CN108526366A - Self-lubricating hot forged mould and preparation method thereof based on Sialon ceramics - Google Patents
Self-lubricating hot forged mould and preparation method thereof based on Sialon ceramics Download PDFInfo
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- CN108526366A CN108526366A CN201810301741.1A CN201810301741A CN108526366A CN 108526366 A CN108526366 A CN 108526366A CN 201810301741 A CN201810301741 A CN 201810301741A CN 108526366 A CN108526366 A CN 108526366A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
- B21J5/02—Die forging; Trimming by making use of special dies ; Punching during forging
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/105—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing inorganic lubricating or binding agents, e.g. metal salts
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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
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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Abstract
The invention discloses a kind of self-lubricating hot forged moulds based on Sialon ceramics, interior mold including outer mold and in outer mold, wherein, the interior mold includes nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase, wherein, nickel chromium triangle matrix is mutually NiCr alloy powders, and ceramic hard is mutually Sialon ceramic powders, and lubrication is mutually CaF2Nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase three-phase powder are uniformly mixed using ball mill, then interior mold are prepared by the method for powder metallurgy by powder.Self-lubricating hot forged mould proposed by the present invention based on Sialon ceramics, solves the problems, such as that fretting wear and lubricant pollution occur under high temperature environment for hot forged mould.
Description
Technical field
The present invention relates to high temperature self-lubricating composite fields, especially design a kind of self-lubricating hot-forging die based on Sialon ceramics
Tool and preparation method thereof.
Background technology
In the forging of mold, extrusion process of production, the phenomenon that often will appear die wear, especially in the high temperature environment,
Wear phenomenon is more notable.Due to the presence of fretting wear, the service life for causing mold declines.And industrial mold cost at
This is high, it is desirable that mold will have longer service life under high temperature environment, how effectively overcome mold in a high temperauture environment
Fretting wear is very necessary.
In industrial processes, it is often used organic lubricant grease or lubricant.And the organic lubricant grease being often used exists
Oxygenolysis can occur under hot environment, lubricant effect is poor, and lubricant grease causes working environment certain pollution.In precision
In process, there is quite high requirement to the cleanliness factor of processing environment, and lubricant grease causes mold certain pollution.
The lubricant of use usually contains solids, i.e., adds kollag again in oil base or water base lubricant, such as：Graphite,
Molybdenum disulfide and other kollags.Die surface is with lubricator handled, although there is good lubricant effect, causes work
Make the pollution of environment.In being hot-forged process, there is quite high requirement to processing environment, and lubricant causes production environment
Certain pollution, affects the health of producers.During actual production, there is an urgent need under a kind of hot environment from
The material of lubrication.
Invention content
The main purpose of the present invention is to provide a kind of self-lubricating hot forged mould based on Sialon ceramics and its preparation sides
Method, it is intended to solve the problems, such as that fretting wear and lubricant pollution occur under high temperature environment for hot forged mould.
To achieve the above object, the present invention provides a kind of self-lubricating hot forged mould based on Sialon ceramics, including external mold
Tool and the interior mold in outer mold, wherein the interior mold includes nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating
Phase, wherein
Nickel chromium triangle matrix is mutually NiCr alloy powders, and ceramic hard is mutually Sialon ceramic powders, and lubrication is mutually CaF2Powder utilizes
Nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase three-phase powder are uniformly mixed by ball mill, then the side for passing through powder metallurgy
Interior mold is prepared in method.
Preferably, interior mold further includes stearic acid particles, with nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase one
It rises and interior mold is made by the method for powder metallurgy.
Preferably, the mass fraction of NiCr alloy powders is 70%-90%, and the mass fraction of Sialon ceramic powders is 2%-
15%, CaF2Mass fraction be powder 2%-15%, the mass fractions of stearic acid particles is 1%-2%.
Preferably, nickel chromium triangle matrix is mutually Ni80Cr20.
Present invention further propose that a kind of preparation method based on the above-mentioned self-lubricating hot forged mould based on Sialon ceramics,
Include the following steps：
Weigh appropriate NiCr metal powders, Sialon ceramic powders, CaF2After powder and stearic acid particles, by the powder after weighing
End is put into metal can, and stainless steel ball is added, and vacuum nitrogen filling gas shielded carries out ball milling by ball mill and mixes powder；
The powder mixed is positioned over sinter molding in electron tubes type sintering furnace by mold compression moulding；
After the sample sintered is by polishing, it is prepared into inserts, is applied in hot forged mould.
