CN100548922C - Titanium nitride-TiB2-titanium silicide composite diphase material and in-situ reaction preparation method - Google Patents
Titanium nitride-TiB2-titanium silicide composite diphase material and in-situ reaction preparation method Download PDFInfo
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- CN100548922C CN100548922C CNB200710044847XA CN200710044847A CN100548922C CN 100548922 C CN100548922 C CN 100548922C CN B200710044847X A CNB200710044847X A CN B200710044847XA CN 200710044847 A CN200710044847 A CN 200710044847A CN 100548922 C CN100548922 C CN 100548922C
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- 239000000463 material Substances 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000010936 titanium Substances 0.000 title claims description 49
- 229910052719 titanium Inorganic materials 0.000 title claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 13
- 229910021341 titanium silicide Inorganic materials 0.000 title claims description 13
- 238000006243 chemical reaction Methods 0.000 title abstract description 19
- 238000011065 in-situ storage Methods 0.000 title abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 33
- 229910008484 TiSi Inorganic materials 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 10
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 239000011812 mixed powder Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 229910033181 TiB2 Inorganic materials 0.000 claims 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 4
- 230000001681 protective effect Effects 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 239000002184 metal Substances 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000011230 binding agent Substances 0.000 abstract description 10
- 230000003078 antioxidant effect Effects 0.000 abstract description 7
- 229910000765 intermetallic Inorganic materials 0.000 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 239000000919 ceramic Substances 0.000 abstract description 5
- 238000005520 cutting process Methods 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000013001 point bending Methods 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- 238000013461 design Methods 0.000 description 6
- 238000002791 soaking Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910004339 Ti-Si Inorganic materials 0.000 description 2
- 229910010978 Ti—Si Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 230000000181 anti-adherent effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 150000002738 metalloids Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000004482 other powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910021332 silicide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
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Abstract
The present invention relates to Ti
5Si
3(perhaps TiSi
2) intermetallic compound is as the TiN-TiB of binding agent
2-Ti
5Si
3(perhaps TiSi
2) ceramic base composite diphase material and in-situ reaction preparation method.Adopt general T i, BN and Si in the preparation process
3N
4Powder is starting raw material, and reaction in has been introduced at present as yet the Ti that commercial powder is not sold
5Si
3(perhaps TiSi
2) third phase, obtained and the close density of interpolation metal sintering, can reach more than 98%.Microhardness is 10-20GPa, three-point bending resistance intensity 〉=700MPa, K
IC〉=7MPam
1/2, have very strong resistance of oxidation in the air.Room-temperature conductivity＞1 * 10
5Ω
-1M
-1Material of the present invention has high rigidity, good wear-resistant and antioxidant property or the like, our preparation method's preparation cycle is short, energy consumption is low, environmental friendliness, production cost significantly reduces, the excellent material performance of preparing, the cutting processing of can discharging, be suitable as cutter material or wear parts or the like, have good industrial prospect.
Description
Technical field
The present invention relates to a kind of titanium nitride-TiB2-titanium silicide composite diphase material and in-situ reaction preparation method, or rather, relate to a kind of with Ti
5Si
3(perhaps TiSi
2) intermetallic compound is as the TiN-TiB of binding agent
2-Ti
5Si
3(perhaps TiSi
2) structural ceramics composite diphase material and in-situ reaction preparation method thereof.
Background technology
TiN, TiB
2And TiC has high fusing point, hardness and good specific conductivity etc., thereby is used as heat resistant and wear resistant and decreases material, surface decoration material, fused salt electrolysis electrode and electrical contact etc.TiN-TiB
2Perhaps Ti (C, N)-TiB
2Composite diphase material has the over-all properties more superior than monophase materials, can be as cutting tool material and wear parts etc.Prepared TiN-30wt%TiB such as employing pressure sinterings such as K.Shobu in the document 1 (Journal of the AmericanCeramic Society, 70:103 (1987))
2Composite diphase material, shearing resistance has reached 700MPa, and hardness is 18GPa, and fracture toughness property has reached 3MPam
1/2But what hinder that it further develops application is problems such as sintering temperature height, toughness are low, manufacturing cost height.In order further to reduce sintering temperature, improve toughness of material, the material supply section scholar adopts metal (as Co, Ni, Fe etc.) to reduce TiN-TiB as binding agent
2Sintering temperature, improve the toughness of material.As binding agent, TiN-TiB has been prepared in 1600 ℃ of reaction hot-pressings such as employing Ni such as Zhang Guojun in the document 2 (Joumal of the American Ceramic Society, 78:2331 (1995))
2Composite diphase material.Result of study has obviously improved TiN-TiB when finding the Ni addition less than 1wt%
2The sintering character of material, the high tenacity that obtains material has reached 6.20 ± 0.21MPam
1/2Patent about cermet material and preparation method also has a lot, as Chinese patent ZL02139790.2, ZL03132641.2, U.S. Pat 10/679,379, European patent EP 1422305A2 and Japanese Patent JP2004169187A etc.
