CN104576261B - A kind of processing technology of the cold cathode X-ray tube based on CNT - Google Patents
A kind of processing technology of the cold cathode X-ray tube based on CNT Download PDFInfo
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- CN104576261B CN104576261B CN201410854114.2A CN201410854114A CN104576261B CN 104576261 B CN104576261 B CN 104576261B CN 201410854114 A CN201410854114 A CN 201410854114A CN 104576261 B CN104576261 B CN 104576261B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
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Abstract
The present invention relates to a kind of processing technology of the cold cathode X-ray tube based on CNT, the cold cathode X-ray tube includes body, negative electrode, anode and grid are set in the body, and the negative electrode application CNT is prepared from, and the CNT need to be through following process：By longitudinal growth in substrate surface CNT be placed in dilution 30 40% HF solution in soak, the free end cluster of the CNT of longitudinal growth is gathered in a bit.CNT is processed, the specific surface area of treated CNT is enable to be increased dramatically, realize that electronics is assembled, further increase field emission effect, X-ray intensity and the electron emission directionality of the cold cathode X-ray tube made using the CNT.
Description
Technical field
A kind of the present invention relates to improve electronic emission performance technical field, more particularly to cold the moon based on CNT
The processing technology of pole X-ray tube.
Background technology
Roentgen roentgen was found that X ray in 1895.X ray is between particle and material by high-speed motion
Occur interact and produce, its essence is a kind of electromagnetic wave, wavelength between 0.01～10nm, with very strong penetration power
And lethality, organism can be penetrated and kill its internal cell, therefore, it is widely used in radiation treatment and profit
The field of elementary analysiss is carried out to material with the fluorescence of X ray.X ray has special physics, chemistry and biological effect
Property, is widely used in production and medical domain, while also also generating great shadow to medical science and scientific progress
Ring.
CNT is found within 1991.CNT has superior electrology characteristic, chemical property and physical aspect, makes
It becomes one of semi-conducting material for being widely studied in nanosecond science and technology.Using the growth technique that CNT is ripe
Vapor deposition method is learned, in conjunction with its field emission characteristicses, X ray can be produced.The X ray that application CNT is produced, can
Being applied to medical domain carries out radiation treatment, and cancerous cell fixed point irradiation is killed, and solves Traditional x-ray source temperature height, sends out
Hot problem that is high, effectively can not carrying out fixed point irradiation kill to cancerous cell, and carbon nano pipe arrayization can also be well
Improve the intensity of x-ray source.
MEMS (Micro-Electro-Mechanical System, MEMS) technology is extensively should 21 century
The core technology of multiple fields is used, and this technology can make biochip, sensor chip, SOC systems etc. finer
Change.Therefore, CNT graphic array can more accurately be realized based on MEMS technology, realizes that carbon nanometer cold-cathode field is sent out
Penetrate, improve the intensity of X ray and the conversion ratio in same area area.But, basic semiconductor technology energy is adopted at present
The size of the carbon tube nanometer tube figuring that enough accomplishes is micron-sized, it is desirable to further improve the intensity of X ray, it is necessary to improve
Patterned size, can so bring the problems such as cost raising.
In addition, it is a kind of the more commonly used method for realizing carbon tube nanometer tube figuring nanostructured that ion beam is inscribed, but
This mode using equipment in generally all carry the optical system that involves great expense, still there is high cost.
The product of Conventional X-ray tubes is mainly based on reflective in the market.And great majority are used with heat
The X-ray tube of negative electrode, this X-ray tube simple structure, low price, but a lot of limitation are there is also, respectively：
(1) operating temperature is high, causes the restricted lifetime of X-ray tube, energy consumption big, and the X-ray tube work of some improvement
When, in addition it is also necessary to cooled cathode；
(2) volume is big, it is impossible to enough meet the application requirement of X-ray tube miniaturization；
(3) electron emission directionality are poor, need to protect vessel wall damage, and also limit X-ray tube spatial resolution enters one
Step is improved；
(4) when working, preheating time is long, it is impossible to realize instantaneous work.
Content of the invention
It is an object of the invention to proposing a kind of processing technology of the cold cathode X-ray tube based on CNT, carbon is received
Mitron is processed, and enables the specific surface area of treated CNT to be increased dramatically, and is realized that electronics is assembled, is entered one
Field emission effect, X-ray intensity and the electron emission that step improves the cold cathode X-ray tube made using the CNT is fixed
Tropism.
It is that the present invention is employed the following technical solutions up to this purpose：
A kind of processing technology of the cold cathode X-ray tube based on CNT, the cold cathode X-ray tube include body,
Negative electrode, anode and grid are set in the body, and the negative electrode application CNT is prepared from, the CNT need through
Hereinafter process：
Longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, makes longitudinal direction
The free end cluster of the CNT of growth gathers in a bit.
Wherein, the CNT is cylinder, a diameter of 10 nanometers of the cylinder, and the height of the cylinder is
3-5 microns；
Described longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, tool
Body is：
By longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in soak 1-2 minutes.
Wherein, described by longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in soak 1-
2 minutes, specially：
By longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in immersion 1 point 20 seconds.
Wherein, the longitudinal growth is in the preparation process of the CNT of substrate surface, including：
(1) with heavy doping silicon chip as substrate, one layer of PMMA glue of spin coating, obtains sample one over the substrate；
(2) sample one is placed in baking 1-3 minutes in 60-70 DEG C of temperature, sample two is obtained；
(3) one layer of UV glue of spin coating on the PMMA glue-lines of the sample two, obtains sample three, the surface of the sample three
The gross thickness of PMMA glue-lines and UV glue-lines is 100-120nm；
(4) previously prepared plastic formwork is attached on the UV glue-lines of the sample three, carries out nano impression process, obtain
Sample four, the dutycycle of the plastic formwork is 1:1；
(5) sample four is placed under ultraviolet light, exposes the 30-40 seconds, peeled off the plastic formwork, obtain sample five,
The gross thickness of the PMMA glue-lines and UV glue-lines of the surface convex portion of the sample five is 200-250nm；
(6) sample five is placed in CVD growth stove, using ethanol as the carrier for providing hydrogen, is cracked using ethanol
Vapor deposition method, make to grow longitudinal growth on the substrate in the CNT of substrate surface.
