CN107385255B - The preparation method of solid solution based ceramic metal blade material and obtained blade material - Google Patents

The preparation method of solid solution based ceramic metal blade material and obtained blade material Download PDF

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CN107385255B
CN107385255B CN201710569764.6A CN201710569764A CN107385255B CN 107385255 B CN107385255 B CN 107385255B CN 201710569764 A CN201710569764 A CN 201710569764A CN 107385255 B CN107385255 B CN 107385255B
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powder
grinding
sintering
dosage
tac
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CN107385255A (en
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杨天恩
熊计
倪磊
肖雅
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Sichuan University
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Sichuan University
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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
    • 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
    • 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
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • 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
    • B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
    • 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
    • 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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention discloses a kind of preparation method of solid solution based ceramic metal blade material and obtained blade materials, wherein, the method is first to (Ti, W) C powder carries out pre-grinding, then and after Co powder, NbC powder and TaC powder mixed grinding, filtering and drying, green compact are pressed into, vacuum-sintering and low pressure sintering is finally carried out, obtains blade material.In the present invention, pre-grinding is carried out to (Ti, W) C powder, refines crystal grain, size distribution tends to uniformly, in this way, being conducive to improve the intensity of material；Using the TaC powder of the part or all of fictitious hosts valuableness of NbC powder, the cost of material is significantly reduced, meanwhile, the hardness and toughness of material do not reduce not only, get a promotion instead, to reduce the abrasion of blade.

Description

The preparation method of solid solution based ceramic metal blade material and obtained blade material
Technical field
The invention belongs to ceramic tip Material Field more particularly to solid solution based ceramic metal blade materials, specifically Ground, the blade material for being related to the preparation method of solid solution based ceramic metal blade material and obtaining.
Background technique
Traditional WC-TiC-Co series hard alloy (YT series hard alloy), since the addition of TiC is thus with higher hard Degree and abrasion resistance properties in machining such as turning, milling, are used as cutter material in drilling.But WC-TiC-Co Hard alloy includes WC and the widely different hard phase of two kinds of physical properties of TiC, wherein the thermal expansion coefficient of WC and TiC, elasticity Modulus, microhardness, density are respectively 3.84 × 10-5With 7.74 × 10-5℃-1, 713 and 316GPa, 1780 and 3200MPa, 15.7 and 4.93g/cm3, cause tissue median surface stress to increase, be easy to cause the formation and extension of micro-crack in cutting process, The case where break resistance is weaker, shows biggish brittleness, is easy to appear tipping in interrupted cuts such as millings or fractures.
Increase with modern manufacturing industry to metal cutting efficiency requirements, high-speed cutting processing is at inexorable trend, and in height In fast machining, the service temperature of cutter can reach 600~1000 DEG C.Cutter material is needed under such high-temperature machining environment It includes high temperature hardness, high-temperature oxidation resistance etc. that material, which has superior high-temperature behavior,.Wherein, TaC is a kind of effective, raising gold Belong to the refractory carbides additive of ceramic high temperature performance.Adding TaC in cermet and can playing inhibits crystal grain to grow up, improve The effects of elevated temperature strength, hardness, inoxidizability.But prices are rather stiff by TaC, the cost of material is caused to obviously increase.
Therefore, it is necessary to seek a kind of additive replacement or part that cost is relatively low but does not influence metal ceramic material as high temperature performance Instead of TaC, to reduce cost.
Summary of the invention
To solve the above-mentioned problems, present inventor has performed sharp studies, carry out pre-grinding to (Ti, W) C powder first, so TaC powder is substituted using part or all of NbC powder afterwards, in this way, not only reducing cost, and ensure that the performance of material, thus Complete the present invention.
One aspect of the present invention provides a kind of preparation method of solid solution based ceramic metal blade material, be embodied in Under several aspects:
(1) a kind of preparation method of solid solution based ceramic metal blade material, wherein the described method comprises the following steps:
Step 1 carries out pre-grinding to (Ti, W) C powder；
Co powder, NbC powder and TaC powder are added in (Ti, W) C powder of step 1 pre-grinding by step 2, are then successively carried out After grinding, filtering and drying, it is pressed into green compact；
Step 3 passes sequentially through forming agent abjection, the sintering of solid phase stage and liquid phase stage sintering to the green compact that step 2 obtains Carry out vacuum-sintering；
Step 4 carries out low pressure sintering in low-pressure sintering furnace, obtains the solid solution based ceramic metal blade material.
(2) method according to above-mentioned (1), which is characterized in that in step 1,
Diameter is used to carry out pre-grinding for the sintered carbide ball of 4~8mm, it is preferred to use diameter is that the WC-8%Co of 6mm is hard Matter alloying pellet carries out pre-grinding；And/or
Use dehydrated alcohol for abrasive media, preferably its dosage is 200~500mL, more preferably 300~400mL；With/ Or
Ball material weight ratio is (5~15): 1, preferably (8~12): 1；And/or
Grinding rate is 50~90r/min, preferably 60~70r/min；And/or
The pre-grinding carries out 1~108h, preferably 5~72h of progress, more preferably 36~72h of progress, such as 48h.
(3) method according to above-mentioned (1) or (2), which is characterized in that in step 2,
The partial size of Co powder is 0.5~2 μm, preferably 0.8~1.5 μm, more preferably 1.0~1.2 μm；And/or
Based on the green compact of 100 parts by weight, the dosage of Co powder is 10~20%, preferably 14~16%, more preferably 15%.
(4) method according to one of above-mentioned (1) to (3), which is characterized in that in step 2,
The partial size of NbC powder and TaC powder is 0.8~2 μm, preferably 1.0~1.8 μm, more preferably 1.0~1.5 μm； And/or
Based on the green compact of 100 parts by weight, total dosage of NbC powder and TaC powder is 5~12%, preferably 7~9%, more preferably It is 8%.
