CN109807330A - A method of POROUS TITANIUM is prepared by titanium sesquioxide - Google Patents
A method of POROUS TITANIUM is prepared by titanium sesquioxide Download PDFInfo
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- CN109807330A CN109807330A CN201910159503.6A CN201910159503A CN109807330A CN 109807330 A CN109807330 A CN 109807330A CN 201910159503 A CN201910159503 A CN 201910159503A CN 109807330 A CN109807330 A CN 109807330A
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- titanium
- porous
- porous titanium
- preform
- sesquioxide
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- 239000010936 titanium Substances 0.000 title claims abstract description 89
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 76
- GQUJEMVIKWQAEH-UHFFFAOYSA-N titanium(III) oxide Chemical compound O=[Ti]O[Ti]=O GQUJEMVIKWQAEH-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000001110 calcium chloride Substances 0.000 claims abstract description 27
- 239000007787 solid Substances 0.000 claims abstract description 21
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 20
- 239000011812 mixed powder Substances 0.000 claims abstract description 14
- 238000005245 sintering Methods 0.000 claims abstract description 14
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 9
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000009702 powder compression Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 5
- 235000021110 pickles Nutrition 0.000 abstract description 5
- 229910009973 Ti2O3 Inorganic materials 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 5
- 210000000988 bone and bone Anatomy 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007943 implant Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 208000020442 loss of weight Diseases 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 210000000963 osteoblast Anatomy 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- Powder Metallurgy (AREA)
Abstract
The present invention relates to a kind of methods by titanium sesquioxide preparation POROUS TITANIUM, belong to POROUS TITANIUM preparation technical field.The present invention is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；By Ti2O3/CaCl2Mixed powder compression moulding obtains preform；Preform is placed in 30 ~ 120min of sintering under the conditions of vacuum or argon atmosphere, temperature are 850 ~ 1000 DEG C and obtains porous presoma；It is 10 in pressure‑1Under the conditions of ~ 10Pa, temperature are 900 ~ 1200 DEG C, porous 4 ~ 12h of presoma is restored using calcium steam；30 ~ 240min of reduzate is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and pickle liquor；Solid A is alternately washed with deionized water and dehydrated alcohol, then vacuum drying obtains flake porous titanium；By flake porous titanium be placed in temperature be 1200 ~ 1400 DEG C at 2 ~ 4h of vacuum-sintering up to POROUS TITANIUM.There are two types of pore-size distributions, the respectively micropore of 4 ~ 15 μm of the macropore in 50 ~ 200 μm of aperture and aperture for the POROUS TITANIUM tool of the method for the present invention preparation.
Description
Technical field
The present invention relates to a kind of methods by titanium sesquioxide preparation POROUS TITANIUM, belong to POROUS TITANIUM preparation technical field.
Background technique
Porous metal material is in addition to common metal attribute, because having this feature of a large amount of gaps, in equipment loss of weight, inhales
The fields such as energy damping, chemical industry catalysis, heat-insulated heat exchange, noise elimination noise reduction show excellent performance.Porous metals titanium be Titanium with
The composite material of gas also has good biocompatibility, high specific strength, bullet not only with the characteristic of common porous metal
Property modulus can reconcile the excellent properties such as good corrosion resistance, therefore in environmental protection, aerospace, nuclear industry, biomedicine and chemical industry catalysis etc.
Field has huge application prospect.Especially in field of biomedicine, the formation of POROUS TITANIUM hole increases bone and planting body
Contact area can substantially reduce the compression that bone is born on unit area, weaken or eliminate stress barrier effect；Porous structure
Adherency, the differentiation and growth for being conducive to osteoblast promote Bone Ingrowth hole, reinforce the connection of implant and bone, while advantageous
In the transmission of moisture and nutriment.In addition, good hole and huge specific surface area are also admirably suitable for chemical industry catalysis and petroleum
Crack industry demand, therefore porous titanium material preparation and application more and more attention has been paid to.
The method for preparing POROUS TITANIUM both at home and abroad at present, which is substantially all, uses titanium valve for raw material, and wherein titanium powder sintering process is mesh
Preceding most study and most mature preparation POROUS TITANIUM method realize the Kong Te such as different porosities and different pore size by placeholder
Sign, but the POROUS TITANIUM prepared at present is difficult into bulk because the intergranular bonding strength of titanium is low.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of method by titanium sesquioxide preparation POROUS TITANIUM, this
Invention is realized as titanium source using the reduction of calcium steam and vacuum-sintering using titanium sesquioxide prepares POROUS TITANIUM by titanium sesquioxide.
A method of POROUS TITANIUM is prepared by titanium sesquioxide, the specific steps are as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；
(3) preform of step (2) is placed in vacuum or argon atmosphere, sintering 30 under the conditions of temperature is 850 ~ 1000 DEG C ~
120min obtains porous presoma；
It (4) is 10 in pressure-1~ 10Pa, temperature be 900 ~ 1200 DEG C under the conditions of, using calcium steam reduction step (3) it is porous before
Drive 4 ~ 12h of body；
(5) 30 ~ 240min of reduzate of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and acidleach
Liquid；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1200 ~ 1400 DEG C at 2 ~ 4h of vacuum-sintering up to POROUS TITANIUM；
The mass ratio of titanium sesquioxide powder and calcium chloride is (4 ~ 6) in the step (1): 1；
The pressure of compression moulding is 2 ~ 10Mpa in the step (2), and the shape of preform is cylindrical block or spherical shape；
Step (3) vacuum degree is not higher than 20Pa；
The concentration of dilute hydrochloric acid solution is not higher than 4% in the step (5).
