CN108050043A - A kind of vacuum extractor, pumped vacuum systems and its vacuum pumping method - Google Patents
A kind of vacuum extractor, pumped vacuum systems and its vacuum pumping method Download PDFInfo
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- CN108050043A CN108050043A CN201810009145.6A CN201810009145A CN108050043A CN 108050043 A CN108050043 A CN 108050043A CN 201810009145 A CN201810009145 A CN 201810009145A CN 108050043 A CN108050043 A CN 108050043A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
- F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
- F04B37/00—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00
- F04B37/06—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00 for evacuating by thermal means
- F04B37/08—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00 for evacuating by thermal means by condensing or freezing, e.g. cryogenic pumps
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
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- Chemical Kinetics & Catalysis (AREA)
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- Organic Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Compressors, Vaccum Pumps And Other Relevant Systems (AREA)
Abstract
The invention discloses a kind of vacuum extractor (100), including：Cryogenic pump (101), air entry are communicated to the exhaust outlet of vacuum chamber (200), for being evacuated vacuum chamber (200) so as to reach vacuum in vacuum chamber (200)；Forerunner pumps (102), and air entry divides two-way, is connected to the exhaust outlet of cryogenic pump (101) all the way, and another way is connected to the exhaust outlet of vacuum chamber (200)；Preceding step valve (103) is arranged on the pipeline that forerunner is pumped between (102) and vacuum chamber (200)；Regeneration valve (104) is arranged on the pipeline that forerunner is pumped between (102) and cryogenic pump (101).The vacuum extractor of the present invention is worked at the same time using cryogenic pump and forerunner's pump, improve the pumping efficiency of the device, the gas trapped in extraction cryogenic pump in time and the gas of accumulation are pumped by forerunner, reduce the heat load of cryogenic pump, shorten the recovery time of cryogenic pump so that cryogenic pump being capable of the long-time service in the environment of high temperature ventilates environment.
Description
Technical field
The present invention relates to vacuum pumping technology field more particularly to a kind of vacuum extractor, pumped vacuum systems and its vacuumize
Method.
Background technology
Electro beam physics vapour deposition (EB-PVD) technology is that the vacuum chamber in equipment is extracted vacuum by vacuum pump, is reached
To after certain vacuum level requirements, electronics is generated with the cathode filament of electric current heating electron gun, negatively charged electron beam is at a high speed
During flying to high potential anode, accelerate by acceleration pole, focused on further through electromagnetic lens, the power increase of electron beam, then
After secondary focusing, energy density is up to 105W/m2More than.High-energy density electron beam makes target in part microsecond
Temperature raises up to ten thousand degrees Celsius, even if target is placed in cold-crucible, heat has little time to spread within the short time, target moment
It is melted and gentle turns to steam.Steam is on the deposition rate of 4um/min~10um/min to substrate under magnetic deflection field effect
And form coating.
In the prior art, generally use diffusion pump and molecular pump are taken out the vacuum chamber of electro beam physics vapour deposition equipment true
Sky, but the pumping efficiency of diffusion pump and molecular pump it is low, it is necessary to time it is long, it is not easy to it is true to obtain the minimum cleaning of limiting pressure
It is empty.Cryogenic pump can obtain the cleaning vacuum that the speed of exhaust is maximum, limiting pressure is minimum, thus be widely used it is general, it is but existing
Have in technology, cryogenic pump is usually applied to low temperature environment, and the vacuum chamber of electro beam physics vapour deposition equipment leads to oxygen for high temperature
Environment, it is thus impossible to which cryogenic pump to be directly applied to the vacuum chamber of electro beam physics vapour deposition equipment, reason is as follows：
1st, since cryogenic pump is the vacuum pump using low-temperature surface condensed gas, refrigerant is helium, utilizes helium
Captured gas achievees the purpose that pumping, and the normal working temperature of helium is 10K or so, and hot environment can influence the work of helium
Make, therefore cryogenic pump is not suitable for using in hot environment.
2nd, the vacuum drying oven of electro beam physics vapour deposition equipment needs logical oxygen to cross metal oxide to steam during the work time
Oxygen supply, and the vacuum environment of logical oxygen can cause gas to accumulate.It, will not be actively since the principle that cryogenic pump vacuumizes is trapping type
Exhaust, if cryogenic pump can cause the exhaust velocity of cryogenic pump to continuously decrease used in the environment of ventilation, therefore cryogenic pump is unsuitable for
It is used for a long time in the environment of ventilation.
Therefore, the heat load of cryogenic pump how is reduced, shortens the recovery time of cryogenic pump so that cryogenic pump can be in high temperature
Long-time service under ventilation environment is the technical issues of those skilled in the art are badly in need of solving.
