CN102452797A - Preparation method of medicinal glass bottle inner wall coating - Google Patents
Preparation method of medicinal glass bottle inner wall coating Download PDFInfo
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- CN102452797A CN102452797A CN2010105198504A CN201010519850A CN102452797A CN 102452797 A CN102452797 A CN 102452797A CN 2010105198504 A CN2010105198504 A CN 2010105198504A CN 201010519850 A CN201010519850 A CN 201010519850A CN 102452797 A CN102452797 A CN 102452797A
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Abstract
The invention discloses a preparation method of a medicinal glass bottle inner wall coating, which comprises the following steps: putting the medicinal glass bottle into a reaction cavity of the atomic layer deposition equipment, and carrying out vacuum treatment on the reaction cavity; pressing a certain amount of first precursor into a reaction cavity in a pulse mode, soaking and adsorbing the pressed first precursor on the inner wall of a medicinal glass bottle, and exhausting to remove redundant first precursor; a certain amount of second precursor is pressed into the reaction cavity in a pulse mode, the pressed second precursor reacts and adsorbs the first precursor on the surface of the inner wall of the medicinal glass bottle, and redundant second precursor and reaction byproducts are removed through air suction; repeating the steps until a coating film with the required thickness is deposited on the inner wall of the medicinal glass bottle; the first precursor is a silicon-containing precursor, and the second precursor is an oxygen-containing precursor; or the first precursor is an oxygen-containing precursor, and the second precursor is a silicon-containing precursor. The medicinal glass bottle prepared by the method can ensure the stability and purity of the medicament.
Description
Technical field
The present invention refers in particular to a kind of preparation method of medicinal glass bottle inside coating about a kind of coating process.
Background technology
Pharmaceutical glass is a main branch of medical packaging industry, also is an important component part of whole medicine industry.It has irreplaceable performance and advantage, in China by extensively as the pharmaceutical glass packaging vessel of all kinds of formulations such as injection powder injection, aqueous injection, infusion solution, tablet, pill, oral liquid and freeze-drying, vaccine, blood products.Yet; Pharmaceutical glass as wrapping material all will directly contact medicine; And great majority also will carry out the medicine storage of long period; So some component in the glass possibly perhaps caused the mutual migration of composition by the medicine that is contacted stripping, also possibly caused the flake phenomenon by soup long period of soaking, erosion.Therefore, the performance of pharmaceutical glass and quality directly affect the quality of medicine, and be closely bound up with people's health and safety.
At present, normal borosilicate glass bottle and the soda-lime glass bottle that uses in China's pharmaceutical industries exists acid resistance, the weak problem of alkali resistance.In the course of processing of vial, vial hot briquetting meeting causes basic oxide to be separated out; After annealing, this basic oxide residue is stayed this vial surface, the alkalescence of this vial is increased, and cleaning process can not effectively be removed this basic oxide; Through behind the certain hour, these basic oxide are discharged in the soup of storage, thereby cause the stability of drug products variation.Even the borosilicate glass bottle of high resistibility is not complete inertia yet, in disinfection or storage process, basic ion (especially sodium ion), aluminum ion etc. still can take place and leak into the situation the medicine from glass surface in the surface that contacts with medicine.
Summary of the invention
Main purpose of the present invention is to provide a kind of preparation method of medicinal glass bottle inside coating, through the medicinal glass bottle of this method preparation, can guarantee the stability and the purity of medicament.