Yet people find in theory and the real application research in the past few decades, use the metal adhesive sintered ceramic material to have the shortcoming of some essence.The one, meeting reduces the hardness of material, and the 2nd, the antioxidant property of reduction material, the 3rd, as the cutter cutting metal time, the cementing metal is easily with being cut metal reaction.And in using as cutter material and high-temperature structural material, these performances (hardness, antioxidant property and and be cut reactionlessness between the metal) are relatively more crucial exactly.Intermetallic compound has the mechanical property between pottery and metal, and the high-temperature oxidation resistance stronger than metal arranged.So intermetallic compound is considered to substitute the material of conventional metals binding agent.Wherein Ti-Si composition such as TiSi
2Or Ti
5Si
3A lot of attentions have been attracted.As Ti
5Si
3Has the low (4.32g/cm of density
3), fusing point height (2130 ℃), Young's modulus height (160GPa), normal temperature and hot hardness height, solidity to corrosion reach characteristics such as high-temperature oxidation resistance excellence well, just caused people's attention before more than 50 years.Strong bond makes it show excellent wear-resistant material wearing and tearing and anti-adhesive wear performance in conjunction with character between the prevailing atom of its high rigidity, high elastic coefficient and covalent linkage thereof.The more important thing is that people infer that the Ti-Si compound can become TiN-TiB
2The binding agent that system is suitable is because relative TiN of their fusing point and TiB
2Still low is many, and brittle-ductile transition temperature (Ti
5Si
3Brittle transition temperature be 1000 ℃, and TiSi
2Lower, be 805 ℃) the above viscous deformation that metalloid can take place.In research work in the past, Ti
5Si
3(perhaps TiSi
2) be added to the antioxidant property that improves the TiN coating in the TiN coating, as document 3 (Thin Solid Films, 315:336 (1998)) and document 4 (Surface and CoatingTechnology, 133-134:336 (1998)) etc.In addition, people such as Kim adopts high energy ball mill method to prepare TiN/TiB in the document 5 (Intermetallics, 15:206 (2007))
2/ Ti-Silicide (Ti
5Si
3Perhaps TiSi
2) nanometer complex phase powder, find that powder has good thermostability.But research work and patent as binding agent sintering structure ceramic block material aspect yet there are no relevant report.The present invention attempts to use Ti
5Si
3(perhaps TiSi
2) this intermetallic compound is as TiN-TiB
2The binding agent of system complex phase ceramic and substitute traditional metal adhesive, thus reach the purpose that improves its comprehensive mechanical property and high-temperature oxidation resistance.
Because Ti
5Si
3(perhaps TiSi
2) also there is not commercial powder, if preparation contains Ti
5Si
3(perhaps TiSi
2) composite diphase material, generally need prepare Ti earlier
5Si
3(perhaps TiSi
2) powder, then with other powder mixes mutually, final sintering is prepared corresponding composite diphase material.Adopt SPS reaction in method, can save the step of synthetic separately, processing and batch mixing, in addition can rapid reaction prepare and have the compact grained composite diphase material.Therefore, the present invention intends adopting SPS reaction in synthesis of densified TiN-TiB
2-Ti
5Si
3(perhaps TiSi
2) compound composite diphase material between ceramic-metal.
Summary of the invention
The object of the present invention is to provide a kind of titanium nitride-TiB2-titanium silicide composite diphase material and preparation method, that is provide a kind of provide have superior mechanical property and antioxidant property, the good TiN-TiB of sintering character
2-Ti
5Si
3(perhaps TiSi
2) composite diphase material.Ti wherein
5Si
3(perhaps TiSi
2) volume content be 5～40%, TiB
2Volume content be 30～10%, surplus is TiN.And provide preparation method simple to operate accordingly, easy control of process conditions.
The technical problem to be solved in the present invention is: adopt original position discharge plasma (SPS) reaction method, and the adjusting process parameter, preparation is with Ti
5Si
3(perhaps TiSi
2) intermetallic compound is as the TiN-TiB of binding agent
2-Ti
5Si
3(perhaps TiSi
2) composite diphase material.This kind method can obviously reduce TiN-TiB
2The sintering temperature of composite diphase material shortens sintering time.And it is adjusted and controlled to obtain high comprehensive mechanical property such as fracture toughness property etc. by adjusting proportioning etc.
