CN107142449B - A kind of preparation method of high-precision very small dimensions self-supporting beryllium film - Google Patents
A kind of preparation method of high-precision very small dimensions self-supporting beryllium film Download PDFInfo
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- CN107142449B CN107142449B CN201710307426.5A CN201710307426A CN107142449B CN 107142449 B CN107142449 B CN 107142449B CN 201710307426 A CN201710307426 A CN 201710307426A CN 107142449 B CN107142449 B CN 107142449B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0005—Separation of the coating from the substrate
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
Abstract
The invention discloses a kind of preparation methods of high-precision very small dimensions self-supporting beryllium film, successively the following steps are included: processing high-precision step in copper block surface；Fine gtinding copper step end face roughness is to nanometer scale；In copper step end face hydatogenesis aluminium film；Beryllium film is deposited on aluminium film surface；Removal aluminium film substrate is reacted using NaOH solution, obtains high-precision very small dimensions self-supporting beryllium film；The present invention greatly improves the dimensional accuracy of very small dimensions self-supporting beryllium film, and precision is up to 1 μm；And resulting self-supporting beryllium film surface is smooth, no sand holes, and regular shape is superior in quality.
Description
Technical field
The present invention relates to self-supporting beryllium film technical fields, it is more particularly related to a kind of minimum ruler of high-precision
The preparation method of very little self-supporting beryllium film.
Background technique
Beryllium (Be) is one of rare metal, compared with other low ordinal number metal materials, with density is low, fusing point is high, intensity
And the features such as elasticity modulus is high, specific heat capacity is big, X-ray transparent rate is high, controllable thermal neutron scattering, unique physical chemistry
Property makes it have important application value in nuclear industry, aerospace, metallurgical industry and high-tech area.
Self-supporting beryllium film refers to no substrate supports and self-existent beryllium film, " high-precision very small dimensions of the invention
Self-supporting beryllium film " refers to that shape (round or rectangular) size is less than 1mm, is typically in the range of tens of to hundreds of unless stated otherwise
μm, dimensional accuracy is up to 1 μm, with a thickness of 1 μm ~ 10 μm of accurate self-supporting beryllium film.High-precision very small dimensions self-supporting beryllium film
It is usually used in the state equation target in laser physics experiment, X-ray filter disc on certain precision instruments etc., the target or filter disc are for certainly
Support the outer dimension required precision of beryllium film high, conventional self-supporting film preparation method is unable to satisfy requirement.
At present it has been reported that the preparation method of large scale self-supporting beryllium film, the general exposure mask conduct for using certain size
Self-supporting beryllium film shape, the dimensional accuracy of exposure mask is not generally high, while in deposition film due to caused by mask thicknesses
Shadow effect, the size and mask dimensions for eventually leading to self-supporting beryllium film have differences, this kind of method is for preparation high-precision
The applicability of very small dimensions self-supporting beryllium film is lower.
Summary of the invention
The object of the invention is that a kind of high-precision very small dimensions self-supporting beryllium film is provided, to solve the above problems.
To achieve the goals above, the technical solution adopted by the present invention is that such: a kind of high-precision very small dimensions are from propping up
Support beryllium film preparation method, successively the following steps are included:
(a) high-precision step is processed in copper block surface；
(b) fine gtinding copper step end face roughness is to nanometer scale；
(c) in copper step end face hydatogenesis aluminium film；
(d) beryllium film is deposited on aluminium film surface；
(e) using NaOH solution reaction removal aluminium film substrate, high-precision very small dimensions self-supporting beryllium film is obtained.
As a preferred technical scheme: copper billet body described in step (a) is pure copper material, and the size of the copper billet body is
10mm × 10mm × 10mm ~ 15mm × 15mm × 15mm, high-precision step are processed using accurate digital control, and step height 1mm ~
2mm, step profile (round or rectangular) size are less than 1mm, and the terrace precision control is at 1 μm.
