CN104694896B - A kind of surface treatment method of heavy antisepsis bolt - Google Patents
A kind of surface treatment method of heavy antisepsis bolt Download PDFInfo
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- CN104694896B CN104694896B CN201510078399.XA CN201510078399A CN104694896B CN 104694896 B CN104694896 B CN 104694896B CN 201510078399 A CN201510078399 A CN 201510078399A CN 104694896 B CN104694896 B CN 104694896B
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Abstract
The present invention relates to a kind of surface treatment method of heavy antisepsis bolt, this handling process first passes through magnetron sputtering technique and constructs the first protecting film in bolt surface of the work, this first protecting film is formed bolt surface of the work is alternately laminated by Cr layer and Cr N shell, pure Cr film has intensive bacillar structure structure, and Cr N shell has preferable tight structure, the generation of slow pure Cr film column crystal can not only be hindered, the space leading to due to pure Cr layer columnar crystal structure can also preferably be filled up, tentatively improve bolt workpiece Corrosion Protection；Then construct the second protecting film outside the first protecting film, due to polymer monomer methyl methacrylate small volume, easily enter the defect on bolt surface, in gap, by the catalysis of azodiisobutyronitrile, methyl methacrylate polymerizing curable in the defect of the first protecting film, gap, the defect on bolt surface, gap are filled up, has been further ensured that bolt workpiece has preferable antiseptic property.
Description
Technical field
The present invention relates to heavy antisepsis handling process technical field, refer specifically to a kind of surface treatment method of heavy antisepsis bolt.
Background technology
In daily life and commercial production manufacture, bolt is requisite machine components, and it is referred to as rice of industry,
It is widely used in electronic product, engineering goods, digital product, power equipment, electronic product, ship, vehicle, hydraulic engineering, very
In to chemical experiment.Bolt in use, often because the burn into friction on bolt surface, abrasion the problems such as and lead to lost efficacy
Or destroy, thus affecting the service life of bolt, or even bring more serious potential safety hazard.Especially more severe in environmental condition
The occasion carved, the protection to bolt is put forward higher requirement.
Traditional surface protection technique is using plating, chemical plating method plating protection film in surface of the work, but institute
The thin film obtaining is combined poor with workpiece substrate, and the waste liquid producing during plating can be to causing severe environmental pollution.Magnetic
Control sputtering is a kind of eco-friendly physical gas phase deposition technology, is one of method for manufacturing thin film of great development prospect, this skill
Art is increasingly extensive to be applied in the preparation field of workpiece substrate surfacecti proteon film.Thin film using magnetron sputtering technique preparation has
Following advantage：(1) pollution-free；(2) deposit the smooth densification of film surface obtaining, thickness is uniform, controllability is good：(3) thin film with
Substrate combinating strength is high.But, due to by the shadow effect during magnetron sputtering deposition and low atomic migration energy power restriction, magnetic
The thin film that control sputtering sedimentation obtains is often the columnar crystal structure with more intercrystalline pore, and the space of column intergranular easily becomes thin
The weak location of film protection, corrosive liquid can be diffused rapidly to by these spaces and reach matrix, thus leading to the corruption to matrix for the thin film
Erosion protective action premature failure.
Therefore, for the process of surface treatment of current heavy antisepsis bolt, await further being improved.
Content of the invention
The technical problem to be solved is to provide a kind of table of heavy antisepsis bolt for the above-mentioned state of the art
Face processing method, this technique can form on bolt surface that layer of surface is smooth, consistency is high, film-substrate cohesion is high protection is thin
Film, effectively improves the antiseptic property of bolt.
