CN107403655A - A kind of X ray neutral filter and preparation method thereof - Google Patents
A kind of X ray neutral filter and preparation method thereof Download PDFInfo
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- CN107403655A CN107403655A CN201710684005.4A CN201710684005A CN107403655A CN 107403655 A CN107403655 A CN 107403655A CN 201710684005 A CN201710684005 A CN 201710684005A CN 107403655 A CN107403655 A CN 107403655A
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
- G21K1/10—Scattering devices; Absorbing devices; Ionising radiation filters
Abstract
The present invention relates to a kind of X ray neutral filter and preparation method thereof, is related to soft x-ray radiation stream quantitative measurment field.The preparation method includes：The first conductive metal layer is formed in a side surface of substrate；Photoresist layer is formed in a side surface of first conductive metal layer away from substrate, exposure, develop forms hole array after photoresist layer, electroplates to form the second conductive metal layer in the photoresist layer with hole array, and the sample of hole array must be had by removing remaining photoresist；Remove substrate and the first conductive metal layer.Effectively improve surface uniformity, attenuation characteristic and the production efficiency of X ray neutral filter.X ray neutral filter made from above-mentioned preparation method, the uniform pore diameter in each hole, hole sidewall, the surface uniformity of X ray neutral filter are good in hole array so that X-ray transparent rate has high consistency, and soft x-ray radiation stream can be achieved and quantitatively accurately measure.
Description
Technical field
The present invention relates to soft x-ray radiation stream quantitative measurment field, and more particularly to a kind of X ray neutral filter and its
Preparation method.
Background technology
In inertial confinement fusion field, hohlraum physicses, radiation transport, radiation ablation, radiopacity and implosion are moved
Mechanics, it is required for carrying out the quantitative measurment of soft x-ray radiation stream.The measurement of radiant flux typically uses X ray flat response X ray two
Pole pipe (XRD) detector.In measurement process, fragment caused by laser target shooting may adhere on multiple filter or punch filter
Piece, so as to influence the measurement accuracy of radiant flux；On the other hand, as the increase of laser energy, radiant flux increase cause flat response
Detector is operated in nonlinear area, beyond detector working range.Therefore, neutral filter is used to eliminate chips affect
The problems such as with detector saturation.
Neutral filter has the characteristic to X-ray attenuation, and the X ray for the different-waveband that pass through uniformly can be declined
Subtract, and the hot spot for ensureing to be transmitted on XRD detectors has high homogeneity.
Traditional neutral filter realizes uniform hole array by the way of laser boring, so as to reach to X ray
Attenuation, but have the following disadvantages：(1) surface uniformity is poor：The method of laser boring is that tantalum piece is burnt by laser
Punching is realized in erosion, and due to the unstability of the limitation of hot spot, and thermal ablation, the aperture for causing laser boring to prepare is uneven,
Poor (2) the taper hole phenomenon of surface uniformity of attenuator：The hole prepared by way of micro- laser boring, due to the ablated surface time
Long, the base ablation time is short, and taper hole is presented in the hole of preparation, so as to cause X-ray transparent rate curve to have certain slope, is not
One fixed numerical value, it is impossible to be considered as neutral filter.(3) preparation efficiency is low：The mode of laser boring is less efficient, with having
The increase of area is imitated, hole number sharply increases, and causes to punch time increase, reduces production efficiency.
The content of the invention
It is an object of the invention to provide a kind of X ray neutral filter, and it has uniform hole array, and in hole array
The uniform pore diameter in each hole, hole sidewall, the surface uniformity of X ray neutral filter are good so that X-ray transparent rate has height
Uniformity is spent, soft x-ray radiation stream can be achieved and quantitatively accurately measure.
Another object of the present invention is to provide a kind of preparation method of above-mentioned X ray neutral filter, effectively improve X and penetrate
Surface uniformity, attenuation characteristic and the production efficiency of line neutral filter.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of preparation method of X ray neutral filter, including：
The first conductive metal layer is formed in a side surface of substrate.
Photoresist layer is formed in a side surface of first conductive metal layer away from substrate, exposure, is developed after photoresist layer
Hole array is formed, electroplates to form the second conductive metal layer in the photoresist layer with hole array, removing remaining photoresist must have
There is the sample of hole array.
Remove substrate and the first conductive metal layer.
The present invention proposes that X ray neutral filter made from method is prepared as above in one kind.