Wherein, described preparation process (2), specially：The sample one is placed in 65 DEG C of temperature and is toasted 2 minutes, obtained
Arrive sample two；
The gross thickness of the PMMA glue-lines and UV glue-lines on the surface of the sample three is 110nm；
The time of exposure of preparation process (5) is 35 seconds.
Wherein, after preparation process (5), before preparation process (6), also include preparation process：
(5a) sample five is carried out plasma etching, to remove after nano impression process, on five surface of the sample
The PMMA glue and UV glue of unwanted region residual.
Wherein, after preparation process (5), before preparation process (6), also include preparation process：
(5b) configure the solution of 1ppm with octadecyl trichlorosilane alkane and toluene in proportion, the sample five is placed in this
In solution after immersion 12-18 minutes, then it is placed in immersion 1-2 minutes in acetone.
Wherein, described preparation process (5b), specially：
The sample five is placed in the solution by the solution for configuring 1ppm in proportion with octadecyl trichlorosilane alkane and toluene
Middle immersion 15 minutes after, then be placed in acetone soak 1 point 30 seconds.
Wherein, the preparation process of the plastic formwork, including：
(1) one layer of photoresist of spin coating on rigid substrate, obtains middle product one；
(2) previously prepared mask plate is attached on the photoresist layer of the middle product one, carries out photoetching treatment, in obtaining
Between product two, the dutycycle of the mask plate is 1:1；
(3) the middle product two are carried out reactive ion etching, obtains middle product three, the etching pattern of the middle product three
Bossing thickness be 90-110nm；
(4) using the middle product three, overmolded process is carried out, the plastic formwork is prepared.
Wherein, the thickness of the bossing of the etching pattern of the middle product three is 100nm.
Wherein, the preparation process (4) of the plastic formwork, specifically includes：
(4a) by 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and 40-60 is micro-
The thick PET thin film of rice is laid in the surface of the polydimethylsiloxane, obtains middle product four；
(4b) by the meso sample four in 75-85 DEG C, 35-45 minutes are solidified, by the PET thin film from described
Peel off on rigid substrate, obtain the PET template.
Wherein, the mask plate is the circular film film that surface arranges array pattern.
Wherein, the photoresist includes positive photoresist and negative photoresist；The positive photoresist is AZ5214 photoetching
Glue or S1805 photoresists, the negative photoresist are SU8-3010 photoresists；
When using the positive photoresist, before the preparation process (1) of the plastic formwork, also include：
Release treatment is done on rigid substrate surface, the release treatment includes Surface Treatment with Plasma and smoked HMDS process.
Wherein, the condition of the reactive ion etching is：
Etching gas are CF4/Ar, and the throughput of etching gas is 30/10sccm, and etching power is 170W, build-up of luminance pressure
For 4Pa, etch period is 30 seconds 3 minutes.
Wherein, the preparation process (4a) of the plastic formwork, specifically includes：
By 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and thick by 50 microns
PET thin film is laid in the surface of the polydimethylsiloxane, obtains middle product four；
The preparation process (4b) of the plastic formwork, specifically includes：
By the meso sample four in 80 DEG C, solidify 40 minutes, by the PET thin film from the rigid substrate
Peel off, obtain the PET template.
Wherein, the negative electrode is rectangle, and the length of the rectangle is 5mm, and the width of the rectangle is 2mm.
Wherein, the body be cylindrical tube, a diameter of 20mm of the cylindrical tube, the cylindrical tube
Length is 80mm.
Wherein, 200 microns of the gate distance negative electrode, the voltage that the grid is applied in is in 0.3-5 kilovolt ranges.
Wherein, the anode is less than or equal to 5 millimeters with the distance of negative electrode, and the voltage that the anode is applied in is in 20-65 thousand
In the range of volt.
Wherein, the grid and anode are copper electrode.
Wherein, the body arranges the beryllium glass that a block length is 200 microns in the part of reflection X-ray.
Wherein, with the horizontal 30-40 ° of angle, the vacuum in the body is 10 to the anode-5Pa.
The beneficial effects of the present invention is：A kind of processing technology of the cold cathode X-ray tube based on CNT, described cold
Cathode X ray tube includes body, arranges negative electrode, anode and grid in the body, the negative electrode application CNT prepare and
Into the CNT need to be through following process：CNT of the longitudinal growth in substrate surface is placed in the 30-40% of dilution
HF solution in soak, the free end cluster of the CNT of longitudinal growth is gathered in a bit.CNT is processed, make through
The specific surface area for crossing the CNT for processing can be increased dramatically, and realize that electronics is assembled, further increase using the carbon
The field emission effect of the cold cathode X-ray tube that nanotube makes, X-ray intensity and electron emission directionality.
Description of the drawings
For the technical scheme being illustrated more clearly that in the embodiment of the present invention, below will be to institute in embodiment of the present invention description
The accompanying drawing for using is needed to be briefly described, it should be apparent that, drawings in the following description are only some enforcements of the present invention
Example, for those of ordinary skill in the art, on the premise of not paying creative work, can be with according to present invention enforcement
The content of example and these accompanying drawings obtain other accompanying drawings.
Fig. 1 is the CNT effect contrast figure before and after the disposal methods of the CNT provided through the present invention.
Fig. 2 is the aligned carbon-nanotubes SEM figures of the disposal methods of the CNT provided through the present invention.
Fig. 3 be the present invention provide longitudinal growth in substrate surface CNT preparation flow figure.
