CN104690271B - A kind of power injection molding of inexpensive hydrogenation dehydrogenation titanium powder - Google Patents
A kind of power injection molding of inexpensive hydrogenation dehydrogenation titanium powder Download PDFInfo
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- CN104690271B CN104690271B CN201510074938.2A CN201510074938A CN104690271B CN 104690271 B CN104690271 B CN 104690271B CN 201510074938 A CN201510074938 A CN 201510074938A CN 104690271 B CN104690271 B CN 104690271B
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Abstract
The present invention relates to the forming technology of titanium alloy, a kind of power injection molding of inexpensive hydrogenation dehydrogenation titanium powder is specifically disclosed.The step of technique is：Hydrogenation dehydrogenation titanium powder and alloying element powder, additive powder and binding agent are mixed, feeding is made by mixing, granulation；Then the method for using ultrasonic assistant injection moulding, produces green compact；Remove the binding agent in green compact by solvent degreasing and thermal debinding again；Finally sinter at high temperature, produce finished product.The technique is raw material using cheap hydrogenation dehydrogenation titanium powder, prepares titanium alloy product low cost, is adapted to large-scale industrial production.
Description
Technical field
The present invention relates to the forming technology of titanium alloy, and in particular to a kind of powder injection of inexpensive hydrogenation dehydrogenation titanium powder into
Shape technique.
Background technology
Titanium and its alloy have low-density, high specific strength, highly corrosion resistant, good bio-compatibility, in chemical industry, biology
The fields such as medical treatment, aviation, navigation, automobile have a wide range of applications.But be due to that titanium and its alloy melting point be high, under high temperature chemically
The features such as matter is active, hardness is higher, is considered as industrially difficult to machine material always.The powder injection-molded work of titanium alloy
For a kind of advanced powder metallurgical technique, titanium alloy product with complex shape can be directly produced, it is not necessary to substantial amounts of
Post-processing processing procedure, thus obtained extensive attention in industrial quarters.
In the powder injection forming of titanium alloy, the sized spherical titanium powder manufactured by atomization is widely used.It is this
The impurity content of titanium valve is low, good fluidity, and easy to manufacture goes out qualified titanium alloy product.But sized spherical titanium powder is expensive,
Cause the powder injection forming product of titanium alloy to hold at high price, hinder titanium alloy product promoting the use of in industrial quarters.
In addition to sized spherical titanium powder, industrial quarters has a kind of inexpensive hydrogenation dehydrogenation titanium powder, and its price is the ten of sized spherical titanium powder
/ mono- or so.But the poor fluidity of hydrogenation dehydrogenation titanium powder, it is not easy to shape, and the impurity content such as oxygen, nitrogen, carbon is high, very
Difficulty produces qualified product.
The content of the invention
The technical problems to be solved by the invention are, in order to overcome it is of the prior art it is above-mentioned it is not enough there is provided one kind it is low into
The power injection molding of this hydrogenation dehydrogenation titanium powder.
Above-mentioned technical problem to be solved by this invention is solved by the following technical programs：
A kind of power injection molding of inexpensive hydrogenation dehydrogenation titanium powder, is comprised the following steps：
S1. premix：Hydrogenation dehydrogenation titanium powder, additive powder are carried out being pre-mixed to obtain mixed-powder；Described additive powder
End is rare-earth boride or/and rare earth hydride powder；
S2. knead, granulate：First mixed-powder is heated, binding agent is then added, after mixing is uniform, then passes through comminutor
Manufacture the feeding granulated；
S3. injection moulding：Feeding is heated, is then expelled in mould and shaped using injection machine；Treat that feeding solidifies
After take out, produce green compact；
S4. solvent degreasing, thermal debinding：Green compact are dipped into organic solvent and carry out solvent degreasing；Green compact are then taken out, are dried in the air
Degreasing sintered stove is put into after dry, remaining binding agent is removed by thermal debinding；
S5. sinter：The vacuum of sintering furnace is adjusted, is sintered at high temperature, finished product is obtained after cooling.
The present invention uses rare earth hydride or/and rare-earth boride as additive, in high temperature sintering, these rare earths
Compound can decompose generation rare earth element, and rare earth element can react with such as oxygen nitrogen etc. of the impurity element in hydrogenation dehydrogenation titanium powder, generation
Oxide or nitride distribution improve the intensity of material on crystal boundary.Additionally due to the impurity content in titanium alloy significantly drops
Low, the moulding of material is greatly improved.
Preferably, the rare-earth boride described in S1. is selected from：LaB6, CeB6, PrB6, NdB6, SmB6, EuB6, YB6 and/
Or ZrB6；S1. the rare earth hydride described in is selected from：LaH2, CeH2, PrH2, NdH2, SmH2, EuH2, YH2 and/or ZrH2.
Preferably, the addition of the additive powder in S1. is the 0~1.5% of mixed-powder gross weight.The present invention is added
Micro additive powder, addition can be 0.01%, 0.1%, 0.5%, 1.0%, the 1.5% of mixed-powder gross weight.
Preferably, the heating described in S2. refers to be heated to 120~180 DEG C.
Preferably, the heating described in S3. refers to be heated to 130~160 DEG C.
Preferably, the sintering described in S5., specific method is：The vacuum of sintering furnace is increased to 10-2~10-3Pa, temperature
Degree gradually rises to 1250~1350 DEG C, and cool to obtain finished product after sintering 2~3 hours.
Preferably, alloying element powder is additionally added in S1., with hydrogenation dehydrogenation titanium powder, additive powder be pre-mixed
Mixed-powder.
It is highly preferred that described alloying element powder be aluminium, Fan, Molybdenum, vanadium, tantalum, niobium, iron, manganese, chromium, cobalt, nickel, copper, silicon,
Tin and/or zr element powder.
Most preferably, described alloying element powder is aluminium and the plain powder of vanadium.
It is highly preferred that the addition of the alloying element powder is the 5~30% of mixed-powder gross weight.
The addition species and consumption of alloying element, those skilled in the art can reasonable selections according to actual needs.
Preferably, the particle diameter of above-mentioned hydrogenation dehydrogenation titanium powder, additive powder and alloying element powder is respectively less than 45 microns.
Preferably, the addition of mixed-powder is the 50~60% of mixed-powder and binding agent cumulative volume；Binding agent plus
It is the 40~50% of mixed-powder and binding agent cumulative volume to enter amount；
It is highly preferred that described high polymer binder, contains the high density for accounting for high polymer binder gross weight 45~50%
Polyethylene, 45~50% paraffin and 2~5% stearic acid.
Preferably, the injection moulding described in S3., ultrasonic signal is applied in shaping on mould.
It is highly preferred that the specific method of the application ultrasonic signal on mould is：10~30mm's of mould gate
The transducer of 20~40kHz ultrasonic waves drive is installed in distance.
The method that the present invention employs special ultrasonic assistant shaping in process of injection molding, enhances the stream of feeding
Dynamic property, so as to reduce the defect in green compact, improves the yield rate of green compact.
Preferably, described in S4. solvent degreasing, the specific method of thermal debinding are：Green compact are dipped into hexane solution,
30~45 DEG C are heated to, 6~24 hours are incubated, solvent degreasing is carried out；Green compact are then taken out, degreasing sintered stove is put into after drying,
The temperature of degreasing sintered stove is slowly raised 400~600 DEG C, remaining binding agent is removed by thermal debinding.
Beneficial effect：(1) titanium alloy product that produces of the present invention, density and mechanical property all and use high pure spherical titanium valve
The titanium alloy product of manufacture is similar or even more preferably, therefore can significantly reduce the cost of titanium alloy powder injection moulding.(2) originally
The method that invention employs special ultrasonic assistant shaping in process of injection molding, enhances the mobility of feeding, so that
The defect in green compact is reduced, the yield rate of green compact is improved.
Brief description of the drawings
Fig. 1 is the power injection molding flow chart of inexpensive hydrogenation-dehydrogenation titanium valve.
