CN101491700B - Preparation method of carbon fiber reinforced magnesium-containing hydroxylapatite bone-cement composite material - Google Patents

Preparation method of carbon fiber reinforced magnesium-containing hydroxylapatite bone-cement composite material Download PDF

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CN101491700B
CN101491700B CN2009100213577A CN200910021357A CN101491700B CN 101491700 B CN101491700 B CN 101491700B CN 2009100213577 A CN2009100213577 A CN 2009100213577A CN 200910021357 A CN200910021357 A CN 200910021357A CN 101491700 B CN101491700 B CN 101491700B
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magnesium
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carbon fiber
suspension
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CN101491700A (en
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黄剑锋
李娟莹
曹丽云
李抗
王文静
殷立雄
吴建鹏
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a method for preparing a nanotube-reinforced magnesium-substituted hydroxyapatite and bone cement composite, which comprises the following steps of: mixing a solution of urea, a solution of ammonium phosphate and a solution of calcium nitrate, adding a solution of magnesium nitrate into the mixed solution, placing the mixture in a microwave chemical reactor for reaction to obtain a white suspension, and removing a supernatant of the suspension through filtration to obtain F; placing F in an alumina crucible to be calcined in a muffle furnace and grinding the calcined F in an agate mortar to obtain magnesium-substituted hydroxyapatite powder; adding a silane coupling agent KH550 and absolute ethanol into the magnesium-substituted hydroxyapatite powder and subjecting to mixture to ultrasonic dispersion to obtain G; placing nanotubes into deionized water, adding carboxymethyl cellulose sodium and potassium persulfate into the deionized water and subjecting the mixture to ultrasonic dispersion to obtain H; adding citric acid and a solution of sodium citrate into a sample of H to obtain L2; and placing a sample of G in a watch glass, adding the solution L2 into the watch glass, transferring the mixture to a mould for curing and obtaining the target product.