(5) method according to one of above-mentioned (1) to (4), which is characterized in that in step 2,
Based on the green compact of 100 parts by weight, the dosage of NbC powder is that the dosage of 2~10%, TaC powder is 0~6%；Preferably, The dosage of NbC powder is that the dosage of 4~8%, TaC powder is 0~4%；It is highly preferred that the dosage of NbC powder is 6~8%, TaC powder Dosage is 0~2%；And/or
The amount ratio of NbC powder and TaC powder is (0.5~10): (0~1), preferably (1~7): (0~1), more preferably (3 ~5): (0~1).
(6) method according to one of above-mentioned (1) to (5), which is characterized in that in the grinding of step 2, SD rubber is added Gum forming agent, it is preferable that its dosage is 2~10%, it is highly preferred that its dosage is 3~7%, such as 5% and 6%.
(7) method according to one of above-mentioned (1) to (6), which is characterized in that in step 3,
The forming agent abjection is following to be carried out: being kept the temperature 0.2~3h under 300~800 DEG C, 5~20Pa, is deviate from forming agent； Preferably, 0.5~2h is kept the temperature under 400~700 DEG C, 10~15Pa, deviates from forming agent；It is highly preferred that in 500~600 DEG C, 10 1~2h is kept the temperature under~15Pa, deviates from forming agent；And/or
0.5~2h is kept the temperature under 1000~1500 DEG C, 3~15Pa carries out the sintering of solid phase stage；Preferably, in 1200~ 1300 DEG C, 1~1.5h of heat preservation carries out the sintering of solid phase stage under 5~10Pa；And/or
0.5~4h is kept the temperature under 1200~1600 DEG C, 0.5~8Pa carries out liquid phase stage sintering；Preferably, in 1300~ 1500 DEG C, 1~3h of heat preservation carries out liquid phase stage sintering under 1~5Pa；It is highly preferred that being kept the temperature under 1350~1450 DEG C, 1~5Pa 1h carries out liquid phase stage sintering.
(8) method according to one of above-mentioned (1) to (7), which is characterized in that in step 4, in protective gas pressure 5~10MPa of power, keep the temperature at 1000~1800 DEG C and carry out low pressure sintering under 30~120min, it is preferable that in argon pressure 5~ 10MPa, keep the temperature at 1200~1600 DEG C and carry out low pressure sintering under 30~100min, it is highly preferred that in 5~10MPa of argon pressure, It is kept the temperature at 1300~1500 DEG C under 40~80min and carries out low pressure sintering.
Another aspect of the present invention provides a kind of solid solution based ceramic metal blade material, is embodied in following side Face:
(9) a kind of solid solution based ceramic metal blade material preferably uses above-mentioned (1) to (8) the method to prepare, It being characterized in that, the material is made of a kind of composition, and the composition includes Co powder, WC powder and NbC powder, and optional TaC powder.
(10) material according to above-mentioned (9), which is characterized in that in the material
The total content of NbC powder and TaC powder is 5~12%, preferably 7~9%, more preferably 8%；And/or
The dosage of NbC powder is that the dosage of 2~10%, TaC powder is 0~6%；Preferably, the dosage of NbC powder is 4~8%, The dosage of TaC powder is 0~4%；It is highly preferred that the dosage that the dosage of NbC powder is 6~8%, TaC powder is 0~2%；And/or
The amount ratio of NbC powder and TaC powder is (0.5~10): (0~1), preferably (1~7): (0~1), more preferably (3 ~5): (0~1).
Detailed description of the invention
Fig. 1 shows the microstructure figure for the material that embodiment 1 and embodiment 3~5 obtain；
Fig. 2 shows the SEM figures that experimental example 1 carries out (Ti, W) C solid-solution powder that the pre- ball milling of different time obtains；
Fig. 3 shows the XRD diagram that experimental example 2 carries out (Ti, W) C solid-solution powder that the pre- ball milling of different time obtains.
Specific embodiment
Present invention will now be described in detail, and the features and advantages of the invention will become more with these explanations It is clear, clear.
One aspect of the present invention discloses a kind of preparation method of solid solution based ceramic metal blade material, wherein the side Method the following steps are included:
Step 1 carries out pre-grinding to (Ti, W) C powder.
Wherein, general (Ti, W) C powder can have remnants C, cause crystal grain bigger than normal, size distribution is wider.Therefore, in this hair In bright, pre-grinding is carried out to (Ti, W) C powder, keeps (Ti, W) C powder particles broken, refines crystal grain, size distribution tends to uniformly, this Sample is conducive to the intensity for improving material.
A kind of preferred embodiment according to the present invention, in step 1, in (Ti, W) the C powder, TiC: WC weight ratio It is 30: 70.
Wherein, described (Ti, W) the C powder is (Ti0.42,W0.58) TiC:WC weight ratio is 30:70 in C, close to saturation (Ti, W) C powder.According to TiC-WC puppet binary phase diagraml, at a temperature of sintering cemented carbide, maxima solubility of the WC in TiC is 72 ~75%, commercially available (W, Ti) C solid solution has different saturation degrees (WC solid solubility), there is not satisfying for TiC:WC=50:50 and 40:60 And solid solution, there are nearly saturated solid solution and supersaturated solid solution of 17:83 of 30:70 etc..Using doing for unsaturated solid solution Raw material prepares hard alloy, the ring structure of solid solution phase easy to form (internal layer WC content is lower, and outer layer WC content is higher)； Raw material is done using oversaturated solid solution and prepares hard alloy, is easy that the coarse WC of strip is precipitated during the sintering process, causes The performance of alloy declines.For these reasons, the research of this paper uses the solid solution for the TiC:WC=30:70 being closely saturated.
