CN109226775A - A kind of preparation method of the dedicated titanium powder of porous titanium film or titanium alloy powder - Google Patents
A kind of preparation method of the dedicated titanium powder of porous titanium film or titanium alloy powder Download PDFInfo
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- CN109226775A CN109226775A CN201811160706.9A CN201811160706A CN109226775A CN 109226775 A CN109226775 A CN 109226775A CN 201811160706 A CN201811160706 A CN 201811160706A CN 109226775 A CN109226775 A CN 109226775A
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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
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/023—Hydrogen absorption
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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Abstract
The invention discloses a kind of dedicated titanium powder of porous titanium film or the preparation method of titanium alloy powder, this method comprises: one, compacting is obtained into titanium block or titanium alloy block is placed in flue；Two, flue is vacuumized and is kept the temperature；Three, the hydrogenation that hydrogen carries out self- propagating is filled with into flue；Four, titanium block or titanium alloy block suction hydrogen are saturated to obtain titantium hydride block or titantium hydride alloy block；Five, it pulverizes and sieves；Six, coarse powder is broken；Seven, heat preservation dehydrogenation obtains titanium powder or titanium alloy dehydrogenation powder；Eight, it smashes and is sieved and obtains titanium powder and titanium alloy powder through magnetic separation and flotation.The present invention meets the hydrogenation that the supply of thermal energy required for hydrogenation continues carries out self- propagating using the heat that hydrogenation is released, the heat that reaction generates is reduced to increase, the hydrogenation for avoiding titanium block or titanium alloy block is not thorough, improve the degree of titanium block or the hydrogenation embrittlement of titanium alloy block, it finally obtains thinner granularity and uniform titanium powder or titanium alloy powder, improves the quality of titanium valve or Titanium Powder.
Description
Technical field
The invention belongs to powder metallurgical technologies, and in particular to a kind of dedicated titanium powder of porous titanium film or titanium alloy powder
Preparation method.
Background technique
Hydrometallurgy operating condition is very harsh, not only to bear the strong corrosion of many media, still suffers from certain
Load, domestic many hydrometallurgy enterprises are all being widely used POROUS TITANIUM and titanium alloy film technological improvement or are replacing traditional filtering
Separator.In addition, the industries such as chlor-alkali, water process have the huge market demand to POROUS TITANIUM anode film at present, about need every year more
Hole Ni―Ti anode is up to 5000 tons or so.The solid-liquor separation of activated carbon and liquid in " the big infusion " of pharmaceutical industry, it is also desirable to hole
Uniformly, the porous titanium film of the high-quality of consistency of thickness needs porous titanium film about 10000m every year2.In addition, beer, beverage industry
Filtering need to use the porous titanium film of high-quality about 50000m2.Prepare that these porous titanium films are total about to need titanium valve tons up to ten thousand.
And to improve environmental protection, low pollution, corrosion resistance and the ability to bear (mechanical property of porous titanium or titanium alloy metal film
Can), it is necessary to reduce its oxygen content and iron content, its corresponding important foundation raw material also just need hypoxemia, low iron content and
Fine granularity, corrosion resistant high-quality titanium or titanium alloy powder.The whole world is made a general survey of, many countries including China possess relatively
The technology of preparing of mature titanium valve has substantially met the demand of conventional powder metallurgical preparation densification or porous titanium products, but batch
Its oxygen content of the titanium or titanium alloy powder of supply and iron content are higher, can not meet the requirement of high-quality titanium or titanium alloy powder.
With the fast development in the fields such as hydrometallurgy, energy environment protection, pharmaceutical industry, beer, beverage, defence and military, to high-quality
The demand of fine titanium powder is more and more.The mainstream preparation method of high-volume titanium or titanium alloy powder is HDH method (HDH) at present,
However during hydrogenation becomes fragile, since hydrogenation is an exothermic process, reaction speed quickly, in mass production with
The increase of hydride doses, the short time heat of aggregation can be increase accordingly, and the titanium or titanium alloy temperature made is increased rapidly and melted,
Cause material hydrogenation impermeable, also non-breakable, the powder of preparation is thicker, and furthermore the oxygen content of powder and iron content are also relatively high,
It is not able to satisfy the requirement of the corrosion-resistant POROUS TITANIUM of high-precision and titanium alloy film.Fig. 1 is the SEM figure of the titanium powder of prior art preparation,
It will be seen from figure 1 that the titanium powder size particles difference that prior art preparation obtains is larger, powder is thicker, adheres to above particle
There is attritive powder, easily causes oxidation or even exothermic oxidation is on fire, and attritive powder is often oxide powder.
Summary of the invention
Technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing, a kind of porous titanium film is special
With titanium or titanium alloy powder preparation method.This method controls titanium block or titanium alloy block hydriding process, utilizes hydrogenation
The heat that reaction is released meets the hydrogenation that the supply of thermal energy required for hydrogenation continues carries out self- propagating, reduces anti-
The heat that should be generated increases, and the hydrogenation for avoiding titanium block or titanium alloy block is not thorough, and improves titanium block or the hydrogenation embrittlement of titanium alloy block
Degree, finally obtain thinner granularity and uniform titanium powder or titanium alloy powder, improve the product in titanium valve or Titanium Powder
Matter.
