CN110055382B - Manufacturing method of torsional shear type stud - Google Patents

Manufacturing method of torsional shear type stud Download PDF

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Publication number
CN110055382B
CN110055382B CN201910388093.2A CN201910388093A CN110055382B CN 110055382 B CN110055382 B CN 110055382B CN 201910388093 A CN201910388093 A CN 201910388093A CN 110055382 B CN110055382 B CN 110055382B
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treatment
manufacturing
blank
shear type
torsional shear
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CN110055382A (en
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杨照军
汪豪豪
张楠楠
陈元
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Anhui Changjiang Fasteners Co Ltd
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Anhui Changjiang Fasteners Co Ltd
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    • 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
    • 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
    • C23C14/02Pretreatment of the material to be coated
    • 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
    • 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
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • 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
    • C23C14/58After-treatment
    • C23C14/5873Removal of material
    • C23C14/588Removal of material by mechanical treatment
    • 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
    • C23FNON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F17/00Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
    • 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions

Abstract

The invention discloses a manufacturing method of a torsional shear type stud, which comprises the following steps: s1, annealing the blank; s2, carrying out acid washing treatment on the annealed blank, cleaning, immersing in an oxalic acid solution, and plating the composite coating agent on the surface of the blank subjected to the oxalic acid treatment by using an electron beam evaporation coating method to obtain a pretreated wire rod; s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire. The coating agent provided by the invention adopts a phosphorus-free material, is good in environmental protection, and the coated stud is high in corrosion resistance and oxidation resistance, so that the service life of the stud can be effectively prolonged, the processing technology is reasonable and easy to operate, the service lives of equipment and a die are prolonged, batch production can be realized, and the economic benefit is high.

Description

Manufacturing method of torsional shear type stud
Technical Field
The invention relates to the technical field of stud machining processes, in particular to a manufacturing method of a torsional shear type stud.
Background
The stud machining process flow comprises the following steps: hot rolling wire rod- (cold drawing), spheroidizing (softening) annealing, pickling, cold drawing, cold forging forming, thread processing, heat treatment and inspection. In the patent with publication number CN103192022A, the workpiece is strongly contracted in the process sequence, the stress is very large, the impact force on a grinding tool and equipment is strong, and the service life of a die is greatly reduced; the strong shrinkage process has high requirements on surface phosphating treatment of raw materials, the service life of a die can be greatly shortened due to a slightly poor phosphating film, a phosphorus-containing substance is used for forming the film and is not environment-friendly, the phosphorus emission of metals such as phosphate and the like can cause rich nutrition in land and rivers, the environment is seriously polluted, the phosphating soaking time is long, the processing efficiency is low, and although the problems of environment protection and processing efficiency can be solved due to the use of a coating agent, the corrosion and rust prevention capability is still poor, the adhesive force is weak, so that a manufacturing method of the torsional shear type stud is designed to solve the problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a manufacturing method of a torsional shear type stud, which improves the adhesive force of a coating on the surface of the obtained torsional shear type stud and has excellent corrosion resistance and rust resistance.
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank;
s2, carrying out acid washing treatment on the annealed blank, cleaning, immersing in an oxalic acid solution, and plating the composite coating agent on the surface of the blank subjected to the oxalic acid treatment by using an electron beam evaporation coating method to obtain a pretreated wire rod;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire.
Preferably, in S1, the annealing process specifically operates as follows: and heating to 680-760 ℃, keeping the temperature for 3-4 h in the heating process, then preserving the heat for 4-6 h, cooling to below 550 ℃, cooling at the speed of 2-4 ℃/min, and cooling to the normal temperature along with the furnace.
Preferably, in S2, the electron beam evaporation coating method comprises tabletting the composite coating agent, placing on a copper target of an electron beam vacuum coater, wherein the vacuum degree of a vacuum chamber in the electron beam vacuum coater is 1 × 10-4~1.5×10-4And Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.1-0.2 mm/s.