Fig. 2 is the sintering process flow chart in power injection molding.
Embodiment
The present invention is explained further below in conjunction with specific embodiment, but embodiment does not do any type of limit to the present invention
It is fixed.
In the embodiment of the present invention method of testing of product density referring to：Metal Powder Industries
Federation(MPIF)Standard 42。
In the embodiment of the present invention method of testing of tensile strength referring to：Metal Powder Industries
Federation(MPIF)Standard 50。
In the embodiment of the present invention method of testing of elongation percentage referring to：Metal Powder Industries Federation
(MPIF)Standard 59。
The method of testing of green wares rate is in the embodiment of the present invention：100 are randomly selected from the green compact produced to enter
Row detection, removes and the sample of the defects such as crackle, suture, surface flow liner substantially occurs, calculates gained finished product yield.
Embodiment 1 manufactures the power injection molding of pure titanium parts with inexpensive hydrogenation dehydrogenation titanium powder
Hydrogenation-dehydrogenation titanium valve and the LaB6 powder for accounting for mixed-powder gross weight 1wt.% are well mixed, mixed-powder is obtained,
Then add account for cumulative volume be 45vol.% high polymer binder (50wt.% HDPE, 45wt.% paraffin and
5wt.% stearic acid), metal dust is heated to 160 DEG C first in banbury, HDPE, paraffin and hard is then gradually adding
Resin acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.Carried out at 140 DEG C by way of ultrasonic assistant
Injection moulding, produces green compact (yield rate>90%).In the solution for green compact being dipped into 40 DEG C of n-hexane, 24 hours are incubated
Carry out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.Remove remaining viscous by thermal debinding at 450 DEG C
Tie agent.The vacuum of sintering furnace is increased to 10-3Temperature, is gradually risen to 1320 DEG C, sintering cools after 3 hours by Pa.After sintering
Product density about 97%, tensile strength 550MPa, elongation percentage is 15%.
Embodiment 2 manufactures the power injection molding of Ti6Al4V parts with inexpensive hydrogenation-dehydrogenation titanium valve
Hydrogenation-dehydrogenation titanium valve and account for mixed-powder gross weight be 6wt.% aluminium powder, 4wt.% vanadium powder and
1wt.% LaB6 powder is well mixed, then add account for high polymer binder that cumulative volume is 45vol.% (50wt.%'s
HDPE, 45wt.% paraffin and 5wt.% stearic acid), metal dust is heated to 160 DEG C first in banbury, so
After be gradually added HDPE, paraffin and stearic acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.It is logical at 140 DEG C
The mode for crossing ultrasonic assistant carries out injection moulding, produces green compact (yield rate>90%).Green compact be dipped into 40 DEG C just oneself
In the solution of alkane, it is incubated 24 hours and carries out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.It is logical at 450 DEG C
Cross thermal debinding and remove remaining binding agent.The vacuum of sintering furnace is increased to 10-3Temperature, is gradually risen to 1300 DEG C, burning by Pa
Knot cools after 2.5 hours.Product density about 98% after sintering, tensile strength 895MPa, elongation percentage is 10%.
Embodiment 3 manufactures the power injection molding of pure titanium parts with inexpensive hydrogenation dehydrogenation titanium powder
Hydrogenation-dehydrogenation titanium valve and the YH2 powder for accounting for mixed-powder gross weight 0.5wt.% are well mixed, mixed powder is obtained
End, then add account for cumulative volume be 42vol.% high polymer binder (50wt.% HDPE, 47wt.% paraffin and
3wt.% stearic acid), metal dust is heated to 160 DEG C first in banbury, HDPE, paraffin and hard is then gradually adding
Resin acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.Carried out at 140 DEG C by way of ultrasonic assistant
Injection moulding, produces green compact (yield rate>90%).In the solution for green compact being dipped into 40 DEG C of n-hexane, 24 hours are incubated
Carry out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.Remove remaining viscous by thermal debinding at 450 DEG C
Tie agent.The vacuum of sintering furnace is increased to 10-2Temperature, is gradually risen to 1300 DEG C, sintering cools after 3 hours by Pa.After sintering
Product density about 96%, tensile strength 535MPa, elongation percentage is 13%.
