CN106319438A - Rare earth catalytic permeation QPQ composition and method for manufacturing high-speed cutting tool by QPQ process - Google Patents
Rare earth catalytic permeation QPQ composition and method for manufacturing high-speed cutting tool by QPQ process Download PDFInfo
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Abstract
The invention discloses a rare earth catalytic permeation QPQ composition and a method for manufacturing a high-speed cutting tool by a QPQ process, and belongs to the metal surface treatment technology. A nitriding speed of a conventional QPQ process is relatively slow, the thickness of a nitrided layer formed on the surface of a metal is relatively small, the hardness of a corresponding depth is also relatively smaller, and the grain size of the nitrided layer is relatively low; the rare earth catalytic permeation QPQ composition contains a QPQ base salt, and a salt solution of the QPQ base salt contains CNO<->; the composition contains a rare earth compound as a catalytic permeation agent; the rare earth compound is a solid mixture of La carbonate and Ce carbonate according to the weight ratio of 1:3 to 3:1. The method comprises that the rare earth catalytic permeation QPQ composition is melted into a liquid state to become the salt solution, and a workpiece is immersed into the salt solution for nitridation. Compared with a conventional QPQ salt, the permeation rate is increased; the formed compound layer is 10 [mu]m or more deeper than a conventional QPQ compound layer, and the hardness of the corresponding depth is increased by 100 HV or more; the structure of the nitrided layer is increased by 1 grain size grade.
Description
Technical field
The invention belongs to metal surface treatment technology, a kind of method that rare earth catalytic cementation QPQ compositions and QPQ technique manufacture high-speed cutting instrument.
Background technology
Existing QPQ technique nitriding speed is relatively slow, and the thickness of the nitriding layer that metal surface is formed is less, and the hardness of corresponding depth is the least, and the grain size of nitriding layer is relatively low.
Summary of the invention
The technical assignment of the technical problem to be solved in the present invention and proposition is to overcome existing QPQ technique nitriding speed slower, the thickness of the nitriding layer that metal surface is formed is less, the hardness of corresponding depth is the least, the defects such as the grain size of nitriding layer is relatively low, it is provided that a kind of method that rare earth catalytic cementation QPQ compositions and QPQ technique manufacture high-speed cutting instrument.
For reaching above-mentioned purpose, the rare earth catalytic cementation QPQ compositions of the present invention, containing QPQ base salt, containing CNO in melted QPQ base salt - It is characterized in that: containing rare earth compound as energizer in said composition, described rare earth compound is the 0.0001-10% of described QPQ base salt weight, described rare earth compound is the solid mixture of La carbonate and Ce carbonate, comprises the ion of following percentage by weight in melted rare earth catalytic cementation QPQ compositions:
Na+=10~40wt%,
K+=8~25wt%,
CO3 2- =15~45wt%,
Cl - =10~20%,
CNO - =10~42%,
La3+=0.0001~10wt%,
Ce3+=0.0001~10wt%,
The percentage by weight sum of each ion is 100%.
Concrete, described La carbonate is 1:3~3:1 with the weight ratio of Ce carbonate.
As optimization technique means: comprise the ion of following percentage by weight in melted rare earth catalytic cementation QPQ compositions:
Na+=12~26wt%,
K+=12.0~18.0wt%,
CO3 2- =18~42wt%,
Cl - =10.0~16.0%,
CNO - =32.0~38.0%,
La3+=0.001~6wt%,
Ce3+=0.001~6wt%,
The percentage by weight sum of each ion is 100%.
For reaching above-mentioned purpose, the QPQ technique of the present invention manufactures the method for high-speed cutting instrument, nitrogenize to form nitriding layer in high-speed cutting tool surfaces including to high-speed cutting execution of instrument, it is characterized in that: described nitridation is to melt as saline solution by the rare earth catalytic cementation QPQ compositions of the present invention, and it is maintained at 520-650 DEG C, high-speed cutting instrument is immersed described saline solution 60-240min.
As optimization technique means: the rare earth catalytic cementation QPQ compositions of the present invention is added nitriding furnace and melts as saline solution, high-speed cutting instrument is lifted into described nitriding furnace to immerse saline solution.
As optimization technique means: described CNO - Weight concentration less than saline solution 32% time, in saline solution, add the appropriate rare earth catalytic cementation QPQ compositions described in any one of claim 1-3.
