CN105693095A - Method for preparing diopside-based microcrystal material with aluminum oxide as nucleation agent - Google Patents

Method for preparing diopside-based microcrystal material with aluminum oxide as nucleation agent Download PDF

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Publication number
CN105693095A
CN105693095A CN201610153150.5A CN201610153150A CN105693095A CN 105693095 A CN105693095 A CN 105693095A CN 201610153150 A CN201610153150 A CN 201610153150A CN 105693095 A CN105693095 A CN 105693095A
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diopside
aluminium sesquioxide
nucleation
aluminum oxide
temperature
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张宾杰
王蕾
王祝敏
王国胜
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Shenyang University of Chemical Technology
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Shenyang University of Chemical Technology
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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
    • 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
    • C03C10/0036—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 SiO2, Al2O3 and a divalent metal oxide as main constituents
    • C03C10/0045—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 SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/10—Ceramics or glasses
    • A61L27/105—Ceramics or glasses containing Al2O3
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • 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
    • 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
    • C03C10/0036—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 SiO2, Al2O3 and a divalent metal oxide as main constituents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00—Materials or treatment for tissue regeneration
    • A61L2430/02—Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dermatology (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a method for preparing a diopside-based microcrystal material with aluminum oxide as the nucleation agent and relates to a microcrystal material preparing method. Magnesium nitrate and calcium nitrate are taken as raw materials and aluminum oxide is taken as the nucleation agent to obtain wet gel containing aluminum oxide; the wet gel containing aluminum oxide is dried to obtain dried gel; heat treatment is conducted on the obtained dried gel at different nucleation temperatures, the relationship between nucleation temperature and devitrification temperature is studied, and the optimal nucleation temperature is obtained; at the optimal nucleation temperature, sintering heat treatment is conducted on the dried gel continuously to prepare the diopside-based microcrystal material containing aluminum oxide, and biological activity evaluation is conducted on the prepared material. The preparing method is simple, and energy consumption during sintering can be reduced by taking aluminum oxide as the nucleation agent; the prepared diopside-based microcrystal material is uniform in distribution, hydroxyapatite formation can be induced on the surface after the material is soaked in simulated body fluid, and therefore the material can be applied to the medical field as a bone material.