The present invention solves the technical scheme that adopted of above-mentioned technical problem：A kind of surface treatment side of heavy antisepsis bolt
Method is it is characterised in that comprise the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 70～80 DEG C and cleans in ultrasonic cleaner
20～60min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
B, a is processed after bolt workpiece be completely submerged in the hydrochloric acid solution that mass concentration is 5～15wt%, under room temperature
5～15min is cleaned in ultrasonic cleaner；Take out bolt workpiece, clean the salt removing bolt surface of the work with pure water
Acid solution；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 20～30min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, make the angle of chromium target head and horizontal plane 45 °～90 ° it
Between；Bolt workpiece is placed on the indoor work rest of vacuum, evacuation so that the indoor vacuum of vacuum be less than or equal to 1 ×
10-3Pa；It is working gas using noble gases, with ion source, surface of the work is carried out, adjust the air pressure of ion source work
Scope is 2 × 10-2～7 × 10-2Pa, power is 100～150W, and scavenging period is 10～50min；
B, using noble gases be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 0.1～
10Pa, unit target sputtering power is 1～5W/cm2, sputtering sedimentation Cr film is carried out to bolt workpiece using at least one sputtering palladium,
Sputtering time is 100～1500s；
C, it is working gas using the mixed gas of nitrogen and noble gases, sputtering sedimentation Cr-N is carried out to bolt workpiece
Film, operating air pressure is 0.1～10Pa, and unit target sputtering power is 1～5W/cm2, using at least one sputtering palladium to bolt workpiece
Carry out sputtering sedimentation Cr-N film, sputtering time is 100～1500s；
D, it is repeated in step b, step c 5～25 times, make pure Cr layer and Cr-N layer alternately laminated in bolt surface of the work
Form the multi-layer film structure of periodic arrangement；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 5～10 DEG C/min, is warming up to 500
It is incubated 1～3h, then furnace cooling after～600 DEG C；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 3～8%
In, and add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.1～0.3%, then at 50～60 DEG C, stand 6～8h, take out and dry.
As a further improvement on the present invention, the chemical alkali liquor described in step (1) includes sodium hydroxide, sodium phosphate, silicon
Sour sodium, sulphonic acids surfactant and deionized water, described sodium hydroxide, sodium phosphate, sodium silicate, sulphonic acids surfactant
Concentration is respectively 10～15g/L, 60～70g/L, 10～15g/L, 0.1～0.5wt%.Wherein, sodium hydroxide is a kind of highly basic,
There is very strong saponifying ability, react with saponified oil and can generate water-soluble sodium soap；Sodium phosphate has preferable oil removing
Effect and cushioning effect, itself washing property is good, in addition with certain emulsifying capacity；Sodium silicate has preferable surface activity
With certain saponifying ability, it is one of optimal wetting agent, emulsifying agent and dispersant in alkaloid compound；Surfactant can remove
Go non-soap carburetion, in the molecular structure of surfactant, contain hydrophilic group and hydrophobic group, hydrophobic group adsorbs oily and molten
On the interface of liquid, hydrophilic group is combined with water, in the presence of surfactant molecule aligns, oil-solution interface
Surface tension can reduce, and under the effect such as solution convection current and stirring, greasy dirt just can readily depart from piece surface.
Preferably, described sulphonic acids surfactant is sulphosuccinates, alkylbenzenesulfonate, alkyl sulfonic acid
One of salt, α olefin sulfonate.
Preferably, described noble gases are one of helium, neon, argon, Krypton.
Improve further, after in described step (2), a step terminates, before b step starts, regulating fender and chromium target phase
Right, open the corresponding power supply of chromium target and carry out pre-sputtering 5～30min.Using such process, can by the impurity on chromium target surface and
Other pollutant sputter on baffle plate, to improve the thin film purity being splashed to bolt workpiece substrate surface.
Further, in described step (2) step c, nitrogen and the flow-rate ratio of noble gases are 4～6: 10.In this flow
Than under, the Main Ingredients and Appearance of coating is Cr2N, and containing pure Cr and CrN on a small quantity, thus on the basis eliminating Cr layer columnar crystal structure
On so that Cr film and Cr-N film is organically combined, further enhance the antiseptic property of bolt workpiece.
Preferably, ion source is utilized to provide ion beam assisted depositing in described step (2), ion source running voltage is 140
～160V, operating current is 0.7～1.2A；Using additional power source hot donut, vacuum indoor temperature is 50～300 DEG C；Profit
Apply the bias of 0～400V with additional power source between work rest and vacuum chamber.