Preferably, ball mill ball milling mixes powder 4-6 hours.
Preferably, take out mixed powder, when with mold and hydraulic device compression moulding, pressure control 20 MPa ~
30MPa, 1 min -2min of dwell time.
Preferably, the good style of compression moulding is placed in when being heated in vacuum tube furnace, 400 is heated within the 1h times
DEG C, 0.5h is kept the temperature at 400 DEG C, is warming up to 1200 DEG C using 2h, 2h is kept the temperature under 1200 DEG C of environment；800 DEG C are cooled to through 1h,
30min is kept the temperature, 400 DEG C is cooled to by 1h, cools to room temperature with the furnace.
Preferably, the pressure of vacuum tube furnace is controlled 1 × 10-3Pa~9.9×10-2Pa。
Preferably, the style of sinter molding silicon carbide paper sanding and polishing, to remove the oxide skin on its surface.
Preferably, metallographic microstructure is observed, is prepared again after being tested by hardness, electron probe and high temperature friction and wear
At inserts.
Self-lubricating hot forged mould proposed by the present invention based on Sialon ceramics, can meet hot forged mould under high temperature environment
Requirement to material self-lubricating effect, while it is dirty to avoid the environment caused by using conventional lubrication grease in existing industrial production
Dye problem.
Description of the drawings
Fig. 1 is that the present invention is based on CaF in the self-lubricating hot forged mould of Sialon ceramics2Self-lubricating membrane formation mechanism schematic diagram；
Fig. 2 (a) is the high temperature friction and wear the present invention is based on the self-lubricating hot forged mould of Sialon ceramics under 600 DEG C of environment
Shape appearance figure；
Fig. 2 (b) is the high temperature friction and wear the present invention is based on the self-lubricating hot forged mould of Sialon ceramics under 600 DEG C of environment
Shape appearance figure；
Fig. 3 is CaF2Add the influence schematic diagram to material system high temperature friction coefficient；
Fig. 4 is that the present invention is based on the flow diagrams of the preparation method of the self-lubricating hot forged mould of Sialon ceramics；
Fig. 5 is that the present invention is based on hot-forging dies made of the preparation method fourth embodiment of the self-lubricating hot forged mould of Sialon ceramics
Structural schematic diagram.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific implementation mode
It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.
The present invention proposes a kind of self-lubricating hot forged mould based on Sialon ceramics.
Referring to figs. 1 to Fig. 3, a kind of self-lubricating hot forged mould based on Sialon ceramics, including outer mold and embedded in outer
Interior mold in mold, wherein the interior mold includes nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase, wherein
Nickel chromium triangle matrix is mutually NiCr alloy powders, and ceramic hard is mutually Sialon ceramic powders, and lubrication is mutually CaF2Powder utilizes
Nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase three-phase powder are uniformly mixed by ball mill, then the side for passing through powder metallurgy
Interior mold is prepared in method.
Further, interior mold further includes stearic acid particles, with nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase
Interior mold is made by the method for powder metallurgy together.Stearic acid content is too low to cause powder to stick tank in mechanical milling process, make
At wastage of material, and stearic acid has certain influence to powder pressing forming, and content is too low, and sample is easily broken when compacting；
Since stearic acid is impurity phase, too high levels cause harmful effect to product properties.
Preferably, nickel chromium triangle matrix is mutually Ni80Cr20.It is preferred that the mass fraction of NiCr alloy powders is 70%-90%,
The mass fraction of Sialon ceramic powders is 2%-15%, CaF2Mass fraction be powder 2%-15%, the quality of stearic acid particles
Score is 1%-2%.
When Sialon ceramic contents are excessively high, since ceramic sintering temperature is higher, influence the problems such as powder wetability causes
Sintered article performance is poor, and material internal is unable to densified sintering product, and internal bond strength difference is in powdery.And Sialon ceramic content shadows
Hardness, the wearability of product are rung, content is too low to make composite-material abrasive decline.Sialon ceramics additive amounts are found after exploration
Hardness number highest, wearability are best when being 5%.And CaF2As lubricant medium, additive amount is more, and material self-lubricating property is better,
But then, CaF2The bond strength and wearability of material can be reduced by increasing.It can be obtained by Fig. 2 a and Fig. 2 b, CaF2In height
Self-lubricating effect under warm environment is apparent, and sample wear morphology obviously becomes smooth.