Description

A kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide
Technical field
The present invention relates to a method preparing micro crystal material, particularly relate to a kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide。
Background technology
China's diopside reserves are very abundant, and distribution is extremely extensive, therefore accelerates the development and utilization to diopside, and the development that ceramics is following is had great strategic significance。All the time, it is the stone material that a kind of value is very low that diopside all be it is believed that, the diopside of unique function is a kind of multifunctional material with broad prospect of application in fact。Such as: as a kind of novel additive for saving energy raw material, diopside can realize the low temperature fast firing of pottery, the physicochemical property of improvement pottery, has significantly high using value。In building industry, the combination property of diopside material is superior to wollastonite；In high frequency porcelain field, diopside porcelain is better than again steatite ceramic。In electronic apparatus industry, owing to diopside base microcrystal glass material has high intensity, wearability, excellent thermal property and electric property, it is widely used in field of power electronics。At biomedical sector, diopside base micro crystal material, owing to having good chemical stability, bio-compatibility or biological activity etc., can be used as dental material, synthetic bone material etc.。Therefore, we should performance and preparation method to diopside and associated materials thereof research and develop further, makes full use of this important mineral resources of diopside。
In recent years, along with going deep into that microcrystal glass material is studied, the preparation method of microcrystal glass material have also been obtained good development, especially sol-gel process。Compared with tradition entirety crystallize method and sintering process, specifically having the advantages of of sol-gel process: 1. can prepare the microcrystal glass material of certain target components that traditional method can not be prepared；2. sol-gel process is reacted from solution, prepared product material high uniformity；3. the material specific surface area that prepared by sol-gel process is big, granule is little, porosity is high, is conducive to the control of sintering and preparation process；4., compared with traditional overall crystallize method and sintering process, sol-gel process heat treatment temperature is low, is conducive to energy-conserving and environment-protective。
Just because of adopting microcrystal glass material prepared by sol-gel process to contain the mesoporous of substantial amounts of 5 ~ 100nm or macropore, its specific surface area is up to ten thousand times with bioactive devitrified glass prepared by crystallize method of entirety, and specific surface area is more big, can be more form amorphous calcium phosphate to provide more ≡ Si-OH one-tenth nuclear space, so the degradation speed of microcrystal glass material prepared of sol-gel process and surface form the speed of hydroxyapatite (HPA) layer also faster, the biological activity having is also higher。It addition, containing substantial amounts of OH in the devitrified glass prepared of sol-gel process-Race, it is possible to form peptide bond by the approach of mental retardation with the protein in living organism, realizes bone bonding quickly, and the biological activity of microcrystal glass material is highly beneficial。Therefore the method is greatly expanded the compositing range with bioactive devitrified glass, and people begin attempt to prepare the microcrystal glass material of different component by sol-gel process, and study its application in biological activity。
Summary of the invention
It is an object of the invention to provide a kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide, the present invention utilizes aluminium sesquioxide as Nucleating Agent, sol-gel process is adopted to prepare diopside base micro crystal material, method is simple, with low cost, reduce the energy resource consumption in sintering process, be conducive to occurring physics and chemisorbed in simulated body fluid, biomedical sector can be applied in as bone material。
It is an object of the invention to be achieved through the following technical solutions:
A kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide, described method includes with magnesium nitrate, calcium nitrate for raw material, and aluminium sesquioxide is Nucleating Agent, adopts sol-gel process to prepare the wet gel containing aluminium sesquioxide；Wet gel containing aluminium sesquioxide is dried to obtain xerogel；By gained xerogel heat treatment under different nucleation temperatures, inquire into the relation of nucleation temperature and recrystallization temperature, obtain the nucleation temperature of the best；Under best nucleation temperature, continue xerogel is sintered heat treatment, prepare the diopside base micro crystal material containing aluminium sesquioxide, and obtained material is carried out Bioactivity evaluations；
Detailed process includes:
(1) preparation of colloidal sol: weigh four water-calcium nitrate, magnesium nitrate hexahydrate, nine water aluminum nitrates, add one by one in flask, add dehydrated alcohol, then stir to being completely dissolved, weigh tetraethyl orthosilicate, dehydrated alcohol, add in there-necked flask one by one, mix homogeneously, the nitrate solution of mixing is slowly dropped in there-necked flask, and stirring obtains colloidal sol；
(2) preparation of gel: prepared colloidal sol ageing is become wet gel, wet gel is dried and obtains xerogel；