The content of the invention
(1) goal of the invention
It is low by setting the object of the present invention is to provide a kind of vacuum extractor, pumped vacuum systems and vacuum pumping method
Temperature pump is evacuated vacuum chamber, makes the vacuum degree that requirement is rapidly achieved in vacuum chamber, is used in combination, carried with forerunner's pump by cryogenic pump
The pumping efficiency of the high device, while forerunner's pump is worked at the same time with cryogenic pump, the gas that extraction cryogenic pump traps in time
With the gas of accumulation, the heat load of cryogenic pump is reduced, shortens the recovery time of cryogenic pump, solves prior art high temperature
Heat load under logical oxygen environment causes the recovery time of cryogenic pump progressively longer so that cryogenic pump cannot be in the case where high temperature leads to oxygen environment
The technical issues of long-time service.
(2) technical solution
To solve the above problems, the first aspect of the present invention provides a kind of vacuum extractor, including:Cryogenic pump is inhaled
Gas port is communicated to the exhaust outlet of vacuum chamber, for being evacuated the vacuum chamber so as to reach vacuum in the vacuum chamber；Forerunner pumps,
Its air entry divides two-way, is connected to the exhaust outlet of the cryogenic pump all the way, and another way is connected to the exhaust outlet of the vacuum chamber；Before
Step valve is arranged on the pipeline between forerunner's pump and the vacuum chamber；Regeneration valve is arranged on forerunner's pump and institute
It states on the pipeline between cryogenic pump.By the way that cryogenic pump is set to be evacuated vacuum chamber, make the vacuum that requirement is rapidly achieved in vacuum chamber
Degree is used in combination, the pumping efficiency of the device improved by cryogenic pump with forerunner's pump, while forerunner's pump and cryogenic pump are simultaneously
Work extracts the gas that cryogenic pump traps and the gas accumulated out, reduces the heat load of cryogenic pump, shorten cryogenic pump in time
Recovery time.
Further, main control valve is provided in the cryogenic pump, for controlling pipeline between the cryogenic pump and the vacuum chamber
Break-make.
Further, forerunner's pump includes：Lobe pump, air entry divide two-way, are connected to the row of the cryogenic pump all the way
Gas port, another way are connected to the exhaust outlet of the vacuum chamber；Mechanical pump, air entry are connected to the exhaust outlet of the lobe pump.
Further, the vacuum extractor further includes vacuum meter, is arranged between the cryogenic pump and the regeneration valve
Pipeline on, for detecting the vacuum degree in the pipeline.
Further, the vacuum extractor further includes the first cold-trap, be arranged on the preceding step valve and the vacuum chamber it
Between pipeline on, for absorbing the vapor in the vacuum chamber, to reduce the heat load of the cryogenic pump.
Further, the vacuum extractor further includes the second cold-trap, be arranged on the cryogenic pump and the vacuum chamber it
Between pipeline on, for stopping the oil vapour volatilized in the vacuum pump；Heating element is provided in second cold-trap, is used
It heats to remove the coagulation in the coagulation to the second cold-trap surface.
Further, heating element is provided in second cold-trap, added for the coagulation to the second cold-trap surface
Heat is to remove the coagulation.
Another aspect provides a kind of pumped vacuum systems, including vacuum extractor and vacuum described above
Room；The exhaust outlet of the vacuum chamber is connected with the air entry of the vacuum extractor.
Further, the exhaust outlet of the vacuum chamber is provided with shutter, for reducing the vacuum chamber to the cryogenic pump
Heat radiation.
Further, cooling-part is provided on the outer wall of the vacuum chamber, for reducing the temperature of the vacuum chamber.
Further, having heaters is set in the vacuum chamber, for heating sample.
It is yet another aspect of the present invention to provide a kind of vacuum pumping method, for pumped vacuum systems described above, including with
Lower step：
Main control valve and preceding step valve are closed, opens regeneration valve, starts mechanical pump and lobe pump, when the vacuum degree of cryogenic pump reaches
During the first preset value, the regeneration valve is closed；
Start the cryogenic pump, make the compressor operating in the cryogenic pump, until the helium temperature in the cryogenic pump
Reach operating temperature；
The preceding step valve is opened, the vacuum chamber is taken out in advance using the mechanical pump, treats the vacuum of the vacuum chamber
After degree reaches the second preset value, when opening the lobe pump and being evacuated to vacuum degree and reach three preset values, the preceding step valve is closed,
Open the main control valve；
Heater in the vacuum chamber is started to work, and when temperature reaches the first preset temperature value, opens oxygen valve；
When helium temperature gos up to the second preset temperature value, mechanical pump and lobe pump are opened, and opens regeneration valve.