As optimization technique means: before carrying out described nitridation, the high-speed cutting instrument through temper is sequentially carried out clamping, defat/eliminate rust, cleans, preheat, after carrying out described nitridation, high-speed cutting instrument is sequentially polished, aoxidizes, cleans, is dried, immersion oil.Further, described clamping is that by shape, size, workpiece to be nitrogenized is loaded specific frock;Described defat/rust cleaning is workpiece to be nitrogenized to be put into industrial ultrasonic clean device, and ultrasonic degreasing/rust cleaning, the time is 20-40min;Described cleaning is to put the workpiece in rinse bath, washs 2-5 time with clear water;Described preheating is that work piece hoisting to be nitrogenized enters shaft furnace, preheats temperature 350-420 DEG C, temperature retention time 60min.
As optimization technique means: first high-speed cutting instrument is carried out temper and is then carried out continuously described nitridation, after carrying out described nitridation, high-speed cutting instrument is sequentially polished, aoxidizes, cleans, is dried, immersion oil.
As optimization technique means:
Workpiece after nitridation is carried out dry blasting in described polishing or/and wet abrasive blasting;
Described oxidation is workpiece clean, that be dried to be hung in shaft furnace carry out oxidation processes, oxidizing temperature 340-400 DEG C, temperature retention time 20-60min;
Described cleaning is that the workpiece after aoxidizing hangs out, and pre-cooling 3min the most in atmosphere is then placed in cold rinse bank cleaning;
Described dry be by cold water wash after workpiece be sequentially placed in the hot water storgae of two 70-100 DEG C, be impregnated with 10-20min respectively, finally carry in air, workpiece completes to be dried;
Described immersion oil is to be immersed by workpiece in oils and fats to adhere to one layer of oils and fats to improve the outward appearance of surface of the work at surface of the work.
The invention has the beneficial effects as follows:
1. the rare earth catalytic cementation QPQ compositions (RE-QPQ salt) of the present invention improves infiltration rate than conventional QPQ salt, shortens the process time (nitriding speed can improve 30-100%);
2. the compound layer that the rare earth catalytic cementation QPQ compositions (RE-QPQ salt) of the present invention is formed in metal surface than conventional QPQ compound layer depth 10 μm more than, the hardness of corresponding depth improves more than 100HV;The tissue of nitriding layer improves 1 grain size number.
The mechanism of the present invention is:
Rare earth element has high chemism, with N, O, strong chemical reaction occurs, and decomposes at surface of the work, generates more N, C atom with greater activity, Accelerate nitriding kinetics;
The atomic radius of rare earth element is big more than ferrum, and therefore after rare earth atom is by surface of the work absorption/solid solution, surface of the work iron atom distortion of lattice increases, and surface can be increased, and makes N, C atom be easier to by surface of the work absorption, solid solution, diffusion;
Rare earth element can accelerate the reduction of surface of the work oxide.
Detailed description of the invention
The present invention will be further described below.
The rare earth catalytic cementation QPQ compositions of the present invention, containing QPQ base salt, containing CNO in melted QPQ base salt - Containing rare earth compound as energizer in said composition, rare earth compound is the 0.0001-10% of QPQ base salt weight, and rare earth compound is the solid mixture of La carbonate and Ce carbonate, comprises the ion of following percentage by weight in melted rare earth catalytic cementation QPQ compositions:
Na+=10~40wt%,
K+=8~25wt%,
CO3 2- =15~45wt%,
Cl - =10~20%,
CNO - =10~42%,
La3+=0.0001~10wt%,
Ce3+=0.0001~10wt%,
The percentage by weight sum of each ion is 100%.
Concrete, La carbonate is 1:3~3:1 with the weight ratio of Ce carbonate.
In order to obtain more preferably technique effect, melted rare earth catalytic cementation QPQ compositions comprises the ion of following percentage by weight:
Na+=12~26wt%,
K+=12.0~18.0wt%,
CO3 2- =18~42wt%,
Cl - =10.0~16.0%,
CNO - =32.0~38.0%,
La3+=0.001~6wt%,
Ce3+=0.001~6wt%,
The percentage by weight sum of each ion is 100%.
RE-QPQ salt based on the invention described above, the QPQ technique of the present invention manufacture the method for high-speed cutting instrument it is crucial that to the nitridation of high-speed cutting execution of instrument to form nitriding layer in high-speed cutting tool surfaces, technical points: nitridation is to melt as saline solution by the RE-QPQ salt of the present invention, and it is maintained at 520-650 DEG C (nitriding temperature), high-speed cutting instrument is immersed saline solution 60-240min.
Concrete, it is the RE-QPQ salt of the present invention to add nitriding furnace melt as saline solution, high-speed cutting instrument is lifted into nitriding furnace to immerse saline solution.
Work as CNO - Weight concentration less than saline solution 32% time, in saline solution, add the RE-QPQ salt of the appropriate present invention.