In such scheme, the first protection film thickness of step (2) gained bolt surface of the work is 4～15 μm.
Compared with prior art, it is an advantage of the current invention that：
(1) plating Cr film has good adhesion to matrix material, can effectively improve wear-resistant, the anticorrosion of matrix material
Performance, the present invention is coated with Cr film and the Cr-N film of alternating deposit using the method for magnetron sputtering in bolt surface of the work, pure
Cr film has intensive bacillar structure structure, and Cr-N layer has preferable tight structure, can not only hinder slow pure Cr film post
The brilliant generation of shape, can also preferably fill up the space leading to due to pure Cr layer columnar crystal structure, formed layer of surface smooth,
The first protecting film that consistency is high, film-substrate cohesion is high, tentatively improves bolt workpiece Corrosion Protection；
(2) Main Ingredients and Appearance of Cr-N film is Cr2N, and containing pure Cr and CrN on a small quantity, thus eliminating Cr layer column crystal knot
So that Cr film can be organically combined with Cr-N film on the basis of structure, further enhance the antiseptic property of bolt workpiece；
(3) by magnetron sputtering after bolt surface of the work forms the first protecting film being made up of Cr film and Cr-N film,
Construct the second finer and closely woven protecting film on bolt surface again, due to polymer monomer methyl methacrylate small volume,
Easily enter the defect on bolt surface, in gap, and, by the catalysis of azodiisobutyronitrile, methyl methacrylate is
Polymerizing curable in the defect of one protecting film, gap, the defect on bolt surface, gap is filled up, has been further ensured that spiral shell
Bolt workpiece has preferable antiseptic property；
(4) after building the first protecting film, before structure the second protecting film, carry out heat treatment, can increase by the first protection
Adhesion between film and bolt workpiece substrate, improves case hardness and the rub resistance power of the first protecting film, eliminates residual stress.
Specific embodiment
With reference to embodiments the present invention is described in further detail.
Embodiment 1：
The surface treatment method of the heavy antisepsis bolt of the present embodiment comprises the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 70 DEG C and cleans in ultrasonic cleaner
60min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
Above-mentioned chemistry alkali liquor includes sodium hydroxide, sodium phosphate, sodium silicate, alkyl diphenyl base oxide disulfonate
(DOWFAX 2A1) and deionized water, wherein, sodium hydroxide, sodium phosphate, sodium silicate, alkyl diphenyl base oxide disulfonate
The concentration of (DOWFAX 2A1) is respectively 10g/L, 60g/L, 15g/L, 0.1wt%；
B, a is processed after bolt workpiece be completely submerged in mass concentration be 10wt% hydrochloric acid solution in, under room temperature in
10min is cleaned in ultrasonic cleaner；Take out bolt workpiece, the hydrochloric acid cleaning removal bolt surface of the work with pure water is molten
Liquid；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 25min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 50 °；?
Bolt workpiece is placed on the indoor work rest of vacuum, and evacuation is so that the indoor vacuum of vacuum is 1 × 10-3Pa；Using inertia
Gas is working gas, with ion source, surface of the work is carried out, and the air pressure range adjusting ion source work is 2 × 10-2Pa,
Power is 120W, and scavenging period is 30min；
Regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering 5min；
B, using helium be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 5Pa, unit target
Sputtering power is 2W/cm2, sputtering sedimentation Cr film is carried out using at least one sputtering palladium to bolt workpiece, sputtering time is 100s；
C, it is working gas using the mixed gas of nitrogen and helium, nitrogen is 4: 10 with the flow-rate ratio of helium, to bolt
Workpiece carries out sputtering sedimentation Cr-N film, and operating air pressure is 5Pa, and unit target sputtering power is 1W/cm2, using at least one sputtering
Palladium carries out sputtering sedimentation Cr-N film to bolt workpiece, and sputtering time is 800s；
D, it is repeated in step b, step c 10 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
Utilize ion source to provide ion beam assisted depositing when each step in this step (2) is carried out, ion source works simultaneously
Voltage is 145V, and operating current is 0.7A；Using additional power source hot donut, vacuum indoor temperature is 50 DEG C；Using additional
Power supply applies the bias of 0V between work rest and vacuum chamber；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 5 DEG C/min, after being warming up to 600 DEG C
Insulation 1h, then furnace cooling；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 3%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.1%, then at 50 DEG C, stand 8h, take out and dry.
