CN106735175A - A kind of mass preparation method of the titanium-based air suction element of hole high - Google Patents
A kind of mass preparation method of the titanium-based air suction element of hole high Download PDFInfo
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- CN106735175A CN106735175A CN201611256309.2A CN201611256309A CN106735175A CN 106735175 A CN106735175 A CN 106735175A CN 201611256309 A CN201611256309 A CN 201611256309A CN 106735175 A CN106735175 A CN 106735175A
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Abstract
The present invention provides a kind of mass preparation method of the titanium-based air suction element of hole high, comprises the following steps：Under argon gas protective condition, titanium valve and the mixture of molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder mix to uniform, obtain the raw material of titanium-based；Under inert gas shielding, the raw material of titanium-based is well mixed with ammonium hydrogen carbonate, adds organic binder bond, form injection feeding；Injection feeding is deposited on modified wire, through cold isostatic compaction, the release demoulding is taken out, and forms blank；Under vacuum conditions, blank is placed in carries out chemical degreasing treatment in trichloro ethylene, take out cooling, obtains chemical degreasing blank；Chemical degreasing blank is carried out into high temperature sintering in vacuum sintering furnace, cooling obtains the titanium-based air suction element of high hole of the porosity higher than 50% after coming out of the stove.Preparation process is simple of the present invention is easy to operate, and the porosity of air suction element is high, and controllability is good, and pumping property is excellent.
Description
Technical field
The invention belongs to getter material technical field, and in particular to a kind of mass of the titanium-based air suction element of hole high
Preparation method.
Background technology
With developing rapidly for electronic technology and vacuum technique, people are to electronic material and the performance of vacuum material
Requirement higher is constantly proposed, and the renewal of gettering material is progressive then as one of key technology for promoting its development.Air-breathing material
Material refers under certain condition, have the material of sp act to some (certain) gases.Because it has excellent usability
Can, make it in the fields such as electronic vacuum technology in occupation of irreplaceable critical role.And due to use environment condition
Badly, performance requirement is strict, improves existing gettering material, development of new gettering material and is closed as numerous scientific workers
Note and the object of research.
Titanium-based nonevaporable getter because with good pumping property, bond strength high, relatively low manufacturing cost, because
This be particularly well-suited to store hydrogen storage equipment, particle accelerator, plasma fuser and some need to maintain the exhaust sealed-off of vacuum
It is the new getter that can not be substituted in existing gettering material in equipment.Titanium molybdenum getter and titanium zirconium vanadium getter are non-titanium-baseds
The study hotspot of evaporable air-absorbing agent, from IV B races element titanium as matrix, while adding, fusing point is high, steam is forced down, itself
Bond strength anti-sintering molybdenum, zirconium, vanadium high etc., because molybdenum is the strong β phases stable element of titanium, its addition is greatly lowered
α → β phase transition temperatures of titanium so that alloy not only has a porosity high, and with the higher hydrogen ratio and very low inhaled
Hydrogen desorption equilibrium pressure, with preferable pumping property, relatively low activationary temperature.But at present, titanium maxter alloy and titanium zirconium vanadium are closed
Gold as the research of getter also in the starting stage, the combination property and mass production capabilities of titanium-based nonevaporable getter with
Foreign countries compare still larger gap.Therefore study highly porous titanium-based air suction element mass production have it is highly important
Meaning.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of mass preparation method of the titanium-based air suction element of hole high,
Using air-breathing powder, ammonium hydrogen carbonate and organic binder bond as raw material, chemical degreasing and vacuum degreasing are combined, will be injected into
Type technology is combined with metal support, and the porosity for preparing air suction element is high, is not less than 50%, and surface area is big, activation
Temperature is low, and gettering rate is high, and gulp capacity is big, and preparation cost is low, can industrialized mass production, the product stability of batch production
Good, economic worth is high.
In order to solve the above technical problems, the technical scheme is that：
A kind of mass preparation method of the titanium-based air suction element of hole high, comprises the following steps：
(1) under argon gas protective condition, by the mixture of titanium valve and molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder, according to
Weight ratio is 7-9:1-3 mixing 10-24h obtains the raw material of titanium-based to uniform；
(2) under inert gas shielding, the raw material of titanium-based prepared by step (1) is well mixed with ammonium hydrogen carbonate, adds
Organic binder bond, forms injection feeding, and the wherein volume fraction of the raw material of titanium-based is 30-70%；
(3) injection feeding prepared by step (2) is deposited on modified wire, through cold isostatic compaction, unloads pressure-off
Mould takes out, and forms blank；
(4) under the vacuum state of vacuum ＜ 5Pa, blank prepared by step (3) is placed in 50-80 DEG C of trichloro ethylene
In carry out chemical degreasing treatment 4-12h, take out cooling, obtain chemical degreasing blank；
(5) chemical degreasing blank prepared by step (4) is carried out into high temperature sintering in vacuum sintering furnace, cooling is obtained after coming out of the stove
The titanium-based air suction element of the hole high to porosity higher than 50%.