In order to ensure the quality of QPQ technique, before carrying out nitridation the high-speed cutting instrument through temper sequentially carried out clamping, defat/eliminate rust, cleans, preheat, after nitrogenizing, high-speed cutting instrument is sequentially polished, aoxidizes, cleans, is dried, immersion oil.First high-speed cutting instrument can also be carried out temper and be then carried out continuously nitridation, after nitrogenizing, high-speed cutting instrument is sequentially polished, aoxidize, clean, be dried, immersion oil.Temper is combined by the method for the latter with QPQ process, so can omit the clamping of former approach, defat/eliminate rust, clean, preheats.
In the present invention: clamping is that by shape, size, workpiece to be nitrogenized is loaded specific frock;Defat/rust cleaning is workpiece to be nitrogenized to be put into industrial ultrasonic clean device, and ultrasonic degreasing/rust cleaning, the time is 20-40min;
Described cleaning is to put the workpiece in rinse bath, washs 2-5 time with clear water;Described preheating is that work piece hoisting to be nitrogenized enters shaft furnace, preheats temperature 350-420 DEG C, temperature retention time 60min;Workpiece after polishing nitridation carries out dry blasting or/and wet abrasive blasting (generally selects dry blasting, workpiece after will nitrogenizing carries out manual sandblasting/polishing, left hand takes some products, right hand sand jet outlet alignment product head blade, sandblasting 3-15min, according to product size, select air pressure, sand fineness;Carry out wet abrasive blasting if desired);Oxidation is workpiece clean, that be dried to be hung in shaft furnace carry out oxidation processes, oxidizing temperature 340-400 DEG C, temperature retention time 20-60min;Cleaning is that the workpiece after aoxidizing hangs out, and pre-cooling 3min the most in atmosphere is then placed in cold rinse bank cleaning;Be dried be by cold water wash after workpiece be sequentially placed in the hot water storgae of two 70-100 DEG C, be impregnated with 10-20min respectively, finally carry in air, workpiece completes to be dried;Immersion oil is to be immersed by workpiece in oils and fats to adhere to one layer of oils and fats to improve the outward appearance of surface of the work at surface of the work.
Conventional cleaning is to put the workpiece in sink, or manual operations, or logical compressed air makes water flow, and advantage is low cost, and shortcoming is that man-hour is long, cleans the most thorough.Major part producer is all to adopt in this way.The advantage that the present invention uses industrial ultrasonic to clean is that cleaning efficiency is high, and cleaning Du Genggao has the advantage that man-hour is short, surface of the work is without rust/fat residue, and surface is cleaner, improves nitriding effect, and extending service life of RE-QPQ salt, weak point is that a cost of investment is higher.
The product category that present invention can apply to includes: high-speed steel class fiber cropsization bore the high speed cutting elements such as (including the product of the various sizes specification of M2, M35, M42 trade mark), high-speed steel class chit drill.
Following table is various sample test Data Comparison:
Claims (10)
1. rare earth catalytic cementation QPQ compositions, containing QPQ base salt, containing CNO in melted QPQ base salt - It is characterized in that: containing rare earth compound as energizer in said composition, described rare earth compound is the 0.0001-10% of described QPQ base salt weight, described rare earth compound is the solid mixture of La carbonate and Ce carbonate, comprises the ion of following percentage by weight in melted rare earth catalytic cementation QPQ compositions:
Na+=10~40wt%,
K+=8~25wt%,
CO3 2- =15~45wt%,
Cl - =10~20%,
CNO - =10~42%,
La3+=0.0001~10wt%,
Ce3+=0.0001~10wt%,
The percentage by weight sum of each ion is 100%.
Rare earth catalytic cementation QPQ compositions the most according to claim 1, is characterized in that: described La carbonate is 1:3~3:1 with the weight ratio of Ce carbonate.
3. according to the rare earth catalytic cementation QPQ compositions according to any one of claim 1-3, it is characterized in that: the ion comprising following percentage by weight in melted rare earth catalytic cementation QPQ compositions:
Na+=12~26wt%,
K+=12.0~18.0wt%,
CO3 2- =18~42wt%,
Cl - =10.0~16.0%,
CNO - =32.0~38.0%,
La3+=0.001~6wt%,
Ce3+=0.001~6wt%,
The percentage by weight sum of each ion is 100%.
4.QPQ technique manufactures the method for high-speed cutting instrument, nitrogenize to form nitriding layer in high-speed cutting tool surfaces including to high-speed cutting execution of instrument, it is characterized in that: described nitridation is to melt as saline solution by the rare earth catalytic cementation QPQ compositions described in any one of claim 1-3, and it is maintained at 520-650 DEG C, high-speed cutting instrument is immersed described saline solution 60-240min.
