CN114836596A - Powder vanadinizing agent and laser remelting composite vanadinizing strengthening method for tool and die cutter - Google Patents
Powder vanadinizing agent and laser remelting composite vanadinizing strengthening method for tool and die cutter Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 139
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 238000005728 strengthening Methods 0.000 title claims abstract description 12
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 50
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 27
- 229910000628 Ferrovanadium Inorganic materials 0.000 claims abstract description 25
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 25
- PNXOJQQRXBVKEX-UHFFFAOYSA-N iron vanadium Chemical compound [V].[Fe] PNXOJQQRXBVKEX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims abstract description 21
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims abstract description 21
- 229940045803 cuprous chloride Drugs 0.000 claims abstract description 21
- 230000008595 infiltration Effects 0.000 claims abstract description 16
- 238000001764 infiltration Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims description 35
- 238000005496 tempering Methods 0.000 claims description 20
- 238000011282 treatment Methods 0.000 claims description 18
- 238000007789 sealing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- 238000011068 loading method Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 229910001315 Tool steel Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 4
- 229910052720 vanadium Inorganic materials 0.000 claims description 4
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000013532 laser treatment Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 230000002262 irrigation Effects 0.000 claims description 2
- 238000003973 irrigation Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 3
- 238000000498 ball milling Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 20
- 150000003839 salts Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- INZDTEICWPZYJM-UHFFFAOYSA-N 1-(chloromethyl)-4-[4-(chloromethyl)phenyl]benzene Chemical compound C1=CC(CCl)=CC=C1C1=CC=C(CCl)C=C1 INZDTEICWPZYJM-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000035777 life prolongation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/06—Surface hardening
- C21D1/09—Surface hardening by direct application of electrical or wave energy; by particle radiation
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
- C21D1/32—Soft annealing, e.g. spheroidising
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING 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
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/22—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for drills; for milling cutters; for machine cutting tools
-
- 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
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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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/60—After-treatment
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Organic Chemistry (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a powder vanadizing agent, which comprises: rare earth oxide powder: 1-4%; alumina powder: 40-50%; ferrovanadium powder: 40-50%; ammonium chloride powder: 1-4%; cuprous chloride powder: 1% -2%; the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder are uniformly mixed, and the sum of the mass percentages of the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder is 100%. Rare earth oxide, alumina powder, ferrovanadium powder and ammonium chloride powder in different mass ratios are adopted for ball milling and mixing, and the infiltration layer is compact, the toughness is good, and the surface is smooth. The invention also provides a method for strengthening the laser remelting composite vanadinizing of the tool and die cutter, which adopts laser pretreatment to be easy to operate, has high speed of forming a permeable layer and strong binding force between the permeable layer and a substrate.
Description
Technical Field
The invention relates to a powder vanadinizing agent and a method for strengthening laser remelting composite vanadinizing of a tool and a die cutter, belonging to the field of chemical heat treatment.
Background
With the increasingly harsh service conditions, the requirements of the tool and die cutter on the properties of hardness, wear resistance, corrosion resistance and the like are continuously improved, and the traditional carburization, nitridation, boronization and the like cannot meet the requirements of the service properties, so that a surface layer with higher strength and more wear resistance is required for strengthening the tool and die cutter. The vanadium carbide coating has the characteristics of high hardness, high wear resistance, low brittleness, high bonding strength with a matrix, seizure resistance and the like, and can be applied to dies such as a blanking die, a drawing die, a cold heading die, a forming die and the like, so that the service life of a tool die cutter is greatly prolonged. The currently used vanadinizing methods mainly include salt bath vanadinizing and powder vanadinizing. The salt bath vanadizing has the effects of specific gravity segregation and corrosion, and residual salt is adhered to the surface of a workpiece after the vanadizing, so that inconvenience is brought to subsequent treatment. The reusability of the powder vanadizing agent needs to be improved.
The Chinese patent application 201710667744.2 provides a salt bath vanadizing agent, the surface hardness of the vanadizing layer is higher after the vanadizing process is implemented, but the thickness of the vanadizing layer is thinner, and a lot of salt is adhered to the surface of the workpiece after the vanadizing, which brings inconvenience to the subsequent polishing treatment.