(3) advantageous effect
The above-mentioned technical proposal of the present invention has following beneficial technique effect：
Vacuum extractor provided by the invention, pumped vacuum systems and vacuum pumping method, by setting cryogenic pump to vacuum
Room is evacuated, and since cryogenic pump can rapidly adsorb steam, oil vapour, shortens pumpdown time, is made to be rapidly achieved in vacuum chamber and be wanted
The vacuum degree asked is used in combination, the pumping efficiency of the device improved by cryogenic pump and forerunner pump, at the same forerunner pump with it is low
Temperature pump works at the same time, and can extract the gas of accumulation in gas and cryogenic pump that cryogenic pump traps out in time, reduce cryogenic pump
Heat load shortens the recovery time of cryogenic pump, to maintain the high-efficiency air suction efficiency that cryogenic pump is ventilated in high temperature under environment so that
Cryogenic pump being capable of the long-time service in the environment of high temperature ventilation.By the vacuum extractor of the present invention, pumped vacuum systems and take out true
Short side method is applied to electro beam physics vapour deposition equipment so that the vacuum chamber of electro beam physics vapour deposition equipment can be obtained quickly
Higher vacuum is obtained, therefore can effectively ensure to heat the temperature and quality of sample；Due to being provided with oxygen valve in vacuum chamber, lead to
It crosses oxygen valve and locally leads to oxygen for vacuum chamber, improve the oxygen saturation steamed and cross metal oxide；Since cryogenic pump can rapidly be inhaled
Attached water vapour, oil vapour, therefore the vacuum pumping rate of vacuum chamber is can greatly improve, vacuum-deposited quality is effectively improved, is carried
The interface bond strength of high substrate and coating, so as to which the quality of sample is crossed in the steaming for improving acquisition.
Description of the drawings
Fig. 1 is the structure diagram of a kind of vacuum extractor that the embodiment of the present invention one provides and vacuum chamber；
Fig. 2 is a kind of method flow diagram of vacuum pumping method provided by Embodiment 2 of the present invention；
Fig. 3 is the temperature of the cryogenic pump of the cryogenic pump and common usage in vacuum pumping method provided by Embodiment 2 of the present invention
The curve comparison figure changed over time with vacuum degree.
Reference numeral：
100th, vacuum extractor, 101, cryogenic pump, 101a, main control valve, 102, forerunner's pump, 102a, lobe pump, 102b, machine
Tool pumps, and 103, preceding step valve, 104, regeneration valve, 105, vacuum meter, the 106, first cold-trap, the 107, second cold-trap, 200, vacuum chamber,
201st, shutter, 202, cooling-part, 203, heater, 203a, burner hearth, 203b, resistance wire, 204, oxygen valve, 205, first
Temperature-measuring part, the 206, second temperature-measuring part, 207, crucible, 208, crucible cooling-part.
Specific embodiment
Understand to make the object, technical solutions and advantages of the present invention clearer, With reference to embodiment and join
According to attached drawing, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit this hair
Bright scope.In addition, in the following description, the description to known features and technology is omitted, to avoid this is unnecessarily obscured
The concept of invention.
Before detailed description of the present invention vacuum extractor, electro beam physics vapour deposition (EB-PVD) skill is introduced first
The characteristics of art technique：
1. the raising of electron beam generator power processes up to higher temperature material, can almost evaporate all substances,
(such as tungsten, platinum) can also utilize the technique to evaporate even if the relatively low element of saturated vapour pressure (such as Mo, Nb)；
2. beam power can easily be accommodated, beam spot size and position are easily controllable, are conducive to accurately control coating layer thickness；
3. crucible uses water cooling, chemically reacted so as to avoid evaporation material under high temperature with crucible, can also avoid earthenware
Crucible exhaust pollution film layer；
4. being heated the substrate using electron beam, substrate temperature can be stablized, it is easily controllable, sedimentary is avoided from heating source
Pollution；
5. with other evaporation coating method ratios, evaporation rate and sedimentation rate height are (respectively up to 10kg/h~15kg/h and 100 μ
M/min~150 μm/min), good process repeatability；The particularly appearance of high-power electron gun, make to prepare large-sized plate with
And multilayer material becomes a reality；
6. the atomic group energy evaporated in deposition process is relatively low, weakens bed boundary diffusion, immixture, be conducive to obtain
Multilayer material with clear, bright and sharp interface；
7. select appropriate technological parameter, can obtain with by the ingredient of evaporation material is identical, constituent content is basically identical
Coating；
8. there is higher combination power between substrate and coating, herein, substrate refers to the sample of preparation vapor deposition；
9. the deposition of coating carries out under vacuum conditions, be conducive to prevent pollution and the oxygen of substrate and coating material
Change, therefore the higher coating of quality can be obtained；
10. the strain tolerance limit of obtained coating is high, significantly improve the thermal shock resistance of coating, better than plasma spray heat
Hinder the strength of coating prepared.
Heat load in the vacuum chamber of electro beam physics vapour deposition equipment mostlys come from three aspects：
1. the heat radiation from furnace body side；
2. under viscous stream mode, gas molecule carries away heat；
3. heat transfer and radiations heat energy from pumping hole pipeline.
Since the heat load of above-mentioned three aspects so that the recovery time of cryogenic pump is progressively longer.Wherein, 3. heat source can lead to
The elimination of increase water-cooling structure is crossed, but if it is desired that cryogenic pump long-time service in the case where high temperature leads to the vacuum chamber environment of oxygen, just necessary
Solve above-mentioned 1. 2. two kinds of heat loads.
The embodiment of the invention discloses a kind of vacuum extractor, a kind of pumped vacuum systems and a kind of vacuum pumping method.With
It is lower to be described in detail respectively：
Embodiment one
The present embodiment introduces the vacuum extractor of the present invention and vacuumizes and be by taking electro beam physics vapour deposition equipment as an example
System.
