CN107385386A - A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology - Google Patents
A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and co-penetration technology Download PDFInfo
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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
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Abstract
A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant and technique, it is characterized in that described diffusion medium is the salt bath B-V co-penetrant using boron oxide as base salt, mainly it is made up of boron oxide, sodium fluoride, boron carbide, barium chloride, vanadic anhydride by certain mass percent.Technique be workpiece surface is polished, clean after be put into the crucible equipped with salt bath medium, in 950 DEG C of environment, be incubated 4h, carry out boron-vanadium co-penetration.The co-penetration layer thickness that the present invention obtains is 167 μm~182 μm, and average infiltration rate can reach 41.75~45.5 μm/h, and its infiltration rate is 2~3 times of traditional diffusion medium.It is 2~3 times using borax as base salt between surface microhardness can reach 2481.9~2849.5HV, is 6~7 times of matrix hardness.Infiltration layer and matrix are in metallurgical binding, and its adhesion can reach 63N.Coefficient of friction can be down to 0.13, and wearability is improved significantly.And the residual salt for oozing the workpiece after processing is easily cleared up.High abrasion, the parts of high rigidity can be needed extensively using surface, there is very big economic benefit.
Description
Technical field
The present invention relates to thermo-chemical treatment field, the formula and co-penetration technology of especially a kind of B-V co-penetrant are specific next
Say it is a kind of high rigidity, high infiltration rate and big infiltration layer to be prepared in alloy mold steel surface by the method that chemical thermal diffusion reaction deposits
And the boron-vanadium co-penetration layer of other excellent properties.
Background technology
Alloy die steel is widely used in auto parts and components and Making mold due to its excellent combination property.But in actual work
Make under environment, most alloy die steel can still wear because of surface transition and fail.Therefore die surface treatment technology
Making mold performance, service life etc. can be directly related to.Wherein equipment is simple, operates due to possessing for TD salt baths implantation technique
Conveniently, production cost is low and the infiltration layer of formation has excellent performance and favored by scholars.Salt bath vanadizing and ooze
Boron can improve material surface hardness and wearability, but single boronising due to produce boron it is crisp and make boronizing technology in application by
To a definite limitation, and single vanadinizing is thin about 10 μm because of infiltration layer, it is impossible in by big load.Salt bath boron-vanadium co-penetration new technology can
Overcome the crisp vanadium of boron thin, and there is the hardness higher than single infiltration layer and low coefficient of friction and good wearability.Applied to mould
Obvious technical economic benefit can be obtained on the fields such as tool, auto parts.So-called boron-vanadium co-penetration is exactly to be oozed simultaneously to steel surface
Enter the technical process of vanadium metal and boron atom.
Current TD salt bath implantation techniques can obtain more satisfactory hardness and thickness in singly oozing, but be led in permeation
Its effect of domain just significantly decreases.And using borax as base salt, oozed element is there is although being used widely
Species is few, is oozed that workpiece material species is few, it is warm high to ooze, infiltration layer is thin, salt bath viscosity is big, workpiece glues salt and cleans that residual salt is difficult, sets more
It is standby（Crucible etc.）The problems such as seriously corroded, seriously limit application.In order to solve the problem present invention present in traditional TD processing
One kind is proposed with B2O3 For the new salt bath B-V co-penetrant of base salt.Pass through new boron-vanadium co-penetration salt compared to traditional salt bath medium
The infiltration layer that bath agent is put possesses higher hardness, and infiltration rate and alloying layer thickness are greatly improved, and viscous salinity decrease workpiece
Easy to clean.The corrosivity of related equipment is substantially reduced.And there is good operability and huge economic value.
The content of the invention
The purpose of the present invention is to be directed to the defects of current alloy die steel wearability is inadequate, there is provided one kind is with B2O3For base
New the salt bath B-V co-penetrant and its co-infiltrating method of salt, new diffusion medium can greatly improve the hardness of co-penetration layer, thickness and
Infiltration rate, and the residual salt of osmosis work-piece is easy to clear up, and the corrosivity of related equipment is substantially reduced.With good operability
With huge economic value.