Key problem in technology of the present invention is by selecting commercially available Ti, BN and Si
3N
4Powder is that raw material, design raw material are formed proportioning, optimized processing parameter, the control microstructure develops, obtain on the basis with the sintering temperature that reduces material have meticulous microstructure, favorable conductive, antioxidant property and mechanical property sintered material.At first design raw material and form proportioning, pass through traditional mechanical batch mixing then, carry out discharge plasma reaction in sintering at last, main by control SPS sintering process parameter, comprise sintering temperature, pressure, temperature rise rate, soaking time etc.Following each step is specifically arranged:
1) selection of material powder and preparation
With commercially available commercial Ti, BN and Si
3N
4Powder is a raw material, according to different volumes content design proportioning, carries out the material powder weighing, utilizes mechanical ball milling then, carries out batch mixing in the alcohol medium.The material purity that uses is all greater than 99%, and particle diameter is less than 10 μ m..The ball mill mixing process generally adopts planetary ball mill, and rotational speed of ball-mill is that 150-250rpm, ball material weight ratio are that 4: 1, ball milling time are 18-24h, wet-milling in alcohol or acetone.Resulting wet mixing slurry is placed in the baking oven, is being lower than under alcohol or the acetone volatilization temperature oven dry 20-24 hour, crosses 320 mesh sieves at last and obtains raw material mixed powder less than 45 μ m.
Press (9-6x) Ti+2xBN+ (1-x) Si during the design proportioning
3N
4→ (4-2x) TiN+xTiB
2+ (1-x) Ti
5Si
3Perhaps (11-8x) Ti+2xBN+ (2-2x) Si
3N
4→ (8-6x) TiN+xTiB
2+ (3-3x) TiSi
2Batching, 0＜x in the formula＜1; Carry out.
2) reaction in sintering
Described reaction in sintering is to utilize SPS sintering method agglomerating under vacuum, high-purity argon gas or high pure nitrogen atmosphere; In preparation process, need strict control process parameters, comprise sintering temperature, pressure, temperature rise rate, soaking time etc.The agglomerating temperature range is 1300～1600 ℃; The temperature rise rate scope is 80～200 ℃/min; Determine that according to the different initial particle size of powder etc. the concrete sintered heat insulating time is 5-30min, preferentially recommend 10-15min; Pressure range is 50～70MPa.Described high-purity Ar or N
2Purity is more than 99.99%, in the time of 1000 ℃, applies 5-15MPa in advance.
The invention provides a kind of reaction in and prepare TiN-TiB
2-Ti
5Si
3(perhaps TiSi
2) method of composite diphase material.Adopt common commercial powder, with the control microstructure, guaranteeing TiN-TiB by reaction sintering
2On the good mechanical performance of material and the basis of electroconductibility, original position is introduced Ti
5Si
3(perhaps TiSi
2) binding agent, obviously having improved the sintered density of material, can reach more than 98%.Preparation cycle is short, energy consumption is low, environmental friendliness, and production cost significantly reduces; The material mechanical performance height of preparing, antioxidant property is superior, has high specific conductivity, the cutting processing of can discharging, thus have good industrial prospect.
Description of drawings
Fig. 1 is original position discharge plasma sintering TiN-TiB provided by the invention
2-Ti
5Si
3The X ray diffracting spectrum of sample.Contrast powdery diffractometry standard card can judge to have only TiN, TiB in the synthetic composite diphase material
2And Ti
5Si
3Three kinds of materials do not have other impurity substances to generate.
Fig. 2 is sintering TiN-TiB
2-Ti
5Si
3The SEM micro-structure diagram of sample.Can see that three-phase is evenly distributed.
Embodiment
Raw material powder is pressed Ti in the final product
5Si
3Theoretical volume content is the 20vol.% batching.React as follows:
(9-6x)Ti+2xBN+(1-x)Si
3N
4→(4-2x)TiN+xTiB
2+(1-x)Ti
5Si
3
Prepare burden according to design result then, with Ti, BN and Si
3N
4Place ball grinder, with alcohol medium ball milling wet mixing 20h, rotating speed is 250rpm, carries out drying and screening then.Dried powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.