Embodiment 2：
The surface treatment method of the heavy antisepsis bolt of the present embodiment comprises the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 75 DEG C and cleans in ultrasonic cleaner
40min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
Above-mentioned chemistry alkali liquor includes sodium hydroxide, sodium phosphate, sodium silicate, DBSA and deionized water, wherein,
Sodium hydroxide, sodium phosphate, sodium silicate, the concentration of DBSA are respectively 12g/L, 70g/L, 13g/L, 0.3wt%；
B, a is processed after bolt workpiece be completely submerged in mass concentration be 10wt% hydrochloric acid solution in, under room temperature in
5min is cleaned in ultrasonic cleaner；Take out bolt workpiece, clean the hydrochloric acid solution removing bolt surface of the work with pure water；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 30min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 45 °；?
Bolt workpiece is placed on the indoor work rest of vacuum, and evacuation is so that the indoor vacuum of vacuum is 0.5 × 10-3Pa；Using lazy
Property gas be working gas, with ion source, surface of the work is carried out, adjust ion source work air pressure range be 4 × 10- 2Pa, power is 150W, and scavenging period is 10min；
Regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering 30min；
B, using neon be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 0.1Pa, unit
Target sputtering power is 1W/cm2, sputtering sedimentation Cr film is carried out using at least one sputtering palladium to bolt workpiece, sputtering time is
1000s；
C, it is working gas using the mixed gas of nitrogen and neon, nitrogen is 5: 10 with the flow-rate ratio of neon, to bolt
Workpiece carries out sputtering sedimentation Cr-N film, and operating air pressure is 2Pa, and unit target sputtering power is 2W/cm2, using at least one sputtering
Palladium carries out sputtering sedimentation Cr-N film to bolt workpiece, and sputtering time is 100s；
D, it is repeated in step b, step c 15 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
Utilize ion source to provide ion beam assisted depositing when each step in this step (2) is carried out, ion source works simultaneously
Voltage is 140V, and operating current is 1.0A；Using additional power source hot donut, vacuum indoor temperature is 100 DEG C；Using additional
Power supply applies the bias of 400V between work rest and vacuum chamber；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 6 DEG C/min, after being warming up to 500 DEG C
Insulation 2h, then furnace cooling；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 4%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.2%, then at 55 DEG C, stand 7h, take out and dry.
Embodiment 3：
The surface treatment method of the heavy antisepsis bolt of the present embodiment comprises the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 80 DEG C and cleans in ultrasonic cleaner
20min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
Above-mentioned chemistry alkali liquor includes sodium hydroxide, sodium phosphate, sodium silicate, cocoyl isethionate (SCI-65) and goes
Ionized water, wherein, sodium hydroxide, sodium phosphate, sodium silicate, the concentration of cocoyl isethionate (SCI-65) are respectively 15g/
L, 65g/L, 10g/L, 0.5wt%；
B, a is processed after bolt workpiece be completely submerged in the hydrochloric acid solution that mass concentration is 5wt%, in super under room temperature
8min is cleaned in sound wave washer；Take out bolt workpiece, clean the hydrochloric acid solution removing bolt surface of the work with pure water；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 20min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 80 °；?