(3) preparation of powder body: gained xerogel is sintered into nucleus and pulverizes, and sieves and obtains powder body；
(4) preparation of finished product: by the powder body tabletting after heat treatment, make disk, be placed in heating furnace by disk, heats up and naturally cools to room temperature after being incubated, obtaining the micro crystal material sintered；
(5) configuration simulated body fluid, assess biological activity: preparation simulated body fluid, mix homogeneously is lowered the temperature in a water bath, add water, plastic containers seal, put into refrigerator。
A kind of described method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide, the preparation of described colloidal sol obtains colloidal sol after 60 DEG C of stirred in water bath, dissolving, mixing。
A kind of described method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide, the ageing in the water-bath of 60 DEG C of the colloidal sol being prepared into of described gel, obtain xerogel at 120 DEG C of drying baker inner dryings。
Advantages of the present invention and effect be:
1. the present invention for Nucleating Agent and adopts sol-gal process with aluminium sesquioxide, prepares diopside base micro crystal material。Aluminium sesquioxide is that Nucleating Agent adopts sol-gel process can reduce recrystallization temperature, and the distribution of material prepared is uniform。
2. the present invention reduces recrystallization temperature, it is possible to reduce prepares the energy resource consumption in sintering process at material, and occurs when the distribution of material prepared uniformly is conducive to material to soak in simulated body fluid chemically and physically to adsorb, to induce the formation of hydroxyapatite。
3. the diopside base micro crystal material containing aluminium sesquioxide that the present invention prepares, soaks rear surface in simulated body fluid and can induce the formation of hydroxyapatite, such that it is able to be applied to the biomedical sector of bone material。
4. the present invention is with Nucleating Agent, and magnesium nitrate, calcium nitrate are raw material, and raw material is easy to get, and method is simple, and cost is low。Utilize aluminium sesquioxide can reduce recrystallization temperature as Nucleating Agent, reduce energy consumption；The diopside base micro crystal material structure distribution of preparation is uniform, and there is cavernous structure on surface；After the diopside base micro crystal material containing aluminium sesquioxide of preparation soaks in simulated body fluid, surface can induce hydroxyapatite to be formed。
Accompanying drawing explanation
Fig. 1 is the technology of the present invention route sketch；
Fig. 2 is the XRD figure that xerogel sinters to 1100 DEG C after 650 DEG C of coring process；
The diopside base micro crystal material that Fig. 3 is prepared does not soak front SEM figure；
Fig. 4 is SEM figure after material soaks 11 days in simulated body fluid。
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail。
The ultimate principle of the present invention
Sol-gel process is to have the compound of high chemical active ingredient as presoma, these raw materials are uniformly coordinated under liquid phase, then be hydrolyzed-condensation chemical reaction, just stable vitreosol system is defined in the solution, colloidal sol is aged, is slowly polymerized between gel particle, forms particle space network or the three-dimensional polymer being skeleton with presoma, it is filled with the solvent lost flowability between particle space network, then forms gel；Gel drying, sloughs solvent therebetween and becomes xerogel or the aeroge of a kind of porous space structure；After processing then through sintering curing process heat, prepare the material of molecular level or even nanoscale structures。Its most basic reaction is as follows:
(1) solvation: the metal cation Mz+ of the predecessor that can ionize---slaine attracts hydrone to form solvent unit M (H2O)The valence mumber of M ion (z be), for keeping its ligancy and having the trend of strong release H+。
M(H2O)?M(H2O) n-1(OH) (n-1) ++ H+
(2) hydrolysis: unionized formula molecule predecessor, such as the atomicity that metal alkoxide M (OR) n, n are metal M, R represents alkyl, reacts with water:
M(OR)n+xH2O → M(OH) x(OR) n-x+xROH
Reaction can continue and carry out, until generating M (OH) n。
(3) polycondensation reaction, can be divided into:
Dehydration polycondensation :-M-OH+HO-M → M-O-M-+H2O
Lose alcohol polycondensation :-M-OR+HO-M → M-O-M-+ROH
Reaction product is the sol ion of different size and structure。
Hydroxyapatite (HAP) is to grow up the eighties in 20th century, is used clinically for dentistry and the novel of orthopaedics fills up graft materials。Owing to the chemical composition of hydroxyapatite and crystal structure and people's bone are essentially identical, and new bone growth can be brought out, therefore there is good biological activity and biocompatibility, implanting in human body and can carry out chemical bond with when injected organism tissue and be replaced by when injected organism tissue gradually, its powder can be used as the material for repairing at Cranial defect position。
Porous material can simulate the organizational structure of human bone well, in the porosity of bone, pore-size and through situation etc., it is thus possible to meet the requirement of porous bone tissue renovation material。The type material developed is expected to be more conducive to growing into of blood vessel, cell, osseous tissue etc. after implanting。
