CN107385388A - A kind of new salt bath vanadizing agent for preparing super abrasive Vanadized layer and its technique - Google Patents
A kind of new salt bath vanadizing agent for preparing super abrasive Vanadized layer and its technique Download PDFInfo
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- CN107385388A CN107385388A CN201710667744.2A CN201710667744A CN107385388A CN 107385388 A CN107385388 A CN 107385388A CN 201710667744 A CN201710667744 A CN 201710667744A CN 107385388 A CN107385388 A CN 107385388A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING 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
- C23C12/00—Solid state diffusion of at least one non-metal element other than silicon and at least one metal element or silicon into metallic material surfaces
- C23C12/02—Diffusion in one step
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Abstract
A kind of new salt bath vanadizing agent for preparing super abrasive Vanadized layer and its technique, it is characterized in that described vanadinizing agent is formulated by boron oxide, sodium fluoride, vanadic anhydride, barium chloride, boron carbide by certain mass percent.Vanadinizing technique for will it is well mixed after raw material pour into corundum crucible, be warming up to 1000 DEG C of temperature, to temperature after be incubated 15 min and penetration enhancer is melted uniformly, be then cooled to 950 DEG C, obtained vanadinizing agent；Sample is put into the penetration enhancer salt bath matched somebody with somebody and got ready, and the groundwork face of sample is kept vertical with salt bath flow direction as far as possible, insulation 4h takes out air cooling, i.e., Vanadized layer is made in substrate surface.Vanadized layer case hardness prepared by the present invention（2935‑3012HV）For matrix hardness（400HV）7.3 7.5 times；The interface binding power of infiltration layer and matrix is 76N；Coefficient of friction is only 0.1 to belong to super abrasive infiltration layer.With simple to operate, the advantages of high comprehensive performance.
Description
Technical field
The present invention relates to metal surface properties modification field, especially a kind of mould steel TD Salt-Bath Vanadizing agent and its work
Skill.It is specifically a kind of to prepare that hardness is big, super abrasive in 42CrMo steel surfaces by the method that chemical thermal diffusion reaction deposits
Vanadized layer.
Background technology
As current industrial process promotes rapidly, manufacturing proposes higher requirement to the performance of mould steel.Mould
Although tool steel tool itself has good wearability and toughness, still because abrasion is failed, therefore in actual condition
It is necessary to improve its hardness and anti-wear performance using process for modifying surface.Since the 1960s, Surface Technics are fluffy
The exhibition of breaking out, in order to meet the increasingly fast-developing high request to material surface property, it developed at many surfaces
The new method of reason, wherein Japanese Toyota center Research Institute goes out the vanadinizing in borax bath, oozes niobium, oozes the element method such as button
(Toyota Diffusion Coating Process, abbreviation TD method).Its principle is to use diffusion method, forms steel surface and is oozed
The infiltration layer of the carbide of metal, chromium solid solution, boride etc., it is mainly used in the Making mold and zero of the industries such as automobile, metallurgy
On part.
TD technologies are a kind of cheap, surface strengthening technologies of process stabilizing, thus obtain the high praise of numerous scholars.VC
Coating has the advantages such as hardness is high, coefficient of friction is low as hard wear-resistant coating, can effectively improve the anti-wear performance of mould steel.
Hole German army et al. have studied the friction and wear behavior of Cr12MoV steel surface salt bath vanadizings, and its coefficient of friction measured is left 0.5
It is right；Li Ainong et al. have studied the performance of Cr12 steel surface salt bath vanadizings, and obtained layer surface coefficient of friction is 0.32.Due to
The material surface coating wear resistance that current research comes out is limited, therefore studies more resistant coating and have important meaning.In addition
Salt bath vanadizing technique is mainly based on borax base salt at present, but there is salt bath viscosity is big, poor fluidity, and it is more that workpiece glues salt, clearly
Wash the problems such as residual salt is difficult, and corrosion of crucible is serious.The present invention is also made that certain improvement in this respect, that is, uses B2O3Substitute boron
Sand, these defects are overcome well.