In order to solve the above technical problems, the technical solution adopted by the present invention is that: a kind of dedicated titanium powder of porous titanium film or titanium
The preparation method of alloy powder, the flue and heating furnace shell for the dual-purpose heating stove that this method uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge are provided between fire door and hydrogen inlet, it is special
Sign is, method includes the following steps:
Step 1: considering titanium sponge, titanium bits or titanium alloy to be worth doing compression moulding, titanium block or titanium alloy block are obtained, then by titanium block
Or titanium alloy block is placed in the flue of dual-purpose heating stove；The titanium bits or titanium alloy bits are passing through purified treatment using preceding；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum is to vacuum degree to 10-3Then flue is heated in furnace shell since push-in sealed end and is heated to 150 DEG C~250 DEG C by Pa
It is kept the temperature, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa or more to vacuumize
And heat preservation, it then opens hydrogen valve and is filled with the hydrogen that dew point is less than -40 DEG C into flue, when the Hydrogen Vapor Pressure in flue is
When 0.12MPa~0.18MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature liter in flue
When up to 480 DEG C~670 DEG C and pressure are begun to decline, it is filled with hydrogen into flue, increases when the pressure rapid decrease in flue
Hydrogenation intake simultaneously stops heating, and titanium block or titanium alloy block is made to carry out the hydrogenation of self- propagating；The hydrogenation of the self- propagating
Hydrogen Vapor Pressure during reaction in flue is 0.1MPa~0.4MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It is kept the temperature to 650 DEG C~700 DEG C, when titanium block or titanium alloy block inhale pressure gauge numerical value after hydrogen is saturated and do not change, stopping adds
Heat obtains titantium hydride block or titantium hydride alloy block, and titantium hydride block is taken out after the temperature in flue is down to 60 DEG C or titantium hydride closes
Gold bullion；Hydrogen Vapor Pressure during temperature in the flue is down to 60 DEG C in flue is in 0.2MPa or more；
Step 5: titantium hydride block obtained in step 4 or titantium hydride alloy block are carried out under the protection of inert gas thick
It crushes, then crosses 60 meshes, obtained screenings is titantium hydride coarse powder or hydrogenation titanium alloy coarse powder；
Step 6: using inert gas flow mill by titantium hydride coarse powder obtained in step 5 or hydrogenation titanium alloy coarse powder into
Row is broken, obtains titanium hydride powders or hydrogenation titanium alloy powder；
Step 7: titanium hydride powders obtained in step 6 or hydrogenation titanium alloy powder are fitted into rectangle nickel boat and are spread
It is flat, then rectangle nickel boat is fitted into vacuum drying oven, and cover POROUS TITANIUM PLATE above every layer of rectangle nickel boat, using diffusion pump
And it is no more than 10 to vacuum degree is evacuated in vacuum drying oven using mechanical pump as fore pump-2Pa is again heated to 200 DEG C and is kept the temperature,
Continuing to be evacuated to the vacuum degree in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders or hydrogenation titanium alloy
Powder carries out heat preservation dehydrogenation, obtains titanium dehydrogenation powder or titanium alloy dehydrogenation powder；
Step 8: crossing 60 meshes after titanium dehydrogenation powder obtained in step 7 or titanium alloy dehydrogenation powder are smashed, then use
Middle high energy product NdFeB permanent magnet carries out iron removal by magnetic separation more than three times, then use quality purity for 99.99% inert gas
Flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain titanium powder or titanium alloy powder；The titanium powder or titanium alloy
The mass content of iron in powder is no more than 0.1%, and the mass content of oxygen is no more than 0.18%.
The present invention, for raw material, using the hydrogenation of self- propagating, utilizes hydrogenation with titanium sponge, titanium bits or titanium alloy bits
The heat of releasing meets the supply of thermal energy required for hydrogenation continues, and hydrogenation continuity is maintained constantly to carry out down
It goes, since the heat that titanium block or titanium alloy block hydrogenation are released has been utilized, with the progress of hydrogenation, reacts generation
Heat increases less, and the temperature of titanium block or titanium alloy block to be hydrogenated increases limited, will not generate melting phenomenon, thus titanium block or
Titanium alloy block is hydrogenated, and avoids titanium block or the hydrogenation of titanium alloy block is not thorough phenomenon, improve titanium block or the hydrogenation of titanium alloy block
The degree of embrittlement, is conducive to subsequent broken, finally obtains thinner granularity and uniform titanium powder or titanium alloy powder, improves
Quality in titanium powder or titanium alloy powder；Simultaneously in the hydriding process of entire self- propagating, according to hydrogen consumption situation
Adjustment hydrogen intake in time remains that Hydrogen Vapor Pressure is positive pressure in flue, avoids oxidation caused by outside air penetrates into,
Reduce the oxygen content in titanium powder or titanium alloy powder.
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that step 6
The quality purity of the broken inert gas used for 99.99%, it is described it is broken during in inert gas flow mill
Oxygen content is 100ppm~300ppm, and the revolving speed of grading wheel is 2500 revs/min~4000 revs/min in inert gas flow mill；Institute
It states titanium hydride powders or hydrogenates the granularity of titanium alloy powder no more than -100 mesh.By the grading wheel for adjusting inert gas flow mill
Revolving speed controls titanium hydride powders or hydrogenates the particle size range of titanium alloy powder, keeps titanium hydride powders or hydrogenation titanium alloy powder abundant
Dehydrogenation substantially increases dehydrogenation rate
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that step 7
The titanium hydride powders or hydrogenation titanium alloy powder pave after with a thickness of 5mm~30mm.The titantium hydride in nickel boat will be laid on
Powder or the thickness limit for hydrogenating titanium alloy powder avoid powder while improving nickel boat filling amount in 5mm~30mm
Adhesion agglomeration is conducive to the rate and efficiency that improve powder dehydrogenation.
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that step 7
It is middle that rectangle nickel boat is fitted into vacuum drying oven using gradient layer dress method, the detailed process of the gradient layer dress method are as follows: length is narrow
Nickel boat is placed on the upper layer of vacuum drying oven, and short wide nickel boat is placed on to the lower layer of vacuum drying oven, until whole nickel boats are packed into vacuum drying oven, often
Length of the layer nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width, and every layer of nickel boat is being both placed in one layer of nickel boat just
Lower position.The filling amount of nickel boat is increased using gradient layer method, to improve dehydrogenation efficiency, and is conducive to the saturating of hydrogen
Out.
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that step 7
Described in be heated to 700 DEG C carry out heat preservation dehydrogenation during, when the vacuum degree in vacuum drying oven be 30Pa when, turn off diffusion pump,
Vacuum drying oven is vacuumized using mechanical pump.Illustrate that the removing amount of hydrogen is larger when the vacuum degree in vacuum drying oven is 30Pa,
Therefore turn off the small diffusion pump of exhaust capacity, be evacuated using the small mechanical pump of exhaust capacity, be conducive to be taken off in vacuum drying oven
The discharge of the hydrogen removed.