Fig. 4 is the preparation flow figure of the plastic formwork that the present invention is provided.
Fig. 5 is the optical picture of the plastic formwork that the present invention is provided.
Fig. 6 is the design drawing of the mask plate that the present invention is provided.
Fig. 7 is the design principle figure of the cold cathode X-ray tube based on CNT that the present invention is provided.
Fig. 8 is that the Flied emission of the cold cathode X-ray tube based on CNT that traditional X-ray tube and the present invention are provided is bent
Line comparison diagram.
Fig. 9 is that the cold cathode X-ray tube based on CNT that the present invention is provided faces structure chart.
Figure 10 is the 3 dimensional drawing of the cold cathode X-ray tube based on CNT that the present invention is provided.
Figure 11 is the profile of the cold cathode X-ray tube based on CNT that the present invention is provided.
Description of the drawings is as follows：
1- bodys, 2- negative electrodes, 3- anodes, 4- grids；5- beryllium glasses.
Specific embodiment
For make present invention solves the technical problem that, the technical scheme that adopts and the technique effect that reaches clearer, below
Accompanying drawing will be combined to be described in further detail the technical scheme of the embodiment of the present invention, it is clear that described embodiment is only
It is a part of embodiment of the invention, rather than whole embodiments.Embodiment in based on the present invention, those skilled in the art exist
The every other embodiment obtained under the premise of not making creative work, belongs to the scope of protection of the invention.
Fig. 1 is refer to, which is the CNT effect before and after the disposal methods of the CNT provided through the present invention
Comparison diagram.
A kind of processing technology of the cold cathode X-ray tube based on CNT, the cold cathode X-ray tube include body,
Negative electrode, anode and grid are set in the body, and the negative electrode application CNT is prepared from, the CNT need through
Hereinafter process：
Longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, makes longitudinal direction
The free end cluster of the CNT of growth gathers in a bit.
Cluster gathers the specific surface area that improve CNT in the CNT of a bit, it is achieved that electronics is assembled, also further
Improve the field emission effect using cold cathode X-ray tube obtained in the CNT, X-ray intensity and electron emission to orient
Property.
Specific surface area refers to the gross area that unit mass material has, including external surface area, two class of internal surface area, GB
Unit is /g.
HF solution is the aqueous solution of Fluohydric acid., is one kind of weak acid.
Wherein, the CNT is cylinder, a diameter of 10 nanometers of the cylinder, and the height of the cylinder is
3-5 microns；
Described longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, tool
Body is：
By longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in soak 1-2 minutes.
Wherein, described by longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in soak 1-
2 minutes, specially：
By longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in immersion 1 point 20 seconds.
Fig. 2 is refer to, which is the aligned carbon-nanotubes SEM of the disposal methods of the CNT provided through the present invention
Figure.
It can be seen that soak 1-2 minutes during the CNT of above-mentioned specification to be placed in the HF solution of the 35% of dilution, special
Be not 1 point 20 seconds, it is possible to allow the free end cluster of CNTs of the overwhelming majority to gather in middle part a bit.
Refer to Fig. 3, its be the present invention provide longitudinal growth in substrate surface CNT preparation flow figure.
Wherein, the longitudinal growth is in the preparation process of the CNT of substrate surface, including：
(1) with heavy doping silicon chip as substrate, one layer of PMMA glue of spin coating, obtains sample one over the substrate；
(2) sample one is placed in baking 1-3 minutes in 60-70 DEG C of temperature, sample two is obtained；
(3) one layer of UV glue of spin coating on the PMMA glue-lines of the sample two, obtains sample three, the surface of the sample three
The gross thickness of PMMA glue-lines and UV glue-lines is 100-120nm；
(4) previously prepared plastic formwork is attached on the UV glue-lines of the sample three, carries out nano impression process, obtain
Sample four, the dutycycle of the plastic formwork is 1:1；
(5) sample four is placed under ultraviolet light, exposes the 30-40 seconds, peeled off the plastic formwork, obtain sample five,
The gross thickness of the PMMA glue-lines and UV glue-lines of the surface convex portion of the sample five is 200-250nm；
(6) sample five is placed in CVD growth stove, using ethanol as the carrier for providing hydrogen, is cracked using ethanol
Vapor deposition method, make to grow longitudinal growth on the substrate in the CNT of substrate surface.
By the element of conduction is added in the semi-conductor silicon chip of tetravalence, such as add the boron of trivalent or the phosphorus of pentavalent etc.
The electric conductivity of semiconductor silicon can be improved.The more, the electric conductivity of silicon sheet material is stronger for the amount of addition.According to the difference of additional proportion,
Semi-conductor silicon chip can be divided into silicon chip, middle doped silicon wafer and heavy doping silicon chip is lightly doped.Heavy doping silicon chip doping content is high, its resistance
Rate can reach 2 × 10-2Ω·cm.
PMMA (polymethyl methacrylate, polymethylmethacrylate) glue, light transmittance up to 90%-92%,
There is excellent against weather and electrical insulating property, transparency is high, and price is low, it is easy to the advantages of machining.
It is ultraviolet that UV glue (Ultraviolet Rays glue, without shadow glue, light-sensitive emulsion, ultraviolet cured adhesive) is that one kind must pass through
The curable adhesive of linear light irradiation.The principle of solidification of UV glue is light trigger (or photosensitizer) in UV glue in ultraviolet
Under irradiation, living radical or cation after absorbing ultraviolet light, can be produced, trigger monomer polymerization, cross-linking chemistry reaction make gluing
Agent is converted into solid-state by liquid within the several seconds.
Nanometer embossing directly can mechanically be existed using physics mechanism on the premise of electronics and photon is not used
Nanometer-scale pattern is constructed on photoresist.Just because of this mechanism so that nanometer embossing is no longer influenced by photon and spreads out
The restriction with electron scattering is penetrated, nano-scale pattern can be prepared in large area.Simultaneously as the equipment letter used by nanometer embossing
Single, preparation time is short, and impression block can be reused, thus apply the technology prepare cost needed for nano graph also compared with
Low.