Description

The method for preparing of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material
Technical field
The present invention relates to a kind of method for preparing that strengthens magnesium-containing hydroxylapatite bone-cement composite material, particularly a kind of method for preparing of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material.
Background technology
Hydroxyapatite is the important component part of vertebrates skeleton and tooth; Have good biocompatibility and biological activity; The human body osteocyte can directly form chemical bond on hydroxyapatite, and bond strength is high, good stability, therefore is widely used as bone and substitutes and bone grafting material.But the intensity of hydroxyapatite own is low, fragility is big; Can only be used in that alveolar ridge increases, non-bearing material aspects such as the replacement of ear ossiculum and maxillofacial bone reparation; And be difficult to be applied to the load-bearing bone aspect, therefore need strengthen the toughness reinforcing study on the modification of Denging to hydroxyapatite.Magnesium is a kind of trace element in the human body, contains magnesium 20g~30g in the healthy adult human body approximately, accounts for 0.05% of human body proportion.In present research, come the research report of modified hydroxylapatite performance less in hydroxyapatite, adding magnesium, the research of in hydroxyapatite, adding modified hydroxylapatites such as silicon, zinc has been seen in the part document.Tang Xiao loves people such as [Tang Xiaolian, Xiao Xiufeng, Liu Rongfang, the hydro-thermal synthesis and structure of siliceous hydroxyapatite characterizes, Chinese Journal of Inorganic Chemistry, 2005,21 (10): 1500-1504] with Ca (NO 3) 2, (NH 4) 3PO 4With ethyl orthosilicate be raw material, under certain pH conditions, adopt hydrothermal synthesis method to prepare the siliceous hydroxy apatite powder of nanometer.Li Mingou people such as [Li Mingou, Xiao Xiufeng, Liu Rongfang, the hydro-thermal synthesis and structure sign of zinc-containing hydroxyapatite, silicate journal, 2008,36 (3): 378-382] is with Ca (NO 3) 2, (NH 4) 3PO 4And Zn (NO 3) 2Be reaction raw materials; Adopt hydrothermal synthesis method, under the condition of pH>11, control certain reaction temperature, time and heat treatment temperature; Prepared zinc-containing hydroxyapatite, and the zinc-containing hydroxyapatite powder body have high-crystallinity and suitable stoichiometric proportion and crystal formation.
Polyacrylonitrile-based carbon fibre has just used as bio-medical material since being born, and has high strength, high-modulus characteristics, and behind the implant into body; With bone compatible good, not carcinogenic, not irritated, do not cause inflammation and [Wang Huiyu, perinaphthene such as toxic reaction; Zhou He quickly, surface treatment of carbon fibers is to the influence of biological bone cement binding ability, functional material; 2008,5 (39): 845-850].At present, toughness reinforcing mainly the concentrating on of the enhancing of hydroxyapatite bone cement or calcium phosphate bone cement added fiber (mainly being carbon fiber), Zhao Ping [Zhao Ping in single hydroxyapatite bone cement or calcium phosphate bone cement; Sun Kangning, Zhu Guangnan, carbon fiber strengthens calcium phosphate cement composite material; Silicate journal, 2005,33 (1): 32-35] etc. the people to adopt carbon fiber be that wild phase is to improve the mechanical property of calcium phosphate bone cement; Find that carbon fiber is after surface treatment; Can improve the interface bond strength between itself and the bone cement greatly, effectively transmitted load significantly improves the mechanical property of the composite of preparation.
Though these methods can both can't satisfy the requirement of clinical operation operation fully in the mechanical property that improves material in varying degrees, the method for preparing that has is also relatively more difficult, not easy to operate, and cost is higher.
Summary of the invention
The objective of the invention is to overcome above-mentioned deficiency; A kind of preparation technology is provided the method for preparing of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material simple, with low cost; The prepared composite material has higher rupture strength, can satisfy the requirement of clinical operation operation.
For achieving the above object, the technical scheme that the present invention adopts is:
1): the preparation of magnesium-containing hydroxyapatite powder body
A. analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 0.45mol/l~1.20mol/l, 0.15mol/l~0.60mol/l, 0.25mol/l~0.90mol/l, 0.25mol/l~0.90mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 3: 2: 1~6: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 0.08~3.50ml in the microwave chemical reaction appearance in 60 ℃~220 ℃ reaction 1h~7h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 3~5 times, and the gained identified as samples is designated as F;
G, with sample F in 40 ℃~100 ℃ down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 700 ℃~1100 ℃ calcining 2h~6h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 3min~15min;