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that step 7
It is middle that heat preservation dehydrogenation, the detailed process of the phase by phase method heat preservation dehydrogenation are carried out using phase by phase method are as follows: to be first 700 DEG C in temperature
Under the conditions of keep the temperature dehydrogenation 1h~12h, be then cooled to 650 DEG C of heat preservation dehydrogenase 34 h~12h, then be cooled to 600 DEG C of heat preservation dehydrogenations, when
When vacuum degree in vacuum drying oven is 0.1Pa, stop heating and furnace cooling.Dehydrogenation is both improved using phase by phase method heat preservation dehydrogenation
Rate, in turn avoid it is powder sintered agglomeration it is agglomerating, ensure that the particle uniformity of powder, to obtain after reducing dehydrogenation reaction
Titanium dehydrogenation powder or titanium alloy dehydrogenation powder breaking strength and broken time, further reduced it is broken for a long time caused by oxygen contain
The increase of amount.
The preparation method of a kind of dedicated titanium powder of above-mentioned porous titanium film or titanium alloy powder, which is characterized in that in described
High energy product NdFeB permanent magnet is the external rubber-coated middle high energy product NdFeB permanent magnet for having high-coercive force.Outside packet
The middle high energy product NdFeB permanent magnet for having high-coercive force of rubber is covered to have the impurity such as iron in titanium powder or titanium alloy powder
There is stronger removing adsorption capacity, advantageously reduces the impurity contents such as iron in titanium powder or titanium alloy powder, improve titanium powder
Or the quality of titanium alloy powder.
Compared with the prior art, the present invention has the following advantages:
1, the present invention uses the hydrogenation of self- propagating, is met using the heat that titanium block or titanium alloy block hydrogenation are released
The supply of thermal energy required for titanium block or titanium alloy block hydrogenation continue maintains hydrogenation continuity constantly to carry out down
It goes, with the progress of hydrogenation, the heat for reacting generation increases the temperature raising of less, to be hydrogenated titanium block or titanium alloy block
It is limited, melting phenomenon will not be generated, so that titanium block or titanium alloy block are hydrogenated, avoids titanium block or the hydrogenation of titanium alloy block not
Thorough phenomenon improves the degree of titanium block or the hydrogenation embrittlement of titanium alloy block, be conducive to it is subsequent broken, finally obtain granularity it is relatively thin and
Uniform titanium powder or titanium alloy powder, improve the quality in titanium powder or titanium alloy powder.
2, the hydrogenation of self- propagating of the invention by itself exothermic heat of reaction maintain reaction continuity, reaction speed compared with
Fastly, the production cycle of titanium powder or titanium alloy powder is shortened, in addition without heating, has saved the energy.
3, in hydriding process of the present invention by controlling the Hydrogen Vapor Pressure especially self- propagating in entire hydrogenation process
Hydrogen Vapor Pressure, Hydrogen Vapor Pressure and hydriding process after hydrogenation in temperature-fall period temperature, it is indirectly real
Now to the control of hydrogenation process, be conducive to the progress of the hydrogenation of self- propagating, avoid titanium block or titanium alloy block inhales hydrogen
Product embrittlement degree caused by content is reduced is low, non-breakable, improves the rate of hydrogenation；Titantium hydride block is avoided simultaneously
Or in titantium hydride alloy block oxygen content increase, and then reduce the oxygen content in titanium valve or Titanium Powder, further improve
Quality in titanium valve or Titanium Powder.
4, titanium hydride powders or hydrogenation titanium alloy powder are fitted into nickel boat using gradient layer dress method and carry out sublevel by the present invention
Section method keeps the temperature dehydrogenation, covers POROUS TITANIUM PLATE on nickel boat, avoids titanium hydride powders or hydrogenates the oxidation of titanium alloy powder and miscellaneous
Matter pollution, and gradient layer method increases the filling amount of nickel boat, to improve dehydrogenation efficiency, and is conducive to appearing for hydrogen；
Using phase by phase method heat preservation dehydrogenation both improve dehydrogenation rate, in turn avoid it is powder sintered agglomeration it is agglomerating, ensure that of titanium valve
Grain uniformity, thus the breaking strength of the titanium powder or titanium alloy coarse powder that are obtained after reducing dehydrogenation reaction and broken time, into
One step reduces the increase of caused oxygen content broken for a long time.
5, the present invention obtains titanium hydride powders or hydrogenation titanium alloy powder using inert gas flow worn-off is broken, passes through adjusting
The classification wheel speed control titanium hydride powders of inert gas flow mill or the particle size range for hydrogenating titanium alloy powder, make hydride powder
End or the hydrogenation abundant dehydrogenation of titanium alloy powder, substantially increase dehydrogenation rate.
6, the entire hydrogenation process of the present invention is hydrogenated using positive pressure, and Hydrogen Vapor Pressure maintains 0.1MPa or more always and controls certainly
Hydrogen Vapor Pressure in the hydriding process of sprawling is 0.1MPa~0.2MPa, avoids wink in the hydriding process of self- propagating
Between largely inhale hydrogen generation negative pressure appearance, ensure that the purity of hydrogen；After the hydrogenation of self- propagating, Hydrogen Vapor Pressure is always
It is maintained at 0.2MPa or more, avoids the increase phenomenon that low pressure or negative pressure seep oxygen into furnace and generate oxygen content in power, further
Improve the quality of titanium powder or titanium alloy powder.
7, the present invention further reduced iron content, oxygen in titanium powder or titanium alloy powder using magnetic separation and floatation process
The quality that the content of content and impurity dust, more a step improve titanium powder or titanium alloy powder.
8, the titanium powder or titanium alloy powder particle surface that the present invention is prepared are clean, and no ultra-fine grain attachment is not allowed
Oxidizable and kindling, oxygen content is low, and powder size is relatively uniform, and particle is polygon diamond shape of uniform size, has and relatively closes
Suitable mobility is no more than 0.1% with conjunction formability, the mass content of the iron in titanium powder or titanium alloy powder is chewed, the quality of oxygen
Content is no more than 0.18%, and quality is higher, meets the raw materials requirement for preparing corrosion-resistant porous titanium film.
