CN102936705A - Preparation method of medical iron-based non-crystal material - Google Patents
Preparation method of medical iron-based non-crystal material Download PDFInfo
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- CN102936705A CN102936705A CN2012105108776A CN201210510877A CN102936705A CN 102936705 A CN102936705 A CN 102936705A CN 2012105108776 A CN2012105108776 A CN 2012105108776A CN 201210510877 A CN201210510877 A CN 201210510877A CN 102936705 A CN102936705 A CN 102936705A
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Abstract
The invention relates to a preparation method of a medical iron-based non-crystal material and belongs to a non-crystal alloy based on iron as a main component. The preparation method comprises the following steps of: calculating and preparing required raw materials according to atom percentage at.% of various elements in target alloy (Fe75Si10B15)98Nb2: iron particles, silicon particles, boron particles and niobium particles, wherein the mass percentage of the purities of all the raw materials is 99.99%; placing all the raw materials in a vacuum arc furnace, and melting under the protection of high-purity argon to obtain Fe-Si-B-Nb alloy ingot; and then carrying out blow casting on melted Fe-Si-B-Nb alloy in a vacuum melt-spun machine to form a (Fe75Si10B15)98Nb2 non-crystal alloy strip serving as the medical iron-based non-crystal material. The preparation method disclosed by the invention overcomes the defects that the preparation process by using the existing titanium alloy as a biological material is complicated to operate, mass is not easy to control, raw material price is expensive, and cost is high.
Description
Technical field
Technical scheme of the present invention relates to the amorphous alloy of making main composition with iron, specifically medical Fe-based amorphous material preparation method.
Background technology
In recent years, along with the clinically expansion of medical metal material range of application, some shortcomings of this class material display gradually, mainly all have certain defective in biocompatibility, totally nontoxic and material cost aspect higher.Therefore research and develop novel have excellent biological activity, totally nontoxic and cheap medical metal material and have great Research Significance and broad application prospect.
In the prior art, medical metal material is titanium alloy mostly.CN101560685 discloses " a kind of method of preparing bioactive coating on titanium alloy surface ", adopts to prepare bioactive coating at titanium alloy surface with differential arc oxidation and the heat treated operation of alkali, then soaks to generate hydroxyapatite in simulated body fluid." a kind of preparation method of bioactive composite material " that CN102068717A discloses adopts method powder metallurgy sintered, secondary oxidative treatments is processed and done to differential arc oxidation in autoclave, makes to have stronger bioactive matrix material.Titanium alloy is as preparation technology's complicated operation of biomaterial, and quality is wayward, and the prices of raw and semifnished materials are expensive, and cost is higher.
The rich content of ferro element in the middle of the earth's crust is one of the most frequently used metallic element.Iron not only has excellent mechanical property, and to the human body totally nontoxic, is one of element of needed by human.Fe-based amorphous material also has excellent biological activity, and preparation technology is easy, thereby has good development prospect aspect medical metal material.
Yet prior art does not also have medical Fe-based amorphous material.CN101492794 discloses " Fe-based amorphous alloy material and uses thereof ", and the composition of this material represents to satisfy following formula: Fe with atomic ratio
100-a-b-c-d-eNi
aCr
bP
cT
dD
e, this material is used to spraying, preparation powder core, absorbing material, magneto sensor and force sensing element.CN101509106 discloses " a kind of Fe-based amorphous alloy material and preparation method thereof ", comprises the chemical composition of following weight part: Fe:91.0-93.5; Si:5.2-6.6; B:2.5-3.3; Cr:0.05-0.25; Cu:0.010-0.030; C:0.05-0.20 is mainly for the preparation of the iron core of transformer.
Summary of the invention
Technical problem to be solved by this invention is: medical Fe-based amorphous material preparation method is provided, has overcome existing titanium alloy as preparation technology's complicated operation of biomaterial, quality is wayward, and the prices of raw and semifnished materials are expensive, the shortcoming that cost is higher.