The Chinese patent application 202110168240.2 provides a vanadizing agent for a pin shaft of a timing chain of an engine, which is a powder vanadizing agent. The good surface vanadium layer is obtained by the process, but the treatment process time is long, and the repeated utilization rate of the penetration agent is not high.
Disclosure of Invention
The invention designs and develops a powder vanadinizing agent, which adopts rare earth oxide to catalyze vanadinizing, adopts rare earth oxide, alumina powder, ferrovanadium powder and ammonium chloride powder with different mass ratios to be ball-milled and mixed, and has compact infiltration layer, good obdurability and smooth surface.
The invention designs and develops a strengthening method for laser remelting composite vanadinizing of a tool and a die cutter, which adopts laser pretreatment to be easy to operate, has high production speed of a permeable layer and strong binding force between the permeable layer and a substrate.
The technical scheme provided by the invention is as follows:
a powder vanadizing agent comprising:
the powder vanadinizing agent comprises the following components:
rare earth oxide powder: 1-4%;
alumina powder: 40-50%;
ferrovanadium powder: 40-50%;
ammonium chloride powder: 1-4%;
cuprous chloride powder: 1% -2%;
the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder are uniformly mixed, and the sum of the mass percentages of the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder is 100%.
Preferably, the rare earth oxide has a purity of greater than 99%; the vanadium content in the ferrovanadium powder is more than 40%, and the granularity is 100-300 meshes; the alumina powder is spherical, and the granularity is 50-200 meshes; the ammonium chloride and the cuprous chloride are analytical pure reagents.
Preferably, the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder are fully mixed in a ball mill for 10-20 min according to the proportion.
The strengthening method of laser remelting composite vanadizing for tool and die cutter uses the powder vanadizing agent and comprises the following steps:
step one, laser remelting: after spheroidizing annealing is carried out on the small-sized die tool to be infiltrated, pulse laser remelting treatment is carried out on the surface of the small-sized die tool, the laser treatment current is 180-260A, the pulse width is 3ms, and the pulse frequency is 30 Hz;
step two, batching and sample loading: pouring part of prepared vanadinizing agent into a vanadinizing tank, enabling powder of the vanadinizing agent to account for 1/2-1/3 of the volume of the vanadinizing tank, placing a small tool and die cutter to be infiltrated into the vanadinizing tank, continuously adding the vanadinizing agent until the small tool and die cutter to be infiltrated is completely covered with the vanadinizing agent, and ensuring that a tool and die cutter steel piece is placed in the middle of the vanadinizing tank;
step three, vanadinizing: sealing the vanadinizing tank, then carrying out drying and exhaust treatment, cooling and sealing, then putting the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 1-7 h at 920-980 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again for heating, performing oil cooling after heat preservation, cooling to room temperature, and tempering.
Preferably, in the step one, after the laser remelting and before the vanadinizing process, the surface of the tool steel piece is pretreated, and the method comprises the following steps:
and (3) grinding the surface of the tool steel piece of the tool and die by using No. 120-1000 abrasive paper, mechanically polishing to ensure that the surface roughness Ra is less than or equal to 0.6um, ultrasonically cleaning for 10-20 min by using absolute ethyl alcohol, and drying.
Preferably, the tempering condition includes:
and (3) putting the quenched infiltrating irrigation into an oven at 180-200 ℃ for low-temperature tempering for 1.5-3 h, and air-cooling to room temperature after tempering.
Preferably, in the third step, the temperature of the drying exhaust treatment is 200-300 ℃, and the exhaust treatment time is 30 min.
The invention has the following beneficial effects:
the raw material powder of the vanadinizing agent can be repeatedly used for 3-5 times, the utilization rate is high, and the cost is low.
The strengthening method of the laser remelting composite vanadinizing of the tool and die cutter has the advantages of convenient operation, high production speed of the infiltration layer, compact and uniform infiltration layer, strong bonding of the infiltration layer and the matrix, smooth and flat surface, effective improvement of the wear resistance of the tool and die cutter steel piece, service life prolongation, low cost and wide application space in industrial production.
Drawings
FIG. 1 is a structural morphology diagram of a vanadia layer of example 1 after laser remelting pretreatment according to the present invention.
FIG. 2 is a structural morphology diagram of a vanadia layer of example 2 after laser remelting pretreatment according to the present invention.