I. the magnesium-containing hydroxyapatite powder body is put into beaker and add the silane coupler KH550 of its mass percent 0.5%~2.5%; The dehydrated alcohol that then splashes into 1ml~5ml is as solvent; Under ultrasonic power 80w~200w, room temperature condition; Ultra-sonic dispersion 15min~60min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 50%~63% HNO for the carbon fiber of 6 μ m with average length 3Soak 10min~60min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 30min~90min, 60 ℃~100 ℃ following drying for standby;
B, get the carbon fiber that 24-48g handled and place the there-necked flask that fills 30ml~60ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 1.0%~5.0% is to stir 30min~60min under 300rpm~600rpm at rotating speed; Then, to the potassium peroxydisulfate initiator that wherein adds carbon fiber quality 0.5%~2.5%, under ultrasonic power 80w~200w, room temperature condition; Ultra-sonic dispersion 15min~60min, the gained identified as samples is designated as H;
3): the preparation of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material
A. citric acid is configured to the solution of 0.1mol/l~0.5mol/l, is labeled as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 20-40% 1With solution L 1The sodium citrate of mass percent 15.0%~35.0% makes mixed solution L 2
C. the sample G that takes by weighing quality and be 5g~18g adds the solution L of 1ml~15ml in surface plate 2, at room temperature with Glass rod stirring, the 3min~15min that is in harmonious proportion, treat behind 3min~12min it to be moved in mould, curing molding promptly gets needed product under the pressure of 15MPa~35MPa.
The present invention adopts the microwave chemical reaction method can prepare the magnesium-containing hydroxyapatite powder body; Adopt blending method and Manual pressure molding can prepare carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material; The rupture strength of prepared composite material reaches 30.0MPa~100.5MPa; And carbon fiber is uniformly dispersed in matrix, and carbon fiber combines with basal body interface well, is the bio-medical material that has application prospect.
The specific embodiment
Embodiment 1:1): the preparation of magnesium-containing hydroxyapatite powder body
A, analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 0.45mol/l, 0.40mol/l, 0.90mol/l, 0.50mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 5: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 0.85ml in the microwave chemical reaction appearance in 100 ℃ of reaction 5h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 3 times, and the gained identified as samples is designated as F;
G, with sample F in 40 ℃ of down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 1000 ℃ of calcining 3h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 15min;
I, the magnesium-containing hydroxyapatite powder body is put into beaker and added the silane coupler KH550 of its mass percent 0.5%; The dehydrated alcohol that then splashes into 5ml is as solvent; Under ultrasonic power 200w, room temperature condition, ultra-sonic dispersion 15min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 50% HNO for the carbon fiber of 6 μ m with average length 3Soak 60min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 30min, and is subsequent use 70 ℃ of down dry backs;
B, get the carbon fiber that 24g handled and place the there-necked flask that fills the 30ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 5% is to stir 40min under the 500rpm at rotating speed; Then, to wherein adding carbon fiber quality 2.5,1.3,0.5,1.8% potassium peroxydisulfate initiator, under ultrasonic power 120w, room temperature condition; Ultra-sonic dispersion 45min, the gained identified as samples is designated as H;
3): the preparation of carbon fibre reinforced zinc-containing hydroxylapatite bone cement composite
A, the solution that citric acid is configured to 0.5mol/l are designated as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 26% 1With solution L 1The sodium citrate of mass percent 25% makes mixed solution L 2
C, get 18g sample G in surface plate, add the solution L of 15ml 2, at room temperature stir 8min with Glass rod, leave standstill behind the 9min it is moved in mould, curing molding promptly gets needed product under the pressure of 35MPa.
Embodiment 2:1): the preparation of magnesium-containing hydroxyapatite powder body
A, analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 0.70mol/l, 0.15mol/l, 0.60mol/l, 0.25mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 3: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 0.08ml in the microwave chemical reaction appearance in 160 ℃ of reaction 3h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 4 times, and the gained identified as samples is designated as F;
G, with sample F in 60 ℃ of down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 700 ℃ of calcining 6h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 10min;
I, the magnesium-containing hydroxyapatite powder body is put into beaker and added the silane coupler KH550 of its mass percent 1.2%; The dehydrated alcohol that then splashes into 3ml is as solvent; Under ultrasonic power 150w, room temperature condition, ultra-sonic dispersion 30min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 60% HNO for the carbon fiber of 6 μ m with average length 3Soak 20min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 50min, and is subsequent use 90 ℃ of down dry backs;