Preferably, in S2, one or two of nitric acid, hydrochloric acid and sulfuric acid are selected as the pickling agent in the pickling process, and H in the pickling agent+The concentration of (b) is 0.5 to 10 mol/L.
Preferably, in S2, the concentration of the oxalic acid solution is 0.8-1.2 mol/L.
Preferably, in S2, the composite film agent includes the following raw materials by weight percent: 25-35% of zirconium oxide, 8-12% of silicon dioxide, 15-20% of aluminum oxide, 3-8% of ferric nitrate, 5-10% of nitric acid, 5-12% of thickening agent and the balance of organic solvent; preferably, the mass fraction of the nitric acid is 60-70%, and the thickening agent is a polyurethane modified polyether thickening agent.
Preferably, in S2, the composite coating agent is prepared by the following steps: adding zirconium oxide into an organic solvent, uniformly stirring at 75-90 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain the composite coating agent.
Preferably, in S2, the organic solvent used in the preparation of the composite skin film agent is at least one of absolute ethyl alcohol, methanol, isopropanol and acetone.
Preferably, in S3, the stud obtained by the reduction of the double offset ring teeth is deburred by a grinding machine, and a finished torsional shear type stud is obtained after the stud is qualified.
In the invention S1, the stud blank is annealed to obtain uniform and fine pearlite, so that the plasticity of the blank is improved, and the production requirement of actual processing is met.
In S2, the acid washing can wash away the oxide film generated by annealing on the blank, the surface of the blank after acid washing is rough, and the adhesive force of the subsequent coating is improved;
in S2, the acid washing can wash away the oxide film generated by annealing on the blank, the surface of the blank after acid washing is rough, and the adhesive force of the subsequent coating is improved; because the surface of the alumina is uneven and the distribution among pores is wide, the alumina can be used as a carrier in the composite coating agent, the adsorbed zirconia and the silicon dioxide are combined to form a composite material, the zirconia adsorbed on the alumina mainly exists in a long-chain structure of Zr-O-Zr, the silicon dioxide can play a role in stabilizing the zirconia in the alumina, stabilize the tetragonal phase of the zirconia, achieve the function of fine grain strengthening, hinder the growth of zirconia grains, enable the structure of a coating film to be more compact, enable the surface of the obtained coating film to be smooth and have good luster, and simultaneously, because the connection among the three is tight, further improve the quality of the coating film, enable the density of the coating film to be high, have good adhesion, and also have high corrosion resistance, strong oxidation resistance and good stability; the thickening agent is matched with the three components, so that the compactness of the texture structure of the coating film is further improved, the coating thickness of the surface of the blank is improved, and the corrosion resistance and the oxidation resistance of the coating film are further improved; meanwhile, the composite coating agent is adopted to carry out coating treatment on the wire rod by an electron beam evaporation coating method, and because the solid composite coating agent is used for coating, cleaning and subsequent sewage treatment are not needed after coating, so that water resources are saved, the coating cost is reduced, the film forming is faster, the continuous film forming of the wire rod is facilitated, and the economic benefit of stud processing is improved.
In the invention, in S3, the intermediate diameter direct reduction teeth are arranged in the front, chamfers are arranged in the front, the blank is annealed in S1, the blank shaping is improved, the intermediate diameter direct reduction teeth do not cause overlarge stress of the stud, the pre-reduction teeth are easy to form, the service lives of equipment and a die are greatly prolonged, the operation is more convenient, after the blank annealed in S1 is subjected to acid pickling and coating treatment of a coating agent in S2, on one hand, the corrosion resistance and oxidation resistance of the surface of a wire rod are greatly improved, on the other hand, the coating has high density and smooth surface, when the equipment is subjected to heading, fine heading and rod reduction in the subsequent S3, the clamping is stable, the processing stability is high, and the high-precision torsional shear type stud is obtained.