A kind of beneficial effect of X ray neutral filter provided in an embodiment of the present invention and preparation method thereof is：
Combined by using photoetching and microplating technique, prepare the neutral filter of the X ray with uniform hole array,
Perforating efficiency is effectively improved, improves production efficiency, the uniform pore diameter in each hole, the surface uniformity of attenuator is good, effectively solves cone
Hole phenomenon, the precision of the final neutral filter for improving X ray.
The X ray neutral filter as made from the above method has a uniform hole array, and in hole array each hole hole
Footpath is uniform, hole sidewall, and the surface uniformity of X ray neutral filter is good so that and X-ray transparent rate has high consistency,
Soft x-ray radiation stream can be achieved quantitatively accurately to measure.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below by embodiment it is required use it is attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore be not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the preparation method schematic flow sheet for the X ray neutral filter that preferred embodiments of the present invention provide；
Fig. 2 is the structural representation for the X ray neutral filter that present pre-ferred embodiments provide；
The surface uniformity data for the X ray neutral filter that Fig. 3 preferred embodiments of the present invention provide；
The surface micro-image for the X ray neutral filter that Fig. 4 preferred embodiments of the present invention provide；
The X-ray transparent rate for the X ray neutral filter that Fig. 5 preferred embodiments of the present invention provide.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
X ray neutral filter of the embodiment of the present invention and preparation method thereof is specifically described below.
Referring to Fig. 1, a kind of preparation method of X ray neutral filter, it includes：
A) the first conductive metal layer is formed in a side surface of substrate.
B) photoresist layer is formed in a side surface of first conductive metal layer away from substrate, light is formed at after exposure, development
Photoresist layer forms hole array, electroplates to form the second conductive metal layer in the photoresist layer with hole array, removes remaining photoetching
Glue must have the sample of hole array.
C) substrate and the first conductive metal layer in sample are removed.
Specifically, in step a), substrate is oxidized silicon chip, is easy to subsequently remove.
First conductive metal layer is formed in substrate deposition by magnetron sputtering technique, as plating seed layer, wherein, magnetic control
Sputtering technology can effectively improve the efficiency of plated film, while make the first conductive metal layer surface smooth, more easy-formation.
First conductive metal layer can be the materials such as copper, gold, silver, such as the first conductive metal layer can be copper or gold.The
One conductive metal layer can be used as corrosion barrier layer during subsequent corrosion substrate, and the precision of final products is effectively ensured,
And the chemical property of gold is more stable, therefore, it is highly preferred that the first conductive metal layer is gold.
The thickness of the first conductive metal layer is 20-50nm simultaneously；And/or second conductive metal layer thickness >=20 μm.I.e.
When the thickness of first conductive metal layer is 20-50nm, for example, the first conductive metal layer thickness for 20nm, 25nm, 30nm,
40nm, 45nm or 50nm etc., the thickness of the second conductive metal layer can with >=20 μm, or<20μm.
Second conductive metal layer can be the materials such as copper, gold, silver, such as the second conductive metal layer can be copper or gold.It is excellent
Selection of land, because the second conductive metal layer is final product, but stress inside it be present, therefore easy stress production in production process
Raw fold, the precision and yield rate of product are influenceed, it is preferred that the material of the first conductive metal layer and the second conductive gold
It is identical to belong to the material of layer, can effectively discharge the stress of the second conductive metal layer, effectively improve the precision and finished product of product
Rate.
It is highly preferred that the material of the first conductive metal layer is gold, the material of the second conductive metal layer is gold, effectively improves X
The yield rate of ray neutral filter, it is not only convenient for removing in step d), while the second conductive metal layer after removal does not have
Metal penetrates into, and the precision of X ray neutral filter is effectively ensured.
In step b), to photoresist layer front baking before exposure, after exposure to photoresist layer after dry, effectively determine photoresist
Type.Preferably, in preferred embodiments of the present invention, front baking is：After 55-65 DEG C is dried 13-20min, 30- is dried at 85-95 DEG C
40min；It is highly preferred that front baking is：After 60 DEG C are dried 15min, 35min is dried at 90 DEG C, effectively removes the solvent in photoresist, together
The adhesion of Shi Zengqiang photoresists, discharge the stress in photoresist film prevents photoresist from staining equipment simultaneously.
Preferably, in preferred embodiments of the present invention, rear dry is：After 65-75 DEG C is dried 13-20min, in 85-95 DEG C of baking
45-55min；It is highly preferred that rear dry is：After 65 DEG C are dried 15min, 50min is dried at 90 DEG C, is effectively evaporated molten inside photoresist
Agent, photoresist is hardened solidification, be convenient for follow-up development, plating.
Preferably, the thickness of photoresist is at least 20 μm, i.e., photoresist is thick glue, therefore preferably uses ultraviolet
Carve, it is highly preferred that exposure is uv-exposure 20-30s.It is preferred that photoresist is SU-8 photoresists or AZ4620 photoresists,
It is highly preferred that photoresist is SU-8 photoresists, after forming thick glue, lithographic results are more preferably.
Specifically, develop 2.7-3.3min, prevent developing time it is too short caused by underdevelop, develop it is incomplete and aobvious
Cross and develop caused by shadow overlong time, influence the performance of final obtained X ray neutral filter.
Carried out using developer solution corresponding with above-mentioned photoresist, such as the special developer solutions of SU-8 corresponding with SU-8 photoresists
Development, i.e., dissolved soluble above-mentioned photoresist by developer solution, and hole array is formed in photoresist layer.Wherein, the Kong Zhen
Row with cylinder into array by uniformly forming more.Preferably, a diameter of 30-40 μm of each cylinder；Preferably, each cylinder
A diameter of 35 μm；And/or the spacing between the axis of two cylinders of arbitrary neighborhood is 80-120 μm；It is highly preferred that any phase
Spacing between the axis of two adjacent cylinders is 100 μm, makes the light transmittance of final obtained X ray neutral filter more preferably,
Effective attenuation X ray.
Electroplate to form the second conductive metal layer in the photoresist layer with hole array, it is preferable that rate of deposition control exists
2.5-3.5 μm/h, it is highly preferred that rate of deposition is controlled in 3 μm/h, the conductive metal layer of uniformly-coating second, make the second conductive gold
Belong to formable layer rate height and surfacing.Then, the sample with hole array is obtained after removing remaining photoresist.
Wherein, the hole array on sample herein and the hole array of photoresist layer are complementary, form complete entity, i.e. sample
On hole array in each hole and photoresist layer hole array in each cylinder correspond.Hole array i.e. on sample
In, the aperture in each hole is 30-40 μm；Preferably, the aperture in each hole is 35 μm；And/or the hole in two holes of arbitrary neighborhood
Spacing is 80-120 μm；Preferably, the pitch of holes between two holes of arbitrary neighborhood is 100 μm, is made in final obtained X ray
The light transmittance of property attenuator more preferably, effective attenuation X ray.
Preferably, soaked after electroplating the second conductive metal layer in nmp solution, can effectively remove remaining photoresist, together
When on the second conductive metal layer, the first metal material layer and substrate without influence.
Due in preferred embodiments of the present invention, X ray neutral filter is used alone, in order to ensure its it is long-term keep compared with
Good precision, it is preferable that before made annealing treatment sample with the first conductive metal layer in removing substrate；It is highly preferred that
Make annealing treatment and handle 2.5-4h in 145-160 DEG C；3h is handled in 150 DEG C it is highly preferred that making annealing treatment, effectively removing its inside should
Power, its precision is set to keep longer time.
After annealing, substrate and the first conductive metal layer are removed, obtains X ray neutral filter.
In preferred embodiments of the present invention, substrate is removed by acid corrosion；Preferably, acid is 2-7 by volume ratio：1 hydrogen
Fluoric acid and concentrated nitric acid, such as volume ratio are 2：1、3：1、4：1、5：1、6：1 or 7：The ratio mixing gained of 1 grade, wherein, hydrofluoric acid
For the general hydrofluoric acid sold in market, concentrated nitric acid is the general concentrated nitric acid sold in market, is not limited herein.Meanwhile removed by acid corrosion
During substrate, the first conductive metal layer can be used as corrosion barrier layer, prevent the conductive metal layer of acid corrosion second, influence final products
Precision.
After removing substrate, then it is soaked in ultrasonic wave in alcohol and cleans 10-23min, remove the first conductive metal layer.It is preferred that
Ground, remove the X ray neutral filter that the first conductive metal layer can obtain different size by laser scribing.
Referring to Fig. 2, the present invention also provides the X ray neutral filter as made from the above method, it has uniform hole
Array, and in hole array each hole uniform pore diameter, hole sidewall, the surface uniformity of X ray neutral filter is good so that X
Radiolucent rate has high consistency, and soft x-ray radiation stream can be achieved and quantitatively accurately measure.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of X ray neutral filter, it is made by following methods：
1) 40nm the first conductive metal layer is deposited on 2 cun of oxidized silicon chips by magnetron sputtering technique.