The present invention solves this technical problem the technical scheme that adopts: medical Fe-based amorphous material preparation method, and step is:
The first step is equipped with raw material
According to target alloy (Fe
75Si
10B
15)
98Nb
2In each element atomic percent at.% calculate and be equipped with the raw material of required quality: abrasive grit, silicon grain, boron grain and niobium piece, the mass percent of all material purities are 99.99%;
Second step, melting prepare the Fe-Si-B-Nb alloy cast ingot
Be positioned in the vacuum arc fumace being equipped with all good raw materials in the first step, again the pure zirconium of 7g independently is positioned in the vacuum arc fumace and does not contact with mother alloy, under the protection of high-purity argon gas, carry out melting, the electric current of melting progressively is increased to 180A～250A from 30A, repeat melting 4 times, the time of each melting is 38～42 seconds, furnace cooling, obtain the Fe-Si-B-Nb alloy cast ingot, the atomic percent of element nb is 2% in this Fe-Si-B-Nb alloy cast ingot, and the atomic percent of all the other elements is the alloy of 75%Fe, 10%Si and 15%B;
In the 3rd step, preparation Fe-Si-B-Nb AMORPHOUS ALLOY RIBBONS is as medical Fe-based amorphous materials for later use
The polishing of the Fe-Si-B-Nb alloy cast ingot that makes in the second step is removed put into vacuum behind the top layer of oxidation and get rid of the band machine, again vacuum is got rid of with the SiC abrasive paper for metallograph of the copper wheel in the machine with 800#, 1000#, 1200# and 1800# and polish smooth successively, then the Fe-Si-B-Nb alloy cast ingot of above-mentioned polishing being removed the top layer of oxidation is heated to 1400～1600 ℃ of fusings, is 6.0 * 10 in vacuum tightness
-4Pa～8.0 * 10
-4Pa, to get rid of tape speed be 39m/s～45m/s and to blow casting pressure be under the condition of 1Pa, the Fe-Si-B-Nb alloy of fusing blown cast become (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS, (the Fe that makes
75Si
10B
15)
98Nb
2The length of AMORPHOUS ALLOY RIBBONS is 100～300cm, and width is 1～2mm, and thickness is 25～35 μ m, as medical Fe-based amorphous materials for later use.
Above-mentioned medical Fe-based amorphous material preparation method, used raw material is all by commercially available, and equipment used is the known existing apparatus of those skilled in the art, and used technique is that those skilled in the art can grasp.
The invention has the beneficial effects as follows: compared with prior art, outstanding substantive distinguishing features of the present invention is: evidence, Fe-based amorphous material does not need through any processing treatment, will generate one deck hydroxyapatite layer through of short duration immersion in giving birth to liquid solution.Fe-based amorphous material can self-assembling formation one deck hydroxyapatite layer in human body, and hydroxyapatite (HA) is the chief component of vertebrates bone and tooth, has admirably biocompatibility.Bone up to 50% all is that the inorganic hydroxyapatite by even composition consists of, and the content of hydroxyapatite is more than 96% in people's the enamel.Therefore hydroxyapatite layer can promote fast growth recovery of bone, and Fe-based amorphous material can be used as bone at medical field and substitutes and repair materials.Compared with prior art, marked improvement of the present invention is: Fe-based amorphous biomaterial is compared with titanium alloy, nickelalloy biomedical metal material, preparation technology is simple, need not carry out surface treatment to material, and just contacting with body fluid can spontaneous generation one deck the film of hydroxyapatite; Fe-based amorphous biomaterial is compared with titanium alloy, nickelalloy biological metal embedded material, and security is higher, because the Fe element is the essential element of human body, the component in the Fe-based amorphous alloy of the present invention all is to the avirulent composition of human body; Fe-based amorphous biomaterial is compared with titanium alloy, nickelalloy biological metal embedded material, and the raw material of Fe-based amorphous alloy of the present invention is easy to get and low price, and preparation process is easy, and production cost is low.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the stereoscan photograph after 24 hours in SBF solution.
Fig. 2 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the energy spectrum analysis figure after 24 hours in SBF solution.
Fig. 3 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the stereoscan photograph after 72 hours in SBF solution.
Fig. 4 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the energy spectrum analysis figure after 72 hours in SBF solution.
Fig. 5 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the stereoscan photograph after 120 hours in SBF solution.
Fig. 6 is that the present invention makes (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is soaked the energy spectrum analysis figure after 120 hours in SBF solution.