One of technical scheme is：
A kind of high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant, it is characterised in that：It is with boron oxide（B2O3）For base
The salt bath B-V co-penetrant of salt, mainly by boron oxide（B2O3）, sodium fluoride（NaF）, boron carbide（B4C）, barium chloride（BaCl2）, five
V 2 O（V2O5）Composition, wherein, boron oxide（B2O3）Mass percent for 44 ~ 53.8%, sodium fluoride（NaF）Quality hundred
Divide than being 22.2 ~ 27.5%, vanadic anhydride（V2O5）Mass percent for 4.4 ~ 4.5%, barium chloride（BaCl2）Quality hundred
Divide than being 4.4 ~ 5.3%, boron carbide（B4C）Mass percent be 8.4 ~ 25%；The mass percent sum of each component is 100%.
Use B2O3Substitute traditional borax, because of B2O3Have under the high temperature conditions and dissolve alkaline metal oxide well
Property, and compared to borax, B2O3Corrosivity can not prepare by force the more preferable infiltration layer of surface quality in the reaction；The B2O3For
Analyze it is pure, its content be more than 90%；B4C is pure for chemistry, and its content is more than 99%；V2O5 Pure to analyze, its content is 99.9%.
The two of technical scheme are：
A kind of alloy die steel surface salt bath boron-vanadium co-penetration side based on high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant
Method, it is characterised in that it comprises the following steps：
（1）According in above-mentioned salt bath boron-vanadium co-penetration agent prescription mass percent weigh raw material and mechanical mixture it is uniform after be put into earthenware
It is standby in crucible；
（2）Matrix material pre-processes：Matrix material selects 42CrMo steel, first that raw material wire cutting is big into 10 × 10 × 3mm
Small sample, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, surface is thrown to roughness areRa1 μm, then acetone ultrasonic wave clean to note 10min, alcohol flushing drying, be made sample；
（3）Boron-vanadium co-penetration processing：Crucible equipped with the common agent of salt bath boron vanadium is put into chamber type electric resistance furnace, is heated to 1000 ± 50
DEG C, 15 ± 5 min of insulation make salt bath boron vanadium, and agent is melted uniformly altogether, is then cooled to 950 DEG C of permeation temperature, boron-vanadium co-penetration is made
Agent；Sample is put into the boron-vanadium co-penetration salt bath matched somebody with somebody and got ready, and the groundwork face of sample is kept and salt bath flowing side as far as possible
To vertical, 4 ± 0.5h of held for some time taking-up oil quenchings, i.e., in the obtained boron vanadium layers of 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 1 ± 0.5h or so；
Well mixed be placed in corundum crucible of the B-V co-penetrant prepared is capped before experiment, then is put into high-temperature seal adhesive sealing
45min drying is incubated in baking oven in 100 DEG C.180 after the sample progress oil quenching of taking-up, specimen surface are cleaned up after experiment
2h is tempered at DEG C.
The beneficial effects of the invention are as follows：
（1）The invention provides the new salt bath B-V co-penetrant formula of a kind of high rigidity, high infiltration rate and big infiltration layer.With
Under the conditions of 42CrMo steel is matrix, 950 DEG C of insulation 4h, 2481.9 are can reach under infiltration layer extexine microhardness 200gf pressure~
It is to obtain 1.5~2 times of infiltration layer by base salt of borax between 2849.5HV, is 6~7 times of matrix hardness.
（2）The alloying layer thickness that is obtained using the method on workpiece is big, infiltration rate is fast, using 42CrMo steel as matrix, 950 DEG C of guarantors
Under the conditions of warm 4h, its infiltration layer maximum gauge can reach 167~182 μm, and average infiltration rate can reach 41.75~45.5 μm/h.It oozes
Speed is 2~3 times of traditional diffusion medium.