2) after a side surface spin coating thickness of first conductive metal layer away from substrate is 35 μm of SU-8 photoresists, 60
DEG C dry 15min, then 90 DEG C dry 35min after, after uv-exposure 24s, 65 DEG C dry 15min, then 90 DEG C dry 50min,
Then after using the special developing liquid developing 3min of SU-8, the hole array being made up of cylinder is formed in photoresist layer.
3) pulse microplating technique is used in the photoresist layer with hole array, electroplate 20 μm with 3 μm/h speed the
After two conductive metal layers, remaining photoresist is removed by being soaked in nmp solution, obtains the sample with hole array.
Wherein, 35 μm of the aperture in each hole in the hole array of sample, 100 μm of the pitch of holes in two holes of arbitrary neighborhood.
4) it is 4 with volume ratio after 150 DEG C of insulation 3h are made annealing treatment to be in temperature by sample:1 hydrofluoric acid and dense nitre
The mixed solution of acid corrodes to silicon chip, after corrosion terminates at the first conductive metallic material layer automatically, is put into alcohol ultrasonic
Ripple cleans 15min, removes the first conductive metallic material layer, and X ray neutral filter is made in laser scribing.
Wherein, the first conductive metal layer and the second conductive metal layer are layer gold.
Embodiment 2
A kind of X ray neutral filter, it is made by following methods：
1) 50nm the first conductive metal layer is deposited on 2 cun of oxidized silicon chips by magnetron sputtering technique.
2) after a side surface spin coating thickness of first conductive metal layer away from substrate is 25 μm of SU-8 photoresists, 55
DEG C dry 13min, then 85 DEG C dry 30min after, after uv-exposure 26s, 65 DEG C dry 16min, then 85 DEG C dry 40min,
Then after using the special developing liquid developing 2.7min of SU-8, the hole array being made up of cylinder is formed in photoresist layer.
3) pulse microplating technique is used in the photoresist layer with hole array, 25 μm is electroplated with 2.5 μm/h speed
After second conductive metal layer, remaining photoresist is removed by being soaked in nmp solution, obtains the sample with hole array.
Wherein, 30 μm of the aperture in each hole in the hole array of sample, 84 μm of the pitch of holes in two holes of arbitrary neighborhood.
4) it is 7 with volume ratio after 145 DEG C of insulation 4h are made annealing treatment to be in temperature by sample:1 hydrofluoric acid and dense nitre
The mixed solution of acid corrodes to silicon chip, after corrosion terminates at the first conductive metallic material layer automatically, is put into alcohol ultrasonic
Ripple cleans 15min, removes the first conductive metallic material layer, and X ray neutral filter is made in laser scribing.
Wherein, the first conductive metal layer and the second conductive metal layer are layer gold.
Embodiment 3
A kind of X ray neutral filter, it is made by following methods：
1) 20nm the first conductive metal layer is deposited on 2.5 cun of oxidized silicon chips by magnetron sputtering technique.
2) after a side surface spin coating thickness of first conductive metal layer away from substrate is 40 μm of SU-8 photoresists, 65
DEG C dry 15min, then 95 DEG C dry 30min after, after uv-exposure 27s, 65 DEG C dry 20min, then 90 DEG C dry 52min,
Then after using the special developing liquid developing 3.4min of SU-8, the hole array being made up of cylinder is formed in photoresist layer.
3) pulse microplating technique is used in the photoresist layer with the hole array being made up of cylinder, with 3.1 μm/h speed
After rate electroplates 30 μm of the second conductive metal layer, remaining photoresist is removed by being soaked in nmp solution, is obtained with hole array
Sample.
Wherein, 40 μm of the aperture in each hole in the hole array of sample, 112 μm of the pitch of holes in two holes of arbitrary neighborhood.
First conductive metal layer and the second conductive metal layer are layer gold.
Test example
Using X ray neutral filter obtained by the present invention, in Institute of High Energy Physcis, Academia Sinica's Synchrotron Radiation
Enterprising rower location survey amount, using 4B7B bunch therein, it is equal 70-1600eV energy area scope X ray neutral filter face is carried out
Even property measurement.