In the present invention, it can be reduced using (Ti, W) C replacement WC and TiC mixing hard phase as the method for main hard phase Residual stress caused by as two kinds of phase physical property differences of WC and TiC, and then improve the fracture toughness of alloy and impact tough Property, therefore can reduce the formation and extension of crackle in cutter material during interrupted cut, it reduces the tipping of cutter or fractures.
In the prior art, it relates to carbon black directly react metal oxide, it is multiple by carbonizing reduction reaction preparation Formula carbide of solid solution, still, in this way, needing after raw material in proportion ingredient by dry grinding, pressing boat, in 1800-2300 DEG C of carbon Change, is then crushed, is sieved, under these conditions, first, to improve powder purity, impurity content is reduced, is needed at high temperature for a long time Heat preservation, to realize the formation of complete carbonization and single phase solid solution, therefore the compound solid solution powder granularity prepared is thicker；Due to The crystallite dimension of powder is larger, if being mixed with metal simultaneously compared with thin, the lesser other ingredients of crystallite dimension raw material with particle Ceramics, it is likely that cause local hard phase abnormal grain growth or the phenomenon that nonuniform organization occur；Second, if carbonization is endless Entirely, then it is not readily available single-phase compound solid solution, and remaining carbon black will lead to the carbon content in the cermet preparation in later period It is higher, and carbon content is higher, and liquid phase sintering conditions can be made to reduce, to be easy that crystal grain is promoted to grow up, causes hardness not high.
A kind of preferred embodiment according to the present invention, in step 1, use diameter for the sintered carbide ball of 4~8mm into Row pre-grinding.
In further preferred embodiment, in step 1, use diameter for the WC-8%Co sintered carbide ball of 6mm Carry out pre-grinding.
Wherein, the main purpose ground when prepared by cermet mixture is to transfer energy to powder by grinding Grain, grinding efficiency height have a direct relation with mill ball size, and grinding bulb diameter is small, the gap between ball and ball with regard to smaller, Contact to powder and grinding frequency are relatively high, so the small big sphere of sphere diameter group of diameter has higher grinding efficiency. Generally, the ball of fine grain or sub- fine grain mixture ball milling 6mm, such grinding efficiency is high, if using the grinding for being lower than 4mm Ball then bad discharging.In addition, selection WC-8%Co sintered carbide ball, is because of the higher hard alloy of Co content, hardness is lower, Wearability is deteriorated, and when ball milling, the loss of abrading-ball is big, and the part being worn be equivalent to impurity and influence powder raw material at Point；The lower hard alloy of Co content, hardness is higher, but brittleness is also bigger, and in ball milling, abrading-ball falls above ball grinder When impacting powder raw material, it is possible to brittle failure occur, to also increase the loss of abrading-ball and influence the ingredient of powder raw material.
A kind of preferred embodiment according to the present invention uses dehydrated alcohol for abrasive media in step 1.
In further preferred embodiment, in step 1, the dosage of dehydrated alcohol is 200~500mL.
In embodiment still more preferably, in step 1, the dosage of dehydrated alcohol is 300~400mL.
Wherein, dehydrated alcohol is used to carry out wet ball grinding for abrasive media, the dosage of dehydrated alcohol should not be very little, Tai Shaohui Cause to grind insufficient, also it is difficult should not to will lead to the recycling of later period liquid phase too much too much.
A kind of preferred embodiment according to the present invention, in step 1, in carrying out pre-grinding, ball material weight ratio is (5 ~15): 1, grinding rate is 50~90r/min.
In further preferred embodiment, in step 1, carry out pre-grinding in, ball material weight ratio be (8~ 12): 1, grinding rate is 60~70r/min.
A kind of preferred embodiment according to the present invention, in step 1, the pre-grinding carry out 1~108h.
In further preferred embodiment, the pre-grinding carries out 5~72h.
In embodiment still more preferably, the pre-grinding carries out 36~72h, such as 48h.
Wherein, if beforehand research time consuming is less than 1h, (Ti, W) C powder particles degree of crushing is inadequate；If beforehand research time consuming is greater than 108h, then the granularity variation of powder is obvious when being not so good as initial, this is because the granularity of powder is already below the gap between abrading-ball, The effect of ball milling refinement reduces.
Co powder, NbC powder and TaC powder are added in (Ti, W) C powder of step 1 pre-grinding by step 2, are then successively carried out After grinding, filtering and drying, it is pressed into green compact.
A kind of preferred embodiment according to the present invention, in step 2, the partial size of Co powder are 0.5~2 μm.
In further preferred embodiment, in step 2, the partial size of Co powder is 0.8~1.5 μm.
In embodiment still more preferably, in step 2, the partial size of Co powder is 1.0~1.2 μm.
It wherein, in the present invention, is bonding phase with Co powder.
A kind of preferred embodiment according to the present invention, in step 2, based on the green compact of 100 parts by weight, the dosage of Co powder It is 10~20%.
In further preferred embodiment, in step 2, based on the green compact of 100 parts by weight, the dosage of Co powder is 14 ~16%.
In embodiment still more preferably, in step 2, based on the green compact of 100 parts by weight, the dosage of Co powder is 15%.
Wherein, in the present invention it is possible to realize the preparation that blade material is carried out using the Co of high-content, wherein Co content Higher, toughness of material improves, but hardness reduces, and therefore, in the prior art, the content of Co is less, is usually no more than 10%, because excessively will affect hardness.But in invention, crystal grain can be refined using NbC powder and/or TaC powder, improve material Therefore the hardness of material in the present invention, realizes the addition of high-content Co, the toughness for not only increasing material does not influence material also The hardness of material；On the other hand, the NbC powder that the present invention uses is better than TaC powder to the wetability of Binder Phase Co, therefore, to sum up, In material of the present invention, the addition of high-content is may be implemented in Co.