Drawings
Fig. 1 is a process flow diagram of S3 in the method for manufacturing a torsional shear type stud according to the present invention.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank wire, wherein the annealing operation is as follows: heating to 680 ℃, keeping the temperature for 3h in the heating process, then preserving the heat for 4h, cooling to below 550 ℃, cooling at the speed of 2 ℃/min, and cooling to normal temperature along with the furnace;
s2, use of H+The annealed ingot was subjected to acid pickling with nitric acid having a concentration of 0.5 mol/L, washed,immersing the wire rod into an oxalic acid solution with the concentration of 0.8 mol/L, and plating the composite coating agent on the surface of the blank after the oxalic acid treatment by using an electron beam evaporation coating method to obtain a pretreated wire rod;
the electron beam evaporation coating process includes tabletting the composite coating agent, and setting the laminated composite coating agent on the copper target of electron beam vacuum coating machine with vacuum degree of 1 × 10-4Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.1 mm/s;
the composite coating agent comprises the following raw materials in percentage by weight: 6% of zirconium oxide, 8% of silicon dioxide, 17% of aluminum oxide, 8% of ferric nitrate, 6% of nitric acid with the mass fraction of 60%, 9% of polyurethane modified polyether thickening agent and the balance of absolute ethyl alcohol;
the composite coating agent adopts the following preparation process: adding zirconium oxide into absolute ethyl alcohol, stirring uniformly at 75 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain a composite coating agent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire rods, carrying out deburring treatment on the stud obtained through the plum blossom tooth shrinking treatment by using a grinding machine, and obtaining a torsional shear type stud finished product after the stud is qualified through inspection.
Example two
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank wire, wherein the annealing operation is as follows: heating to 700 ℃, keeping the temperature for 3.2h in the heating process, then preserving the heat for 4.5h, then cooling to below 550 ℃, keeping the temperature at 2.5 ℃/min, and cooling to the normal temperature along with the furnace;
s2, use of H+The annealed blank is subjected to acid pickling treatment by hydrochloric acid with the concentration of 2 mol/L, washed, immersed into oxalic acid solution with the concentration of 0.9 mol/L, and then the composite coating agent is coated on the surface of the blank after the oxalic acid treatment by an electron beam evaporation coating method to obtain a pre-treated blankProcessing the wire rod;
the electron beam evaporation coating process includes tabletting the composite coating agent, and setting the laminated composite coating agent on the copper target of electron beam vacuum coating machine with vacuum degree of 1.1 × 10-4Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.14 mm/s;
the composite coating agent comprises the following raw materials in percentage by weight: 33% of zirconium oxide, 11% of silicon dioxide, 16% of aluminum oxide, 5% of ferric nitrate, 5% of nitric acid with the mass fraction of 65%, 8% of SN-THICKENER612NC thickener and the balance of methanol;
the composite coating agent adopts the following preparation process: adding zirconium oxide into methanol, stirring uniformly at 78 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain a composite coating agent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire rods, carrying out deburring treatment on the stud obtained through the plum blossom tooth shrinking treatment by using a grinding machine, and obtaining a torsional shear type stud finished product after the stud is qualified through inspection.
EXAMPLE III
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank wire, wherein the annealing operation is as follows: heating to 720 ℃, keeping the temperature for 3.6h in the heating process, then preserving the heat for 5h, then cooling to below 550 ℃, keeping the temperature at 3 ℃/min, and cooling to the normal temperature along with the furnace;
s2, use of H+The annealed blank is subjected to acid pickling treatment by using sulfuric acid with the concentration of 4 mol/L, the blank is immersed into oxalic acid solution with the concentration of 1.2 mol/L after being cleaned, and then the composite coating agent is coated on the surface of the blank after the oxalic acid treatment by using an electron beam evaporation coating method to obtain a pretreated wire rod;
the electron beam evaporation coating specifically operates as follows: the composite coating agent is pressed into sheets and put into a copper target of an electron beam vacuum coating machineIn the electron beam vacuum coater, the vacuum degree of the vacuum chamber is 1.5 × 10-4Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.16 mm/s;
the composite coating agent comprises the following raw materials in percentage by weight: 27% of zirconium oxide, 9% of silicon dioxide, 18% of aluminum oxide, 5% of ferric nitrate, 6% of nitric acid with the mass fraction of 66%, 10% of hydrophobic modified polyurethane thickener and the balance of isopropanol;
the composite coating agent adopts the following preparation process: adding zirconium oxide into isopropanol, stirring uniformly at 80 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain a composite coating agent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire rods, carrying out deburring treatment on the stud obtained through the plum blossom tooth shrinking treatment by using a grinding machine, and obtaining a torsional shear type stud finished product after the stud is qualified through inspection.