Technical solution of the present invention is described in further detail below by drawings and examples.
Detailed description of the invention
Fig. 1 is the SEM figure of the titanium powder of prior art preparation.
Fig. 2 is the mixed-powder obtained after titanium powder prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 5 mixes
SEM figure.
Specific embodiment
Embodiment 1
The flue and heating furnace shell for the dual-purpose heating stove that the preparation method of the present embodiment uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge, the party are provided between fire door and hydrogen inlet
Method the following steps are included:
Step 1: considering purified treated the titanium of 3kg to be worth doing compression moulding, obtain titanium block, then by titanium block be placed in it is dual-purpose plus
In the flue of hot stove；The purified treatment of the titanium bits is followed successively by and picks separation, soda acid is washed, is washed and is dried；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum to vacuum degree is 10-3Pa, then by flue since in push-in heating furnace shell and being heated to 150 DEG C sealed end and keep the temperature
To remove gas, oil and the moisture on titanium block, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa to vacuumize and protect
Then temperature is filled with the hydrogen that dew point is -41 DEG C into flue by hydrogen inlet, when the Hydrogen Vapor Pressure in flue is
When 0.12MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 530 DEG C
And pressure is filled with hydrogen into flue when beginning to decline, and increases hydrogen intake when the pressure rapid decrease in flue and stops
It only heats, titanium block is made to carry out the hydrogenation of self- propagating；Hydrogen pressure during the hydrogenation of the self- propagating in flue
Power is 0.1MPa~0.2MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It keeping the temperature to 680 DEG C, pressure gauge numerical value does not change after titanium block inhales hydrogen saturation, and stop heating, obtains titantium hydride block, when
Temperature in flue takes out titantium hydride block after being down to 60 DEG C；Hydrogen during temperature in the flue is down to 60 DEG C in flue
Atmospheric pressure is in 0.2MPa or more；
Step 5: titantium hydride block obtained in step 4 is carried out coarse crushing under the protection of argon gas, 60 meshes are then crossed,
Obtained screenings is titantium hydride coarse powder；
Titantium hydride coarse powder obtained in step 5 is crushed Step 6: being ground using inert gas flow, is hydrogenated
Titanium powder；The broken inert gas used for the argon gas of quality purity 99.99%, it is described it is broken during inert gas
Oxygen content in airflow milling is 100ppm, and the revolving speed of grading wheel is 2500 revs/min in inert gas flow mill；The hydride powder
The granularity at end is -120 mesh；
Step 7: titanium hydride powders obtained in step 6 are fitted into rectangle nickel boat and are paved, gradient is then used
Rectangle nickel boat is fitted into vacuum drying oven by layer dress method, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, using diffusion pump
It and by fore pump of mechanical pump is 10 to vacuum degree is evacuated in vacuum drying oven-2Pa is again heated to 200 DEG C and is kept the temperature, and continues
The vacuum degree being evacuated in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders progress phase by phase method heat preservation
Dehydrogenation obtains titanium dehydrogenation powder；The titanium hydride powders pave after with a thickness of 5mm；The detailed process of the gradient layer dress method are as follows:
The narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, short wide nickel boat is placed on to the lower layer of vacuum drying oven, until whole nickel boats are packed into
Vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width, and every layer of nickel boat is both placed in one layer
The following position directly of nickel boat；It is described be heated to 700 DEG C carry out heat preservation dehydrogenation during, when the vacuum degree in vacuum drying oven be 30Pa
When, turn off diffusion pump, vacuum drying oven is vacuumized using mechanical pump；The detailed process of the phase by phase method heat preservation dehydrogenation are as follows:
Dehydrogenation 1h is first kept the temperature under conditions of temperature is 700 DEG C, is then cooled to 650 DEG C of heat preservation dehydrogenase 34 h, then be cooled to 600 DEG C of heat preservations
Dehydrogenation stops heating and furnace cooling when the vacuum degree in vacuum drying oven is 0.1Pa；
Step 8: 60 meshes are crossed after titanium dehydrogenation powder obtained in step 7 is smashed, then using external rubber-coated
The middle high energy product NdFeB permanent magnet for having high-coercive force carries out iron removal by magnetic separation three times, then uses quality purity for 99.99%
Argon gas flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain titanium powder；The quality of iron contains in the titanium powder
Amount is 0.1%, and the mass content of oxygen is 0.16%.
