CN109536763A - A kind of sintering process of miniature cemented carbide pellet - Google Patents
A kind of sintering process of miniature cemented carbide pellet Download PDFInfo
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- CN109536763A CN109536763A CN201811516444.5A CN201811516444A CN109536763A CN 109536763 A CN109536763 A CN 109536763A CN 201811516444 A CN201811516444 A CN 201811516444A CN 109536763 A CN109536763 A CN 109536763A
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- sintering
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
- C22C1/053—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds
- C22C1/055—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor with in situ formation of hard compounds using carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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Abstract
The invention discloses a kind of sintering process of miniature cemented carbide pellet.It is put into graphite, is covered with carbon felt, then be sintered by mixing cemented carbide pellet blank with sintering filler.Cemented carbide pellet is heated evenly during the sintering process, will not mutually be bonded；Sintering filler will not be spread, and be had no adverse effects to combustion furnace.The cemented carbide pellet porosity that the present invention is sintered is small, and appearance is consistent, and hardness is high.
Description
Technical field
The present invention relates to hard alloy technical fields, more particularly, to a kind of agglomerant of miniature cemented carbide pellet
Skill.
Background technique
Hard alloy refers to hard compounds and binding metal insoluble metal one made of powder metallurgical technique
Kind alloy material.Cemented carbide pellet is a kind of important high hardness material of surfacing and sufacing, by using heap
The modes such as weldering meet the functional requirements such as wear resistant corrosion resistant in conjunction with basis material, extend the service life of equipment and workpiece.Hard
Alloy spherolite has many advantages, such as that hardness is high, wear-resisting, anticorrosive, counter-bending, can replace all steel ball class products.It is suitable for heaps
Its surfacing on various tools and part, is formed the mill layer of layer of surface hardening, to improve work by weldering, surfacing, spraying method
Has the service life of part.
At present the technology of preparing and technique of cemented carbide pellet mainly pass through granulation, suppress, sintering and etc. prepare and
At.The raw producer of cemented carbide pellet mostly uses aluminium oxide that carbon black is added to make filler and carries out compacting sintering.The granularity phase of alumina powder
To thicker, during the sintering process cemented carbide pellet can be caused to squeeze, folder inside cemented carbide pellet finished product can be made in this way
Miscellaneous particle in irregular shape even broken particle, influences the porosity and service performance of cemented carbide pellet.Simultaneously in sintering process
In, sintering filler can be spread in sintering furnace burner hearth, polluted, influenced the service life of agglomerating plant.Due to hard alloy
Contain binding metal in spherolite, the problem of cemented carbide pellet sintered article is easy to appear bonding needs subsequent manually to be broken
Broken processing separates spherolite.
Summary of the invention
In order to solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of sintering of miniature cemented carbide pellet
Technique by the way that cemented carbide pellet blank and filler and steel ball to be put into graphite, then is put into sintering after graphite is covered
Furnace is sintered to avoid and mutually bond between cemented carbide pellet, moreover it is possible to prevent sintering filler to be diffused in sintering furnace burner hearth and expand
It dissipates, influences agglomerating plant work.Sintered carbide ball grain appearance prepared by the present invention is consistent, and hardness is high, and wearability is good, can apply to
Industrial production.
The purpose of the present invention is achieved through the following technical solutions:
A kind of sintering process of miniature cemented carbide pellet, comprising the following steps:
S1. sintering filler is prepared
S11. carbon black powders are added and are uniformly mixed through deoxygenating in calcined aluminium oxide；
S12. the mixed material in step S11 is subjected to ball milling；
S13. the material handled well in step S12 is crossed into sieve, weeds out agglomerated grain, obtain sintering filler；
S2. the sintering filler prepared in step S1 is mixed with spherolite blank, steel ball, then takes out steel ball；
S3. by the spherolite blank being uniformly mixed in step S2 and sintering filler filling graphite, graphite is covered with carbon felt
Box top, then be sintered after pushing down carbon felt with graphite cover board, obtain miniature cemented carbide pellet.
Further, the quality of carbon black powders is the 3~4% of filler gross mass in step S12.
The present invention needs strict control carbon content, the excessively high sintered products that will lead to of carbon content go out when preparation is sintered filler
There is poor carbon phase, can damage cemented carbide pellet end properties in existing carburizing phase, the too low sintered products that will lead to of carbon content.
Further, ball milling is carried out using ball grinding cylinder in step S12, abrading-ball used in ball grinding cylinder is steel ball, and ratio of grinding media to material is
5:1, Ball-milling Time are 2 hours.
