CN108624782A - A method of preparing biological titanium alloy - Google Patents
A method of preparing biological titanium alloy Download PDFInfo
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- CN108624782A CN108624782A CN201710178053.6A CN201710178053A CN108624782A CN 108624782 A CN108624782 A CN 108624782A CN 201710178053 A CN201710178053 A CN 201710178053A CN 108624782 A CN108624782 A CN 108624782A
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- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 74
- 238000000034 method Methods 0.000 title claims abstract description 37
- 229910052751 metal Inorganic materials 0.000 claims abstract description 111
- 239000011575 calcium Substances 0.000 claims abstract description 41
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 41
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 39
- 230000009467 reduction Effects 0.000 claims abstract description 39
- 239000010936 titanium Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims description 113
- 239000000203 mixture Substances 0.000 claims description 105
- 239000000463 material Substances 0.000 claims description 87
- 239000002184 metal Substances 0.000 claims description 82
- 238000006722 reduction reaction Methods 0.000 claims description 54
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 49
- 239000003795 chemical substances by application Substances 0.000 claims description 37
- 239000012298 atmosphere Substances 0.000 claims description 35
- 239000000292 calcium oxide Substances 0.000 claims description 30
- 239000007789 gas Substances 0.000 claims description 30
- 238000000498 ball milling Methods 0.000 claims description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 19
- 239000001110 calcium chloride Substances 0.000 claims description 19
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 19
- 239000000126 substance Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 150000002739 metals Chemical class 0.000 claims description 12
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 11
- 239000011261 inert gas Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011812 mixed powder Substances 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 238000004886 process control Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 32
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052791 calcium Inorganic materials 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 50
- 229910052786 argon Inorganic materials 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 17
- 229910045601 alloy Inorganic materials 0.000 description 15
- 239000000956 alloy Substances 0.000 description 15
- 235000019580 granularity Nutrition 0.000 description 14
- 238000001035 drying Methods 0.000 description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 8
- 238000005275 alloying Methods 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 235000013339 cereals Nutrition 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- -1 isopropyl alcohols Chemical class 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 229910001092 metal group alloy Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- CSDQQAQKBAQLLE-UHFFFAOYSA-N 4-(4-chlorophenyl)-4,5,6,7-tetrahydrothieno[3,2-c]pyridine Chemical compound C1=CC(Cl)=CC=C1C1C(C=CS2)=C2CCN1 CSDQQAQKBAQLLE-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910003074 TiCl4 Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 229960000074 biopharmaceutical Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000010485 coping Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 208000005368 osteomalacia Diseases 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002927 oxygen compounds Chemical class 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
- 238000004876 x-ray fluorescence Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of method preparing biological titanium alloy, and the biological titanium alloy includes Ti and other metallic elements in addition to Ti, is to restore TiO by using Ca2It is obtained with the hopcalite of the metallic element.The present invention prepares biological titanium alloy by the way that using metal oxide as raw material, calcium is reducing agent, using solid state reduction method, significantly reduces energy consumption and production cost, improves production efficiency, is advantageously implemented industrialized production.
Description
Technical field
The invention belongs to titanium alloy technical fields, relate in particular to a kind of preparation method of biologic medical titanium alloy.
Background technology
It is main at present to be planted for human body although titanium alloy has been obtained for being widely applied in biomedical sector
Enter the material C P Ti of body（Industrially pure titanium alloy）And Ti-6Al-4V（Titanium -6wt% aluminium -4wt% vanadium）It is not ideal biology
Medical material because above-mentioned material in human body may be by tissue corrosion, and releases V and Al, to cause nerveous system
System damage or osteomalacia.In recent years many studies have shown that be added to the alloying element Ta with good biological compatibility,
The titanium alloy of the formation such as Nb, Zr, Mo, Sn is the new bio medical material for substituting above-mentioned conventional titanium alloy.This kind of titanium alloy with
The conventional titanium alloys such as Ti-6Al-4V compare the lower Young's modulus having and excellent bio-compatibility.