A kind of preferred embodiment according to the present invention, in step 2, the partial size of NbC powder and TaC powder are 0.8~2 μ m。
In further preferred embodiment, the partial size of NbC powder and TaC powder is 1.0~1.8 μm.
In embodiment still more preferably, in step 2, the partial size of NbC powder and TaC powder is 1.0~1.5 μ m。
Wherein, TaC powder is added in cermet and can be played inhibits crystal grain to grow up, improve elevated temperature strength, hardness, antioxygen The effects of property changed, meanwhile, NbC powder equally has the function of refining crystal grain, and therefore, the partial size of the two cannot be too big, but also not It is preferably too small, it is too small easy to reunite.
A kind of preferred embodiment according to the present invention, in step 2, based on the green compact of 100 parts by weight, NbC powder and TaC Total dosage of powder is 5~12%.
In further preferred embodiment, in step 2, based on the green compact of 100 parts by weight, NbC powder and TaC powder Total dosage is 7~9%.
In embodiment still more preferably, in step 2, based on the green compact of 100 parts by weight, NbC powder and TaC powder Total dosage be 8%.
Wherein, TaC is a kind of refractory carbides additive that is effective, improving metal ceramic material as high temperature performance, still, TaC Prices are rather stiff, and the cost of material is caused to obviously increase, and therefore, in the present invention, is replaced using cheap NbC powder Part or all of TaC powder.
Specifically: (1) currently, the commercially available price of NbC powder is only the 1/4~1/5 of TaC powder, therefore, replacing part with NbC powder Or cost can be significantly reduced in whole TaC powder；(2) NbC powder is better than TaC powder to the wetability of Binder Phase Co in cermet, The increase of wetability can reduce the hole in material and improve the intensity of material；(3) the room temperature hardness of NbC powder and TaC powder point Not Wei 2400HV and 1800HV, NbC powder is higher than TaC powder, moreover, the hardness of NbC powder is slower with the raising decline of temperature, and And there is the high temperature hardness for being apparently higher than TaC powder, this is highly advantageous to high-speed cutting；(4) NbC powder and TaC powder and steel is viscous Junction temperature is respectively 1250 DEG C and 1200 DEG C, so NbC powder ratio TaC powder has more excellent when ceramic tool cuts steel Good anti stick wear resistance.
A kind of preferred embodiment according to the present invention, in step 2, based on the green compact of 100 parts by weight, the use of NbC powder Amount is that the dosage of 2~10%, TaC powder is 0~6%.
In further preferred embodiment, in step 2, based on the green compact of 100 parts by weight, the dosage of NbC powder is 4 The dosage of~8%, TaC powder is 0~4%.
In embodiment still more preferably, in step 2, based on the green compact of 100 parts by weight, the dosage of NbC powder Dosage for 6~8%, TaC powder is 0~2%.
Wherein, in the present invention, part or all of TaC powder is substituted using cheap NbC powder, in this way, not only reducing Cost, moreover, inventor has found by many experiments, the performance of material will not only decline, can be risen instead, especially When NbC powder replacement TaC powder is more, specifically, when NbC powder dosage is more than (or substitution completely) TaC powder, the hardness of material It is promoted with fracture toughness, this is in the unexpected of inventor, but experimental result provides such conclusion really.Cause This using NbC powder part substitution or complete substitution TaC powder, not only greatly reduces cost, but also significantly in the present invention Improve the mechanical performance of material.
A kind of preferred embodiment according to the present invention, in step 2, the amount ratio of NbC powder and TaC powder be (0.5~ 10): (0~1).
In further preferred embodiment, in step 2, the amount ratio of NbC powder and TaC powder is (1~7): (0~ 1)。
In embodiment still more preferably, in step 2, the amount ratio of NbC powder and TaC powder is (3~5): (0 ~1).
Wherein, it in invention, when the dosage of NbC powder is more compared with TaC powder, can not only significantly reduce costs, but also can be with Effectively improve the hardness and toughness of material.
In the present invention, TaC powder is replaced without being using the reason of substances such as similar ZrC powder only with NbC powder: In vacuum, Co is 35 ° to the angle of wetting of ZrC powder in cermet, and wetability is bad, results in hole in material and increases, fine and close The decline of degree, so that the bending strength of material and hardness decline.
A kind of preferred embodiment according to the present invention, in step 2, use diameter for the sintered carbide ball of 4~8mm into Row grinding.
In further preferred embodiment, in step 2, use diameter for the WC-8%Co sintered carbide ball of 6mm It is ground.
A kind of preferred embodiment according to the present invention uses dehydrated alcohol for abrasive media in step 2.
In further preferred embodiment, the dosage of dehydrated alcohol is 200~500mL.
In embodiment still more preferably, the dosage of dehydrated alcohol is 300~400mL.
Wherein, dehydrated alcohol is used to carry out wet ball grinding for abrasive media, the dosage of dehydrated alcohol should not be very little, Tai Shaohui Raw material is caused not to be completely covered by dehydrated alcohol, so that raw material is easy to oxidize in process of lapping, it is also unsuitable too many, it can lead too much Cause grinding efficiency decline.
A kind of preferred embodiment according to the present invention, in step 2, ball material weight ratio are (5~15): 1, grinding rate For 50~90r/min, milling time is 24~60h.
In further preferred embodiment, ball material weight ratio is (8~12): 1, grinding rate is 60~70r/min, Milling time is 24~40h, such as 36h.
The agent of SD rubber-moulding is added in the grinding of step 2 in a kind of preferred embodiment according to the present invention.