The reaction sintering process is carried out under vacuum condition, and sintering temperature is 1450 ℃; Temperature rise rate is 80～200 ℃/min; Soaking time is 10min; Adopt two step pressing mode, temperature is 1000 ℃ and applies 15MPa earlier that holding stage institute applied pressure is 70MPa when arriving 1450 ℃ of sintering temperatures.The relative density of the sintered compact that is obtained is 98%, and microhardness is 10-20GPa, three-point bending resistance intensity 〉=700MPa, K
IC=7.5MPam
1/2, do not have obvious oxidation below 1000 ℃.Room-temperature conductivity is 1.7 * 10
5Ω
-1M
-1Prepared TiN-TiB
2-Ti
5Si
3The x diffractogram as shown in Figure 1, the composite diphase material of preparation only contains TiN, TiB
2And Ti
5Si
3Three-phase;
Raw material powder is pressed TiSi in the final product
2Theoretical volume content is the 20vol.% batching.React as follows:
(11-8x)Ti+2xBN+(2-2x)Si
3N
4→(8-6x)TiN+xTiB
2+(3-3x)TiSi
2
Prepare burden according to design result then, with Ti, BN and Si
3N
4Place ball grinder, with alcohol medium ball milling wet mixing 24h, rotating speed is 250rpm, carries out drying and screening then.Dried powder is packed into behind the graphite jig, put into SPS equipment and carry out sintering.
The reaction sintering process is carried out under vacuum or high-purity argon gas condition, and sintering temperature is 1400 ℃; Temperature rise rate is 80～200 ℃/min; Soaking time is 15min; Adopt two step pressing mode, elder generation's applied pressure was 16MPa when temperature rose to 1000 ℃, and 1400 ℃ of holding stage institute applied pressures are 50MPa.The relative density of the sintered compact that is obtained is 98%, and microhardness is 10-20GPa, three-point bending resistance intensity 〉=700MPa, K
IC=7.1MPam
1/2, do not have obvious oxidation below 900 ℃.Room-temperature conductivity 5.3 * 10
5Ω
-1M
-1
Claims (9)
1, a kind of titanium nitride-TiB2-titanium silicide composite diphase material is characterized in that described composite diphase material consists of: TiN-TiB
2-Ti
5Si
3Or TiN-TiB
2-TiSi
2, wherein, TiB
2Volume content is 30-10%, Ti
5Si
3Or TiSi
2Volume content be 5-40%, surplus is TiN.
2, prepare titanium nitride-TiB2 as claimed in claim 1-titanium silicide composite diphase material, it is characterized in that preparation process is:
A) select Ti, BN, Si
3N
4Powder is a raw material, according to (9-6x) Ti+2xBN+ (1-x) Si
3N
4→ (4-2x) TiN+xTiB
2+ (1-x) Ti
5Si
3Perhaps (11-8x) Ti+2xBN+ (2-2x) Si
3N
4→ (8-6x) TiN+xTiB
2+ (3-3x) TiSi
2Batching, 0＜x in the formula＜1;
B) the planetary ball mill batch mixing, dry and sieve;
C) discharge plasma sintering;
The rotational speed of ball-mill of described ball mill mixing is 150-250rpm;
Described discharge plasma agglomerating temperature is 1300-1600 ℃; Temperature rise rate is 80-200 ℃/min; The sintered heat insulating time is 5-30min; Applying pressure is 50-70MPa, applies at twice, applies pre-pressure in the time of 1000 ℃.
3, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, it is characterized in that the ball milling time in the step b) is 18-24 hour.
4, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, it is characterized in that the pre-pressure that sintering applies when being warming up to 1000 ℃ is 5-15MPa.
5, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, the protective atmosphere that uses when it is characterized in that sintering is vacuum, high-purity argon gas or high pure nitrogen, and high pure nitrogen or high-purity argon gas are more than 99.99%.
6, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, the purity that it is characterized in that the raw material that uses is all more than 99%, and particle diameter is all less than 10 μ m.
7, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, it is characterized in that the discharge plasma sintering; The sintered heat insulating time is 10-15min.
8, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, the medium when it is characterized in that batch mixing is ethanol or acetone, and the ball material mass ratio during batch mixing is 4: 1.
9, by the preparation method of the described titanium nitride-TiB2 of claim 2-titanium silicide composite diphase material, it is characterized in that the oven dry of batch mixing slurry is to be lower than under alcohol or the acetone volatilization temperature dry 20-24 hour, sieve after the drying to make＜mixed powder of 45 μ m.
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| CN102898140B (en) * | 2012-10-10 | 2014-04-09 | 武汉理工大学 | Titanium diboride-titanium nitride nano heterostructure composite ceramic powder and preparation method thereof |
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