CN105045036A - Wax paper mask and preparation method thereof - Google Patents
Wax paper mask and preparation method thereof Download PDFInfo
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- CN105045036A CN105045036A CN201510528675.8A CN201510528675A CN105045036A CN 105045036 A CN105045036 A CN 105045036A CN 201510528675 A CN201510528675 A CN 201510528675A CN 105045036 A CN105045036 A CN 105045036A
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Abstract
The invention provides a preparation method for a wax paper mask and application thereof. The preparation method comprises the following steps of: exposing polymethyl methacrylate with weight-average molecular weight of 50,000 to 950,000 in a condition of exposure dose of 210-430 micro C/cm<2>; carrying out photographic fixing and developing to obtain the wax paper mask. The wax paper mask obtained according to the preparation method is formed in one time, meanwhile, the mask simultaneously contains a thin film layer and a support layer, the thin film layer is used for forming nano particles and contains holes, the support layer contains a larger cavity, the cavity in the support layer is located below the holes, the cross section area of the cavity is larger than the cross section areas of the holes, and thus, the mask and a substrate can be tightly combined. When the preparation method is used for forming the nano particles, a vignetting effect is effectively reduced.
Description
Technical field
The invention belongs to field of nanometer technology, particularly relate to a kind of paraffin paper mask and preparation method thereof.
Background technology
Stencilling art is a kind of widely used technology preparing micro-nano structure.Its usually uses film of one deck perforate as deposition mask, by the pore appearance of film surface determine through nanoparticle deposition form the nanostructured identical with pore appearance.Stencilling art possesses other advantages not available for micro-nano technology means many: such as do not need to make with photoresist; Mask can be reused; Can be used for processing sandwich construction etc.Stencilling art is made to have important Research Prospects in existing scientific research and commercial production just because of these significant advantages.
But, disclosed stencilling art produces halation effect due to the intrinsic gap between mask and substrate at present, and then affect the physical property of the nanostructured obtained, namely when stencil mask and substrate contact, due to the local out-of-flatness of macro surface, make the space that always there are about 10 microns between mask and substrate, now when nano particle deposits to substrate surface by mask hole, due to the existence of pin hole effect, the actual figure obtained just has obvious broadening thus the physical property of the final nanostructured that we obtain of impact.In addition, stencilling art also exists in application process such as that mask hole is blocked, and stencil mask physical strength such as not easily to be broken at the problem, thus develops new stencil mask and remains one of important research direction in current micro-nano technology field.
Summary of the invention
In view of this, technical matters to be solved by this invention is to provide paraffin paper mask and preparation method thereof, when paraffin paper mask provided by the invention is applied to stencilling art, can significantly reduce halation effect.
The invention provides a kind of preparation method of paraffin paper mask, comprising:
To the coating sample exposure of polymethylmethacrylate, development and fixing, obtain stencil mask,
The weight-average molecular weight of described polymethylmethacrylate is 50000 ~ 950000;
The exposure dose of described exposure is 210 ~ 430 μ C/cm
2.
Preferably, the sample of described coating polymethylmethacrylate is prepared in accordance with the following methods:
Substrate applies polymethyl methacrylate solution, obtains the sample applying polymethylmethacrylate,
The solution of described polymethylmethacrylate is the organic solution of polymethylmethacrylate,
Described organic solvent is one or both in chloroform and methyl ether.
Preferably, in described polymethyl methacrylate solution, the mass percentage of polymethylmethacrylate is 1wt% ~ 9wt%.
Preferably, the mode of described coating is spin coating.
Preferably, the rotating speed of described spin coating is 2000 ~ 6000rpm.
Preferably, in the sample of described coating polymethylmethacrylate, the thickness of polymethylmethacrylate is 0.1 ~ 1.5 micron.
Preferably, described exposure is electron beam exposure, deep UV lithography, extreme ultraviolet exposure or X-ray exposure.
Preferably, the time of described development is 30 seconds ~ 120 seconds.
Preferably, the described fixing time is 30 seconds ~ 120 seconds.
The invention provides a kind of stencil mask, prepared by the preparation method of paraffin paper mask provided by the invention.
Compared with prior art, the invention provides a kind of preparation method of paraffin paper mask, is 210 ~ 430 μ C/cm by being the polymethylmethacrylate of 50000 ~ 950000 by weight-average molecular weight at exposure dose
2condition under expose, then fixing, development obtains paraffin paper mask, make the stencil mask prepared while disposal molding, this mask contains for the shaping thin layer containing hole of nano particle simultaneously and contains the larger supporting layer of cavity, and the cavity in supporting layer is positioned at the below in hole, and the cross-sectional area of cavity is greater than the cross-sectional area of hole, and then this mask and substrate can be combined closely, wherein, supporting layer containing cavity act as gap, micro-interval, and the thickness of this supporting layer is less than the thickness of whole paraffin paper mask, 1 micron can be low to moderate, for nano particle shaping time, can obviously reduce halation effect.
