CN105274375B - Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle - Google Patents
Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle Download PDFInfo
- Publication number
- CN105274375B CN105274375B CN201510723476.2A CN201510723476A CN105274375B CN 105274375 B CN105274375 B CN 105274375B CN 201510723476 A CN201510723476 A CN 201510723476A CN 105274375 B CN105274375 B CN 105274375B
- Authority
- CN
- China
- Prior art keywords
- powder
- tnzs
- elastic modulus
- sills
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Powder Metallurgy (AREA)
Abstract
The present invention relates to TNZS alloys, the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle is based especially on, is comprised the following steps：First, it is with Ti, Nb, Zr, Sn, TiO2, HA powder be raw material through high-energy ball milling twice be prepared into mixed-powder prepare.Then, mixed-powder is carried out into conventional molding to handle.Finally, molding gained briquetting is subjected to vacuum non-pressure sintering processing, acquisition face composition is uniform, the 5wt.%TiO of high elastic modulus2/ TNZS and 5wt.%HA/TNZS titanium base materials.The present invention solves the not enough problem of TNZS alloy elastics modulus well as a kind of preparation method of titanium base material, and preparation technology is simple, has widened application of the titanium in Aero-Space, communications and transportation and weaponry field.
Description
Technical field
The present invention relates to TNZS alloys, it is based especially on that nano-ceramic particle is compound to prepare high elastic modulus Ti sills
Method,
Specifically, it is a kind of high elastic modulus 5wt.%TiO2/ TNZS and 5wt.%HA/TNZS titanium base materials preparation side
Method.
Background technology
Ti-24Nb-4Zr-7.9Sn（TNZS）Alloy high comprehensive performance, but its modulus of elasticity is relatively low, can not also meet boat
Empty space flight and the requirement in weaponry field, and the addition of Nb, Zr element make it that the technology of preparing proposition to alloy is higher
It is required that, limit its extensive use in space flight, communications and transportation and weaponry；Therefore, need to be to this β of new generation of TNZS alloys
Type Titanium Alloy expansion deeper into research, and contain TiO2The springform on titanium surface can be greatly enhanced with HA titanium base materials
Amount；High-energy ball milling, also known as mechanical alloying, belong to one kind of PM technique, and it is by technical process and technological parameter
Influence, the time of proper extension high-energy ball milling, can refine the microstructure of powder, tissue changes, and improve alloying journey
Degree, the equipment that vacuum non-pressure sintering technology is used is simple, is regulated and controled by the control of the technological parameters such as sintering temperature, sintering time
Course of reaction optimizes the purpose of material structure to reach.
The present invention is made using high-energy ball milling twice with the PM technique that routinely molding, vacuum non-pressure sintering are combined
The standby 5wt.%TiO2/TNZS and 5wt.%HA/TNZS titanium base materials containing refractory metal Nb, pass through TiO2Imitated with HA nanometer
Should, the modulus of elasticity of TNZS sills is increased considerably, the combination property of TNZS sills is improved.As far as the applicant is aware, not yet
Have and 5wt.%TiO is prepared using powder metallurgic method2/ TNZS and 5wt.%HA/TNZS titanium base materials report.
The content of the invention
That the present invention is a kind of high elastic modulus 5wt.%TiO2/ TNZS and 5wt.%HA/TNZS titanium base materials preparation side
Method, the 5wt.%TiO that the invention is obtained2/ TNZS and 5wt.%HA/TNZS titanium base materials have that face composition is uniform and modulus of elasticity is high
The advantages of, and preparation method is simple to operate, easy realization, economical.
The technical scheme is that：
A kind of high elastic modulus 5wt.%TiO2The preparation method of/TNZS titanium base materials, it is characterized in that entering according to following steps
OK：
1st, twice prepared by high-energy ball milling mixed-powder：Ti-24Nb-4Zr-7.9Sn is first prepared by composition（TNZS）Mixed powder
End, after first time high-energy ball milling, adds TiO2Nanometer powder, TiO2Nanometer powder accounts for addition TiO2After nanometer powder
After the 5% of TNZS mixed-powder quality, second of high-energy ball milling, drying in vacuum drying chamber, sieving are placed in.