Bolt workpiece is placed on the indoor work rest of vacuum, and evacuation is so that the indoor vacuum of vacuum is 0.8 × 10-3Pa；Using lazy
Property gas be working gas, with ion source, surface of the work is carried out, adjust ion source work air pressure range be 6 × 10- 2Pa, power is 100W, and scavenging period is 50min；
Regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering 25min；
B, using argon be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 2Pa, unit target
Sputtering power is 4W/cm2, sputtering sedimentation Cr film is carried out using at least one sputtering palladium to bolt workpiece, sputtering time is 600s；
C, it is working gas using the mixed gas of nitrogen and argon, nitrogen is 5.5: 10 with the flow-rate ratio of argon, to spiral shell
Bolt workpiece carries out sputtering sedimentation Cr-N film, and operating air pressure is 0.1Pa, and unit target sputtering power is 3W/cm2, adopt at least one
Sputtering palladium carries out sputtering sedimentation Cr-N film to bolt workpiece, and sputtering time is 1000s；
D, it is repeated in step b, step c 5 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
Utilize ion source to provide ion beam assisted depositing when each step in this step (2) is carried out, ion source works simultaneously
Voltage is 150V, and operating current is 1.2A；Using additional power source hot donut, vacuum indoor temperature is 300 DEG C；Using additional
Power supply applies the bias of 200V between work rest and vacuum chamber；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 7 DEG C/min, after being warming up to 550 DEG C
Insulation 3h, then furnace cooling；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 6%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.3%, then at 60 DEG C, stand 6h, take out and dry.
Embodiment 4：
The surface treatment method of the heavy antisepsis bolt of the present embodiment comprises the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 76 DEG C and cleans in ultrasonic cleaner
50min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
Above-mentioned chemistry alkali liquor includes sodium hydroxide, sodium phosphate, sodium silicate, α olefin sulfonate and deionized water, wherein, hydrogen
Sodium oxide, sodium phosphate, sodium silicate, the concentration of α olefin sulfonate are respectively 13g/L, 64g/L, 12g/L, 0.2wt%；
B, a is processed after bolt workpiece be completely submerged in mass concentration be 15wt% hydrochloric acid solution in, under room temperature in
12min is cleaned in ultrasonic cleaner；Take out bolt workpiece, the hydrochloric acid cleaning removal bolt surface of the work with pure water is molten
Liquid；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 27min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 90 °；?
Bolt workpiece is placed on the indoor work rest of vacuum, and evacuation is so that the indoor vacuum of vacuum is 1 × 10-3Pa；Using inertia
Gas is working gas, with ion source, surface of the work is carried out, and the air pressure range adjusting ion source work is 7 × 10-2Pa,
Power is 130W, and scavenging period is 40min；
Regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering 20min；
B, using Krypton be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 10Pa, unit target
Sputtering power is 5W/cm2, sputtering sedimentation Cr film is carried out using at least one sputtering palladium to bolt workpiece, sputtering time is
1500s；
C, it is working gas using the mixed gas of nitrogen and Krypton, nitrogen is 6: 10 with the flow-rate ratio of Krypton, to bolt
Workpiece carries out sputtering sedimentation Cr-N film, and operating air pressure is 7Pa, and unit target sputtering power is 4W/cm2, using at least one sputtering
Palladium carries out sputtering sedimentation Cr-N film to bolt workpiece, and sputtering time is 600s；
D, it is repeated in step b, step c 20 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
Utilize ion source to provide ion beam assisted depositing when each step in this step (2) is carried out, ion source works simultaneously
Voltage is 155V, and operating current is 0.8A；Using additional power source hot donut, vacuum indoor temperature is 200 DEG C；Using additional
Power supply applies the bias of 300V between work rest and vacuum chamber；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 9 DEG C/min, after being warming up to 520 DEG C
Insulation 1.5h, then furnace cooling；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 7%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.25%, then at 51 DEG C, stand 7h, take out and dry.