The content of the invention
The purpose of the present invention is to be directed to this limited problem of Most current mould steel anti-wear performance, there is provided it is a kind of with
B2O3Dare for the new salt bath vanadizing agent of base salt and its vanadinizing work, the invention can quickly obtain fine and close and super resistance in workpiece surface
The Vanadized layer of mill, and vanadinizing technique provided by the invention has good operability and excellent economy, while can pole
The residual salt cleaning difficulty of the big corrosivity for reducing salt bath medium and workpiece surface.
One of technical scheme is：
A kind of new salt bath vanadizing agent for preparing super abrasive Vanadized layer, it is characterised in that it is with boron oxide（B2O3）For base salt
Salt bath B-V co-penetrant, mainly by boron oxide（B2O3）, sodium fluoride（NaF）, boron carbide（B4C）, barium chloride（BaCl2）, five oxidation
Two vanadium（V2O5）Composition；The mass percent of each component is respectively：Boron oxide（B2O3）52-53.3%, sodium fluoride（NaF）24-
26.7%th, vanadic anhydride（V2O5）10.2-12.2%, barium chloride（BaCl2）5-7%, boron carbide（B4C）4-4.8%, each component
Mass percent sum is 100%.
The B4C and V2O5Mol ratio be 1.3；The B2O3Pure to analyze, its content is not less than 90%；V2O5For analysis
Pure, content is not less than 99.5%；B4C content is not less than 90%.
The two of technical scheme are：
A kind of new salt bath vanadizing technique for preparing super abrasive Vanadized layer, it is characterised in that it comprises the following steps：
（1）Mass percent according to the formula of the new salts vanadinizing agent described in claim 1 weighs raw material and mechanical mixture is equal
It is put into after even standby in crucible；
（2）Matrix material pre-processes：Raw material are processed into the sample of required size first, surface is clear through oil removing, deionized water
Sand paper polishing and mechanical polishing are carried out after washing, surface is thrown to roughness isRa1 μm, then acetone ultrasonic wave cleaning 10min, then
With being dried up after alcohol flushing, sample is made；
（3）Boron-vanadium co-penetration processing：Penetration enhancer after will be well mixed is poured into corundum crucible, is warming up to 1000 ± 50 DEG C, insulation 15
± 5min makes penetration enhancer melt uniformly, is then cooled to 950 DEG C, and vanadinizing agent is made；Sample is put into the vanadinizing agent matched somebody with somebody and got ready
The processing of row salt bath, and the groundwork face of sample is kept vertical with salt bath flow direction, 4 ± 0.5h of insulation takes out oil quenching, i.e.,
In matrix material（42CrMo steel）Boron vanadium layers are made in surface；
（4）Washed samples：Sample is gently tapped, the residual salt in its surface is come off, if still there is residual salt to adhere to, can be heated to water bath
100 DEG C are boiled 1h or so.
Well mixed be placed in corundum crucible of the penetration enhancer prepared is capped before experiment, then baking is put into high-temperature seal adhesive sealing
30min drying is incubated in case in 100 DEG C.
The sample of taking-up is subjected to oil quenching after experiment, specimen surface is tempered 2h after cleaning up at 180 DEG C.
The beneficial effects of the invention are as follows：
（1）The invention provides a kind of new salt bath vanadizing of preparation super abrasive Vanadized layer simple to operate, processing performance is excellent
Agent and its technique.
（2）Vanadized layer case hardness prepared by the present invention（2935-3012HV）For matrix hardness（400HV）7.3-7.5
Times；The interface binding power of infiltration layer and matrix is 76N；Coefficient of friction is only 0.1 to belong to super abrasive infiltration layer.The operation letter of the present invention
Single, obtained infiltration layer has excellent combination property, especially wearability, had great importance to process for modifying surface.