Nanometer embossing principle is basically identical, and simply technique is simpler, practical and cheap.Wherein, hot padding is three
Plant one of typical nanometer embossing process.
Hot padding (Hot embossing) technique includes the preparation of hot pressing die plate, applies polymer, prepares polymer figure
Shape and transfer polymerization thing figure.
Hot pressing die plate need to possess following condition：
(1) high rigidity：Pressing mold and do not allow during removing mould yielding and impaired；
(2) low-expansion coefficient：Avoid figure deformation caused by degree of thermal expansion difference and high pressure；
(3) good anti-stickiness energy：Polymer energy complete wetting template surface during pressing mold, when removing mould, polymer can be complete with substrate
Fully separating.
Summary condition is limited, and hot padding phase templates generally select Si and SiO2Material.
The polymer for being used as hot padding glue need to meet three below condition：
(1) polymer is amorphous state, can flow under external force and deform upon；
(2) thermal coefficient of expansion and pressure contractions coefficient are little；
(3) relative to substrate, there is higher dry etching selectivity.
PMMA glue is the most hot padding glue of application because the number-average molecular weight of its cast panel polymer up to 2.2 ×
104, coating is highly uniform, and can be dissolved in own monomer, chloroform, acetic acid, ethyl acetate, acetone and other organic solvent.
Chemical vapor deposition (CVD) is the technology for depositing multiple materials being most widely used in semi-conductor industry,
Its operation principle is two or more gaseous starting materials to be imported to a reaction interior, then gaseous starting materials phase
There is chemical reaction between mutually, form a kind of new material, deposit to wafer surface.
Wherein, described preparation process (2), specially：The sample one is placed in 65 DEG C of temperature and is toasted 2 minutes, obtained
Arrive sample two；
The gross thickness of the PMMA glue-lines and UV glue-lines on the surface of the sample three is 110nm；
The time of exposure of preparation process (5) is 35 seconds.
Wherein, after preparation process (5), before preparation process (6), also include preparation process：
(5a) sample five is carried out plasma etching, to remove after nano impression process, on five surface of the sample
The PMMA glue and UV glue of unwanted region residual.
Plasma etching, is modal a kind of form in dry etching, and its principle is the gas to be exposed to electronics regions
Body is plasma, thus produces the gas of ionized gas and release high energy electron composition, to form plasma or ion, ionization
Gas atom can discharge enough strength with surface expulsion power with tightly jointing material or etching material list by electric field acceleration
Face.
Wherein, after preparation process (5), before preparation process (6), also include preparation process：
(5b) configure the solution of 1ppm with octadecyl trichlorosilane alkane and toluene in proportion, the sample five is placed in this
In solution after immersion 12-18 minutes, then it is placed in immersion 1-2 minutes in acetone.
Wherein, described preparation process (5b), specially：
The sample five is placed in the solution by the solution for configuring 1ppm in proportion with octadecyl trichlorosilane alkane and toluene
Middle immersion 15 minutes after, then be placed in acetone soak 1 point 30 seconds.
Fig. 4 is refer to, which is the preparation flow figure of the plastic formwork that the present invention is provided.
Wherein, the preparation process of the plastic formwork, including：
(1) one layer of photoresist of spin coating on rigid substrate, obtains middle product one；
(2) previously prepared mask plate is attached on the photoresist layer of the middle product one, carries out photoetching treatment, in obtaining
Between product two, the dutycycle of the mask plate is 1:1；
(3) the middle product two are carried out reactive ion etching, obtains middle product three, the etching pattern of the middle product three
Bossing thickness be 90-110nm；
(4) using the middle product three, overmolded process is carried out, the plastic formwork is prepared.
Wherein, the thickness of the bossing of the etching pattern of the middle product three is 100nm.
Photoresist is also known as photoresist, being made up of photosensitive resin, sensitizer and solvent these three main components, right
Light activated mixing liquid.After photosensitive resin is through illumination, photocuring reaction can soon occur in exposure region so that this material
Physical property, particularly dissolubility, affinity etc. occur significant change.Process through appropriate solvent again, dissolve solubility portion
Point, you can obtain required image.This is that photoresist is imaged lithography process.
The key step of photoetching treatment includes：Substrate pre-treatment-resist coating-front baking (soft baking)-alignment and exposure-aobvious
Shadow-after bake (post bake)-etching-removal photoresist.
Reactive ion etching is to reach the technology for carving decorations purpose with ion beam as carving decorations means, and its resolution is limited to particle
Enter the path domain that substrate and ion energy exhaust process.The minimum diameter of ion beam about 10nm, so ion etching
It is also 10nm that structure is minimum.Compare electronics to interact with solid, ion scattering effect in solids is less, and can be with very fast
The direct write speed quarter decorations that carry out less than 50nm, so reactive ion etching is a kind of Perfected process of nanometer processing.
Fig. 5 is refer to, which is the optical picture of the plastic formwork that the present invention is provided.
Wherein, the preparation process (4) of the plastic formwork, specifically includes：
(4a) by 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and 40-60 is micro-
The thick PET thin film of rice is laid in the surface of the polydimethylsiloxane, obtains middle product four；
(4b) by the meso sample four in 75-85 DEG C, 35-45 minutes are solidified, by the PET thin film from described
Peel off on rigid substrate, obtain the PET template.
Through experimental verification, the preparation process of the plastic formwork has high repeatable and ease for operation, by this
The electrology characteristic of patterned material for preparing of preparation process be very outstanding.The process of the CNT that the present invention is provided
Method, through lot of experiment validation, also demonstrates which can further improve the electrology characteristic of CNT.These are for follow-up carbon
The research of nano-tube material characteristic suffers from huge help.