For achieving the above object, the present invention provides a kind of preparation method of medicinal glass bottle inside coating, comprising:
Step S10: medicinal glass bottle is put into the reaction cavity of atomic layer deposition apparatus, said reaction cavity is carried out vacuum-treat;
Step S20: a certain amount of first presoma pulse is pressed in the said reaction cavity, and first presoma that is pressed into soaks into absorption at said medicinal glass bottle inwall, bleeds and removes unnecessary said first presoma;
Step S30: a certain amount of second presoma pulse is pressed in the said reaction cavity; Said first presoma reaction absorption on second presoma that is pressed into and the said medicinal glass bottle inner wall surface is bled and is removed unnecessary said second presoma and byproduct of reaction;
Step S40: repeating said steps S20 and step S30 are until the coating film of said medicinal glass bottle inwall deposition desired thickness;
Wherein, said first presoma is for containing silicon precursor, and said second presoma is for containing the oxygen presoma; Perhaps, said first presoma is for containing the oxygen presoma, and said second presoma is for containing silicon precursor.
Said a certain amount of first presoma pulse is pressed into said reaction cavity before, said step S20 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.
Said a certain amount of second presoma pulse is pressed into said reaction cavity before, said step S30 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.
Among said step S20 and the step S30, the burst length is respectively 0.015-50S.
Among said step S20 and the step S30, the time of bleeding is respectively 0.015-120S.
Among the said step S10, after the vacuum-treat, the vacuum tightness of said reaction cavity is 101Pa to 10-2Pa.
Among said step S20 and the step S30, said first presoma and said second presoma get in the said reaction cavity through carrier gas.
The said silicon precursor that contains is the inorganic or organic silicide that contains Siliciumatom, includes: SiCl
4, Si (OCH
2CH
3)
4, Si (N (CH
3)
2)
4, Si (N (CH
3)
2)
3Cl, CH
3OSi (NCO)
3, Si (NCO)
4, SiH
2(N (CH
3)
2)
2, SiH (N (CH
3)
2)
3, H
2N (CH
2)
3Si (OC
2H
5)
3Or (Bu
tO)
3SiOH.
The said oxygen presoma that contains is gas or the liquid substance that contains Sauerstoffatom, includes: H
2O, O
2, H
2O
2, O
3Or O plasma body.
Said catalyzer includes: NH for containing amino ionic compound
3, pyridine (C
5H
5N) or C
2H
5N.
Compared with prior art; The preparation method of medicinal glass bottle inside coating of the present invention; At medicinal glass bottle internal surface uniform deposition one deck silicon oxide film; This silicon oxide film chemisorption is in this medicinal glass bottle internal surface, and effectively the impurity of insulating glass bottle and metals ion move in medicament, guarantees the stability and the purity of medicament.In addition, the preparation method of medicinal glass bottle inside coating of the present invention, simple to operate, be easy to realize, through the Control Circulation pulse number, realize gauge control, and deposition uniformity is good.
Description of drawings
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the embodiments of the invention synoptic diagram.
Embodiment
Relevant technology contents of the present invention and detailed description, existing conjunction with figs. is explained as follows:
As shown in Figure 1, the preparation method for medicinal glass bottle inside coating of the present invention comprises:
Step S10: medicinal glass bottle is put into the reaction cavity of atomic layer deposition apparatus, said reaction cavity is carried out vacuum-treat; Wherein, after the vacuum-treat, the vacuum tightness of said reaction cavity can be 10
1Pa to 10
-2Pa.In addition, the temperature of said reaction cavity can be 10 ℃ to 500 ℃.In addition, according to the size of reaction cavity, can deposit the medicinal glass bottle of a plurality of identical or different model sizes simultaneously.
Step S20: a certain amount of first presoma pulse is pressed in the said reaction cavity, and first presoma that is pressed into soaks into absorption at said medicinal glass bottle inwall, bleeds and removes unnecessary said first presoma; Promptly; Because said reaction cavity has been done vacuum-treat; Said first presoma is owing in pressure reduction the is pressed into said reaction cavity, and the special-purpose valve body through being provided with, and can realize that the said first presoma pulse feeds in the said reaction cavity; This special use valve body is commercially available matured product, repeats no more at this; Wherein, the burst length can be 0.015-50S, and the time of bleeding can be 0.015-120S.In addition, said first presoma gets into reaction cavity through carrier gas, and said carrier gas can not participated in the rare gas element that reacts for nitrogen, argon gas etc., and carrier gas flux is 1-300sccm, not as limit, can adjust accordingly according to practical application.
Step S30: a certain amount of second presoma pulse is pressed in the said reaction cavity; Said first presoma reaction absorption on second presoma that is pressed into and the said medicinal glass bottle inner wall surface is bled and is removed unnecessary said second presoma and byproduct of reaction; This reaction process is identical with said first presoma, repeats no more; Wherein, the burst length can be 0.015-50S, and the time of bleeding can be 0.015-120S.In addition, said second presoma gets into reaction cavity through carrier gas, and said carrier gas can not participated in the rare gas element that reacts for nitrogen, argon gas etc., and carrier gas flux is 1-300sccm, not as limit, can adjust accordingly according to practical application.
Step S40: repeating said steps S20 and step S30 are until the coating film of said medicinal glass bottle inwall deposition desired thickness.
Wherein, said first presoma among the step S20 is for containing silicon precursor, and said second presoma among the step S30 is for containing the oxygen presoma; Perhaps, said first presoma among the step S20 is for containing the oxygen presoma, and said second presoma among the step S30 is for containing silicon precursor.Particularly: the said silicon precursor that contains is the inorganic or organic silicide that contains Siliciumatom, can include: SiCl
4, Si (OCH
2CH
3)
4, Si (N (CH
3)
2)
4, Si (N (CH
3)
2)
3Cl, CH
3OSi (NCO)
3, Si (NCO)
4, SiH
2(N (CH
3)
2)
2, SiH (N (CH
3)
2)
3, H
2N (CH
2)
3Si (OC
2H
5)
3Or (Bu
tO)
3SiOH.The said oxygen presoma that contains is gas or the liquid substance that contains Sauerstoffatom, can include: H
2O, O
2, H
2O
2, O
3, O plasma body etc.
In addition, in order to improve reaction efficiency, said a certain amount of first presoma pulse is pressed into said reaction cavity before, said step S20 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.Wherein, the burst length can be 0.015-50S, and said catalyzer can include: NH for containing amino ionic compound
3, pyridine (C
5H
5N), C
2H
5N etc.
In addition, in order to improve reaction efficiency, said a certain amount of second presoma pulse is pressed into said reaction cavity before, said step S30 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.Wherein, the burst length can be 0.015-50S, and said catalyzer can include: NH for containing amino ionic compound
3, pyridine (C
5H
5N), C
2H
5N etc.
Adopt the preparation method of medicinal glass bottle inside coating of the present invention, the thickness of sedimentary silicon oxide film on the medicinal glass bottle inwall can be controlled between several nanometers and the hundreds of micron, and thickness is when 30～500nm scope, and barrier property is better.Therefore, can pass through the Control Circulation pulse number, realize gauge control.
Below, further specify the present invention through specific embodiment of the present invention.
Embodiment one
As shown in Figure 2, in the present embodiment, the preparation method of medicinal glass bottle inside coating comprises the steps:
Low borosilicate glass bottle 10 is positioned in the reaction cavity of atomic layer deposition apparatus, and reaction cavity vacuum tightness is 10
-2Pa, the reaction cavity temperature is 500 ℃, pulse O
30.015s, the 0.05s that bleeds, pulse H then
2N (CH
2)
3Si (OC
2H
5)
30.015s 0.05s bleeds.
Wherein, select for use nitrogen as carrier gas, carrier gas flux is 20sccm.The alternate cycles pulse is 500 times successively, and the silicon oxide film thickness 20 that obtains is 45nm.
Embodiment two
In the present embodiment, the preparation method of medicinal glass bottle inside coating comprises the steps:
The soda-lime glass bottle is positioned in the reaction cavity of atomic layer deposition apparatus, reaction cavity vacuum tightness is 10
-1Pa, the reaction cavity temperature is 10 ℃, pulse pyridine 0.8s, pulse SiCl again
430s, the 60s that bleeds, pulse pyridine 0.8s, pulse H more then
2O 50s, 120s bleeds.
Wherein, select for use argon gas as carrier gas, carrier gas flux is 150sccm.Cycle pulse is 800 times successively, and the silicon oxide film thickness that obtains is 80nm.
Embodiment three
In the present embodiment, the preparation method of medicinal glass bottle inside coating comprises the steps:
Neutral borosilicate glass bottle is positioned in the reaction cavity of atomic layer deposition apparatus, and reaction cavity vacuum tightness is 10
-1Pa, the reaction cavity temperature is 150 ℃, pulse Si (N (CH
3)
2)
450s, the 120s that bleeds, pulsed plasma O then
2/ N
23s, 15s bleeds.
Wherein, select for use argon gas as carrier gas, carrier gas flux is 1sccm.Cycle pulse is 3000 times successively, and the silicon oxide film thickness that obtains is 240nm.
Embodiment four
In the present embodiment, the preparation method of medicinal glass bottle inside coating comprises the steps:
The high-boron-silicon glass bottle is positioned in the reaction cavity of atomic layer deposition apparatus, reaction cavity vacuum tightness is 10
1Pa, the reaction cavity temperature is 250 ℃, pulse H
2N (CH
2)
3Si (OC
2H
5)
35s, the 25s that bleeds, pulse H then
2O 5s, the 25s that bleeds, pulse O afterwards
33s, 80s bleeds.
Wherein, select for use nitrogen as carrier gas, carrier gas flux is 300sccm.Cycle pulse is 50 times successively, and the silicon oxide film thickness that obtains is 30nm.
Embodiment five
In the present embodiment, the preparation method of medicinal glass bottle inside coating comprises the steps:
Neutral borosilicate glass bottle is positioned in the reaction cavity of atomic layer deposition apparatus, and reaction cavity vacuum tightness is 10 ° of Pa, and the reaction cavity temperature is 30 ℃, pulse NH
350s, pulse SiCl again
410s, the 60s that bleeds, pulse NH then
30.015s, pulse H again
2O 5s, 30s bleeds.
Wherein, select for use nitrogen as carrier gas, carrier gas flux is 30sccm.Cycle pulse is 5000 times successively, and the silicon oxide film thickness that obtains is about 500nm.
Above-mentionedly being merely preferred embodiment of the present invention, is not to be used for limiting the scope that the present invention implements.Be that all equalizations of doing according to claims of the present invention change and modification, be claim of the present invention and contain.
Claims (10)
1. the preparation method of a medicinal glass bottle inside coating is characterized in that, comprising:
Step S10: medicinal glass bottle is put into the reaction cavity of atomic layer deposition apparatus, said reaction cavity is carried out vacuum-treat;
Step S20: a certain amount of first presoma pulse is pressed in the said reaction cavity, and first presoma that is pressed into soaks into absorption at said medicinal glass bottle inwall, bleeds and removes unnecessary said first presoma;
Step S30: a certain amount of second presoma pulse is pressed in the said reaction cavity; Said first presoma reaction absorption on second presoma that is pressed into and the said medicinal glass bottle inner wall surface is bled and is removed unnecessary said second presoma and byproduct of reaction;
Step S40: repeating said steps S20 and step S30 are until the coating film of said medicinal glass bottle inwall deposition desired thickness;
Wherein, said first presoma is for containing silicon precursor, and said second presoma is for containing the oxygen presoma; Perhaps, said first presoma is for containing the oxygen presoma, and said second presoma is for containing silicon precursor.
2. the method for claim 1 is characterized in that, said a certain amount of first presoma pulse is pressed into said reaction cavity before, said step S20 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.
3. the method for claim 1 is characterized in that, said a certain amount of second presoma pulse is pressed into said reaction cavity before, said step S30 also comprises: a certain amount of catalyzer pulse is pressed in the said reaction cavity.