Fig. 1 is the structure diagram of a kind of vacuum extractor that the embodiment of the present invention one provides and vacuum chamber.
Fig. 1 is refer to, the present embodiment provides a kind of vacuum extractor 100, including：Cryogenic pump 101, forerunner's pump 102, prime
Valve 103, regeneration valve 104.
Cryogenic pump 101, air entry are communicated to the exhaust outlet of vacuum chamber 200, for being evacuated vacuum chamber 200 so that vacuum
Reach vacuum in room 200.
In the present embodiment, vacuum chamber 200 is the vacuum drying oven of electro beam physics vapour deposition equipment.But the present invention is not with this
For limitation, vacuum chamber 200 can be the device that all needs vacuumize, and include but not limited to vacuum drying oven, vacuum cavity.
Fig. 1 is refer to, main control valve 101a is provided in cryogenic pump 101, for controlling the cryogenic pump 101 and vacuum chamber 200
Between pipeline break-make.
Forerunner's pump 102, air entry divides two-way, is connected to the exhaust outlet of cryogenic pump 101 all the way, for extracting cryogenic pump out
The gas of accumulation, to reduce the temperature of cryogenic pump 101, reaches reduction cryogenic pump in 101 gases trapped and cryogenic pump 101
The purpose of 101 heat loads, the high-efficiency air suction efficiency that cryogenic pump 101 is maintained to ventilate in high temperature under environment so that cryogenic pump 101 is applicable in
In high temperature ventilation environment.Another way is connected to the exhaust outlet of vacuum chamber 200, for being evacuated in advance to vacuum chamber 200, it is therefore an objective to so that
Reach certain vacuum degree in vacuum chamber 200, create conditions for the work of cryogenic pump 101.
Specifically, in the present embodiment, forerunner's pump 102 includes lobe pump 102a and mechanical pump 102b.
The air entry of lobe pump 102a divides two-way, is connected to the exhaust outlet of cryogenic pump 101 all the way, and another way is connected to vacuum
The exhaust outlet of room 200.
The air entry of mechanical pump 102b is connected to the exhaust outlet of lobe pump 102a.
Specifically, being first evacuated in advance to vacuum chamber 200 by mechanical pump 102b, reach certain vacuum degree, while mechanical pump
102b can also extract the gaseous impurity in vacuum chamber 200, create conditions for the work of lobe pump 102a.Lobe pump 102a is to vacuum
The further pre- pumping of room 200, obtains certain vacuum degree, creates conditions for the work of cryogenic pump 101.
Meanwhile mechanical pump 102b can also extract the gaseous impurity in vacuum chamber 200, item is created in the work for being lobe pump 102a
Part.
In the present embodiment, preceding step valve 103 is arranged on the pipeline between forerunner's pump 102 and vacuum chamber 200, for controlling
The break-make of pipeline between forerunner's pump 102 and vacuum chamber 200.
Specifically, preceding step valve 103 is arranged on the pipeline between the air entry of lobe pump 102a and the exhaust outlet of vacuum chamber 200
On, for controlling the break-make of the pipeline between lobe pump 102a and vacuum chamber 200, the vacuum degree in vacuum chamber 200 is extracted into
The environment of 101 Effec-tive Function of cryogenic pump.
In the present embodiment, regeneration valve 104 is arranged on the pipeline between forerunner's pump 102 and cryogenic pump 101, for controlling
The break-make of pipeline between forerunner's pump 102 and cryogenic pump 101.
Specifically, regeneration valve 104 is arranged on the pipeline between the air entry of lobe pump 102a and the exhaust outlet of cryogenic pump 101
On, for controlling the break-make of the pipeline between lobe pump 102a and cryogenic pump 101, trapped to extract cryogenic pump 101 out in time
Gas and cryogenic pump 101 in accumulation gas.
In the present embodiment, which further includes vacuum meter 105, is arranged on cryogenic pump 101 and regeneration valve
On pipeline between 104, for detecting the vacuum degree in the pipeline.
In the present embodiment, which further includes：
First cold-trap 106 is arranged on preceding pipeline between step valve 103 and vacuum chamber 200, for absorbing vacuum chamber
Vapor in 200, to reduce the heat load of cryogenic pump 101.
In the present embodiment, which further includes：
Second cold-trap 107 is arranged on the pipeline between cryogenic pump 101 and vacuum chamber 200, for stopping vacuum pump
The oil vapour volatilized in 101.
Specifically, vacuum pump 101 can volatilize oil vapour when working, oil vapour is encountered 107 postcooling of the second cold-trap and is become
Fluid oil is simultaneously flowed back to along cold-trap wall in vacuum pump 101, and oil vapour is avoided to enter the environment that vacuum chamber 200 pollutes vacuum chamber 200.
In the present embodiment, heating element is provided in the second cold-trap 107, for the condensation to 107 surface of the second cold-trap
Object heats to remove coagulation.