Currently, main using the titanium ingot for producing traditional Kroll methods and required various metal alloys member both at home and abroad
Vacuum melting produces titanium alloy to element together, and wherein Kroll methods are with TiCl4For raw material, reducing agent is made using magnesium, high temperature also
To TiCl in former reacting furnace4It carries out long-time reduction and obtains titanium.When the method for further using vacuum melting produces titanium
When alloy, due to differing greatly between metal simple-substance fusing point（Such as the fusing point of metal Mo is 2623 DEG C, the fusing point of metal Ta is
3290 DEG C, and the fusing point of metal Ti is 1670 DEG C）, it is difficult by certain alloying elements when causing using above method production titanium alloy
It is added in titanium alloy to titanium alloy of the production with complicated ingredient, and the alloying element usually added is very expensive, leads
Cause production cost higher；In addition, the volatilization of metal is very serious in Vacuum Melting, the additional consumption of metal is caused, and
Using this method produce titanium alloy energy consumption is larger, environmental pollution is serious and less efficient, be unfavorable for realizing industrialized production.
Therefore, how urgently to be solved as this field using low energy consumption, low cost, efficient method production biological titanium alloy
Project certainly.
Invention content
In view of the above-mentioned problems, the present invention proposes a kind of method preparing biological titanium alloy.The present invention prepares biological titanium and closes
The method of gold is prepared using solid state reduction method by the way that using metal oxide as raw material, calcium is reducing agent, significantly reduces production
Energy consumption and production cost, improve production efficiency, are advantageously implemented industrialized production.
Specifically, present invention employs following technical schemes：
A method of biological titanium alloy is prepared, the biological titanium alloy includes Ti and other metallic elements in addition to Ti,
It is characterized in that, the method includes：Metal oxide mixture and reduction agent composition are prepared first, then by metal oxide
Mixture is mixed to get mixtures of materials with reduction agent composition, then mixtures of materials is put into reacting furnace and carries out reduction reaction
Reducing metal powder is obtained, finally obtained reducing metal powder is cleaned, is dried, titanium alloy powder is obtained, wherein institute
It includes the oxide of contained metallic element or the oxide of part metals element in biological titanium alloy to state metal oxide mixture
With the simple substance of part metals element, reduction agent composition include the Ca powder of amount for being enough reducing metal oxide, CaO powder and
CaCl2The mixture of powder.
Preferably, the preparation of metal oxide mixture include oxide by titanyl compound and other metallic elements or
The mixture ground and mixed of the simple substance of the oxide and part metals element of part metals element, obtains in the other metallic elements of person
Metal oxide mixture powder.Further, ground and mixed include oxide by titanyl compound and other metallic elements or
The mixture of the simple substance of the oxide and part metals element of part metals element presses ratio of grinding media to material 1 in the other metallic elements of person:1 to
10:1 is fitted into ball grinder, with 200~1000 revs/min of rotating speed ball milling 10~30 minutes on centrifugal ball mill, then will
Mixed powder is dry at 90~110 DEG C, obtains metal oxide mixture powder.Further, it is ground on ball mill
When mill, anhydrous isopropyl alcohol is added as process control agent, additive amount is the volume of mixture being added in ball grinder by volume
1~5%.
In a preferred embodiment, the preparation for restoring agent composition includes by Ca powder, CaO powder and CaCl2Powder is mixed,
Obtain reduction agent composition, the grain size of wherein Ca powder is 100 mesh hereinafter, the grain size of CaO powder is 300~800 mesh, CaCl2Powder
Grain size is 300~800 mesh, and the amount of Ca is Ca theoretical chemistries needed for the oxide of reducing metal element in the reduction agent composition
1.2-3 times of metering, the weight of CaO are the 40-50%, CaCl of Ca weight2Weight be CaO weight 1-20%.
Still in a preferred embodiment, metal oxide mixture and restore agent composition mixing include will be golden
Belong to oxide mixture and restore agent composition ball milling mixing 0.5-2 hours under inert gas atmosphere, obtains mixtures of materials.
In another preferred embodiment, it includes that mixtures of materials exists that mixtures of materials carries out reduction reaction in reacting furnace
It is heated to 900-1200 DEG C in reacting furnace and keeps the temperature 30-90 minutes, the metal powder restored.Further, when reduction reaction
Atmosphere in reacting furnace is the non-oxidizing atmosphere comprising inert gas and reducibility gas.
Preferably, mixtures of materials is put into reacting furnace before progress reduction reaction, is in advance pressed into mixtures of materials
20-100 millimeters of diameter, high 20-100 millimeters of lump material.