FIG. 3 is a structural morphology diagram of a vanadia layer of example 3 after laser remelting pretreatment according to the present invention.
FIG. 4 is a structural morphology diagram of a vanadizing layer of comparative example 1 after laser remelting pretreatment according to the present invention.
Detailed Description
The present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
As shown in fig. 1-4, the invention provides a powder vanadizing agent, which adopts rare earth oxide to catalyze vanadizing, adopts rare earth oxide, alumina powder, ferrovanadium powder and ammonium chloride powder with different mass ratios to be ball-milled and mixed, has compact infiltration layer, good obdurability and flat surface, and comprises:
rare earth oxide powder: 1-4%;
alumina powder: 40-50%;
ferrovanadium powder: 40-50%;
ammonium chloride powder: 1-4%;
cuprous chloride powder: 1% -2%;
and fully mixing the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder in a ball mill for 10-20 min according to the proportion, wherein the sum of the mass percentages of the rare earth oxide powder, the alumina powder, the ferrovanadium powder and the ammonium chloride powder is 100%.
The purity of the rare earth oxide is more than 99%, the content of vanadium in the ferrovanadium powder is more than 40%, the granularity is 100-300 meshes, the alumina powder is spherical, the granularity is 50-200 meshes, and ammonium chloride and cuprous chloride are analytical pure reagents.
The invention also provides a method for strengthening the laser remelting composite vanadinizing of the tool and die cutter, and the solid vanadinizing agent prepared by the method comprises the following steps:
step one, laser remelting: after spheroidizing annealing is carried out on the small-sized die tool to be infiltrated, pulse laser remelting treatment is carried out on the surface of the small-sized die tool, the laser treatment current is 180-260A, the pulse width is 3ms, and the pulse frequency is 30 Hz;
after laser remelting and before a vanadinizing process, pretreating the surface of a tool and die cutter steel piece, wherein the pretreatment comprises the following steps: and (3) grinding the surface of the tool steel piece of the tool and die by using No. 120-1000 abrasive paper, mechanically polishing to ensure that the surface roughness Ra is less than or equal to 0.6um, ultrasonically cleaning for 10-20 min by using absolute ethyl alcohol, and drying.
Step two, batching and sample loading: firstly, pouring the prepared vanadinizing agent into a vanadinizing tank, enabling powder of the vanadinizing agent to account for 1/2-1/3 of the volume of the vanadinizing tank, placing the small-sized die tool to be subjected to vanadinizing in the vanadinizing tank, continuously adding the vanadinizing agent until the small-sized die tool to be subjected to vanadinizing is completely covered with the vanadinizing agent, and ensuring that a die tool steel piece is placed in the middle of the vanadinizing tank;
step three, vanadinizing: sealing the vanadinizing tank, then carrying out drying and exhaust treatment at 200-300 ℃ for 30min, cooling and sealing, then putting the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 1-7 h at 920-980 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again for heating, performing oil cooling after heat preservation, immediately putting the sample into an oven at 180-200 ℃ for low-temperature tempering for 1.5-3 h after cooling to room temperature, and performing air cooling to room temperature.
Example 1
Step one, carrying out laser remelting on a sample under the condition that the current is 180A, the pulse width is 3ms, and the frequency is 30 Hz:
step two, batching and sample loading: pouring the prepared vanadinizing agent into a vanadinizing tank, enabling the powder to account for 1/2-1/3 of the volume of the vanadinizing tank, placing a small tool and die cutter to be infiltrated into the infiltrating tank, and continuously adding the vanadinizing agent until the tool and die cutter to be infiltrated is completely covered, so as to ensure that a tool and die cutter steel piece is placed in the infiltrating tank;
wherein, vanadinizing agent includes: 48.5 percent of alumina powder, 48.5 percent of ferrovanadium powder, 1 percent of ammonium chloride powder, 1 percent of cuprous chloride powder and 1 percent of rare earth oxide powder;
step three, sealing the vanadinizing tank, then carrying out drying and exhausting treatment for 30min at 300 ℃, cooling and sealing, then placing the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 7h at 920 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again, heating the sample to 860 ℃, carrying out oil cooling after heat preservation, immediately placing the sample into an oven at 180 ℃ after cooling to the room temperature, carrying out low-temperature tempering for 3 hours, and carrying out air cooling to the room temperature.