Fig. 6 is refer to, which is the design drawing of the mask plate that the present invention is provided.
Wherein, the mask plate is the circular film film that surface arranges array pattern.
Wherein, the photoresist includes positive photoresist and negative photoresist；The positive photoresist is AZ5214 photoetching
Glue or S1805 photoresists, the negative photoresist are SU8-3010 photoresists；
When using the positive photoresist, before the preparation process (1) of the plastic formwork, also include：
Release treatment is done on rigid substrate surface, the release treatment includes Surface Treatment with Plasma and smoked HMDS process.
Wherein, the condition of the reactive ion etching is：
Etching gas are CF4/Ar, and the throughput of etching gas is 30/10sccm, and etching power is 170W, build-up of luminance pressure
For 4Pa, etch period is 30 seconds 3 minutes.
Wherein, the preparation process (4a) of the plastic formwork, specifically includes：
By 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and thick by 50 microns
PET thin film is laid in the surface of the polydimethylsiloxane, obtains middle product four；
The preparation process (4b) of the plastic formwork, specifically includes：
By the meso sample four in 80 DEG C, solidify 40 minutes, by the PET thin film from the rigid substrate
Peel off, obtain the PET template.
The plastic formwork prepared by nanometer embossing, can reuse, and utilization rate is high, contributes to being efficiently completed
The nano-scale array patternization of CNT is processed；
The present invention prepares the rigid substrate of minimum fineness based on MEMS technology, and obtains the modern designs of plastics by overmolded process
Plate.The method can be reused in nanometer embossing, copy the figure of the minimum dimension that wants, and substantially increase preparation
The efficiency and yield rate of technique, it is also possible to according to the different growth techniques of CNT, neatly be completed using the method
Using the CNT as the preparation of X-ray source device.
The processing method of the CNT that the present invention is provided, on the one hand can provide the carbon of the fine pattern for possessing minimum dimension
Nanotube, reduces the cost of the CNT of manufacture nano-scale, and the relatively simple easy realization of nano-imprint process；Another
Aspect, after preparing nano level carbon nano pipe array figure, under same size, the quantity of figure can be improved, and make whole carbon nanometer
The specific surface area of tube material is lifted, and further increases field emission effect, X-ray intensity and the electron emission for producing X ray
Directionality, the x-ray source for effectively providing for radiation treatment field.
Summary preparation process, CNT prepares handling process to be included：
It is to be prepared with the vapor deposition method that ethanol is cracked on silicon due to growing CNT, and substrate needs conduction,
So the substrate that selects here is heavy doping silicon chip.
Before preparing and processing CNT, need first to design mask plates.The size of mask plate is according to follow-up
Come determined, the size of space of array pattern can also affect the preparation and growth of CNT, more influence whether for the requirement of operation
The definition of the follow-up X ray figure produced based on the CNT, therefore, this step is that comparison is crucial.
Before preparing and processing CNT, in addition it is also necessary to first prepare a plastic formwork.Preparing the rotation of plastic formwork
In adhesive process, need the species that photoresist is selected according to the graphic structure of mask plate, the difference of photoresist species can make corresponding
Photoresist process parameter is also different, but the plastic formwork that they finally prepare is consistent, that is, complete the figure for requiring.Make
When using positive photoresist, early stage release treatment, such as Surface Treatment with Plasma (beating plasma) and smoked HMDS process to be done.Photoetching
Processing procedure includes exposed and developed, and exposed and developed is to realize patterned committed step, different time of exposure and aobvious
The shadow time can directly affect graphical effect.In last reactive ion etching, the etching power of equipment, etch period, build-up of luminance pressure
By force, the parameter such as the throughput of etching gas, etching gas also can all affect etching effect, where it is desirable to which the form height that makes is
100 nanometers, i.e., the thickness of the bossing of the etching pattern of described middle product three is 100nm.Plastic formwork is based on middle product
Three overmoldeds are prepared from.By configured 1:10 PDMS is dropped on rigid template, controls the amount of drop, by 40-60 microns
Micron thick PET thin film tiling of thickness, particularly 50 is got on, and is slowly paved using the toughness of PDMS, in 75-85 DEG C, spy
Be not at 80 DEG C, solidification 35-45 minutes, particularly 40 minutes, then at leisure by PET thin film take off from rigid substrate
Come, such piece of plastic template is with regard to overmolded success.The preparation method of the plastic formwork is simple, can keep good complete
Property, to repeat to turn over rate processed high.But the etching pattern structure of the figure and rigid substrate of plastic formwork is contrary.
Longitudinal growth is prepared in the CNT of substrate surface, rotation need to be determined according to the dutycycle of figure in plastic formwork
The height of gluing.First spin coating PMMA glue as nano impression in buffering (sacrifice) layer, in temperature 60-70 DEG C, particularly 65 DEG C
Lower baking 1-3 minutes, particularly 2 minutes, the height of UV glue is controlled, the flexiplast template of preparation is attached to the sample of spin coating glue
On, it is placed in ultraviolet nanometer marking press, evacuation is simultaneously extruded, i.e., nano impression processes post-exposure 30-40 seconds, particularly 35 seconds,
Take out sample four to take flexiplast template away, desired structure is just basically completed, then sample five is lost with plasma reaction machine engraving,
Because the UV glue and PMMA glue that have residual after nano impression stay in unwanted region, can with rational plasma reaction parameter
With by exposed for silicon chip out.
The solution that 1ppm is configured in proportion with octadecyl trichlorosilane alkane and toluene, sample five is put and is soaked in the solution
12-18 minutes, particularly 15 minutes, thus the region to exposing silicon chip done close and distant water process, due to depositing for PMMA glue-lines
, place in acetone immersion 1-2 minutes, be particularly 1 point 30 seconds, to remove protective layer, whole process is just done to sample five
Hydrophobe graphical.
