CN208586061U

CN208586061U - Ultrapure helium purification equipment

Info

Publication number: CN208586061U
Application number: CN201820817390.5U
Authority: CN
Inventors: 许少鹏; 何经余
Original assignee: Fujian Jiu Ce Gas Group Co Ltd
Current assignee: Fujian jiuce Gas Co., Ltd
Priority date: 2018-05-30
Filing date: 2018-05-30
Publication date: 2019-03-08
Anticipated expiration: 2028-05-30

Abstract

The utility model relates to a kind of ultrapure helium purification equipments, including purifier, the inner cavity of the purifier is provided with polishing pipe, getter is filled in the polishing pipe, the outer wall of the polishing pipe is wound with electric heating tube, one end of the polishing pipe is provided with the first air inlet entered to 5N helium, and the other end of the polishing pipe is provided with the first gas outlet to the discharge of 6N helium.The design of the utility model structure is simple, rationally, by purity is that 5N helium purify as 6N helium using getter, efficient convenient, energy conservation and environmental protection has broad application prospects.

Description

Ultrapure helium purification equipment

Technical field

The utility model relates to a kind of ultrapure helium purification equipments.

Background technique

Electron level ultrapure helium is used as purgative gas, pressurization gas in semiconductor fabrication, also serves as carrier gas and protection gas.It answers extensively For industries such as semiconductor integrated circuit IC, liquid crystal display LCD, light emitting semiconductor device LED and solar battery PV.Closely Nian Lai, as the energy resources such as Global Oil gradually decrease and environmental pollution, influence of the greenhouse effects to weather, countries in the world are big Power develops clean energy resource and power-saving technology, pays close attention to low-carbon economy.Under this background, the solar battery in China and half Conductor luminescent device and related industry are grown rapidly, and electron level ultrapure helium market is boundless.

5N helium refers to that purity is 99.999% helium, and 6N helium refers to that purity is 99.9999% helium, existing Ultrapure helium purification equipment unreasonable structural design, have significant limitation.

Utility model content

In view of the deficiencies in the prior art, the technical problem to be solved by the utility model is to provide a kind of purifying of ultrapure helium to fill It sets, it is not only reasonable in design but also efficiently convenient.

In order to solve the above-mentioned technical problem, the technical solution of the utility model is: a kind of ultrapure helium purification equipment, including pure Change device, the inner cavity of the purifier is provided with polishing pipe, and getter is filled in the polishing pipe, and the outer wall of the polishing pipe twines It is wound with electric heating tube, one end of the polishing pipe is provided with the first air inlet entered to 5N helium, described to polish the another of pipe One end is provided with the first gas outlet to the discharge of 6N helium.

Further, the purifier is connected by heat exchanger, cooler with molding machine by escape pipe sequence.

Further, 5N helium heat exchanger channels and 6N helium heat exchanger channels, the 5N helium are provided in the heat exchanger The second air inlet and the second gas outlet are provided on heat exchanger channels, second air inlet is through air inlet pipe and 5N helium stock bottle phase Connection, second gas outlet are connected through escape pipe with the first air inlet, are provided with third on the 6N helium heat exchanger channels Air inlet and third gas outlet, the third air inlet are connected through air inlet pipe with the first gas outlet, the third gas outlet warp Escape pipe is connected with cooler.

Further, it is provided with insulating layer outside the electric heating tube, closing aluminium sheet is provided with outside the insulating layer.

Further, the molding machine is connected through escape pipe with 6N helium tank.

Further, it connects between escape pipe, connection molding machine and the 6N helium tank between the cooler and molding machine Escape pipe on be provided with analysis valve and blow valve.

Further, it connects and is provided with decompression in the air inlet pipe between the 5N helium stock bottle and 5N helium heat exchanger channels Valve.

Further, the getter uses zirconium vanadium iron getter.

Compared with prior art, the utility model has the following beneficial effects: the design of the utility model structure is simple, closes Purity is that 5N helium purify as 6N helium using getter by reason, and efficient convenient, energy conservation and environmental protection has broad application prospects.

