TWI814496B - 玻璃陶瓷複合材料 - Google Patents
玻璃陶瓷複合材料 Download PDFInfo
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- TWI814496B TWI814496B TW111127436A TW111127436A TWI814496B TW I814496 B TWI814496 B TW I814496B TW 111127436 A TW111127436 A TW 111127436A TW 111127436 A TW111127436 A TW 111127436A TW I814496 B TWI814496 B TW I814496B
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- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000002241 glass-ceramic Substances 0.000 title claims abstract description 26
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 19
- 239000011521 glass Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims 1
- 210000000988 bone and bone Anatomy 0.000 abstract description 17
- 239000000919 ceramic Substances 0.000 abstract description 11
- 230000000593 degrading effect Effects 0.000 abstract 1
- 230000000278 osteoconductive effect Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 19
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 239000000463 material Substances 0.000 description 10
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 238000000227 grinding Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 210000002449 bone cell Anatomy 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910019440 Mg(OH) Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 239000005313 bioactive glass Substances 0.000 description 2
- 239000005312 bioglass Substances 0.000 description 2
- 239000012620 biological material Substances 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 239000012943 hotmelt Substances 0.000 description 2
- 239000007943 implant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000006060 molten glass Substances 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000000735 allogeneic effect Effects 0.000 description 1
- 239000003462 bioceramic Substances 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 229940099112 cornstarch Drugs 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000005297 material degradation process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000963 osteoblast Anatomy 0.000 description 1
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000012890 simulated body fluid Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229940078499 tricalcium phosphate Drugs 0.000 description 1
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 1
- 235000019731 tricalcium phosphate Nutrition 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/40—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L27/42—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix
- A61L27/427—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material having an inorganic matrix of other specific inorganic materials not covered by A61L27/422 or A61L27/425
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/58—Materials at least partially resorbable by the body
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
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Abstract
本發明係關於玻璃陶瓷複合材料，是具降解性與骨傳導的複合材料是由CaO-MgO-SiO
2(CMS玻璃) + CaMgSi
2O
6(CMS陶瓷) 與CaSO
4(CS陶瓷) 所組成，此合成之複合材料除了CaO-MgO-SiO
2玻璃以外，主要還包含結晶相CaMgSi
2O
6以及CaSO
4二個陶瓷，其中，CMS玻璃以及CMS陶瓷皆具有高機械強度、生物相容性和骨傳導性，而CaSO
4具有快速降解以促進骨頭向內生長的特性。
Description
本發明係有關於玻璃陶瓷複合材料，特別係關於一種CaO-MgO-SiO
2玻璃 + CaMgSi
2O
6陶瓷 (簡稱CMS玻璃陶瓷) 及CaSO
4(CS陶瓷) 的複合材料。
現代醫學中，以生醫植入物置入生物體內，取代原有之關節、椎間盤或牙根…等等的醫療行為，已經是相當成熟之技術，因此，各種生醫植入物之結構、材料相關之研究也成了目前生醫領域的發展重點之一。
自體材料 (人骨) 和異體材料 (動物骨) 作為骨移植物的替代品引入最早出現在70年代，然而合成材料 (例如：氫氧機磷灰石，三鈣磷酸鹽，硫酸鈣和生物活性玻璃)，因為成本較低，且可大量生產，具有商業優勢。市面上的生物玻璃由二氧化矽 (SiO
2)、氧化鈣 (CaO)、氧化鈉 (Na
2O)、五氧化二磷(P
2O
5) 組成，在模擬體液解離 (Si
4+, Ca
2+, Na
+, P
5+) 成份刺激新骨的形成，與其他合成材料相比，它還具有更大的與骨骼和軟組織連接的能力。然而做為骨移植物，生物活性玻璃的降解性不夠好，需要搭配降解性較高的生物陶瓷材料 (硫酸鈣) 促進早期成骨細胞新生。
現有的人工骨材中，對於能否提供人骨復原復健的強度，以及是否最終能被人體自行吸收，甚至是能否促進人體的骨細胞分化仍具有需要被克服的問題。
是以，本案發明人在觀察上述議題後，而遂有本發明之產生。
為達上述目的，本發明提供一種具降解性與骨傳導的玻璃陶瓷複合材料，應用於生物體及/或生物材料中，主要包含CaO-MgO-SiO
2玻璃相，CaMgSi
2O
6結晶相以及CaSO
4結晶相，其中，CaMgSi
2O
6結晶相具有高機械強度、生物相容性和骨傳導性，而CaSO
4結晶相具有快速降解以促進骨頭向內生長的特性。
較佳地，CaO-MgO-SiO
2的玻璃合成製程比例與步驟包含：配粉、生粉混合、熔融玻璃及粉末細磨。
較佳地，在配粉步驟中，CaCO
3：Mg(OH)
2：SiO
2= 25:25:50 mol % + 8.5wt% ZrO
2(玻璃陶瓷成核劑)。
在生粉混合步驟中，粉：球：水 (20:60:20 wt%) 混合，轉速180 rpm維持20分鐘，且使用適當篩網過篩，並以170ﾟC烘箱烘乾粉末。
在熔融玻璃步驟中，將溫度設定在1500ﾟC 持溫2小時後將玻璃水淬。
在粉末細磨步驟中，使用打磨機打磨適當時間，以比例粉：球：水 = (13:79:8 wt%) 混合，並細磨到約1μm，再使用篩網過篩，以170ﾟC 烘箱烘乾粉末，完成CaO-MgO-SiO
2玻璃製作。
接下來將本發明複合材料的進行多孔性支架的合成，其比例與步驟如下所述：首先是配製漿料，選擇CaO-MgO-SiO
2(CMS玻璃) 和二水硫酸鈣 (CaSO
4·2H
2O，簡稱CS2H)，依照CMS:CS2H重量比=3:0、2:1、1:1、1:2、0:3共五種比例配置好粉末，並以粉末：水：黏結劑重量比=50:31.2:18.8的比例進行轉子攪拌混合(500rpm, 5min)；接著將海綿浸泡，使用PU材質海綿，以熱熔線將海綿切割成1.5cm
3，並將海綿吸滿漿料，用170ﾟC烘箱將海綿烘乾；最後將海綿以800-1300ﾟC溫度2小時的時間燒結，即完成本發明CaO-MgO-SiO
2玻璃 + CaMgSi
2O
6陶瓷與CaSO
4陶瓷複合材料的進行多孔性支架的合成。
爲使熟悉該項技藝人士瞭解本發明之目的、特徵及功效，茲藉由下述具體實施例，並配合所附之圖式，對本發明詳加說明如下。
本發明玻璃陶瓷複合材料是由CaO-MgO-SiO
2玻璃+CaMgSi
2O
6陶瓷與CaSO
4陶瓷所組成的，應用於生物體及/或生物材料中，由實驗中可以發現，傳統應用於人工骨材的材料CS的優勢在於快速降解以促進骨骼向內生長，而本發明玻璃陶瓷複合材料中的CMS優勢在於高機械強度、高生物相容性和高骨傳導性，本發明將兩種材料進行複合組成玻璃陶瓷複合材料。
本發明具降解性與骨傳導的玻璃陶瓷複合材料，主要包含CMS (CaO-MgO-SiO
2玻璃相+CaMgSi
2O
6結晶相) 以及CS (CaSO
4結晶相)，其中，CaMgSi
2O
6結晶相具有高機械強度、生物相容性和骨傳導性，而CaSO
4結晶相具有快速降解以促進骨頭向內生長的特性。
具體地，CaO-MgO-SiO
2的玻璃合成製程比例與步驟包含：配粉、生粉混合、熔融玻璃及粉末細磨。
具體地，在配粉步驟中，CaCO
3：Mg(OH)
2：SiO
2(25:25:50 mol %)+ 8.5wt% ZrO
2(玻璃陶瓷成核劑)。
在生粉混合步驟中，粉：球：水 (20:60:20 wt%) 混合，轉速180 rpm維持20分鐘，且使用篩網過篩，並以170ﾟC烘箱烘乾粉末。
在熔融玻璃步驟中，將溫度設定在1500ﾟC持溫2小時後將玻璃水淬。
在粉末細磨步驟中，使用打磨機30g/20min，以比例粉：球：水(13:79:8 wt%) 混合，並細磨到約1μm，再使用篩網過篩，以170ﾟC烘箱烘乾粉末，完成CaO-MgO-SiO
2生物玻璃製作。
接下來將本發明複合材料的進行多孔性支架的合成，其比例與步驟如下所述：首先是配製漿料CaO-MgO-SiO
2玻璃和CaSO
4·2H
2O陶瓷，依照CMS:CS2H重量比例=3:0、2:1、1:1、1:2、0:3共五種比例配置好粉末，並以粉末：水：黏結劑=(50:31.25:18.75 wt%)的比例進行漿料調配，經過轉子攪拌混合 (500rpm, 5min)；接著使用PU材質海綿浸泡上述不同比例漿料，以熱熔線將海綿切割成1.5cm
3，並將海綿吸滿漿料，用170ﾟC烘箱將海綿烘乾；最後將浸泡不同比例漿料(CMS:CS2H重量比=3:0、2:1、1:1、1:2 wt)的海綿以900ﾟC溫度2小時的時間燒結，而浸泡漿料(CMS:CS2H重量比= 0:3 wt)的海綿以1100ﾟC溫度1小時的時間燒結，即完成本發明複合材料的進行多孔性支架的合成。
具體地，本發明的複合材料在實驗中的特性與數據如圖1-6所顯示。
在複合材料的孔隙率部分，從圖1中可以看見，當CMS：CS2H的重量比例分別為3:0、2:1、1:1、1:2和0:3的行情下，除了只包含CMS的複合材料之外，其餘比例的複合材料之孔隙率皆大於70%，符合標準。
在複合材料的機械強度部分，從圖2中可以看見，當CMS：CS2H的重量比例分別為3:0、2:1的情形下，具有更好的機械強度。
複合材料降解後的酸鹼值部分，在常理或常規來說，pH值要介於7-8之間是最適合細胞生長的，因此透過圖3可以看見，浸泡於Tris-HCl溶液120小時，本發明的複合材料當CMS：CS2H的重量比例分別為3:0、2:1、1:1、1:2和0:3的形情下，降解後的pH值都位於7-8之間。
在複合材料降解後損失重量的量測部分，若降解損失的重量越多代表離子釋放更多有助於骨細胞的生長，效果越好，從圖4中可以看見，當CMS：CS2H的重量比例分別為3:0、2:1、1:1、1:2和0:3的情形下，本發明在含有CS2H條件下的複合材料明顯具有較大的重量損失，也就是說具有較快的降解速率，可以促進初期骨細胞生長進骨材裡面。
在複合材料降解釋出的離子濃度實驗部分，從圖5及圖6中可以看見，當CMS：CS2H的重量比例分別為3:0、2:1、1:1、1:2和0:3的行情下，複合材料將發展成(CaO-MgO-SiO
2+CaMgSi
2O
6)
x(CaSO
4)
y，簡稱CMS
xCS
y，CMS
xCS
y降解後得到Ca, Mg, Si, S離子，由圖5中得知在極端溶液(citric acid solution)中，CMS玻璃陶瓷的降解性能較低，CMS玻璃陶瓷含有CS硫酸鈣的複合材料降解性較高，而由圖6中得知在Tris-HCl模擬體液中，CMS玻璃陶瓷降解出的離子濃度，含有CS硫酸鈣的複合材料降解性較高。
具體地，玻璃陶瓷複合材料中CMS及CS較佳的重量比例為3:0~1:2之間。
最後，再將本發明的技術特徵及其可達成之技術功效彙整如下：
其一，藉由本發明之玻璃陶瓷複合材料，提高生物相容性。
其二，根據本發明之玻璃陶瓷複合材料，快速降解以促進骨骼向內生長。
其三，根據本發明之玻璃陶瓷複合材料，高機械強度和高骨傳導性。
以上係藉由特定的具體實施例說明本發明之實施方式，所屬技術領域具有通常知識者可由本說明書所揭示之內容輕易地瞭解本發明之其他優點及功效。
以上所述僅為本發明之較佳實施例，並非用以限定本發明之範圍；凡其它未脫離本發明所揭示之精神下所完成之等效改變或修飾，均應包含在下述之專利範圍內。
無
圖1為根據本發明玻璃陶瓷複合材料的特性實驗數據圖；
圖2為根據本發明玻璃陶瓷複合材料的特性實驗數據圖；
圖3為根據本發明玻璃陶瓷複合材料的特性實驗數據圖；
圖4為根據本發明玻璃陶瓷複合材料的特性實驗數據圖；
圖5為根據本發明玻璃陶瓷複合材料的特性實驗數據圖；以及
圖6為根據本發明玻璃陶瓷複合材料的特性實驗數據圖。
Claims (1)
- 一種玻璃陶瓷複合材料，其包含：CaO-MgO-SiO2、CaMgSi2O6以及CaSO4，其中CaO-MgO-SiO2為玻璃相，CaMgSi2O6為結晶相，CaSO4為結晶相，並且其中該玻璃陶瓷複合材料由CaO-MgO-SiO2玻璃和CaSO4．2H2O以2：1、1：1或1：2的重量比經燒結製成。
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|---|---|---|---|
| TW111127436A TWI814496B (zh) | 2022-07-21 | 2022-07-21 | 玻璃陶瓷複合材料 |
| US18/121,342 US20240025800A1 (en) | 2022-07-21 | 2023-03-14 | Glass-ceramic composite material |
| CN202310831587.XA CN117427222A (zh) | 2022-07-21 | 2023-07-07 | 玻璃陶瓷复合材料 |
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|---|---|---|---|
| TW111127436A TWI814496B (zh) | 2022-07-21 | 2022-07-21 | 玻璃陶瓷複合材料 |
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|---|---|
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ID=88965895
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| Country | Link |
|---|---|
| US (1) | US20240025800A1 (zh) |
| CN (1) | CN117427222A (zh) |
| TW (1) | TWI814496B (zh) |
-
2022
- 2022-07-21 TW TW111127436A patent/TWI814496B/zh active
-
2023
- 2023-03-14 US US18/121,342 patent/US20240025800A1/en active Pending
- 2023-07-07 CN CN202310831587.XA patent/CN117427222A/zh active Pending
Non-Patent Citations (1)
| Title |
|---|
| 期刊 Hanxu Zhang,…etc., 〝3D-printed composite, calcium silicate ceramic doped with CaSO4·2H2O:Degradation performance and biocompatibility〞, Journal of the Mechanical Behavior of Biomedical Materials, Vol.121, Available online 13 June 2021, 104642. |
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| Publication number | Publication date |
|---|---|
| CN117427222A (zh) | 2024-01-23 |
| US20240025800A1 (en) | 2024-01-25 |
| TW202404920A (zh) | 2024-02-01 |
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