It can effectively ensure that the dimensional accuracy of copper step using accurate digital control processing, and high-precision step dimension is to guarantee pole
The key of small size self-supporting beryllium film precision.
As a preferred technical scheme: fine gtinding described in step (b) is carried out using high-efficiency and precision polishing machine.
As further preferred technical solution: the fine gtinding method are as follows: the polishing disk up and down of polishing machine is distinguished
With the reverse rotation of different rotary direction, lapping liquid uses particle for the diamond polishing liquid of micro-nano magnitude or oxide cmp liquid,
Step end face roughness value after grinding is characterized with probe-type contourgraph, and value is less than 50nm, thin to meet deposition of soluble
To the roughness requirements of substrate when film.
As a preferred technical scheme: aluminium film described in step (c) is prepared using thermal evaporation, and 0.5 μm of aluminium film thickness ~
1 μm, surface roughness Ra value is no more than 50nm.
As a preferred technical scheme: beryllium film described in step (d) is deposited using magnetron sputtering, and beryllium film is with a thickness of 1 μ
M ~ 10 μm, beryllium film surface roughness Ra value are no more than 100nm.
As a preferred technical scheme: NaOH solution described in step (e), concentration value are ‰ ~ 6wt. of 3wt. ‰.
Aluminium film as soluble substrate can be reacted with the NaOH solution of debita spissitudo and be removed, to obtain height
Precision very small dimensions self-supporting beryllium film.
For the present invention using the copper step of NC super machining as self-supporting beryllium film shape, step profile precision is controllable
At 1 μm, and pole can be greatly improved in shadow effect of the step protruded when avoiding using mask deposition beryllium film, the two combination
The dimensional accuracy of small size self-supporting beryllium film.The present invention is using the metal aluminium film of hydatogenesis as soluble lining simultaneously
Bottom is different from other self-supported membranes and prepares common solvable inorganic salts substrate, and the crystal structure of aluminium film substrate densification can be improved
Beryllium film deposition quality, self-supporting beryllium film surface is smooth after demoulding, no sand holes, and regular shape is superior in quality.
Compared with the prior art, the advantages of the present invention are as follows: the present invention greatly improves very small dimensions self-supporting beryllium film
Dimensional accuracy, precision is up to 1 μm；And resulting self-supporting beryllium film surface is smooth, no sand holes, and regular shape is quality
It is good.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that the fine copper block of step is machined in the embodiment of the present invention；
Fig. 2 is the structural schematic diagram in the embodiment of the present invention after fine gtinding step end face；
Fig. 3 is the structural schematic diagram in the embodiment of the present invention after deposition of aluminum film-substrate；
Fig. 4 is that the structural schematic diagram after beryllium film is deposited in the embodiment of the present invention；
Fig. 5 is that the structural schematic diagram after aluminium film substrate is removed in the embodiment of the present invention.
In figure: 1, fine copper block；2, step；3, step end face；4, aluminium film；5, beryllium film.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings.
Embodiment:
A kind of preparation method of high-precision very small dimensions self-supporting beryllium film, successively the following steps are included:
Step 1: processing high-precision step in copper block surface accurate digital control
The present embodiment using 10mm × 10mm × 10mm fine copper block as matrix (inventor is experimentally confirmed,
The present invention may be implemented in 10mm × 10mm × 10mm ~ 15mm × 15mm × 15mm size), choose installation way appropriate,
Cutter, chip parameter etc. process high-precision step in copper block surface layered milling accurate digital control, and step height 1mm ~
2mm.It is general up to 1 μm since numerical control processing mode precision is high, using the processing method, the shape (round or rectangular) of step
Size accurately controls a certain numerical value between tens of μm to hundreds of μm.The step profile size be high-precision very small dimensions from
The outer dimension for supporting beryllium film, by controlling the outer dimension of copper step accurately to ensure that high-precision self-supporting beryllium indirectly
The dimensional accuracy of film.The step is as shown in Figure 1.
Step 2: fine gtinding copper step end face roughness is to nanometer scale
Since the surface roughness after copper step end face numerical control processing is higher, generally between 0.4 μm ~ 0.8 μm, Wu Faman
To the roughness requirements of substrate when sufficient deposition film, it is necessary to be polished directly to it.The present embodiment is polished using high-efficiency and precision
Machine finely polishes the end face of copper step, and the polishing disk up and down of polishing machine with the reverse rotation of different rotary direction, is thrown respectively
Light pressure can be completed by adjusting upper polishing disk pressure.In polishing process, copper step is fixed on lower polishing disk, end face court
On, polishing disk pressure in adjusting, and it is aided with the polishing fluid (diamond polishing of different polishing disk materials, different-grain diameter and ingredient
Liquid or oxide cmp liquid), polishing revolving speed etc., copper step end face is finally polished to surface roughness Ra value less than 50nm, slightly
Rugosity value is characterized using probe-type contourgraph.The step is as shown in Figure 2.
Step 3: in copper step end face hydatogenesis aluminium film
It after copper step after polishing is cleaned using absolute alcohol, is put into thermal evaporation deposition room, crucible uses BN
Material, and high pure metal aluminium wire (99.99at.%) is put into as evaporation raw material in crucible.Baffle is placed in right above evaporation source
Settling chamber is closed in position, opens vacuum system, until vacuum degree is up to 1 × 10-5Pa.AC power source is opened, heating electricity is slowly increased
Be depressed into 1050 DEG C of evaporating temperature, open baffle and start that aluminium film formally is deposited, at this time aluminium film growth rate about 65nm/min ~
70nm/min, after several minutes, aluminium film thickness is up to 0.5 μm ~ 1 μm.Heating voltage is slowly reduced afterwards to zero-bit, closes alternating current
Vacuum system is closed in source, opens settling chamber, and the copper step after aluminium film has been deposited in taking-up.The step is as shown in Figure 3.
Step 4: depositing beryllium film in aluminium film surface magnetic control sputtering
Using Deposited By Dc Magnetron Sputtering beryllium film, sputtering beryllium target size is 3 inches of diameter, thickness 5mm in experiment, pure
Spend 99at.%.The copper step that aluminium film has been deposited is put into magnetic control sputtering device immediately below sputtering target at 100mm, sample introduction is closed
Window is separately turned on mechanical pump and molecular pump, until vacuum degree is up to 1 × 10-5Pa.It opens Ar air cock and keeps Ar air-flow meter
Size is 5sccm, and adjusting slide valve opening degree to vacuum chamber sputtering pressure is 0.4Pa, opens shielding power supply, observes vacuum chamber
Whether interior aura is normal, raising sputtering power to 140W, adjusting substrate DC bias to 60V, the life of beryllium film under this sputtering condition
Long rate is 15.5nm/min, and the sedimentation time of required thickness beryllium film is extrapolated by beryllium film growth rate.After the completion of deposition, close
Shielding power supply closes back bias voltage, closes Ar air-flow meter, closes Ar air cock, closes molecular pump, mechanical pump respectively, is depositing
Interior is filled with high-purity N2Gas, until maintaining an equal level with external atmosphere pressure, opens settling chamber to maintain the hypoxemia degree in magnetic control sputtering device
Sample introduction window takes out the copper step that beryllium film has been deposited on aluminium film substrate.The step is as shown in Figure 4.
Step 5: reacting removal aluminium film substrate using NaOH solution, high-precision very small dimensions self-supporting beryllium film is obtained
By in the copper step merging NaOH solution after the deposition beryllium film on aluminium film substrate, gone using NaOH and reactive aluminum
Except aluminium film substrate, NaOH solution concentration is that (inventor is experimentally confirmed 3wt. ‰, ‰ ~ 6wt. of 3wt. ‰ in the present embodiment
Concentration be able to achieve the present invention).Since beryllium is Amphoteric Materials, will react with the NaOH of high concentration, but in low concentration
It is not reacted substantially in NaOH solution, while NaOH is not also reacted with copper block materials.In this way in lossless beryllium film
Under the conditions of remove aluminium film substrate, to obtain the self-supporting beryllium film of high-precision very small dimensions, and with strainer by it from solution
In pull out to be transferred in distilled water and impregnate, to remove the chemical substance for being adhered to beryllium film surface, finally pulled out with strainer
It dries, experimental procedure terminates.The step is as shown in Figure 5.