Sample five is placed in CVD growth stove, using ethanol as the carrier of offer hydrogen, in the presence of a catalyst,
Its growth time is controlled, the CNT for requiring height is grown.The 30-40% of configuration dilution, particularly 35% HF solution pair
CNT is processed, by longitudinal growth in substrate surface CNT be placed in dilution 30-40%, particularly 35%
HF solution in soak 1-2 minutes, particularly 1 point 20 seconds, the CNT of longitudinal growth can be made to gather one with a point cluster
Rise, improve the overall specific surface area of semi-conducting material.
For traditional preparation device technology, carbon tube nanometer tube figuring can be confined to the size of component graphics, that is, not
Very little specification can be made.Certainly the requirement for completing more small dimension can also be gone by introducing more advanced equipment, but can be brought
Problem on cost, the processing method of the CNT that the present invention is provided, can neatly change according to the growth technique of CNT
Become and prepare effect, solve and make up these problems well.
The CNT that a kind of processing method of the above-mentioned CNT of application is prepared.
The CNT that is prepared based on the processing method of above-mentioned CNT that the present invention is provided, has been substantially met carbon and has been received
The requirement of mitron nano-scale specification, in same units area, figure number also improves a lot, and then further can carry
The high ray image resolution formed based on the x-ray source that the CNT is produced and definition.
Fig. 7 is refer to, which is the design principle figure of the cold cathode X-ray tube based on CNT that the present invention is provided.
The cold cathode X-ray tube, including body 1, arranges negative electrode 2, anode 3 and grid 4, the negative electrode 2 in the body 1
The above-mentioned CNT of application is prepared from.
Wherein, the CNT is cylinder, a diameter of 10 nanometers of the cylinder, and the height of the cylinder is
3-5 microns；
The negative electrode 2 is rectangle, and the length of the rectangle is 5mm, and the width of the rectangle is 2mm.
Wherein, the body 1 be cylindrical tube, a diameter of 20mm of the cylindrical tube, the cylindrical tube
Length be 80mm.
Wherein, apart from 200 microns of negative electrode, the voltage that the grid 4 is applied in is in 0.3-5 kilovolt ranges for the grid 4.
Wherein, the anode 3 is less than or equal to 5 millimeters with the distance of negative electrode 2, and the voltage that the anode 3 is applied in is in 20-65
In kilovolt range.
Wherein, the grid 4 and anode 3 are copper electrode.
Wherein, the body 1 arranges the beryllium glass 5 that a block length is 200 microns in the part of reflection X-ray.
Wherein, with the horizontal 30-40 ° of angle, the vacuum in the body 1 is 10 to the anode 3-5Pa.
Fig. 8 is refer to, which is the cold cathode X-ray tube based on CNT that traditional X-ray tube and the present invention are provided
Flied emission curve comparison figure.
Flied emission curve, i.e. F-N (Fowler-Nordheim) curve be judge electronic emission performance important according to
According to.According to the conclusion of field emission theory, the curve of F-N is closer to the curve of linear relationship, and its field emission effect is better.
F-N curves in Fig. 8 shown in A correspond to the F-N curves of traditional X-ray tube.
F-N curves in Fig. 8 shown in B correspond to the F-N curves of the cold cathode X-ray tube that the present invention is provided.
Can be seen that carbon nanometer obtained in the processing method of the CNT provided through the present invention from A, B contrast of Fig. 8
Pipe as the aligned carbon-nanotubes of negative electrode F-N curves closer to linear relationship curve, its field emission effect is more preferable.
Fig. 9, Figure 10 and Figure 11 is refer to, which is the cold cathode X-ray tube based on CNT that the present invention is provided respectively
Face structure chart, 3 dimensional drawing and profile.
The cold cathode X-ray tube based on CNT that the present invention is provided, mainly by body 1, negative electrode 2, anode 3, grid 4
With two groups of high voltage power supply compositions, wherein grid 4 is to do field emission, for the electronics in vitalizing semiconductor material, can control
Focal spot size processed and the tube wall for preventing high-velocity electrons from clashing into body 1.
CNT prepared by the processing method of the CNT provided using the present invention does negative electrode 2, the 2 carbon nanometer of negative electrode
The free end cluster of the longitudinal growth of pipe gathers in a bit, improves the specific surface area of CNT, it is achieved that electronics is assembled, and also enters one
It is fixed that step improves field emission effect using cold cathode X-ray tube obtained in the CNT, X-ray intensity and electron emission
Tropism, it is possible to reduce the focusing electrode before grid 4, makes the preparation technology of cold cathode X-ray tube more simplified.
For radiotherapy that is more portable and being preferably applied in medical domain, the volume of X-ray tube is typically intended to
Smaller, so the cold cathode X-ray tube that the present invention is provided goes out a diameter of 20 millimeters using glass processing, length is 80 millimeters
Body 1.
Experimental verification, the cut-in voltage of the CNT for growing out be in hectovolt between kilovoltage, so, set
, at 200 microns, the electrode machining of grid-control is away from 200 microns of distances of negative electrode for the pole plate distance of the cut-in voltage of cold cathode X-ray tube
Place, the power supply of applying is in 0.3-5 kilovolt ranges；
For ensureing that the X-ray energy of cold cathode X-ray tube focuses on out the rule as 5 millimeters × 2 millimeters of carbon nanotube-sample
Lattice, save focusing electrode this step operation, using the good directionality of CNT, need to keep the anode 3 of cold cathode X-ray tube with
In the range of 5 millimeters, the power supply of applying is in 20-65 kilovolt ranges for the distance of negative electrode 2.
For cost-effective, the grid 4 and anode 3 of the cold cathode X-ray tube based on CNT that the present invention is provided all make
Use copper electrode；As glass is with Absorption to X ray, a block length is adopted for 200 in the part for reflecting X ray
The beryllium glass 5 of micron；There is 30 ° -40 ° of angle with horizontal plane in the copper electrode of anode 3；And ensure that the vacuum in pipe is 10- 5Pa.