Embodiment 2
The flue and heating furnace shell for the dual-purpose heating stove that the preparation method of the present embodiment uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge, the party are provided between fire door and hydrogen inlet
Method the following steps are included:
Step 1: 100kg titanium sponge compression moulding is obtained titanium block, then titanium block is placed in the flue of dual-purpose heating stove
In；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum to vacuum degree is 10-3Pa, then by flue since in push-in heating furnace shell and being heated to 250 DEG C sealed end and keep the temperature
To remove gas, oil and the moisture on titanium block, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa to vacuumize and protect
Then temperature is filled with the hydrogen that dew point is -45 DEG C into flue by hydrogen inlet, when the Hydrogen Vapor Pressure in flue is
When 0.18MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 480 DEG C
And pressure is filled with hydrogen into flue when beginning to decline, and increases hydrogen intake when the pressure rapid decrease in flue and stops
It only heats, titanium block is made to carry out the hydrogenation of self- propagating；Hydrogen pressure during the hydrogenation of the self- propagating in flue
Power is 0.2MPa~0.4MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It keeping the temperature to 650 DEG C, pressure gauge numerical value does not change after titanium block inhales hydrogen saturation, and stop heating, obtains titantium hydride block, when
Temperature in flue takes out titantium hydride block after being down to 60 DEG C；Hydrogen during temperature in the flue is down to 60 DEG C in flue
Atmospheric pressure is in 0.2MPa or more；
Step 5: titantium hydride block obtained in step 4 is carried out coarse crushing under the protection of argon gas, 60 meshes are then crossed,
Obtained screenings is titantium hydride coarse powder；
Titantium hydride coarse powder obtained in step 5 is crushed Step 6: being ground using inert gas flow, is hydrogenated
Titanium powder；The broken inert gas used for the argon gas of quality purity 99.99%, it is described it is broken during inert gas
Oxygen content in airflow milling is 300ppm, and the revolving speed of grading wheel is 4000 revs/min in inert gas flow mill；The hydride powder
The granularity at end is -320 mesh；
Step 7: titanium hydride powders obtained in step 6 are fitted into rectangle nickel boat and are paved, gradient is then used
Rectangle nickel boat is fitted into vacuum drying oven by layer dress method, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, using diffusion pump
It and by fore pump of mechanical pump is 9 × 10 to vacuum degree is evacuated in vacuum drying oven-3Pa is again heated to 200 DEG C and is kept the temperature, after
The continuous vacuum degree being evacuated in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders progress phase by phase method guarantor
Warm dehydrogenation obtains titanium dehydrogenation powder；The titanium hydride powders pave after with a thickness of 30mm；The detailed process of the gradient layer dress method
Are as follows: the narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, short wide nickel boat is placed on to the lower layer of vacuum drying oven, until whole nickel boats fill
Enter vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width, and every layer of nickel boat is both placed in one
The following position directly of layer nickel boat；It is described be heated to 700 DEG C carry out heat preservation dehydrogenation during, when the vacuum degree in vacuum drying oven is
When 30Pa, turn off diffusion pump, vacuum drying oven is vacuumized using mechanical pump；The detailed process of the phase by phase method heat preservation dehydrogenation
Are as follows: dehydrogenation 12h is first kept the temperature under conditions of temperature is 700 DEG C, is then cooled to 650 DEG C of heat preservation dehydrogenation 12h, then be cooled to 600
DEG C heat preservation dehydrogenation, when the vacuum degree in vacuum drying oven be 0.1Pa when, stop heating and furnace cooling；
Step 8: 60 meshes are crossed after titanium dehydrogenation powder obtained in step 7 is smashed, then using external rubber-coated
The middle high energy product NdFeB permanent magnet for having high-coercive force carries out four iron removal by magnetic separation, then uses quality purity for 99.99%
Argon gas flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain titanium powder；The quality of iron contains in the titanium powder
Amount is 0.04%, and the mass content of oxygen is 0.18%.
Embodiment 3
The flue and heating furnace shell for the dual-purpose heating stove that the preparation method of the present embodiment uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge, the party are provided between fire door and hydrogen inlet
Method the following steps are included:
Step 1: considering purified treated the TC4 titanium alloy of 10kg to be worth doing compression moulding, TC4 titanium alloy block is obtained, then will
TC4 titanium alloy block is placed in the flue of dual-purpose heating stove；The purified treatment of the TC4 titanium alloy bits, which is followed successively by, picks separation, acid
Alkali cleaning, washing and drying；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum is to vacuum degree to 10-3Pa, then by flue since in push-in heating furnace shell and being heated to 200 DEG C sealed end and keep the temperature
To remove gas, oil and moisture on TC4 titanium alloy block, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 2 × 10-2Turn off when Pa vacuum valve stopping vacuumize and
Then heat preservation is filled with the hydrogen that dew point is -43 DEG C into flue by hydrogen inlet, when the Hydrogen Vapor Pressure in flue is
When 0.15MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 670 DEG C
And pressure is filled with hydrogen into flue when beginning to decline, and increases hydrogen intake when the pressure rapid decrease in flue and stops
It only heats, TC4 titanium alloy block is made to carry out the hydrogenation of self- propagating；During the hydrogenation of the self- propagating in flue
Hydrogen Vapor Pressure is 0.1MPa~0.3MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It is kept the temperature to 700 DEG C, pressure gauge numerical value does not change after TC4 titanium alloy block inhales hydrogen saturation, stops heating, is hydrogenated
TC4 titanium alloy block takes out hydrogenation TC4 titanium alloy block after the temperature in flue is down to 60 DEG C；Temperature in the flue is down to
Hydrogen Vapor Pressure during 60 DEG C in flue is in 0.2MPa or more；
Step 5: hydrogenation TC4 titanium alloy block obtained in step 4 is carried out coarse crushing under the protection of argon gas, then mistake
60 meshes, obtained screenings are hydrogenation TC4 titanium alloy coarse powder；
Step 6: being crushed hydrogenation TC4 titanium alloy coarse powder obtained in step 5 using inert gas flow mill, obtain
To hydrogenation TC4 titanium alloy powder；The broken inert gas used is described broken for the argon gas of quality purity 99.99%
In the process inert gas flow mill in oxygen content be 150ppm, inert gas flow mill in grading wheel revolving speed be 4000 turns/
Point；The granularity of the hydrogenation TC4 titanium alloy powder is -200 mesh；
Step 7: hydrogenation TC4 titanium alloy powder obtained in step 6 to be fitted into rectangle nickel boat and pave, then adopt
Rectangle nickel boat is fitted into vacuum drying oven with gradient layer dress method, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, is used
Diffusion pump and be 10 to vacuum degree is evacuated in vacuum drying oven by fore pump of mechanical pump-2Pa is again heated to 200 DEG C and is protected
Temperature, continuing to be evacuated to the vacuum degree in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders progress sublevel
Section method keeps the temperature dehydrogenation, obtains TC4 titanium alloy dehydrogenation powder；It is described hydrogenation TC4 titanium alloy powder pave after with a thickness of 8mm；It is described
The detailed process of gradient layer dress method are as follows: the narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, short wide nickel boat is placed on vacuum drying oven
Lower layer, until whole nickel boats are packed into vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width,
And every layer of nickel boat is both placed in the following position directly of one layer of nickel boat；It is described be heated to 700 DEG C carry out heat preservation dehydrogenation during,
When the vacuum degree in vacuum drying oven is 30Pa, turns off diffusion pump, vacuum drying oven is vacuumized using mechanical pump；It is described stage by stage
The detailed process of method heat preservation dehydrogenation are as follows: first keep the temperature dehydrogenation 6h under conditions of temperature is 700 DEG C, be then cooled to 650 DEG C of heat preservations
Dehydrogenation 6h, then 600 DEG C of heat preservation dehydrogenations are cooled to, when the vacuum degree in vacuum drying oven is 0.1Pa, stop heating and furnace cooling；
Step 8: 60 meshes are crossed after TC4 titanium alloy dehydrogenation powder obtained in step 7 is smashed, then using external cladding
Rubber have high-coercive force middle high energy product NdFeB permanent magnet carry out five iron removal by magnetic separation, then use quality purity for
99.99% argon gas flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain TC4 titanium alloy powder；It is described
The mass content of iron is 0.03% in TC4 titanium alloy powder, and the mass content of oxygen is 0.16%.