The utility model is described in more detail with reference to the accompanying drawings and detailed description.

Detailed description of the invention

Fig. 1 is the organigram of the utility model embodiment.

Fig. 2 is the organigram of the utility model embodiment purifier.

Fig. 3 is the organigram of the utility model embodiment heat exchanger.

Fig. 4 is the schematic cross-sectional view in the direction the utility model embodiment Fig. 3 A-A.

In figure: 1- purifier, 101- polishing pipe, 102- getter, 103- electric heating tube, the first air inlet of 104-, 105- First gas outlet, 106- insulating layer, 107- close aluminium sheet, 108- fixed frame, 109- thermocouple, 2- heat exchanger, 201- second into Port, the second gas outlet 202-, 203- third air inlet, 204- third gas outlet, 3- cooler, 4- molding machine, 5-5N helium Stock bottle, 6-6N helium tank, 7- analyze valve, 8- blow valve, 9- pressure reducing valve.

Specific embodiment

In order to make the above-mentioned features and advantages of the utility model more obvious and understandable, special embodiment below, and cooperate attached drawing, It is described in detail below.

As shown in Fig. 1 ~ 4, a kind of ultrapure helium purification equipment, including purifier 1, the inner cavity of the purifier 1 are provided with throwing Light pipe 101, the polishing pipe 101 is interior to be filled with getter 102, and the outer wall of the polishing pipe 101 is wound with electric heating tube 103, One end of the polishing pipe 101 is provided with the first air inlet 104 entered to 5N helium, the other end of the polishing pipe 101 It is provided with the first gas outlet 105 to the discharge of 6N helium；The electric heating tube 103 heats getter 102, to air-breathing Agent is activated, until getter is all saturated, to improve ultrapure helium purification efficiency.

In the utility model embodiment, the purifier 1 passes through heat exchanger 2, cooler 3 and film by escape pipe sequence Press 4 is connected.

In the utility model embodiment, it is provided with 5N helium heat exchanger channels in the heat exchanger 2 and the heat exchange of 6N helium is logical Road, the second air inlet 201 and the second gas outlet 202 are provided on the 5N helium heat exchanger channels, and second air inlet 201 passes through Air inlet pipe is connected with 5N helium stock bottle 5, and second gas outlet 202 is connected through escape pipe with the first air inlet 104, institute It states and is provided with third air inlet 203 and third gas outlet 204 on 6N helium heat exchanger channels, the third air inlet 203 is through air inlet Pipe is connected with the first gas outlet 105, and the third gas outlet 204 is connected through escape pipe with cooler 3；5N helium is from 5N helium Gas stock bottle 5, air inlet pipe, the second air inlet 201,5N helium heat exchanger channels, the first air inlet 104, which enter getter 102, to carry out Absorption type purifying, obtains 6N helium through the first gas outlet 105, escape pipe, third air inlet 203,6N helium heat exchanger channels, third Gas outlet 204, cooler 3 enter molding machine 4, bottle using 6N helium tank 6 after detection is qualified；The heat exchanger The 6N helium of 2 pairs of high temperature carries out first time cooling, and the cooler 3 carries out second to the 6N helium of high temperature and cools down, described to change Hot device 2 reduces the energy consumption of cold air device, while the heat transfer of 6N helium to 5N helium is improved 5N helium by the heat exchanger 2 The temperature of gas, to reduce the energy consumption of electric heating tube 103, energy conservation and environmental protection.

In the utility model embodiment, tubular heat exchanger is used in the heat exchanger 2, A-A is upper and lower two in attached drawing 3 The orifice plate at end, distance is 1.5 meters between orifice plate, in 17 holes being distributed on long 1.5 meters of 1/4 stainless steel EP pipe insertion orifice plate And it welds, totally 17；The orifice plate circumference and 89 × 4.5 stainless steel polishing pipe of ￠, 101 inner wall of upper and lower ends weld, and it is stainless to form 1/4 In steel EP pipe and outer two channels of pipe；Logical 6N helium forms 6N helium heat exchanger channels in 1/4 stainless steel EP pipe, manages outer logical 5N helium 5N helium heat exchanger channels are formed, two strands of gas carry out heat exchange by tube wall.

