CN102943194B - Diamond-Ti(C,N) base metal ceramic composite material and preparation method - Google Patents
Diamond-Ti(C,N) base metal ceramic composite material and preparation method Download PDFInfo
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- CN102943194B CN102943194B CN201210448271.4A CN201210448271A CN102943194B CN 102943194 B CN102943194 B CN 102943194B CN 201210448271 A CN201210448271 A CN 201210448271A CN 102943194 B CN102943194 B CN 102943194B
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Abstract
The invention discloses a diamond-Ti(C,N) base metal ceramic composite material which can guarantee the abrasive resistance while the hardness is improved, and a preparation method. The preparation method for the diamond-Ti(C,N) base metal ceramic composite material comprises the following steps of: 1) preparing powder mixture, wherein powder additive in the raw material of the powder mixture consists of particulate matters of which the average particle diameter is 20-70micrometers, each particle consists of a diamond particle core and a metal coating covered on the surface of the diamond particle core, and each metal coating is selected from at least one of Co and Ni; and 2) forming, i.e. processing the powder mixture into a compact by pressure forming; and 3) sintering, specially sintering the compact at the sintering pressure of 20-40Mpa by the discharge plasma technology, heating the compact to 1100-1250DEG C when sintering is carried out for 30-40 minutes, keeping warm for 2-10 minutes, and cooling to obtain the diamond-Ti(C,N) base metal ceramic composite material.
Description
Technical field
The present invention relates generally to a kind of ceramic-metal composite and preparation method thereof, is specifically related to diamond-Ti(C, N) based ceramic metal matrix material and preparation method thereof.
Background technology
Ti(C, N) based ceramic metal is that a class be take Ti(C, N) powder mix of powder or TiC and TiN is hard phase main raw material, the metals such as Co, Ni, Cu of take are bonding phase raw material, and conventionally also add WC, TaC, NbC, Mo
2c, VC, Cr
3c
2deng transition metal carbides, through the formed matrix material of batch mixing-mold pressing-sintering, mainly for the manufacture of cutting tool.Wherein, the range of choice of bonding phase metal is wider, as just proposed in the patent documentation of CN102046823A, can in iron family metal, choose arbitrarily.
In order to improve Ti(C, N) hardness of based ceramic metal and cutting ability, present inventor once directly added diamond and carried out mechanically mixing in raw material, had made a kind of contain adamantine Ti(C, N more afterwards by existing mode) based ceramic metal matrix material.In high speed cutting test, find, this material is not enough to adamantine hold, and in high-speed machining process, diamond easily comes off; In addition, although the hardness of this material is significantly improved, wear resistance, fracture toughness property and bending strength are unsatisfactory.
Contriver further studies discovery, cause the reason of the problems referred to above to mainly contain following several respects: first, the adamantine wetting property of Binder Phase metal pair is poor, cannot effectively stop the formation at diamond and transition metal carbides interface, causes material matrix lower to adamantine hold; The second, the easy thermal damage of diamond during high temperature sintering, thereby the wear resistance of reduction material; The 3rd, high temperature sintering causes adamantine surperficial greying, makes whole decline of wear resistance, fracture toughness property and bending strength of material.
Summary of the invention
The application aims to provide a kind of diamond that can guarantee wear resistance when improving hardness-Ti(C, N) based ceramic metal matrix material and preparation method thereof.
For the application's diamond-Ti(C, N) based ceramic metal matrix material, this material is to be prepared by following methods, the step that the method comprises is:
1) prepare powdered mixture
The component of raw material and proportioning (weight percent)
Ti(C, N) powder: 40%～60%
Iron family metal: 10%～15%
Powder additive: 10%～20%
Transition metal carbides: all the other
The particulate matter that described powder additive is 20 microns～70 microns by median size forms, and these particulate matter are to consist of bortz core and the metal plating that is coated on bortz wicking surface, and described metal plating is selected from least one in Co, Ni;
According to above-mentioned component and proportioning, by described Ti(C, N) powder, iron family metal, powder additive and transition metal carbides mix, and makes powdered mixture;
2) moulding
By pressure forming, above-mentioned powdered mixture is made to pressed compact;
3) sintering
Adopt plasma discharging technology to carry out sintering to above-mentioned pressed compact, during sintering, pressed compact is heated to 1100 ℃～1250 ℃ and be incubated 2 minutes～10 minutes in 30 minutes～40 minutes, sintering pressure is 20Mpa～40Mpa, after cooling, obtain described diamond-Ti(C, N) based ceramic metal matrix material.