High temperature friction coefficient when lines are using NiCr-Sialon as hot forged mould above in reference Fig. 3, Fig. 3 is to temperature
The curve graph of degree, below lines be with NiCr-Sialon-CaF2The song of high temperature friction coefficient when as hot forged mould to temperature
Line chart.From figure 3, it can be seen that being not added with CaF2Material under 600 DEG C of high temperature friction environment, friction coefficient 0.4, and adding
10% CaF is added2Material friction coefficient drop to 0.2, it can thus be appreciated that CaF2It is with obvious effects in the present invention.In view of it is each at
/ multiple performance influences each other, and above-mentioned is optimum range.
Wherein there are two types of phases for Sialon ceramics：α-Sialon ceramic abrasive resistances are outstanding, β-Sialon ceramics toughnesses are preferable；
Sialon ceramics are formed by three kinds of different ceramic combinations, including：α/β-Si3N4、Al2O3, AlN, it is compound according to a certain percentage and
At.Si3N4Mass fraction be 40% ~ 55%, Al2O3Mass fraction be 20% ~ 35%, AlN mass fraction be 5% ~ 15%.When
Within this range, the comprehensive performance of Sialon ceramics is more excellent for proportioning.
Self-lubricating hot forged mould proposed by the present invention based on Sialon ceramics, can meet hot forged mould under high temperature environment
Requirement to material self-lubricating effect, while it is dirty to avoid the environment caused by using conventional lubrication grease in existing industrial production
Dye problem.In addition, because metal-based self-lubricating toughness of material is preferable, wearability is insufficient；Ceramic based self-lubricating material high abrasion resistance,
Toughness is poor.Toughness is preferable in preferably ceramic of the present invention and anti abrasive β-Sialon ceramics and the excellent nickel chromium triangle of high-temperature behavior close
Golden Ni80Cr20.Two kinds of heat-resisting materials haveing excellent performance are compounded to form cermet, preferably and wear-resisting to meet toughness
Characteristic.Although metal and alloy material toughness, machinability and electrical and thermal conductivity are preferable, there is also many deficiencies, such as：
Wear-resisting, corrosion-resistant and heat-resisting quantity is poor.Ceramic material is met the tendency of since it compensates for the deficiency of metal and alloy material well
And give birth to, it needs if the two is combined together and can meet modernization development and cost can be saved.The β-that the present invention chooses
Sialon ceramics have following features：Si3N4Composite ceramics are in Si3N4-Al2O3There are β-Si in system3N4Solid solution, it be by
Al2O3In Al, O atom aliquot replacement Si3N4In Si, N atom form simple solid solution, the solid solution be Sialon pottery
Porcelain.Wherein β-Sialon ceramics are being in Si3N4On the basis of develop, other than having wear-resisting feature, also have both the spy of good toughness
Point, due to the high temperature resistant, wear-resisting of ceramics, the characteristics such as good toughness, the present invention is added to cermet system as hardening constituent
In.And the metal_based material that the present invention chooses has the property that for Ni80Cr20：It is good high-temperature mechanical property, heat-resisting and resistance to
Oxidation susceptibility.Nichrome high-temperature behavior is excellent, still has good mechanical performance at 500 DEG C or more, and at high temperature, Ni-based
Material surface, which is oxidized easily, generates NiO, with good adhesion and plasticity, also has certain high temperature lubricating and makees
With.
Present invention further propose that a kind of preparation method of the self-lubricating hot forged mould based on Sialon ceramics.
With reference to Fig. 4, a kind of preparation method of the self-lubricating hot forged mould based on Sialon ceramics includes the following steps：
Step S10 weighs appropriate NiCr metal powders, Sialon ceramic powders, CaF2After powder and stearic acid particles, it will claim
Powder after amount is put into metal can, and stainless steel ball is added, and vacuum nitrogen filling gas shielded carries out ball milling by ball mill and mixes powder；
Step S20, the powder mixed are positioned over sinter molding in electron tubes type sintering furnace by mold compression moulding；
Step S30 is prepared into inserts after the sample sintered is by polishing, applies in hot forged mould.
In step S10, ball mill ball milling mixes powder 4-6 hours.Ball-milling Time is too short to make material mix uneven, time mistake
Cold welding occurs between long powder, powder particle is thicker.
