CN110524003A - The preparation method of nearly ball-type titanium valve - Google Patents
The preparation method of nearly ball-type titanium valve Download PDFInfo
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- CN110524003A CN110524003A CN201910953844.0A CN201910953844A CN110524003A CN 110524003 A CN110524003 A CN 110524003A CN 201910953844 A CN201910953844 A CN 201910953844A CN 110524003 A CN110524003 A CN 110524003A
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- preparation
- titanium valve
- type titanium
- nearly ball
- titanium
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1277—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using other metals, e.g. Al, Si, Mn
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
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- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a kind of preparation methods of nearly ball-type titanium valve, belong to 3D printing technical field of material.The present invention is to solve the relatively low technical problem of prior art preparation sized spherical titanium powder with high costs, complex process, recovery rate, provides a kind of preparation method of nearly ball-type titanium valve, comprising: be uniformly mixed titanium dioxide with additive, be pressed into prefabricated material；Reduction reaction is carried out in closed reaction vessel, obtains reducing material；Reducing material obtains metallic titanium powder in irregular shape through broken, acidleach, washing and drying；Shape correction is finally carried out in airflow milling, obtains subsphaeroidal titanium valve.For the present invention compared with the conventional preparation techniques of sized spherical titanium powder, equipment requirement is low, and Cheng Benneng is greatly reduced, and prepared titanium valve has the advantages that subsphaeroidal, oxygen content is low etc..
Description
Technical field
The invention belongs to 3D printing technical field of material, and in particular to a kind of preparation method of nearly ball-type titanium valve.
Background technique
Titanium is the indispensable critical material of the national economic development, since its density is small, corrosion-resistant, specific strength is high, biological
The advantages that excellent in compatibility, is widely used in the fields such as aerospace, petrochemical industry, energy source and power, bio-medical.However,
Since the poor processability of titanium, processing cost are high, the low efficiency of the part with complicated structure is manufactured, the application of titanium is significantly limited.3D is beaten
Print technology, which can disposably melt material, is polymerized to type, or the mode successively printed constructs the object of 3D shape, has quick
The advantages that molding, Yi Shixian personalized customization, required powder should have the features such as low good fluidity, oxygen content, Song Bigao, therefore
The generally spherical titanium valve of 3D printing titanium article raw material.
Currently, sized spherical titanium powder mainly uses inert gas atomizer, plasma rotating electrode atomization and the atomization of plasma fuse
The methods of be made, equipment cost needed for these techniques is expensive, and the recovery rate of fine grain titanium valve (≤45 μm) is generally relatively low, causes
Titanium valve product price is extremely expensive, therefore develops a kind of simple process, low cost, and titanium valve quality and mobile performance meet 3D and beat
Print technique require technology become there is an urgent need to.
Summary of the invention
The technical problem to be solved by the present invention is to prior art preparation sized spherical titanium powders with high costs, complex process, recovery rate
It is relatively low.
The technical proposal adopted by the invention to solve the above technical problems is that providing a kind of preparation side of nearly ball-type titanium valve
Method comprising following steps:
A, titanium dioxide is uniformly mixed with additive, is pressed into prefabricated material；
B, in closed reaction vessel, metallic reducing agent is placed in reactor lower part, prefabricated material is placed on reactor
Portion, centre are separated using partition, reduction reaction are carried out under inert gas shielding, obtains reducing material；
C, reducing material is crushed under inert gas protection, then carries out acidleach, then washed, dry, obtains shape and do not advise
Metallic titanium powder then；
D, metallic titanium powder in irregular shape is subjected in airflow milling Shape correction, obtains subsphaeroidal titanium valve.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step A, the quality of the titanium dioxide and additive
Than for 4~2:1.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step A, the additive is CaCl2Or MgCl2。
Wherein, the preparation method of nearly ball-type titanium valve described above, in step A, the pressure of the compacting be 0.1MPa~
5MPa, the quality of single prefabricated material are 5g~60g.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step B, the metallic reducing agent be metal K, Ca,
At least one of Na or Mg；The dosage of the metallic reducing agent is the 120%~200% of titanium dioxide quality.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step B, the temperature of the reduction reaction is 900~
1100 DEG C, the time is 4~7h.
Wherein, the preparation method of nearly ball-type titanium valve described above, it is described broken are as follows: to be crushed to granularity and be less than in step C
80 μm of accountings are greater than 98%.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step C, the acidleach are as follows: use mass concentration
3%~5% dilute hydrochloric acid leach, leach liquid-solid ratio >=20mL:1g, 20~30 DEG C of extraction temperature, 10~15min of extraction time.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step C, the washing are as follows: be first washed with water 2~3
It is secondary, then with alcohol rinse 1~2 time.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step C, the drying are as follows: 60~70 DEG C of vacuum are dry
Dry 8h~12h.
Wherein, the preparation method of nearly ball-type titanium valve described above, in step D, the airflow milling is using argon gas as grinding
Gas is ground, it is in 120 ° of modes that two nozzles, which are arranged, in 180 ° or three nozzles in airflow milling, and grinding air pressure is 0.1~1MPa, is ground
Time consuming is 3~10min.