The beneficial effects of the present invention are:
(1) present invention is realized using the reduction of calcium steam and vacuum-sintering directly by titanium sesquioxide system using titanium sesquioxide as titanium source
Standby POROUS TITANIUM；
(2) POROUS TITANIUM prepared by the present invention, pore structure are derived from Ti2O3The removing of oxygen and addition of C aCl in structure2Wave
Hair, makes it have two kinds of pore size distributions, the respectively micropore of 4 ~ 15 μm of the macropore in 50 ~ 200 μm of aperture and aperture, can meet multiple dimensioned
The demand in hole.
Detailed description of the invention
Fig. 1 is the SEM figure of the flake porous titanium of embodiment 1；
Fig. 2 is the EDS figure of the flake porous titanium of embodiment 1；
Fig. 3 is the SEM figure of the flake porous titanium of embodiment 2；
Fig. 4 is the SEM figure of the flake porous titanium of embodiment 3；
Fig. 5 is the SEM comparison diagram of the flake porous titanium of embodiment 4 and POROUS TITANIUM, and wherein a is that the SEM of flake porous titanium schemes, and b is more
The SEM of hole titanium schemes.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1: a method of POROUS TITANIUM is prepared by titanium sesquioxide, the specific steps are as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；Wherein titanium sesquioxide powder
The mass ratio of end and calcium chloride is 6:1；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；Wherein preform with a thickness of
5mm；Wherein the pressure of compression moulding is 4Mpa, and the diameter of preform is 10mm, and the shape of preform is cylindrical block；
(3) preform of step (2) is placed in vacuum, temperature is sintered 30min under the conditions of being 850 DEG C and obtains porous presoma；
Wherein vacuum degree is 15Pa；
(4) under the conditions of pressure is 9Pa, temperature is 1000 DEG C, using the porous presoma 6h of calcium steam reduction step (3)；
(5) the reduzate 120min of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and pickle liquor；Its
The concentration of middle dilute hydrochloric acid solution is 3.7%；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1300 DEG C at vacuum-sintering 3h up to POROUS TITANIUM；Wherein vacuum degree
It is 10-3Pa；
The SEM of the flake porous titanium of the present embodiment scheme as shown in Figure 1, the flake porous titanium of the present embodiment EDS figure as shown in Fig. 2, from
Fig. 1 and Fig. 2 is it is found that ingredient is Titanium, and titanium particle is skeleton in microstructure, is coupled between Titanium particle, growth is constituted
Porous structure.
Embodiment 2: a method of POROUS TITANIUM is prepared by titanium sesquioxide, the specific steps are as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；Wherein titanium sesquioxide powder
The mass ratio of end and calcium chloride is 4:1；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；Wherein preform with a thickness of
8mm；Wherein the pressure of compression moulding is 2Mpa, and the diameter of preform is 10mm, and the shape of preform is cylindrical block；
(3) preform of step (2) is placed in argon atmosphere, temperature is sintered 60min under the conditions of being 900 DEG C and obtains porous forerunner
Body；
It (4) is 10 in pressure-1Under the conditions of Pa, temperature are 1000 DEG C, using the porous presoma 6h of calcium steam reduction step (3)；
(5) the reduzate 180min of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and pickle liquor；Its
The concentration of middle dilute hydrochloric acid solution is 3%；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1350 DEG C at vacuum-sintering 2.5h up to POROUS TITANIUM；Wherein vacuum
Degree is 10-2Pa；
The SEM of the flake porous titanium of the present embodiment schemes as shown in figure 3, as can be seen from Figure 3, there are two types of pore size distributions for POROUS TITANIUM tool, respectively
The micropore of 3 ~ 10 μm of the macropore and aperture that 80 ~ 200 μm of aperture.
Embodiment 3: a method of POROUS TITANIUM is prepared by titanium sesquioxide, the specific steps are as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；Wherein titanium sesquioxide powder
The mass ratio of end and calcium chloride is 5:1；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；Wherein preform with a thickness of
6mm；Wherein the pressure of compression moulding is 4Mpa, and the diameter of preform is 15mm, and the shape of preform is cylindrical block；
(3) by the preform of step (2) be placed in argon atmosphere, temperature be 1000 DEG C under the conditions of sintering 120min obtain it is porous before
Drive body；
(4) under the conditions of pressure is 5Pa, temperature is 900 DEG C, using the porous presoma 12h of calcium steam reduction step (3)；
(5) the reduzate 120min of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and pickle liquor；Its
The concentration of middle dilute hydrochloric acid solution is 3%；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1200 DEG C at vacuum-sintering 3h up to POROUS TITANIUM；Wherein vacuum degree
It is 10-3Pa；
The SEM of the flake porous titanium of the present embodiment schemes as shown in figure 4, as can be seen from Figure 4, there are two types of pore size distributions for POROUS TITANIUM tool, respectively
The micropore that the macropore and aperture that 50 ~ 150 μm of aperture are 2 ~ 10 μm.