Embodiment 4
The flue and heating furnace shell for the dual-purpose heating stove that the preparation method of the present embodiment uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge, the party are provided between fire door and hydrogen inlet
Method the following steps are included:
Step 1: considering purified treated the Ti600 titanium alloy of 10kg to be worth doing compression moulding, Ti600 titanium alloy block is obtained, so
Ti600 titanium alloy block is placed in the flue of dual-purpose heating stove afterwards；The purified treatment of the Ti600 titanium alloy bits, which is followed successively by, picks
Separation, soda acid are washed, wash and are dried；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum is to vacuum degree to 10-3Pa, then by flue since in push-in heating furnace shell and being heated to 200 DEG C sealed end and keep the temperature
To remove gas, oil and moisture on Ti600 titanium alloy block, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa to vacuumize and protect
Then temperature is filled with the hydrogen that dew point is -44 DEG C into flue by hydrogen inlet, when the Hydrogen Vapor Pressure in flue is
When 0.15MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 620 DEG C
And pressure is filled with hydrogen into flue when beginning to decline, and increases hydrogen intake when the pressure rapid decrease in flue and stops
It only heats, Ti600 titanium alloy block is made to carry out the hydrogenation of self- propagating；During the hydrogenation of the self- propagating in flue
Hydrogen Vapor Pressure be 0.1MPa~0.2MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It is kept the temperature to 650 DEG C, pressure gauge numerical value does not change after Ti600 titanium alloy block inhales hydrogen saturation, stops heating, obtains hydrogen
Change Ti600 titanium alloy block, hydrogenation Ti600 titanium alloy block is taken out after the temperature in flue is down to 60 DEG C；Temperature in the flue
Hydrogen Vapor Pressure during degree is down to 60 DEG C in flue is in 0.2MPa or more；
Step 5: hydrogenation Ti600 titanium alloy block obtained in step 4 is carried out coarse crushing under the protection of argon gas, then
60 meshes are crossed, obtained screenings is hydrogenation Ti600 titanium alloy coarse powder；
Step 6: be crushed hydrogenation Ti600 titanium alloy coarse powder obtained in step 5 using inert gas flow mill,
Obtain hydrogenation Ti600 titanium alloy powder；The broken inert gas used is described broken for the argon gas of quality purity 99.99%
Oxygen content in broken process in inert gas flow mill is 150ppm, and the revolving speed of grading wheel is 3000 in inert gas flow mill
Rev/min；The granularity of the hydrogenation Ti600 titanium alloy powder is -100 mesh；
Step 7: hydrogenation Ti600 titanium alloy powder obtained in step 6 is fitted into rectangle nickel boat and is paved, then
Rectangle nickel boat is fitted into vacuum drying oven using gradient layer dress method, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, is adopted
It is 10 to vacuum degree is evacuated in vacuum drying oven with diffusion pump and by fore pump of mechanical pump-2Pa is again heated to 200 DEG C and is protected
Temperature, continuing to be evacuated to the vacuum degree in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to hydrogenation Ti600 titanium alloy powder
It carries out phase by phase method and keeps the temperature dehydrogenation, obtain Ti600 titanium alloy dehydrogenation powder；It is described to hydrogenate the thickness after Ti600 titanium alloy powder is paved
Degree is 10mm；The detailed process of the gradient layer dress method are as follows: the narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, by short wide nickel boat
It is placed on the lower layer of vacuum drying oven, until whole nickel boats are packed into vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few,
The more 40mm of width, and every layer of nickel boat is both placed in the following position directly of one layer of nickel boat；It is described to be heated to 700 DEG C to carry out heat preservation de-
During hydrogen, when the vacuum degree in vacuum drying oven is 30Pa, turn off diffusion pump, vacuum drying oven take out using mechanical pump true
It is empty；The detailed process of the phase by phase method heat preservation dehydrogenation are as follows: first keep the temperature dehydrogenation 1h under conditions of temperature is 700 DEG C, then drop
Temperature is to 650 DEG C of heat preservation dehydrogenation 8h, then is cooled to 600 DEG C of heat preservation dehydrogenations, when the vacuum degree in vacuum drying oven is 0.1Pa, stop plus
Heat and furnace cooling；
Step 8: 60 meshes are crossed after Ti600 titanium alloy dehydrogenation powder obtained in step 7 is smashed, then using external packet
Cover rubber have high-coercive force middle high energy product NdFeB permanent magnet carry out four iron removal by magnetic separation, then use quality purity for
99.99% argon gas flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain Ti600 titanium alloy powder；It is described
The mass content of iron is 0.08% in Ti600 titanium alloy powder, and the mass content of oxygen is 0.17%.