In the utility model embodiment, it is provided with insulating layer 106 outside the electric heating tube 103, outside the insulating layer 106 It is provided with closing aluminium sheet 107；Fixed frame 108 and thermocouple 109 are additionally provided in the purifier 1.

In the utility model embodiment, the molding machine 4 is connected through escape pipe with 6N helium tank 6.

In the utility model embodiment, escape pipe, the connection molding machine 4 between the cooler 3 and molding machine 4 are connected Analysis valve 7 and blow valve 8 are provided on escape pipe between 6N helium tank 6；The effect of entrance analysis site is monitoring purifying The purification effect of device 1, fills bottle into the compression of molding machine 4 again after purity qualification, and the effect of exit analysis point is that monitoring passes through membrane pressure Whether the gas of machine 4 is contaminated, so as to the discriminatory analysis of purity exception.

In the utility model embodiment, the 4th air inlet and the 4th gas outlet, the film are provided on the cooler 3 The 5th air inlet and the 5th gas outlet are provided on press 4, the 4th air inlet is connected through escape pipe with third gas outlet 204 It connects, the 4th gas outlet is connected through escape pipe with the 5th air inlet, and the 5th gas outlet is through escape pipe and 6N helium tank 6 It is connected.

In the utility model embodiment, the air inlet between the 5N helium stock bottle 5 and 5N helium heat exchanger channels is connected Pressure reducing valve 9 is provided on pipe.

In the utility model embodiment, the getter 102 uses zirconium vanadium iron getter.

In the utility model embodiment, the air-breathing mechanism of zirconium vanadium iron getter is as follows:

Zirconium vanadium iron getter breathing process is divided into three steps: being that active gases molecule enters zirconium vanadium iron getter table first Face is simultaneously decomposed, and then active gases and zirconium vanadium iron getter surface generate chemisorption, is finally active gas at a certain temperature Body molecule is to spreading inside zirconium vanadium iron getter particles；After zirconium vanadium iron getter works a period of time or exposure atmosphere, activity Gas molecule stops spreading into zirconium vanadium iron getter body, zirconium vanadium iron getter particles surface form one layer by oxide and The passivation layer of carbide composition；In order to restore the air suction function of zirconium vanadium iron getter, diffusion process is improved by heating method Kinetic energy makes the gas molecule on zirconium vanadium iron getter particles surface to internal diffusion, to eliminate passivation layer, restores zirconium vanadium iron air-breathing The gettering ability of agent；This process is called the activation of zirconium vanadium iron getter, zirconium vanadium iron getter can activate repeatedly for several times, until All until saturation.

Zirconium vanadium iron getter can be 500 DEG C or so in temperature and be activated, so being applied in purification for gas；Zirconium vanadium After iron getter is activated, when active gases encounters clean zirconium vanadium iron getter alloys particle surface, with alloying pellet table Face forms stable compound, i.e., the various foreign gases in helium form stable each in zirconium vanadium iron getter alloys particle surface Kind compound, and it is trapped in alloying pellet surface, it is not carried over purifier 1, to achieve the purpose that purified gases.

In the utility model embodiment, the volume of zirconium vanadium iron getter needed for calculating:

The volume of zirconium vanadium iron getter is calculated according to the air speed that gas treatment amount and zirconium vanadium iron getter allow:

Vk=V/w0

In formula: Vk --- the volume (m3) of required zirconium vanadium iron getter；

The gas flow (Nm3/h) of V --- processing；

The air speed (h-1) that w0 --- zirconium vanadium iron getter allows

Zirconium vanadium iron getter air speed is considered that processing tolerance is 15 Nm3/h by 2500 h-1；

That is: Vk=V/w0=15 ÷ 2500=0.006 m3.