Further, steel ball is the steel ball of Φ 15, Φ 10, Φ 8mm, ratio are as follows: 2:2:1.
Further, sieve mesh number is 80 mesh in step S13.
Further, the steel ball that steel ball is Φ 3mm in step S2, spherolite blank and steel ball, the mass fraction for being sintered filler
Than for 20:6:1.
Further, incorporation time is 5min in step S2.
Since sintering filler fineness is smaller, when mixing with spherolite blank, it is difficult uniformly to be wrapped in around spherolite blank.
The steel ball that Φ 3mm is added in the present invention in mixed process is mixed together, and by the extruding of steel ball, makes spherolite blank and sintering filler
It is uniformly mixed, then takes out steel ball.
Further, in step S3 sintering process be continuous sintering, including argon gas sintering, vacuum-sintering, partial pressure be sintered, it is cold
But four-stage.
Further, the technical process of argon gas sintering are as follows: preceding 80min is at the uniform velocity warming up to 320 DEG C from 20 DEG C, then keeps the temperature
80min, subsequent 180min is at the uniform velocity warming up to 470 DEG C from 320 DEG C, then keeps the temperature 140min, and subsequent 150min at the uniform velocity heats up from 470 DEG C
To 620 DEG C, then 90min is kept the temperature, in argon gas sintering process, argon flow 18L/min, furnace pressure is no more than 40mbar；With
60min carries out Tuo Wake sintering afterwards.
By using existing Tuo Wake sintering process, it is more thorough to guarantee that the residual forming agent in the entire burner hearth of sintering furnace excludes
Bottom keeps product surface color uniform, bright, the care and maintenance of advantageous sintering furnace.
Further, the technical process of vacuum-sintering are as follows: after extracting furnace gas out, preceding 50min at the uniform velocity heats up from 620 DEG C
To 800 DEG C, then keep the temperature 50min, subsequent 70min is at the uniform velocity warming up to 1150 DEG C from 800 DEG C, then keeps the temperature 50min, subsequent 50min from
1150 DEG C are at the uniform velocity warming up to 1350 DEG C.
Further, the technical process of sintering is divided are as follows: argon gas is filled in sintering furnace, air pressure in furnace is made to maintain 180
~200mbar, then in 1350 DEG C of heat preservation 20min, subsequent 45min is warming up to 1440 DEG C from 1350 DEG C, then keeps the temperature 20min, connects
Be filled with high pressure argon gas, so that air pressure is risen to 58bar, keep the temperature 40min.
Further, the technical process of cooling stage are as follows: first naturally cool to 950 DEG C, then open insulating layer, carry out fast
It is cold, when temperature is down to room temperature, furnace gas is discharged to normal pressure, then takes out cemented carbide pellet out of furnace.
Compared with prior art, the beneficial effects of the present invention are:
The present invention is sintered again by the way that cemented carbide pellet to be packed into graphite with sintering filler, thermally conductive uniform, is burnt
It is good to tie effect.During the sintering process, due to there is the presence of sintering filler between cemented carbide pellet, so adjacent hard alloy
Spherolite will not be bonded mutually, separated spherolite without hand breaking after the completion of sintering, saved the production time.
Cemented carbide pellet is mixed with sintering filler and is sintered by the present invention, and thermally conductive uniform, sintering effect is good, production
Cemented carbide pellet hardness is high, and appearance is consistent with uniform particle sizes, and wearability is good.
The present invention loads cemented carbide pellet and filler is sintered using graphite as loading tool, then is covered with carbon felt
Raw material are covered, the diffusion in production of sintering filler is can effectively prevent, influences sintering furnace normal work.
Detailed description of the invention
Fig. 1 is cemented carbide pellet metallograph made from embodiment 1.
Fig. 2 is cemented carbide pellet metallograph made from comparative example 1.
Fig. 3 is that graphite loads spherolite and is sintered the schematic diagram of filler.
Wherein 1 is graphite cover board, and 2 be carbon felt, and 3 be graphite, and 4 be sintering filler, and 5 be spherolite blank.