（3）It is in metallurgical binding with matrix, in embodiment one and the infiltration layer interface cohesion obtained under this diffusion medium is preferable
The adhesion of its infiltration layer of kind and matrix can reach 63N, and fretting wear coefficient is down to 0.13, and wearability is greatly improved.
（4）B-V co-penetrant provided by the invention, without any toxicity, to surrounding environment without any pollution.And reduce boron
Corrosion of the V co-penetrant to crucible and fixture.
（5）The co-penetration layer thickness that the present invention obtains is 167 μm~182 μm, average infiltration rate can reach 41.75~45.5 μm/
H, its infiltration rate are 2~3 times of traditional diffusion medium.It is with borax between surface microhardness can reach 2481.9~2849.5HV
It it is 6~7 times of matrix hardness for 2~3 times of base salt.Infiltration layer and matrix are in metallurgical binding, and its adhesion can reach 63N.Rub
0.13 can be down to by wiping coefficient, and wearability is improved significantly.And the residual salt for oozing the workpiece after processing is easily cleared up.Can be extensive
Using surface need high abrasion, high rigidity parts, have very big economic benefit.
Brief description of the drawings
Fig. 1 be embodiment one sample experiment after boron-vanadium co-penetration layer cross sectionization dye SEM shape appearance figures.
Fig. 2 be embodiment one sample experiment after boron-vanadium co-penetration layer surface XRD spectrum.
Fig. 3 be embodiment one sample experiment after the interface cohesion of boron-vanadium co-penetration layer and matrix try hard to.
Fig. 4 be embodiment one sample experiment after boron-vanadium co-penetration layer the friction coefficient frictional wear experiment carry out the time
Change.
Fig. 5 be embodiment one sample experiment after boron-vanadium co-penetration layer fretting wear SEM scheme.
Fig. 6 be embodiment two sample experiment after boron-vanadium co-penetration layer cross sectionization dye SEM shape appearance figures.
Fig. 7 be embodiment three sample experiment after boron-vanadium co-penetration layer cross sectionization dye SEM shape appearance figures.
Embodiment：
The present invention is further illustrated with example below in conjunction with the accompanying drawings.
Embodiment one.
As Figure 1-5
The salt bath B-V co-penetrant of the present embodiment is by boron oxide（B2O3）53.8g, sodium fluoride（NaF）27.5g, vanadic anhydride
（V2O5）5g, barium chloride（BaCl2）5.3g, boron carbide（B4C）8.4g is formed, and the B-V co-penetrant mechanical mixture prepared is uniform
After be placed in corundum crucible and be capped, then be put into high-temperature seal adhesive sealing in baking oven and 45 ± 5min drying be incubated in 100 ± 10 DEG C.
（1）Matrix material pre-processes：Matrix material of the present invention selects 42CrMo steel, first by raw material wire cutting into 10 ×
The sample of 10 × 3mm sizes, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, by surface throw to
Roughness isRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made sample；
（2）Boron-vanadium co-penetration processing：Crucible equipped with the common agent of salt bath boron vanadium is put into chamber type electric resistance furnace, is heated to 1000 ± 50
DEG C, 15 ± 5 min of insulation make salt bath boron vanadium, and agent is melted uniformly altogether, is then cooled to 950 DEG C of permeation temperature, boron-vanadium co-penetration is made
Agent；Sample is put into the boron-vanadium co-penetration salt bath matched somebody with somebody and got ready, and the groundwork face of sample is kept and salt bath flowing side as far as possible
To vertical, 4 ± 0.5h of held for some time taking-up oil quenchings, i.e., in the obtained boron vanadium layers of 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；If carrying out 180 DEG C of+2h tempering during specific implementation again after specimen surface cleans up, imitate
Fruit is more preferably.