2nd, the method for conventional molding processing：Mixed-powder prepared by step 1 is pressed, and obtains briquetting.
3rd, vacuum non-pressure sintering is handled：The compressing briquetting of step 2 is subjected to vacuum non-pressure sintering.
A kind of preparation method of high elastic modulus 5wt.%HA/TNZS titanium base materials, it is characterized in that entering according to following steps
OK：1st, twice prepared by high-energy ball milling mixed-powder：Ti-24Nb-4Zr-7.9Sn is first prepared by composition（TNZS）Mixed-powder, warp
After first time high-energy ball milling, HA nanometer powders are added, HA nanometer powders account for the TNZS mixed-powders added after HA nanometer powders
After the 5% of quality, second of high-energy ball milling, drying in vacuum drying chamber, sieving are placed in.
2nd, the method for conventional molding processing：Mixed-powder prepared by step 1 is pressed, and obtains briquetting.
3rd, vacuum non-pressure sintering is handled：The compressing briquetting of step 2 is subjected to vacuum non-pressure sintering.
Further, Ti-24Nb-4Zr-7.9Sn, its component is calculated by percentage to the quality, respectively Ti powder：64.1%, Nb
Powder:24 %, Zr powder:4 %, Sn powder：7.9%.
Further, the ball-milling technology of first time high-energy ball milling is：Planetary ball mill, ratio of grinding media to material 10:1,300r/min ball
48h is ground, ball milling 1h shuts down 15min.
Further, the ball-milling technology of second of high-energy ball milling is：300r/min ball millings 1h.
Further, compressing technique is：Pressing pressure is 18MPa, the min of pressurize 5, produces required briquetting, briquetting
A diameter of 30mm, thickness is 10 mm.
Further, the technique of vacuum non-pressure sintering is：Vacuum 7.8 10-1Pa, 10 DEG C/min of heating rate, it is first pre-
Burn to 600 DEG C of 2 h of insulation, be warming up to 800 DEG C of insulation 2h, then be warming up to 1000 DEG C of insulation 2h, be finally warming up to 1250
DEG C insulation 2h, rear furnace cooling.
Further, the TiO2The particle diameter of nanometer powder is 40nm, the particle diameter of the HA nanometer powders<100nm.
The beneficial effects of the invention are as follows：
（1）The powder metallurgy skill that the present invention is combined by " high-energy ball milling-routine molding-vacuum non-pressure sintering twice "
Art, obtain two kinds of face distributed components TNZS metal alkyl materials, for titanium provide it is a kind of can industrialized production system
Preparation Method.
（2）5wt.%TiO prepared by the present invention2The modulus of elasticity of/TNZS and 5wt.%HA/TNZS titanium base materials is respectively
103.93 GPa and 119.43 GPa, compare TNZS（64.00GPa）62.39% and 86.61% has been respectively increased.
（3）The present invention is applicable not only to the preparation of TNZS base titanium alloys, applies also for the preparation of various model titaniums.
Brief description of the drawings
Fig. 1 is the XRD analysis spectrum of TNZS mixed-powders.
Fig. 2 is to utilize the 5wt.%TiO obtained by present invention preparation2The XRD analysis spectrum of/TNZS mixed-powders.
Fig. 3 is the XRD analysis spectrum using the 5wt.%HA/TNZS mixed-powders obtained by present invention preparation.
Fig. 4 is to utilize the 5wt.%TiO obtained by present invention preparation2/ TNZS mixed-powders, 5wt.%HA/TNZS mixed-powders
With the SEM surface topographies of TNZS mixed-powders.
Fig. 5 is the XRD analysis spectrum of TNZS titanium base materials.
Fig. 6 is to utilize the 5wt.%TiO obtained by present invention preparation2The XRD analysis spectrum of/TNZS titanium base materials.
Fig. 7 is the XRD analysis spectrum using the 5wt.%HA/TNZS titanium base materials obtained by present invention preparation.
Fig. 8 is to utilize the 5wt.%TiO obtained by present invention preparation2/ TNZS titanium base materials, 5wt.%HA/TNZS titanium base materials
With the SEM surface topographies of TNZS titanium base materials.