In further preferred embodiment, the dosage of the SD rubber-moulding agent is 2~10%.
In embodiment still more preferably, the dosage of the SD rubber-moulding agent is 3~7%, such as 5% He 6%.
Wherein, since the material is mainly made of refractory metal tungsten carbide and Binder Phase cobalt, powder is in pressing process In, it can not form under pressure, therefore, in compacting need that forming agent is added.And the performance of forming agent is to directly affect One key factor of blank and sintered products performance.In the present invention, using SD forming agent, wherein SD forming agent is a kind of Transparent egg white color or yellow solution, nontoxic, have no irritating odor, good dispersion can be evenly dispersed in grinding In mixed material, viscosity is good, and product can show good mouldability after doping.
A kind of preferred embodiment according to the present invention crosses 300~500 meshes in step 2.
In further preferred embodiment, in step 2,400 meshes are crossed.
A kind of preferred embodiment according to the present invention, in step 2, the drying are vacuum drying.
In further preferred embodiment, in step 2, the drying carries out at 1~6Pa, 80~120 DEG C.
In embodiment still more preferably, in step 2, the drying at 2~5Pa, 90~100 DEG C into Row.
A kind of preferred embodiment according to the present invention suppresses green compact under 300~600MPa in step 2.
In further preferred embodiment, in step 2, green compact are suppressed under 400~500MPa.
Step 3 passes sequentially through forming agent abjection, the sintering of solid phase stage and liquid phase stage sintering to the green compact that step 2 obtains Carry out vacuum-sintering.
Wherein, sintering can remove the hole in workpiece, so that it is become completely (or substantially) closely knit, make porous powder Green compact becomes the product with certain tissue and performance.
A kind of preferred embodiment according to the present invention, forming agent abjection is following to be carried out: in 300~800 DEG C, 5~ 0.2~3h is kept the temperature under 20Pa, deviates from forming agent.
In further preferred embodiment, in step 3, the forming agent abjection is following to be carried out: in 400~700 DEG C, 0.5~2h is kept the temperature under 10~15Pa, deviate from forming agent.
In embodiment still more preferably, in step 3, forming agent abjection is following to be carried out: in 500~ 600 DEG C, 1~2h is kept the temperature under 10~15Pa, deviate from forming agent.
Wherein, initial stage of sintering is increased with temperature, and SD- forming agent is gradually decomposed and vaporized, and excludes sintered body, meanwhile, Contact stress between powder particle gradually eliminates, and binder Co powder, which starts to generate, to be restored and recrystallize, and diffusion into the surface starts to send out Raw, briquetting intensity increases.
A kind of preferred embodiment according to the present invention is kept the temperature under 1000~1500 DEG C, 3~15Pa in step 3 0.5~2h carries out the sintering of solid phase stage.
In further preferred embodiment, in step 3, under 1200~1300 DEG C, 5~10Pa keep the temperature 1~ 1.5h carries out the sintering of solid phase stage.
Wherein, at this stage, there is apparent shrink in solid phase reaction and diffusion aggravation, Plastic Flow enhancing, sintered body.
A kind of preferred embodiment according to the present invention is kept the temperature under 1200~1600 DEG C, 0.5~8Pa in step 3 0.5~4h carries out liquid phase stage sintering.
In further preferred embodiment, in step 3, under 1300~1500 DEG C, 1~5Pa keep the temperature 1~3h into The sintering of row liquid phase stage.
In embodiment still more preferably, in step 3, under 1350~1450 DEG C, 1~5Pa keep the temperature 1h into The sintering of row liquid phase stage.
Wherein, at this stage, there is liquid phase in sintered body, and contraction is quickly completed, and then generates crystalline transition, forms alloy Elementary organization and structure.
Step 4 carries out low pressure sintering in low-pressure sintering furnace, obtains the solid solution based ceramic metal blade material.
A kind of preferred embodiment according to the present invention, in step 4, in 5~10MPa of protective gas pressure, 1000 It is kept the temperature at~1800 DEG C under 30~120min and carries out low pressure sintering.
In further preferred embodiment, in step 4, at 5~10MPa of argon pressure, 1200~1600 DEG C Low pressure sintering is carried out under 30~100min of heat preservation.
In embodiment still more preferably, in step 4, in 5~10MPa of argon pressure, 1300~1500 DEG C Low pressure sintering is carried out under 40~80min of lower heat preservation.
According to a further aspect of the invention, a kind of solid solution based ceramic metal blade material is provided, above-mentioned side is preferably used Method preparation, wherein the material is made of a kind of composition, and the composition includes Co powder, WC powder and NbC powder, and optional TaC powder.
A kind of preferred embodiment according to the present invention, in the material, the total content of NbC powder and TaC powder is 5~ 12%.
In further preferred embodiment, in the material, based on the green compact of 100 parts by weight, NbC powder and TaC The total content of powder is 7~9%.
In embodiment still more preferably, in the material, based on the green compact of 100 parts by weight, NbC powder and The total content of TaC powder is 8%.
Wherein, TaC is a kind of refractory carbides additive that is effective, improving metal ceramic material as high temperature performance, still, TaC Prices are rather stiff, and the cost of material is caused to obviously increase, and therefore, in the present invention, is replaced using cheap NbC powder Part or all of TaC powder.
A kind of preferred embodiment according to the present invention, in the material, the dosage of NbC powder are 2~10%, TaC powder Dosage be 0~6%.
In further preferred embodiment, in the material, the dosage of NbC powder is the dosage of 4~8%, TaC powder It is 0~4%.
In embodiment still more preferably, in the material, the dosage of NbC powder is the use of 6~8%, TaC powder Amount is 0~2%.
