CN101700411B - Method for preparing glass microfibre reinforcement nano-hydroxyapatite biological composite coating - Google Patents
Method for preparing glass microfibre reinforcement nano-hydroxyapatite biological composite coating Download PDFInfo
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- CN101700411B CN101700411B CN200910218836A CN200910218836A CN101700411B CN 101700411 B CN101700411 B CN 101700411B CN 200910218836 A CN200910218836 A CN 200910218836A CN 200910218836 A CN200910218836 A CN 200910218836A CN 101700411 B CN101700411 B CN 101700411B
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Abstract
The invention relates to a method for preparing a glass microfibre reinforcement nano-hydroxyapatite biological composite coating, comprising the following steps of: firstly, mixing Ca(NO3)2.4H2O and (NH2)2HPO4 and adding distilled water to dissolve; then adding urea powder to make the mixture into mixed liquor; putting a generating head of a multi-frequency phonochemistry generator into the mixed liquor, filtering and drying after phonochemistry synthesis, then obtaining nano-HAp powder; dispersing the nano-HAp powder, analytically pure chitosan and glass microfibre in isopropanol, then obtaining suspending liquid; pouring the suspending liquid into a hydrothermal electrophoresis reaction kettle; putting the reaction kettle in a precise constant temperature oven, galvanizing and depositing; then drying and finally obtaining the composite coating. Nano-hydroxyapatite powder is prepared by using a phonochemistry synthesis method, and therefore, the prepared composite coating is compact and even, the crystalline phase of the coating is stable, the bonding strength can be greatly increased; and the expected bonding strength reaches 20-40MPa.
Description
Technical field
The present invention relates to a kind of method for preparing of biological composite coating, be specifically related to a kind of method for preparing of glass microfibre reinforcement nano-hydroxyapatite biological composite coating.
Background technology
Bone reparation in recent years and bone alternate material become one of research focus of researcheres in the biomaterial research field.
Hydroxyapatite (is called for short HA or HAP, its molecular formula Ca
10(PO
4)
6(OH)
2) be the main component of inanimate matter in the body bone tissue, it has excellent biological compatibility, biological activity and the connection of bone property, the damaged reparation of body bone tissue with rebuild, be considered to a kind of human body implantation body material of tool potentiality.Yet the fragility of hydroxyapatite is big, can not bear load limit its range of application (Jiang Geng, Wang Ping Hua, Changjiang University's journal, 2008,5 (3): 20).Given this,, combine the excellent mechanical properties of medical metal material and the good biological property of hydroxyapatite, prepared the Metal Substrate biological coating at medical metal (titanium alloy, steel alloy) surface-coated hydroxyapatite coating layer.
Yet the fatigue behaviour of metal is relatively poor, easily release metal ions; Cause the inefficacy of implant; The organic macromolecule-based of employing biological coating is also arranged, produce poisonous monomer in body fluid, also make implant come off and lose efficacy but degraded can take place organic high molecular compound.
Carbon/carbon (C/C) composite is a kind of new material that international field of new is given priority to, and has function and architectural characteristic concurrently, excellent combination property, and as bone reparation and bone substitution material, the chemistry of material with carbon element, physiological property are stablized superior biocompatibility.Carbon/carbon (C/C) composite material toughness is good; Can overcome the fragility of single material with carbon element, and intensity is high, fatigue properties are superior, particularly its elastic modelling quantity and people's bone photo are worked as; Therefore be a kind of biomaterial that has potentiality; Have application prospect (Gao Lin, Lin Jiarui.Histological observation of carbonaceous materialscontaining hydroxyapat ite [C] .The International Conference onCarbon 2002,2002; Beijing, China.).But, also need combine just can prepare the biomaterial of function admirable with the material of biologically active as bio-inert material.
People such as Huang Jianfeng, Zhu Guangyan (Zhu Guangyan, Huang Jianfeng, Wu Jianpeng; Cao Liyun, He Haiyan, Rare Metals Materials and engineering; 2007; 2 (36): 749-753) utilize the hydrothermal electrodeposition method C matrix surface prepared nano level hydroxyapatite coating layer, cause thermal decomposition and spraying process non-linear of HAp when electrochemical deposition method overcomes traditional plasma spraying because of high temperature, and can be through thickness, surface texture and the porosity etc. of the accurate control coating of experiment parameter such as control electric current, voltage, temperature; But the coating of this method preparation and the adhesion of adhesion between the matrix and coating self are not enough, restrict it and further develop.
People such as Cao Liyun, Li Yinghua (Li Yinghua, Cao Liyun, Huang Jianfeng; Once mediate banyan; China Tissue Engineering Study and clinical rehabilitation, 2008,41 (12): 8143-8146) adopt the hydro-thermal electrophoresis method prepared C the base chitosan HAp composite biological coating; The good mechanical property of C/C composite is combined with the good biological of HAp, chitosan is active, and the bone of preparing a new generation substitutes and repair materials.But, still exist between coating and the matrix, the not high problem of adhesion between coating and the coating.