Embodiment
Embodiment 1
The first step is equipped with raw material
According to target alloy (Fe
75Si
10B
15)
98Nb
2In each element atomic percent at.% calculate and be equipped with the raw material of required quality: abrasive grit 6.081g, boron grain 0.235g, silicon grain 0.408g and niobium piece 0.275g, the mass percent of all material purities is 99.99%;
Second step, melting prepare the Fe-Si-B-Nb alloy cast ingot
Be positioned in the vacuum arc fumace being equipped with all good raw materials in the first step, again the pure zirconium of 7g independently is positioned in the vacuum arc fumace and does not contact with mother alloy, as the deoxygenation material, under the protection of high-purity argon gas, carry out melting, the electric current of melting progressively is increased to 180A from 30A, repeat melting 4 times, the time of each melting is 38 seconds, furnace cooling, obtain the Fe-Si-B-Nb alloy cast ingot, the atomic percent of element nb is 2% in this Fe-Si-B-Nb alloy cast ingot, and the atomic percent of all the other elements is the alloy of 75%Fe, 10%Si and 15%B;
In the 3rd step, preparation Fe-Si-B-Nb AMORPHOUS ALLOY RIBBONS is as medical Fe-based amorphous materials for later use
The polishing of the Fe-Si-B-Nb alloy cast ingot that makes in the second step is removed put into vacuum behind the top layer of oxidation and get rid of the band machine, again vacuum is got rid of with the SiC abrasive paper for metallograph of the copper wheel in the machine with 800#, 1000#, 1200# and 1800# and polish smooth successively, then the Fe-Si-B-Nb alloy cast ingot of above-mentioned polishing being removed the top layer of oxidation is heated to 1400 ℃ of fusings, is 6.0 * 10 in vacuum tightness
-4Pa, to get rid of tape speed be 39m/s and to blow casting pressure be under the condition of 1Pa, the Fe-Si-B-Nb alloy of fusing blown cast become (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS, (the Fe that makes
75Si
10B
15)
98Nb
2The length of AMORPHOUS ALLOY RIBBONS is 100cm, and width is 2mm, and thickness is 35 μ m, as medical Fe-based amorphous materials for later use.
The 4th step, biocompatibility test
The compound method of simulated body fluid is: add successively in order KCl 0.40g/L, NaCl 8.00g/L, NaHCO in aqueous solvent
30.35g/L, MgSO
47H
2O 0.20g/L, CaCl
22H
2O 0.19g/L, KH
2PO
40.06g, Na
2HPO
412H
2O0.09g/L and C
6H
12O
612H
2O 1.00g/L is mixed with the solution of aequum.With (the Fe that makes in the 3rd step
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is inserted in the above-mentioned simulated body fluid and is soaked, and soaks after 24 hours, shown in the stereoscan photograph of Fig. 1, begins to form hydroxyapatite on the surface of Fe base non-crystalline material, and hydroxyapatite is 9.57% in the fraction of coverage of specimen surface; Calculate from the energy spectrum analysis figure of Fig. 2, the Ca/P atomic ratio of gained hydroxyapatite is 1.41, in its normal ratio range (1.33～1.67).The hydroxyapatite prepared medical Fe-based amorphous material of spontaneous generation explanation the present embodiment in a short time has excellent biocompatibility.
Embodiment 2
The first step is equipped with raw material
According to target alloy (Fe
75Si
10B
15)
98Nb
2In each element atomic percent at.% calculate and be equipped with the raw material of required quality: abrasive grit 6.081g, boron grain 0.235g, silicon grain 0.408g and niobium piece 0.275g, the mass percent of all material purities is 99.99%;
Second step, melting prepare the Fe-Si-B-Nb alloy cast ingot
Be positioned in the vacuum arc fumace being equipped with all good raw materials in the first step, again the pure zirconium of 7g independently is positioned in the vacuum arc fumace and does not contact with mother alloy, as the deoxygenation material, under the protection of high-purity argon gas, carry out melting, the electric current of melting progressively is increased to 215A from 30A, repeat melting 4 times, the time of each melting is 40 seconds, furnace cooling, obtain the Fe-Si-B-Nb alloy cast ingot, the atomic percent of element nb is 2% in this Fe-Si-B-Nb alloy cast ingot, and the atomic percent of all the other elements is the alloy of 75%Fe, 10%Si and 15%B;
In the 3rd step, preparation Fe-Si-B-Nb AMORPHOUS ALLOY RIBBONS is as medical Fe-based amorphous materials for later use
The polishing of the Fe-Si-B-Nb alloy cast ingot that makes in the second step is removed put into vacuum behind the top layer of oxidation and get rid of the band machine, again vacuum is got rid of with the SiC abrasive paper for metallograph of the copper wheel in the machine with 800#, 1000#, 1200# and 1800# and polish smooth successively, then the Fe-Si-B-Nb alloy cast ingot of above-mentioned polishing being removed the top layer of oxidation is heated to 1500 ℃ of fusings, is 7.0 * 10 in vacuum tightness
-4Pa, to get rid of tape speed be 42m/s and to blow casting pressure be under the condition of 1Pa, the Fe-Si-B-Nb alloy of fusing blown cast become (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS, (the Fe that makes
75Si
10B
15)
98Nb
2The length of AMORPHOUS ALLOY RIBBONS is 200cm, and width is 1.5mm, and thickness is 30 μ m, as medical Fe-based amorphous materials for later use.