The cold cathode X-ray tube based on CNT that the present invention is provided can realize the miniaturization of X-ray tube and portable
Change, reduce operating temperature, improve service life, and the superior electrology characteristic of CNT causes cold cathode X-ray tube to work
Instantaneously can carry out, the directionality of launching electronics are also run well than traditional X ray.The cold cathode X-ray tube, based on nano impression
Technology prepares patterned device, and using the graphical device as negative electrode, grows carbon nanomaterial, pass through in cathode substrate
The field emission characteristic of semi-conducting material is realizing X ray.Nanometer embossing can accomplish the nano-structure array of cathode material,
The exposure dose of X ray is improved, the application on therapeutic treatment is completed.The cold cathode X-ray tube solves traditional hot cathode body
The problems such as product is big, cooling negative electrode power consumption is big, and the high voltage power supply that it needs is low, it is not necessary to heat and cool down, temporal properties are good.
The design of the cold cathode X-ray tube so as to possess portable feature, the in addition unique electrology characteristic of CNT and cold cathode
Advantage, can reduce work calorieses, improve the transformation efficiency of X ray, increase the metering of X ray, so as to increase which in radiation
The application value of property therapy field, and can put into production and realize industrialization.The advantage that the cold cathode X-ray tube is present, can be big
Amount applies fixed point in radiation treatment to kill in cancerous cell field, and small volume, X-ray intensity be big, the spy of life-span length
Point can be generalized on market, realized a large amount of productions, be expected to replace traditional X-ray tube.The graphic array of this nanostructured is cloudy
Pole implementation method can also improve x-ray imaging quality and resolution.
The present invention utilizes CNT in the application of medical domain, in conjunction with technology such as nano impression, MEMS, using reflection-type
X ray tubular construction, adds gate control electrode to realize the cold cathode X-ray tube of portable type, miniaturization, compensate for Traditional x-ray
Shortcoming, effectively can put goods on the market, and carry out industrialization production.
It is an advantage of the current invention that：
The plastic formwork prepared by nanometer embossing, can reuse, improve and prepare carbon tube nanometer tube figuring
The efficiency and utilization rate of technique；
Nanometer embossing can realize nanoscale structures, and compare the technique that other realize nanostructured, reduces system
Make cost and easily operate, easily realize；
The design and realization of cold cathode X-ray tube, can realize the purpose of x-ray source small volume, miniaturization and portability；
Cold cathode X-ray tube can accomplish instantaneous work, it is not necessary to preheating time, and it is little to generate heat during working, using the longevity
Life length；
The CNT processed using HF solution, improves its specific surface area, further increases its field emission special
Property, improve the efficiency for producing X ray；
A kind of processing technology of the cold cathode X-ray tube based on CNT, is processed to CNT, is made through place
The specific surface area of the CNT of reason can be increased dramatically, and realize that electronics is assembled, further increase using the carbon nanometer
The field emission effect of the cold cathode X-ray tube that pipe makes, X-ray intensity and electron emission directionality.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's
Thought, will change in specific embodiments and applications, and this specification content is should not be construed as to the present invention
Restriction.
Claims (21)
1. a kind of processing technology of the cold cathode X-ray tube based on CNT, it is characterised in that the cold cathode X-ray tube
Including body, negative electrode, anode and grid are set in the body, the negative electrode application CNT is prepared from, and the carbon is received
Mitron need to be through following process：
Longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, makes longitudinal growth
The free end cluster of CNT gather in a bit；
Described longitudinal growth is soaked in the HF solution of the CNT 30-40% that is placed in dilution of substrate surface, specially：
By longitudinal growth in substrate surface CNT be placed in dilution 35% HF solution in immersion 1 point 20 seconds.
2. the processing technology of the cold cathode X-ray tube based on CNT according to claim 1, it is characterised in that institute
CNT is stated for cylinder, a diameter of 10 nanometers of the cylinder, the height of the cylinder is 3-5 microns.
3. the processing technology of the cold cathode X-ray tube based on CNT according to claim 1, it is characterised in that institute
Longitudinal growth is stated in the preparation process of the CNT of substrate surface, including：
(1) with heavy doping silicon chip as substrate, one layer of PMMA glue of spin coating, obtains sample one over the substrate；
(2) sample one is placed in baking 1-3 minutes in 60-70 DEG C of temperature, sample two is obtained；
(3) one layer of UV glue of spin coating on the PMMA glue-lines of the sample two, obtains sample three, the PMMA on the surface of the sample three
The gross thickness of glue-line and UV glue-lines is 100-120nm；
(4) previously prepared plastic formwork is attached on the UV glue-lines of the sample three, carries out nano impression process, obtain sample
Four, the dutycycle of the plastic formwork is 1:1；
(5) sample four is placed under ultraviolet light, exposes the 30-40 seconds, peeled off the plastic formwork, obtain sample five, described
The gross thickness of the PMMA glue-lines and UV glue-lines of the surface convex portion of sample five is 200-250nm；
(6) sample five is placed in CVD growth stove, using ethanol as the carrier for providing hydrogen, the gas cracked using ethanol
The phase sedimentation method, make to grow longitudinal growth on the substrate in the CNT of substrate surface.
4. the processing technology of the cold cathode X-ray tube based on CNT according to claim 3, it is characterised in that
Preparation process (2), specially：The sample one is placed in 65 DEG C of temperature and is toasted 2 minutes, obtain sample two；
The gross thickness of the PMMA glue-lines and UV glue-lines on the surface of the sample three is 110nm；
The time of exposure of preparation process (5) is 35 seconds.