In step S20, when with mold and hydraulic device compression moulding, pressure was controlled in 20 MPa ~ 30MPa, dwell time
1 min -2min。
The good style of compression moulding is placed in when being heated in vacuum tube furnace, 400 DEG C is heated within the 1h times, 400
DEG C heat preservation 0.5h, be warming up to 1200 DEG C using 2h, 2h kept the temperature under 1200 DEG C of environment；800 DEG C are cooled to through 1h, heat preservation
30min is cooled to 400 DEG C by 1h, cools to room temperature with the furnace.
The pressure of vacuum tube furnace is controlled 1 × 10-3Pa~9.9×10-2Pa。
In step S30, the style silicon carbide paper sanding and polishing of sinter molding, to remove the oxide skin on its surface.
After the sample sintered is by polishing, metallographic microstructure is observed, hardness, electron probe and high temperature friction are passed through
Inserts is prepared into after wear testing again.It specifically, can be by high temperature friction and wear machine come the high temperature friction performance of verifying articles.
This preparation method is illustrated with next embodiment.
Case study on implementation 1
A kind of NiCr-Sialon-CaF2Self-lubricating mold materials, are prepared by the following method.
1, NiCr-Sialon-CaF is configured2Powder：Take 80 parts of Ni80Cr20 powder, 10 parts of Sialon powder, CaF2Powder
10 parts, 1.5 parts of forming agent stearic acid；First vacuum nitrogen filling gas disposal, ball milling mixing 5 hours, ratio of grinding media to material 1 are placed in metal can:
6, rotating speed 200r/min；
2, the good powder sieving of ball milling mixing is handled, sieve pore size is 200 mesh, and the powder configured takes powder in a mold
Compression moulding, pressure size choose 22Mpa, dwell time 1min；
3, the style of compression moulding is placed in crucible, and 1200 degrees Celsius are heated in vacuum tube furnace, keeps the temperature two hours；
4, the temperature program of vacuum tube furnace：By 1 hour, it is heated to 400 DEG C；400 DEG C of heat preservation 30min；Using two hours
1200 DEG C are heated to, 2 hours are kept the temperature at 1200 DEG C；800 DEG C were cooled to by 1 hour, 400 DEG C were cooled to using 1 hour, with
Stove is cooled to room temperature；
5, the samples with water grinding machine sanding and polishing that will be prepared carries out 600 DEG C of high temperature friction examination on high temperature friction and wear machine
It tests, obtains the friction coefficient of material prepared.Wear morphology is referring to attached drawing 2 (a), (b), and friction coefficient is referring to attached drawing 3.
6, material is soldered in hot-forging die liner with high-frequency induction brazing technology.Structural scheme of mechanism is referring to attached drawing 5.
The preparation method of self-lubricating hot forged mould proposed by the present invention based on Sialon ceramics, passes through the side of powder metallurgy
Method prepares the solid self lubricant material with high intensity, and powder metallurgic method is simple for process, low manufacture cost, can make full use of each material
The performance of material solves the problems, such as that each material wetability is inadequate, produces high-precision part, save material.
It these are only the preferred embodiment of the present invention, be not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure transformation made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (10)
1. a kind of self-lubricating hot forged mould based on Sialon ceramics, which is characterized in that including outer mold and be embedded in outer mold
In interior mold, wherein the interior mold includes nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase, wherein
Nickel chromium triangle matrix is mutually NiCr alloy powders, and ceramic hard is mutually Sialon ceramic powders, and lubrication is mutually CaF2Powder utilizes
Nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase three-phase powder are uniformly mixed by ball mill, then the side for passing through powder metallurgy
Interior mold is prepared in method.
2. the self-lubricating hot forged mould as described in claim 1 based on Sialon ceramics, which is characterized in that interior mold further includes
Stearic acid particles are made interior together with nickel chromium triangle matrix phase, ceramic hard phase and self-lubricating phase by the method for powder metallurgy
Mold.
3. the self-lubricating hot forged mould as claimed in claim 2 based on Sialon ceramics, which is characterized in that NiCr alloy powders
Mass fraction be 70%-90%, the mass fractions of Sialon ceramic powders is 2%-15%, CaF2Mass fraction be powder 2%-
15%, the mass fraction of stearic acid particles is 1%-2%.