4. like claim 1,2 or 3 described methods, it is characterized in that among said step S20 and the step S30, the burst length is respectively 0.015-50S.
5. the method for claim 1 is characterized in that, among said step S20 and the step S30, the time of bleeding is respectively 0.015-120S.
6. the method for claim 1 is characterized in that, among the said step S10, after the vacuum-treat, the vacuum tightness of said reaction cavity is 10
1Pa to 10
-2Pa.
7. the method for claim 1 is characterized in that, among said step S20 and the step S30, said first presoma and said second presoma get in the said reaction cavity through carrier gas.
8. the method for claim 1 is characterized in that, the said silicon precursor that contains is the inorganic or organic silicide that contains Siliciumatom, includes: SiCl
4, Si (OCH
2CH
3)
4, Si (N (CH
3)
2)
4, Si (N (CH
3)
2)
3Cl, CH
3OSi (NCO)
3, Si (NCO)
4, SiH
2(N (CH
3)
2)
2, SiH (N (CH
3)
2)
3, H
2N (CH
2)
3Si (OC
2H
5)
3Or (Bu
tO)
3SiOH.
9. the method for claim 1 is characterized in that, the said oxygen presoma that contains is gas or the liquid substance that contains Sauerstoffatom, includes: H
2O, O
2, H
2O
2, O
3Or O plasma body.
10. like claim 2 or 3 described methods, it is characterized in that said catalyzer includes: NH for containing amino ionic compound
3, pyridine (C
5H
5N) or C
2H
5N.
Priority Applications (1)
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|---|---|---|---|
| CN201010519850.4A CN102452797B (en) | 2010-10-19 | 2010-10-19 | Method for preparing coating on inner wall of medicinal glass bottle |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010519850.4A CN102452797B (en) | 2010-10-19 | 2010-10-19 | Method for preparing coating on inner wall of medicinal glass bottle |
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| CN102452797B CN102452797B (en) | 2014-08-20 |
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| CN105050977A (en) * | 2012-11-30 | 2015-11-11 | 康宁股份有限公司 | Sulfide solid electrolyte material, lithium solid battery and method of preparing sulfide solid electrolyte material |
| US10023495B2 (en) | 2012-11-30 | 2018-07-17 | Corning Incorporated | Glass containers with improved strength and improved damage tolerance |
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| US11608290B2 (en) | 2012-06-28 | 2023-03-21 | Corning Incorporated | Delamination resistant glass containers with heat-tolerant coatings |
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| US10307333B2 (en) | 2012-11-30 | 2019-06-04 | Corning Incorporated | Glass containers with delamination resistance and improved damage tolerance |
| US10117806B2 (en) | 2012-11-30 | 2018-11-06 | Corning Incorporated | Strengthened glass containers resistant to delamination and damage |
| US11951072B2 (en) | 2012-11-30 | 2024-04-09 | Corning Incorporated | Glass containers with improved strength and improved damage tolerance |
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| WO2015132443A1 (en) * | 2014-03-03 | 2015-09-11 | Picosun Oy | Protecting an interior of a gas container with an ald coating |
| US10899659B2 (en) | 2014-09-05 | 2021-01-26 | Corning Incorporated | Glass articles and methods for improving the reliability of glass articles |
| EP3368430A4 (en) * | 2015-10-27 | 2019-07-24 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Internally coated vessel for housing a metal halide |
| CN109205014A (en) * | 2017-06-30 | 2019-01-15 | 黄期骏 | Bottle body texture manufacturing method and structure thereof |
| CN113623529A (en) * | 2020-08-19 | 2021-11-09 | 赵永刚 | Sampling tank for storing ambient air sample |
| CN113529046A (en) * | 2021-08-09 | 2021-10-22 | 梁存军 | High-temperature vapor phase coating machine for sampling tank of Suma tank |
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