Wherein, in the present invention, part or all of TaC powder is substituted using cheap NbC powder, in this way, not only reducing Cost, moreover, inventor has found by many experiments, the performance of material will not only decline, can be risen instead, especially When NbC powder replacement TaC powder is more, specifically, when NbC powder dosage is more than (or substitution completely) TaC powder, the hardness of material It is promoted with fracture toughness, this is in the unexpected of inventor, but experimental result provides such conclusion really.Cause This using NbC powder part substitution or complete substitution TaC powder, not only greatly reduces cost, but also significantly in the present invention Improve the physical property of material.
A kind of preferred embodiment according to the present invention, in the material, the amount ratio of NbC powder and TaC powder are (0.5 ~10): (0~1).
In further preferred embodiment, in the material, the amount ratio of NbC powder and TaC powder is (1~7): (0 ~1).
In embodiment still more preferably, in the material, the amount ratio of NbC powder and TaC powder is (3~5): (0~1).
Wherein, it in invention, when the dosage of NbC powder is more compared with TaC powder, can not only significantly reduce costs, but also can be with Effectively improve the hardness and toughness of material.
Wherein, the content of each component is also consistent in the content of other each components and the above method in the material obtained.
Possessed by of the invention the utility model has the advantages that
(1) present invention carries out pre-grinding to (Ti, W) C powder, refines crystal grain, size distribution tends to uniformly, in this way, favorably In the intensity for improving material；
(2) present invention use the part or all of fictitious hosts valuableness of NbC powder TaC powder, on the one hand can, significantly reduce The cost of material；
(3) present invention uses the TaC powder of the part or all of fictitious hosts valuableness of NbC powder, on the other hand also found, material Hardness and toughness do not reduce not only, get a promotion instead, to reduce the abrasion of blade；
(4) present invention realizes the addition of high-content Co, improves the toughness of material.
Embodiment
The present invention is further described below by way of specific embodiment.But these embodiments are only exemplary, not Any restrictions are constituted to protection scope of the present invention.
Embodiment 1
Raw material is weighed by weight percentage prepares solid solution based ceramic metal, the Co that wherein granularity is 1.17 μm accounts for 15%, Granularity is that 1.45 μm of NbC accounts for 6%, and granularity is that 1.36 μm of TaC accounts for 2%, and it is 2.6 μm of (Ti, W) C that remaining, which is granularity, (Ti, W) C is (Ti0.42,W0.58) C, the weight ratio of TiC and WC therein are 30:70.
(1) (Ti, W) C powder is added to tumbling ball mill and carries out pre-grinding processing, mill ball is the WC- of Φ 6mm 8wt%Co sintered carbide ball, ball material weight ratio are 8:1, and abrasive media is dehydrated alcohol, additional amount 300mL, grinding rate For 60r/min, milling time 36h.
(2) Co powder, NbC powder, TaC powder will be added after solid solution raw material pre-grinding and remixes grinding 36h.Mix abrasive lapping Afterwards, cermet slurry is filtered through 400 mesh, and vacuum drying treatment temperature is 100 DEG C, vacuum degree 5Pa.SD rubber-moulding agent Additional amount is 6wt%.Mixture is pressed into green compact at 400MPa.
(3) green compact keep the temperature 2h at 600 DEG C in vacuum drying oven, and vacuum degree is to remove forming agent under 15Pa.It is in sintering temperature 1250 DEG C, 1.5h is kept the temperature, vacuum degree is that the sintering of solid phase stage is completed under 10Pa.It is 1420 DEG C in sintering temperature, soaking time is Liquid phase stage sintering is completed under 1h, vacuum degree 5Pa.
(4) cermet sintered is placed in low-pressure sintering furnace, low pressure sintering carries out at 1450 DEG C, soaking time For 75min, argon pressure 5MPa.
Prepared solid solution based ceramic metal consistency is 99.15%, Vickers hardness 1800MPa, and fracture toughness is 11.2MPa·m1/2, microstructure is as shown in figure 1 shown in a.
Embodiment 2
Raw material is weighed by weight percentage and prepares solid solution based ceramic metal, and the Co that wherein granularity is 1 μm accounts for 15%, granularity 7% is accounted for for 1.22 μm of NbC, granularity is that 1.08 μm of TaC accounts for 1%, remaining is that granularity is 4.5 μm of (Ti, W) C, (Ti, W) C For (Ti0.42,W0.58) C, the weight ratio of TiC and WC therein are 30:70.
(1) (Ti, W) C powder is added to tumbling ball mill and carries out pre-grinding processing, mill ball is the WC- of Φ 6mm 8wt%Co sintered carbide ball, ball material weight ratio are 12:1, and abrasive media is dehydrated alcohol, additional amount 400mL, grinding speed Degree is 70r/min, milling time 48h.
(2) Co powder, NbC powder, TaC powder will be added after solid solution raw material pre-grinding and remixes grinding 36h.After mixing abrasive lapping Cermet slurry is filtered through 400 mesh, and vacuum drying treatment temperature is 90 DEG C, vacuum degree 2Pa.The addition of SD rubber-moulding agent Amount is 5wt%.Mixture is pressed into green compact at 500MPa.
(3) green compact keep the temperature 1.2h at 550 DEG C in vacuum drying oven, and vacuum degree is to remove forming agent under 10Pa.In sintering temperature It is 1220 DEG C, soaking time 1h, vacuum degree is that the sintering of solid phase stage is completed under 5Pa.It is 1400 DEG C, when heat preservation in sintering temperature Between be 1h, vacuum degree be 1Pa under complete liquid phase stage sintering.
(4) cermet being just sintered is placed in low-pressure sintering furnace, low pressure sintering carries out at 1480 DEG C, soaking time For 45min, argon pressure 8MPa.