Embodiment 5：The surface treatment method of the heavy antisepsis bolt of the present embodiment comprises the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, is heated to 78 DEG C and cleans in ultrasonic cleaner
30min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
Above-mentioned chemistry alkali liquor includes sodium hydroxide, sodium phosphate, sodium silicate, α-sodium olefin sulfonate and deionized water, wherein, hydrogen
Sodium oxide, sodium phosphate, sodium silicate, the concentration of α-sodium olefin sulfonate are respectively 11g/L, 65g/L, 13g/L, 0.4wt%；
B, a is processed after bolt workpiece be completely submerged in mass concentration be 12wt% hydrochloric acid solution in, under room temperature in
12min is cleaned in ultrasonic cleaner；Take out bolt workpiece, the hydrochloric acid cleaning removal bolt surface of the work with pure water is molten
Liquid；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, clear in ultrasonic cleaner under room temperature
Wash 23min, take out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 60 °；?
Bolt workpiece is placed on the indoor work rest of vacuum, and evacuation is so that the indoor vacuum of vacuum is 1 × 10-3Pa；Using inertia
Gas is working gas, with ion source, surface of the work is carried out, and the air pressure range adjusting ion source work is 5 × 10-2Pa,
Power is 140W, and scavenging period is 20min；
Regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering 10min；
B, using argon be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 7Pa, unit target
Sputtering power is 3W/cm2, sputtering sedimentation Cr film is carried out using at least one sputtering palladium to bolt workpiece, sputtering time is 800s；
C, it is working gas using the mixed gas of nitrogen and argon, nitrogen is 4.5: 10 with the flow-rate ratio of argon, to spiral shell
Bolt workpiece carries out sputtering sedimentation Cr-N film, and operating air pressure is 10Pa, and unit target sputtering power is 5W/cm2, splashed using at least one
Penetrate palladium and bolt workpiece is carried out with sputtering sedimentation Cr-N film, sputtering time is 1500s；
D, it is repeated in step b, step c 25 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
Utilize ion source to provide ion beam assisted depositing when each step in this step (2) is carried out, ion source works simultaneously
Voltage is 155V, and operating current is 1.1A；Using additional power source hot donut, vacuum indoor temperature is 150 DEG C；Using additional
Power supply applies the bias of 250V between work rest and vacuum chamber；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 10 DEG C/min, is warming up to 550 DEG C
It is incubated 2h, then furnace cooling afterwards；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 3%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is methyl methacrylate quality
0.2%, then at 57 DEG C, stand 7h, take out and dry.
Performance test is carried out to the bolt workpiece after processing in the various embodiments described above, wherein, salt spray test is pressed in GB5938
Property salt spray test (NSS) measure, corrosion electric current density and corrosion potential are obtained by dynamic polarization curve.Concrete test result is such as
Shown in table 1.
Table 1
It can be seen that, the bolt workpiece after the surface treatment method through the present invention is processed has excellent Corrosion Protection.
Alkyl diphenyl base oxide disulfonate (DOWFAX 2A1) in the present embodiment has along trade purchased from Guangzhou peak one hundred
Limit company, DBSA is purchased from Kunshan southeast chemical materialss company limited, cocoyl isethionate (SCI-65)
Purchased from Guangzhou Hong Chang Chemical Co., Ltd., α-sodium olefin sulfonate is purchased from that Yingkou City is prosperous and industrial chemicals company limited.