Embodiment 4 manufactures the power injection molding of pure titanium parts with inexpensive hydrogenation dehydrogenation titanium powder
Hydrogenation-dehydrogenation titanium valve and the YH2 powder for accounting for mixed-powder gross weight 0.5wt.% are well mixed, mixed powder is obtained
End, then add account for cumulative volume be 40vol.% high polymer binder (45wt.% HDPE, 50wt.% paraffin and
5wt.% stearic acid), metal dust is heated to 160 DEG C first in banbury, HDPE, paraffin and hard is then gradually adding
Resin acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.Carried out at 140 DEG C by way of ultrasonic assistant
Injection moulding, produces green compact (yield rate>90%).In the solution for green compact being dipped into 40 DEG C of n-hexane, 24 hours are incubated
Carry out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.Remove remaining viscous by thermal debinding at 450 DEG C
Tie agent.The vacuum of sintering furnace is increased to 10-2Temperature, is gradually risen to 1320 DEG C, sintering cools after 3 hours by Pa.After sintering
Product density about 97%, tensile strength 520MPa, elongation percentage is 11%.
Embodiment 5 manufactures the power injection molding of Ti6Al4V parts with inexpensive hydrogenation-dehydrogenation titanium valve
Hydrogenation-dehydrogenation titanium valve and account for mixed-powder gross weight be 6wt.% aluminium powder, 4wt.% vanadium powder and
1.2wt.% ZrH2 powder is well mixed, then add account for high polymer binder that cumulative volume is 50vol.% (45wt.%'s
HDPE, 50wt.% paraffin and 5wt.% stearic acid), metal dust is heated to 180 DEG C first in banbury, so
After be gradually added HDPE, paraffin and stearic acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.It is logical at 160 DEG C
The mode for crossing ultrasonic assistant carries out injection moulding, produces green compact (yield rate>90%).Green compact be dipped into 40 DEG C just oneself
In the solution of alkane, it is incubated 24 hours and carries out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.It is logical at 450 DEG C
Cross thermal debinding and remove remaining binding agent.The vacuum of sintering furnace is increased to 10-3Temperature, is gradually risen to 1300 DEG C, burning by Pa
Knot cools after 2 hours.Product density about 98% after sintering, tensile strength 895MPa, elongation percentage is 12%.
Embodiment 6 manufactures the power injection molding of Ti6Al4V parts with inexpensive hydrogenation-dehydrogenation titanium valve
Hydrogenation-dehydrogenation titanium valve and account for mixed-powder gross weight be 6wt.% aluminium powder, 4wt.% vanadium powder and
0.7wt.% CeB6 powder is well mixed, then add account for high polymer binder that cumulative volume is 40vol.% (50wt.%'s
HDPE, 48wt.% paraffin and 2wt.% stearic acid), metal dust is heated to 150 DEG C first in banbury, so
After be gradually added HDPE, paraffin and stearic acid.After mixing is uniform, then the feeding granulated by comminutor manufacture.It is logical at 130 DEG C
The mode for crossing ultrasonic assistant carries out injection moulding, produces green compact (yield rate>90%).Green compact be dipped into 40 DEG C just oneself
In the solution of alkane, it is incubated 24 hours and carries out solvent degreasing.Green compact are then taken out, degreasing sintered stove is put into after drying.It is logical at 450 DEG C
Cross thermal debinding and remove remaining binding agent.The vacuum of sintering furnace is increased to 10-3Temperature, is gradually risen to 1250 DEG C, burning by Pa
Knot cools after 2 hours.Product density about 97% after sintering, tensile strength 868MPa, elongation percentage is 9%.