Specific embodiment
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with embodiment, but this hair
Bright protection scope is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, it is no intended to limit of the invention
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1
The present embodiment provides a kind of sintering process of miniature cemented carbide pellet, the specific steps are as follows:
S1. sintering filler is prepared
S11. carbon black powders are added and are uniformly mixed through deoxygenating in calcined aluminium oxide, obtain mixture, the matter of carbon black powder
Amount is the 3.5% of mixture quality；
S12. the mixture prepared in step S11 investment ball grinding cylinder is subjected to ball milling, ratio of grinding media to material 5:1 is ground in ball grinding cylinder
Ball is the steel ball of Φ 15, Φ 10, Φ 8mm, and Ball-milling Time is 2 hours, obtains ball milling material；
S13. the ball milling material prepared in step S12 is crossed into 80 meshes, removes agglomerated grain, obtains sintering filler；
S2. by the sintering filler prepared in step S1 and spherolite blank, the steel ball of Φ 3mm is mixed, and three's mass ratio is 20:
The steel ball of Φ 3mm is taken out after 6:1,5min；
S3. the spherolite blank being uniformly mixed in step S2 and sintering filler are fitted into graphite, cover graphite with carbon felt
Box top, then be sintered after pushing down carbon felt with graphite cover board, sintering process is as follows: graphite is put into the sintering of argon atmosphere
In furnace, preceding 80min is at the uniform velocity warming up to 320 DEG C from 20 DEG C, then keeps the temperature 80min, and subsequent 180min is at the uniform velocity warming up to 470 from 320 DEG C
DEG C, then 140min is kept the temperature, and subsequent 150min is at the uniform velocity warming up to 620 DEG C from 470 DEG C, then keeps the temperature 90min, in the above process, argon gas
Flow is 18L/min, and furnace pressure is no more than 40mbar, and subsequent 60min carries out Tuo Wake sintering；Then extract furnace gas out extremely
Vacuum state, 50min is at the uniform velocity warming up to 800 DEG C from 620 DEG C, then keeps the temperature 50min, and subsequent 70min is at the uniform velocity warming up to from 800 DEG C
1150 DEG C, then 50min is kept the temperature, subsequent 50min is at the uniform velocity warming up to 1350 DEG C from 1150 DEG C；Then argon gas is filled in sintering furnace,
So that air pressure in furnace is maintained 180~200mbar, is then warming up in 1350 DEG C of heat preservation 20min, subsequent 45min from 1350 DEG C
1440 DEG C, then 20min is kept the temperature, it is then filled with high pressure argon gas, so that air pressure in furnace is risen to 58bar, keeps the temperature 40min；It is then naturally cold
But to 950 DEG C, insulating layer is then opened, carries out rapid cooling, when temperature is down to room temperature, then discharge furnace gas to normal pressure will
Cemented carbide pellet takes out out of furnace.
Embodiment 2
The present embodiment provides a kind of sintering process of miniature cemented carbide pellet, the specific steps are as follows:
S1. sintering filler is prepared
S11. carbon black powders are added and are uniformly mixed through deoxygenating in calcined aluminium oxide, obtain mixture, the matter of carbon black powder
Amount is the 3% of mixture quality；
S12. the mixture prepared in step S11 investment ball grinding cylinder is subjected to ball milling, ratio of grinding media to material 5:1 is ground in ball grinding cylinder
Ball is the steel ball of Φ 15, Φ 10, Φ 8mm, and Ball-milling Time is 2 hours, obtains ball milling material；
S13. the ball milling material prepared in step S12 is crossed into 80 meshes, removes agglomerated grain, obtains sintering filler；
S2. by the sintering filler prepared in step S1 and spherolite blank, the steel ball of Φ 3mm is mixed, and three's mass ratio is 20:
The steel ball of Φ 3mm is taken out after 6:1,5min；
S3. the spherolite blank being uniformly mixed in step S2 and sintering filler are fitted into graphite, cover graphite with carbon felt
Box top, then be sintered after pushing down carbon felt with graphite cover board, sintering process is as follows: graphite is put into the sintering of argon atmosphere
In furnace, preceding 80min is at the uniform velocity warming up to 320 DEG C from 20 DEG C, then keeps the temperature 80min, and subsequent 180min is at the uniform velocity warming up to 470 from 320 DEG C
DEG C, then 140min is kept the temperature, and subsequent 150min is at the uniform velocity warming up to 620 DEG C from 470 DEG C, then keeps the temperature 90min, in the above process, argon gas
Flow is 18L/min, and furnace pressure is no more than 40mbar, and subsequent 60min carries out Tuo Wake sintering；Then extract furnace gas out extremely
Vacuum state, 50min is at the uniform velocity warming up to 800 DEG C from 620 DEG C, then keeps the temperature 50min, and subsequent 70min is at the uniform velocity warming up to from 800 DEG C
1150 DEG C, then 50min is kept the temperature, subsequent 50min is at the uniform velocity warming up to 1350 DEG C from 1150 DEG C；Then argon gas is filled in sintering furnace,
So that air pressure in furnace is maintained 180~200mbar, is then warming up in 1350 DEG C of heat preservation 20min, subsequent 45min from 1350 DEG C
1440 DEG C, then 20min is kept the temperature, it is then filled with high pressure argon gas, so that air pressure in furnace is risen to 58bar, keeps the temperature 40min；It is then naturally cold
But to 950 DEG C, insulating layer is then opened, carries out rapid cooling, when temperature is down to room temperature, then discharge furnace gas to normal pressure will
Cemented carbide pellet takes out out of furnace.