Claims (8)
1. a kind of surface treatment method of heavy antisepsis bolt is it is characterised in that comprise the following steps：
(1) pretreatment of bolt workpiece
A, bolt workpiece is completely submerged in chemical alkali liquor, be heated to 70～80 DEG C of cleanings 20 in ultrasonic cleaner～
60min；Take out bolt workpiece, clean the chemical alkali liquor removing bolt surface of the work with pure water；
B, a is processed after bolt workpiece be completely submerged in the hydrochloric acid solution that mass concentration is 5～15wt%, in super under room temperature
5～15min is cleaned in sound wave washer；Take out bolt workpiece, the hydrochloric acid cleaning removal bolt surface of the work with pure water is molten
Liquid；
C, b is processed after bolt workpiece be completely submerged in ethanol or acetone, under room temperature in ultrasonic cleaner clean 20
～30min, takes out standby；
The structure of (2) first protecting films
First protecting film is built in bolt surface of the work using magnetron sputtering technique, concrete steps include：
A, be more than in vacuum indoor location purity 98% chromium target, the angle making chromium target head and horizontal plane is between 45 °～90 °；
Bolt workpiece is placed on the indoor work rest of vacuum, evacuation is so that the indoor vacuum of vacuum is less than or equal to 1 × 10- 3Pa；It is working gas using noble gases, with ion source, surface of the work is carried out, adjust the air pressure model of ion source work
Enclose for 2 × 10-2～7 × 10-2Pa, power is 100～150W, and scavenging period is 10～50min；
B, using noble gases be working gas, bolt workpiece is carried out with sputtering sedimentation Cr film, operating air pressure be 0.1～10Pa,
Unit target sputtering power is 1～5W/cm2, sputtering sedimentation Cr film is carried out to bolt workpiece using at least one sputtering target, during sputtering
Between be 100～1500s；
C, it is working gas using the mixed gas of nitrogen and noble gases, bolt workpiece is carried out with sputtering sedimentation Cr-N film, work
Making air pressure is 0.1～10Pa, and unit target sputtering power is 1～5W/cm2, using at least one sputtering target, bolt workpiece is carried out
Sputtering sedimentation Cr-N film, sputtering time is 100～1500s；
D, it is repeated in step b, step c 5～25 times, make pure Cr layer and Cr-N layer in the alternately laminated formation of bolt surface of the work
The multi-layer film structure of periodic arrangement；
(3) heat treatment of bolt workpiece
Step (2) gained bolt workpiece is placed in Muffle furnace, setting programming rate is 5～10 DEG C/min, it is warming up to 500～
It is incubated 1～3h, then furnace cooling after 600 DEG C；
The structure of (4) second protecting films
Step (3) gained bolt workpiece is immersed in the methanol solution of the methyl methacrylate that mass concentration is 3～8%,
And add azodiisobutyronitrile in this solution, the quality making this azodiisobutyronitrile is the 0.1 of methyl methacrylate quality
～0.3%, then at 50～60 DEG C, stand 6～8h, take out and dry.
2. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Institute in step (1)
The chemical alkali liquor stated includes sodium hydroxide, sodium phosphate, sodium silicate, sulphonic acids surfactant and deionized water, described hydroxide
Sodium, sodium phosphate, sodium silicate, sulphonic acids surfactant concentration be respectively 10～15g/L, 60～70g/L, 10～15g/L,
0.1～0.5wt%.
3. a kind of heavy antisepsis bolt according to claim 2 surface treatment method it is characterised in that：Described sulphonic acids
Surfactant is one of sulphosuccinates, alkylbenzenesulfonate, alkylsulfonate, α olefin sulfonate.
4. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Described indifferent gas
Body is one of helium, neon, argon, Krypton.
5. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Described step (2)
After middle a step terminates, before b step starts, regulating fender is relative with chromium target, opens the corresponding power supply of chromium target and carries out pre-sputtering
5～30min.
6. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Described step (2) c
In step, nitrogen and the flow-rate ratio of noble gases are 4～6: 10.
7. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Described step (2)
Middle utilization ion source provides ion beam assisted depositing, and ion source running voltage is 140～160V, and operating current is 0.7～1.2A；
Using additional power source hot donut, vacuum indoor temperature is 50～300 DEG C；Using additional power source between work rest and vacuum chamber
Apply the bias of 0～400V.
8. a kind of heavy antisepsis bolt according to claim 1 surface treatment method it is characterised in that：Step (2) gained
First protection film thickness of bolt surface of the work is 4～15 μm.
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| CN112111697A (en) * | 2020-08-19 | 2020-12-22 | 张清苗 | Preparation method of heavy anti-corrosion alloy connecting bolt |
| CN113529033B (en) * | 2021-06-11 | 2023-04-07 | 中国科学院宁波材料技术与工程研究所 | Preparation method of protective coating and protective coating prepared by preparation method |
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| CN101343740A (en) * | 2007-11-30 | 2009-01-14 | 湖州金泰科技股份有限公司 | Film coating process for aluminium alloy wheel hub |
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