（3）Vanadized layer prepared by the present invention and matrix are in metallurgical binding, and the adhesion of infiltration layer and matrix is 76N；Vanadized layer
With excellent anti-wear performance, the coefficient of friction of its infiltration layer is only 0.1, and the coefficient of friction of matrix is 0.25.
（4）Vanadized layer thickness prepared by the present invention is 9 μm, and layer surface is clean, does not corrode.
（5）Vanadinizing agent provided by the invention is without any toxicity, to surrounding environment without any pollution.
Brief description of the drawings
Fig. 1 is the Vanadized layer cross-sectional view of embodiment one.
Fig. 2 is the Vanadized layer cross section EDS energy spectrum diagrams of embodiment one.
Fig. 3 is that the combination between the Vanadized layer of embodiment one and matrix is tried hard to.
Fig. 4 is the coefficient of friction experimental result picture of the vanadinizing layer surface of embodiment one.
Fig. 5 is the vanadinizing layer surface abrasion shape appearance figure of embodiment one
Fig. 6 is the coefficient of friction experimental result picture on original sample surface.
Fig. 7 is original sample surface abrasion shape appearance figure.
Embodiment：
The present invention is further illustrated with reference to the accompanying drawings and examples.
Embodiment one
As shown in figs. 1-7.
The salt bath vanadizing agent of the present invention is by boron oxide（B2O3）53.3g, sodium fluoride（NaF）26.7g, vanadic anhydride
（V2O5）10.7g, barium chloride（BaCl2）5g, boron carbide（B4C）4.3g composition.
Vanadinizing technique is：Workpiece surface pretreatment-vanadinizing processing-cleaning workpiece
（1）According to vanadinizing agent prescription mass percent weigh raw material and mechanical mixture it is uniform after be put into it is standby in crucible；Specifically
Well mixed be placed in corundum crucible of the penetration enhancer prepared is capped during implementation, then with high-temperature seal adhesive sealing be put into baking oven in
It is standby after 100 DEG C of insulation 30min drying.
（2）Matrix material pre-processes：With 42CrMo steel（Or similar material）As matrix material, wire cutting is used（Or other machines add
Work method）The sample of 10 × 10 × 3mm sizes is cut to, surface carries out sand paper polishing after oil removing, deionized water cleaning
And mechanical polishing, surface is thrown to roughness it isRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made
Sample；
（3）Vanadinizing processing：Raw material after will be well mixed is poured into corundum crucible, is warming up to 1000 ± 50 DEG C, insulation 15 ± 5
Min makes penetration enhancer melt uniformly, is then cooled to 950 DEG C, and vanadinizing agent is made；Sample is put into the penetration enhancer salt bath matched somebody with somebody and got ready, and
The groundwork face of sample is set to keep vertical with salt bath flow direction as far as possible, 4 ± 0.5h of held for some time takes out oil quenching, that is, exists
Vanadized layer is made in 42CrMo steel surfaces；
（4）Washed samples：Sample is gently tapped, the residual salt in its surface is come off, if still there is residual salt to adhere to, can be heated to water bath
100 DEG C are boiled 1h or so；Also the sample of taking-up can be subjected to oil quenching and clean in surface clean after the test during specific implementation
2h is tempered at 180 DEG C afterwards, further to improve surface quality.
Detected after taking out sample.It it is 9 μm through SEM detection embodiment one Vanadized layer maximum gauges, hardness is
2999.1HV, AdhesionStrength are about 76 N, skin-friction coefficient 0.1.
The Vanadized layer cross-sectional view of 42CrMo steel after the processing of the present embodiment vanadinizing is as shown in figure 1, Vanadized layer cross section
EDS energy spectrum diagrams as shown in Fig. 2 vanadinizing layer surface coefficient of friction experimental result as shown in figure 3, vanadinizing layer surface abrasion pattern such as
Shown in Fig. 4.And the coefficient of friction experimental result without vanadinizing before processing is as shown in figure 5, surface abrasion pattern is as shown in Figure 6.