Fig. 1 is refer to, the present embodiment also provides a kind of pumped vacuum systems, including 100 He of vacuum extractor described above
Vacuum chamber 200.
Wherein, the exhaust outlet of vacuum chamber 200 is connected with the air entry of vacuum extractor 100, right using vacuum extractor 100
Vacuum chamber 200 vacuumizes so that vacuum chamber 200 obtains higher vacuum degree.
Specifically, the air entry of vacuum extractor 100 includes the air entry of cryogenic pump 101 and the air-breathing of lobe pump 102a
Mouthful.The exhaust outlet of vacuum chamber 200 respectively with the air entry of the cryogenic pump 101 in vacuum extractor 100 and lobe pump 102a
Air entry connects.
In the present embodiment, the exhaust outlet of the vacuum chamber 200 is provided with shutter 201, for reducing vacuum chamber 200 to low
The heat radiation of temperature pump 101.
In the present embodiment, cooling-part 202 is provided on the outer wall of the vacuum chamber 200, for reducing vacuum chamber 200
Temperature reduces heat radiation of the vacuum chamber 200 to cryogenic pump 101 by reducing the temperature of vacuum chamber 200.
Optionally, cooling-part 202 reduces the temperature of vacuum chamber 200 by the way of recirculated cooling water.But the present invention
System is not limited, cooling-part 202 can also reduce the temperature of vacuum chamber 200 using other types of cooling.
Optionally, cooling-part 202 includes：First circulation water pipe, second circulation water pipe, inlet and outlet.
Specifically, first circulation water pipe is arranged on vacuum chamber 200 on the side wall of 101 one side of cryogenic pump, for reducing
The temperature of vacuum chamber 200, while also it is used for absorbing the heat transfer and radiations heat energy of 101 pumping hole pipeline of cryogenic pump.Second circulation water
Pipe is arranged on the side wall of the one side opposite with first circulation water pipe, for reducing the temperature of vacuum chamber 200.Water inlet and water outlet
Mouth is arranged on the roof of vacuum chamber 200, for being connected respectively with extraneous cooling water source and outlet pipe.First circulation water pipe is set
There are the first water inlet end and the first water outlet, second circulation water pipe is provided with the second water inlet end and the second water outlet, the first water inlet end
It is connected with the second water inlet end by water inlet with extraneous cooling water source, the first water outlet and the second water outlet are by water outlet and outside
Boundary's outlet pipe connection.
In the present embodiment, heater 203 is additionally provided in vacuum chamber 200, for heating sample, reaches its surface temperature
To 1000 DEG C or so, herein, sample refers to the sample of preparation vapor deposition, i.e. substrate.
Optionally, heater 203 is three-dimensional resistance pharoid, but the present invention is not limited system, heater 203
Or the heater of other structures.
Specifically, heater 203 includes：Burner hearth 203a and resistance wire 203b.
Burner hearth 203a is arranged in vacuum chamber 200.
Optionally, the shape of burner hearth 203a is cylindrical shape, including top plate and side wall.But the present invention is not limited system, stove
Thorax 203a or other shapes.
Optionally, the material of burner hearth 203a is corundum ceramic, for reducing the heat radiation of resistance wire 203b.But the present invention is not
As limitation, burner hearth 203a or other can reduce the material of heat radiation.
Resistance wire 203b is arranged in burner hearth 203a.
Optionally, resistance wire 203b uses the quartz glass seal of tube, for preventing the material of resistance wire 203b under high temperature from expanding
It is scattered to pollution vacuum environment in vacuum chamber 200.But the present invention is not limited system, and resistance wire 203b can also use other forms
Sealing.
In the present embodiment, oxygen valve 204 is additionally provided in vacuum chamber 200, is arranged on the burner hearth 203a of heater 203
It is interior, it is that the evaporation metal oxide of electro beam physics vapour deposition equipment supplies oxygen for locally leading to oxygen in vacuum chamber 200, with
Improve the oxygen saturation steamed and cross metal oxide.
Optionally, the oxygen flow that oxygen valve 204 provides is up to 100sccm.
Specifically, oxygen valve 204 is the situation of metal oxide for target.Due to electro beam physics vapour deposition equipment
It is usually used in evaporation metal oxide, at this time with beam bombardment metal oxide, it is made to generate high-order then vaporization.Super
In high vacuum chamber, the metal oxide of vaporization can generate deoxidation phenomenon due to vapour pressure, and the coating for causing to actually obtain is in ingredient
The upper meeting with design generates segregation.Therefore, in burner hearth 203a oxygen valve 204 is set to lead to oxygen, it is ensured that be aoxidized in evaporation metal
It is unlikely to deoxidation during object.
In the present embodiment, vacuum chamber 200 further includes the first temperature-measuring part 205, is arranged on the burner hearth of heater 203
On the inner wall of 203a, for the heating temperature of HEATER FOR MEASURING 203.
Specifically, since the environment residing for heater 203 is relatively closed, main thermaltransmission mode is radiates, burner hearth 203a
Interior temperature gradient is low, and therefore, what the first temperature-measuring part 205 measured is both the heating temperature and sample temperature of heater 203.