At present; Both at home and abroad to improve C composite material surface and hydroxyapatite adhesion research mainly depositing operation with C in the matrix surface modification, and do not appear in the newspapers as yet for the research of adopting glass microfiber to strengthen the bond strength of figure layer and substrate combinating strength and coating inside.
Summary of the invention
The object of the present invention is to provide the method for preparing of the simple glass microfibre reinforcement nano-hydroxyapatite biological composite coating of a kind of technology; The prepared composite coating has higher binding strength, higher uniformity and compactness; Do not need follow-up treatment process, prevented phase transformation and the cracking of coating in subsequent technique effectively.
For achieving the above object, the technical scheme that the present invention adopts is:
1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is 1: 1.50～1.90 mixing, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.035～0.25mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=1: 4.6～10.4 add the carbamide powder body and process mixed liquor, stir; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 100-300w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer HAp;
2) preparation of the little short fiber of glass
Get the staple glass fibre that specification is C-9, after adding entry and in fiberizer, staple glass fibre being worn into the fibre glass that length range is 5～25 μ m, take out and in 60 ℃～90 ℃ baking oven, dry;
3) get nanometer HAp, analytical pure chitosan and glass microfiber by 10: (1-3): it is 4～13g/L that mass ratio (1-3) is dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol, and behind magnetic agitation 3～15h, ageing 1～5h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor then; Put it in the exact constant temperature baking oven, in 80 ℃～140 ℃, be incubated 1h, regulation voltage is in 45V～120V scope; Powered-down behind energising deposition 8min～35min; Stop deposition, treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
Specification of the present invention is that the staple glass fibre of C-9 adopts east, Chinese Shenyang to ring the staple glass fibre of producing.
The present invention utilizes the sonochemistry synthetic method to prepare nano level hydroxy apatite powder, simultaneously, adopts the hydro-thermal electrophoresis method to prepare the enhanced nano-hydroxyapatite biological composite coating (G of glass microfiber
(f)-HA/CS), the prepared composite coating is evenly fine and close, and the coating crystalline phase is stable, and bond strength has very big raising, and the expection bond strength reaches between 20MPa～40MPa.
Description of drawings
Fig. 1 is the prepared G of the present invention
(f)The SEM figure of-HA/CS composite coating.
The specific embodiment
Embodiment 1:1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is mixing in 1: 1.57, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.04mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=adding carbamide powder body was processed mixed liquor in 1: 5, stirred; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 100w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer Hap powder body;
2) preparation of the little short fiber of glass
Getting east, Chinese Shenyang, to ring the specification of producing be after the staple glass fibre of C-9 adds entry and in fiberizer, staple glass fibre worn into the fibre glass that length range is 5～25 μ m, to take out and in 60 ℃ baking oven, dry;
3) getting nanometer HAp, analytical pure chitosan and glass microfiber, to be dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol by 10: 1: 1 mass ratio be 6g/L, and behind the magnetic agitation 3h, ageing 2h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor puts it in the exact constant temperature baking oven then, in 80 ℃, is incubated 1h; Regulation voltage is at 110V, and powered-down behind the energising deposition 10min stops deposition; Treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
Embodiment 2:1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is mixing in 1: 1.67, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.08mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=adding carbamide powder body was processed mixed liquor in 1: 6, stirred; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 200w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer Hap powder body;
2) preparation of the little short fiber of glass
Getting east, Chinese Shenyang, to ring the specification of producing be after the staple glass fibre of C-9 adds entry and in fiberizer, staple glass fibre worn into the fibre glass that length range is 5～25 μ m, to take out and in 60 ℃ baking oven, dry;
3) getting nanometer HAp, analytical pure chitosan and glass microfiber, to be dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol by 10: 1: 1 mass ratio be 8g/L, and behind the magnetic agitation 6h, ageing 25h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor puts it in the exact constant temperature baking oven then, in 100 ℃, is incubated 1h; Regulation voltage is at 110V, and powered-down behind the energising deposition 20min stops deposition; Treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
Embodiment 3:1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is mixing in 1: 1.77, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.12mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=adding carbamide powder body was processed mixed liquor in 1: 7, stirred; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 300w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer Hap powder body;
2) preparation of the little short fiber of glass
Getting east, Chinese Shenyang, to ring the specification of producing be after the staple glass fibre of C-9 adds entry and in fiberizer, staple glass fibre worn into the fibre glass that length range is 5～25 μ m, to take out and in 60 ℃ baking oven, dry;