Prepared solid solution based ceramic metal consistency is 99.05%, Vickers hardness 1805MPa, and fracture toughness is 10.9MPa·m1/2。
Embodiment 3
The process of embodiment 1 is repeated, difference is that NbC powder accounts for 8%, and does not add TaC powder.
The Vickers hardness of prepared solid solution based ceramic metal is 1820MPa, fracture toughness 10.8MPam1/2, Microstructure is as shown in figure 1 shown in b.
Embodiment 4
The process of embodiment 1 is repeated, difference is that NbC powder accounts for 4%, TaC powder and accounts for 4%.
The Vickers hardness of prepared solid solution based ceramic metal is 1750MPa, fracture toughness 10.5MPam1/2, Microstructure is as shown in figure 1 shown in c.
Embodiment 5
The process of embodiment 1 is repeated, difference is that NbC powder accounts for 2%, TaC powder and accounts for 6%.
The Vickers hardness of prepared solid solution based ceramic metal is 1725MPa, fracture toughness 10.4MPam1/2, Microstructure is as shown in figure 1 shown in d.
Comparative example
Comparative example 1
The preparation process of embodiment 1 is repeated, difference is: TaC powder accounts for 8%, and does not add NbC powder.
The Vickers hardness of prepared solid solution based ceramic metal is 1760MPa.
Wherein, NbC powder is used compared with comparative example 1, in Examples 1 to 5 and partly or entirely replaces TaC powder, is obtained The hardness of material does not reduce too much, therefore, illustrates not lead to material in the case where reducing cost using NbC powder Hardness declines to a great extent.Also, in Examples 1 to 3, when the NbC powder dosage of use is more, the hardness of obtained material is instead It is higher than the hardness of comparative example, it further illustrates, when NbC powder dosage is more, not only significantly reduces cost, meanwhile, material Hardness be improved.
Comparative example 2
The preparation process of embodiment 1 is repeated, difference is: not adding NbC powder and TaC powder.
The Vickers hardness of prepared solid solution based ceramic metal is 1450MPa.
When not adding NbC powder and TaC powder, the hardness of material reduces obvious, illustrates, the presence of NbC powder and TaC powder can be with Crystal grain is refined, the hardness of material is improved.
Comparative example 3
The preparation process of embodiment 1 is repeated, difference is: the dosage of NbC powder is respectively 1%, 2%, 3% and 4%, and not Add TaC powder.
The Vickers hardness of prepared solid solution based ceramic metal be respectively 1530MPa, 1560MPa, 1611MPa, 1652MPa。
By it compared with embodiment 2~3,4 groups of hardness tested in comparative example 3 are lower, illustrate, in the material In material, the dosage of the NbC powder as refinement crystal grain cannot be very little.
Comparative example 4
The preparation process of embodiment 1 is repeated, difference is: the dosage of TaC powder is respectively 1%, 2%, 3% and 4%, and not Add NbC powder.
The Vickers hardness of prepared solid solution based ceramic metal be respectively 1510MPa, 1580MPa, 1596MPa, 1590MPa。
By it compared with embodiment 2~3,4 groups of hardness tested in comparative example 4 are lower, illustrate, in the material In material, the dosage of the TaC powder as refinement crystal grain cannot be very little.
Meanwhile in conjunction with comparative example 3~4 it is found that as refinement crystal grain TaC powder and/or NbC powder dosage it is most important, Its dosage cannot be very little, will lead to hardness reduction very little.
Comparative example 5
The preparation process of embodiment 1 is repeated, difference is: pre- ball milling not being carried out to (Ti, W) C.
The Vickers hardness of prepared solid solution based ceramic metal is 1615MPa.
Comparative example 5 and embodiment 1 are compared, when ball milling pre- without (Ti, W) C solid solution, the hardness of material drops It is low obvious, illustrate, the crystallite dimension of (Ti, W) C solid-solution powder can be refined by pre- ball milling, thus after significantly improving sintering The hardness of material.
Experimental example
Experimental example 1
To embodiment 1 use (Ti, W) C solid-solution powder carry out the pre- ball milling of 0h, 36h, 72h and 108h respectively, then into Row SEM test, as a result as shown in Figure 2, wherein a is pre- ball milling 0h, and b is pre- ball milling 36h, and c is pre- ball milling 72h, and d is pre- ball milling 108h。
Wherein:
Original (Ti, W) C solid-solution powder particle without obvious corner angle, shows squarish it can be seen from Fig. 2 (a) Or it is round, powder size distribution is wider, and wherein larger particles are close to 3~5 μm, and about 0.5 μm of little particle；
Pass through the ball milling of 36h it can be seen from Fig. 2 (b), (Ti, W) C solid-solution powder particle starts to be broken, granularity Distribution tends to uniformly, and the bulky grain in starting powder is broken, and about 1~2 μm of powder mean particle sizes；
72h is extended to Ball-milling Time it can be seen from Fig. 2 (c), (Ti, W) C solid-solution powder further refines, and obtains Ultra-fine grade (0.5 μm) solid-solution powder；
When Ball-milling Time continues to extend to 108h it can be seen from Fig. 2 (d), the granularity variation of powder has been not so good as initially Shi Mingxian, this is because the granularity of powder, already below the gap between abrading-ball, the effect of ball milling refinement reduces, therefore, pre- ball Grinding efficiency can be reduced instead by carrying out ball milling after being ground to a certain degree again.
Experimental example 2
To embodiment 1 use (Ti, W) C solid-solution powder carry out the pre- ball milling of 0h, 36h, 72h and 108h respectively, then into Row XRD test, as a result as shown in Figure 3.
Can be seen from figure 3,35.91 °, 41.71 °, 60.45 °, 72.37 ° and 76.14 ° angularly near diffraction maximum It is corresponding with the diffraction surfaces such as (111), (200), (220), (311) and (222) respectively.