Example four
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank wire, wherein the annealing operation is as follows: heating to 740 ℃, keeping the temperature for 4h in the heating process, then preserving the heat for 5.5h, then cooling to below 550 ℃, wherein the cooling speed is 3.5 ℃/min, and cooling to normal temperature along with the furnace;
s2, use of H+The mixed solution of hydrochloric acid and sulfuric acid with the concentration of 8 mol/L is used for carrying out acid cleaning treatment on the annealed blank, after cleaning, the blank is immersed into oxalic acid solution with the concentration of 1.0 mol/L, and then the composite coating agent is coated on the surface of the blank after the oxalic acid treatment by utilizing an electron beam evaporation coating method to obtain a pretreated wire rod;
the electron beam evaporation coating process includes tabletting the composite coating agent, and setting the laminated composite coating agent on the copper target of electron beam vacuum coating machine with vacuum degree of 1.3 × 10-4Pa, plating the composite coating agent on oxalic acid at room temperatureThe moving speed of the blank after the treatment of the Chinese herbal acid in the film coating process is 0.18 mm/s;
the composite coating agent comprises the following raw materials in percentage by weight: 30% of zirconium oxide, 10% of silicon dioxide, 18% of aluminum oxide, 5% of ferric nitrate, 8% of nitric acid with the mass fraction of 65%, 8% of hydrophobic modified polyurethane and the balance of acetone;
the composite coating agent adopts the following preparation process: adding zirconium oxide into acetone, stirring uniformly at 85 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain a composite coating agent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire rods, carrying out deburring treatment on the stud obtained through the plum blossom tooth shrinking treatment by using a grinding machine, and obtaining a torsional shear type stud finished product after the stud is qualified through inspection.
EXAMPLE five
A manufacturing method of a torsional shear type stud comprises the following steps:
s1, annealing the blank wire, wherein the annealing operation is as follows: heating to 760 ℃, keeping the temperature for 4h in the heating process, then preserving the heat for 6h, then cooling to below 550 ℃, keeping the cooling speed at 4 ℃/min, and cooling to the normal temperature along with the furnace;
s2, use of H+The mixed solution of hydrochloric acid and nitric acid with the concentration of 10 mol/L is used for carrying out acid cleaning treatment on the annealed blank, the blank is immersed into oxalic acid solution with the concentration of 1.2 mol/L after being cleaned, and then the composite coating agent is coated on the surface of the blank after the oxalic acid treatment by utilizing an electron beam evaporation coating method to obtain a pretreated wire rod;
the electron beam evaporation coating process includes tabletting the composite coating agent, and setting the laminated composite coating agent on the copper target of electron beam vacuum coating machine with vacuum degree of 1.5 × 10-4Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.2 mm/s;
the composite coating agent comprises the following raw materials in percentage by weight: 35% of zirconium oxide, 12% of silicon dioxide, 20% of aluminum oxide, 8% of ferric nitrate, 10% of nitric acid with the mass fraction of 70%, 5% of polyurethane modified polyether thickening agent and the balance of acetone;
the composite coating agent adopts the following preparation process: adding zirconium oxide into acetone, stirring uniformly at 90 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain a composite coating agent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire rods, carrying out deburring treatment on the stud obtained through the plum blossom tooth shrinking treatment by using a grinding machine, and obtaining a torsional shear type stud finished product after the stud is qualified through inspection.
Comparative example 1
The only difference from example five is that no silica was added.
Comparative example No. two
The only difference from example five is that no alumina was added.