Optionally, the first temperature-measuring part 205 is thermocouple, but the present invention is not limited system, the first temperature-measuring part 205
Can be other temperature elements.
In the present embodiment, vacuum chamber 200 further includes the second temperature-measuring part 206, is arranged on the inner wall of vacuum chamber 200
On, for measuring the inner wall temperature of vacuum chamber 200, when temperature is more than alarm temperature, start alarm.
Optionally, the second temperature-measuring part 206 is thermocouple, but the present invention is not limited system, the second temperature-measuring part 206
Can be other temperature elements.
In the present embodiment, crucible 207 and crucible cooling-part 208 are additionally provided in the vacuum chamber 200.
Crucible 207, it is corresponding with 203 position of heater, for placing target.In the present embodiment, target is metal
Oxide.
In the present embodiment, crucible 207 is additionally provided with pedestal.
Optionally, the pedestal of crucible 207 is made of asbestos shingle, for heat-insulated.
Crucible cooling-part 208, the pedestal close to crucible 207 is set, for cooling down the pedestal of crucible 207, to ensure
The normal operation of the electronic equipment of the base-adjacent of crucible 207 such as electron gun.
Optionally, crucible cooling-part 208 reduces the temperature of the pedestal of crucible 207 by the way of recirculated cooling water.
But the present invention is not limited system, and crucible cooling-part 208 can also reduce the pedestal of crucible 207 using other types of cooling
Temperature.
Specifically, crucible cooling-part 208 be the 3rd circulating water pipe, the 3rd circulating water pipe be provided with the 3rd water inlet end and
3rd water outlet.3rd water inlet end is connected to the water inlet of cooling-part 202, and the 3rd water outlet is connected to cooling-part 202
Water outlet.
Vacuum extractor 100 in the present embodiment is with strong applicability, it is not limited to electro beam physics vapour deposition equipment
Vacuum chamber 200, be also applied for other need high temperature ventilation environment vacuum system.
Embodiment two
Fig. 2 is a kind of method flow diagram of vacuum pumping method provided by Embodiment 2 of the present invention
Fig. 2 is refer to, the present embodiment provides a kind of vacuum pumping method, the pumped vacuum systems suitable for embodiment one, bag
Include following steps：
S1 closes main control valve 101a and preceding step valve 103, opens regeneration valve 104, starts mechanical pump 102b and lobe pump
102a when the vacuum degree of cryogenic pump 101 reaches the first preset value, closes regeneration valve 104.
Specifically, step S1 is the regenerative process of cryogenic pump 101, it is therefore an objective to provide working environment for cryogenic pump 101.
Optionally, the first preset value is 1.0 × 10-4torr。
S2 starts cryogenic pump 101, makes the compressor operating in cryogenic pump 101, until the helium temperature in cryogenic pump 101
Reach operating temperature.
Specifically, the purpose of step S2 is in order to enable helium temperature reaches the operating temperature needed for its captured gas, with
Into pumping preparation state.After helium temperature reaches its operating temperature, pumping is achieved the purpose that by captured gas.
Optionally, the operating temperature range of helium is 10~20K.
Preferably, the operating temperature value of helium is 11K.
The temperature of cryogenic pump 101 into helium during pumping preparation state is lower, and the working time is longer, but cryogenic pump 101
Limit minimum operating temperature for 10K, therefore helium operating temperature it is optimal be 11K.
S3, step valve 103 before opening, takes out vacuum chamber 200 using mechanical pump 102b, treats the vacuum of vacuum chamber 200 in advance
After degree reaches the second preset value, when opening lobe pump 102a and being evacuated to vacuum degree and reach three preset values, step valve 103 before closing,
Open main control valve 101a.
Step S3 is the pre- pumping step of vacuum chamber 200.
Optionally, the second preset value of vacuum degree is 1.0 × 10-2torr。
Optionally, the 3rd preset value of vacuum degree is 1.0 × 10-3torr。
S4, the heater 203 in vacuum chamber 200 is started to work, and when temperature reaches the first preset temperature value, opens oxygen
Valve 204.
Specifically, step S4 is the course of work of vacuum chamber 200, treat that the first temperature-measuring part 205 detects burner hearth 203a's
When temperature value is the first preset temperature value, oxygen valve 204 is opened, oxygen is locally led in vacuum chamber 200, is electron beam physical vapor
The evaporation metal oxide oxygen supply of depositing device steams the oxygen saturation for crossing metal oxide to improve.
Optionally, the first preset temperature value is 1000 DEG C.
S5 when helium temperature gos up to the second preset temperature value, opens mechanical pump 102b and lobe pump 102a, and opens
Regeneration valve 104.
Step S5 is to be combined vacuumizing to vacuum chamber 200 using mechanical pump 102b, lobe pump 102a and cryogenic pump 101
Step.
Optionally, the second preset temperature value is 15K.
Specifically, after cryogenic pump 101 is started to work, since cryogenic pump 101 can rapidly adsorb steam, oil vapour, so as to
Pumpdown time is shortened, simultaneously because the gas of extraction is high-temperature gas out of vacuum chamber 200 so that the helium in cryogenic pump 101
Gas temperature recovery, so as to influence the efficiency of helium captured gas.At this point, starting mechanical pump 102b and lobe pump 102a, pass through machine
Tool pump 102b and lobe pump 102a takes gas and the interior gas accumulated of cryogenic pump 101 that cryogenic pump 101 traps away in time, with drop
Heat load in low cryogenic pump 101 reaches the temperature for reducing cryogenic pump 101 so that helium temperature maintains in cryogenic pump 101
The purpose of its operating temperature.
Simultaneously as the vacuum chamber 200 of electro beam physics vapour deposition equipment needs logical oxygen to be crossed to steam during the work time
Metal oxide supplies oxygen, and the vacuum environment of logical oxygen can so that gas is accumulated, since the principle that cryogenic pump 101 vacuumizes is trapping
Type, will not initiative exhaust, if the environment that cryogenic pump 101 is used individually in ventilation can be led so that gas is accumulated in cryogenic pump 101
The exhaust velocity of cryogenic pump 101 is caused to continuously decrease, the efficiency of its captured gas is influenced, so as to influence its pumping efficiency.This implementation
The vacuum pumping method of example takes the gas of accumulation in cryogenic pump 101 away by using mechanical pump 102b and lobe pump 102a, greatly in time
The big recovery time for shortening cryogenic pump 101, the high-efficiency air suction efficiency that cryogenic pump 101 is maintained to ventilate in high temperature under environment so that
Cryogenic pump 101 is suitable for high temperature ventilation environment.
Fig. 3 is the temperature of the cryogenic pump of the cryogenic pump and common usage in vacuum pumping method provided by Embodiment 2 of the present invention
The curve comparison figure changed over time with vacuum degree.
Refer to Fig. 3, curve A be the cryogenic pump 101 in vacuum extractor 100 of the present invention temperature with vacuum degree at any time
The curve of variation.Curve B is the curve that the temperature of the cryogenic pump of common usage and vacuum degree change over time.In figure, HP refers to temperature
Spend coordinate, unit K；HG refers to vacuum degree, unit Torr；TIME refers to time, unit minute.
From the figure 3, it may be seen that vacuum extractor 100 using the present invention, the true system 200 of pumping and vacuum pumping method, compared to
For common usage, the speed that the temperature of cryogenic pump 101 changes over time is enabled to reduce, extending cryogenic pump 101 can be
Usage time in the environment of high temperature ventilation, so as to long-time service.
It, can by the vacuum pumping method of the present invention vacuumizing for the vacuum chamber 200 of electro beam physics vapour deposition equipment
Vacuum pumping rate is greatly improved, effectively improves vacuum-deposited quality, improves the interface bond strength of substrate and coating, from
And improve the quality steamed and cross sample.
The vacuum extractor, pumped vacuum systems and vacuum pumping method of the present embodiment are suitable for electro beam physics vapour deposition
Equipment, but the present invention is not limited system, and vacuum extractor of the invention, pumped vacuum systems and vacuum pumping method are equally applicable
High temperature ventilation the environment equipment and system that vacuumize are needed in other.
It is contemplated that a kind of vacuum extractor, pumped vacuum systems and vacuum pumping method are protected, by setting cryogenic pump
Vacuum chamber is evacuated, since cryogenic pump can rapidly adsorb steam, oil vapour, shortens pumpdown time, making can be quick in vacuum chamber
Reach the vacuum degree of requirement, be used in combination by cryogenic pump with forerunner's pump, the pumping efficiency of the device improved, while forerunner
Pump is worked at the same time with cryogenic pump, can be extracted the gas of accumulation in gas and cryogenic pump that cryogenic pump traps out in time, be reduced low
The heat load of temperature pump shortens the recovery time of cryogenic pump, is imitated with the high-efficiency air suction that cryogenic pump is maintained to ventilate in high temperature under environment
Rate so that cryogenic pump being capable of the long-time service in the environment of high temperature ventilation.By the present invention vacuum extractor, pumped vacuum systems with
And vacuum pumping method is applied to electro beam physics vapour deposition equipment so that the vacuum chamber of electro beam physics vapour deposition equipment can
Higher vacuum is quickly obtained, therefore can effectively ensure to heat the temperature and quality of sample；It is aerobic due to being set in vacuum chamber
Air valve locally leads to oxygen for vacuum chamber by oxygen valve, improves the oxygen saturation steamed and cross metal oxide；Since cryogenic pump can be fast
Steam, oil vapour are adsorbed fastly, therefore can greatly improve the vacuum pumping rate of vacuum chamber, effectively improve vacuum-deposited matter
Amount improves the interface bond strength of substrate and coating, so as to which the quality of sample is crossed in the steaming for improving acquisition.
It should be appreciated that the above-mentioned specific embodiment of the present invention is used only for exemplary illustration or explains the present invention's
Principle, without being construed as limiting the invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into scope and border or this scope and the equivalents on border and repairing
Change example.