5. the processing technology of the cold cathode X-ray tube based on CNT according to claim 3, it is characterised in that institute
After stating preparation process (5), before preparation process (6), also include preparation process：
(5a) sample five is carried out plasma etching, to remove after nano impression process, is not required on five surface of the sample
The PMMA glue and UV glue of the region residual that wants.
6. the processing technology of the cold cathode X-ray tube based on CNT according to claim 3, it is characterised in that institute
After stating preparation process (5), before preparation process (6), also include preparation process：
(5b) configure the solution of 1ppm with octadecyl trichlorosilane alkane and toluene in proportion, the sample five is placed in the solution
After middle immersion 12-18 minutes, then it is placed in immersion 1-2 minutes in acetone.
7. the processing technology of the cold cathode X-ray tube based on CNT according to claim 6, it is characterised in that institute
Preparation process (5b) is stated, specially：
The solution that 1ppm is configured in proportion with octadecyl trichlorosilane alkane and toluene, the sample five is placed in the solution and is soaked
Bubble 15 minutes after, then be placed in acetone soak 1 point 30 seconds.
8. the processing technology of the cold cathode X-ray tube based on CNT according to claim 3, it is characterised in that institute
The preparation process of plastic formwork is stated, including：
(1) one layer of photoresist of spin coating on rigid substrate, obtains middle product one；
(2) previously prepared mask plate is attached on the photoresist layer of the middle product one, carries out photoetching treatment, obtain middle product
Two, the dutycycle of the mask plate is 1:1；
(3) the middle product two are carried out reactive ion etching, obtain middle product three, the etching pattern of the middle product three convex
The thickness for playing part is 90-110nm；
(4) using the middle product three, overmolded process is carried out, the plastic formwork is prepared.
9. the processing technology of the cold cathode X-ray tube based on CNT according to claim 8, it is characterised in that institute
The thickness for stating the bossing of the etching pattern of middle product three is 100nm.
10. the processing technology of the cold cathode X-ray tube based on CNT according to claim 8, it is characterised in that institute
The preparation process (4) of plastic formwork is stated, is specifically included：
(4a) by 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and 40-60 microns is thick
PET thin film be laid in the surface of the polydimethylsiloxane, obtain middle product four；
(4b) by the meso sample four in 75-85 DEG C, 35-45 minutes are solidified, by the PET thin film from the rigidity
Peel off on base material, obtain the PET template.
The processing technology of 11. cold cathode X-ray tubes based on CNT according to claim 8, it is characterised in that：
The mask plate is the circular film film that surface arranges array pattern.
The processing technology of 12. cold cathode X-ray tubes based on CNT according to claim 8, it is characterised in that：
The photoresist includes positive photoresist and negative photoresist；The positive photoresist is AZ5214 photoresists or S1805
Photoresist, the negative photoresist are SU8-3010 photoresists；
When using the positive photoresist, before the preparation process (1) of the plastic formwork, also include：
Release treatment is done on rigid substrate surface, the release treatment includes Surface Treatment with Plasma and smoked HMDS process.
The processing technology of 13. cold cathode X-ray tubes based on CNT according to claim 8, it is characterised in that：
The condition of the reactive ion etching is：
Etching gas are CF4/Ar, and the throughput of etching gas is 30/10sccm, and etching power is 170W, and build-up of luminance pressure is
4Pa, etch period are 30 seconds 3 minutes.
The processing technology of 14. cold cathode X-ray tubes based on CNT according to claim 10, it is characterised in that：
The preparation process (4a) of the plastic formwork, specifically includes：
By 1:10 polydimethylsiloxane drops in the etching pattern surface of the middle product three, and 50 microns of thick PET are moulded
Material thin film is laid in the surface of the polydimethylsiloxane, obtains middle product four；
The preparation process (4b) of the plastic formwork, specifically includes：
By the meso sample four in 80 DEG C, solidify 40 minutes, the PET thin film is shelled from the rigid substrate
From the acquisition PET template.
The processing technology of 15. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that：
The negative electrode is rectangle, and the length of the rectangle is 5mm, and the width of the rectangle is 2mm.
The processing technology of 16. cold cathode X-ray tubes based on CNT according to claim 15, it is characterised in that
The body is cylindrical tube, and a diameter of 20mm of the cylindrical tube, the length of the cylindrical tube are 80mm.
The processing technology of 17. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that institute
200 microns of gate distance negative electrode is stated, the voltage that the grid is applied in is in 0.3-5 kilovolt ranges.
The processing technology of 18. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that institute
, less than or equal to 5 millimeters, the voltage that the anode is applied in is in 20-65 kilovolt ranges for the distance that anode is stated with negative electrode.
The processing technology of 19. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that institute
State grid and anode is copper electrode.
The processing technology of 20. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that institute
State body and the beryllium glass that one block length is 200 microns is set in the part of reflection X-ray.
The processing technology of 21. cold cathode X-ray tubes based on CNT according to claim 1, it is characterised in that institute
The angle that anode is with the horizontal 30-40 ° is stated, the vacuum in the body is 10-5Pa.
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| CN101047086A (en) * | 2005-03-28 | 2007-10-03 | 北京汉纳源纳米科技有限公司 | Nano carbon pipe composite field-emission source and manufacturing method thereof |
| CN101148247A (en) * | 2007-08-16 | 2008-03-26 | 郑州大学 | Carbon nanometer tube/silicon honeycomb array preparing method |
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| CN104078293A (en) * | 2013-03-26 | 2014-10-01 | 上海联影医疗科技有限公司 | Field emission electron source and preparation method thereof |
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| CN101047086A (en) * | 2005-03-28 | 2007-10-03 | 北京汉纳源纳米科技有限公司 | Nano carbon pipe composite field-emission source and manufacturing method thereof |
| CN101148247A (en) * | 2007-08-16 | 2008-03-26 | 郑州大学 | Carbon nanometer tube/silicon honeycomb array preparing method |
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