Beneficial effects of the present invention:
The present invention is lower relative to costs of material such as titanium sponge, titanium alloys using titanium dioxide as raw material, with CaCl2、MgCl2Deng
Chloride is additive, not only contributes to fine grain titanium valve and is formed, while being conducive to sequential reduction reaction, then with K, Ca, Na
Or the metals such as Mg are reducing agent, keep raw material reaction more complete；Compared with prior art, equipment requirement is low for the method for the present invention, cost
It can be greatly reduced, prepared titanium valve has the advantages that subsphaeroidal, oxygen content is low etc..
Detailed description of the invention
Fig. 1 is the stereoscan photograph of the subsphaeroidal powder of the present invention.
Specific embodiment
Specifically, the preparation method of nearly ball-type titanium valve comprising following steps:
A, titanium dioxide is uniformly mixed with additive, is pressed into prefabricated material；
B, in closed reaction vessel, metallic reducing agent is placed in reactor lower part, prefabricated material is placed on reactor
Portion, centre are separated using partition, reduction reaction are carried out under inert gas shielding, obtains reducing material；
C, reducing material is crushed under inert gas protection, then carries out acidleach, then washed, dry, obtains shape and do not advise
Metallic titanium powder then；
D, metallic titanium powder in irregular shape is subjected in airflow milling Shape correction, obtains subsphaeroidal titanium valve.
In the present invention, using CaCl2、MgCl2Equal chlorides are additive, which volatilizees generation in temperature-rise period
A large amount of holes；The mass ratio for controlling titanium dioxide and additive is 4~2:1, can make portions additive and TiO2Reaction generates metatitanic acid
Calcium or magnesium titanate are conducive to the progress of reaction.
To make prefabricated material have suitable intensity, and it is conducive to react with reducing agent, the pressure suppressed in step A of the present invention is
0.1MPa~5MPa, the quality of single prefabricated material are 5g~60g.
In step B, metallic reducing agent is at least one of metal K, Ca, Na or Mg；The dosage titanium white of metallic reducing agent
The 120%~200% of silty amount；The temperature of reduction reaction is 900~1100 DEG C, and the time is 4~7h.
For in step C, less than 80 μm accountings of the crushing material after reduction to granularity are first greater than 98% convenient for leaching.Institute
State acidleach are as follows: CaCl is leached using 3%~5% dilute hydrochloric acid of mass concentration2Equal by-products leach liquid-solid ratio >=20mL:1g, maximum
The dissolution of limit reduction titanium, 20~30 DEG C of extraction temperature, 10~15min of extraction time.
In step C, leaching is finished, and is first washed with water 2~3 times, then with alcohol rinse 1~2 time, to remove impurity；Then exist
60~70 DEG C of vacuum drying 12h again.
In step D, the pollution of titanium valve elements such as Fe in shaping processing process can be effectively avoided using airflow milling；Institute
Airflow milling is stated using argon gas as grinding gas, it is in 120 ° of modes that two nozzles, which are arranged, in 180 ° or three nozzles in airflow milling,
Grinding air pressure is 0.1~1MPa, and milling time is 3~10min.
Below by embodiment, invention is further described in detail, but does not therefore limit the scope of the present invention
Among the embodiment described range.
Embodiment 1
Use in the market that titanium dioxide is raw material, TiO2It is 99.2%, first by titanium dioxide 1000g and addition of C aCl2According to
Briquetting, clamp dog pressure are 1MPa to mass ratio 2:1 after evenly mixing, and Φ 30 × 7mm cylinder prefabricated section is made；By metal Ca
2000g is placed in reactor lower part, and prefabricated section is placed in reactor top, and centre is separated using partition with holes, then welded
Seal reactor；Reactor is heated to 1000 DEG C in Muffle furnace, argon gas is protected when heating, soaking time 6h, reaction knot
Reactor is taken out after beam；
Product is crushed to granularity and is greater than 98% less than 80 μm, is leached using 4% dilute hydrochloric acid of concentration, liquid-solid ratio is leached
30mL:1g, 25 DEG C of temperature, time 15min, after the completion of acidleach, washing 3 times, alcohol rinse 1 time, 60 DEG C of dryings of vacuum oven
12h obtains metallic titanium powder in irregular shape；
Shape correction is carried out to titanium valve using the airflow milling of three nozzles, using argon gas as grinding gas, grinds air pressure
0.5MPa, milling time 5min obtain subsphaeroidal titanium valve；As shown in Figure 1, titanium valve surface flatness is higher, sphericity is preferable, oxygen
Content is 1300PPM.