Additionally preferably, the step of being cleaned and dried to reducing metal powder includes using a concentration of 10-20%vol, temperature
The cleaned and reduced metal powder of acetum that degree is 50-100 DEG C is then adopted to remove Calcium oxide dissolution and washes with water metal powder
End, and be dried under 90-110 DEG C and atmosphere of inert gases, obtain titanium alloy powder.
Compared with the production technology of existing biological titanium alloy, the preparation method of biological titanium alloy of the invention at least has
Following advantages：
One, compared with traditional method production titanium alloy using vacuum melting, the present invention using metal oxide as raw material, make by calcium
Be reducing agent by solid-state synthsis produce titanium alloy, be easier to realize the production of the titanium alloy containing complicated ingredient, avoid due to
Differing greatly between metal simple-substance fusing point causes certain alloying elements to be difficult to be added in titanium alloy, while with each metal alloy
The oxide of ingredient replaces metal simple-substance to produce titanium alloy, significantly reduces production cost；In addition during reduction reaction
Alloying component needed for directly being formed, significantly reduces energy consumption and production cost, also avoids because golden in Vacuum Melting
Belong to the additional consumption that volatilization causes metal；
Two, in titanium alloy production technology of the invention, titanium alloy is produced as reducing agent using the lower calcium metal of price, greatly
Ground reduces production cost（The price of calcium be far below existing common reducing agent magnesium, and about calcium hydride 1/2 to 1/3）；Together
Batch mixing and briquetting technique productions titanium alloy new Shi Caiyong, improves the stability of titanium alloy final product quality, continous way is made to produce
It is possibly realized, further improves production efficiency, be advantageously implemented industrialized production；
Three, the present invention carries out in-situ reducing reaction production titanium using metal oxide as raw material at a temperature of less than melting point metal
Alloy, each production process is pollution-free, and production technology is environmentally protective, and production efficiency is higher.
Description of the drawings
Fig. 1 is the stereoscan photograph of Ti-15Mo alloys prepared by the embodiment of the present invention 1；
Fig. 2 is the stereoscan photograph of Ti-12Mo-6Zr-2Fe alloys prepared by the embodiment of the present invention 2；
Fig. 3 is the stereoscan photograph of Ti-15Mo-5Zr-3Al alloys prepared by the embodiment of the present invention 3；
Fig. 4 is the stereoscan photograph of Ti-25Nb-5Zr-8Sn alloys prepared by the embodiment of the present invention 4；
Fig. 5 is the stereoscan photograph of Ti-34Nb-9Zr-8Ta alloys prepared by the embodiment of the present invention 5.
Specific implementation mode
The biological titanium alloy prepared using the method for the present invention can be used for preparing various medical products, such as can be used for passing through powder
Last metallurgical or superposition manufacture（3D printing）Technology manufactures various biopharmaceutical products, including Artificial Intervention joint or orthopaedics repair member
Part etc..
The method according to the present invention for preparing biological titanium alloy is as follows：
Step a：By the mixture of the oxide and metal simple-substance of the oxide of metallic element in biological titanium alloy or metallic element
It is mixed with reducing agent, obtains mixtures of materials；
Step b：The obtained mixtures of materials of step a is pressed into lump material；
Step c：The obtained lump materials of step b are restored, reducing metal powder is obtained；
Step d：The reducing metal powder that step c is obtained is cleaned, is dried, titanium alloy powder is obtained.