Fig. 9 is to utilize the 5wt.%TiO obtained by present invention preparation2/ TNZS titanium base materials, 5wt.%HA/TNZS titanium base materials
With the springform spirogram of TNZS titanium base materials.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention will be further described.
Embodiment 1
A kind of preparation method of high elastic modulus 5wt.%TiO2/TNZS titanium base materials, comprises the following steps：
1st, twice prepared by high-energy ball milling mixed-powder：First prepare Ti-24Nb-4Zr-7.9Sn（TNZS）Mixed-powder, each group
The mass percent divided is respectively Ti powder：64.1%, Nb powder:24 %, Zr powder:4 %, Sn powder：7.9%, through first time high energy ball
Mill（Planetary ball mill, ratio of grinding media to material 10:1,300r/min ball milling 48h, ball milling 1h shut down 15min）Afterwards, TiO is added2Nano powder
End（Granularity 40nm）, prepare containing the TiO that mass fraction is 5%2/ TNZS mixed-powders, continue high-energy ball milling（300r/min balls
Grind 1h）, it is placed in drying in vacuum drying chamber, sieving.
2nd, the method for conventional molding processing：The YB32- that mixed-powder prepared by step 1 is manufactured in Nantong forging equipment factory
100 hydraulic presses are pressed（Pressing pressure is 18Mpa, the min of pressurize 5）, produce required briquetting（A diameter of 30mm, thickness
For 10 mm）.
3rd, vacuum non-pressure sintering is handled：The compressing briquetting of step 2 is placed on WZS-20 type two-chamber vacuum sintering furnaces
Carry out pressureless sintering；Wherein vacuum 7.8 10-1Pa, 10 DEG C/min of heating rate, sintering process are first pre-burning to 600 DEG C of guarantors
2 h of temperature, are warming up to 800 DEG C of insulation 2h, then are warming up to 1000 DEG C of insulation 2h, are finally warming up to 1250 DEG C of insulation 2h, with
Furnace cooling afterwards.
5wt.%TiO is obtained using above-mentioned steps2Removed in the XRD spectrums of/TNZS mixed-powders and detect Srilankite
TiO2Presence, also Rutile TiO2With Anatase TiO2（Fig. 1, shown in 2）；Alloying phenomenon is obvious after ball milling, particle
Shape become comparison rule, without obvious corner angle；Size is obviously reduced, and maximum particle size is no more than 35 μm（Such as Fig. 4 a, b institute
Show）；Using 5wt.%TiO made from the above method2/ TNZS titanium base material things are divided by outside generation α-Ti phases and β-Ti phases, due to adding
Plus 5wt.% TiO2, also detect Rutile Type TiO2And Anatase TiO2(as shown in Figure 5,6)；It is right according to Fig. 8 b patterns
Than TNZS titanium base material tissues（Shown in Fig. 8 a）, TiO2/ TNZS also by with 1,2,3,4 four Qu Wei represent it is greyish black, grey, greyish white,
White four phase composition, phase composition is substantially similar to TNZS, and simply constituent content is otherwise varied；Add 5wt.% TiO2So that TiO2
Compare and be evenly distributed in TiO2In/TNZS agglomerated materials, so that oxygen element content is relatively high in most of region；
As shown in figure 9, compared with TNZS titanium base materials, the modulus of elasticity of 5wt.%TiO2/TNZS titanium base materials is 103.93 GPa, than
TNZS（64.00GPa）Improve 62.39%.
Embodiment 2
A kind of preparation method of high elastic modulus 5wt.%HA/TNZS titanium base materials：
The present embodiment and embodiment 1 are similar, difference be by mass fraction be 5% TiO2Powder replaces with 5wt.%
HA nanometer powders.