B, get the carbon fiber that 32g handled and place the there-necked flask that fills the 40ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 3% is to stir 60min under the 300rpm at rotating speed; Then, to the potassium peroxydisulfate initiator that wherein adds carbon fiber quality 1.3%, under ultrasonic power 150w, room temperature condition; Ultra-sonic dispersion 30min, the gained identified as samples is designated as H;
3): the preparation of carbon fibre reinforced zinc-containing hydroxylapatite bone cement composite
A, the solution that citric acid is configured to 0.3mol/l are designated as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 33% 1With solution L 1The sodium citrate of mass percent 15% makes mixed solution L 2
C, get 10g sample G in surface plate, add the solution L of 6ml 2, at room temperature stir 12min with Glass rod, leave standstill behind the 5min it is moved in mould, curing molding promptly gets needed product under the pressure of 20MPa.
Embodiment 3:1): the preparation of magnesium-containing hydroxyapatite powder body
A, analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 1.0mol/l, 0.6mol/l, 0.25mol/l, 0.90mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 6: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 3.50ml in the microwave chemical reaction appearance in 60 ℃ of reaction 7h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 5 times, and the gained identified as samples is designated as F;
G, with sample F in 100 ℃ of down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 900 ℃ of calcining 5h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 10min;
I, the magnesium-containing hydroxyapatite powder body is put into beaker and added the silane coupler KH550 of its mass percent 2.0%; The dehydrated alcohol that then splashes into 1ml is as solvent; Under ultrasonic power 100w, room temperature condition, ultra-sonic dispersion 450min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 55% HNO for the carbon fiber of 6 μ m with average length 3Soak 40min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 90min, and is subsequent use 100 ℃ of down dry backs;
B, get the carbon fiber that 40g handled and place the there-necked flask that fills the 50ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 1% is to stir 30min under the 600rpm at rotating speed; Then, to wherein adding carbon fiber quality 2.5,1.3,0.5,1.8% potassium peroxydisulfate initiator, under ultrasonic power 80w, room temperature condition; Ultra-sonic dispersion 60min, the gained identified as samples is designated as H;
3): the preparation of carbon fibre reinforced zinc-containing hydroxylapatite bone cement composite
A, the solution that citric acid is configured to 0.1mol/l are designated as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 20% 1With solution L 1The sodium citrate of mass percent 30% makes mixed solution L 2
C, get 5g sample G in surface plate, add the solution L of 1ml 2, at room temperature stir 3min with Glass rod, leave standstill behind the 3min it is moved in mould, curing molding promptly gets needed product under the pressure of 25MPa.
Embodiment 4:1): the preparation of magnesium-containing hydroxyapatite powder body
A, analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 1.20mol/l, 0.30mol/l, 0.45mol/l, 0.70mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 4: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 2.00ml in the microwave chemical reaction appearance in 220 ℃ of reaction 1h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 5 times, and the gained identified as samples is designated as F;
G, with sample F in 80 ℃ of down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 1100 ℃ of calcining 2h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 7min;
I, the magnesium-containing hydroxyapatite powder body is put into beaker and added the silane coupler KH550 of its mass percent 2.5%; The dehydrated alcohol that then splashes into 4ml is as solvent; Under ultrasonic power 80w, room temperature condition, ultra-sonic dispersion 60min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 63% HNO for the carbon fiber of 6 μ m with average length 3Soak 10min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 70min, and is subsequent use 60 ℃ of down dry backs;
B, get the carbon fiber that 48g handled and place the there-necked flask that fills the 60ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 4% is to stir 50min under the 400rpm at rotating speed; Then, to the potassium peroxydisulfate initiator that wherein adds carbon fiber quality 1.8%, under ultrasonic power 200w, room temperature condition; Ultra-sonic dispersion 15min, the gained identified as samples is designated as H;
3): the preparation of carbon fibre reinforced zinc-containing hydroxylapatite bone cement composite
A, the solution that citric acid is configured to 0.4mol/l are designated as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 40% 1With solution L 1The sodium citrate of mass percent 35% makes mixed solution L 2
C, get 13g sample G in surface plate, add the solution L of 10ml 2, at room temperature stir 15min with Glass rod, leave standstill behind the 12min it is moved in mould, curing molding promptly gets needed product under the pressure of 15MPa.

