed, sodium lauryl sulphate, ethylene glycol n-butyl ether and/or urea addn, contain SODIUMNITRATE and/or resolvability titanium ion, wherein, hydrofluoric acid 35-65 grams per liter, nitric acid 100-180 grams per liter, ethylene glycol n-butyl ether 5-8 grams per liter, SODIUMNITRATE 10-12 grams per liter, urea 10-15 grams per liter, sodium lauryl sulphate 0.3-0.5 grams per liter, resolvability titanic ion 0-30 grams per liter, water 730-850 grams per liter.
2. use the milling titanium alloy technology of the described milling solution of claim 1, comprise the steps:
(a) anneal titanium alloy workpiece, and to workpiece surface oil removing degreasing;
(b) soak workpiece with hot alkaline solution, use hot water, cold water cleaning workpiece then respectively; Adopt sodium hydroxide 250～300 grams per liters, sodium dichromate 99 11～14 grams per liters, SODIUMNITRATE 11～14 grams per liters to form alkaline solution, preferred temperature is that 95～110 ℃, time are that 5～10 minutes processing parameter soaks workpiece;
(c) pickling workpiece;
(d) cold water cleans and dry workpiece;
(e) dip-coating strippability protection glue;
(f) at room temperature thorough solidified glue film;
(g) delineation milling figure;
(h) peel off the protection glue in milling zone;
(i) with containing the above-mentioned milling solubilisate miller part of sodium lauryl sulphate and/or SODIUMNITRATE, and in the milling process, every 4～5 minutes to solution stirring one time 30 seconds;
(j) clean and remove the protection glue in non-milling zone.
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