The wherein above-described step a for obtaining mixed material includes the following steps：
Step a1：The oxide of the oxide of metallic element or metallic element is mixed with metal simple-substance, obtains metal oxygen
Compound mixture；
Preferably, in the step a1, using ball-grinding machine by the oxide of the oxide of metallic element or metallic element with gold
Belong to simple substance and carry out ball milling mixing, obtains metal oxide mixture；It is highly preferred that addition anhydrous isopropyl alcohol is carried out as adjuvant
Ball milling mixing, it is further preferred that the volume of the anhydrous isopropyl alcohol is the oxidation of the oxide or metallic element of metallic element
The 1-5% of the mixed volume of object and metal simple-substance, preferably 3%；
It is highly preferred that in the step a1, by the mixed of the oxide and metal simple-substance of the oxide of metallic element or metallic element
It closes object and presses ratio of grinding media to material 1:1 to 10:1, preferably 2:1 is fitted into ball grinder, be added anhydrous isopropyl alcohol, on centrifugal ball mill with
200~1000 revs/min, preferably 600 revs/min of rotating speed ball milling 10~30 minutes, preferably 30 minutes, then by mixed powder
At 90~110 DEG C, it is dried at preferably 100 DEG C, obtains metal oxide mixture；
Step a2：By Ca powder, CaO powder and CaCl2Powder is mixed, and reduction agent composition is obtained；Preferably, the grain of the Ca powder
Diameter is 100 mesh hereinafter, the grain size of CaO powder is 300~800 mesh, CaCl2The grain size of powder is 300~800 mesh, preferably 600 mesh；
1.2-3 times of Ca theoretical stoichiometrics needed for oxide of the amount of Ca for reducing metal element in the reduction agent composition；Institute
The 40-50% for the weight that the weight for stating CaO is Ca, preferably 50%；CaCl2Weight be CaO weight 1-20%, preferably 10%；
Step a3：By obtained metal oxide mixture and restore agent composition ball milling mixing 0.5- under inert gas atmosphere
2 hours, preferably 1 hour, obtain mixtures of materials.
Further, the step b described in above method includes：The mixtures of materials that step a is obtained in 50-200KPa,
It is preferred that being pressed into lump material under 100KPa and inert gas atmosphere；
Preferably, the obtained mixtures of materials of step a is pressed by cylindrical block material using hydraulic press；
Preferably, the size of the cylindrical block material is 20-100 millimeter of diameter, 20-100 millimeters high, and preferably diameter 50 is in the least
Rice, it is 50 millimeters high.
In addition, in step c described in above method, the lump material that step b is obtained is with the rate of 10 DEG C/min
600 DEG C are heated to from room temperature, is then heated to 900-1200 DEG C with the rate of 20 DEG C/min, and keeps the temperature 30-90 minutes, preferably 60
Minute, obtain reducing metal powder；
Preferably, lump material step b obtained carries out reduction reaction in continuous oven；
Preferably, lump material step b obtained is under inert gas and reducibility gas atmosphere, more preferable argon gas and hydrogen
Reduction reaction is carried out under atmosphere, further preferably carries out reduction reaction under 95vol% argon gas+5vol% hydrogen atmospheres.
In the process described above, the step d being cleaned and dried to reducing metal powder includes：Using a concentration of
10-20%vol, temperature are 50-100 DEG C, the cleaned and reduced metal powder of acetum that preferred concentration 20%, temperature are 60 DEG C,
Calcium oxide dissolution to be removed；Then adopt and wash with water metal powder, and under 90-110 DEG C preferably 110 DEG C and argon gas atmosphere into
Row drying, obtains titanium alloy powder.
In preferred embodiments, the preparation method of preferred biological titanium alloy of the invention is as follows.But it answers
Understand, scheme as shown below is only that the purpose illustrated shows preferred or preferably even best side therein
Case, and industry personnel can carry out details adjustment according to the protocol combination actual conditions described in file.Therefore following
Shown in concrete scheme function only as exemplary effect, be construed as limiting without coping with protection scope of the present invention.
Step 1：Raw material mixes
The mixture of the oxide and metal simple-substance of the oxide of metallic element or metallic element is pressed into ratio of grinding media to material 2:1 is packed into ball milling
In tank, 2ml anhydrous isopropyl alcohols are added, it, then will mixing with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill
Powder afterwards is dry at 100 DEG C, obtains metal oxide mixture；Granularity is more than the calcium powder of 5 mesh, more than the oxygen of 400 mesh
Change calcium powder and mixed more than 400 mesh calcium chloride powders, obtain reduction agent composition, the wherein amount of Ca is reducing metal element
1.2-3 times of theoretical stoichiometric needed for oxide, the wherein weight of CaO are the 50% of Ca；CaCl2Weight be CaO 10%；
Metal oxide mixture is fitted into together with reduction agent composition in ball grinder under an argon atmosphere, by ratio of grinding media to material 2:1 is packed into
Ball milling 60 minutes, obtain mixtures of materials in ball grinder.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in continuous reactor below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1100-1200 DEG C, and keep the temperature 60 minutes, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20vol%, temperature is used to be soaked for 60 DEG C of acetum
It steeps and stirs, after replacing acetum three times, metal powder is cleaned with deionized water（Cleaning process in this step can root
It is multiple according to needing to clean, to obtain clean metal powder completely）, then metal powder is dried under 110 DEG C and argon gas atmosphere
It is dry to obtain titanium alloy powder.
The present invention is with TiO2And the oxide of various alloying elements（Including Nb2O5、MoO3、ZrO2、Ta2O5、Al2O3Deng few
It is added in the form of metal powder if measuring metal such as Fe, Sn）For raw material, in-situ reducing is carried out at a temperature of less than melting point metal
Various metal oxide components are reduced into metal phase, and make each metal component by reaction respectively in reduction process using calcium
Phase counterdiffusion is carried out under high temperature action ultimately forms titanium alloy powder.
The present invention produces titanium alloy using metal oxide as raw material, using calcium as reducing agent.Wherein calcium is to be easy to obtain
Alkaline earth metal, reproducibility is higher than magnesium.According to calculation of thermodynamics data, the oxidation reaction of calcium（1）Gibbs it is free
The oxidation reaction of magnesium-yttrium-transition metal can be below at any temperature.
2Ca + O2= 2CaO （1）
Thus it proves, all transition group metallic oxides can be by calcium reduction.Section transitions race gold according to the present invention
It is as follows by the reaction of calcium reduction to belong to oxide：
TiO2+ 2Ca = Ti + 2CaO （2）
MoO3+ 3Ca = Mo + 3CaO （3）
ZrO2+ 2Ca = Zr + 2CaO （4）
Nb2O5+ 5Ca = 2Nb + 5CaO （5）
Ta2O5+ 5Ca = 2Ta + 5CaO （6）
By above-mentioned reaction, each transition group metallic oxide can be reduced to magnesium-yttrium-transition metal simple substance, due to main in alloy
Alloying element is β-Ti stable elements, therefore other alloying elements can form stable β by High temperature diffusion and Ti and consolidate
Solution.
The present invention produces titanium alloy using calcium metal as reducing agent, significantly reduces production cost, improves reduction
Efficiency, basic reaction equation such as formula（2）-（6）It is shown.In addition, calcium oxide and chlorine is further added in the present invention in the reaction
Change calcium production titanium alloy, wherein calcium oxide and calcium chloride are simultaneously not involved in reaction, but respectively as interval dose and fluxing agent, wherein
Calcium oxide is as interval dose for increasing TiO2The distance between particle, to avoid reduction after metallic particles contact with each other and
It sticks together；And calcium chloride is used to increase reducing agent compound mobility during the reaction and increases and exists as fluxing agent
The mobility of the CaO generated in reaction process.Preferably, the weight of the CaO of addition be Ca 40-50%, preferably 50%；It is added
CaCl2Weight be CaO 1-20%, preferably 10%.
Preferably, the present invention is in mixing process（By the oxide of metallic element or the oxide and metal of metallic element
During simple substance is mixed）Isopropanol is added as process control agent（PCA, Process Control Agent）, to change
The uniformity of kind material mixing and the uniformity of each component particle size distribution.
Preferably, it in titanium alloy preparation method of the invention, is gone back again after lump material is pressed into after material is mixed
Original reaction, reason for doing so is that：The reaction that metal oxide is reduced to simple substance is the solid phase reaction of diffusion control, by object
Material is pressed into the diffusion length that the bulk with constant density is conducive between particle and keeps stablizing, and uniform lump material shape
Shape and size are conducive to obtain the repeatability of technique, such as temperature gradient uniformity when heating inside each lump material,
So as to produce uniform alloy powder finished product；Meanwhile material is pressed into the blocky filling for being convenient for material, and block
Shape material is conducive to continuously be transmitted in process of production, to improve production efficiency, is conducive to industrialized production.
The present invention is described below with reference to specific embodiments.It will be appreciated by those skilled in the art that these embodiments are only
For illustrating the present invention, do not limit the scope of the invention in any way.Experimental method in following embodiments, such as without special
Illustrate, is conventional method.Reagent material as used in the following examples etc. is commercially available products unless otherwise specified.
The granularity of all metal oxide powders is more than 400 mesh.
Embodiment 1The preparation of Ti-15Mo alloys
Step 1：Raw material mixes
Weigh 141.7g TiO2With 22.5g MoO3, by ratio of grinding media to material 2:1 is fitted into the ball grinder of 1 liter capacity, and addition 2ml is anhydrous
Isopropanol, with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill, then by mixed powder at 100 DEG C
It is dry, obtain metal oxide mixture；It weighs 321g granularities and is more than 400 mesh calcium oxide more than the calcium powder of 5 mesh, 150g granularities
Powder and 15g, granularity are more than 400 mesh calcium chloride powders, and reduction agent composition is obtained after mixing；Under an argon atmosphere by metal oxide
Mixture is fitted into together with reduction agent composition in ball grinder, by ratio of grinding media to material 2:1, which is fitted into ball milling 60 in the ball grinder of 3 liter capacities, divides
Clock obtains mixtures of materials.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Shape material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in reduction reaction furnace below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1100 DEG C, and keep the temperature 60 minutes at 1100 DEG C, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20vol%, temperature is used to be soaked for 60 DEG C of acetum
It steeps and stirs, after replacing acetum three times, metal powder is cleaned with deionized water, then by metal powder at 110 DEG C
And drying obtains titanium alloy powder under argon gas atmosphere.
The scanning electron microscope of the above-mentioned titanium alloy powder being prepared（SEM）Photo is as shown in Figure 1.
Embodiment 2The preparation of Ti-12Mo-6Zr-2Fe alloys
Step 1：Raw material mixes
Weigh 133.3g TiO2、18.0g MoO3、8.1g ZrO2With 2g straight iron powders, by ratio of grinding media to material 2:1 is packed into the ball of 1 liter capacity
In grinding jar, 2ml anhydrous isopropyl alcohols are added, with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill, then will be mixed
Powder after conjunction is dry at 100 DEG C, obtains metal oxide mixture；Weigh 308g granularities more than 5 mesh calcium powders, 150g
Degree is more than 400 mesh calcium chloride powders more than 400 mesh calcium oxide powders and 15g granularities, and reduction agent composition is obtained after mixing；In argon gas
Metal oxide mixture is fitted into together with reduction agent composition in ball grinder under atmosphere, by ratio of grinding media to material 2:1 is packed into 3 liter capacities
Ball grinder in ball milling 60 minutes, obtain mixtures of materials.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Shape material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in reduction reaction furnace below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1150 DEG C, and keep the temperature 60 minutes at 1150 DEG C, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20%, temperature is used to be impregnated simultaneously for 60 DEG C of acetum
Stirring, after replacing acetum three times, metal powder is cleaned with deionized water, then by metal powder in 110 DEG C and argon
Drying obtains titanium alloy powder under gas atmosphere.
The scanning electron microscope of the above-mentioned titanium alloy powder being prepared（SEM）Photo is as shown in Figure 2.
Embodiment 3The preparation of Ti-15Mo-5Zr-3Al alloys
Step 1：Raw material mixes
Weigh 128.3g TiO2、22.5g MoO3、6.8g ZrO2With 11.3g Al2O3, by ratio of grinding media to material 2:1 is packed into 1 liter capacity
In ball grinder, 2ml anhydrous isopropyl alcohols are added, with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill, then will
Mixed powder is dry at 100 DEG C, obtains metal oxide mixture；Weigh 316g granularities more than 5 mesh calcium powders, 150g
Degree is more than 400 mesh calcium chloride powders more than 400 mesh calcium oxide powders and 15g granularities, and reduction agent composition is obtained after mixing；In argon gas gas
Metal oxide mixture is fitted into together with reduction agent composition in ball grinder under atmosphere, by ratio of grinding media to material 2:1 is packed into 3 liter capacities
Ball milling 60 minutes, obtain mixtures of materials in ball grinder.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Shape material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in reduction reaction furnace below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1180 DEG C, and keep the temperature 60 minutes at 1180 DEG C, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20%, temperature is used to be impregnated simultaneously for 60 DEG C of acetum
Stirring, after replacing acetum three times, metal powder is cleaned with deionized water, then by metal powder in 110 DEG C and argon
Drying obtains titanium alloy powder under gas atmosphere.
The scanning electron microscope of the above-mentioned titanium alloy powder being prepared（SEM）Photo is as shown in Figure 3.
Embodiment 4The preparation of Ti-25Nb-5Zr-8Sn alloys
Step 1：Raw material mixes
Weigh 105.0g TiO2、71.5g Nb2O5、5.4g ZrO2With 8g pure tin powder, by ratio of grinding media to material 2:1 is packed into the ball of 1 liter capacity
In grinding jar, 2ml anhydrous isopropyl alcohols are added, with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill, then will be mixed
Powder after conjunction is dry at 100 DEG C, obtains metal oxide mixture；272g granularities are weighed more than 5 mesh calcium powders, 130g granularities
It is more than 400 mesh calcium chloride powders more than 400 mesh calcium oxide powders and 12g granularities, reduction agent composition is obtained after mixing；In argon gas atmosphere
It is lower to be fitted into metal oxide mixture in ball grinder together with reduction agent composition, by ratio of grinding media to material 2:1 is packed into the ball of 3 liter capacities
Ball milling 60 minutes, obtain mixtures of materials in grinding jar.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Shape material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in reduction reaction furnace below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1150 DEG C, and keep the temperature 60 minutes at 1150 DEG C, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20vol%, temperature is used to be soaked for 60 DEG C of acetum
It steeps and stirs, after replacing acetum three times, metal powder is cleaned with deionized water, then by metal powder at 110 DEG C
And drying obtains titanium alloy powder under argon gas atmosphere.
The scanning electron microscope of the above-mentioned titanium alloy powder being prepared（SEM）Photo is as shown in Figure 4.
Embodiment 5The preparation of Ti-34Nb-9Zr-8Ta alloys
Step 1：Raw material mixes
Weigh 81.7g TiO2、97.2g Nb2O5、12.2g ZrO2With 19.5g Ta2O5, by ratio of grinding media to material 2:1 is packed into 1 liter capacity
In ball grinder, 2ml anhydrous isopropyl alcohols are added, with 600 revs/min of rotating speed ball milling 30 minutes on centrifugal ball mill, then will
Mixed powder is dry at 100 DEG C, obtains metal oxide mixture；Weigh 262g granularities more than 5 mesh calcium powders, 130g
Degree is more than 400 mesh calcium chloride powders more than 400 mesh calcium oxide powders and 15g granularities, and reduction agent composition is obtained after mixing；In argon gas gas
Metal oxide mixture is fitted into together with reduction agent composition in ball grinder under atmosphere, by ratio of grinding media to material 2:1 is packed into 3 liter capacities
Ball milling 60 minutes, obtain mixtures of materials in ball grinder.
Step 2：Briquetting
Mixtures of materials prepared by step 1 is pressed into cylindrical block at 100KPa and the argon gas atmosphere of drying using hydraulic press
Shape material（It is 50 millimeters of diameter, 50 millimeters high）.
Step 3：Reduction
Lump material is placed in the reaction utensil of heat-resisting steel, pad is conveyed into titanium sheet in reduction reaction furnace below, atmosphere in stove
For 95vol% argon gas+5vol% hydrogen；Material is heated to 600 DEG C with the rate of 10 DEG C/min from room temperature, then with 20 DEG C/min
Rate be heated to 1150 DEG C, and keep the temperature 60 minutes at 1150 DEG C, obtain reducing metal powder.
Step 4：Washing
Obtained reducing metal powder is put into descaling bath, a concentration of 20vol%, temperature is used to be soaked for 60 DEG C of acetum
It steeps and stirs, after replacing acetum three times, metal powder is cleaned with deionized water, then by metal powder at 110 DEG C
And drying obtains titanium alloy powder under argon gas atmosphere.
The scanning electron microscope of the above-mentioned titanium alloy powder being prepared（SEM）Photo is as shown in Figure 5.
Composition test
XRF is carried out to titanium alloy prepared by embodiment 1-5（X-ray fluorescence）Analysis, to test the component content in each alloy.Respectively
Component content in alloy is as shown in table 1.
Titanium alloy XRF analysis result prepared by 1 embodiment 1-5 of table
Embodiments of the present invention are described in detail above in conjunction with the drawings and specific embodiments, but above to the present invention
The description of specific implementation mode is not intended to limit the present invention, and those skilled in the art can make various changes or change according to the present invention
Shape should all belong to scope of the appended claims of the present invention without departing from the spirit of the present invention.