After the above is completed, the second and third vanadification of the infiltrant is carried out under the same parameter values.
Example 2
Step one, carrying out laser remelting on a sample under the condition that the current is 260A, the pulse width is 3ms, and the frequency is 30 Hz:
step two, batching and sample loading: pouring the prepared vanadinizing agent into a vanadinizing tank, enabling the powder to account for 1/2-1/3 of the volume of the vanadinizing tank, placing a small tool and die cutter to be infiltrated into the infiltrating tank, and continuously adding the vanadinizing agent until the tool and die cutter to be infiltrated is completely covered, so as to ensure that a tool and die cutter steel piece is placed in the infiltrating tank;
wherein, vanadinizing agent includes: 45% of alumina powder, 45% of ferrovanadium powder, 4% of ammonium chloride powder, 2% of cuprous chloride powder and 4% of rare earth oxide powder;
step three, sealing the vanadinizing tank, then carrying out drying and exhausting treatment at 300 ℃ for 30min, cooling and sealing, then putting the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 7h at 980 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again, heating the sample to 860 ℃, carrying out oil cooling after heat preservation, immediately placing the sample into an oven at 180 ℃ after cooling to the room temperature, carrying out low-temperature tempering for 3 hours, and carrying out air cooling to the room temperature.
After the above is completed, the second and third vanadification of the infiltrant is carried out under the same parameter values.
Example 3
Step one, carrying out laser remelting on a sample under the condition that the current is 200A, the pulse width is 3ms, and the frequency is 30 Hz:
step two, batching and sample loading: pouring the prepared vanadinizing agent into a vanadinizing tank, enabling the powder to account for 1/2-1/3 of the volume of the vanadinizing tank, placing a small tool and die cutter to be infiltrated into the infiltrating tank, and continuously adding the vanadinizing agent until the tool and die cutter to be infiltrated is completely covered, so as to ensure that a tool and die cutter steel piece is placed in the infiltrating tank;
wherein, 47% of alumina powder, 47% of ferrovanadium powder, 4% of ammonium chloride powder, 1% of cuprous chloride powder and 1% of rare earth oxide powder;
step three, sealing the vanadinizing tank, then carrying out drying and exhausting treatment for 30min at 300 ℃, cooling and sealing, then placing the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 7h at 940 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into the infiltration tank filled with alumina powder again, heating the sample to 860 ℃, carrying out oil cooling after heat preservation, immediately placing the sample into an oven at 180-200 ℃ after cooling to room temperature, carrying out low-temperature tempering for 3 hours, and carrying out air cooling to the room temperature.
After the above contents are completed, the second and third vanadization of the infiltration agent are carried out under the same parameter values.
Comparing the results of the third vanadizing in examples 1 to 3, the thickness of the impregnation layer is 11 μm, 13 μm and 15 μm as shown in fig. 1, 2 and 3, and thus the optimal mixing ratio of the vanadizing agent is determined as the mixing ratio in example 3: 47 percent of alumina powder, 47 percent of ferrovanadium powder, 4 percent of ammonium chloride powder, 1 percent of cuprous chloride powder and 1 percent of rare earth oxide powder, and after three times of vanadinizing under the condition, the specific vanadinizing layer is thickest and the vanadinizing effect is good.
Comparative example 1
The coupon was not laser remelted:
step one, batching and sample loading: pouring the used vanadinizing agent for 2 times into a vanadinizing tank to enable the powder to account for 1/2-1/3 of the volume of the vanadinizing tank, placing the small tool and die cutter to be infiltrated into the infiltration tank, and continuously adding the vanadinizing agent until the tool and die cutter to be infiltrated is completely covered, so as to ensure that the tool and die cutter steel piece is placed in the middle of the infiltration tank;
wherein, 47 percent of alumina powder, 47 percent of ferrovanadium powder, 4 percent of ammonium chloride powder, 1 percent of cuprous chloride powder and 1 percent of rare earth oxide powder;
step two, sealing the vanadinizing tank, then carrying out drying and exhausting treatment for 30min at 300 ℃, cooling and sealing, then placing the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 7h at 940 ℃;
step three, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again, heating the sample to 860 ℃, carrying out oil cooling after heat preservation, immediately placing the sample into an oven at 180 ℃ after cooling to the room temperature, carrying out low-temperature tempering for 3 hours, and carrying out air cooling to the room temperature.
