CN101496907A - Method for TiNi alloy stent with phosphorus injection and slow neutron irradiation activation - Google Patents

Method for TiNi alloy stent with phosphorus injection and slow neutron irradiation activation Download PDF

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Publication number
CN101496907A
CN101496907A CNA2009100713506A CN200910071350A CN101496907A CN 101496907 A CN101496907 A CN 101496907A CN A2009100713506 A CNA2009100713506 A CN A2009100713506A CN 200910071350 A CN200910071350 A CN 200910071350A CN 101496907 A CN101496907 A CN 101496907A
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China
Prior art keywords
phosphorus
tini alloy
specific embodiment
neutron irradiation
slow neutron
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CNA2009100713506A
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Chinese (zh)
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高智勇
赵兴科
隋解和
蔡伟
吴冶
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Harbin Institute of Technology
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Harbin Institute of Technology
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Priority to CNA2009100713506A priority Critical patent/CN101496907A/en
Publication of CN101496907A publication Critical patent/CN101496907A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a method for irradiation and activation of slow neutrons after a TiNi alloy stent is injected with phosphorus, and relates to a method for phosphorus injection for the TiNi alloy stent. The method solves the problem that rays have weak penetrability after the TiNi alloy stent is injected with the phosphorus in the prior art. The method comprises the following steps of: 1, chemical polishing; 2, phosphorus injection; and 3, irradiation and activation of the slow neutrons; and the TiNi alloy stent injected with the phosphorus is obtained. The TiNi alloy stent which is prepared by the method and is injected with the phosphorus has strong ray penetrability. The method is simple and has convenient operation.