Embodiment 5
The flue and heating furnace shell for the dual-purpose heating stove that the preparation method of the present embodiment uses can be freely separating, the flue
Both ends be respectively fire door end and sealed end, fire door end is connect with vacuum system, water cooling system and hydrogen inlet respectively, furnace
It is provided with vacuum valve between Men Duanyu vacuum system, hydrogen valve and pressure gauge, the party are provided between fire door and hydrogen inlet
Method the following steps are included:
Step 1: considering purified treated the titanium of 10kg to be worth doing compression moulding, obtain titanium block, then by titanium block be placed in it is dual-purpose plus
In the flue of hot stove；The purified treatment of the titanium bits is followed successively by and picks separation, soda acid is washed, is washed and is dried；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is taken out using mechanical pump as fore pump to flue
Vacuum is to vacuum degree to 10-3Pa, then by flue since in push-in heating furnace shell and being heated to 250 DEG C sealed end and keep the temperature
To remove gas, oil and the moisture on titanium block, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa to vacuumize and protect
Then temperature is filled with the hydrogen that dew point is -46 DEG C into flue by hydrogen inlet, when the Hydrogen Vapor Pressure in flue is
When 0.12MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 530 DEG C
And pressure is filled with hydrogen into flue when beginning to decline, and increases hydrogen intake when the pressure rapid decrease in flue and stops
It only heats, titanium block is made to carry out the hydrogenation of self- propagating；Hydrogen pressure during the hydrogenation of the self- propagating in flue
Power is 0.2MPa~0.3MPa；
Step 4: the intake for reducing hydrogen makes flue hydrogen after the hydrogenation of the self- propagating described in the step 3
Pressure gauge numerical value at gas air inlet is maintained at 0.2MPa or more, then increases the temperature in flue using heating furnace shell heating
It keeping the temperature to 700 DEG C, pressure gauge numerical value does not change after titanium block inhales hydrogen saturation, and stop heating, obtains titantium hydride block, when
Temperature in flue takes out titantium hydride block after being down to 60 DEG C；Hydrogen during temperature in the flue is down to 60 DEG C in flue
Atmospheric pressure is in 0.2MPa or more；
Step 5: titantium hydride block obtained in step 4 is carried out coarse crushing under the protection of argon gas, 60 meshes are then crossed,
Obtained screenings is titantium hydride coarse powder；
Titantium hydride coarse powder obtained in step 5 is crushed Step 6: being ground using inert gas flow, is hydrogenated
Titanium powder；The broken inert gas used for the argon gas of quality purity 99.99%, it is described it is broken during inert gas
Oxygen content in airflow milling is 150ppm, and the revolving speed of grading wheel is 3000 revs/min in inert gas flow mill；The hydride powder
The granularity at end is -160 mesh；
Step 7: titanium hydride powders obtained in step 6 are fitted into rectangle nickel boat and are paved, gradient is then used
Rectangle nickel boat is fitted into vacuum drying oven by layer dress method, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, using diffusion pump
It and by fore pump of mechanical pump is 10 to vacuum degree is evacuated in vacuum drying oven-2Pa is again heated to 200 DEG C and is kept the temperature, and continues
The vacuum degree being evacuated in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders progress phase by phase method heat preservation
Dehydrogenation obtains titanium dehydrogenation powder；The titanium hydride powders pave after with a thickness of 12mm；The detailed process of the gradient layer dress method
Are as follows: the narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, short wide nickel boat is placed on to the lower layer of vacuum drying oven, until whole nickel boats fill
Enter vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width, and every layer of nickel boat is both placed in one
The following position directly of layer nickel boat；It is described be heated to 700 DEG C carry out heat preservation dehydrogenation during, when the vacuum degree in vacuum drying oven is
When 30Pa, turn off diffusion pump, vacuum drying oven is vacuumized using mechanical pump, the detailed process of the phase by phase method heat preservation dehydrogenation
Are as follows: dehydrogenase 13 h is first kept the temperature under conditions of temperature is 700 DEG C, is then cooled to 650 DEG C of heat preservation dehydrogenation 6h, then be cooled to 600 DEG C
Dehydrogenation is kept the temperature, when the vacuum degree in vacuum drying oven is 0.1Pa, stops heating and furnace cooling；
Step 8: 60 meshes are crossed after titanium dehydrogenation powder obtained in step 7 is smashed, then using external rubber-coated
The middle high energy product NdFeB permanent magnet for having high-coercive force carries out four iron removal by magnetic separation, then uses quality purity for 99.99%
Argon gas flotation removes SiO2、Al2O3And oxidation fine particle dusts, obtain titanium powder；The quality of iron contains in the titanium powder
Amount is 0.013%, and the mass content of oxygen is 0.15%.
Fig. 2 is the mixed-powder obtained after titanium powder prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 5 mixes
SEM figure, figure it is seen that the titanium powder that the present invention is prepared is adhered to without ultra-fine grain, particle surface is clean, it is not easy to
Oxidation and kindling, powder size is relatively uniform, and particle is polygon diamond shape of uniform size, with appropriate mobility and
Chew conjunction formability.
By Fig. 1 it is found that preparation method of the invention meets hydrogenation using the heat that hydrogenation is released compared with Fig. 2
The supply of thermal energy required for continuing carries out the hydrogenation of self- propagating, and the hydrogenation for avoiding titanium block is not thorough, and improves titanium block
The degree for hydrogenating embrittlement, finally obtains that granularity is thinner and uniform titanium powder, improves the quality of titanium valve.