Wherein, the equation that aluminium is reacted with NaOH are as follows:
2Al+2NaOH+2H2O=2NaAlO2+3H2
Due to the hypertoxicity of metallic beryllium, above-mentioned Overall Steps must have stringent safeguard procedures, and preparation step is special
Beryllium prevention room in carry out, dust containing beryllium is discharged into atmosphere after filtering, while beryllium film preparation facilities is placed in shield,
Operator dresses integrated protective clothing and respirator works, it is ensured that environment and personnel safety.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (7)
1. a kind of preparation method of high-precision very small dimensions self-supporting beryllium film, which is characterized in that successively the following steps are included:
(a) high-precision step is processed in copper block surface；
(b) fine gtinding copper step end face roughness is to nanometer scale；
(c) in copper step end face hydatogenesis aluminium film；
(d) beryllium film is deposited on aluminium film surface；
(e) using NaOH solution reaction removal aluminium film substrate, high-precision very small dimensions self-supporting beryllium film is obtained.
2. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 1, it is characterised in that: step
(a) copper billet body described in is pure copper material, the size of the copper billet body between 10mm × 10mm × 10mm ~ 15mm × 15mm ×
15mm, high-precision step using accurate digital control process, step height 1mm ~ 2mm, step profile size be less than 1mm, described
Rank precision controlling is at 1 μm.
3. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 1, it is characterised in that: step
(b) fine gtinding described in is carried out using high-efficiency and precision polishing machine.
4. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 3, it is characterised in that: described
Fine gtinding method are as follows: the polishing disk up and down of polishing machine respectively with different rotary direction reverse rotation, lapping liquid use particle for
The diamond polishing liquid or oxide cmp liquid of micro-nano magnitude, the step end face roughness value probe-type contourgraph after grinding
Characterization, value are less than 50nm.
5. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 1, it is characterised in that: step
(c) aluminium film described in is prepared using thermal evaporation, and 0.5 μm ~ 1 μm of aluminium film thickness, surface roughness Ra value is no more than 50nm.
6. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 1, it is characterised in that: step
(d) beryllium film described in is deposited using magnetron sputtering, and with a thickness of 1 μm ~ 10 μm, beryllium film surface roughness Ra value does not surpass beryllium film
Cross 100nm.
7. the preparation method of high-precision very small dimensions self-supporting beryllium film according to claim 1, it is characterised in that: step
(e) NaOH solution described in, concentration value are ‰ ~ 6wt. of 3wt. ‰.
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| CN109136831B (en) * | 2018-08-16 | 2020-04-24 | 广州本康环保科技有限公司 | A mass thickness of 700-2Self-supporting germanium film and preparation method thereof |
| CN109082634B (en) * | 2018-08-16 | 2020-04-24 | 广州本康环保科技有限公司 | A mass thickness of 500-2Self-supporting gallium film and preparation method thereof |
| CN109136832B (en) * | 2018-08-16 | 2020-04-24 | 广州本康环保科技有限公司 | A mass thickness of 600-2Self-supporting indium film and preparation method thereof |
| CN109023230B (en) * | 2018-08-16 | 2020-04-24 | 广州本康环保科技有限公司 | A mass thickness of 700-2Self-supporting tin film and preparation method thereof |
| CN110004404A (en) * | 2019-05-07 | 2019-07-12 | 晏梦雨 | A kind of preparation method of self-supporting micron copper foil |
| CN111681782B (en) * | 2020-06-18 | 2022-06-07 | 中国工程物理研究院激光聚变研究中心 | Method for manufacturing impedance matching target |
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