Microcrystal glass material prepared by sol-gel process is adopted to contain the mesoporous of substantial amounts of 5 ~ 100nm or macropore, its specific surface area is up to ten thousand times with bioactive devitrified glass prepared by crystallize method of entirety, and specific surface area is more big, can be more form amorphous calcium phosphate to provide more ≡ Si-OH one-tenth nuclear space, so the degradation speed of microcrystal glass material prepared of sol-gel process and surface form the speed of hydroxyapatite (HAP) layer also faster, the biological activity having is also higher。
The basic scheme of the present invention
The first step, with magnesium nitrate, calcium nitrate for raw material, aluminium sesquioxide is Nucleating Agent, adopts sol-gel process to prepare the wet gel containing aluminium sesquioxide；Second step, is dried to obtain xerogel by the wet gel containing aluminium sesquioxide；3rd step, by gained xerogel heat treatment under different nucleation temperatures, inquires into the relation of nucleation temperature and recrystallization temperature, obtains the nucleation temperature of the best；4th step, under best nucleation temperature, continues xerogel is sintered heat treatment, prepares the diopside base micro crystal material containing aluminium sesquioxide, and obtained material is carried out Bioactivity evaluations。
The technical method of the present invention
The present invention is with aluminium sesquioxide for Nucleating Agent, and magnesium nitrate, calcium nitrate are raw material, adopts sol-gal process to prepare the diopside base micro crystal material containing aluminium sesquioxide。After soaking in simulated body fluid, surface defines hydroxyapatite, have evaluated its biological activity, it is possible to be applied to biomedical sector as bone material。
Specific embodiment of the present invention
(1) preparation of colloidal sol
1. accurately weigh four water-calcium nitrate 21.58g, magnesium nitrate hexahydrate 23.52g, nine water aluminum nitrate 0.54g respectively, add one by one in the single port flask of 500ml, add 21mL dehydrated alcohol, in 60 DEG C of water-baths, then heat magnetic agitation to being completely dissolved。
2. distinguish precise tetraethyl orthosilicate (TEOS) 38.5g, dehydrated alcohol 21mL, add in the there-necked flask of 500ml one by one, electric stirring 0.5h, mix homogeneously in the water-bath of 60 DEG C。
3. by mixed uniformly nitrate solution dislocation bulb shape separatory funnel on there-necked flask in 1., by controlling the rotary-piston of separatory funnel, making the solution in separatory funnel be slowly dropped in there-necked flask, its process is maintained under 60 DEG C of water bath condition along with constantly stirring, backflow。After completion of dropwise addition, now pH value is about 2 ~ 3, and the mixed solution dislocation in there-necked flask continues stirring in the beaker of 250ml, until solution becomes slightly thickness, stops stirring, obtains colloidal sol。
(2) preparation of gel
1. by obtained colloidal sol ageing 48h in the water-bath of 60 DEG C, wet gel is formed。
2. then by the wet gel air dry oven inner drying 10h at 120 DEG C, xerogel is obtained。
(3) preparation of powder body
Gained xerogel Muffle furnace is calcined 2h (formation nucleus) respectively at different temperatures, and taking-up agate mortar is pulverized, and crosses 120 mesh sieves, obtains the powder body after different pre-nucleation temperature heat treatment。
(4) preparation of finished product
1. powder body after pre-for difference nucleation temperature heat treatment is used respectively tablet machine at 30MPa lower sheeting, makes the disk that diameter is Φ 26mm × 5mm。
2. disk is placed in temperature programming stove, is to slowly warm up to 600 DEG C of insulation 2h with the speed of 10 DEG C/min, is continuously heating to 1100 DEG C afterwards and is incubated 1h, naturally cooling to room temperature subsequently, obtaining the micro crystal material sample sintered。
(5) configuration simulated body fluid, assesses biological activity。
Simulated body fluid (SBF) is prepared according to the method reported such as TadashiKokubo。
First, the plastic beaker of 1000ml adds the distilled water of 700ml, and puts into magnetic rotor, cover vinyl cover, with heat collecting type constant-temperature heating magnetic stirring apparatus, the distilled water in plastic beaker is heated to 36.5 ± 1.5 DEG C。Then, maintain the temperature at 36.5 ± 1.5 DEG C, the medicine in table 1 is pressed sequence number from 1 to 8 successively pass into solution, do not dissolve several reagent chemicals simultaneously, re-dissolved after being completely dissolved will be waited next。After front 8 medicines have dissolved, the adjustment solution that adds water is to 900ml, and ensures that solution temperature is at about 36.5 DEG C, is then inserted in solution by the test electrode of pH meter, and now pH value is 2.0。Finally, it is gradually added into No. 9 (trishydroxymethylaminomethane) and No. 10 (a small amount of HCl) medicines, for constantly regulating the pH value of solution, until Tris(trishydroxymethylaminomethane) be completely dissolved, solution is finally 7.40 at 36.5 DEG C of accurate pH value, and ensures that solution temperature fluctuates less than 0.1 DEG C/min。Take out the electrode of pH meter and rinse, flushed water is added solution。Pouring the solution after adjusting the volumetric flask of 1000ml into, scrub previous container with water, point will scrub solution several times and pour volumetric flask into, add water constant volume line, cover lid。After solution mix homogeneously in volumetric flask, being cooled to 20 DEG C in a water bath, then add water volumetric flask graduation mark。Plastic containers seal, and put into the refrigerator of 5 ~ 10 DEG C, are finished in 30 days。
The medicine needed for 1000ml simulated body fluid prepared by table 1
。