Claims (10)
1. a kind of method preparing biological titanium alloy, the biological titanium alloy includes Ti and other metallic elements in addition to Ti,
It is characterized in that, the method includes：Metal oxide mixture and reduction agent composition are prepared first, then aoxidize metal
Object mixture is mixed to get mixtures of materials with reduction agent composition, then mixtures of materials is put into reacting furnace and restore instead
Reducing metal powder should be obtained, finally obtained reducing metal powder is cleaned, is dried, titanium alloy powder is obtained, wherein
The metal oxide mixture includes the oxidation of the oxide or part metals element of contained metallic element in biological titanium alloy
The simple substance of object and part metals element, reduction agent composition include the Ca powder of amount for being enough reducing metal oxide, CaO powder and
CaCl2The mixture of powder.
2. the method as described in claim 1 for preparing biological titanium alloy, which is characterized in that the preparation of metal oxide mixture
It include the oxide of part metals element in oxide or the other metallic elements by titanyl compound and other metallic elements
With the mixture ground and mixed of the simple substance of part metals element, metal oxide mixture powder is obtained.
3. the method as claimed in claim 2 for preparing biological titanium alloy, which is characterized in that ground and mixed includes by the oxidation of titanium
The oxide and part metals element of part metals element in the oxide or other metallic elements of object and other metallic elements
Simple substance mixture press ratio of grinding media to material 1:1 to 10:1 is fitted into ball grinder, with 200~1000 revs/min on centrifugal ball mill
Rotating speed ball milling 10~30 minutes, it is then that mixed powder is dry at 90~110 DEG C, obtain metal oxide mixture
Powder.
4. the method as claimed in claim 3 for preparing biological titanium alloy, which is characterized in that when being ground on ball mill, be added
For anhydrous isopropyl alcohol as process control agent, additive amount is the 1~5% of the volume of mixture being added in ball grinder by volume.
5. the as described in claim 1 method for preparing biological titanium alloy, which is characterized in that the preparation for restoring agent composition includes
By Ca powder, CaO powder and CaCl2Powder is mixed, and reduction agent composition is obtained, and the wherein grain size of Ca powder is 100 mesh hereinafter, CaO
The grain size of powder is 300~800 mesh, CaCl2The grain size of powder is 300~800 mesh, and the amount of Ca is reduction in the reduction agent composition
1.2-3 times of Ca theoretical stoichiometrics needed for the oxide of metallic element, the weight of CaO are the 40-50%, CaCl of Ca weight2's
Weight is the 1-20% of CaO weight.
6. the method as described in claim 1 for preparing biological titanium alloy, which is characterized in that metal oxide mixture and reduction
The mixing of agent composition includes by metal oxide mixture and restoring agent composition ball milling mixing under inert gas atmosphere
0.5-2 hours, obtain mixtures of materials.
7. the as described in claim 1 method for preparing biological titanium alloy, which is characterized in that mixtures of materials in reacting furnace into
Row reduction reaction includes that mixtures of materials is heated to 900-1200 DEG C in reacting furnace and keeps the temperature 30-90 minutes, is restored
Metal powder.
8. the method as claimed in claim 7 for preparing biological titanium alloy, which is characterized in that atmosphere when reduction reaction in reacting furnace
It encloses to include the non-oxidizing atmosphere of inert gas and reducibility gas.
9. the method as described in claim 1 for preparing biological titanium alloy, which is characterized in that mixtures of materials is put into reacting furnace
Before carrying out reduction reaction, mixtures of materials is pressed into 20-100 millimeters of diameter, high 20-100 millimeters of lump material in advance.
10. the method for preparing biological titanium alloy as described in claim 1, which is characterized in that carried out to reducing metal powder clear
It includes using a concentration of 10-20%vol, temperature for the cleaned and reduced metal powder of 50-100 DEG C of acetum to wash dry step
It to remove Calcium oxide dissolution, then adopts and washes with water metal powder, and done under 90-110 DEG C and atmosphere of inert gases
It is dry, obtain titanium alloy powder.
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| CN109290586A (en) * | 2018-10-19 | 2019-02-01 | 重庆大学 | A kind of preparation method of high-purity vanadium powder |
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Application publication date: 20181009 |