Comparative example No. three
The only difference from example five is that no thickener was used.
Comparative example No. four
The difference from the fifth embodiment is only that a phosphating solution is used, wherein the phosphating solution comprises 96-98 g/L g of zinc dihydrogen phosphate, 7-8 g/L g of ammonium molybdate, 8-9 g/L g of magnesium sulfate, 25-26 g/L g of calcium nitrate, 1-2 g/L g of hydrofluoric acid, 9-10 g/L g of phosphoric acid, 12-13 g/L g of nitric acid, 6.5-7 g/L g of nickel nitrate, 2.5-3 g/L g of sodium nitrite and 5-5.5 g/L g of tartaric acid, and the solvent is water.
Comparative example five
The torsional shear type stud obtained in the patent of the manufacturing method for cold forging of the torsional shear type stud is used as a fifth comparative example, the application number of the torsional shear type stud is 201210006249.4, the application date is 2012, month 01 and 10, the publication number is CN103192022A, and the publication date is 2013, month 07 and 10.
In the above examples I to V and comparative examples I to III, a chamber type electron beam evaporation coater YQDH-500ZZS was used.
The studs made in example five and those made in comparative examples one to five were subjected to performance testing, the results of which were as follows:
salt spray test/d Etch width/mm Water boiling experiment
EXAMPLE five 48 <2 Level 0
Comparative example 1 31 >2 Stage 2
Comparative example No. two 30 >2 Stage 2
Comparative example No. three 32 >2 Stage 2
Comparative example No. four 27 >2 Stage 2
Comparative example five 21 >2 Stage 2
The salt spray test described above was performed according to ASTM B117-2003 salt spray test standards; carrying out an artificial atmosphere corrosion test according to GB/T10125, scratching a cross scratch on the surface of the stud by using a scratching knife, carrying out a neutral salt spray test for 700 hours on each sample to be tested, and observing and measuring the corrosion width of the scratched part; the water boiling test is to boil the sample to be tested in boiling water for 1 hour, and the adhesive force of each sample to be tested is tested by adopting a grid marking method according to GB/T9286-1998, so as to obtain a grade result.
As can be seen from the table above, the number of days for resisting saline and alkaline corrosion of the stud obtained in the fifth embodiment is far greater than that of the studs obtained in the first to fifth comparative examples, which shows that the stud obtained in the fifth embodiment has good membrane compactness and strong corrosion and oxidation resistance, and meanwhile, the corrosion resistance of the stud obtained in the fifth embodiment is obviously superior to that of the studs obtained in the first to fifth comparative examples; the film on the outer side of the stud obtained in the fifth embodiment after water boiling has good adhesive capacity, and meets the national grade requirements, while the studs obtained in the fifth group of comparative examples have different degrees of shedding after water boiling, and the high temperature resistance and the adhesive force of a coating film or a phosphating film are poor;
meanwhile, the experimental results of the fifth example, the fourth comparative example and the fifth comparative example show that: the fifth process adopts the strong shrinkage process, so that the stress is large, the impact force on a grinding tool and equipment is strong, the service life of the die is greatly reduced, the requirement of the strong shrinkage process on surface phosphating treatment of raw materials is high, and the service life of the die is greatly reduced if a phosphating film is slightly poor; in the second step, the fine upsetting and the chamfering are also greatly stressed, so that the influence on a die, materials and equipment is great; the third step needs to process a small diameter to prepare for tooth reduction, and the process is redundant; in the processing technology of the fifth embodiment and the fourth comparative example, the composite coating agent or the phosphating solution is adopted to carry out film coating treatment on the workpiece, the time of a salt spray resistance test is obviously longer than that of the fifth comparative example, the medium-diameter direct tooth shrinkage is carried out, a chamfer is arranged in the front of the medium-diameter direct tooth shrinkage, the tooth shrinkage is easy to form, the design stress is reasonable, the service lives of equipment and a die are greatly prolonged, and the operation is more convenient; and the composite coating agent and the processing technology are matched with each other in the fifth embodiment, so that the corrosion resistance of the stud obtained in the fifth embodiment is far superior to that of the stud obtained in the fourth embodiment, and meanwhile, the abrasion of equipment and a die can be reduced.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (9)

1. A manufacturing method of a torsional shear type stud is characterized by comprising the following steps:
s1, annealing the blank;
s2, carrying out acid washing treatment on the annealed blank, cleaning, immersing in an oxalic acid solution, and plating the composite coating agent on the surface of the blank subjected to the oxalic acid treatment by using an electron beam evaporation coating method to obtain a pretreated wire rod;
the composite coating agent comprises the following raw materials in percentage by weight: 25-35% of zirconium oxide, 8-12% of silicon dioxide, 15-20% of aluminum oxide, 3-8% of ferric nitrate, 5-10% of nitric acid, 5-12% of thickening agent and the balance of organic solvent;
s3, sequentially carrying out material breaking treatment, heading treatment, head fine heading, tail end chamfering treatment, rod shrinking treatment and tail end plum blossom tooth shrinking treatment on the pretreated wire.