The 4th step, biocompatibility test
The compound method of simulated body fluid is: add successively in order KCl 0.40g/L, NaCl 8.00g/L, NaHCO in aqueous solvent
30.35g/L, MgSO
47H
2O 0.20g/L, CaCl
22H
2O 0.19g/L, KH
2PO
40.06g, Na
2HPO
412H
2O0.09g/L and C
6H
12O
612H
2O 1.00g/L is mixed with the solution of aequum.With (the Fe that makes in the 3rd step
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is inserted in the above-mentioned simulated body fluid and is soaked, and soaks after 72 hours, shown in the stereoscan photograph of Fig. 3, forms great amount of hydroxy group phosphatic rock on the surface of Fe base non-crystalline material, and hydroxyapatite reaches 40.96% in the fraction of coverage of specimen surface; Calculate from the energy spectrum analysis figure of Fig. 4, the Ca/P atomic ratio of gained hydroxyapatite is 1.55, in its normal ratio range (1.33～1.67).The hydroxyapatite prepared medical Fe-based amorphous material of spontaneous a large amount of generation explanation the present embodiment in a short time has excellent biocompatibility.
Embodiment 3
The first step is equipped with raw material
According to target alloy (Fe
75Si
10B
15)
98Nb
2In each element atomic percent at.% calculate and be equipped with the raw material of required quality: abrasive grit 6.081g, boron grain 0.235g, silicon grain 0.408g and niobium piece 0.275g, the mass percent of all material purities is 99.99%;
Second step, melting prepare the Fe-Si-B-Nb alloy cast ingot
Be positioned in the vacuum arc fumace being equipped with all good raw materials in the first step, again the pure zirconium of 7g independently is positioned in the vacuum arc fumace and does not contact with mother alloy, as the deoxygenation material, under the protection of high-purity argon gas, carry out melting, the electric current of melting progressively is increased to 250A from 30A, repeat melting 4 times, the time of each melting is 42 seconds, furnace cooling, obtain the Fe-Si-B-Nb alloy cast ingot, the atomic percent of element nb is 2% in this Fe-Si-B-Nb alloy cast ingot, and the atomic percent of all the other elements is the alloy of 75%Fe, 10%Si and 15%B;
In the 3rd step, preparation Fe-Si-B-Nb AMORPHOUS ALLOY RIBBONS is as medical Fe-based amorphous materials for later use
The polishing of the Fe-Si-B-Nb alloy cast ingot that makes in the second step is removed put into vacuum behind the top layer of oxidation and get rid of the band machine, again vacuum is got rid of with the SiC abrasive paper for metallograph of the copper wheel in the machine with 800#, 1000#, 1200# and 1800# and polish smooth successively, then the Fe-Si-B-Nb alloy cast ingot of above-mentioned polishing being removed the top layer of oxidation is heated to 1600 ℃ of fusings, is 8.0 * 10 in vacuum tightness
-4Pa, to get rid of tape speed be 45m/s and to blow casting pressure be under the condition of 1Pa, the Fe-Si-B-Nb alloy of fusing blown cast become (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS, (the Fe that makes
75Si
10B
15)
98Nb
2The length of AMORPHOUS ALLOY RIBBONS is 300cm, and width is 1mm, and thickness is 25 μ m, as medical Fe-based amorphous materials for later use.
The 4th step, biocompatibility test
The compound method of simulated body fluid is: add successively in order KCl 0.40g/L, NaCl 8.00g/L, NaHCO in aqueous solvent
30.35g/L, MgSO
47H
2O 0.20g/L, CaCl
22H
2O 0.19g/L, KH
2PO
40.06g, Na
2HPO
412H
2O0.09g/L and C
6H
12O
612H
2O 1.00g/L is mixed with the solution of aequum.With (the Fe that makes in the 3rd step
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS is inserted in the above-mentioned simulated body fluid and is soaked, and soaks after 120 hours, shown in the stereoscan photograph of Fig. 5, is thick with hydroxyapatite on the surface of Fe base non-crystalline material, and hydroxyapatite reaches 71.83% in the fraction of coverage of specimen surface; Calculate from the energy spectrum analysis figure of Fig. 6, the Ca/P atomic ratio of gained hydroxyapatite is 1.61, in its normal ratio range (1.33～1.67).The hydroxyapatite prepared medical Fe-based amorphous material of spontaneous a large amount of generation explanation the present embodiment in a short time has excellent biocompatibility.