Accompanying drawing explanation
Fig. 1 is the structural representation of paraffin paper mask in different treatment steps;
Fig. 2 is the paraffin paper mask SEM figure dorsad that the embodiment of the present invention 1 prepares;
Fig. 3 is the SEM figure that the paraffin paper mask using the embodiment of the present invention 1 to prepare carries out the nano-pattern that nanometer paraffin paper printed deposit obtains;
Fig. 4 is the paraffin paper mask SEM figure dorsad that the embodiment of the present invention 2 prepares.
Embodiment
The invention provides a kind of preparation method of paraffin paper mask, comprising:
To the coating sample exposure of polymethylmethacrylate, development and fixing, obtain stencil mask,
The weight-average molecular weight of described polymethylmethacrylate is 50000 ~ 950000;
The exposure dose of described exposure is 210 ~ 430 μ C/cm
2.
According to the present invention, to the coating sample exposure of polymethylmethacrylate, development and fixing, obtain stencil mask;
Wherein, the weight-average molecular weight of described polymethylmethacrylate is preferably 50000 ~ 950000, and more preferably 100000 ~ 800000, most preferably be 450000 ~ 600000, most preferably be 495000 ~ 550000; In the sample of described coating polymethylmethacrylate, the thickness of polymethylmethacrylate is preferably 1 ~ 5 micron, is more preferably 1.2 ~ 2 microns.
Described exposure is preferably electron beam exposure, deep UV lithography, extreme ultraviolet exposure or X-ray exposure, is more preferably electron beam exposure; Described exposure dose is preferably 210 ~ 430 μ C/cm
2, be more preferably 250 ~ 380 μ C/cm
2, most preferably be 300 ~ 350 μ C/cm
2; When exposing for electron beam exposure, the accelerating potential of described electron beam is preferably 10KeV ~ 20KeV;
The sample of coating polymethylmethacrylate of the present invention is preferably prepared in accordance with the following methods:
Substrate applies polymethylmethacrylate (PMMA) solution, obtains the sample applying polymethylmethacrylate; Wherein, the kind of the present invention to backing material is not particularly limited, and well known to a person skilled in the art the backing material that can be applied to and prepare nano gap, and the present invention is preferably the compound substrate of silicon dioxide and silicon; The thickness of described substrate is preferably 100nm ~ 1 μm, is more preferably 200nm ~ 800nm, most preferably is 300nm ~ 500nm; The solution of described polymethylmethacrylate is preferably the organic solution of polymethylmethacrylate; Described organic solvent be preferably in chloroform and methyl ether one or both; In described polymethyl methacrylate solution, the mass percentage of polymethylmethacrylate is 1wt% ~ 9wt%, is more preferably 4wt% ~ 6wt%.
The mode of the present invention to coating is not particularly limited, coating method well known in the art, the present invention preferably adopts spin-coating method to be spin-coated on substrate by polymethyl methacrylate solution, wherein, the rotating speed of spin coating is preferably 2000 ~ 6000 revolutions per seconds, more preferably 2000 revolutions per seconds; The present invention also comprises dries the sample scribbling polymethylmethacrylate, and the temperature of wherein drying is preferably 170-220 DEG C, more preferably 180 DEG C, and the time of oven dry is preferably 1 ~ 5 minute, more preferably 4 minutes.
According to the present invention, in described development, development time is preferably 30 seconds ~ 120 seconds, is more preferably 60 seconds ~ 90 seconds; Described fixing in, fixing time is preferably 30 seconds ~ 120 seconds, is more preferably 60 seconds ~ 80 seconds.
In addition, in exposed, the restriction that the present invention is not special to the selection of exposure area, those skilled in the art can select exposure area according to required pattern according to the common practise of this area.
According to the present invention, the paraffin paper mask obtained after fixing and substrate can also depart from by the present invention, and the mode of disengaging be paraffin paper mask and substrate are departed from by being hydrolyzed, and described hydrolysis is carried out under alkaline environment, and preferably, the pH value of hydrolysis environment is preferably 11 ~ 14; The alkali of alkaline environment is provided to be NaOH or potassium hydroxide.
According to the present invention, after hydrolysis, the present invention also comprises and will be hydrolyzed the paraffin paper mask washed with de-ionized water obtained, the sodium hydroxide solution that removing mask surface is residual.