5wt.%HA/TNZS mixed-powder mechanical alloyings phenomenon is obtained using above-mentioned steps substantially, the XRD spectrums of powder
In except detecting Srilankite TiO2Presence, also Rutile TiO2 and Anatase TiO2（Fig. 1, shown in 3）；Particle
Occur in that the phenomenon of reunion and cold welding so that the difficult aggravation of powder fining finally tends to the rock-steady structure of ellipsoid；Particle by
Refined to collective effects such as crushing, extruding and mechanical grindings, size is obviously reduced, and maximum particle size is no more than 35 μm（Such as
Shown in Fig. 4 c）；Using in 5wt.%HA/TNZS titanium base materials made from the above method in addition to α-Ti, β-Ti and HA is detected, also
Detect Ti2O、CaTiO3, CaO and TixPyCenotype, and it is because HA non-refractories, at 1000 DEG C that these cenotypes, which can be generated,
Easily decompose and reacted with Ti into (as shown in Fig. 5,7) above；According to Fig. 8 c shape appearance figures, TNZS titanium base material groups are contrasted
Knit（Shown in Fig. 8 a）, 5wt.%HA/TNZS tissue and 5%TiO2/ TNZS is substantially similar, and simply surface distributed has more uniform contain
The small white spots tissue of calcium phosphorous compound composition；As shown in figure 9, compared with TNZS titanium base materials, 5wt.%HA/TNZS titanium-based materials
The modulus of elasticity of material is 119.43 GPa, compares TNZS（64.00GPa）Improve 86.61%.
Part that the present invention does not relate to is same as the prior art or can be realized using prior art.
Claims (9)
1. based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle, it is characterized in that entering according to following steps
OK：
(1) twice prepared by high-energy ball milling mixed-powder：Ti-24Nb-4Zr-7.9Sn mixed-powders are first prepared by composition, through first
After secondary high-energy ball milling, TiO is added2Nanometer powder, TiO2Nanometer powder accounts for addition TiO2Ti-24Nb-4Zr- after nanometer powder
After the 5% of 7.9Sn mixed-powder quality, second of high-energy ball milling, drying in vacuum drying chamber, sieving are placed in；
(2) method of conventional molding processing：Mixed-powder prepared by step 1 is pressed, and obtains briquetting；
(3) vacuum non-pressure sintering is handled：The compressing briquetting of step 2 is subjected to vacuum non-pressure sintering.
2. based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle, it is characterized in that entering according to following steps
OK：
1st, twice prepared by high-energy ball milling mixed-powder：Ti-24Nb-4Zr-7.9Sn mixed-powders are first prepared by composition, through for the first time
After high-energy ball milling, HA nanometer powders are added, HA nanometer powders account for the Ti-24Nb-4Zr-7.9Sn added after HA nanometer powders and mixed
Close after the 5% of powder quality, second of high-energy ball milling, be placed in drying in vacuum drying chamber, sieving；
2nd, the method for conventional molding processing：Mixed-powder prepared by step 1 is pressed, and obtains briquetting；
3rd, vacuum non-pressure sintering is handled：The compressing briquetting of step 2 is subjected to vacuum non-pressure sintering.
3. as claimed in claim 1 or 2 be combined the method for preparing high elastic modulus Ti sills based on nano-ceramic particle, its
It is characterized in：Ti-24Nb-4Zr-7.9Sn, its component is calculated by percentage to the quality, respectively Ti powder：64.1%, Nb powder:24%,
Zr powder:4%, Sn powder：7.9%.
4. as claimed in claim 1 or 2 be combined the method for preparing high elastic modulus Ti sills based on nano-ceramic particle, its
It is characterized in：The ball-milling technology of first time high-energy ball milling is：Planetary ball mill, ratio of grinding media to material 10:1,300r/min ball milling 48h, ball milling
1h shuts down 15min.
5. as claimed in claim 1 or 2 be combined the method for preparing high elastic modulus Ti sills based on nano-ceramic particle, its
It is characterized in：The ball-milling technology of second of high-energy ball milling is：300r/min ball millings 1h.
6. as claimed in claim 1 or 2 be combined the method for preparing high elastic modulus Ti sills based on nano-ceramic particle, its
It is characterized in：Compressing technique is：Pressing pressure is 18MPa, pressurize 5min, produces required briquetting, a diameter of 30mm of briquetting,
Thickness is 10mm.
7. as claimed in claim 1 or 2 be combined the method for preparing high elastic modulus Ti sills based on nano-ceramic particle, its
It is characterized in：The technique of vacuum non-pressure sintering is：Vacuum 7.8 10-1Pa, 10 DEG C/min of heating rate, first pre-burning to 600 DEG C of guarantors
Warm 2h, be warming up to 800 DEG C insulation 2h, then be warming up to 1000 DEG C insulation 2h, be finally warming up to 1250 DEG C insulation 2h, after it is cold with stove
But.
