CN101342404A - Method for manufacturing different-plane metal hollow fine needle for transdermal drug administration - Google Patents
Method for manufacturing different-plane metal hollow fine needle for transdermal drug administration Download PDFInfo
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- CN101342404A CN101342404A CN 200810042163 CN200810042163A CN101342404A CN 101342404 A CN101342404 A CN 101342404A CN 200810042163 CN200810042163 CN 200810042163 CN 200810042163 A CN200810042163 A CN 200810042163A CN 101342404 A CN101342404 A CN 101342404A
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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
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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
- A61M2037/0053—Methods for producing microneedles
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Abstract
The present invention relates to a fabrication method of a hetero-planar metallic hollow microneedle used for transdermal delivery, which belongs to the technical field of medical apparatuses. Firstly, photoresist is spincoated on a silicon oxide substrate, a silicon oxide window is exposed after exposure and development, and silicon oxide is etched; secondly, with the silicon oxide as a mask, silicon is etched, so that a reverse rectangular pyramid pattern is formed; thirdly, a metallic conductive layer is spluttered, and a metal layer is then plated; fourthly, the plated bottom of the reverse metallic rectangular pyramid is removed, and a microchannel is cut; and finally, the silicon is removed, and the hetero-planar metallic hollow microneedle is produced. Compared with the prior art, the present invention ensures that the hetero-planar metallic microneedle possesses a microchannel, moreover, the fabrication technique is simple, and the cost is low. The microneedle can easily pierce the skin and continuously deliver medicine.
Description
Technical field
The present invention relates to a kind of metal hollow fine needle manufacture method of medical equipment technical field, specifically, what relate to is a kind of different-plane metal hollow fine needle manufacture method that is used for transdermal administration.
Background technology
The novel medicine-feeding technology of a class occurring at present is transdermal administration.Transdermal administration is in the skin surface administration, makes medicine to pass through each layer of skin near constant speed, absorbs through blood capillary to enter body circulation generation whole body or local therapeutic effects.The micropin that micro-electromechanical technology (MEMS) is made obtains extensive concern in the transdermal administration field.Human body skin is made up of horny layer (10～15 micron thickness), active epidermal area (50～100 micron thickness) and skin corium.Horny layer is made up of the horn cell of densification, is the major obstacle that the medicine percutaneous is carried.Be epidermal area below the horny layer, contain competent cell and a spot of nervous tissue, but do not have blood vessel.Being skin corium below the epidermal area, is the key component of skin, contains a large amount of living cells, nervous tissue and vascular tissue.MEMS micropin size is at micron order, do not contact with nerve after therefore thrusting skin, avoided patient is caused pain.In addition, the MEMS micropin has caused real physical channel at skin, so medicine can be easy to pass the horny layer intravasation.The MEMS microneedle configuration is similar to the syringe needle of conventional syringe, and needle point is symmetrical taper shape or asymmetric beveled, and structure can be divided into hollow and solid microneedles internally, and the tip end of empty micropin has cavity to be attached thereto, and solid microneedles does not have cavity; Can be divided into isoplanar micropin (in-plane) and different plane micropin (out-of-plane) from processing technology, the surface that the axle of isoplanar micropin or cavity are parallel to substrate, the axle of different plane micropin or cavity are perpendicular to the surface of substrate.
The various materials that are used for the micropin making at present mainly comprise silicon, metal and PMMA polymer.The excellent performance of silicon materials, be convenient to integrated, cost is low, the processing technology technology maturation.But because easy brittle failure of silicon and its bio-compatibility problem,, need modify as splash-proofing sputtering metal on its surface or be coated with performance and the bio-compatibility that improves the easy brittle failure of silicon with polymer so the silicon micropin can not be directly used in human body therapy.Polymer such as PDMS etc. have fabulous bio-compatibility, can be used as the material of making micropin, but a major defect of polymer micro needle are that mechanical performance is relatively poor, loses efficacy easily when thrusting skin.Metal is hard to be difficult for broken crisply, and metal such as titanium, rustless steel etc. are biocompatible materialses.Description to metal micro-needle mostly is the plane micropin, the document of the especially different plane hollow microneedle of rare different plane micropin.
Find through literature search prior art, " A tapered hollow metallic microneedle arrayusing backside exposure of SU-8 " (using taper hollow metal microneedle array of backside exposure SU-8) that Kabseog Kim etc. deliver on " JOURNAL OFMICROMECHANICS AND MICROENGINEERING " (micromechanics and micro engineering newspaper) (2004 the 14th phase 597 pages---603 pages), propose in this article to adopt backside exposure SU-8 to make taper hollow metal micropin, method is: (1) is from substrate of glass backside exposure ground floor SU-8 glue; (2) on the ground floor SU-8 glue that has exposed, prepare second layer SU-8 glue; (3) by substrate of glass and the ground floor SU-8 glue that exposed, exposure second layer SU-8 glue forms taper SU-8 structure; (4) sputter Cr/Cu on taper SU-8 structure; (5) plated metal nickel; (6) utilize SU-8 glue complanation total; (7) mechanical grinding SU-8 leaves the micropin top; (8) the SU-8 glue of removing complanation also separates the micropin layer from substrate of glass; (9) remove SU-8.Though what the document was made is the taper micropin, the angle that tilts has only 3.08 degree, almost is equal to the cylinder micropin, so be difficult to thrust skin; In addition, the technology of formation SU-8 glue pyramidal structure is also complicated.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of different-plane metal hollow fine needle manufacture method that is used for transdermal administration is provided, make the different-plane metal micropin have fluid channel, and processing technology is simple, cost is low; Micropin thrusts skin easily, has realized successive administration.
The present invention is achieved by the following technical solutions, and the present invention is spin coating photoresist on the silicon oxide substrate at first, exposes the silicon dioxide window, etching silicon dioxide through behind the exposure imaging; Secondly, form the figure of falling the rectangular pyramid with silicon dioxide for mask etching silicon; Follow splash-proofing sputtering metal conductive layer, electroplated metal layer then; Remove the electroplated metal bottom of falling the rectangular pyramid again, leave fluid channel; Remove silicon at last, obtain different-plane metal hollow fine needle.
Fluid channel is left in the described removal electroplated metal bottom of falling the rectangular pyramid, is meant: utilize excess silicon as mask, adopt metal etch liquid to remove the exposed part of etching micropin, leave fluid channel; Perhaps adopt the mechanical grinding finishing method to remove material, the fluid channel of leaving from the back side.
Described substrate is two oxidized silicon chips of throwing of (100) face.
The metal of described electroplated metal layer is meant metallic nickel, rustless steel, gold, titanium.
The thickness of described electroplated metal layer is meant 5-100 μ m.
The described rectangular pyramid that etches down is meant to etch the Si silicon of falling the rectangular pyramid groove that the degree of depth is 200-500 μ m.
Described different-plane metal hollow fine needle is meant the rectangular pyramid metal pin of hollow.
The material of different-plane metal hollow fine needle of the present invention is a metal, has good mechanical property, is easy to thrust skin, compared with prior art, has the following advantages: made the different plane of a kind of metal micropin, made the number of micropin increase greatly; Make a kind of empty micropin, realized successive administration; The angle of inclination of micropin is bigger, thrusts skin easily; The technology of micropin is simple, has reduced cost.
Description of drawings
Fig. 1 is a different-plane metal hollow fine needle processing technology flow chart;
Wherein: 1-1 is that two oxidized silicon chips of throwing are prepared; 1-2 is the spin coating photoresist; 1-3 is exposure imaging and etches SiO
2Window; 1-4 is the etch silicon V-shaped groove; 1-5 is for removing SiO
2And sputter Cu/Cr; 1-6 forms micropin for the plated metal metal.
Fig. 2 is single different-plane metal hollow fine needle axonometric chart;
Wherein: 2-1 is the micropin top side view, and 2-2 is the micropin posterior view.
Fig. 3 is the different-plane metal hollow fine needle array of figure.
The specific embodiment
Below in conjunction with accompanying drawing embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
As shown in Figure 1, provided the implementation process of the different-plane metal hollow fine needle preparation method embodiment that is used for transdermal administration, specifically described as follows.
Embodiment 1:
1, substrate is prepared.Prepare two oxidized silicon chip, thickness 500 μ m, wherein SiO of throwing of a slice (100) face
2About 2～3 μ m of thickness.
2, front whirl coating.The baking substrate is 2～3 hours under 180 ℃ of conditions, positive-glue removing 5 μ m.
3, photoetching development.Utilize a mask plate of having carried out targeted graphical, expose under UV, leaving the length of side after the development is 400 μ m square photoresist windows.
4, etching SiO
2Back side whirl coating protection, the baking sheet is 1 hour under 135 ℃ of conditions, and purpose is that photoresist is not come off in BHF solution.Utilize positive glue as mask, adopt BHF etching liquid (prescription: HF: H
2O: NH
4F=28ml: 170ml: 113g) etching SiO
2, leaving width is 400 μ m square SiO
2Window.
5, remove photoresist.Ultrasonic cleaning is 5 minutes in acetone, removes the photoresist of making mask, because photoresist can be dissolved in down the aqueous slkali in step, exposes SiO
2
6, etching Si.Utilize SiO
2As mask, adopt KOH solution (prescription: KOH: H
2O=44g: 100ml) etch the Si silicon of falling the rectangular pyramid groove that the degree of depth is about 330 μ m.
7, adopt the BHF etching liquid to remove SiO
2, at the positive sputter Cu/Cr (1400 of substrate
/ 100
) as conductive layer.
8, electronickelling thickness is 50 μ m, forms the different-plane metal micropin, and the micropin that form this moment is the hollow micropin.
9, back-etching Si.Adopt KOH solution removal back portion Si, until exposing metal micro-needle height 60 μ m.
10, utilize residue Si as mask, adopt the nickel etching liquid to remove the exposed part of etching micropin.Because micropin is a hollow, behind the micropin top that etches away about 60 μ m height, just leave the fluid channel of about 10 μ m.
11, adopt KOH solution removal residue Si, discharge different-plane metal hollow fine needle.
Embodiment 2:
1, substrate is prepared.Prepare two oxidized silicon chip, thickness 500 μ m, wherein SiO of throwing of a slice (100) face
2About 2～3 μ m of thickness.
2, front whirl coating.The baking substrate is 2～3 hours under 180 ℃ of conditions, positive-glue removing 5 μ m.
3, photoetching development.Utilize a mask plate of having carried out targeted graphical, expose under UV, leaving the length of side after the development is the square photoresist window of 400 μ m.
4, etching SiO
2Back side whirl coating protection, the baking sheet is 1 hour under 135 ℃ of conditions, and purpose is that photoresist is not come off in BHF solution.Utilize positive glue as mask, adopt BHF etching liquid (prescription: HF: H
2O: NH
4F=28ml: 170ml: 113g) etching SiO
2, leaving width is 400 μ m square SiO
2Window.
5, remove photoresist.Ultrasonic cleaning is 5 minutes in acetone, removes the photoresist of making mask, because photoresist can be dissolved in down the aqueous slkali in step.
6, etching Si.Utilize SiO
2As mask, adopt KOH solution (prescription: KOH: H
2O=44g: 100ml) etch the Si silicon of falling the rectangular pyramid groove that the degree of depth is 330 μ m.
7, adopt the BHF etching liquid to remove SiO
2, at the positive sputter Cu/Cr (1400 of substrate
/ 100
).
8, electrogilding thickness is 5 μ m, forms the different-plane metal micropin, and the micropin that form this moment is the hollow micropin.
9, back-etching Si.Adopting KOH solution removal back portion Si thickness is 20 μ m, exposes the metal micro-needle top.
10, adopt mechanical grinding finishing method (CMP) to remove material from the back side, thickness is 20 μ m, because micropin is a hollow, behind the micropin top that polishes off about 20 μ m height, leaves fluid channel.
11, adopt KOH solution removal residue Si, discharge different-plane metal hollow fine needle.
Embodiment 3:
1, substrate is prepared.Prepare two oxidized silicon chip, thickness 500 μ m, wherein SiO of throwing of a slice (100) face
2About 2～3 μ m of thickness.
2, front whirl coating.The baking substrate is 2～3 hours under 180 ℃ of conditions, positive-glue removing 5 μ m.
3, photoetching development.Utilize a mask plate of having carried out targeted graphical, expose under UV, leaving the length of side after the development is the square photoresist window of 400 μ m.
4, etching SiO
2Back side whirl coating protection, the baking sheet is 1 hour under 135 ℃ of conditions, and purpose is that photoresist is not come off in BHF solution.Utilize positive glue as mask, adopt BHF etching liquid (prescription: HF: H
2O: NH
4F=28ml: 170ml: 113g) etching SiO
2, leaving width is 400 μ m square SiO
2Window.
5, remove photoresist.Ultrasonic cleaning is 5 minutes in acetone, removes the photoresist of making mask, because photoresist can be dissolved in down the aqueous slkali in step.
6, etching Si.Utilize SiO
2As mask, adopt KOH solution (prescription: KOH: H
2O=44g: 100ml) etch the Si silicon of falling the rectangular pyramid groove that the degree of depth is 500 μ m.
7, adopt the BHF etching liquid to remove SiO
2, at the positive sputter Cu/Cr (1400 of substrate
/ 100
).
8, electroplating rustless steel thickness is 100 μ m, forms the different-plane metal micropin, and the micropin that form this moment is the hollow micropin.
9, adopt mechanical grinding finishing method (CMP) to remove material from the back side, thickness is 120 μ m, because micropin is a hollow, behind the micropin top that polishes off about 120 μ m height, leaves fluid channel.
10, adopt KOH solution removal residue Si, discharge different-plane metal hollow fine needle.
Shown in Fig. 2-3,1 is micropin needle body part, and 2 is the micropin fluid channel, and 3 is the micropin substrate.The different-plane metal hollow fine needle that is used for transdermal administration that present embodiment is related, its micropin needle body partial shape is the shape of falling the truncated rectangular pyramids, the cross section cone angle can reach 70.6 degree, described cross section cone angle is meant by the axis of symmetry of truncated rectangular pyramids gets a cross section, prolongs the drift angle that two sides of this face obtain.
In order to prove that different-plane metal hollow fine needle can transmit medicine, be the phenol red aqueous solution aids drug of 0.7g/ml with concentration, with phosphate buffer anthropomorphic dummy body fluid environment.Because the phenol red aqueous solution is red, in phosphate buffer, find red phenol red at last, proved that medicine can transmit by micropin.
Claims (7)
1, a kind of different-plane metal hollow fine needle manufacture method that is used for transdermal administration is characterized in that:
At first spin coating photoresist on the silicon oxide substrate exposes the silicon dioxide window, etching silicon dioxide through behind the exposure imaging;
Secondly, form the figure of falling the rectangular pyramid with silicon dioxide for mask etching silicon;
Follow splash-proofing sputtering metal conductive layer, electroplated metal layer then;
Remove the electroplated metal bottom of falling the rectangular pyramid again, leave fluid channel;
Remove silicon at last, obtain different-plane metal hollow fine needle.
2, the manufacture method that is used for the different-plane metal hollow fine needle of transdermal administration according to claim 1, it is characterized in that, the described removal electroplated metal bottom of falling the rectangular pyramid, leave fluid channel, be meant: utilize excess silicon as mask, adopt metal etch liquid to remove the exposed part of etching micropin, leave fluid channel; Perhaps adopt the mechanical grinding finishing method to remove material, the fluid channel of leaving from the back side.
3, the different-plane metal hollow fine needle manufacture method that is used for transdermal administration according to claim 1 is characterized in that, described substrate is two oxidized silicon chips of throwing of (100) face.
4, the different-plane metal hollow fine needle manufacture method that is used for transdermal administration according to claim 1 is characterized in that, the metal of described electroplated metal layer is meant a kind of in metallic nickel, rustless steel, gold, the titanium.
5, the different-plane metal hollow fine needle manufacture method that is used for transdermal administration according to claim 1 is characterized in that, the thickness of described electroplated metal layer is meant 5 μ m-100 μ m.
6, the different-plane metal hollow fine needle manufacture method that is used for transdermal administration according to claim 1 is characterized in that, the described rectangular pyramid that etches down is meant to etch the Si silicon of falling the rectangular pyramid groove that the degree of depth is 200 μ m-500 μ m.
7, the different-plane metal hollow fine needle manufacture method that is used for transdermal administration according to claim 1 is characterized in that, described different-plane metal hollow fine needle is meant the rectangular pyramid metal pin of hollow.
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|---|---|---|---|
| CN 200810042163 CN101342404B (en) | 2008-08-28 | 2008-08-28 | Method for manufacturing different-plane metal hollow fine needle for transdermal drug administration |
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|---|---|---|---|
| CN 200810042163 CN101342404B (en) | 2008-08-28 | 2008-08-28 | Method for manufacturing different-plane metal hollow fine needle for transdermal drug administration |
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|---|---|
| CN101342404A true CN101342404A (en) | 2009-01-14 |
| CN101342404B CN101342404B (en) | 2010-04-14 |
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| CN101829394A (en) * | 2010-04-27 | 2010-09-15 | 上海交通大学 | Method for preparing step micro-needle array |
| CN102526870A (en) * | 2012-01-09 | 2012-07-04 | 上海交通大学 | Anomalous plane hollow microneedle based on surface micro processing process and preparation method thereof |
| CN101623535B (en) * | 2009-08-06 | 2012-07-18 | 上海交通大学 | Preparation method of hollow medical metal micro-needle |
| CN103889499A (en) * | 2011-10-28 | 2014-06-25 | 凸版印刷株式会社 | Hollow needles manufacturing method and hollow needles |
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