Description

The method of slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus
Technical field
The present invention relates to a kind of TiNi alloy bracket and annotate the method for phosphorus.
Background technology
The TiNi alloy is ideal vascular stent material, be particularly useful for making meticulous coronary stent and coating stent of medicine etc., the TiNi alloy bracket have implant surgery simple, be easy to the location, advantage such as post, active force is even with blood vessel wall, have very wide application prospect.
Intravascular stent need be got involved the implant into body that learns a skill by the X-ray, is used for the treatment of the pathological changes of the acute obturation of blood vessel, interlayer and restenosis.The quality of intravascular stent therapeutic effect is with can accurately implant lesion locations closely related.For same material, the diameter of scaffolding thread is big more or tube wall is thick more, its X-ray observability is good more, the accuracy of implanting is just high more, but, the restenosis incidence rate of its postoperative blood vessel is also improved thereupon, therefore under the prerequisite that guarantees support force because the contact area of material and blood vessel wall also increases, wish to obtain the support that filament or thin-walled are made, but thing followed problem is exactly the observability variation.
Used radiant stand mostly is the surface injection at present 32The stainless steel stent of P, the deficiency that this radiant stand exists be ray penetrance a little less than, penetration depth is about 5mm.For the accuracy that improves implantation position with help the postoperative follow-up investigations, should further improve the X-light observability of TiNi alloy intervention support.
Summary of the invention
The objective of the invention is to annotate the problem a little less than the ray penetrance behind the phosphorus, and provide a kind of TiNi alloy bracket to annotate the method for slow neutron irradiation activation behind the phosphorus in order to solve TiNi alloy bracket in the prior art.
The TiNi alloy bracket annotates that the method for slow neutron irradiation activation realizes according to the following steps behind the phosphorus: one, chemical polishing: it is 40~60 ℃ HF/HNO that the TiNi alloy bracket is put into temperature 3/ H 2Soak 5~15s in the O system, put into acetone ultrasonic waves for cleaning 20~60min again, dry up then; Two, annotate phosphorus: employing red phosphorus is ion source, and with the vaporization of ion source heating evaporation, high voltage pulse makes it ionizing, is 30~90KV at injecting voltage then, and injection rate is 4 * 10 17P/cm 2, pulse current is 20~30A, frequency is 100~200Hz, pulse width is 40~60 μ s, grid are 0.3~1kV, two grid are the condition of the 0.5~1.5kV phosphorus of making a bet; Three, slow neutron irradiation activation: at slow-neutron flux is 5.88 * 10 17N/m 2S, slow neutron irradiation dose are 1.69 * 10 22N/m 2Condition under irradiation 6~12h, promptly get the TiNi alloy bracket of annotating phosphorus; Step 1 HF/HNO wherein 3/ H 2The O system is by HF, HNO 3And H 2O 1:2:10 by weight mixes.
The TiNi alloy bracket process slow neutron radioactivation of the notes phosphorus that the inventive method makes, thereby its ray penetrance is strengthened, penetration depth surpasses 12mm.
Description of drawings
Fig. 1 is a surface applied 32The ray picture of the TiNi alloy bracket of P emitting isotope, Fig. 2 are the ray picture that the specific embodiment 38 makes product, and Fig. 3 makes the ray penetration depth survey map of product for the specific embodiment 38.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises the combination in any between each specific embodiment.
The specific embodiment one: present embodiment TiNi alloy bracket annotates that the method for slow neutron irradiation activation realizes according to the following steps behind the phosphorus: one, chemical polishing: it is 40~60 ℃ HF/HNO that the TiNi alloy bracket is put into temperature 3/ H 2Soak 5~15s in the O system, put into acetone ultrasonic waves for cleaning 20~60min again, dry up then; Two, annotate phosphorus: employing red phosphorus is ion source, and with the vaporization of ion source heating evaporation, high voltage pulse makes it ionizing, is 30~90KV at injecting voltage then, and injection rate is 4 * 10 17P/cm 2, pulse current is 20~30A, frequency is 100~200Hz, pulse width is 40~60 μ s, grid are 0.3~1kV, two grid are the condition of the 0.5~1.5kV phosphorus of making a bet; Three, slow neutron irradiation activation: at slow-neutron flux is 5.88 * 10 17N/m 2S, slow neutron irradiation dose are 1.69 * 10 22N/m 2Condition under irradiation 6~12h, promptly get the TiNi alloy bracket of annotating phosphorus; Step 1 HF/HNO wherein 3/ H 2The O system is by HF, HNO 3And H 2O 1:2:10 by weight mixes.
Red phosphorus in the present embodiment step 2 is chemical pure.
The specific embodiment two: what present embodiment and the specific embodiment one were different is that temperature is 45~55 ℃ in the step 1.Other is identical with the specific embodiment one.
The specific embodiment three: what present embodiment and the specific embodiment one were different is that temperature is 50 ℃ in the step 1.Other is identical with the specific embodiment one.
The specific embodiment four: what present embodiment and the specific embodiment one were different is that temperature is 40 ℃ in the step 1.Other is identical with the specific embodiment one.
The specific embodiment five: what present embodiment and the specific embodiment one were different is that temperature is 60 ℃ in the step 1.Other is identical with the specific embodiment one.
The specific embodiment six: what present embodiment was different with the specific embodiment one or two is that soak time is 7~13s in the step 1.Other is identical with the specific embodiment one or two.
The specific embodiment seven: what present embodiment was different with the specific embodiment one or two is that soak time is 10s in the step 1.Other is identical with the specific embodiment one or two.
The specific embodiment eight: what present embodiment was different with the specific embodiment one or two is that soak time is 5s in the step 1.Other is identical with the specific embodiment one or two.
The specific embodiment nine: what present embodiment was different with the specific embodiment one or two is that soak time is 15s in the step 1.Other is identical with the specific embodiment one or two.
The specific embodiment ten: that present embodiment and the specific embodiment six are different is ultrasonic waves for cleaning 25~50min in the step 1.Other is identical with the specific embodiment six.
The specific embodiment 11: that present embodiment and the specific embodiment six are different is ultrasonic waves for cleaning 30min in the step 1.Other is identical with the specific embodiment six.
The specific embodiment 12: that present embodiment and the specific embodiment six are different is ultrasonic waves for cleaning 20min in the step 1.Other is identical with the specific embodiment six.