8. as claimed in claim 1 based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle, it is special
Levying is：The TiO2The particle diameter of nanometer powder is 40nm.
9. as claimed in claim 2 based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle, it is special
Levying is：The particle diameter of the HA nanometer powders<100nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510723476.2A CN105274375B (en) | 2015-10-29 | 2015-10-29 | Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510723476.2A CN105274375B (en) | 2015-10-29 | 2015-10-29 | Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105274375A CN105274375A (en) | 2016-01-27 |
| CN105274375B true CN105274375B (en) | 2017-10-27 |
Family
ID=55144195
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510723476.2A Active CN105274375B (en) | 2015-10-29 | 2015-10-29 | Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105274375B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN108611528B (en) * | 2018-05-09 | 2020-06-23 | 西南交通大学 | Graphene reinforced titanium-based/nano HA composite material and preparation method thereof |
| 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 |
| 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 |
| 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 |
| 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 |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7625520B2 (en) * | 2003-11-18 | 2009-12-01 | Dwa Technologies, Inc. | Manufacturing method for high yield rate of metal matrix composite sheet production |
| CN102618774B (en) * | 2012-04-17 | 2014-03-12 | 江苏大学 | Manufacturing method of metal matrix nanocomposites with high toughness |
-
2015
- 2015-10-29 CN CN201510723476.2A patent/CN105274375B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105274375A (en) | 2016-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105274375B (en) | Based on the compound method for preparing high elastic modulus Ti sills of nano-ceramic particle | |
| CN107829007B (en) | A kind of method that high-entropy alloy and powder metallurgic method prepare high-entropy alloy block | |
| CN105499576B (en) | A kind of method that powder metallurgy prepares porous titanium-aluminium alloy | |
| CN102717086B (en) | Method for preparing high-niobium titanium-aluminum alloy spherical micro powder in short process | |
| CN102618774B (en) | Manufacturing method of metal matrix nanocomposites with high toughness | |
| CN105950944B (en) | A kind of high-melting-point high-entropy alloy NbMoTaWVTi and preparation method thereof | |
| CN103130506A (en) | Method for preparing superfine titanium carbonitride | |
| CN105127436B (en) | A kind of vacuum induction melting aerosolization preparation method of titanium or titanium alloy spherical powder | |
| CN103361532B (en) | Sosoloid toughened metal ceramic and preparation method thereof | |
| CN107475547A (en) | A kind of preparation method of double yardstick titanium alloy materials | |
| CN106119604B (en) | A kind of Y2O3Ti 8Si 1.4Zr alloys of alloying and preparation method thereof | |
| CN109868404A (en) | A kind of hard alloy axle sleeve and preparation method thereof | |
| CN109881072A (en) | A kind of hard alloy seal ring and preparation method thereof | |
| CN106244852B (en) | A kind of Ti 8Si alloys of Zr alloyings and preparation method thereof | |
| CN106756599A (en) | The preparation method of cBN High Speed Steel Composites and cBN High Speed Steel Composites | |
| CN103553619A (en) | Titanium carbide and vanadium carbide composite material as well as production method and application thereof | |
| CN104451217A (en) | Preparation method of ultrafine cemented carbide | |
| CN104493155A (en) | Manufacturing method of CuSn10 alloy bronze powder | |
| CN105463249B (en) | A kind of high-strength low mould medical beta Ti alloy materials and preparation method thereof | |
| CN107746280A (en) | A kind of high-compactness TiB2The preparation method of ceramic target | |
| CN107520441A (en) | A kind of powder metallurgical gear material of anti-pressure and abrasion-proof and preparation method thereof | |
| CN104162678B (en) | A kind of method utilizing intercrystalline corrosion to prepare high-compressibility water atomization stainless steel powder | |
| CN103710576B (en) | The high-strength nickel niobium alloy material that a kind of scandium, tantalum strengthen | |
| CN103447545B (en) | Method for preparing iron-based friction material by utilizing vacuum carbothermal in-situ reactive sintering from vanadium-titanium magnetite | |
| CN105908042B (en) | Nb‑Ti‑Zr‑Nb5Si3Composite and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |