CN109173039A - The preparation method of inverted funnel shape silicon substrate solid array of microneedles - Google Patents
The preparation method of inverted funnel shape silicon substrate solid array of microneedles Download PDFInfo
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- CN109173039A CN109173039A CN201810941632.6A CN201810941632A CN109173039A CN 109173039 A CN109173039 A CN 109173039A CN 201810941632 A CN201810941632 A CN 201810941632A CN 109173039 A CN109173039 A CN 109173039A
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- etching
- monocrystalline silicon
- silicon
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- microneedles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M37/00—Other apparatus for introducing media into the body; Percutany, i.e. introducing medicines into the body by diffusion through the skin
- A61M37/0015—Other apparatus for introducing media into the body; Percutany, i.e. introducing medicines into the body by diffusion through the skin by using microneedles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M37/00—Other apparatus for introducing media into the body; Percutany, i.e. introducing medicines into the body by diffusion through the skin
- A61M37/0015—Other apparatus for introducing media into the body; Percutany, i.e. introducing medicines into the body by diffusion through the skin by using microneedles
- A61M2037/0053—Methods for producing microneedles
Abstract
The present invention proposes a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles, comprising the following steps: 1) front side silicon nitride silicon protective film and reverse side silicon nitride protective film are deposited on monocrystalline silicon piece；2) spin coating photoresist carries out photoetching on front side silicon nitride silicon protective film, and the circle that the photoresist after photoetching forms array-like blocks glue film；3) dry etching falls the front side silicon nitride silicon protective film for being exposed to and blocking outside glue film, exposes monocrystalline silicon piece；4) inductively coupled plasma etching system is utilized, using deep silicon etching Bosch technique, anisotropic etching is carried out to monocrystalline silicon piece, the cylindrical body of array-like is etched on monocrystalline silicon piece；5) it removes on monocrystalline silicon piece and blocks glue film；6) isotropism wet etching is carried out to monocrystalline silicon piece using acid etching solution, obtains microneedle array.The solid array of microneedles that high-aspect-ratio, tip diameter and the controllable inverted funnel shape structure of length can be achieved in the present invention is processed.
Description
Technical field
The present invention relates to semiconductor silicon material surface micro-fabrication and manufacturing technology field, specifically a kind of inverted funnel shape silicon substrate
The preparation method of solid array of microneedles.
Background technique
What existing silicon substrate solid array of microneedles wet chemical hair corrosion was mainly combined using anisotropy and isotropism
Method can by parameters such as etching liquid concentration, etching temperature, etch periods during selective etching liquid and accurate control corrosion rate
To prepare solid microneedles three-dimensional mould.Monarch Xiao Li et al. is prepared for one using ultraviolet photolithographic and KOH isotropic etching technology
Determine height silicon materials microneedle array (a kind of production method of polymer solid microneedles, MEMS device and technology, 2009,46
(12)744-749)；Pass through SiO2As sacrificial layer, Xu Qiangang et al. carries out silica-base material using acid etching solution each to same
Property corrosion be prepared for depth and the smaller X-Y scheme of width (a kind of wet sculpture in human hair etching technique of silicon substrate isotropism,
CN102931070A).But influenced by etching crystal orientation, etch rate, this method is merely able to process certain depth-to-width ratio micropin
Point has certain limitation；In addition, the long-time alternating corrosion of highly basic, strong acid has higher requirements to mask.Based on side wall protection
Etching and passivation are divided into two steps using low temperature ICP dry etching technology, utilize SF by principle6As etching gas, C4F8As
Polymer generates gas, etching with passivation alternately, by this periodic manner, can Equilibrium ablation and passivation well,
Anisotropic etch is preferably controlled, can get the structure of very high-aspect-ratio (> 20: 1), side wall is close to 90 degree, but the method is only
Vertical sidewall can be obtained, skew wall face or arcuate structure can not be processed.
Summary of the invention
The present invention proposes a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles, solves and prepares in the prior art
The problem of depth-to-width ratio existing for microneedle array is limited or can not process skew wall face or arcuate structure.
The technical scheme of the present invention is realized as follows:
A kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles, comprising the following steps:
1) (100) crystal face, twin polishing monocrystalline silicon piece are chosen, in the front deposition front side silicon nitride silicon protection of monocrystalline silicon piece
Film deposits reverse side silicon nitride protective film in the reverse side of monocrystalline silicon piece；
2) the spin coating photoresist on front side silicon nitride silicon protective film, using photoetching process by mask plate pattern transfer to photoresist
On, the figure of mask plate is the circular spot of array-like, and the circle that the photoresist after photoetching forms array-like blocks glue film；
3) dry etching falls the front side silicon nitride silicon protective film for being exposed to and blocking outside glue film, exposes monocrystalline silicon piece；
4) inductively coupled plasma etching system is utilized, using deep silicon etching Bosch technique, the list that step 3 is exposed
Crystal silicon chip carries out anisotropic etching, and the cylindrical body of array-like is etched on monocrystalline silicon piece；
5) it removes on monocrystalline silicon piece and blocks glue film；
6) isotropism wet etching is carried out to the monocrystalline silicon piece after step 5 using acid etching solution, obtains microneedle array.
Further, in the step 1, monocrystalline silicon piece is N-type, and electrical resistivity range is 1-10 Ω cm, with a thickness of 700 ±
10μm；
Front side silicon nitride silicon protective film and reverse side silicon nitride protective film are all 500nm thickness, using low-pressure chemical vapor deposition work
Skill is deposited on monocrystalline silicon piece.
Further, in the step 2, the revolving speed of spin coating photoresist is 2500r/min, time 40s, photoresist film thickness
10.6 microns；Then, by monocrystalline silicon piece in 95 DEG C of environment front baking 10min, mask artwork is carried out after monocrystalline silicon piece natural cooling
Shape photoetching exposes 130s, dosage 1539mJ/cm2, then develop in the NMD-W developer solution that concentration is 2.38% 10min,
1min, then the post bake 15min in 100 DEG C of environment are rinsed with deionized water, in mask plate pattern transfer to photoresist；
The diameter of the circular spot of the figure of mask plate is 200 μm, and the center of circle spacing of adjacent circular spot is 500 μm.
Further, in the step 3, dry etching, power 100W, CHF are carried out using reactive ion etching machine3Gas
Flow is 100sccm, vacuum degree 2.5Pa, etch period 108min.
Further, in the step 4, inductively coupled plasma etching system power is 1000W, when etching is with passivation
Between 7s/4s be one circulation, etch rate be 0.42 μm/circulation, monocrystalline silicon piece and block glue film it is anti-etching than be 42:1.
Further, in the step 5, the monocrystalline silicon piece acetone soak and ultrasound 10min that step 4 is obtained, then use
Alcohol impregnates and ultrasound 10min, and deionized water rinses 5min, is dried with nitrogen, then the dry 10min in 100 DEG C of environment.
Further, in the step 6, acid etching solution is 70% HNO that volume ratio is 8:1:13, 49% HF and
The mixed liquor of 100% HAc.
Further, in the step 6, wet etching carries out in mixture of ice and water slot, and uses magnetic agitation, corrosion
Time is 20min.