Claims (11)
1. a kind of vacuum extractor (100), which is characterized in that including：
Cryogenic pump (101), air entry are communicated to the exhaust outlet of vacuum chamber (200), for the vacuum chamber (200) be evacuated with
Make to reach vacuum in the vacuum chamber (200)；
Forerunner pumps (102), and air entry divides two-way, is connected to the exhaust outlet of the cryogenic pump (101) all the way, and another way is connected to
The exhaust outlet of the vacuum chamber (200)；
Preceding step valve (103) is arranged on the pipeline that the forerunner is pumped between (102) and the vacuum chamber (200)；
Regeneration valve (104) is arranged on the pipeline that the forerunner is pumped between (102) and the cryogenic pump (101).
2. vacuum extractor (100) according to claim 1, wherein,
Main control valve (101a) is provided in the cryogenic pump (101), for controlling the cryogenic pump (101) and the vacuum chamber
(200) break-make of pipeline between.
3. vacuum extractor (100) according to claim 1, wherein, the forerunner, which pumps (102), to be included：
Lobe pump (102a), air entry divide two-way, are connected to the exhaust outlet of the cryogenic pump (101), another way connection all the way
To the exhaust outlet of the vacuum chamber (200)；
Mechanical pump (102b), air entry are connected to the exhaust outlet of the lobe pump (102a).
4. the vacuum extractor (100) according to any one in claim 1-3, further includes：
Vacuum meter (105) is arranged on the pipeline between the cryogenic pump (101) and the regeneration valve (104), for detecting
Vacuum degree in the pipeline.
5. the vacuum extractor (100) according to any one in claim 1-3, further includes：
First cold-trap (106) is arranged on the pipeline between the preceding step valve (103) and the vacuum chamber (200), for inhaling
Receive the vapor in the vacuum chamber (200).
6. the vacuum extractor (100) according to any one in claim 1-3, further includes：
Second cold-trap (107) is arranged on the pipeline between the cryogenic pump (101) and the vacuum chamber (200), for hindering
Keep off the oil vapour volatilized in the vacuum pump (101)；
Heating element is provided in second cold-trap (107), for being heated to the coagulation on the second cold-trap (107) surface
To remove the coagulation.
7. a kind of pumped vacuum systems, which is characterized in that including the vacuum extractor as described in any one in claim 1-6
(100) and vacuum chamber (200)；
The exhaust outlet of the vacuum chamber (200) is connected with the air entry of the vacuum extractor (100).
8. pumped vacuum systems according to claim 7, wherein,
The exhaust outlet of the vacuum chamber (200) is provided with shutter (201), for reducing the vacuum chamber (200) to described low
The heat radiation of temperature pump (101).
9. pumped vacuum systems according to claim 7, wherein,
Cooling-part (202) is provided on the outer wall of the vacuum chamber (200), for reducing the temperature of the vacuum chamber (200).
10. pumped vacuum systems according to claim 9, wherein,
Having heaters (203) is set in the vacuum chamber (200), for heating sample.
11. a kind of vacuum pumping method, for the pumped vacuum systems described in any one in claim 7-10, which is characterized in that
Comprise the following steps：
Main control valve (101a) and preceding step valve (103) are closed, opens regeneration valve (104), starts mechanical pump (102b) and lobe pump
(102a) when the vacuum degree of cryogenic pump (101) reaches the first preset value, closes the regeneration valve (104)；
Start the cryogenic pump (101), make the compressor operating in the cryogenic pump (101), until in the cryogenic pump (101)
Helium temperature reach operating temperature；
The preceding step valve (103) is opened, the vacuum chamber (200) is taken out in advance using the mechanical pump (102b), is treated described
After the vacuum degree of vacuum chamber (200) reaches the second preset value, open the lobe pump (102a) and be evacuated to vacuum degree and reach the 3rd
During preset value, the preceding step valve (103) is closed, opens the main control valve (101a)；
Heater (203) in the vacuum chamber (200) is started to work, and when temperature reaches the first preset temperature value, opens oxygen
Air valve (204)；
When helium temperature gos up to the second preset temperature value, mechanical pump (102b) and lobe pump (102a) are opened, and is opened again
Raw valve (104).
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| CN109267033A (en) * | 2018-12-07 | 2019-01-25 | 沈阳爱科斯科技有限公司 | Evaporation coating device and coating system |
| CN110758781A (en) * | 2019-11-12 | 2020-02-07 | 上海卫星装备研究所 | Thermal vacuum equipment with condensable volatile pollutant absorption function and use method |
| CN111304623A (en) * | 2020-02-24 | 2020-06-19 | 西安交通大学 | Ultrahigh vacuum sample introduction and sample treatment dual-purpose system and method |
| CN114561626A (en) * | 2022-02-18 | 2022-05-31 | 华虹半导体(无锡)有限公司 | Physical vapor deposition device and pressure reduction method thereof |
| CN115460760A (en) * | 2022-11-09 | 2022-12-09 | 合肥中科离子医学技术装备有限公司 | Vacuum control system of cyclotron |
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