Claims (1)
1. a kind of power injection molding of inexpensive hydrogenation dehydrogenation titanium powder, it is characterised in that comprise the following steps：
S1. premix：Hydrogenation dehydrogenation titanium powder, additive powder, alloying element powder are carried out being pre-mixed to obtain mixed-powder；Described
Additive powder is rare-earth boride or/and rare earth hydride powder；
S2. knead, granulate：Mixed-powder heats in elder generation, then adds binding agent, after mixing is uniform, then is manufactured by comminutor
The feeding granulated；
S3. injection moulding：Feeding is heated, is then expelled in mould and shaped using injection machine；Taken after after feeding solidification
Go out, produce green compact；
S4. solvent degreasing, thermal debinding：Green compact are dipped into organic solvent and carry out solvent degreasing；Green compact are then taken out, after drying
Degreasing sintered stove is put into, remaining binding agent is removed by thermal debinding；
S5. sinter：The vacuum of sintering furnace is adjusted, is sintered at high temperature, finished product is obtained after cooling；
In S1, the addition of additive powder is the 0 ~ 1.5% of mixed-powder gross weight；Described rare-earth boride is selected from：
LaB6, CeB6, PrB6, NdB6, SmB6, EuB6, YB6And/or ZrB6；Described rare earth hydride is selected from：LaH2,
CeH2, PrH2, NdH2, SmH2, EuH2, YH2And/or ZrH2；Described alloying element powder be aluminium, Fan, Molybdenum, vanadium, tantalum,
Niobium, iron, manganese, chromium, cobalt, nickel, copper, silicon, tin and/or zr element powder；The addition of alloying element powder is mixed-powder gross weight
The 5 ~ 30% of amount；The particle diameter of the hydrogenation dehydrogenation titanium powder, additive powder and alloying element powder is respectively less than 45 microns；
In S2, described heating refers to be heated to 120 ~ 180 DEG C；The addition of mixed-powder is that mixed-powder and binding agent are total
The 50 ~ 60% of volume；The addition of binding agent is the 40 ~ 50% of mixed-powder and binding agent cumulative volume；
Described binding agent is high polymer binder, containing the high density polyethylene (HDPE) for accounting for high polymer binder gross weight 45 ~ 50%,
45 ~ 50% paraffin and 2 ~ 5% stearic acid；
In S3, described heating refers to be heated to 130 ~ 160 DEG C；Described injection moulding, applies in shaping on mould
Ultrasonic signal；It is described on mould apply ultrasonic signal specific method be：In the mm of mould gate 10 ~ 30 distance
The transducer of 20 ~ 40 kHz ultrasonic waves drive is installed；
The specific method of solvent degreasing, thermal debinding described in S4 is：Green compact are dipped into hexane solution, it is heated to 30 ~
45 DEG C, 6 ~ 24 hours are incubated, solvent degreasing is carried out；Green compact are then taken out, degreasing sintered stove is put into after drying, degreasing sintered stove
Temperature be slowly raised 400 ~ 600 DEG C, remaining binding agent is removed by thermal debinding；
S5. the sintering described in, specific method is：The vacuum of sintering furnace is increased to 10-2~10-3Pa, temperature gradually rises to
1250 ~ 1350 DEG C, cool to obtain finished product after sintering 2 ~ 3 hours.
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| CN1172012C (en) * | 2002-12-19 | 2004-10-20 | 北京科技大学 | Method for synthesizing NiTi shape memory alloy porous material |
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| CN102534333A (en) * | 2012-01-05 | 2012-07-04 | 西安建筑科技大学 | Method for preparing fine-grain high-density TZM (Titanium-Zirconium-Molybdenum Allo) alloy |
| CN203526525U (en) * | 2013-10-25 | 2014-04-09 | 西南交通大学 | Device for manufacturing gradient materials |
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Effective date of registration: 20220211 Address after: 518000 building B, chuangxuan Industrial Park, Baihuayuan Road, Guangming Street, Guangming New District, Shenzhen City, Guangdong Province Patentee after: SHENZHEN AILIJIA MATERIALS TECHNOLOGY Co.,Ltd. Address before: 518055 428, second scientific research building, Department of materials, South University of science and technology, No. 1088, Xili Xueyuan Avenue, Nanshan District, Shenzhen, Guangdong Province Patentee before: Yu Peng |