The invention has the benefit that
The present invention passes through inductively coupled plasma body (ICP) dry etching technology and acids to the isotropic etch phase of silicon
In conjunction with, it can be achieved that the solid array of microneedles of high-aspect-ratio, tip diameter and the controllable inverted funnel shape structure of length is processed, obtain
Microneedle array is used for the mold of percutaneous drug delivery micropin；Inverted funnel shape structure can effectively control administration micropin insertion skin depth；
Tip diameter less than 30 μm demoulds when can not only reduce the resistance of administration micropin insertion skin, and replicate administration micropin
More easily；Prepared by the method silicon mould duplication can dissolve or micropin is administered in degradable high molecular material, is to realize greatly
The effective way of molecule cutaneous penetration.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the structural schematic diagram obtained after step 1 deposits；
Fig. 2 is the overlooking structure diagram of Fig. 1；
Fig. 3 is the structural schematic diagram after spin coating photoresist；
Fig. 4 is the overlooking structure diagram of Fig. 3；
Fig. 5 is the structural schematic diagram after photoetching；
Fig. 6 is the overlooking structure diagram of Fig. 5；
Fig. 7 is the structural schematic diagram after step 3 etching；
Fig. 8 is the overlooking structure diagram of Fig. 7；
Fig. 9 is the structural schematic diagram after step 4 etching；
Figure 10 is the overlooking structure diagram of Fig. 9；
Figure 11 is the structural schematic diagram after step 5 is removed photoresist；
Figure 12 is the overlooking structure diagram of Figure 11；
Figure 13 is the structural schematic diagram after step 6 wet etching；
Figure 14 is the overlooking structure diagram of Figure 13；
Figure 15 is the metallographic microscope A of inverted funnel shape silicon substrate solid array of microneedles prepared by the present invention；
Figure 16 is the metallographic microscope B of inverted funnel shape silicon substrate solid array of microneedles prepared by the present invention.
Wherein:
1, monocrystalline silicon piece；2, front side silicon nitride silicon protective film；3, reverse side silicon nitride protective film；4, photoresist；5, glue film is blocked；
6, cylindrical body.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As illustrated in figs. 1-16, the preparation method of the inverted funnel shape silicon substrate solid array of microneedles in the present embodiment, including it is following
Step:
1) (100) crystal face, twin polishing monocrystalline silicon piece 1 are chosen, in the present embodiment, monocrystalline silicon piece 1 is N-type, resistivity 5
Ω cm can choose electrical resistivity range in practical application and be ok in 1-10 Ω cm, with a thickness of 700 ± 10 μm；In monocrystalline
The front deposition front side silicon nitride silicon protective film 2 of silicon wafer 1 deposits reverse side silicon nitride protective film 3 in the reverse side of monocrystalline silicon piece 1；Front
Silicon nitride protective film 2 and reverse side silicon nitride protective film 3 are all thick for 500nm, heavy using low-pressure chemical vapor deposition (LPCVD) technique
Product is on monocrystalline silicon piece 1.
2) the spin coating photoresist 4 on front side silicon nitride silicon protective film 2, using photoetching process by mask plate pattern transfer to photoetching
On glue 4, the figure of mask plate is the circular spot of array-like, and the circle that the photoresist 4 after photoetching forms array-like blocks glue film
5；In the present embodiment, using AZ9260 type photoresist 4, the revolving speed of spin coating photoresist 4 is 2500r/min, time 40s, photoresist
10.6 microns of film thickness；Then, by monocrystalline silicon piece 1 in 95 DEG C of environment front baking 10min, it is laggard to 1 natural cooling of monocrystalline silicon piece
Row mask graph photoetching exposes 130s, dosage 1539mJ/cm2, then shown in the NMD-W developer solution that concentration is 2.38%
Shadow 10min rinses 1min, then the post bake 15min in 100 DEG C of environment with deionized water, mask plate pattern transfer to photoresist 4
On；The diameter of the circular spot of the figure of mask plate is 200 μm, and the center of circle spacing of adjacent circular spot is 500 μm.
3) dry etching falls the front side silicon nitride silicon protective film 2 for being exposed to and blocking outside glue film 5, exposes monocrystalline silicon piece 1；This implementation
In example, dry etching, power 100W, CHF are carried out using reactive ion etching machine3Throughput is 100sccm, and vacuum degree is
2.5Pa, etch period 108min.