The present invention meets the supply of thermal energy required for hydrogenation continues using the heat that hydrogenation is released and carries out
The hydrogenation of self- propagating reduces the heat that reaction generates and increases, and the hydrogenation for avoiding titanium block or titanium alloy block is not thorough, and is improved
Titanium block or the degree of titanium alloy block hydrogenation embrittlement finally obtain thinner granularity and uniform titanium powder or titanium alloy powder, improve
The quality of titanium valve or Titanium Powder.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (7)
1. the preparation method of a kind of dedicated titanium powder of porous titanium film or titanium alloy powder, the furnace for the dual-purpose heating stove that this method uses
Gallbladder and heating furnace shell can be freely separating, and the both ends of the flue are respectively fire door end and sealed end, fire door end respectively with vacuum system
System, water cooling system are connected with hydrogen inlet, and vacuum valve, fire door and hydrogen gas are provided between fire door end and vacuum system
Hydrogen valve and pressure gauge are provided between mouthful, which is characterized in that method includes the following steps:
Step 1: considering titanium sponge, titanium bits or titanium alloy to be worth doing compression moulding, titanium block or titanium alloy block are obtained, then by titanium block or titanium
Alloy block is placed in the flue of dual-purpose heating stove；The titanium bits or titanium alloy bits are passing through purified treatment using preceding；
Step 2: vacuum valve described in opening steps one, is used diffusion pump and is vacuumized using mechanical pump as fore pump to flue
It is 10 to vacuum degree-3Then flue is heated in furnace shell since push-in sealed end and is heated to 150 DEG C~250 DEG C progress by Pa
Heat preservation, while continuing to vacuumize flue；
Step 3: working as the vacuum degree in flue described in step 2 is 10-2Turn off vacuum valve stopping when Pa or more to vacuumize and protect
Then temperature opens hydrogen valve and is filled with the hydrogen that dew point is less than -40 DEG C into flue, when the Hydrogen Vapor Pressure in flue is 0.12MPa
When~0.18MPa, stopping is passed through hydrogen and continues to heat flue using heating furnace shell, when the temperature in flue is increased to 480
DEG C~670 DEG C and pressure is when beginning to decline, it is filled with hydrogen into flue, it is logical to increase hydrogen when the pressure rapid decrease in flue
Enter amount and stop heating, titanium block or titanium alloy block is made to carry out the hydrogenation of self- propagating；The mistake of the hydrogenation of the self- propagating
Hydrogen Vapor Pressure in journey in flue is 0.1MPa~0.4MPa；
Step 4: after the hydrogenation of the self- propagating described in the step 3, reduce hydrogen intake make flue hydrogen into
Pressure gauge numerical value at port is maintained at 0.2MPa or more, is then increased to the temperature in flue using heating furnace shell heating
650 DEG C~700 DEG C are kept the temperature, and when titanium block or titanium alloy block inhale pressure gauge numerical value after hydrogen is saturated and do not change, stopping is heated,
Titantium hydride block or titantium hydride alloy block are obtained, titantium hydride block or hydrogenation titanium alloy are taken out after the temperature in flue is down to 60 DEG C
Block；Hydrogen Vapor Pressure during temperature in the flue is down to 60 DEG C in flue is in 0.2MPa or more；
Step 5: titantium hydride block obtained in step 4 or titantium hydride alloy block are carried out coarse powder under the protection of inert gas
It is broken, 60 meshes are then crossed, obtained screenings is titantium hydride coarse powder or hydrogenation titanium alloy coarse powder；
Step 6: titantium hydride coarse powder obtained in step 5 or hydrogenation titanium alloy coarse powder are carried out brokenly using inert gas flow mill
It is broken, obtain titanium hydride powders or hydrogenation titanium alloy powder；
Step 7: titanium hydride powders obtained in step 6 or hydrogenation titanium alloy powder are fitted into rectangle nickel boat and are paved,
Then rectangle nickel boat is fitted into vacuum drying oven, and covers POROUS TITANIUM PLATE above every layer of rectangle nickel boat, simultaneously using diffusion pump
It is no more than 10 to vacuum degree is evacuated in vacuum drying oven using mechanical pump as fore pump-2Pa is again heated to 200 DEG C and is kept the temperature, after
The continuous vacuum degree being evacuated in vacuum drying oven is 10-2When Pa, continue to be heated to 700 DEG C to titanium hydride powders or hydrogenation Titanium Powder
End carries out heat preservation dehydrogenation, obtains titanium dehydrogenation powder or titanium alloy dehydrogenation powder；
Step 8: cross 60 meshes after titanium dehydrogenation powder obtained in step 7 or titanium alloy dehydrogenation powder are smashed, then use in it is high
Magnetic energy product NdFeB permanent magnet carries out iron removal by magnetic separation more than three times, then use quality purity for 99.99% inert gas flotation
Remove SiO2、Al2O3And oxidation fine particle dusts, obtain titanium powder or titanium alloy powder；The titanium powder or titanium alloy powder
In the mass content of iron be no more than 0.1%, the mass content of oxygen is no more than 0.18%.
2. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
Be, the quality purity of inert gas that uses be crushed described in step 6 as 99.99%, it is described be crushed during inert gas
Oxygen content in airflow milling is 100ppm~300ppm, in inert gas flow mill the revolving speed of grading wheel be 2500 revs/min~
4000 revs/min；The titanium hydride powders or the granularity for hydrogenating titanium alloy powder are not more than -100 mesh.
3. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
Be, titanium hydride powders described in step 7 or hydrogenation titanium alloy powder pave after with a thickness of 5mm~30mm.
4. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
It is, rectangle nickel boat is fitted into vacuum drying oven using gradient layer dress method in step 7, the detailed process of the gradient layer dress method
Are as follows: the narrow nickel boat of length is placed on to the upper layer of vacuum drying oven, short wide nickel boat is placed on to the lower layer of vacuum drying oven, until whole nickel boats fill
Enter vacuum drying oven, length of the every layer of nickel boat than upper one layer of nickel boat is 40mm few, the more 40mm of width, and every layer of nickel boat is both placed in one
The following position directly of layer nickel boat.
5. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
Be, be heated to described in step 7 700 DEG C carry out heat preservation dehydrogenation during, when the vacuum degree in vacuum drying oven be 30Pa when,
Turn off diffusion pump, vacuum drying oven is vacuumized using mechanical pump.
6. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
It is, heat preservation dehydrogenation, the detailed process of the phase by phase method heat preservation dehydrogenation are as follows: first in temperature is carried out using phase by phase method in step 7
Degree keeps the temperature dehydrogenation 1h~12h under conditions of being 700 DEG C, is then cooled to 650 DEG C of heat preservation dehydrogenase 34 h~12h, then be cooled to 600 DEG C
Dehydrogenation is kept the temperature, when the vacuum degree in vacuum drying oven is 0.1Pa, stops heating and furnace cooling.
7. the preparation method of a kind of dedicated titanium powder of porous titanium film according to claim 1 or titanium alloy powder, feature
It is, middle high energy product NdFeB permanent magnet described in step 8 is the external rubber-coated middle high magnetic energy for having high-coercive force
Product NdFeB permanent magnet.
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| CN109226775B (en) | 2020-04-17 |
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