Claims (3)

1. the method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide, it is characterized in that, described method includes with magnesium nitrate, calcium nitrate for raw material, and aluminium sesquioxide is Nucleating Agent, adopts sol-gel process to prepare the wet gel containing aluminium sesquioxide；Wet gel containing aluminium sesquioxide is dried to obtain xerogel；By gained xerogel heat treatment under different nucleation temperatures, inquire into the relation of nucleation temperature and recrystallization temperature, obtain the nucleation temperature of the best；Under best nucleation temperature, continue xerogel is sintered heat treatment, prepare the diopside base micro crystal material containing aluminium sesquioxide, and obtained material is carried out Bioactivity evaluations；
Detailed process includes:
(1) preparation of colloidal sol: weigh four water-calcium nitrate, magnesium nitrate hexahydrate, nine water aluminum nitrates, add one by one in flask, add dehydrated alcohol, then stir to being completely dissolved, weigh tetraethyl orthosilicate, dehydrated alcohol, add in there-necked flask one by one, mix homogeneously, the nitrate solution of mixing is slowly dropped in there-necked flask, and stirring obtains colloidal sol；
(2) preparation of gel: prepared colloidal sol ageing is become wet gel, wet gel is dried and obtains xerogel；
(3) preparation of powder body: gained xerogel is sintered into nucleus and pulverizes, and sieves and obtains powder body；
(4) preparation of finished product: by the powder body tabletting after heat treatment, make disk, be placed in heating furnace by disk, heats up and naturally cools to room temperature after being incubated, obtaining the micro crystal material sintered；
(5) configuration simulated body fluid, assess biological activity: preparation simulated body fluid, mix homogeneously is lowered the temperature in a water bath, add water, plastic containers seal, put into refrigerator。
2. a kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide according to claim 1, it is characterised in that the preparation of described colloidal sol obtains colloidal sol after 60 DEG C of stirred in water bath, dissolving, mixing。
3. a kind of method preparing diopside base micro crystal material for Nucleating Agent with aluminium sesquioxide according to claim 1, it is characterised in that the colloidal sol being prepared into of described gel ageing in the water-bath of 60 DEG C, obtains xerogel at 120 DEG C of drying baker inner dryings。
CN201610153150.5A 2016-03-17 2016-03-17 Method for preparing diopside-based microcrystal material with aluminum oxide as nucleation agent Pending CN105693095A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108853580A (en) * 2017-05-08 2018-11-23 北京幸福益生高新技术有限公司 A kind of preparation method of bonding and the regenerative medicine material for repairing Bone and soft tissue
CN111944336A (en) * 2020-08-07 2020-11-17 齐鲁工业大学 Coating for improving cracking resistance of glass surface and preparation method and application thereof

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Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN1403414A (en) * 2002-09-28 2003-03-19 中国科学院上海硅酸盐研究所 Prepn process of degradeable bioactive porous active calcium silicate ceramic material
CN103170010A (en) * 2013-04-15 2013-06-26 安徽工业大学 Method for preparing diopside coating on titanium alloy surface by sol-gel method

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108853580A (en) * 2017-05-08 2018-11-23 北京幸福益生高新技术有限公司 A kind of preparation method of bonding and the regenerative medicine material for repairing Bone and soft tissue
CN111944336A (en) * 2020-08-07 2020-11-17 齐鲁工业大学 Coating for improving cracking resistance of glass surface and preparation method and application thereof

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Application publication date: 20160622