After the above is completed, the second and third vanadification of the infiltrant is carried out under the same parameter values.
The resulting infiltrated layer had a thickness of 8 μm, as shown in FIG. 4.
Compared with the experimental results obtained in the comparative example 1, the experimental results obtained in the examples 1 to 3 are compared, and the thickness of the vanadinizing layer obtained by adopting laser remelting pretreatment in the examples 1 to 3 is higher than that of the vanadinizing layer obtained in the comparative example 1, so that after the vanadinizing composite treatment before laser remelting provided by the invention is adopted, the growth speed of the vanadinizing layer is high, the structure is compact and uniform, the binding force with a substrate is strong, and the wear resistance of the tool and die cutter can be effectively improved.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (7)
1. The powder vanadinizing agent is characterized by comprising the following components in percentage by mass:
rare earth oxide powder: 1-4%;
alumina powder: 40-50%;
ferrovanadium powder: 40-50%;
ammonium chloride powder: 1-4%;
cuprous chloride powder: 1% -2%;
the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder are uniformly mixed, and the sum of the mass percentages of the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder is 100%.
2. The powder vanadia of claim 1, wherein the rare earth oxide is greater than 99% pure; the vanadium content in the ferrovanadium powder is more than 40%, and the granularity is 100-300 meshes; the alumina powder is spherical, and the granularity is 50-200 meshes; the ammonium chloride and the cuprous chloride are analytical pure reagents.
3. The powder vanadizing agent according to claim 2, wherein the rare earth oxide powder, the alumina powder, the ferrovanadium powder, the ammonium chloride powder and the cuprous chloride powder are fully mixed in a ball mill for 10-20 min according to a proportion.
4. A method for strengthening laser remelting composite vanadinizing of a tool and a die cutter is characterized by comprising the following steps:
step one, laser remelting: after spheroidizing annealing is carried out on the small-sized die tool to be infiltrated, pulse laser remelting treatment is carried out on the surface of the small-sized die tool, the laser treatment current is 180-260A, the pulse width is 3ms, and the pulse frequency is 30 Hz;
step two, batching and sample loading: pouring part of prepared vanadinizing agent into a vanadinizing tank, enabling powder of the vanadinizing agent to account for 1/2-1/3 of the volume of the vanadinizing tank, placing a small tool and die cutter to be infiltrated into the vanadinizing tank, continuously adding the vanadinizing agent until the small tool and die cutter to be infiltrated is completely covered with the vanadinizing agent, and ensuring that a tool and die cutter steel piece is placed in the middle of the vanadinizing tank;
step three, vanadinizing: sealing the vanadinizing tank, then carrying out drying and exhaust treatment, cooling and sealing, then putting the sealed vanadinizing tank into a high-temperature resistance furnace, and preserving heat for 1-7 h at 920-980 ℃;
step four, quenching and tempering: and after the vanadinizing is finished, cooling the sample to room temperature along with the furnace, taking out the sample, burying the tool and die cutter sample into a infiltration tank filled with alumina powder again for heating, performing oil cooling after heat preservation, cooling to room temperature, and tempering.
5. The method for strengthening the laser remelting composite vanadinizing tool of claim 4, wherein in the first step, after the laser remelting and before the vanadinizing process, the surface of the tool steel piece is pretreated, and the method comprises the following steps:
and (3) grinding the surface of the tool steel piece of the tool and die by using No. 120-1000 abrasive paper, mechanically polishing to ensure that the surface roughness Ra is less than or equal to 0.6um, ultrasonically cleaning for 10-20 min by using absolute ethyl alcohol, and drying.
6. The method for strengthening the laser remelting composite vanadinizing tool and tool according to claim 5, wherein the tempering conditions include:
and (3) putting the quenched infiltrating irrigation into an oven at 180-200 ℃ for low-temperature tempering for 1.5-3 h, and air-cooling to room temperature after tempering.
7. The method for strengthening the laser remelting composite vanadinizing of the tool and die cutter according to claim 6, wherein in the third step, the temperature of the drying and exhaust treatment is 200-300 ℃, and the exhaust treatment time is 30 min.
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