Present invention also offers paraffin paper mask prepared by a kind of method provided by the invention; Wherein, described stencil mask have simultaneously for nano particle shaping containing the layer of hole and the supporting layer for supporting the layer containing hole, containing cavity in this supporting layer, and the cavity in supporting layer is positioned at the below in hole, and the cross-sectional area of cavity horizontal direction is greater than the cross-sectional area in hole.When the stencil mask with this structure is for nano particle shaping, halation effect can not be produced; Concrete, the structural representation of this paraffin paper mask is shown in Fig. 1, and Fig. 1 is the structural representation of paraffin paper mask in different treatment steps; Concrete, in Fig. 1, a is the stencil mask obtained after developing fixing, and b is the paraffin paper mask departing from liner plate, and c is the patterning figure using stencil mask to carry out stencilling art.D is the sectional view of the paraffin paper mask described in a figure, as can be seen from figure d, paraffin paper mask of the present invention includes the supporting layer containing frustum cone structure for the shaping layer containing hole of nanoparticle and the below containing pore layer, and the surface area of the upper surface of round platform is greater than the sectional area in hole, the cross section of this frustum cone structure is trapezoidal, and it is to be noted, one containing the layer of hole and supporting layer, in the present invention by using polymethylmethacrylate disposal molding to realize, just in order to needing of describing is defined as two-layer.
The preparation method of paraffin paper mask provided by the invention is 210 ~ 430 μ C/cm by being the polymethylmethacrylate of 50000 ~ 950000 by weight-average molecular weight at exposure dose
2condition under expose, then fixing, development obtains paraffin paper mask, make the stencil mask prepared while disposal molding, this mask simultaneously containing for nano particle shaping containing the layer of hole and the supporting layer for supporting the layer containing hole, containing cavity in this supporting layer, and the cavity in supporting layer is positioned at the below in hole, and the cross-sectional area of cavity is greater than the cross-sectional area of hole, and then this mask and substrate can be combined closely, supporting layer containing cavity act as micro-interval region, the thickness of this supporting layer is less than the thickness of whole paraffin paper mask, 1 micron can be low to moderate, for nano particle shaping time, substantially halation effect can not be produced.
Technical scheme below in conjunction with the embodiment of the present invention is clearly and completely described, and obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
By Si and SiO
2(wherein, the crystal lattice orientation of Si sheet is 111, SiO to the compound substrate of composition
2the thickness of layer is 300 nanometers) cut into the fritter of 1cm × 1cm, by acetone, absolute ethyl alcohol, deionized water ultrasonic five minutes respectively, nitrogen dried up for subsequent use, obtains substrate.
It substrate is the chloroformic solution (mass percentage concentration of PMMA is for 6wt%) of the PMMA671.06 of 950000 with the speed spin coating weight-average molecular weight of 4000rmp, thermal station 180 DEG C of drying glues 4 minutes, obtain the sample that thickness is the coating polymethylmethacrylate of 1.2 microns.
The sample of PMMA spin coating is had to put into electron beam exposure apparatus (Raithe_Line), under the accelerating potential of 15KV, with 300 μ C/cm
2dosage, the minimum step of 25.6nm exposes the figure designed in advance, develops 90 seconds, fixing one minute, obtains the paraffin paper mask containing substrate; Now expose the PMMA photoetching offset plate figure that obtains for tangent plane be the shape shown in Fig. 1-d;
Paraffin paper mask containing substrate is immersed in the KOH solution of 1mol/L, 85 degrees Celsius are soaked 10 minutes, PMMA film with nanoaperture forms independently film from substrate surface disengaging, use the KOH solution of a large amount of washed with de-ionized water film surface remnants, obtain the paraffin paper mask departing from substrate.
By with scanning electron microscope to must with paraffin paper mask observe, the results are shown in Figure 2, Fig. 2 is the paraffin paper mask for preparing of the embodiment of the present invention 1 SEM figure dorsad, as can be seen from the figure, has individual bottom surface to be the cavity of ellipse below the slotted eye of paraffin paper mask.
The stencil mask obtained is applied to the shaping of nano particle, the results are shown in Figure 3, Fig. 3 is the SEM figure that the paraffin paper mask using the embodiment of the present invention 1 to prepare carries out the nanometer rods that nanometer paraffin paper printed deposit obtains, can take a fancy to from figure, the structure of the nanometer rods that nanometer mask prepared by the application of the invention embodiment prepares almost does not have obvious size expansion, much smaller than the size of surrounding housing.
Embodiment 2
By Si and SiO
2(wherein, the crystal lattice orientation of Si sheet is 111, SiO to the compound substrate of composition
2the thickness of layer is 300 nanometers) cut into the fritter of 1cm × 1cm, by acetone, absolute ethyl alcohol, deionized water ultrasonic five minutes respectively, nitrogen dried up for subsequent use, obtains substrate.