3) getting nanometer HAp, analytical pure chitosan and glass microfiber, to be dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol by 10: 2: 2 mass ratio be 10g/L, and behind the magnetic agitation 9h, ageing 2.5h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor puts it in the exact constant temperature baking oven then, in 120 ℃, is incubated 1h; Regulation voltage is at 90V, and powered-down behind the energising deposition 10min stops deposition; Treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
Embodiment 4:1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is mixing in 1: 1.5, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.035mo l/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=adding carbamide powder body was processed mixed liquor in 1: 10.4, stirred; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 260w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer Hap powder body;
2) preparation of the little short fiber of glass
Getting east, Chinese Shenyang, to ring the specification of producing be after the staple glass fibre of C-9 adds entry and in fiberizer, staple glass fibre worn into the fibre glass that length range is 5～25 μ m, to take out and in 90 ℃ baking oven, dry;
3) getting nanometer HAp, analytical pure chitosan and glass microfiber, to be dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol by 10: 3: 3 mass ratio be 4g/L, and behind the magnetic agitation 12h, ageing 1h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor puts it in the exact constant temperature baking oven then, in 140 ℃, is incubated 1h; Regulation voltage is in the 45V scope, and powered-down behind the energising deposition 35min stops deposition; Treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
Embodiment 5:1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is mixing in 1: 1.9, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.25mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=adding carbamide powder body was processed mixed liquor in 1: 4.6, stirred; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 180w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer Hap powder body;
2) preparation of the little short fiber of glass
Getting east, Chinese Shenyang, to ring the specification of producing be after the staple glass fibre of C-9 adds entry and in fiberizer, staple glass fibre worn into the fibre glass that length range is 5～25 μ m, to take out and in 75 ℃ baking oven, dry;
3) getting nanometer HAp, analytical pure chitosan and glass microfiber, to be dispersed in the mass concentration that makes HAp in the analytically pure isopropyl alcohol by 10: 3: 2 mass ratio be 13g/L, and behind the magnetic agitation 15h, ageing 5h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor puts it in the exact constant temperature baking oven then, in 115 ℃, is incubated 1h; Regulation voltage is in the 120V scope, and powered-down behind the energising deposition 8min stops deposition; Treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain composite coating.
As can be seen from Figure 1, coatings prepared combines evenly fine and close, does not have the appearance of obvious crackle and hole.
Claims (2)
1. the method for preparing of glass microfibre reinforcement nano-hydroxyapatite biological composite coating is characterized in that:
1) preparation of nano hydroxyapatite powder
At first, with analytically pure Ca (NO
3)
24H
2O and (NH
2)
2HPO
4By calcium phosphorus mol ratio is 1: 1.50～1.90 mixing, adds dissolved in distilled water then, makes the Ca in the solution
2+Ion concentration is 0.035～0.25mol/L; Again in solution according to Ca (NO
3)
24H
2O and (NH
2)
2HPO
4Gross mass: carbamide=1: 4.6～10.4 add the carbamide powder body and process mixed liquor, stir; Under magnetic agitation, the generation head of multitone chemistry generator is put into above-mentioned mixed liquor, under the ultrasonic power of 100-300w,, be warming up to 70 ℃ of sonochemistry Synthetic 2s hour more respectively synthetic 1.5 hours of 40 ℃ of sonochemistrys; Filter out behind the suspension and clean with distilled water earlier, clean with dehydrated alcohol then, the material that filters out is put into to obtain nano hydroxyapatite powder in 80 ℃ of following dryings in the vacuum drying oven be nanometer HAp;
2) preparation of glass microfiber
Get the staple glass fibre that specification is C – 9, after adding entry and in fiberizer, staple glass fibre being worn into the fibre glass that length range is 5～25 μ m, take out and in 60 ℃～90 ℃ baking oven, dry;
3) get nanometer HAp, analytical pure chitosan and glass microfiber by 10: (1-3): it is 4～13g/L that mass ratio (1-3) is dispersed in the mass concentration that makes nanometer HAp in the analytically pure isopropyl alcohol; Behind magnetic agitation 3～15h, ageing 1～5h gets mixing suspension;
4) C the preparation of substrate
Employing density is 1.7g/cm
32D C/C composite; Cut into 10mm * 10mm * 2mm thin slice; Sand paper with 240#, 600# and 800# places distilled water to clean earlier behind the sanding and polishing successively respectively; After placing the dehydrated alcohol ultrasonic cleaning then, it is dry under 100 ℃ to put into electric drying oven with forced convection, and it is subsequent use that exsiccant bag is put in taking-up;
5) mixing suspension of above-mentioned preparation is poured in the hydro-thermal electrophoresis agitated reactor, compactedness is controlled at 70%, and the C/C substrate is fixed on the negative electrode of hydro-thermal electrophoresis agitated reactor, and is dipped in the suspension; Sealed reactor then; Put it in the exact constant temperature baking oven, in 80 ℃～140 ℃, be incubated 1h, regulation voltage is in 45V～120V scope; Powered-down behind energising deposition 8min～35min; Stop deposition, treat to take out substrate behind the natural cooling, in electric drying oven with forced convection, under 40 ℃, be drying to obtain glass microfibre reinforcement nano-hydroxyapatite biological composite coating.
2. the method for preparing of glass microfibre reinforcement nano-hydroxyapatite biological composite coating according to claim 1 is characterized in that: said specification is that the staple glass fibre of C – 9 adopts east, Chinese Shenyang to ring the staple glass fibre of producing.
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