In the utility model embodiment, the size of purifier 1 is calculated:

It uses the internal diameter of stainless steel polishing pipe 101 for 0.08 m, the zirconium vanadium iron getter filling of purifier 1 is calculated as follows Height H；

Vk=3.14R2 H；

R --- the radius of stainless steel polishing pipe 101 is (m)；

H --- zirconium vanadium iron getter filling height (m)；

That is: H=Vk/3.14R2

Then: m3/3.14 H=0.006 × 0.042=1.2 m.

In the utility model embodiment, power needed for calculating electric heater:

Because zirconium vanadium iron getter activationary temperature is 500 DEG C, 5N helium need to be passed through in entire activation, it is assumed that helium import Temperature is 10 DEG C, and outlet temperature is 500 DEG C；

Reactor institute calorific requirement is calculated as follows:

Q=V Cp △ T

In formula: Q --- reactor institute calorific requirement kilocalorie/h；

V --- processing tolerance 15Nm3/h；

0.22 kilocalorie/m3 DEG C of Cp --- helium specific heat；

△ T --- helium imports and exports the temperature difference DEG C；

That is: Q=15 × 0.22 × (500-10)=1617 kilocalories/h.

Power needed for electric heater is calculated as follows:

Q/860 N=1.1

That is: N=1.1 × 1617/860=2.07 kilowatts

In the utility model embodiment, the utility model, as raw material, is decompressed to using the bottled helium of 5N through pressure reducing valve 9 1.5MPa enters heat exchanger 2, is 15Nm3/h by flowmeter control charge flow rate, and 5N helium enters the 5N helium heat exchange of heat exchanger 2 It exchanges heat behind channel with the 6N helium being discharged in 6N helium heat exchanger channels from purifier 1, the heat for absorbing 6N helium enters back into purifying Device 1 recycles the heat of discharge, energy saving.

5N helium is in purifier 1, because of impurity quilt of zirconium vanadium iron getter under the action of 350 DEG C of high temperature, in 5N helium It removes, 6N helium after purification enters heat exchanger 2 and heat is transmitted to raw material 5N helium, enters back into cooler 3 by air but to normal Then temperature is filled with 6N helium steel cylinder by the compression of molding machine 4, according to the needs of users, pressure is 15 or 20MPa.

1, technical parameter

(1) purification process flow: 15Nm3/h

(2) 1 operating pressure of purifier: 1.5MPa

(3) zirconium vanadium iron getter activationary temperature: 500 DEG C

(4) 1 operating temperature of purifier: 350 DEG C

(5) unstripped gas purity: 99.999%

(6) purity after purifying: 99.9999%

(7) impurity content: (GB/T16943-2009)

Impurity

CO

CO2

N2

O2

CH2

H2O

Content (ppm)

< 0.1

< 0.5

< 0.2

< 0.1

< 0.2

2, prepare before operation

(1) check that all valves are in closed state；

(2) check that power supply is normal, all electric switches are in close state；

(3) check that flowmeter, temperature control instrument are normal；

(4) system pipeline No leakage is checked；

(5) confirmation analysis instrument has been ready；

(6) confirmation raw material helium purity is 99.999%.

3, operating procedure

(1) temperature control box power switch is connected, temperature controller electricity box are devoted oneself to work；

(2) raw gas pressure is decompressed to 0.1~0.2MPa, is passed through a small amount of raw material helium to purification device；

(3) start molding machine 4, the 5N helium that activation is sent into purification device is filled with steel cylinder recycling；

(4) setting operation temperature, is a gradient by every 100 DEG C, and every gradient temperature carries out heating behaviour after 1 hour after stablizing again Make；

(5) when 1 temperature of purifier is raised to 500 DEG C, stablize 2 hours, activate zirconium vanadium iron getter；

(6) when 1 temperature of purifier be raised to 500 DEG C and stablize 2 it is small when after, by temperature control be set as 350 DEG C, purifier 1 is Normal work can be put into；

(7) raw gas pressure is slowly adjusted to 1.5MPa, steps up raw gas flow and reaches 15 Nm3/h, pay attention to maintaining 1 temperature of purifier is 350 DEG C, operating pressure 1.5Mpa；

(8) in 4 entrance analysis site sampling analysis of molding machine, charge flow rate and work are adjusted according to the clean-up effect of purifier 1 Make temperature, finds optimum working parameter.