Used as the preferred of above-mentioned technical proposal, the particle diameter of titanium valve is 25-45 μm in the step (1).
As the preferred of above-mentioned technical proposal, molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium in mixture in the step (1)
The volume ratio of nickel powder is 1:1:1:1, the average grain diameter of mixture is 45 μm.
Used as the preferred of above-mentioned technical proposal, the particle diameter of ammonium hydrogen carbonate is 20-25 μm in the step (2).
Used as the preferred of above-mentioned technical proposal, inert gas is argon gas, the raw material of the titanium-based, carbon in the step (2)
Sour hydrogen ammonium is 1-19 with the mass ratio of organic binder bond:1：1-19, the well mixed mode is total co-blended 2h, per 0.5h
Rest 5min.
Used as the preferred of above-mentioned technical proposal, organic binder bond is paraffin, high density polyethylene (HDPE), gathers in the step (2)
Propylene and stearic mixture, the wherein mass percent of paraffin are 40-85%, and the mass percent of high density polyethylene (HDPE) is
5-20%, polyacrylic mass percent is 5-20%, balance of stearic acid.
Used as the preferred of above-mentioned technical proposal, the wire being modified in the step (3) is resistance to for surface deposits one layer of densification
The Mo alloying metals silk of high-temperature insulating layer, the dense refractory insulating barrier is the mixture of glass dust and magnesium nitrate, and thickness is
50-300μm。
Used as the preferred of above-mentioned technical proposal, the pressure of cold isostatic compaction is 100-190MPa in the step (3), when
Between be 10-30s.
As the preferred of above-mentioned technical proposal, the vacuum ＜ 7 × 10 of step (5) the high temperature sintering-4Pa, sintering temperature
It is 900-930 DEG C to spend, and soaking time is 15-30min.
Compared with prior art, the invention has the advantages that：
(1) preparation process is simple of the present invention, chemical degreasing and vacuum degreasing are combined, by injection molding technology and metal
Supporter is combined, by changing the viscosity of feeding and the form of metal support, control the shape of air suction element, porosity and
Intensity, and by precise control process of injection molding, it is ensured that the stability of air suction element, high efficiency, realize that high-volume is raw
Produce.
(2) the titanium-based air suction element of hole high prepared by the present invention uses air-breathing powder, ammonium hydrogen carbonate and organic binder bond
As raw material, by adjusting air-breathing powder, ammonium hydrogen carbonate and the ratio of organic binder bond, the porosity of gas absorption cell is manipulated
And intensity, by two kinds of pore formers of ammonium hydrogen carbonate and organic binder bond, it is combined with vacuum thermal debinding with reference to chemical degreasing, can be with
Organic binder bond effectively in removing product, it is to avoid influence of the residual carbon to pumping property simultaneously plays pore-creating effect.
(3) the titanium-based air suction element of hole high prepared by the present invention is processed first through Cold pretreatment, then through high temperature sintering, this
The preparation efficiency that processing method can greatly improve air suction element is planted, production cost is reduced, the dimensional accuracy of air suction element is improved
And inhibition, the consumption of binding agent and ammonium hydrogen carbonate can be effectively reduced, improve the activity of air suction element.
(4) porosity of the titanium-based air suction element of hole high prepared by the present invention is high, is not less than 50%, and surface area is big, swashs
Temperature living is low, and gettering rate is high, and gulp capacity is big, and preparation cost is low, can industrialized mass production, the product stabilization of batch production
Property is good, and economic worth is high.
Specific embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples of the invention and explanation
It is for explaining the present invention but not as a limitation of the invention.
Embodiment 1：
(1) it is 9 according to weight ratio under argon gas protective condition:1, by particle diameter for 25 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 24h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 20 μm of bicarbonates by the raw material of 19 parts of titanium-based and 1 part of particle diameter by weight under argon gas protection
Ammonium is well mixed, and adds 19 parts of organic binder bond, total co-blended 2h, rests 5min per 0.5h, forms injection feeding, organic viscous
Knot agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 70%, high
The mass percent of density polyethylene is 10%, and polyacrylic mass percent is 10%, balance of stearic acid.
(3) injection feeding is deposited on surface to deposit the glass dust that a layer thickness is 50 μm exhausted with magnesium nitrate dense refractory
On the Mo alloying metals silk of edge layer, it is molded through the isostatic cool pressing 10s under 190Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 75 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 5h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 930 DEG C
Knot 15min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Embodiment 2：
(1) it is 7 according to weight ratio under argon gas protective condition:3, by particle diameter for 45 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 24h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 25 μm of ammonium hydrogen carbonate by the raw material of 4 parts of titanium-based and 1 part of particle diameter by weight under argon gas protection
It is well mixed, add 1 part of organic binder bond, total co-blended 2h rests 5min per 0.5h, forms injection feeding, organic adhesive
Agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 70%, highly dense
The mass percent for spending polyethylene is 10%, and polyacrylic mass percent is 10%, balance of stearic acid.
(3) feeding will be injected it will be deposited on surface and will deposit glass dust that a layer thickness is 300 μm and magnesium nitrate dense refractory
On the Mo alloying metals silk of insulating barrier, it is molded through the isostatic cool pressing 30s under 130Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 77 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 5h, takes out cooling, obtains chemical degreasing blank.
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 20 DEG C
Knot 20min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Embodiment 3：
(1) it is 4 according to weight ratio under argon gas protective condition:1, by particle diameter for 30 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 24h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 23 μm of ammonium hydrogen carbonate by the raw material of 1 part of titanium-based and 1 part of particle diameter by weight under argon gas protection
It is well mixed, add 1 part of organic binder bond, total co-blended 2h rests 5min per 0.5h, forms injection feeding, organic adhesive
Agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 40%, highly dense
The mass percent for spending polyethylene is 20%, and polyacrylic mass percent is 20%, balance of stearic acid.
(3) feeding will be injected it will be deposited on surface and will deposit glass dust that a layer thickness is 300 μm and magnesium nitrate dense refractory
On the Mo alloying metals silk of insulating barrier, it is molded through the isostatic cool pressing 20s under 100Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 78 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 5h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 900 DEG C
Knot 30min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Embodiment 4：
(1) it is 7 according to weight ratio under argon gas protective condition:2, by particle diameter for 30 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 15h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 20 μm of ammonium hydrogen carbonate by the raw material of 5 parts of titanium-based and 1 part of particle diameter by weight under argon gas protection
It is well mixed, add 5 parts of organic binder bond, total co-blended 2h rests 5min per 0.5h, forms injection feeding, organic adhesive
Agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 60%, highly dense
The mass percent for spending polyethylene is 15%, and polyacrylic mass percent is 10%, balance of stearic acid.
(3) feeding will be injected it will be deposited on surface and will deposit glass dust that a layer thickness is 250 μm and magnesium nitrate dense refractory
On the Mo alloying metals silk of insulating barrier, it is molded through the isostatic cool pressing 25s under 150Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 65 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 8h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 910 DEG C
Knot 20min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Embodiment 5：
(1) it is 8 according to weight ratio under argon gas protective condition:1, by particle diameter for 45 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 10h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 20 μm of bicarbonates by the raw material of 10 parts of titanium-based and 1 part of particle diameter by weight under argon gas protection
Ammonium is well mixed, and adds 5 parts of organic binder bond, total co-blended 2h, rests 5min per 0.5h, forms injection feeding, organic viscous
Knot agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 75%, high
The mass percent of density polyethylene is 5%, and polyacrylic mass percent is 10%, balance of stearic acid.
(3) feeding will be injected it will be deposited on surface and will deposit glass dust that a layer thickness is 300 μm and magnesium nitrate dense refractory
On the Mo alloying metals silk of insulating barrier, it is molded through the isostatic cool pressing 15s under 190Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 70 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 4h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 900 DEG C
Knot 30min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Embodiment 6：
(1) it is 9 according to weight ratio under argon gas protective condition:2, by particle diameter for 25 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 18h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) it is 25 μm of bicarbonates by the raw material of 10 parts of titanium-based and 1 part of particle diameter by weight under argon gas protection
Ammonium is well mixed, and adds 5 parts of organic binder bond, total co-blended 2h, rests 5min per 0.5h, forms injection feeding, organic viscous
Knot agent is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, and the wherein mass percent of paraffin is 75%, high
The mass percent of density polyethylene is 10%, and polyacrylic mass percent is 5%, balance of stearic acid.