At the application diamond-Ti(C, in sintering process when N) prepared by based ceramic metal matrix material, at least one metal plating forming in Co, Ni reacts with transition metal carbides, thereby can effectively stop the formation at bortz core and transition metal carbides interface, strengthened thus material matrix to the hold of bortz core and diamond thermostability, thereby strengthened the wear resistance of material in high-speed machining process when improving ceramic-metal composite hardness.In addition, adopt the application's discharge plasma sintering condition, effectively reduce sintering temperature and reduce sintering time, thereby reduce the graphite transition of bortz core in high-temperature sintering process, strengthen adamantine stability, improve hardness, obdurability and the wear resistance of ceramic-metal composite.It is the particulate matter of 20 microns～70 microns that powder additive adopts median size, can guarantee diamond-Ti(C, N) based ceramic metal matrix material shows excellent cutting and abrasion resistance properties in high-speed machining process.
The weight of described metal plating preferably accounts for 5%～10% of per unit powder additive weight, to realize completely coated to bortz core of metal plating, guarantees material matrix fully controlling bortz core.If the weight of metal plating accounts for the ratio of per unit powder additive weight and is less than 5%, be difficult to realize completely coated to bortz core of metal plating, material matrix can fairly obvious (but still not improving) to the raising of controlling performance of bortz core; If be greater than 10% but the weight of metal plating accounts for the ratio of per unit powder additive weight, metal plating is meeting puffing in electroless plating process, causes metal plating to the adamantine degradation of controlling.
Generally, described iron family metal is selected from one or more in Co, Ni, Fe.
Generally, described transition metal carbides is selected from WC, TaC, NbC, Mo
2one or more in C, VC.
For the application's diamond-Ti(C, N) preparation method of based ceramic metal matrix material, the step that this preparation method comprises is:
1) prepare powdered mixture
The component of raw material and proportioning (weight percent)
Ti(C, N) powder: 40%～60%
Iron family metal: 10%～15%
Powder additive: 10%～20%
Transition metal carbides: all the other
The particulate matter that described powder additive is 20 microns～70 microns by median size forms, and these particulate matter are to consist of bortz core and the metal plating that is coated on bortz wicking surface, and described metal plating is selected from least one in Co, Ni;
According to above-mentioned component and proportioning, by described Ti(C, N) powder, iron family metal, powder additive and transition metal carbides mix, and makes powdered mixture;
2) moulding
By pressure forming, above-mentioned powdered mixture is made to pressed compact;
3) sintering
Adopt plasma discharging technology to carry out sintering to above-mentioned pressed compact, during sintering, pressed compact is heated to 1100 ℃～1250 ℃ and be incubated 2 minutes～10 minutes in 30 minutes～40 minutes, sintering pressure is 20Mpa～40Mpa, after cooling, obtain described diamond-Ti(C, N) based ceramic metal matrix material.
Based on alleged cause, the weight of described metal plating preferably accounts for 5%～10% of per unit powder additive weight.
Generally, described iron family metal is selected from one or more in Co, Ni, Fe.
Generally, described transition metal carbides is selected from WC, TaC, NbC, Mo
2one or more in C, VC.
The application below will be provided for preparing diamond-Ti(C, N) powder additive of based ceramic metal matrix material, and the preparation method of this powder additive.
For this reason, the particulate matter that this powder additive is 20 microns～70 microns by median size forms, and these particulate matter are to consist of bortz core and the metal plating that is coated on bortz wicking surface, and described metal plating is selected from least one in Co, Ni.
Wherein, the weight of described metal plating preferably accounts for 5%～10% of per unit powder additive weight.
The preparation method of above-mentioned powder additive, it step comprising is: by diamond particles successively at SnCl
2solution and PdCl
2in solution, carry out respectively sensitization and activation treatment; Diamond particles after processing is dispersed in to CoSO
4and NiSO
4mixing solutions in, maybe the diamond particles after processing is dispersed in to CoSO
4solution or NiSO
4in solution, thereby obtain mixed slurry; In described mixed slurry, add sodium hypophosphite to carry out Co and/or Ni in the electroless plating on diamond particles surface, take and obtain by bortz core and be coated on the particulate matter that metal plating forms and median size is 20 microns～70 microns of bortz wicking surface.