Embodiment 3
The present embodiment provides a kind of sintering process of miniature cemented carbide pellet, the specific steps are as follows:
S1. sintering filler is prepared
S11. carbon black powders are added and are uniformly mixed through deoxygenating in calcined aluminium oxide, obtain mixture, the matter of carbon black powder
Amount is the 4% of mixture quality；
S12. the mixture prepared in step S11 investment ball grinding cylinder is subjected to ball milling, ratio of grinding media to material 5:1 is ground in ball grinding cylinder
Ball is the steel ball of Φ 15, Φ 10, Φ 8mm, and Ball-milling Time is 2 hours, obtains ball milling material；
S13. the ball milling material prepared in step S12 is crossed into 80 meshes, removes agglomerated grain, obtains sintering filler；
S2. by the sintering filler prepared in step S1 and spherolite blank, the steel ball of Φ 3mm is mixed, and three's mass ratio is 20:
The steel ball of Φ 3mm is taken out after 6:1,5min；
S3. the spherolite blank being uniformly mixed in step S2 and sintering filler are fitted into graphite, cover graphite with carbon felt
Box top, then be sintered after pushing down carbon felt with graphite cover board, sintering process is as follows: graphite is put into the sintering of argon atmosphere
In furnace, preceding 80min is at the uniform velocity warming up to 320 DEG C from 20 DEG C, then keeps the temperature 80min, and subsequent 180min is at the uniform velocity warming up to 470 from 320 DEG C
DEG C, then 140min is kept the temperature, and subsequent 150min is at the uniform velocity warming up to 620 DEG C from 470 DEG C, then keeps the temperature 90min, in the above process, argon gas
Flow is 18L/min, and furnace pressure is no more than 40mbar, and subsequent 60min carries out Tuo Wake sintering；Then extract furnace gas out extremely
Vacuum state, 50min is at the uniform velocity warming up to 800 DEG C from 620 DEG C, then keeps the temperature 50min, and subsequent 70min is at the uniform velocity warming up to from 800 DEG C
1150 DEG C, then 50min is kept the temperature, subsequent 50min is at the uniform velocity warming up to 1350 DEG C from 1150 DEG C；Then argon gas is filled in sintering furnace,
So that air pressure in furnace is maintained 180~200mbar, is then warming up in 1350 DEG C of heat preservation 20min, subsequent 45min from 1350 DEG C
1440 DEG C, then 20min is kept the temperature, it is then filled with high pressure argon gas, so that air pressure in furnace is risen to 58bar, keeps the temperature 40min；It is then naturally cold
But to 950 DEG C, insulating layer is then opened, carries out rapid cooling, when temperature is down to room temperature, then discharge furnace gas to normal pressure will
Cemented carbide pellet takes out out of furnace.
Comparative example 1
This comparative example 1 provides a kind of sintering process of miniature cemented carbide pellet, with implementation referring to the step of embodiment 1
Example 1 is the difference is that the quality of carbon black powder is the 4.5% of mixture quality in step S11.
Comparative example 2
This comparative example 1 provides a kind of sintering process of miniature cemented carbide pellet, with implementation referring to the step of embodiment 1
Example 1 is the difference is that the quality of carbon black powder is the 2.5% of mixture quality in step S11.
The sintered carbide ball granule product prepared to Examples 1 to 3 and comparative example 1~2 carries out properties detection, as a result sees
Table 1.
Table 1
By above-mentioned experimental data can be seen that sintering filler in carbon content it is too high or too low, the sintered carbide ball of sintering
The hardness of grain finished product, the performances such as coercive force and porosity can all be affected.Spherolite blank and sintering are loaded using graphite
The mode that filler is sintered, so that cemented carbide pellet finished product grain size of the invention is uniform, it is not in bonding between spherolite
Problem.