2. The method for manufacturing a torsional shear type stud bolt according to claim 1, wherein in S1, the annealing process is specifically performed as follows: and heating to 680-760 ℃, keeping the temperature for 3-4 h in the heating process, then preserving the heat for 4-6 h, cooling to below 550 ℃, cooling at the speed of 2-4 ℃/min, and cooling to the normal temperature along with the furnace.
3. The method of manufacturing a torsional shear type stud bolt according to any one of claims 1-2, wherein in S2, the electron beam evaporation coating method is performed by placing the composite coating agent sheet on a copper target of an electron beam vacuum coater in which a vacuum chamber has a degree of vacuum of 1 × 10-4~1.5×10-4And Pa, plating the composite coating agent on the surface of the blank after the oxalic acid treatment at room temperature, wherein the moving speed of the blank after the oxalic acid treatment in the plating process is 0.1-0.2 mm/s.
4. The method for manufacturing the torsional shear type stud bolt according to any one of claims 1 to 2, wherein in S2, one or two of nitric acid, hydrochloric acid and sulfuric acid are selected as a pickling agent in the pickling process, and H in the pickling agent is used as H+The concentration of (b) is 0.5 to 10 mol/L.
5. The method for manufacturing a torsional shear type stud bolt according to any one of claims 1 to 2, wherein the concentration of the oxalic acid solution in S2 is 0.8 to 1.2 mol/L.
6. The method for manufacturing the torsional shear type stud bolt according to any one of claims 1-2, wherein in the S2, the mass fraction of the nitric acid is 60-70%, and the thickening agent is a polyurethane modified polyether thickening agent.
7. The method for manufacturing the torsional shear type stud according to any one of claims 1-2, wherein in S2, the composite coating agent is prepared by the following manufacturing process: adding zirconium oxide into an organic solvent, uniformly stirring at 75-90 ℃, adding silicon dioxide, aluminum oxide, ferric nitrate, nitric acid and a thickening agent during stirring to prepare slurry, and drying to obtain the composite coating agent.
8. The method for manufacturing the torsional shear type stud bolt according to any one of claims 1-2, wherein in S2, the organic solvent adopted in the preparation process of the composite coating agent is at least one of absolute ethyl alcohol, methanol, isopropanol and acetone.
9. The method for manufacturing the torsional shear type stud bolt according to claim 1, wherein in S3, the stud bolt obtained through the plum blossom-shaped tooth reduction treatment is deburred by a grinding machine, and a finished torsional shear type stud bolt is obtained after the stud bolt is qualified through inspection.
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CN101177764A (en) * 2007-11-21 2008-05-14 江阴康瑞不锈钢制品有限公司 N-containing martensitic stainless steel wire for high-tension bolt and method for manufacturing the same
CN101992221A (en) * 2009-08-14 2011-03-30 江苏宏泰不锈钢丝绳有限公司 Stainless steel wire on-line coating and drawing production process
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