Embodiment two
The salt bath vanadizing agent of the present invention is by boron oxide（B2O3）52g, sodium fluoride（NaF）24g, vanadic anhydride（V2O5）12.2g、
Barium chloride（BaCl2）7g, boron carbide（B4C）4.8g composition.
Vanadinizing technique is：Workpiece surface pretreatment-vanadinizing processing-cleaning workpiece
（1）According to vanadinizing agent prescription mass percent weigh raw material and mechanical mixture it is uniform after be put into it is standby in crucible；Specifically
Well mixed be placed in corundum crucible of the penetration enhancer prepared is capped during implementation, then with high-temperature seal adhesive sealing be put into baking oven in
It is standby after 100 DEG C of insulation 30min drying.
（2）Matrix material pre-processes：By the use of 42CrMo steel as matrix material, 10 × 10 are cut to wire cutting ×
The sample of 3mm sizes, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, surface are thrown to coarse
Spend and beRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made sample；
（3）Vanadinizing processing：Raw material after will be well mixed is poured into corundum crucible, is warming up to 1000 ± 50 DEG C, insulation 15 ± 5
Min makes penetration enhancer melt uniformly, is then cooled to 950 DEG C, and vanadinizing agent is made；Sample is put into the penetration enhancer salt bath matched somebody with somebody and got ready, and
The groundwork face of sample is set to keep vertical with salt bath flow direction as far as possible, 4 ± 0.5h of held for some time takes out oil quenching, that is, exists
Vanadized layer is made in 42CrMo steel surfaces；
（4）Washed samples：Sample is gently tapped, the residual salt in its surface is come off, if still there is residual salt to adhere to, can be heated to water bath
100 DEG C are boiled 1h or so；Also the sample of taking-up can be subjected to oil quenching and clean in surface clean after the test during specific implementation
2h is tempered at 180 DEG C afterwards, further to improve surface quality.
Detected after taking out sample.Its hardness is 3012HV, and other performances and Cross Section Morphology are similar to embodiment one.
Embodiment three
The salt bath vanadizing agent of the present invention is by boron oxide（B2O3）52.8g, sodium fluoride（NaF）26.7g, vanadic anhydride（V2O5）
10.2g, barium chloride（BaCl2）6.3g, boron carbide（B4C）4g is formed.
Vanadinizing technique is：Workpiece surface pretreatment-vanadinizing processing-cleaning workpiece
（1）According to vanadinizing agent prescription mass percent weigh raw material and mechanical mixture it is uniform after be put into it is standby in crucible；Specifically
Well mixed be placed in corundum crucible of the penetration enhancer prepared is capped during implementation, then with high-temperature seal adhesive sealing be put into baking oven in
It is standby after 100 DEG C of insulation 30min drying.
（2）Matrix material pre-processes：By the use of 42CrMo steel as matrix material, 10 × 10 are cut to wire cutting ×
The sample of 3mm sizes, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, surface are thrown to coarse
Spend and beRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made sample；
（3）Vanadinizing processing：Raw material after will be well mixed is poured into corundum crucible, is warming up to 1000 ± 50 DEG C, insulation 15 ± 5
Min makes penetration enhancer melt uniformly, is then cooled to 950 DEG C, and vanadinizing agent is made；Sample is put into the penetration enhancer salt bath matched somebody with somebody and got ready, and
The groundwork face of sample is set to keep vertical with salt bath flow direction as far as possible, 4 ± 0.5h of held for some time takes out oil quenching, that is, exists
Vanadized layer is made in 42CrMo steel surfaces；
（4）Washed samples：Sample is gently tapped, the residual salt in its surface is come off, if still there is residual salt to adhere to, can be heated to water bath
100 DEG C are boiled 1h or so；Also the sample of taking-up can be subjected to oil quenching and clean in surface clean after the test during specific implementation
2h is tempered at 180 DEG C afterwards, further to improve surface quality.
Detected after taking out sample.Its hardness is 2935HV, and other performances and Cross Section Morphology are similar to embodiment one.