Obviously, above-described embodiment is only intended to clearly illustrate technical solution of the present invention example, and is not
Restriction to embodiments of the present invention.For those of ordinary skill in the art, on the basis of the above description also
It can make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all
Made any modifications, equivalent replacements, and improvements etc. within the spirit and principles in the present invention should be included in right of the present invention and want
Within the protection scope asked.
Claims (10)
1. a kind of sintering process of miniature cemented carbide pellet, which comprises the following steps:
S1. sintering filler is prepared
S11. carbon black powders are added and are uniformly mixed through deoxygenating in calcined aluminium oxide；
S12. the mixed material in step S11 is subjected to ball milling；
S13. the material handled well in step S12 is crossed into sieve, weeds out agglomerated grain, obtain sintering filler；
S2. the sintering filler prepared in step S1 is mixed with spherolite blank, steel ball, then takes out steel ball；
S3. it by the spherolite blank being uniformly mixed in step S2 and sintering filler filling graphite, is covered on graphite with carbon felt
Portion, then be sintered after pushing down carbon felt with graphite cover board, obtain miniature cemented carbide pellet.
2. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that described in step S12
The quality of carbon black powders is the 3 ~ 4% of filler gross mass.
3. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that described in step S12
Ball milling uses ball grinding cylinder, and abrading-ball is steel ball in the ball grinding cylinder, and ratio of grinding media to material 5:1, Ball-milling Time is 2 hours.
4. the sintering process of miniature cemented carbide pellet according to claim 4, which is characterized in that the steel ball includes Φ
15, the steel ball of Φ 10,8 mm of Φ, ratio are as follows: 2:2:1.
5. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that described in step S13
Sieve mesh number is 80 mesh.
6. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that steel described in step S2
Ball is the steel ball of Φ 3mm, and spherolite blank and steel ball are sintered the mass fraction ratio of filler as 20:6:1.
7. the sintering process of miniature cemented carbide pellet according to claim 7, which is characterized in that ball described in step S2
Grain blank diameter is no more than 5mm.
8. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that mixed described in step S2
The conjunction time is 5min.
9. the sintering process of miniature cemented carbide pellet according to claim 1, which is characterized in that burnt described in step S3
Become continuous sintering, including argon gas sintering, vacuum-sintering, partial pressure sintering, cooling four-stage.
10. the miniature cemented carbide pellet of sintering process preparation described in a kind of any one according to claim 1 ~ 9.
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|---|---|---|---|---|
| JPS55119150A (en) * | 1979-03-03 | 1980-09-12 | Tatsuro Kuratomi | Cubic system boron nitride solid solution and preparation thereof |
| JPS6086225A (en) * | 1983-10-15 | 1985-05-15 | Showa Denko Kk | Preparation of sintered body for high hardness tool |
| JPS60138041A (en) * | 1983-12-27 | 1985-07-22 | Ibiden Co Ltd | Ceramic-metal composite body and its manufacture |
| CN102909370A (en) * | 2012-11-09 | 2013-02-06 | 四川科力特硬质合金股份有限公司 | Method for sintering damage-proof filler gasket of hard alloy ball |
| CN103495728A (en) * | 2013-10-14 | 2014-01-08 | 自贡长城硬面材料有限公司 | Pressing method of hard alloy balls |
| CN104294049A (en) * | 2014-09-23 | 2015-01-21 | 福建德隆硬质合金有限公司 | Recovery and reutilization technique of waste hard alloy |
-
2018
- 2018-12-12 CN CN201811516444.5A patent/CN109536763B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55119150A (en) * | 1979-03-03 | 1980-09-12 | Tatsuro Kuratomi | Cubic system boron nitride solid solution and preparation thereof |
| JPS6086225A (en) * | 1983-10-15 | 1985-05-15 | Showa Denko Kk | Preparation of sintered body for high hardness tool |
| JPS60138041A (en) * | 1983-12-27 | 1985-07-22 | Ibiden Co Ltd | Ceramic-metal composite body and its manufacture |
| CN102909370A (en) * | 2012-11-09 | 2013-02-06 | 四川科力特硬质合金股份有限公司 | Method for sintering damage-proof filler gasket of hard alloy ball |
| CN103495728A (en) * | 2013-10-14 | 2014-01-08 | 自贡长城硬面材料有限公司 | Pressing method of hard alloy balls |
| CN104294049A (en) * | 2014-09-23 | 2015-01-21 | 福建德隆硬质合金有限公司 | Recovery and reutilization technique of waste hard alloy |
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