According to the solid solution that JCPDF65-0242, (Ti, W) C powder are formed in TiC as WC, have identical with TiC Face-centered cubic crystal structure belongs to Fm-3m space group, and by the ball milling of different time, (Ti, W) C solid-solution powder is still kept Its cubic structure.
By Fig. 3 it can also be seen that with milling time extension, there is widthization phenomenon in diffraction maximum, especially (220), (311) particularly evident and at (222) diffraction surfaces.It wherein, may be broadening caused by crystallite dimension the reason of diffraction peaks broadening (crystalline size), grain size becomes smaller, and reciprocal ball is caused to become larger, and makes diffraction peak broadening.Therefore, Jade 5.0 is utilized It is calculated, obtaining crystallite dimension is respectively 99nm, 34.6nm, 31.5nm and 29.3nm (with milling time).
Illustrate, pre-grinding can be substantially reduced crystallite dimension, refine crystal grain, also, as milling time is normal, crystal grain by It is decrescence small, it still, grinds the later period, degree of grain refinement reduces, and therefore, general grinding is no more than 72h.
Experimental example 3
SEM test is carried out to the material that embodiment 1 and embodiment 3~5 obtain, obtained microstructure is respectively as schemed Shown in a~d in 1.
Experimental example 4
Model WNMG080408- is made using the blade material that embodiment 1 and embodiment 3~5 and comparative example 1 obtain Then the blade of ZM cuts the 9SiCr alloy tool steel pole (Φ=45mm) by quenching and tempering, In, machining condition: cutting speed Vc=63.62m/min, feed speed f=0.12mm/r, cutting depth ap=0.2mm, cutting Time t=5min；Cutting process: DRY CUTTING does not use cutting fluid.The results are shown in Table 1.
1 cutting experiment result of table
As can be seen from Table 1, comparative example 1 compared to the examples, its do not use NbC, and its wear of the tool flank most serious, Illustrate, the addition of NbC can reduce the degree of wear of knife face.It wherein, is 2wt% when NbC additive amount is 6wt%, TaC additive amount When (embodiment 1), cutting abrasion resistance properties are best.
It is described the invention in detail above in conjunction with detailed description and exemplary example, but these explanations are simultaneously It is not considered as limiting the invention.It will be appreciated by those skilled in the art that without departing from the spirit and scope of the invention, Can be with various equivalent substitutions, modifications or improvements are made to the technical scheme of the invention and its embodiments, these each fall within the present invention In the range of.Scope of protection of the present invention is subject to the appended claims.

Claims (9)

1. a kind of preparation method of solid solution based ceramic metal blade material, which is characterized in that the described method comprises the following steps:
Step 1 carries out pre-grinding to (Ti, W) C powder；
Co powder, NbC powder and TaC powder are added in (Ti, W) C powder of step 1 pre-grinding by step 2, then successively ground, After filtering and drying, it is pressed into green compact；
Step 3 passes sequentially through forming agent abjection, the sintering of solid phase stage and liquid phase stage sintering progress to the green compact that step 2 obtains Vacuum-sintering；
Step 4 carries out low pressure sintering in low-pressure sintering furnace, obtains the solid solution based ceramic metal blade material；
In step 1, diameter is used to carry out pre-grinding for the WC-8%Co sintered carbide ball of 6mm, the pre-grinding carries out 5~ 72h, in (Ti, W) the C powder, TiC: WC weight ratio is 30: 70；
In step 2, the partial size of Co powder is 0.5~2 μm, and the partial size of NbC powder and TaC powder is 0.8~2 μm, is based on 100 weight Part green compact, it be the dosage of 6%, TaC powder is 2% that the dosage of Co powder, which is the dosage of 10~20%, NbC powder,；
In step 3,0.2~3h is kept the temperature under 300~800 DEG C, 5~20Pa, deviates from forming agent；In 1000~1500 DEG C, 3~ 0.5~2h is kept the temperature under 15Pa and carries out the sintering of solid phase stage, and 0.5~4h is kept the temperature under 1200~1600 DEG C, 0.5~8Pa and carries out liquid The sintering of phase stage.
2. the method according to claim 1, wherein in step 1,
Use dehydrated alcohol for abrasive media, dosage is 200~500mL；
Ball material weight ratio is (5~15): 1；
Grinding rate is 50~90r/min；With
The pre-grinding carries out 36~72h.
3. the method according to claim 1, wherein in step 2,
The partial size of Co powder is 0.8~1.5 μm；With
Based on the green compact of 100 parts by weight, the dosage of Co powder is 14~16%.
4. according to the method described in claim 3, it is characterized in that, in step 2,
The partial size of Co powder is 1.0~1.2 μm；With
Based on the green compact of 100 parts by weight, the dosage of Co powder is 15%.
5. the method according to claim 1, wherein in step 2,
The partial size of NbC powder and TaC powder is 1.0~1.8 μm.
6. the agent of SD rubber-moulding is added the method according to claim 1, wherein in the grinding of step 2, Dosage is 2~10%.
7. method according to claim 1 to 6, which is characterized in that in step 3,
The forming agent abjection is following to be carried out: being kept the temperature 0.5~2h under 400~700 DEG C, 10~15Pa, is deviate from forming agent；With/ Or
1~1.5h is kept the temperature under 1200~1300 DEG C, 5~10Pa carries out the sintering of solid phase stage.
8. the method according to the description of claim 7 is characterized in that in step 3,
1~3h is kept the temperature under 1300~1500 DEG C, 1~5Pa carries out liquid phase stage sintering.
9. the method according to claim 1, wherein in step 4, in 5~10MPa of protective gas pressure, It is kept the temperature at 1000~1800 DEG C under 30~120min and carries out low pressure sintering.
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