Specifically measuring method is：X ray neutral filter moves on the direction perpendicular to bunch according to fixed step-length
It is dynamic, the photoelectric current of measurement X ray neutral filter surface diverse location (sample 1# and sample 2#), so as to characterize the surface of filter disc
Uniformity.As a result it is as shown in Figure 3.As seen in Figure 3, neutral filter surface uniformity of the present invention is good, and heterogeneity exists
Within 1%.
Micrometering is carried out on transmission microscopy using X ray neutral filter obtained by the present invention, measures obtained figure
Piece such as Fig. 4.
Using X ray neutral filter obtained by the present invention in Institute of High Energy Physcis, Academia Sinica's Synchrotron Radiation
Demarcation measurement is carried out, using 4B7B bunch therein, having carried out 70-1600eV can area's scope X ray neutral filter transmitance
Measurement.
Measuring method：Neutral filter is directly installed on bunch and carries out quantitative measurment, by contrasting light source source strength
With through the luminous intensity after neutral filter, the transmitance of the X ray of X ray neutral filter is obtained.As a result it is as shown in Figure 5.
As seen in Figure 5, X ray neutral filter provided by the invention has consistent to the X ray of different-energy
Attenuation characteristic, X ray neutral filter 70-1600eV can be in the range of area transmitance for 0.103 ± 0.002 (wherein also
Contain the qualitative influence brought of flashing).
To sum up, X ray neutral filter provided by the invention and preparation method thereof, the preparation method effectively improves X ray
Surface uniformity, attenuation characteristic and the production efficiency of neutral filter, make obtained X ray neutral filter surface uniformity good, make
Obtaining X-ray transparent rate has high consistency, and soft x-ray radiation stream can be achieved and quantitatively accurately measure.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
- A kind of 1. preparation method of X ray neutral filter, it is characterised in that including：The first conductive metal layer is formed in a side surface of substrate；Photoresist layer is formed in a side surface of first conductive metal layer away from the substrate, exposure, is developed after described Photoresist layer forms hole array, electroplates to form the second conductive metal layer in the photoresist layer with hole array, removes remaining institute The sample of hole array must be had by stating photoresist；Remove the substrate and first conductive metal layer.
- 2. preparation method according to claim 1, it is characterised in that remove the substrate and first conductive metal layer The sample is made annealing treatment before；Preferably, make annealing treatment and handle 2.5-4h in 145-160 DEG C；Preferably, make annealing treatment and handle 3h in 150 DEG C.
- 3. preparation method according to claim 1, it is characterised in that the material of first conductive metal layer for gold or Copper；And/or the material of second conductive metal layer is gold or copper；Preferably, the material of first conductive metal layer is identical with the material of second conductive metal layer；It is highly preferred that the material of first conductive metal layer is gold, the material of second conductive metal layer is gold.
- 4. preparation method according to claim 1, it is characterised in that each described in the hole array that the sample has The aperture in hole is 30-40 μm；It is preferred that the aperture in each hole is 35 μm；And/or the pitch of holes in two holes of arbitrary neighborhood is 80-120 μm；It is preferred that the pitch of holes between two holes of arbitrary neighborhood is 100 μm.
- 5. preparation method according to claim 1, it is characterised in thatTo the photoresist layer front baking before exposure, after exposure to the photoresist layer after dry；Preferably, front baking is：After 55-65 DEG C is dried 13-20min, 30-40min is dried at 85-95 DEG C；Preferably, rear dry is：After 65-75 DEG C is dried 13-20min, 45-55min is dried at 85-95 DEG C；Preferably, expose for uv-exposure 20-30s；Preferably, the photoresist is SU-8 photoresists or AZ4620 photoresists.
- 6. preparation method according to claim 1, it is characterised in that the thickness of first conductive metal layer is 20- 50nm；And/orThickness >=20 μm of second conductive metal layer.
- 7. preparation method according to claim 1, it is characterised in that molten in NMP after plating second conductive metal layer Soaked in liquid, remove remaining photoresist.
- 8. preparation method according to claim 1, it is characterised in that substrate is removed by acid corrosion；Preferably, the acid is 2-7 by volume ratio：1 hydrofluoric acid and concentrated nitric acid mixing gained.
- 9. preparation method according to claim 8, it is characterised in that after removing substrate, it is clear to be soaked in ultrasonic wave in alcohol 10-23min is washed, removes first conductive metal layer.
- 10. X ray neutral filter made from the preparation method as described in claim 1-9 any one.
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