Embodiment 2
Use in the market that titanium dioxide is raw material, TiO2It is 99.2%, first by titanium dioxide 1000g and addition of C aCl2According to
Briquetting, clamp dog pressure are 1MPa to mass ratio 2:1 after evenly mixing, and Φ 30 × 7mm cylinder prefabricated section is made；
Each 1000g of active metal Ca, Mg is placed in reactor lower part, prefabricated section is placed in reactor top, and centre is adopted
It is separated with partition with holes, then welded seal reactor；Reactor is heated to 950 DEG C in Muffle furnace, argon gas when heating
Protection, soaking time 6h take out reactor after reaction；
Product is crushed to granularity and is greater than 98% less than 80 μm, is leached using 5% dilute hydrochloric acid of concentration, liquid-solid ratio is leached
25mL:1g, 25 DEG C of temperature, time 10min, after the completion of acidleach, washing 3 times, alcohol rinse 1 time, 60 DEG C of dryings of vacuum oven
12h obtains metallic titanium powder in irregular shape；
Shape correction is carried out to titanium valve using the airflow milling of three nozzles, using argon gas as grinding gas, grinds air pressure
0.4MPa, milling time 7min obtain subsphaeroidal titanium valve, oxygen content 1400PPM.
Embodiment 3
Use in the market that titanium dioxide is raw material, TiO2It is 99.2%, first by titanium dioxide 1000g and addition of C aCl2According to
Briquetting, clamp dog pressure are 1MPa to mass ratio 3:1 after evenly mixing, and Φ 30 × 7mm cylinder prefabricated section is made；
Each 1000g of active metal Ca, Mg is placed in reactor lower part, prefabricated section is placed in reactor top, and centre is adopted
It is separated with partition with holes, then welded seal reactor；Reactor is heated to 950 DEG C in Muffle furnace, argon gas when heating
Protection, soaking time 7h take out reactor after reaction；
Product is crushed to granularity and is greater than 98% less than 80 μm, is leached using 5% dilute hydrochloric acid of concentration, liquid-solid ratio is leached
25mL:1g, 25 DEG C of temperature, time 10min, after the completion of acidleach, washing 3 times, alcohol rinse 1 time, 60 DEG C of dryings of vacuum oven
12h obtains metallic titanium powder in irregular shape；
Shape correction is carried out to titanium valve using the airflow milling of three nozzles, using argon gas as grinding gas, grinds air pressure
0.6MPa, milling time 5min obtain subsphaeroidal titanium valve, oxygen content 1600PPM.
Claims (8)
1. the preparation method of nearly ball-type titanium valve, it is characterised in that: the following steps are included:
A, titanium dioxide is uniformly mixed with additive, is pressed into prefabricated material；
B, in closed reaction vessel, metallic reducing agent is placed in reactor lower part, prefabricated material is placed in reactor top, in
Between separated using partition, reduction reaction is carried out under inert gas shielding, obtains reducing material；
C, reducing material is crushed under inert gas protection, then carries out acidleach, then washed, dry, obtains in irregular shape
Metallic titanium powder；
D, metallic titanium powder in irregular shape is subjected in airflow milling Shape correction, obtains subsphaeroidal titanium valve.
2. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step A, the titanium dioxide with
The mass ratio of additive is 4~2:1.
3. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step A, the additive is
CaCl2Or MgCl2。
4. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step A, the pressure of the compacting
Power is 0.1MPa~5MPa, and the quality of single prefabricated material is 5g~60g.
5. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step B, the metal reduction
Agent is at least one of metal K, Ca, Na or Mg；The dosage of the metallic reducing agent be titanium dioxide quality 120%~
200%.
6. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step B, the reduction reaction
Temperature be 900~1100 DEG C, the time be 4~7h.
7. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step C, at least meet following
One:
It is described broken are as follows: to be crushed to less than 80 μm accountings of granularity greater than 98%；
The acidleach are as follows: leached using 3%~5% dilute hydrochloric acid of mass concentration, leach liquid-solid ratio >=20mL:1g, extraction temperature 20
~30 DEG C, 10~15min of extraction time；
The washing are as follows: be first washed with water 2~3 times, then with alcohol rinse 1~2 time；
The drying are as follows: 60~70 DEG C of vacuum drying 8h~12h.
8. the preparation method of nearly ball-type titanium valve according to claim 1, it is characterised in that: in step D, the airflow milling is adopted
Use argon gas as grinding gas, it is in 120 ° of modes that two nozzles, which are arranged, in 180 ° or three nozzles in airflow milling, and grinding air pressure is
0.1~1MPa, milling time are 3~10min.
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| CN201910953844.0A CN110524003A (en) | 2019-10-09 | 2019-10-09 | The preparation method of nearly ball-type titanium valve |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705720A (en) * | 2020-12-24 | 2021-04-27 | 中国科学院过程工程研究所 | Preparation method of low-oxygen titanium powder |
| CN112725640A (en) * | 2020-12-24 | 2021-04-30 | 中国科学院过程工程研究所 | Method for preparing low-oxygen titanium powder from titanium tetrachloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112705720A (en) * | 2020-12-24 | 2021-04-27 | 中国科学院过程工程研究所 | Preparation method of low-oxygen titanium powder |
| CN112725640A (en) * | 2020-12-24 | 2021-04-30 | 中国科学院过程工程研究所 | Method for preparing low-oxygen titanium powder from titanium tetrachloride |
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