Raw material used in above-described embodiment is all by commercially available, and equipment used is the known existing apparatus of those skilled in the art, and used technique is that those skilled in the art can grasp.
Claims (1)
1. medical Fe-based amorphous material preparation method is characterized in that step is:
The first step is equipped with raw material
According to target alloy (Fe
75Si
10B
15)
98Nb
2In each element atomic percent at.% calculate and be equipped with the raw material of required quality: abrasive grit, silicon grain, boron grain and niobium piece, the mass percent of all material purities are 99.99%;
Second step, melting prepare the Fe-Si-B-Nb alloy cast ingot
Be positioned in the vacuum arc fumace being equipped with all good raw materials in the first step, again the pure zirconium of 7g independently is positioned in the vacuum arc fumace and does not contact with mother alloy, under the protection of high-purity argon gas, carry out melting, the electric current of melting progressively is increased to 180A～250A from 30A, repeat melting 4 times, the time of each melting is 38～42 seconds, furnace cooling, obtain the Fe-Si-B-Nb alloy cast ingot, the atomic percent of element nb is 2% in this Fe-Si-B-Nb alloy cast ingot, and the atomic percent of all the other elements is 75%Fe, 10%Si and 15%B;
In the 3rd step, preparation Fe-Si-B-Nb AMORPHOUS ALLOY RIBBONS is as medical Fe-based amorphous materials for later use
The polishing of the Fe-Si-B-Nb alloy cast ingot that makes in the second step is removed put into vacuum behind the top layer of oxidation and get rid of the band machine, again vacuum is got rid of with the SiC abrasive paper for metallograph of the copper wheel in the machine with 800#, 1000#, 1200# and 1800# and polish smooth successively, then the Fe-Si-B-Nb alloy cast ingot of above-mentioned polishing being removed the top layer of oxidation is heated to 1400～1600 ℃ of fusings, is 6.0 * 10 in vacuum tightness
-4Pa～8.0 * 10
-4Pa, to get rid of tape speed be 39m/s～45m/s and to blow casting pressure be under the condition of 1Pa, the Fe-Si-B-Nb alloy of fusing blown cast become (Fe
75Si
10B
15)
98Nb
2AMORPHOUS ALLOY RIBBONS, (the Fe that makes
75Si
10B
15)
98Nb
2The length of AMORPHOUS ALLOY RIBBONS is 100～300cm, and width is 1～2mm, and thickness is 25～35 μ m, as medical Fe-based amorphous materials for later use.
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Cited By (3)
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|---|---|---|---|---|
| CN105149602A (en) * | 2015-08-16 | 2015-12-16 | 河北工业大学 | Method for preparing amorphous nanometer soft magnetism powder and special collection device of amorphous nanometer soft magnetism powder |
| US11753707B2 (en) | 2019-01-09 | 2023-09-12 | Jingran WANG | Amorphous strip master alloy and method for preparing same |
| RU2805666C2 (en) * | 2020-01-09 | 2023-10-23 | ВАН, Цзяхао | Amorphous sheet alloy and method for its production |
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| WO2010135415A2 (en) * | 2009-05-19 | 2010-11-25 | California Institute Of Technology | Tough iron-based bulk metallic glass alloys |
| CN101838778A (en) * | 2010-06-10 | 2010-09-22 | 中南大学 | Al-Ni-Ce-Pr aluminum-based amorphous alloy and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105149602A (en) * | 2015-08-16 | 2015-12-16 | 河北工业大学 | Method for preparing amorphous nanometer soft magnetism powder and special collection device of amorphous nanometer soft magnetism powder |
| CN105149602B (en) * | 2015-08-16 | 2017-03-08 | 河北工业大学 | A kind of amorphous nano soft magnetism raw powder's production technology and its collection special purpose device |
| US11753707B2 (en) | 2019-01-09 | 2023-09-12 | Jingran WANG | Amorphous strip master alloy and method for preparing same |
| RU2805666C2 (en) * | 2020-01-09 | 2023-10-23 | ВАН, Цзяхао | Amorphous sheet alloy and method for its production |
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|---|---|
| CN102936705B (en) | 2014-09-03 |
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