Part that the present invention does not relate to is identical or can be realized using prior art in prior art.
Claims (6)
1. a kind of new salt bath vanadizing agent for preparing super abrasive Vanadized layer, it is characterised in that it is with boron oxide（B2O3）For base salt
Salt bath boron vanadium agent, mainly by boron oxide（B2O3）, sodium fluoride（NaF）, boron carbide（B4C）, barium chloride（BaCl2）, five oxidation two
Vanadium（V2O5）Composition；The mass percent of each component is respectively：Boron oxide（B2O3）52-53.3%, sodium fluoride（NaF）24-
26.7%th, vanadic anhydride（V2O5）10.2-12.2%, barium chloride（BaCl2）5-7%, boron carbide（B4C）4-4.8%, each component
Mass percent sum is 100%.
2. new salt bath vanadizing agent according to claim 1, it is characterized in that B4C and V2O5Mol ratio be 1.3.
3. new salt bath vanadizing agent according to claim 1, it is characterized in that the B2O3Pure to analyze, its content is not less than
90%；V2O5Pure to analyze, content is not less than 99.5%；B4C content is not less than 90%.
4. a kind of new salt bath vanadizing technique for preparing super abrasive Vanadized layer, it is characterised in that it comprises the following steps：
（1）Mass percent according to the formula of the new salts vanadinizing agent described in claim 1 weighs raw material and mechanical mixture is equal
It is put into after even standby in crucible；
（2）Matrix material pre-processes：Raw material are processed into the sample of required size first, surface is clear through oil removing, deionized water
Sand paper polishing and mechanical polishing are carried out after washing, surface is thrown to roughness isRa1 μm, then acetone ultrasonic wave cleaning 10min, then
With being dried up after alcohol flushing, sample is made；
（3）Boron-vanadium co-penetration processing：Penetration enhancer after will be well mixed is poured into corundum crucible, is warming up to 1000 ± 50 DEG C, insulation 15
± 5min makes penetration enhancer melt uniformly, is then cooled to 950 DEG C, and vanadinizing agent is made；Sample is put into the vanadinizing agent matched somebody with somebody and got ready
The processing of row salt bath, and the groundwork face of sample is kept vertical with salt bath flow direction, 4 ± 0.5h of insulation takes out oil quenching, i.e.,
In matrix material（42CrMo steel）Boron vanadium layers are made in surface；
（4）Washed samples：Sample is gently tapped, the residual salt in its surface is come off, if still there is residual salt to adhere to, can be heated to water bath
100 DEG C are boiled 1h or so.
5. the new salt bath vanadizing technique according to claim 4 for preparing super abrasive Vanadized layer, it is characterized in that will before experiment
Well mixed be placed in corundum crucible of penetration enhancer prepared is capped, then is put into high-temperature seal adhesive sealing in baking oven in 100 DEG C of insulations
30min is dried.
6. the new salt bath vanadizing technique according to claim 4 for preparing super abrasive Vanadized layer, it is characterized in that will after experiment
The sample of taking-up carries out oil quenching, and specimen surface is tempered 2h after cleaning up at 180 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582727A (en) * | 2021-06-16 | 2021-11-02 | 上海大学 | Method for preparing hard metal carbide coating on graphite surface |
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| JP2012031480A (en) * | 2010-07-30 | 2012-02-16 | Daito Kogyo Kk | Surface treatment method for iron alloy material |
| CN106367715A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | Metallic titanium surface salt-bath vanadizing agent and vanadizing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012031480A (en) * | 2010-07-30 | 2012-02-16 | Daito Kogyo Kk | Surface treatment method for iron alloy material |
| CN106367715A (en) * | 2016-09-12 | 2017-02-01 | 江苏大学 | Metallic titanium surface salt-bath vanadizing agent and vanadizing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582727A (en) * | 2021-06-16 | 2021-11-02 | 上海大学 | Method for preparing hard metal carbide coating on graphite surface |
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Application publication date: 20171124 |