Wherein, the introduction volume of Co and/or Ni preferably accounts for 5%～10% of per unit particulate matter weight by the weight of metal plating in the particulate matter preparing and calculates.
With general T i(C, N) based ceramic metal compares, the application's diamond-Ti(C, N) based ceramic metal matrix material has the following advantages:
1, the diamond that the particulate matter that employing consists of Co and/or Ni cladding diamond grain core is manufactured as powder additive-Ti(C, N) based ceramic metal matrix material, its hardness, fracture toughness property and wear resistance are all better than existing Ti(C, N) based ceramic metal.
2, in the application's ceramic-metal composite sintering process, metal plating reacts with transition metal carbides, effectively stoped the formation at diamond and transition metal carbides interface, strengthened material matrix to adamantine hold and prevented adamantine thermal damage, when improving material hardness, having strengthened the wear resistance of material in high-speed machining process.
3, adopt the application's discharge plasma sintering condition, can effectively reduce sintering temperature and greatly reduce sintering time, reduce the graphite transition of diamond particles in high-temperature sintering process, strengthen adamantine stability, improve hardness, obdurability and the wear resistance of ceramic-metal composite.
Accompanying drawing explanation
Fig. 1 is for forming the microtexture schematic diagram of the particulate matter of the application's powder additive.
Embodiment
< test example >
Manufacture diamond-Ti(C, N) based ceramic metal matrix material, then detects the hardness of these ceramic-metal composites, fracture toughness property and wear resisting property.Attention: in order to contrast diamond-Ti(C, N) performance of based ceramic metal matrix material and conventional Ti (C, N) based ceramic metal matrix material, part test example does not add diamond.
The basic step of test is:
1) preparation is by bortz core and be coated on the particulate matter that the metal plating of bortz wicking surface forms
By diamond particles successively at SnCl
2solution and PdCl
2in solution, carry out respectively sensitization and activation treatment; Diamond particles after processing is dispersed in to CoSO
4and NiSO
4mixing solutions in, thereby obtain mixed slurry; In described mixed slurry, add sodium hypophosphite to carry out Co and Ni in the electroless plating on diamond particles surface, take and obtain by bortz core 2 and be coated on the particulate matter (as shown in Figure 1) that metal plating 1 forms and median size is 20 microns～70 microns on bortz core 2 surfaces.
Wherein, the concrete operations of preparation particulate matter are as follows:
A. bortz core is placed in to the SnCl of 0.05mol/L
2in solution, soak 5 minutes, then 0.05mol/L is placed in PdCl
2in solution, soak 4 minutes, obtain the catalytic active center-Pd as chemical nickel plating, cobalt, Pd is adsorbed in diamond surface.
B. the bortz core by after above-mentioned processing is dispersed in to the CoSO of 0.2mol/L
4and NiSO
4mixing solutions in to obtain mixed slurry.
C. described mixed slurry is heated to 70 ℃～90 ℃, add 0.1mol/L sodium hypophosphite, react 10 minutes～30 minutes, carry out Co, Ni electroless plating process and make particulate matter at diamond surface, this particulate matter consists of the metal plating of bortz core and Co, Ni.
2) prepare powdered mixture
By component and the proportioning set, take raw material, in roller milling machine with ratio of grinding media to material (4～6): the speed of 1,20～40 revs/min, the ball milling carrying out 80 hours～100 hours mixes, and prepares powdered mixture.
3) moulding
In powdered mixture, add the forming agents such as paraffin, PEG, stir, after sieving, in mould, pressed compact is made in mold pressing, and molding pressure is 200MPa～400MPa.
4) sintering
Adopt plasma discharging technology to carry out sintering above-mentioned pressed compact, pressed compact is heated to 1100 ℃～1250 ℃ and be incubated 2 minutes～10 minutes during sintering about 35 minutes, sintering pressure is 20Mpa～40Mpa, obtains ceramic-metal composite after cooling.
[table 1]
By bortz core and be coated on the preparation condition of the particulate matter that the metal plating of bortz wicking surface forms
Table 1
Illustrate:
1, test number 1-7 respectively with below each table in test number 1-7 corresponding.