Detected after taking out sample：The maximum gauge of boron-vanadium co-penetration layer is 167 μm after testing, and co-penetration layer extexine is micro-
It is 2481.9HV under hardness 100gf pressure.Thing phase composition VO, V of co-penetration layer4C2.67、 Fe2C、Fe2B、VCXOZ, matrix is together
The interface binding power of infiltration layer is 63N, and coefficient of friction substantially remains in 0.13 and wear extent very little.As Figure 1-5.
Embodiment two.
As shown in Figure 6.
The salt bath B-V co-penetrant of the present embodiment is by boron oxide（B2O3）47g, sodium fluoride（NaF）23.6g, vanadic anhydride
（V2O5）4.7g, barium chloride（BaCl2）4.7g, boron carbide（B4C）20g is formed, and the B-V co-penetrant mechanical mixture prepared is uniform
After be placed in corundum crucible and be capped, then be put into high-temperature seal adhesive sealing in baking oven and 45 ± 5min drying be incubated in 100 ± 10 DEG C.
（1）Matrix material pre-processes：Matrix material of the present invention selects 42CrMo steel, first by raw material wire cutting into 10 ×
The sample of 10 × 3mm sizes, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, by surface throw to
Roughness isRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made sample；
（2）Boron-vanadium co-penetration processing：Crucible equipped with the common agent of salt bath boron vanadium is put into chamber type electric resistance furnace, 1000 DEG C is heated to, protects
15 min of temperature make salt bath boron vanadium, and agent is melted uniformly altogether, is then cooled to 950 DEG C of permeation temperature, B-V co-penetrant is made；By sample
It is put into the boron-vanadium co-penetration 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, protects
Warm certain time 4h takes out oil quenching, i.e., boron vanadium layers 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；If carrying out 180 DEG C of+2h tempering during specific implementation again after specimen surface cleans up, imitate
Fruit is more preferably.
Detected after taking out sample：The maximum gauge of boron-vanadium co-penetration layer is 180 μm after testing, and co-penetration layer extexine is micro-
It is that 2604.9HV, the phase composition of infiltration layer thing and other performances and embodiment one are similar under hardness 100gf pressure.
Embodiment three.
As shown in Figure 7.
Used B-V co-penetrant is by boron oxide（B2O3）44g, sodium fluoride（NaF）22.2g, vanadic anhydride（V2O5）
4.4g, barium chloride（BaCl2）4.4g, boron carbide（B4C）25g form, by the B-V co-penetrant mechanical mixture prepared it is uniform after be placed in
It is capped in corundum crucible, then is put into high-temperature seal adhesive sealing in baking oven and 45 ± 5min drying is incubated in 100 ± 10 DEG C.
（1）Matrix material pre-processes：Matrix material of the present invention selects 42CrMo steel, first by raw material wire cutting into 10 ×
The sample of 10 × 3mm sizes, surface carry out sand paper polishing and mechanical polishing after oil removing, deionized water cleaning, by surface throw to
Roughness isRa1 μm, then acetone ultrasonic wave cleaning 10min, alcohol flushing drying, are made sample；
（2）Boron-vanadium co-penetration processing：Crucible equipped with the common agent of salt bath boron vanadium is put into chamber type electric resistance furnace, 1000 DEG C is heated to, protects
15 min of temperature make salt bath boron vanadium, and agent is melted uniformly altogether, is then cooled to 950 DEG C of permeation temperature, B-V co-penetrant is made；By sample
It is put into the boron-vanadium co-penetration 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, protects
Warm certain time 4h takes out oil quenching, i.e., boron vanadium layers 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；If carrying out 180 DEG C of+2h tempering during specific implementation again after specimen surface cleans up, imitate
Fruit is more preferably.
Detected after taking out sample：The maximum gauge of boron-vanadium co-penetration layer is 182 μm after testing, and co-penetration layer extexine is micro-
It is that 2849.5HV, the phase composition of infiltration layer thing and other performances and embodiment one are similar under hardness 100gf pressure.
