CN105274375A - Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles - Google Patents
Method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles Download PDFInfo
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- CN105274375A CN105274375A CN201510723476.2A CN201510723476A CN105274375A CN 105274375 A CN105274375 A CN 105274375A CN 201510723476 A CN201510723476 A CN 201510723476A CN 105274375 A CN105274375 A CN 105274375A
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Abstract
The invention relates to a TNZS alloy and particularly relates to a method for compounding and preparing high-elastic-modulus Ti-based material based on nano ceramic particles. The method comprises the following steps: firstly taking Ti, Nb, Zr, Sn, TiO2 and HA powder as raw material, carrying out high-energy ball milling twice to prepare mixed powder; then carrying out normal die pressing treatment on the mixed powder; and finally vacuum sintering pressed blocks obtained by die pressing without pressure to obtain uniform-surface-component and high-elastic-modulus Ti-based material containing 5wt% of TiO2/TNZS and 5wt% of HA/TNZS. As a preparation method of the Ti-based material, the problem with insufficient elastic modulus of the TNZS alloy can be effectively solved; the preparation process is simple; the application range of the titanium material in the fields of aerospace, traffic transportation and weapon equipment is expanded.
Description
Technical field
The present invention relates to TNZS alloy, especially prepare the method for high elastic coefficient Ti sill based on nano-ceramic particle compound,
Specifically, be a kind of high elastic coefficient 5wt.%TiO
2the preparation method of/TNZS and 5wt.%HA/TNZS titanium base material.
Background technology
Ti-24Nb-4Zr-7.9Sn(TNZS) alloy high comprehensive performance, but its Young's modulus is lower, also cannot meet the requirement in aerospace and weaponry field, and make the adding of Nb, Zr element the technology of preparing of alloy propose higher requirement, limit its widespread use at space flight, communications and transportation and weaponry; Therefore, more deep research need be launched to the beta titanium alloy of this new generation of TNZS alloy, and containing TiO
2the Young's modulus on titanium material surface significantly can be strengthened with HA titanium base material; High-energy ball milling, also known as mechanical alloying, belong to the one of powder metallurgy technology, it is subject to the impact of technological process and processing parameter, the time of proper extension high-energy ball milling, can make the microtexture refinement of powder, tissue changes, improve alloying level, the equipment that vacuum non-pressure sintering technology adopts is simple, regulates and controls reaction process to reach the object optimizing material structure by the control of the processing parameter such as sintering temperature, sintering time.
The powder metallurgy technology that the present invention adopts twice high-energy ball milling to combine with conventional mold pressing, vacuum non-pressure sintering prepares 5wt.%TiO2/TNZS and the 5wt.%HA/TNZS titanium base material containing refractory metal Nb, passes through TiO
2with the nano effect of HA, increase considerably the Young's modulus of TNZS sill, improve the over-all properties of TNZS sill.According to the knowledge of the applicant, employing powder metallurgic method is not yet had to prepare 5wt.%TiO
2the report of/TNZS and 5wt.%HA/TNZS titanium base material.
Summary of the invention
Of the present invention is a kind of high elastic coefficient 5wt.%TiO
2the preparation method of/TNZS and 5wt.%HA/TNZS titanium base material, the 5wt.%TiO that this invention obtains
2/ TNZS and 5wt.%HA/TNZS titanium base material have face uniform composition and Young's modulus advantages of higher, and preparation method simple to operate, easily realize, economical.
Technical scheme of the present invention is:
A kind of high elastic coefficient 5wt.%TiO
2the preparation method of/TNZS titanium base material, is characterized in that carrying out according to following steps:
1, twice high-energy ball milling mixed powder preparation: first prepare Ti-24Nb-4Zr-7.9Sn(TNZS by composition) mixed powder, after first time high-energy ball milling, then add TiO
2nanometer powder, TiO
2nanometer powder accounts for and adds TiO
25% of TNZS mixed powder quality after nanometer powder, after second time high-energy ball milling, is placed in vacuum drying oven and dries, sieve.
2, the method for conventional mold pressing process: mixed powder step 1 prepared is pressed, and obtains briquetting.
3, vacuum non-pressure sintering process: the briquetting of step 2 compression moulding is carried out vacuum non-pressure sintering.
A kind of preparation method of high elastic coefficient 5wt.%HA/TNZS titanium base material, it is characterized in that carrying out according to following steps: 1, twice high-energy ball milling mixed powder preparation: first prepare Ti-24Nb-4Zr-7.9Sn(TNZS by composition) mixed powder, after first time high-energy ball milling, add HA nanometer powder again, 5% of TNZS mixed powder quality after HA nanometer powder accounts for and adds HA nanometer powder, after second time high-energy ball milling, be placed in vacuum drying oven and dry, sieve.