4) inductively coupled plasma etching system is utilized, using deep silicon etching Bosch technique, the list that step 3 is exposed
Crystal silicon chip 1 carries out anisotropic etching, and the cylindrical body 6 of array-like is etched on monocrystalline silicon piece 1；In the present embodiment, inductance coupling
Conjunction plasma etching system power be 1000W, etching with passivation time 7s/4s be one circulation, etch rate be 0.42 μm/
Circulation, monocrystalline silicon piece 1 and block glue film 5 it is anti-etching than be 42:1；6 height of cylindrical body is 162 μm after etching 380 circulations, directly
204 μm of diameter, side wall and 1 angle of monocrystalline silicon piece are 90 degree.
5) it removes on monocrystalline silicon piece 1 and blocks glue film 5；In the present embodiment, the monocrystalline silicon piece 1 that step 4 obtains is soaked with acetone
Simultaneously ultrasound 10min is steeped, then impregnates simultaneously ultrasound 10min with alcohol, deionized water is rinsed 5min, is dried with nitrogen, then in 100 DEG C of environment
Middle dry 10min.
6) isotropism wet etching is carried out to the monocrystalline silicon piece 1 after step 5 using acid etching solution, obtains micropin battle array
Column.In the present embodiment, acid etching solution be volume ratio be 8:1:1 70% HNO3,49% HF and 100% HAc it is mixed
Close liquid, abbreviation HNA.In order to guarantee the consistency of corrosion rate, wet etching carries out in mixture of ice and water slot, and uses magnetic force
Stirring, etching time 20min；About 90 μm of radial erosion depth after corrosion 20min, depth direction corrodes about 86 μm, silicon nitride
Average corrosion rate in HNA is 9nm/min.
The metallographic microscope of inverted funnel shape silicon substrate solid array of microneedles manufactured in the present embodiment passes through inductance referring to Figure 15 and Figure 16
Coupled plasma (ICP) dry etching technology and acids is combined to the isotropic etch of silicon, it can be achieved that high-aspect-ratio, needle
Sharp diameter and the solid array of microneedles of the controllable inverted funnel shape structure of length are processed, and obtained microneedle array is micro- for percutaneous drug delivery
The mold of needle；Inverted funnel shape structure can effectively control administration micropin insertion skin depth；Tip diameter less than 30 μm, not only
Demoulding is easier when can reduce the resistance of administration micropin insertion skin, and replicate administration micropin.
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
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (8)
1. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles, which comprises the following steps:
1) (100) crystal face, twin polishing monocrystalline silicon piece are chosen, deposits front side silicon nitride silicon protective film in the front of monocrystalline silicon piece,
The reverse side of monocrystalline silicon piece deposits reverse side silicon nitride protective film；
2) the spin coating photoresist on front side silicon nitride silicon protective film, using photoetching process by mask plate pattern transfer to photoresist,
The figure of mask plate is the circular spot of array-like, and the circle that the photoresist after photoetching forms array-like blocks glue film；
3) dry etching falls the front side silicon nitride silicon protective film for being exposed to and blocking outside glue film, exposes monocrystalline silicon piece；
4) inductively coupled plasma etching system is utilized, using deep silicon etching Bosch technique, the monocrystalline silicon that step 3 is exposed
Piece carries out anisotropic etching, and the cylindrical body of array-like is etched on monocrystalline silicon piece；
5) it removes on monocrystalline silicon piece and blocks glue film；
6) isotropism wet etching is carried out to the monocrystalline silicon piece after step 5 using acid etching solution, obtains microneedle array.
2. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as described in claim 1, which is characterized in that described
In step 1, monocrystalline silicon piece is N-type, and electrical resistivity range is 1-10 Ω cm, with a thickness of 700 ± 10 μm；
Front side silicon nitride silicon protective film and reverse side silicon nitride protective film are all 500nm thickness, heavy using low-pressure chemical vapor deposition process
Product is on monocrystalline silicon piece.
3. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 2, which is characterized in that described
In step 2, the revolving speed of spin coating photoresist is 2500r/min, time 40s, 10.6 microns of photoresist film thickness；Then, by monocrystalline
Silicon wafer front baking 10min in 95 DEG C of environment carries out mask graph photoetching after monocrystalline silicon piece natural cooling, exposes 130s, dosage
For 1539mJ/cm2, then develop in the NMD-W developer solution that concentration is 2.38% 10min, 1min is rinsed with deionized water, then
The post bake 15min in 100 DEG C of environment, in mask plate pattern transfer to photoresist；
The diameter of the circular spot of the figure of mask plate is 200 μm, and the center of circle spacing of adjacent circular spot is 500 μm.
4. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 3, which is characterized in that described
In step 3, dry etching, power 100W, CHF are carried out using reactive ion etching machine3Throughput is 100sccm, vacuum degree
For 2.5Pa, etch period 108min.
5. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 4, which is characterized in that described
In step 4, inductively coupled plasma etching system power is 1000W, and etching is a circulation with passivation time 7s/4s, is carved
Lose rate be 0.42 μm/circulation, monocrystalline silicon piece and block glue film it is anti-etching than be 42:1.
6. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 5, which is characterized in that described
In step 5, the monocrystalline silicon piece acetone soak and ultrasound 10min that step 4 is obtained, then simultaneously ultrasound 10min is impregnated with alcohol, it goes
Ionized water rinses 5min, is dried with nitrogen, then the dry 10min in 100 DEG C of environment.
7. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 6, which is characterized in that described
In step 6, acid etching solution is 70% HNO that volume ratio is 8:1:13, 49% HF and 100% HAc mixed liquor.
8. a kind of preparation method of inverted funnel shape silicon substrate solid array of microneedles as claimed in claim 7, which is characterized in that described
In step 6, wet etching carries out in mixture of ice and water slot, and uses magnetic agitation, etching time 20min.
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| CN109893753A (en) * | 2019-04-08 | 2019-06-18 | 苏州泽矽能电子科技有限公司 | A kind of monocrystalline silicon high throughput microneedle configuration |
| CN110002393A (en) * | 2019-04-04 | 2019-07-12 | 中国科学院微电子研究所 | The preparation method of method for selective etching and nanometer pinpoint structure |
| CN110127596A (en) * | 2019-04-15 | 2019-08-16 | 广东工业大学 | A kind of high-aspect-ratio inverted cone-shaped structure manufacturing method |
| CN111675190A (en) * | 2020-06-18 | 2020-09-18 | 苏州恒之清生物科技有限公司 | Preparation method of miniature solid silicon needle |
| CN111812941A (en) * | 2019-04-11 | 2020-10-23 | 中国科学院金属研究所 | High-precision silicon physical mask and manufacturing method thereof |
| CN111943130A (en) * | 2020-07-10 | 2020-11-17 | 深圳市安瑞生物科技有限公司 | Nano needle array and preparation method and application thereof |
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| CN110002393A (en) * | 2019-04-04 | 2019-07-12 | 中国科学院微电子研究所 | The preparation method of method for selective etching and nanometer pinpoint structure |
| CN109893753A (en) * | 2019-04-08 | 2019-06-18 | 苏州泽矽能电子科技有限公司 | A kind of monocrystalline silicon high throughput microneedle configuration |
| CN111812941A (en) * | 2019-04-11 | 2020-10-23 | 中国科学院金属研究所 | High-precision silicon physical mask and manufacturing method thereof |
| CN111812941B (en) * | 2019-04-11 | 2023-10-10 | 中国科学院金属研究所 | High-precision silicon physical mask and manufacturing method thereof |
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| CN111675190A (en) * | 2020-06-18 | 2020-09-18 | 苏州恒之清生物科技有限公司 | Preparation method of miniature solid silicon needle |
| CN111943130A (en) * | 2020-07-10 | 2020-11-17 | 深圳市安瑞生物科技有限公司 | Nano needle array and preparation method and application thereof |
| CN111943130B (en) * | 2020-07-10 | 2021-06-29 | 深圳市安瑞生物科技有限公司 | Nano needle array and preparation method and application thereof |
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