Claims (1)

1. the method for preparing of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material is characterized in that:
1): the preparation of magnesium-containing hydroxyapatite powder body
A. analytically pure carbamide, diammonium phosphate, lime nitrate, magnesium nitrate are configured to the solution of 0.45mol/l~1.20mol/l, 0.15mol/l~0.60mol/l, 0.25mol/l~0.90mol/l, 0.25mol/l~0.90mol/l respectively, solution is labeled as A, B, C, D respectively;
B, solution A, B, C are designated as E with 3: 2: 1~6: 2: 1 volume ratio mix homogeneously;
C, get 100ml E solution behind the D solution that wherein adds 0.08~3.50ml in the microwave chemical reaction appearance in 60 ℃~220 ℃ reaction 1h~7h down;
After d, reaction finish, with getting white suspension behind the microwave chemical reaction appearance natural cooling;
E, white suspension is poured in the beaker, left standstill 24h~168h in the room temperature lower open mouth, suspension is divided into two-layer up and down, and the upper strata is a clear liquid, and lower floor still is a suspension;
F, the elimination supernatant are cleaned lower floor's suspension 2 times with distilled water earlier behind the sucking filtration in the recirculated water vacuum pump, and the reuse dehydrated alcohol cleans 3~5 times, and the gained identified as samples is designated as F;
G, with sample F in 40 ℃~100 ℃ down oven dry;
H, the sample F after will drying put into alumina crucible at Muffle furnace in 700 ℃~1100 ℃ calcining 2h~6h down, treat to take out sample behind the body of heater natural cooling, promptly get the magnesium-containing hydroxyapatite powder body after in agate mortar, grinding 3min~15min;
I. the magnesium-containing hydroxyapatite powder body is put into beaker and add the silane coupler KH550 of its mass percent 0.5%~2.5%; The dehydrated alcohol that then splashes into 1ml~5ml is as solvent; Under ultrasonic power 80w~200w, room temperature condition; Ultra-sonic dispersion 15min~60min, the gained identified as samples is designated as G;
2): SURFACE TREATMENT OF CARBON FIBER and dispersion
A, be that 6mm~10mm, diameter are that to use mass concentration be 50%~63% HNO for the carbon fiber of 6 μ m with average length 3Soak 10min~60min, the reuse mass concentration is 30% hydrogen peroxide pre-oxidation treatment 30min~90min, 60 ℃~100 ℃ following drying for standby;
B, get the carbon fiber that 24-48g handled and place the there-necked flask that fills 30ml~60ml deionized water; And then the sodium carboxymethyl cellulose dispersant that adds carbon fiber quality 1.0%~5.0% is to stir 30min~60min under 300rpm~600rpm at rotating speed; Then, to the potassium peroxydisulfate initiator that wherein adds carbon fiber quality 0.5%~2.5%, under ultrasonic power 80w~200w, room temperature condition; Ultra-sonic dispersion 15min~60min, the gained identified as samples is designated as H;
3): the preparation of carbon nano-tube reinforced magnesium-containing hydroxylapatite bone-cement composite material
A. citric acid is configured to the solution of 0.1mol/l~0.5mol/l, is labeled as L 1
B, sample thief H and to the solution L that wherein adds sample H quality 20-40% 1With solution L 1The sodium citrate of mass percent 15.0%~35.0% makes mixed solution L 2
C. the sample G that takes by weighing quality and be 5g~18g adds the solution L of 1ml~15ml in surface plate 2, at room temperature with Glass rod stirring, the 3min~15min that is in harmonious proportion, treat behind 3min~12min it to be moved in mould, curing molding promptly gets needed product under the pressure of 15MPa~35MPa.
CN2009100213577A 2009-03-03 2009-03-03 Preparation method of carbon fiber reinforced magnesium-containing hydroxylapatite bone-cement composite material Expired - Fee Related CN101491700B (en)

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CN101757685A (en) * 2010-01-22 2010-06-30 孙桂森 Preparation method of medical glass fiber magnesium-containing hydroxyapatite bone cement product
CN101757686A (en) * 2010-01-22 2010-06-30 吴琼 Preparation method of medical compound glass fiber calcium-containing reinforced bone cement product
CN101791429A (en) * 2010-04-01 2010-08-04 李胜 Preparation method of medical composite glass fiber strontium containing enhanced bone cement product

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Li-yun Cao et al.Synthesis of hydroxyapatite nanoparticles in ultrasonic precipitation.《Ceramics Intemational》.2005,第31卷1041-1044. *
曾丽平等.碳纤维改性HA/PMMA生物复合材料力学性能的研究.《塑料科技》.2009,第37卷(第1期),52-55. *

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