4. the self-lubricating hot forged mould as described in claim 1 based on Sialon ceramics, which is characterized in that nickel chromium triangle matrix is mutually
Ni80Cr20。
5. a kind of system based on the self-lubricating hot forged mould based on Sialon ceramics described in any one of Claims 1-4
Preparation Method, which is characterized in that include the following steps：
Weigh appropriate NiCr metal powders, Sialon ceramic powders, CaF2After powder and stearic acid particles, by the powder after weighing
End is put into metal can, and stainless steel ball is added, and vacuum nitrogen filling gas shielded carries out ball milling by ball mill and mixes powder；
The powder mixed is positioned over sinter molding in electron tubes type sintering furnace by mold compression moulding；
After the sample sintered is by polishing, it is prepared into inserts, is applied in hot forged mould.
6. preparation method as claimed in claim 5, which is characterized in that ball mill ball milling mixes powder 4-6 hours.
7. preparation method as claimed in claim 5, which is characterized in that mixed powder is taken out, with mold and hydraulic device pressure
When type is made, pressure is controlled in 20 MPa ~ 30MPa, 1 min -2min of dwell time.
8. preparation method as claimed in claim 5, which is characterized in that the good style of compression moulding to be placed in vacuum tube furnace
When heating, it is heated to 400 DEG C within the 1h times, 0.5h is kept the temperature at 400 DEG C, 1200 DEG C are warming up to using 2h, in 1200 DEG C of rings
2h is kept the temperature under border；800 DEG C are cooled to through 1h, 30min is kept the temperature, is cooled to 400 DEG C by 1h, cools to room temperature with the furnace.
9. preparation method as claimed in claim 5, which is characterized in that the pressure of vacuum tube furnace is controlled 1 × 10-3Pa~9.9
×10-2Pa。
10. preparation method as claimed in claim 5, which is characterized in that the style of sinter molding silicon carbide paper sanding and polishing,
To remove the oxide skin on its surface；After the sample sintered is by polishing, metallographic microstructure is observed, is visited by hardness, electronics
It is prepared into inserts again after needle and high temperature friction and wear test.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810301741.1A CN108526366B (en) | 2018-04-04 | 2018-04-04 | Self-lubricating hot forging die based on Sialon ceramic and preparation method thereof |
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|---|---|---|---|
| CN201810301741.1A CN108526366B (en) | 2018-04-04 | 2018-04-04 | Self-lubricating hot forging die based on Sialon ceramic and preparation method thereof |
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| CN108526366B CN108526366B (en) | 2020-06-19 |
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| WO2017073712A1 (en) * | 2015-10-30 | 2017-05-04 | 住友電気工業株式会社 | Sintered compact and method for producing same |
| CN106925708A (en) * | 2017-04-18 | 2017-07-07 | 武汉理工大学 | Self-lubricating dissimilar materials composite construction hot-forging die and preparation method thereof |
| CN107584125A (en) * | 2017-08-31 | 2018-01-16 | 中国科学院兰州化学物理研究所 | The preparation method of grand based composites is matched in a kind of high-ductility self-lubricating |
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|---|---|---|---|---|
| CN1727420A (en) * | 2005-07-11 | 2006-02-01 | 西安交通大学 | Method for preparing self-lubricating coat in use for high temperature |
| CN103540780A (en) * | 2012-07-12 | 2014-01-29 | 中国科学院兰州化学物理研究所 | Preparation method for high-intensity nickel-based high-temperature self-lubricating composite material |
| CN102899550A (en) * | 2012-09-24 | 2013-01-30 | 江苏利达不锈钢有限公司 | High temperature resistant self-lubricating bearing material and preparation method thereof |
| CN104278226A (en) * | 2013-07-02 | 2015-01-14 | 中国科学院兰州化学物理研究所 | Preparation technology for wide-temperature-range self-lubricating coating |
| WO2017073712A1 (en) * | 2015-10-30 | 2017-05-04 | 住友電気工業株式会社 | Sintered compact and method for producing same |
| CN106925708A (en) * | 2017-04-18 | 2017-07-07 | 武汉理工大学 | Self-lubricating dissimilar materials composite construction hot-forging die and preparation method thereof |
| CN107584125A (en) * | 2017-08-31 | 2018-01-16 | 中国科学院兰州化学物理研究所 | The preparation method of grand based composites is matched in a kind of high-ductility self-lubricating |
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| CN108526366B (en) | 2020-06-19 |
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