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 high rigidity, high infiltration rate and big infiltration layer salt bath B-V co-penetrant, it is characterised in that it is with boron oxide（B2O3）For base
The salt bath B-V co-penetrant of salt, mainly by boron oxide（B2O3）, sodium fluoride（NaF）, boron carbide（B4C）, barium chloride（BaCl2）, five
V 2 O（V2O5）Composition；The mass percent of each component is respectively：Boron oxide（B2O3）44 ~ 53.8%, sodium fluoride（NaF）
22.2 ~ 27.5%, vanadic anhydride（V2O5）4.4 ~ 5%, barium chloride（BaCl2）4.4 ~ 5.3%, boron carbide（B4C）8.4 ~ 25%, respectively
The mass percent sum of component is 100%.
2. salt bath B-V co-penetrant according to claim 1, it is characterized in that using B2O3Substitute traditional borax, because of B2O3In height
There is the property of dissolving alkaline metal oxide well under the conditions of temperature, and compared to borax, B2O3Corrosivity is not strong in the reaction
The more preferable infiltration layer of surface quality can be prepared.
3. salt bath B-V co-penetrant according to claim 1, it is characterized in that the B2O3Pure to analyze, its content is not less than
90%；B4C is pure for chemistry, and its content is not less than 99%；V2O5 Pure to analyze, its content is not less than 99.9%.
4. a kind of alloy die steel surface salt bath boron-vanadium co-penetration method of salt bath B-V co-penetrant based on described in claim 1,
It is characterized in that it comprises the following steps：
（1）According to salt bath boron-vanadium co-penetration agent prescription mass percent weigh raw material and mechanical mixture it is uniform after be put into it is standby in crucible
With；
（2）Matrix material pre-processes：Raw matrix materials wire cutting is obtained into sample, surface is laggard through oil removing, deionized water cleaning
Row sand paper is polished and mechanical polishing, surface is thrown to roughness isRa1 μm, at least 10min then is cleaned with acetone ultrasonic wave, then
Dried up with alcohol flushing, sample is made；
（3）Boron-vanadium co-penetration processing：Crucible equipped with the common agent of salt bath boron vanadium is put into chamber type electric resistance furnace, is heated to 1000 ± 50
DEG C, 15 ± 5min of insulation makes salt bath boron vanadium, and agent is melted uniformly altogether, is then cooled to 950 DEG C of permeation temperature, boron-vanadium co-penetration is made
Agent；Sample is put into the boron-vanadium co-penetration salt bath matched somebody with somebody and got ready, and makes the groundwork face of sample keep hanging down with salt bath flow direction
Directly, it is incubated 4 ± 0.5h and 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 1 ± 0.5h.
5. according to the method for claim 4, it is placed in just it is characterized in that being well mixed the B-V co-penetrant prepared before experiment
It is capped in beautiful crucible, then is put into high-temperature seal adhesive sealing in baking oven and 45 ± 5min drying is incubated in 100 ± 10 DEG C.
6. according to the method for claim 4, it is characterized in that the sample of taking-up is carried out into oil quenching, specimen surface cleaning after experiment
After clean 2h is tempered at 180 DEG C.
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| CN113073290A (en) * | 2021-03-26 | 2021-07-06 | 长沙特耐金属材料科技有限公司 | Preparation method of metal-based material coated with multi-component composite coating |
| CN115125477A (en) * | 2022-06-29 | 2022-09-30 | 常州铂林热处理有限公司 | Composite nitriding heat treatment process |
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| CN113073290A (en) * | 2021-03-26 | 2021-07-06 | 长沙特耐金属材料科技有限公司 | Preparation method of metal-based material coated with multi-component composite coating |
| CN113073290B (en) * | 2021-03-26 | 2021-11-02 | 长沙特耐金属材料科技有限公司 | Preparation method of metal-based material coated with multi-component composite coating |
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Application publication date: 20171124 |
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