CN103938005A - Method for preparing ultra-fine grained titanium and titanium alloy from jet-milled titanium hydride powder - Google Patents
Method for preparing ultra-fine grained titanium and titanium alloy from jet-milled titanium hydride powder Download PDFInfo
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Abstract
The invention belongs to the technical field of powder metallurgy and provides a method for preparing ultra-fine grained titanium and titanium alloy from jet-milled titanium hydride powder. The method comprises the steps of firstly preparing mixed powder of ultra-fine titanium hydride powder or titanium hydride powder and other powder by a jet mill, further adding a small amount of paraffin wax into the well milled powder as forming agent, pressing the powder added with the forming agent to form a blank sample in a certain shape, and placing the blank sample into a sintering furnace for degreasing and sintering; sintering out an ultra-fine grained sintered product with the relative density of above 95% by controlling the heating rate of the furnace, the type of atmosphere in the furnace, the pressure and the vacuum degree of the atmosphere, the degreasing and sintering temperature, the time and other process parameters; then placing the sintered product into a hot isostatic pressing furnace for high-pressure treatment so as to obtain a fully dense ultra-fine grained product. The method provided by the invention has the advantages of simple process and low cost, is suitable for a wide range of titanium alloy types and product sizes, and can realize mass production.
Description
Technical field
The invention belongs to powder metallurgical technology, a kind of preparation method of superfine crystal particle titanium alloy is provided, can be applied in aerospace, chemical industry, boats and ships, automobile, physical culture and medicine equipment etc. and require on the titanium products of light-high-strength.
Background technology
Titanium or titanium alloy is widely used, and has density little, and intensity is high, corrosion resistance excellence, the feature that mechanical behavior under high temperature, antifatigue and creep property are good.Crystal grain to ultra fine grain size by refinement titanium or titanium alloy (is less than 5 μ m), can significantly improves its mechanical property.At present, the possible technique of preparing superfine crystal particle titanium or titanium alloy comprises severe plastic deformation and puts hydrogen processing.
Severe plastic deformation technology comprises equal-diameter bending passage deformation, high pressure torsion, multiaxis forging etc.For example, the employing equal-diameter bending passage deformations such as Wang Xingyun have been prepared superfine crystal particle industrially pure titanium, and the tensile strength of material is brought up to 791MPa from 407MPa, the about 200nm of average grain size; Sergueeva etc. utilize high pressure torsion technology to obtain Ultra-fine Grained Ti-6Al-4V alloy, and the tensile strength of this material reaches 1500MPa; The employing multiaxis forging methods such as Zherebtsov have made Ultra-fine Grained Ti-6A1-4V alloy, and the average grain size of this material is 150nm, and tensile strength is 1400MPa.These class methods are the most feasible current Ultra-fine Grained titanium alloys Preparation Methods, but exist prepared sample size restricted, and passage is many, and complex procedures is high to equipment and mold requirement, the deficiencies such as cost costliness.
Putting hydrogen processing is to ooze hydrogen to titanium alloy, and along with the rising of temperature and the infiltration of hydrogen atom, β phase transition temperature reduces, the phase composite of alloy changes β phase into by alpha+beta rapidly, and hydride forms along crystal boundary and intracrystalline simultaneously, when vacuum annealing, with the reduction of temperature, there is β → α+TiH
2change, hydride decomposes, and in matrix, most of superfluous distortional strain energy is transformed into monovacancy.Interaction between dislocation and room is conducive to subgrain and forms, and then becomes the core of recrystallize, and when dehydrogenation, owing to having there is recrystallize widely in matrix, the axle such as to become tiny for crystal grain like this, thereby obtain close grain titanium alloy.Yang Yang prepares superfine crystal particle titanium alloy by protium facture, and the crystal grain diameter of alloy is decreased to 0.3 ~ 0.5 μ m.
Above two kinds of technology have deficiency separately, the large-scale extrusion equipment of severe plastic deformation Technology Need and high-performance mould, and complex procedures, and energy expenditure is large, and cost is very high, and production efficiency is very low; Put hydrogen treatment technology and can only be used for the grain refining of alloy part kind, have certain limitation.
Summary of the invention
For the deficiencies in the prior art, the present invention aims to provide that a kind of technique is simple, and production cost is low, applied widely, the novel method of preparing superfine crystal particle titanium or titanium alloy material being produced on a large scale.The method does not require the volume size of prepared sample, and operation is few, and cost is low, product performance are high.
Technical scheme of the present invention is:
Airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy, and concrete steps are:
(1) powder process: raw material powder is put into comminution by gas stream crusher machine, obtain
d 50it is the intermediate powder of 0.1 μ m ~ 10 μ m; Described raw material powder is the mixture of titanium hydride powders or titanium hydride powders and other powder, and wherein said other powder refers to and suppresses the hard phase powder of crystal growth and/or prepare titanium alloy metal-powder used; The gas that described micronizer mill uses is one or more in argon gas, nitrogen and hydrogen;
(2) compacting: paraffin is mixed with the organic solvent of solubilized paraffin, obtain solvent; Described intermediate powder is added in described solvent and stirred, obtain mixture; By the dry mixture organic solvent of removing, obtain dried powder, wherein paraffin account for dry after the quality percentage composition of powder be 0.5%-8%, all the other are intermediate powder; Described dried powder is placed on pressing machine and is suppressed by mould, and pressing pressure is 15 MPa ~ 400MPa, obtains base sample after having suppressed;
(3) degreasing: described base sample is put into vacuum sintering furnace and with the temperature rise rate of 0.5 DEG C/min ~ 5 DEG C/min, base sample is heated to 100 DEG C ~ 300 DEG C of skimming temps, be incubated 0.5 h ~ 10h at skimming temp; Wherein, when temperature is before 100 DEG C ~ 200 DEG C, stove internal gas pressure is vacuum, and vacuum tightness is 1 × 10
-4~ 100Pa when temperature is after 100 DEG C ~ 200 DEG C, leads to the degreasing gas that purity is greater than 99.9% in stove, and described degreasing gas is argon gas or hydrogen, and gas flow rate is 20ml/min ~ 20L/min; Reach after degreasing time, stop continuing to pass into gas, degreasing finishes;
(4) sintering: after degreasing finishes, with the temperature rise rate of 0.5 DEG C/min ~ 20 DEG C/min, base sample is heated to 600 DEG C ~ 1250 DEG C of sintering temperatures, the temperature rise period, in stove, be full of hydrogen or argon gas, the pressure of hydrogen or argon gas is 0.01 ~ 10MPa; After titanium hydride has decomposed or when temperature reaches sintering temperature, start at the uniform velocity vacuumizing in stove, furnace pressure uniform descent, through 2 min ~ 60min, vacuum tightness reaches 1 × 10
-4~ 100Pa, is then incubated 0.5 h ~ 6h in sintering temperature, after sintering, cools to room temperature with the furnace, obtains sintered article;
(5) hot isostatic pressing: after sintering finishes, sintered article is proceeded in hot isostatic pressing stove stove and carries out hip treatment, temperature rise rate with 2 DEG C/min ~ 30 DEG C/min is heated to 600 DEG C ~ 1250 DEG C for the treatment of temps by sintered article from room temperature, pressure is 50 MPa ~ 300MPa, atmosphere is argon gas, and the heat-insulation pressure keeping time under treatment temp is 10min ~ 200min; After hot isostatic pressing finishes, furnace cooling, obtains product.
The described gas of step (1) is preferably nitrogen.
The hard phase powder of the described inhibition crystal of step (1) growth is preferably SiC powder, and wherein to account for the massfraction of mixture be 0.5%-1.5% to SiC powder.
The mass ratio of the described paraffin of step (2) and organic solvent is preferably 2:1 ~ 1:4, more preferably 1:2; Described drying temperature is preferably 10 DEG C ~ 100 DEG C, more preferably 50 ~ 80 DEG C.Described organic solvent is preferably normal heptane.
Base sample compacting tool set in step (2) preferably easily moves back mould and opens lobe mould, and pressing pressure is preferably 30 ~ 90MPa.
The application, if prepare titanium alloy, needs to add other metal-powders, can in the raw material powder of step (1), add, and also can in the dried powder of step (2), add.Step (2) is added after preparing titanium alloy metal-powder used and is obtained powdered alloy in dried powder, then alloy powder is suppressed.
Described metal-powder adds kind and ratio determines according to the proportioning of required titanium alloy, and for example, described metal-powder is yttrium powder, the 0.5%-1% that interpolation quality is described powdered alloy.
Preferably 1 ~ 3 DEG C/min of temperature rise rate in step (3), preferably 150 ~ 250 DEG C of skimming temps, soaking time is 4 ~ 8h preferably.
The preferred hydrogen of degreasing gas in step (3), gas purity preferably 99.99 ~ 99.999%, gas flow is 50 ~ 200ml/min preferably.
Preferably 3 ~ 5 DEG C/min of temperature rise rate in step (4), preferably 0.1 ~ 1MPa of hydrogen or argon pressure, preferably 600 ~ 950 DEG C of sintering temperatures, soaking time is 2 ~ 4h preferably.
Preferably 700 ~ 950 DEG C of hip treatment temperature in step (5), pressure is 100 ~ 200MPa preferably.
Wherein about sintering step: after degreasing finishes, can continue to heat up and carry out sintering if equipment is degreasing-sintering integrated equipment; If degreasing and sintering proceed step by step on distinct device, needs to wait to transfer to after degreasing base cool to room temperature again and carries out sintering in agglomerating plant.Temperature rise rate with 0.5 DEG C/min ~ 20 DEG C/min is heated to 600 DEG C ~ 1250 DEG C of sintering temperatures by base sample from skimming temp, from skimming temp be raised between sintering temperature during this period of time in, in stove, be full of hydrogen or argon gas, the pressure of hydrogen or argon gas is 0.01 ~ 10MPa, must strictly control furnace atmosphere pressure, in order to avoid because titanium hydride decomposing hydrogen causes poor distortion and the cracking defect of producing of base sample external and internal pressure; After titanium hydride has decomposed or when temperature reaches sintering temperature, start at the uniform velocity vacuumizing in stove, furnace pressure uniform descent, through 2min ~ 60min, furnace inner gas pressure is down to 1 × 10
-4~ 100Pa, is incubated 0.5 h ~ 6h in sintering temperature, after sintering, cools to room temperature with the furnace, obtains sintered article;
Airflow milling titanium hydride powder is compared ball milling powder, have pollution less, active large feature, it is stable chemical nature in the time of normal temperature, when low-temperature sintering, sintering character is very good, can quick densifying, and grain-size changes little, so eliminate after its hole with hot-pressing technique, can obtain crystal grain tiny, the product of excellent property.
Compared with prior art, advantage of the present invention is:
(1) low, the good product performance of material cost: titanium hydride powder is the intermediate materials in titanium metallurgical production, and price is relatively low; Airflow milling can be prepared superfine titanium hydride powder in enormous quantities, and products obtained therefrom performance is good.
(2) technique is simple, and production efficiency is high: do not need big scale production equipment, easily realize suitability for industrialized production.
(3) applied widely: this method almost can be prepared all superfine crystal particle titanium alloy materials, there is no too many limitation.
Brief description of the drawings
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is the electron scanning micrograph of the superfine titanium hydride powders of airflow milling of present method employing.
Fig. 2 is the Metallograph after the base sample sintering in example 1.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be further described.Percentage composition described in embodiment is quality percentage composition.
Embodiment 1
Raw material powder is added in the n-heptane solution of paraffin, raw material powder is the superfine titanium hydride powder of airflow milling,
d 50=1.5 μ m, powder morphology is as shown in Figure 1; In solution, the quality of paraffin and the mass ratio of titanium hydride powder are 3:97, titanium hydride powder and solution stirring being put into loft drier after evenly dries and makes normal heptane volatilization, loft drier temperature is 60 DEG C, by dried powder, pack into and easily back out lobe mould and suppress, pressing pressure is 72MPa, dwell time 60s; The base sample suppressing is put into sintering oven, mounted stove is vacuumized with high vacuum system, base sample is in vacuum environment; Start, with the temperature rise rate of 3 DEG C/min, base sample is heated to 150 DEG C from room temperature, when furnace temperature reaches 150 DEG C, continue, with the temperature rise rate of 2 DEG C/min, base sample is heated to 250 DEG C; When furnace temperature reaches 150 DEG C, starting to passing into purity in stove is 99.999% mobile argon gas, and gas flow rate is 25ml/min, and stove internal gas pressure is a normal atmosphere; When furnace reaches 250 DEG C, start, at this temperature insulation 5h, after insulation finishes, to stop continuing to pass into argon gas, continue, with the temperature rise rate of 3 DEG C/min, base sample is heated to 950 DEG C; Furnace is between 150 DEG C to 800 DEG C time, and the air pressure in stove is always a normal atmosphere, when furnace reaches 800 DEG C, start with high vacuum system, stove to be vacuumized, stove internal gas pressure in 30min uniform descent to 10Pa; When furnace reaches 950 DEG C, start at this temperature insulation 2h, after sintering finishes, base sample cools to room temperature with the furnace, and holding stage and temperature dropped to before 500 DEG C, continued stove to vacuumize, and vacuum tightness reaches 1 × 10
-4pa; After stove is cooling, base sample is proceeded in hot isostatic pressing stove, with the temperature rise rate of 10 DEG C/min, base sample is heated to 800 DEG C from room temperature, base sample is at 800 DEG C of insulation 1h, and stove internal gas pressure is 100MPa, and gas is argon gas.Fig. 2 has shown the crystal grain situation that base sample is final.The ultimate constituent of base sample is pure titanium, and average grain size is 4.8 μ m, and tensile strength is 717MPa.
Embodiment 2
Raw material powder is added in the n-heptane solution of paraffin, raw material powder is the superfine titanium hydride powder of airflow milling,
d 50=1.5 μ m, powder morphology is as shown in Figure 1; In solution, the quality of paraffin and the mass ratio of titanium hydride powder are 3:97, titanium hydride powder and solution stirring are put into loft drier after evenly and are dried and make normal heptane volatilization, and loft drier temperature is 60 DEG C; In dried powder, add a small amount of yttrium powder and fully mix, yttrium powder
d 50=8.5 μ m, yttrium opaque amount accounts for 0.8% of powder mix; Mixed powder is packed into and easily backs out lobe mould and suppress, and pressing pressure is 150MPa, dwell time 10s; The base sample suppressing is put into sintering oven, mounted stove is vacuumized with high vacuum system, base sample is in vacuum environment; Start, with the temperature rise rate of 4 DEG C/min, base sample is heated to 150 DEG C from room temperature, when furnace temperature reaches 150 DEG C, continue, with the temperature rise rate of 3 DEG C/min, base sample is heated to 250 DEG C; When furnace temperature reaches 150 DEG C, starting to passing into purity in stove is 99.999% mobile argon gas, and gas flow rate is 100ml/min, and stove internal gas pressure is a normal atmosphere; When furnace reaches 250 DEG C, start, at this temperature insulation 8h, when insulation finishes, to stop continuing to pass into argon gas, continue, with the temperature rise rate of 5 DEG C/min, base sample is heated to 950 DEG C; Furnace is between 250 DEG C to 800 DEG C time, and the air pressure in stove is always a normal atmosphere, when furnace reaches 800 DEG C, start with high vacuum system, stove to be vacuumized, stove internal gas pressure in 10min uniform descent to 10Pa; When furnace reaches 950 DEG C, start at this temperature insulation 3h, after sintering finishes, base sample cools to room temperature with the furnace, and holding stage and temperature dropped to before 500 DEG C, continued stove to vacuumize, and vacuum tightness reaches 1 × 10
-4pa; After stove is cooling, base sample is proceeded in hot isostatic pressing stove, with the temperature rise rate of 30 DEG C/min, base sample is heated to 800 DEG C from room temperature, base sample is at 800 DEG C of insulation 1h, and stove internal gas pressure is 100MPa, and gas is argon gas.The ultimate constituent of base sample is the titanium alloy that contains 0.8% yttrium, and tensile strength is 894MPa.
Embodiment 3
?
d 50in the titanium hydride powder of=30 μ m, add a small amount of
d 50the SiC powder of=10 μ m, the massfraction that SiC accounts for mixed powder is 1%; Mixed powder is added to fragmentation in air-flow grinding machine, broken rear powder
d 50=1.5 μ m, add mixed powder in the n-heptane solution of paraffin; In solution, the quality of paraffin and the mass ratio of powder mix are 5:95, powder and solution stirring are put into loft drier after evenly and are dried and make normal heptane volatilization, and loft drier temperature is 50 DEG C, by dried powder, pack into and easily back out lobe mould and suppress, pressing pressure is 200MPa, dwell time 20s; The base sample suppressing is put into sintering oven, mounted stove is vacuumized with high vacuum system, base sample is in vacuum environment; Start, with the temperature rise rate of 3 DEG C/min, base sample is heated to 250 DEG C from room temperature; When furnace temperature reaches 150 DEG C, starting to passing into purity in stove is 99.999% mobile argon gas, and gas flow rate is 50ml/min, and stove internal gas pressure is a normal atmosphere; When furnace reaches 250 DEG C, start, at this temperature insulation 5h, when insulation finishes, to stop continuing to pass into argon gas, continue, with the temperature rise rate of 4 DEG C/min, base sample is heated to 950 DEG C; Furnace is between 250 DEG C to 800 DEG C time, and the air pressure in stove is always a normal atmosphere, when furnace reaches 800 DEG C, start with high vacuum system, stove to be vacuumized, stove internal gas pressure in 5min uniform descent to 10Pa; When furnace reaches 950 DEG C, start at this temperature insulation 4h, after sintering finishes, base sample cools to room temperature with the furnace, and holding stage and temperature dropped to before 500 DEG C, continued stove to vacuumize, and vacuum tightness reaches 1 × 10
-4pa; After stove is cooling, base sample is proceeded in hot isostatic pressing stove, with the temperature rise rate of 10 DEG C/min, base sample is heated to 850 DEG C from room temperature, base sample is at 850 DEG C of insulation 30min, and stove internal gas pressure is 200MPa, and gas is argon gas.The final average grain size of base sample is 4 μ m, and tensile strength is 774MPa.
Claims (10)
1. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy, it is characterized in that, concrete steps are:
(1) powder process: raw material powder is put into comminution by gas stream crusher machine, obtain
d 50it is the intermediate powder of 0.1 μ m ~ 10 μ m; Described raw material powder is the mixture of titanium hydride powders or titanium hydride powders and other powder, and wherein said other powder refers to and suppresses the hard phase powder of crystal growth and/or prepare titanium alloy metal-powder used; The gas that described micronizer mill uses is one or more in argon gas, nitrogen and hydrogen;
(2) compacting: paraffin is mixed with the organic solvent of solubilized paraffin, obtain solvent; Described intermediate powder is added in described solvent and stirred, obtain mixture; By the dry mixture organic solvent of removing, obtain dried powder, wherein paraffin account for dry after the quality percentage composition of powder be 0.5%-8%, all the other are intermediate powder; Described dried powder is placed on pressing machine and is suppressed by mould, and pressing pressure is 15 MPa ~ 400MPa, obtains base sample after having suppressed;
(3) degreasing: described base sample is put into vacuum sintering furnace and with the temperature rise rate of 0.5 DEG C/min ~ 5 DEG C/min, base sample is heated to 100 DEG C ~ 300 DEG C of skimming temps, be incubated 0.5 h ~ 10h at skimming temp; Wherein, when temperature is before 100 DEG C ~ 200 DEG C, stove internal gas pressure is vacuum, and vacuum tightness is 1 × 10
-4~ 100Pa when temperature is after 100 DEG C ~ 200 DEG C, leads to the degreasing gas that purity is greater than 99.9% in stove, and described degreasing gas is argon gas or hydrogen, and gas flow rate is 20ml/min ~ 20L/min; Reach after degreasing time, stop continuing to pass into gas, degreasing finishes;
(4) sintering: after degreasing finishes, with the temperature rise rate of 0.5 DEG C/min ~ 20 DEG C/min, base sample is heated to 600 DEG C ~ 1250 DEG C of sintering temperatures, the temperature rise period, in stove, be full of hydrogen or argon gas, the pressure of hydrogen or argon gas is 0.01 ~ 10MPa; After titanium hydride has decomposed or when temperature reaches sintering temperature, start at the uniform velocity vacuumizing in stove, furnace pressure uniform descent, through 2 min ~ 60min, vacuum tightness reaches 1 × 10
-4~ 100Pa, is then incubated 0.5 h ~ 6h in sintering temperature, after sintering, cools to room temperature with the furnace, obtains sintered article;
(5) hot isostatic pressing: after sintering finishes, sintered article is proceeded in hot isostatic pressing stove stove and carries out hip treatment, temperature rise rate with 2 DEG C/min ~ 30 DEG C/min is heated to 600 DEG C ~ 1250 DEG C for the treatment of temps by sintered article from room temperature, pressure is 50 MPa ~ 300MPa, atmosphere is argon gas, and the heat-insulation pressure keeping time under treatment temp is 10min ~ 200min; After hot isostatic pressing finishes, furnace cooling, obtains product.
2. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, the described gas of step (1) is nitrogen.
3. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, the hard phase powder of the described inhibition crystal of step (1) growth is SiC powder, and wherein to account for the massfraction of mixture be 0.5%-1.5% to SiC powder.
4. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, the mass ratio of the described paraffin of step (2) and organic solvent is 2:1 ~ 1:4, and described drying temperature is 10 DEG C ~ 100 DEG C, and described organic solvent is normal heptane.
5. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, step (2) is added after preparing titanium alloy metal-powder used and is obtained powdered alloy in dried powder, alloy powder is suppressed again, and described metal-powder adds kind and ratio determines according to the proportioning of required titanium alloy.
6. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, the described pressing pressure of step (2) is 30 ~ 90MPa.
7. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, in step (3), degreasing gas is hydrogen, and gas purity is 99.99 ~ 99.999%, and gas flow is 50 ml/min ~ 200ml/min.
8. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, temperature rise rate in step (4) is 3 DEG C/min ~ 5 DEG C/min, the pressure of hydrogen or argon gas is 0.1 MPa ~ 1MPa, sintering temperature is 600 DEG C ~ 950 DEG C, and soaking time is 2 ~ 4h.
9. airflow milling titanium hydride powder is prepared the method for superfine crystal particle titanium or titanium alloy according to claim 1, it is characterized in that, in step (4) stove, reach after sintering temperature, stove internal gas pressure is vacuum always.
10. the method for preparing superfine crystal particle titanium or titanium alloy according to the described airflow milling titanium hydride powder of one of claim 1-9, is characterized in that, the treatment temp in step (5) is 700 DEG C ~ 950 DEG C, and pressure is 100 MPa ~ 200MPa.
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| CN113102753A (en) * | 2020-01-13 | 2021-07-13 | 天津大学 | Indirect 3D printing tungsten-based alloy part degreasing sintering method |
| US20230150052A1 (en) * | 2021-11-17 | 2023-05-18 | Goodrich Corporation | Systems and methods for high strength titanium rod additive manufacturing |
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