(3) feeding will be injected it will be deposited on surface and will deposit glass dust that a layer thickness is 150 μm and magnesium nitrate dense refractory
On the Mo alloying metals silk of insulating barrier, it is molded through the isostatic cool pressing 15s under 190Mpa pressure, the release demoulding is taken out, and forms blank.
(4) under the vacuum state of vacuum ＜ 5Pa, blank is placed in 60 DEG C of trichloro ethylene to be carried out at chemical degreasing
Reason 12h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 930 DEG C
Knot 20min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
Comparative example：
(1) it is 9 according to weight ratio under argon gas protective condition:1, by particle diameter for 25 μm of titanium valves and average grain diameter are 45 μm
Volume ratio be 1:1:1:The mixture mixing 24h of 1 molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder obtains titanium-based to uniform
Raw material.
(2) under argon gas protection, by weight, by the raw material of 19 parts of titanium-based and 19 parts of paraffin, total co-blended 2h,
5min being rested per 0.5h, be molded through the isostatic cool pressing 10s under 190Mpa pressure, the release demoulding is taken out, formation blank.
(3) chemical degreasing blank is placed in vacuum ＜ 7 × 10-4In the vacuum sintering furnace of Pa, high temperature burning is carried out at 930 DEG C
Knot 15min, cooling obtains the titanium-based air suction element of hole high after coming out of the stove.
After testing, embodiment 1-6 prepare hole high titanium-based air suction element porosity and through 700 DEG C activate after
The result of gettering efficiency is as follows：
As seen from the above table, the porosity of the titanium-based air suction element of hole high prepared by the present invention is high, and gettering efficiency is good.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (9)
1. a kind of mass preparation method of the titanium-based air suction element of hole high, it is characterised in that comprise the following steps：
(1) under argon gas protective condition, by titanium valve and the mixture of molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder, according to weight
Than being 7-9:1-3 mixing 10-24h obtains the raw material of titanium-based to uniform；
(2) under inert gas shielding, the raw material of titanium-based prepared by step (1) is well mixed with ammonium hydrogen carbonate, adds organic
Binding agent, forms injection feeding, and the wherein volume fraction of the raw material of titanium-based is 30-70%；
(3) injection feeding prepared by step (2) is deposited on modified wire, through cold isostatic compaction, the release demoulding takes
Go out, form blank；
(4) under the vacuum state of vacuum ＜ 5Pa, blank prepared by step (3) is placed in 50-80 DEG C of trichloro ethylene
Row chemical degreasing processes 4-12h, takes out cooling, obtains chemical degreasing blank；
(5) chemical degreasing blank prepared by step (4) is carried out into high temperature sintering in vacuum sintering furnace, cooling obtains hole after coming out of the stove
The titanium-based air suction element of high hole of the gap rate higher than 50%.
2. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The particle diameter of titanium valve is 25-45 μm in the step (1).
3. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The volume ratio of molybdenum powder, zirconium vanadium iron powder, zirconium aluminium powder and zirconium nickel powder is 1 in mixture in the step (1):1:1:1, mixture it is flat
Equal particle diameter is 45 μm.
4. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The particle diameter of ammonium hydrogen carbonate is 20-25 μm in the step (2).
5. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
Inert gas is argon gas in the step (2), and the mass ratio of the raw material, ammonium hydrogen carbonate and organic binder bond of the titanium-based is 1-
19:1：1-19, the well mixed mode is total co-blended 2h, and 5min is rested per 0.5h.
6. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
Organic binder bond is paraffin, high density polyethylene (HDPE), polypropylene and stearic mixture, wherein paraffin in the step (2)
Mass percent is 40-85%, and the mass percent of high density polyethylene (HDPE) is 5-20%, and polyacrylic mass percent is 5-
20%, balance of stearic acid.
7. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The wire being modified in the step (3) deposits one layer of Mo alloying metals silk of dense refractory insulating barrier, the cause for surface
Close temperature-resistant insulation layer is the mixture of glass dust and magnesium nitrate, and thickness is 50-300 μm.
8. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The pressure of cold isostatic compaction is 100-190MPa in the step (3), and the time is 10-30s.
9. the mass preparation method of the titanium-based air suction element of a kind of hole high according to claim 1, it is characterised in that：
The vacuum ＜ 7 × 10 of step (5) the high temperature sintering-4Pa, sintering temperature is 900-930 DEG C, and soaking time is 15-
30min。
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