QPQ technique the most according to claim 4 manufactures the method for high-speed cutting instrument, it is characterized in that: the rare earth catalytic cementation QPQ compositions described in any one of claim 1-3 is added nitriding furnace and melts as saline solution, high-speed cutting instrument is lifted into described nitriding furnace to immerse saline solution.
QPQ technique the most according to claim 4 manufactures the method for high-speed cutting instrument, it is characterized in that: described CNO - Weight concentration less than saline solution 32% time, in saline solution, add the appropriate rare earth catalytic cementation QPQ compositions described in any one of claim 1-3.
QPQ technique the most according to claim 4 manufactures the method for high-speed cutting instrument, it is characterized in that: before carrying out described nitridation, the high-speed cutting instrument through temper is sequentially carried out clamping, defat/eliminate rust, cleans, preheat, after carrying out described nitridation, high-speed cutting instrument is sequentially polished, aoxidizes, cleans, is dried, immersion oil.
QPQ technique the most according to claim 7 manufactures the method for high-speed cutting instrument, it is characterized in that:
Described clamping is that by shape, size, workpiece to be nitrogenized is loaded specific frock;
Described defat/rust cleaning is workpiece to be nitrogenized to be put into industrial ultrasonic clean device, and ultrasonic degreasing/rust cleaning, the time is 20-40min;
Described cleaning is to put the workpiece in rinse bath, washs 2-5 time with clear water;
Described preheating is that work piece hoisting to be nitrogenized enters shaft furnace, preheats temperature 350-420 DEG C, temperature retention time 60min.
QPQ technique the most according to claim 4 manufactures the method for high-speed cutting instrument, it is characterized in that: first high-speed cutting instrument is carried out temper and is then carried out continuously described nitridation, after carrying out described nitridation, high-speed cutting instrument is sequentially polished, aoxidizes, cleans, is dried, immersion oil.
10. the method manufacturing high-speed cutting instrument according to the QPQ technique described in claim 7 or 9, is characterized in that:
Workpiece after nitridation is carried out dry blasting in described polishing or/and wet abrasive blasting;
Described oxidation is workpiece clean, that be dried to be hung in shaft furnace carry out oxidation processes, oxidizing temperature 340-400 DEG C, temperature retention time 20-60min;
Described cleaning is that the workpiece after aoxidizing hangs out, and pre-cooling 3min the most in atmosphere is then placed in cold rinse bank cleaning;
Described dry be by cold water wash after workpiece be sequentially placed in the hot water storgae of two 70-100 DEG C, be impregnated with 10-20min respectively, finally carry in air, workpiece completes to be dried;
Described immersion oil is to be immersed by workpiece in oils and fats to adhere to one layer of oils and fats to improve the outward appearance of surface of the work at surface of the work.
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CN107130205A (en) * | 2017-05-03 | 2017-09-05 | 成都晟翔科技有限公司 | It is a kind of for environment-friendly type regeneration salt of QPQ techniques and its preparation method and application |
CN108251788A (en) * | 2018-01-11 | 2018-07-06 | 成都赛飞斯金属科技有限公司 | A kind of EMU braking steel back handled through tufftride and soft-nitriding treatment method |
CN108342681A (en) * | 2018-02-02 | 2018-07-31 | 成都晟翔科技有限公司 | A kind of environment-friendly type nitridation salt and its preparation method and application for QPQ techniques |
CN110976880A (en) * | 2019-12-12 | 2020-04-10 | 中山市奥博精密科技有限公司 | Processing technology of golf club head |
CN111500976A (en) * | 2020-05-29 | 2020-08-07 | 江苏奕华新材料科技有限公司 | Nitriding agent for nitrogen-carbon-oxygen co-cementation technology and preparation method thereof |
CN113025952A (en) * | 2021-03-03 | 2021-06-25 | 成都伍田机械技术有限责任公司 | Piston rod and machining method thereof |
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CN107130205A (en) * | 2017-05-03 | 2017-09-05 | 成都晟翔科技有限公司 | It is a kind of for environment-friendly type regeneration salt of QPQ techniques and its preparation method and application |
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CN111500976A (en) * | 2020-05-29 | 2020-08-07 | 江苏奕华新材料科技有限公司 | Nitriding agent for nitrogen-carbon-oxygen co-cementation technology and preparation method thereof |
CN111500976B (en) * | 2020-05-29 | 2023-08-22 | 江苏奕华新材料科技有限公司 | Nitriding agent for nitrocarburizing technology and preparation method thereof |
CN113025952A (en) * | 2021-03-03 | 2021-06-25 | 成都伍田机械技术有限责任公司 | Piston rod and machining method thereof |
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