The specific embodiment 13: that present embodiment and the specific embodiment six are different is ultrasonic waves for cleaning 60min in the step 1.Other is identical with the specific embodiment six.
The specific embodiment 14: what present embodiment and the specific embodiment one, two or ten were different is that injecting voltage is 40~80KV in the step 2.Other is identical with the specific embodiment one, two or ten.
The specific embodiment 15: what present embodiment and the specific embodiment one, two or ten were different is that injecting voltage is 60KV in the step 2.Other is identical with the specific embodiment one, two or ten.
The specific embodiment 16: what present embodiment and the specific embodiment one, two or ten were different is that injecting voltage is 30KV in the step 2.Other is identical with the specific embodiment one, two or ten.
The specific embodiment 17: what present embodiment and the specific embodiment one, two or ten were different is that injecting voltage is 90KV in the step 2.Other is identical with the specific embodiment one, two or ten.
The specific embodiment 18: what present embodiment and the specific embodiment 14 were different is that pulse current is 22~28A in the step 2.Other is identical with the specific embodiment 14.
The specific embodiment 19: what present embodiment and the specific embodiment 14 were different is that pulse current is 25A in the step 2.Other is identical with the specific embodiment 14.
The specific embodiment 20: what present embodiment and the specific embodiment 14 were different is that pulse current is 20A in the step 2.Other is identical with the specific embodiment 14.
The specific embodiment 21: what present embodiment and the specific embodiment 14 were different is that pulse current is 30A in the step 2.Other is identical with the specific embodiment 14.
The specific embodiment 22: what present embodiment and the specific embodiment one, two, ten or 18 were different is that the step 2 medium frequency is 120~180Hz.Other is identical with the specific embodiment one, two, ten or 18.
The specific embodiment 23: what present embodiment and the specific embodiment one, two, ten or 18 were different is that the step 2 medium frequency is 100Hz.Other is identical with the specific embodiment one, two, ten or 18.
The specific embodiment 24: what present embodiment and the specific embodiment one, two, ten or 18 were different is that the step 2 medium frequency is 150Hz.Other is identical with the specific embodiment one, two, ten or 18.
The specific embodiment 25: what present embodiment and the specific embodiment one, two, ten or 18 were different is that the step 2 medium frequency is 200Hz.Other is identical with the specific embodiment one, two, ten or 18.
The specific embodiment 26: what present embodiment and the specific embodiment 22 were different is that pulse width is 45~55 μ s in the step 2.Other is identical with the specific embodiment 22.
The specific embodiment 27: what present embodiment and the specific embodiment 22 were different is that pulse width is 47 μ s in the step 2.Other is identical with the specific embodiment 22.
The specific embodiment 28: what present embodiment and the specific embodiment 22 were different is that pulse width is 40 μ s in the step 2.Other is identical with the specific embodiment 22.
The specific embodiment 29: what present embodiment and the specific embodiment 22 were different is that pulse width is 60 μ s in the step 2.Other is identical with the specific embodiment 22.
The specific embodiment 30: what present embodiment and the specific embodiment one, two, ten, 18 or 26 were different is that grid are 0.5~0.8kV in the step 2.Other is identical with the specific embodiment one, two, ten, 18 or 26.
Specific embodiment hentriaconta-: what present embodiment and the specific embodiment one, two, ten, 18 or 26 were different is that grid are 0.6kV in the step 2.Other is identical with the specific embodiment one, two, ten, 18 or 26.
The specific embodiment 32: what present embodiment and the specific embodiment one, two, ten, 18 or 26 were different is that grid are 0.3kV in the step 2.Other is identical with the specific embodiment one, two, ten, 18 or 26.
The specific embodiment 33: what present embodiment and the specific embodiment one, two, ten, 18 or 26 were different is that grid are 1kV in the step 2.Other is identical with the specific embodiment one, two, ten, 18 or 26.
The specific embodiment 34: what present embodiment and the specific embodiment 30 were different is that two grid are 0.7~1.2kV in the step 2.Other is identical with the specific embodiment 30.
The specific embodiment 35: what present embodiment and the specific embodiment 30 were different is that two grid are 1.0kV in the step 2.Other is identical with the specific embodiment 30.
The specific embodiment 36: what present embodiment and the specific embodiment 30 were different is that two grid are 0.5kV in the step 2.Other is identical with the specific embodiment 30.
The specific embodiment 37: what present embodiment and the specific embodiment 30 were different is that two grid are 1.5kV in the step 2.Other is identical with the specific embodiment 30.
The specific embodiment 38: present embodiment TiNi alloy bracket annotates that the method for slow neutron irradiation activation realizes according to the following steps behind the phosphorus: one, chemical polishing: it is 50 ℃ HF/HNO that the TiNi alloy bracket is put into temperature 3/ H 2Soak 10s in the O system, put into acetone ultrasonic waves for cleaning 30min again, dry up then; Two, annotate phosphorus: employing red phosphorus is ion source, and with the vaporization of ion source heating evaporation, high voltage pulse makes it ionizing, is 60KV at injecting voltage then, and injection rate is 4 * 10 17P/cm 2, pulse current is 25A, frequency is 100Hz, pulse width is 47 μ s, grid are 0.6kV, two grid are the condition of the 1.0kV phosphorus of making a bet; Three, slow neutron irradiation activation: at slow-neutron flux is 5.88 * 10 17N/m 2S, slow neutron irradiation dose are 1.69 * 10 22N/m 2Condition under irradiation 8h, promptly get the TiNi alloy bracket of annotating phosphorus; Step 1 HF/HNO wherein 3/ H 2The O system is by HF, HNO 3And H 2O 1:2:10 by weight mixes.
Surface applied 32The ray picture of the TiNi alloy bracket of P emitting isotope as shown in Figure 1, the ray picture that present embodiment makes product as shown in Figure 2, from Fig. 1 and Fig. 2 as can be seen present embodiment make the image width of product much larger than surface applied 32The image width of the TiNi alloy bracket of P emitting isotope shows that present embodiment makes the hybrid ray particle specific surface coating that product has 32The TiNi alloy bracket of P emitting isotope has higher penetrance.
The ray penetration depth measurement result that present embodiment makes product as shown in Figure 3, the present embodiment penetration depth that makes the ray of product surpasses 12mm as can be seen from Figure 3.

Claims (10)

1, the TiNi alloy bracket is annotated the method for slow neutron irradiation activation behind the phosphorus, it is characterized in that the TiNi alloy bracket annotates that the method for slow neutron irradiation activation realizes according to the following steps behind the phosphorus: one, chemical polishing: it is 40~60 ℃ HF/HNO that the TiNi alloy bracket is put into temperature 3/ H 2Soak 5~15s in the O system, put into acetone ultrasonic waves for cleaning 20~60min again, dry up then; Two, annotate phosphorus: employing red phosphorus is ion source, and with the vaporization of ion source heating evaporation, high voltage pulse makes it ionizing, is 30~90KV at injecting voltage then, and injection rate is 4 * 10 17P/cm 2, pulse current is 20~30A, frequency is 100~200Hz, pulse width is 40~60 μ s, grid are 0.3~1kV, two grid are the condition of the 0.5~1.5kV phosphorus of making a bet; Three, slow neutron irradiation activation: at slow-neutron flux is 5.88 * 10 17N/m2s, slow neutron irradiation dose are 1.69 * 10 22N/m 2Condition under irradiation 6~12h, promptly get the TiNi alloy bracket of annotating phosphorus; Step 1 HF/HNO wherein 3/ H 2The O system is by HF, HNO 3And H 2O 1:2:10 by weight mixes.
2, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 1 is characterized in that temperature is 45~55 ℃ in the step 1.
3, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 1 and 2 is characterized in that soak time is 7~13s in the step 1.
4, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 3 is characterized in that ultrasonic waves for cleaning 25~50min in the step 1.
5, according to the method for slow neutron irradiation activation behind claim 1, the 2 or 4 described TiNi alloy brackets notes phosphorus, it is characterized in that injecting voltage is 40~80KV in the step 2.
6, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 5 is characterized in that pulse current is 22~28A in the step 2.
7, according to the method for slow neutron irradiation activation behind claim 1,2, the 4 or 6 described TiNi alloy brackets notes phosphorus, it is characterized in that the step 2 medium frequency is 120~180Hz.
8, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 7 is characterized in that pulse width is 45~55 μ s in the step 2.
9, according to the method for slow neutron irradiation activation behind claim 1,2,4, the 6 or 8 described TiNi alloy brackets notes phosphorus, it is characterized in that grid are 0.5~0.8kV in the step 2.
10, the method for slow neutron irradiation activation behind the TiNi alloy bracket notes phosphorus according to claim 9 is characterized in that two grid are 0.7~1.2kV in the step 2.
CNA2009100713506A 2009-01-24 2009-01-24 Method for TiNi alloy stent with phosphorus injection and slow neutron irradiation activation Pending CN101496907A (en)

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CNA2009100713506A CN101496907A (en) 2009-01-24 2009-01-24 Method for TiNi alloy stent with phosphorus injection and slow neutron irradiation activation

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101627934B (en) * 2009-08-13 2011-06-08 哈尔滨工业大学 Preparation method for radioactivity TiNi alloy bracket without fringe effect

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101627934B (en) * 2009-08-13 2011-06-08 哈尔滨工业大学 Preparation method for radioactivity TiNi alloy bracket without fringe effect

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Application publication date: 20090805