2, the method for conventional mold pressing process: mixed powder step 1 prepared is pressed, and obtains briquetting.
3, vacuum non-pressure sintering process: the briquetting of step 2 compression moulding is carried out vacuum non-pressure sintering.
Further, Ti-24Nb-4Zr-7.9Sn, its component is calculated by percentage to the quality, is respectively Ti powder: 64.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%.
Further, the ball-milling technology of high-energy ball milling is for the first time: planetary ball mill, ratio of grinding media to material 10:1,300r/min ball milling 48h, ball milling 1h shut down 15min.
Further, the ball-milling technology of second time high-energy ball milling is: 300r/min ball milling 1h.
Further, the technique of compression moulding is: pressing pressure is 18MPa, and pressurize 5min obtains required briquetting, and briquetting diameter is 30mm, and thickness is 10mm.
Further, the technique of vacuum non-pressure sintering is: vacuum tightness 7.810
-1pa, temperature rise rate 10 DEG C/min, first pre-burning to 600 DEG C insulation 2h, is warming up to 800 DEG C of insulation 2h, then is warming up to 1000 DEG C of insulation 2h, is finally warming up to 1250 DEG C of insulation 2h, rear furnace cooling.
Further, described TiO
2the particle diameter of nanometer powder is 40nm, the particle diameter <100nm of described HA nanometer powder.
The invention has the beneficial effects as follows:
(1) powder metallurgy technology that combined by " twice high-energy ball milling-conventional mold pressing-vacuum non-pressure sintering " of the present invention, obtains the TNZS metal alkyl materials of two kinds of face distributed components, for titanium metal provide a kind of can the preparation method of suitability for industrialized production.
(2) 5wt.%TiO for preparing of the present invention
2the Young's modulus of/TNZS and 5wt.%HA/TNZS titanium base material is respectively 103.93GPa and 119.43GPa, than TNZS(64.00GPa) improve 62.39% and 86.61% respectively.
(3) the present invention is not only applicable to the preparation of TNZS base titanium alloy, is also applicable to the preparation of various model titanium material.
Accompanying drawing explanation
Fig. 1 is the XRD analysis spectrum of TNZS mixed powder.
Fig. 2 is the 5wt.%TiO utilizing the present invention to prepare gained
2the XRD analysis spectrum of/TNZS mixed powder.
Fig. 3 is the XRD analysis spectrum utilizing the present invention to prepare the 5wt.%HA/TNZS mixed powder of gained.
Fig. 4 is the 5wt.%TiO utilizing the present invention to prepare gained
2the SEM surface topography of/TNZS mixed powder, 5wt.%HA/TNZS mixed powder and TNZS mixed powder.
Fig. 5 is the XRD analysis spectrum of TNZS titanium base material.
Fig. 6 is the 5wt.%TiO utilizing the present invention to prepare gained
2the XRD analysis spectrum of/TNZS titanium base material.
Fig. 7 is the XRD analysis spectrum utilizing the present invention to prepare the 5wt.%HA/TNZS titanium base material of gained.
Fig. 8 is the 5wt.%TiO utilizing the present invention to prepare gained
2the SEM surface topography of/TNZS titanium base material, 5wt.%HA/TNZS titanium base material and TNZS titanium base material.
Fig. 9 is the 5wt.%TiO utilizing the present invention to prepare gained
2the springform spirogram of/TNZS titanium base material, 5wt.%HA/TNZS titanium base material and TNZS titanium base material.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention will be further described.
Embodiment 1
A preparation method for high elastic coefficient 5wt.%TiO2/TNZS titanium base material, comprises the following steps:
1, twice high-energy ball milling mixed powder preparation: first prepare Ti-24Nb-4Zr-7.9Sn(TNZS) mixed powder; the mass percent of each component is respectively Ti powder: 64.1%; Nb powder: 24%; Zr powder: 4%, Sn powder: 7.9%, through first time high-energy ball milling (planetary ball mill; ratio of grinding media to material 10:1; 300r/min ball milling 48h, ball milling 1h shut down 15min) after, then add TiO
2nanometer powder (granularity 40nm), preparation is the TiO of 5% containing massfraction
2/ TNZS mixed powder, continues high-energy ball milling (300r/min ball milling 1h), is placed in vacuum drying oven and dries, sieve.
2, the method for conventional mold pressing process: mixed powder step 1 prepared is pressed at the YB32-100 hydropress that Nantong forging equipment factory manufactures, and (pressing pressure is 18Mpa, pressurize 5min), obtain required briquetting (diameter is 30mm, and thickness is 10mm).
3, vacuum non-pressure sintering process: the briquetting of step 2 compression moulding is placed on WZS-20 type two-chamber vacuum sintering furnace and carries out pressureless sintering; Wherein vacuum tightness 7.810
-1pa, temperature rise rate 10 DEG C/min, sintering process is first pre-burning to 600 DEG C insulation 2h, is warming up to 800 DEG C of insulation 2h, then is warming up to 1000 DEG C of insulation 2h, is finally warming up to 1250 DEG C of insulations 2h, subsequently furnace cooling.