4, the ultrapure helium of 6N fills bottle

After impurity content is qualified in 4 entrance analysis site sampling analysis helium of molding machine, sampled in 4 exit analysis point of molding machine Impurity content in helium is analyzed, and carries out following preparation:

(1) 6N helium steel cylinder is installed filling framed bent, connect cylinder valve connector, but not tighten；

(2) it after impurity content is qualified in 4 exit analysis point sampling analysis helium of molding machine, slightly opens and fills a bottle manifold valve, gas Go out to discharge from cylinder joint and cylinder valve, a bottle branch pipe is filled in blowing；

(3) after bottle branch pipe blowing completely is filled in confirmation, cylinder valve connector is tightened, 5N helium cylinder valve (recycling steel cylinder) is closed, opens 6N helium cylinder valve, gas are filled with 6N helium steel cylinder；

(4) it when steel cylinder pressure reaches 15 or 20MPa, carrying out filling switching operation, 6N helium is filled with another steel cylinder, with This analogizes.

For indicating the art of positional relationship or shape applied in above-mentioned any technical solution disclosed by the utility model Its meaning includes approximate with its, similar or close state or shape to language unless otherwise stated.

Either component provided by the utility model by multiple individual component parts either assembled, or The separate part that integrally formed technique manufactures.

Finally it should be noted that: above embodiments are only to illustrate the technical solution of the utility model rather than limit it System；Although the utility model has been described in detail with reference to the preferred embodiment, those of ordinary skill in the art should Understand: specific implementation of the utility model can still be modified or is equally replaced to some technical characteristics It changes；Without departing from the spirit of technical solutions of the utility model, should all cover in the claimed technical solution of the utility model In range.

Claims

1. a kind of ultrapure helium purification equipment, it is characterised in that: including purifier, the inner cavity of the purifier is provided with polishing pipe, Getter is filled in the polishing pipe, the outer wall of the polishing pipe is wound with electric heating tube, one end setting of the polishing pipe There is the first air inlet entered to 5N helium, the other end of the polishing pipe is provided with the first outlet to the discharge of 6N helium Mouthful.

2. ultrapure helium purification equipment according to claim 1, it is characterised in that: the purifier is passed through by escape pipe sequence Cross heat exchanger, cooler is connected with molding machine.

3. ultrapure helium purification equipment according to claim 2, it is characterised in that: be provided with 5N helium in the heat exchanger and change The passage of heat and 6N helium heat exchanger channels are provided with the second air inlet and the second gas outlet on the 5N helium heat exchanger channels, described Second air inlet is connected through air inlet pipe with 5N helium stock bottle, and second gas outlet is connected through escape pipe with the first air inlet Connect, be provided with third air inlet and third gas outlet on the 6N helium heat exchanger channels, the third air inlet through air inlet pipe with First gas outlet is connected, and the third gas outlet is connected through escape pipe with cooler.

4. ultrapure helium purification equipment according to claim 1, it is characterised in that: be provided with heat preservation outside the electric heating tube Layer, the insulating layer are provided with closing aluminium sheet outside.

5. ultrapure helium purification equipment according to claim 2, it is characterised in that: the molding machine is through escape pipe and 6N helium Bottle is connected.

6. ultrapure helium purification equipment according to claim 5, it is characterised in that: connect between the cooler and molding machine Escape pipe, be provided with analysis valve and blow valve on the escape pipe between connection molding machine and 6N helium tank.

7. ultrapure helium purification equipment according to claim 3, it is characterised in that: connect the 5N helium stock bottle and 5N helium Pressure reducing valve is provided in air inlet pipe between gas heat exchanger channels.

8. ultrapure helium purification equipment according to claim 1, it is characterised in that: the getter uses zirconium vanadium iron air-breathing Agent.