Wherein, the test of numbering 1-5 adopts the application's powder additive to prepare diamond-Ti(C, N) based ceramic metal matrix material, the test of numbering 6 does not adopt the application's powder additive but still takes the mode of directly adding diamond powder to prepare diamond-Ti(C, N) based ceramic metal matrix material, the test of numbering 7 had not both adopted the application's powder additive, do not take directly to add diamond powder yet, that number prepared by 7 test is traditional Ti(C, N) based ceramic metal matrix material.Therefore in each hurdle that, numbering 6-7 is corresponding, be "-", expression no this item.
[table 2]
Component and the proportioning (weight percent) of preparing the raw material of powdered mixture.
Table 2
Illustrate:
1,, for ease of comparing, in the test of numbering 1-7, transition metal carbides is all selected from WC.But those skilled in the art obviously can determine except WC, such as Mo
2c, TaC, NbC, VC, Cr
3c
2deng other transition metal carbides, all can be used as additive.
2,, for ease of comparing, in the test of numbering 1-7, bonding phase raw material is all selected from Co, Ni.But those skilled in the art obviously can determine except Co, Ni, such as iron family metals such as Fe, all can be used as bonding phase metal.
3, the test of numbering 6 does not adopt the application's powder additive but still takes the mode of directly adding diamond powder to prepare diamond-Ti(C, N) based ceramic metal matrix material, therefore, " powder additive " hurdle of numbering 6 correspondences is "-", represents no this item.
4, the test of numbering 7 had not both adopted the application's powder additive, do not take directly to add diamond powder yet, that number prepared by 7 test is traditional Ti(C, N) based ceramic metal matrix material, therefore, " powder additive " hurdle and " diamond powder " hurdle of numbering 7 correspondences are "-", represent no this item.
5, the test of numbering 1-5 all adopts the application's powder additive, and therefore, numbering " diamond powder " hurdle corresponding to 1-5 is "-", represents no this item.
[table 3]
Sintering condition
Table 3
[table 4]
Test-results
Table 4
Wherein, high speed cutting test conditions is:
Linear velocity: 500m/min
The depth of cut: 0.2mm/min
Bite: 1mm/min
Conclusion (of pressure testing):
1, adopt powder additive that the particulate matter of Co, Ni cladding diamond grain core forms as wild phase raw material, can improve Ti(C, N) hardness, fracture toughness property and the wear resistance of based ceramic metal.
2, adopt the application's discharge plasma sintering condition, can effectively reduce sintering temperature and reduce sintering time, reduce the graphite transition of diamond particles in high-temperature sintering process, improve ceramic-metallic hardness, obdurability and wear resistance.
3, in sintering process, Co, Ni coating and Ti(C, N) the transition metal carbides WC in based ceramic metal reacts, and has strengthened the hold of sintering metal matrix to diamond particles, has strengthened the wear resistance of ceramic-metal composite when improving hardness.
Claims (3)
1. diamond-Ti (C, N) based ceramic metal matrix material, is prepared by following methods, and it step comprising is:
1) prepare powdered mixture
The component of raw material and proportioning (weight percent)
The particulate matter that described powder additive is 20 microns～70 microns by median size forms, and these particulate matter are to consist of bortz core and the metal plating that is coated on bortz wicking surface, and described metal plating is selected from least one in Co, Ni;
The weight of described metal plating accounts for 7%～9% of per unit particulate matter weight;
Described iron family metal is selected from one or more in Co, Ni, Fe;
Described transition metal carbides is selected from WC, TaC, NbC, Mo
2one or more in C, VC;
According to above-mentioned component and proportioning, described Ti (C, N) powder, iron family metal, powder additive and transition metal carbides are mixed, make powdered mixture;
2) moulding
By pressure forming, above-mentioned powdered mixture is made to pressed compact;
3) sintering
Adopt plasma discharging technology to carry out sintering to above-mentioned pressed compact, during sintering, pressed compact is heated to 1200 ℃～1250 ℃ and be incubated 2 minutes～5 minutes in 30 minutes～40 minutes, sintering pressure is 20Mpa～30Mpa, after cooling, obtain described diamond-Ti (C, N) based ceramic metal matrix material.