Embodiment 4: a method of POROUS TITANIUM is prepared by titanium sesquioxide, the specific steps are as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；Wherein titanium sesquioxide powder
The mass ratio of end and calcium chloride is 4:1；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；Wherein preform with a thickness of
5mm；Wherein the pressure of compression moulding is 10Mpa, and the diameter of preform is 15mm, and the shape of preform is cylindrical block
Body；
(3) preform of step (2) is placed in vacuum, temperature is sintered 90min under the conditions of being 950 DEG C and obtains porous presoma；
Wherein vacuum degree is 10Pa；
(4) under the conditions of pressure is 2Pa, temperature is 1000 DEG C, using the porous presoma 8h of calcium steam reduction step (3)；
(5) the reduzate 120min of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and pickle liquor；Its
The concentration of middle dilute hydrochloric acid solution is 3%；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1400 DEG C at vacuum-sintering 2h up to POROUS TITANIUM；Wherein vacuum degree
It is 10-3Pa；
The SEM comparison diagram of the flake porous titanium of the present embodiment and POROUS TITANIUM, wherein a is that the SEM of flake porous titanium schemes, and b is POROUS TITANIUM
SEM figure, as can be seen from Figure 5, POROUS TITANIUM tool is there are two types of pore size distribution, respectively 6 ~ 15 μm of the macropore in 50 ~ 150 μm of aperture and aperture
Micropore.
It is that the embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment party above
Formula can also be made without departing from the purpose of the present invention within the knowledge of a person skilled in the art
Various change out.
Claims (5)
1. a kind of method by titanium sesquioxide preparation POROUS TITANIUM, which is characterized in that specific step is as follows:
(1) it is uniformly mixed titanium sesquioxide powder to obtain Ti with calcium chloride2O3/CaCl2Mixed powder；
(2) by the Ti of step (1)2O3/CaCl2Mixed powder compression moulding obtains preform；
(3) preform of step (2) is placed in vacuum or argon atmosphere, sintering 30 under the conditions of temperature is 850 ~ 1000 DEG C ~
120min obtains porous presoma；
It (4) is 10 in pressure-1~ 10Pa, temperature be 900 ~ 1200 DEG C under the conditions of, using calcium steam reduction step (3) it is porous before
Drive 4 ~ 12h of body；
(5) 30 ~ 240min of reduzate of step (4) is embathed using dilute hydrochloric acid solution, separation of solid and liquid obtains solid A and acidleach
Liquid；
(6) using the solid A of deionized water and dehydrated alcohol alternating washing step (5), then vacuum drying is obtained flake porous
Titanium；
(7) by the flake porous titanium of step (6) be placed in temperature be 1200 ~ 1400 DEG C at 2 ~ 4h of vacuum-sintering up to POROUS TITANIUM.
2. according to claim 1 by the method for titanium sesquioxide preparation POROUS TITANIUM, it is characterised in that: three oxygen in step (1)
The mass ratio for changing two titanium powders and calcium chloride is (4 ~ 6): 1.
3. according to claim 1 by the method for titanium sesquioxide preparation POROUS TITANIUM, it is characterised in that: compacting in step (2)
Molding pressure is 2 ~ 10Mpa, and the shape of preform is cylindrical block or spherical shape.
4. according to claim 1 by the method for titanium sesquioxide preparation POROUS TITANIUM, it is characterised in that: step (3) system is residual
Pressure is not higher than 20Pa.
5. according to claim 1 by the method for titanium sesquioxide preparation POROUS TITANIUM, it is characterised in that: dilute salt in step (5)
The concentration of acid solution is not higher than 4%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111230128A (en) * | 2020-03-11 | 2020-06-05 | 昆明理工大学 | Based on TiH2Method for preparing porous titanium and titanium alloy by adding CaO |
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| CN104131195A (en) * | 2014-08-14 | 2014-11-05 | 昆明理工大学 | Preparation method of biomedical porous titanium |
| CN104212993A (en) * | 2014-07-24 | 2014-12-17 | 昆明理工大学 | Preparation method of porous titanium alloy material |
| CN105200260A (en) * | 2015-08-18 | 2015-12-30 | 昆明理工大学 | Method for preparing porous titanium in in-situ reduction mode from titanium dioxide |
| CN105274361A (en) * | 2015-08-18 | 2016-01-27 | 昆明理工大学 | Method for preparing porous titanium through calcium thermal reduction of titanium dioxide |
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2019
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Patent Citations (5)
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|---|---|---|---|---|
| JP4871406B1 (en) * | 2010-08-06 | 2012-02-08 | 田中貴金属工業株式会社 | Magnetron sputtering target and method for manufacturing the same |
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| CN104131195A (en) * | 2014-08-14 | 2014-11-05 | 昆明理工大学 | Preparation method of biomedical porous titanium |
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