What adopt above-mentioned steps obtains 5wt.%TiO
2except SrilankiteTiO being detected in the XRD spectrum of/TNZS mixed powder
2existence, also have RutileTiO
2with AnataseTiO2(Fig. 1, shown in 2); After ball milling, alloying phenomenon is obvious, and the shape of particle becomes comparison rule, without obvious corner angle; Size obviously reduces, and maximum particle size is no more than 35 μm (as shown in Fig. 4 a, b); Adopt the 5wt.%TiO that aforesaid method is obtained
2/ TNZS titanium base material thing be divided by generate α-Ti phase and β-Ti mutually outside, owing to adding 5wt.%TiO
2, also detect Rutile Type TiO
2and Anatase TiO
2(as shown in Figure 5,6); According to Fig. 8 b pattern, contrast TNZS titanium base material tissue (shown in Fig. 8 a), TiO
2/ TNZS is also by greyish black, grey, greyish white, white four phase composites represented with 1,2,3,4 four Qu Wei, and phase composite and TNZS basic simlarity are that constituent content is distinguished to some extent; Add the TiO of 5wt.%
2, make TiO
2relatively be evenly distributed in TiO
2in/TNZS agglomerated material, thus make oxygen element content in most of region relatively high; As shown in Figure 9, compared with TNZS titanium base material, the Young's modulus of 5wt.%TiO2/TNZS titanium base material is 103.93GPa, than TNZS(64.00GPa) improve 62.39%.
Embodiment 2
A kind of preparation method of high elastic coefficient 5wt.%HA/TNZS titanium base material:
Roughly the same, it is the TiO of 5% that difference is massfraction for the present embodiment and embodiment 1
2powder replaces with 5wt.%HA nanometer powder.
What adopt above-mentioned steps obtains 5wt.%HA/TNZS mixed powder mechanical alloying phenomenon obviously, except SrilankiteTiO being detected in the XRD spectrum of powder
2existence, also have RutileTiO2 and AnataseTiO
2(shown in Fig. 1,3); Having there is the phenomenon of reunion and cold welding in particle, makes the difficulty of powder fining aggravate finally to be tending towards axiolitic rock steady structure; Particle is subject to crushing, extruding and the acting in conjunction such as mechanical grinding and refinement, and size obviously reduces, and maximum particle size is no more than 35 μm (as illustrated in fig. 4 c); In the 5wt.%HA/TNZS titanium base material adopting aforesaid method obtained except α-Ti, β-Ti and HA being detected, also Ti detected
2o, CaTiO
3, CaO and Ti
xp
ycenotype, and these cenotypes can to generate be because HA non-refractory, easily decompose 1000 DEG C more than and react with Ti and form (as Fig. 5,7 shown); According to Fig. 8 c shape appearance figure, contrast TNZS titanium base material tissue (shown in Fig. 8 a), the tissue of 5wt.%HA/TNZS and 5%TiO
2/ TNZS basic simlarity, just surface arrangement is by more uniformly containing the small white spots tissue that calcium phosphorous compound forms; As shown in Figure 9, compared with TNZS titanium base material, the Young's modulus of 5wt.%HA/TNZS titanium base material is 119.43GPa, than TNZS(64.00GPa) improve 86.61%.
The part that the present invention does not relate to prior art that maybe can adopt all same as the prior art is realized.
Claims (8)
1. prepare the method for high elastic coefficient Ti sill based on nano-ceramic particle compound, it is characterized in that carrying out according to following steps:
1), the preparation of twice high-energy ball milling mixed powder: first prepare Ti-24Nb-4Zr-7.9Sn(TNZS by composition) mixed powder, after first time high-energy ball milling, then add TiO
2nanometer powder, TiO
2nanometer powder accounts for and adds TiO
25% of TNZS mixed powder quality after nanometer powder, after second time high-energy ball milling, is placed in vacuum drying oven and dries, sieve;
2), the method for conventional mold pressing process: mixed powder step 1 prepared is pressed, and obtains briquetting;
3), vacuum non-pressure sintering process: the briquetting of step 2 compression moulding is carried out vacuum non-pressure sintering.
2. prepare the method for high elastic coefficient Ti sill based on nano-ceramic particle compound, it is characterized in that carrying out according to following steps:
1), twice high-energy ball milling mixed powder preparation: first prepare Ti-24Nb-4Zr-7.9Sn(TNZS by composition) mixed powder, after first time high-energy ball milling, add HA nanometer powder again, 5% of TNZS mixed powder quality after HA nanometer powder accounts for and adds HA nanometer powder, after second time high-energy ball milling, be placed in vacuum drying oven and dry, sieve;
2), the method for conventional mold pressing process: mixed powder step 1 prepared is pressed, and obtains briquetting;
3), vacuum non-pressure sintering process: the briquetting of step 2 compression moulding is carried out vacuum non-pressure sintering.
3. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2, it is characterized in that: Ti-24Nb-4Zr-7.9Sn, its component is calculated by percentage to the quality, be respectively Ti powder: 64.1%, Nb powder: 24%, Zr powder: 4%, Sn powder: 7.9%.
4. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2; it is characterized in that: the ball-milling technology of high-energy ball milling is for the first time: planetary ball mill; ratio of grinding media to material 10:1,300r/min ball milling 48h, ball milling 1h shut down 15min.
5. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2, is characterized in that: the ball-milling technology of second time high-energy ball milling is: 300r/min ball milling 1h.
6. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2, it is characterized in that: the technique of compression moulding is: pressing pressure is 18MPa, pressurize 5min obtains required briquetting, briquetting diameter is 30mm, and thickness is 10mm.
7. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2, is characterized in that: the technique of vacuum non-pressure sintering is: vacuum tightness 7.810
-1pa, temperature rise rate 10 DEG C/min, first pre-burning to 600 DEG C insulation 2h, is warming up to 800 DEG C of insulation 2h, then is warming up to 1000 DEG C of insulation 2h, is finally warming up to 1250 DEG C of insulation 2h, rear furnace cooling.
8. the method preparing high elastic coefficient Ti sill based on nano-ceramic particle compound as claimed in claim 1 or 2, is characterized in that: described TiO
2the particle diameter of nanometer powder is 40nm, the particle diameter <100nm of described HA nanometer powder.
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Cited By (9)
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| CN106086720A (en) * | 2016-06-15 | 2016-11-09 | 苏州洪河金属制品有限公司 | A kind of composite titan-based rotor material of high speed centrifuge pull resistance and preparation method thereof |
| CN106244852A (en) * | 2016-08-18 | 2016-12-21 | 江苏大学 | A kind of Ti 8Si alloy of Zr alloying and preparation method thereof |
| CN108611528A (en) * | 2018-05-09 | 2018-10-02 | 西南交通大学 | A kind of graphene enhancing titanium-based/nano HA composite material and preparation method |
| CN109055818A (en) * | 2018-09-10 | 2018-12-21 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Cu alloying |
| CN109161725A (en) * | 2018-09-10 | 2019-01-08 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Co alloying |
| CN109182839A (en) * | 2018-08-27 | 2019-01-11 | 江苏大学 | A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy |
| CN109182811A (en) * | 2018-08-27 | 2019-01-11 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying |
| CN109207795A (en) * | 2018-08-27 | 2019-01-15 | 江苏大学 | A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy and preparation method thereof |
| CN109666820A (en) * | 2018-12-19 | 2019-04-23 | 云南大学 | A kind of porous orthopaedics of outer layer of radial structure-function integration is implanted into material and its preparation method and application firmly |
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| CN106086720A (en) * | 2016-06-15 | 2016-11-09 | 苏州洪河金属制品有限公司 | A kind of composite titan-based rotor material of high speed centrifuge pull resistance and preparation method thereof |
| CN106244852A (en) * | 2016-08-18 | 2016-12-21 | 江苏大学 | A kind of Ti 8Si alloy of Zr alloying and preparation method thereof |
| CN106244852B (en) * | 2016-08-18 | 2017-12-19 | 江苏大学 | A kind of Ti 8Si alloys of Zr alloyings and preparation method thereof |
| CN108611528A (en) * | 2018-05-09 | 2018-10-02 | 西南交通大学 | A kind of graphene enhancing titanium-based/nano HA composite material and preparation method |
| CN109182839A (en) * | 2018-08-27 | 2019-01-11 | 江苏大学 | A kind of Y2O3The Ti-4Si/5TiO of alloying2The preparation method of alloy |
| CN109182811A (en) * | 2018-08-27 | 2019-01-11 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Ag alloying |
| CN109207795A (en) * | 2018-08-27 | 2019-01-15 | 江苏大学 | A kind of Zr, Y2O3The Ti-4Si/5TiO of alloying2Alloy and preparation method thereof |
| CN109055818A (en) * | 2018-09-10 | 2018-12-21 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Cu alloying |
| CN109161725A (en) * | 2018-09-10 | 2019-01-08 | 江苏大学 | A kind of preparation method of the Ti-24Nb-4Zr-7.9Sn alloy of Co alloying |
| CN109666820A (en) * | 2018-12-19 | 2019-04-23 | 云南大学 | A kind of porous orthopaedics of outer layer of radial structure-function integration is implanted into material and its preparation method and application firmly |
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