2. the preparation method of diamond-Ti (C, N) based ceramic metal matrix material, the step comprising is:
1) prepare powdered mixture
The component of raw material and proportioning (weight percent)
The particulate matter that described powder additive is 20 microns～70 microns by median size forms, and these particulate matter are to consist of bortz core and the metal plating that is coated on bortz wicking surface, and described metal plating is selected from least one in Co, Ni;
The weight of stating metal plating accounts for 7%～9% of per unit particulate matter weight;
Described iron family metal is selected from one or more in Co, Ni, Fe;
Described transition metal carbides is selected from WC, TaC, NbC, Mo
2one or more in C, VC;
According to above-mentioned component and proportioning, described Ti (C, N) powder, iron family metal, powder additive and transition metal carbides are mixed, make powdered mixture;
2) moulding
By pressure forming, above-mentioned powdered mixture is made to pressed compact;
3) sintering
Adopt plasma discharging technology to carry out sintering to above-mentioned pressed compact, during sintering, pressed compact is heated to 1200 ℃～1250 ℃ and be incubated 2 minutes～5 minutes in 30 minutes～40 minutes, sintering pressure is 20Mpa～30Mpa, after cooling, obtain described diamond-Ti (C, N) based ceramic metal matrix material.
3. the preparation method of diamond-Ti as claimed in claim 2 (C, N) based ceramic metal matrix material, is characterized in that: the step that the preparation method of described powder additive comprises is: by diamond particles successively at SnCl
2solution and PdCl
2in solution, carry out respectively sensitization and activation treatment; Diamond particles after processing is dispersed in to CoSO
4and NiSO
4mixing solutions in, maybe the diamond particles after processing is dispersed in to CoSO
4solution or NiSO
4in solution, thereby obtain mixed slurry; In described mixed slurry, add sodium hypophosphite to carry out Co and/or Ni in the electroless plating on diamond particles surface, take and obtain by bortz core and be coated on the particulate matter that metal plating forms and median size is 20 microns～70 microns of bortz wicking surface; The introduction volume of Co and/or Ni accounts for 7%～9% of per unit particulate matter weight by the weight of metal plating in the particulate matter preparing and calculates.
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| CN103433488B (en) * | 2013-08-12 | 2015-07-01 | 南昌大学 | Preparation method of titanium nitride-ferrous metal ceramics |
| CN106001561B (en) * | 2016-06-03 | 2018-10-23 | 广东工业大学 | A kind of multistage composite cermet, preparation method and shield cutter |
| CN108315628B (en) * | 2016-08-03 | 2020-10-23 | 成都锦钛精工科技有限公司 | (Ti, Me) CN-Co-based coating spraying and 3D printing cermet material and preparation method thereof |
| CN106312048A (en) * | 2016-09-18 | 2017-01-11 | 广东工业大学 | Metal ceramic particle and preparation method and application thereof |
| CN108149100A (en) * | 2017-12-27 | 2018-06-12 | 洛阳神佳窑业有限公司 | Fire-fighting mouth cermet material |
| CN108149099A (en) * | 2017-12-27 | 2018-06-12 | 洛阳神佳窑业有限公司 | A kind of cermet material |
| CN111843165B (en) * | 2020-08-10 | 2021-07-09 | 中国电子科技集团公司第三十八研究所 | Diffusion connection method for diamond micro-channel |
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| CN101591194A (en) * | 2009-05-13 | 2009-12-02 | 桂林矿产地质研究院 | A kind of composite material for superhard cutting tool |
| CN102061417A (en) * | 2009-11-13 | 2011-05-18 | 厦门理工学院 | Nano silicon nitride and boron nitride reinforced titanium carbonitride based cermet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101591194A (en) * | 2009-05-13 | 2009-12-02 | 桂林矿产地质研究院 | A kind of composite material for superhard cutting tool |
| CN102061417A (en) * | 2009-11-13 | 2011-05-18 | 厦门理工学院 | Nano silicon nitride and boron nitride reinforced titanium carbonitride based cermet |
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Denomination of invention: Diamond Ti (C, n) based cermet composites and their preparation methods Effective date of registration: 20220630 Granted publication date: 20141022 Pledgee: Huishang Bank Co.,Ltd. Chengdu Jinsha sub branch Pledgor: CHENGDU MET-CERAMICS ADVANCED MATERIALS Co.,Ltd. Registration number: Y2022510000179 |
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