It substrate is the chloroformic solution (mass percentage concentration of PMMA is for 6wt%) of the PMMA671.06 of 950000 with the speed spin coating weight-average molecular weight of 4000rmp, thermal station 180 DEG C of drying glues 4 minutes, obtain the sample that thickness is the coating polymethylmethacrylate of 1.2 microns.
The sample of PMMA spin coating is had to put into electron beam exposure apparatus (Raithe_Line), under the accelerating potential of 15KV, with 430 μ C/cm
2dosage, the minimum step of 25.6nm exposes the figure designed in advance, develops 90 seconds, fixing one minute, obtains the paraffin paper mask containing substrate; Now expose the PMMA photoetching offset plate figure that obtains for tangent plane be the shape shown in Fig. 1-d;
Paraffin paper mask containing substrate is immersed in the KOH solution of 1mol/L, 85 degrees Celsius are soaked 10 minutes, PMMA film with nanoaperture forms independently film from substrate surface disengaging, use the KOH solution of a large amount of washed with de-ionized water film surface remnants, obtain the paraffin paper mask departing from substrate.
By with scanning electron microscope to must with paraffin paper mask observe, the results are shown in Figure 4, Fig. 4 is the paraffin paper mask for preparing of the embodiment of the present invention 2 SEM figure dorsad, as can be seen from the figure, has individual bottom surface to be the cavity of circle below the slotted eye of paraffin paper mask.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
Claims (10)
1. a preparation method for paraffin paper mask, comprising:
To the coating sample exposure of polymethylmethacrylate, development and fixing, obtain stencil mask,
The weight-average molecular weight of described polymethylmethacrylate is 50000 ~ 950000;
The exposure dose of described exposure is 210 ~ 430 μ C/cm
2.
2. preparation method according to claim 1, is characterized in that, the sample of described coating polymethylmethacrylate is prepared in accordance with the following methods:
Substrate applies polymethyl methacrylate solution, obtains the sample applying polymethylmethacrylate,
The solution of described polymethylmethacrylate is the organic solution of polymethylmethacrylate,
Described organic solvent is one or both in chloroform and methyl ether.
3. preparation method according to claim 2, is characterized in that, in described polymethyl methacrylate solution, the mass percentage of polymethylmethacrylate is 1wt% ~ 9wt%.
4. preparation method according to claim 2, is characterized in that, the mode of described coating is spin coating.
5. preparation method according to claim 4, is characterized in that, the rotating speed of described spin coating is 2000 ~ 6000rpm.
6. preparation method according to claim 1, is characterized in that, in the sample of described coating polymethylmethacrylate, the thickness of polymethylmethacrylate is 0.1 ~ 1.5 micron.
7. preparation method according to claim 1, is characterized in that, described exposure is electron beam exposure.
8. preparation method according to claim 1, is characterized in that, the time of described development is 30 seconds ~ 120 seconds.
9. preparation method according to claim 1, is characterized in that, the described fixing time is 30 seconds ~ 120 seconds.
10. a stencil mask, is prepared by the preparation method described in claim 1 ~ 9 any one.
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| CN201510528675.8A CN105045036B (en) | 2015-08-24 | 2015-08-24 | Wax paper mask and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101025460A (en) * | 2006-02-22 | 2007-08-29 | 中国科学院长春光学精密机械与物理研究所 | Micro optical component positioning structure and micro channel module preparation using micro channel array |
| CN101086966A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院微电子研究所 | Preparation method of nano-scale coulomb island structure |
| CN101382733A (en) * | 2008-09-27 | 2009-03-11 | 中国科学院微电子研究所 | Method for manufacturing nanoscale pattern |
| CN101813884A (en) * | 2010-03-19 | 2010-08-25 | 中国科学技术大学 | Method for preparing nano-structured matrix on surface of uneven substrate |
| CN101872120A (en) * | 2010-07-01 | 2010-10-27 | 北京大学 | Method for preparing patterned graphene |
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2015
- 2015-08-24 CN CN201510528675.8A patent/CN105045036B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101025460A (en) * | 2006-02-22 | 2007-08-29 | 中国科学院长春光学精密机械与物理研究所 | Micro optical component positioning structure and micro channel module preparation using micro channel array |
| CN101086966A (en) * | 2006-06-07 | 2007-12-12 | 中国科学院微电子研究所 | Preparation method of nano-scale coulomb island structure |
| CN101382733A (en) * | 2008-09-27 | 2009-03-11 | 中国科学院微电子研究所 | Method for manufacturing nanoscale pattern |
| CN101813884A (en) * | 2010-03-19 | 2010-08-25 | 中国科学技术大学 | Method for preparing nano-structured matrix on surface of uneven substrate |
| CN101872120A (en) * | 2010-07-01 | 2010-10-27 | 北京大学 | Method for preparing patterned graphene |
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