CN105622081B - A kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic - Google Patents
A kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic Download PDFInfo
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- CN105622081B CN105622081B CN201511026609.7A CN201511026609A CN105622081B CN 105622081 B CN105622081 B CN 105622081B CN 201511026609 A CN201511026609 A CN 201511026609A CN 105622081 B CN105622081 B CN 105622081B
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/22—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in calcium oxide, e.g. wollastonite
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- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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Abstract
The present invention relates to a kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic, the preparation method includes the following steps：In mass ratio 0:100~30:70 weigh silicon dioxide gel and calcium silicate powder, add binding agent, are uniformly mixed, dry aftershaping obtains ceramic body；It is normal pressure-sintered in 800~1300 DEG C of progress to obtained ceramic body, obtain calcium silicates ceramics.It is provided by the invention using silicon dioxide gel as the calcium silicates bioceramic sintering temperature that sintering aid is prepared is low, porosity is low, mechanical property is good.
Description
Technical field
The present invention relates to a kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic, belong to raw
The preparation field of thing ceramics.
Background technology
Bone tissue is connective tissue most hard in human body, is played the role of when maintaining matrix function irreplaceable.So
And since bone defect and disease caused by the reasons such as wound, tumour, congenital abnormality, aging, injury gained in sports and accident are bones
Section's common sympton is, it is necessary to which substantial amounts of bone renovating material is cured and repaired.China is the most country of world population, and bone is repaiied
Multiple material has huge demand.Calcium silicates because it is with excellent bioactivity, biological degradability and biocompatibility, by regarding
For the third generation degradative bioactive material with researching value and application prospect.
Because of its above-mentioned excellent biological property, research of the people to calcium silicates also more to be focused in terms of bioactivity, and right
Its sintering character, the research of mechanical performance are few.Calcium silicates ceramics are prepared with traditional sintering method, even in very high temperature
Under also hard-to-sinter it is fine and close.The defects of this hard-to-sinter, poor mechanical property, greatly limit it and be given birth in biomaterial especially load-bearing
Application in thing Material Field.Though prepare fine and close calcium silicates using discharge plasma sintering process to improve to a certain extent
Mechanical property, increase consistency, but this process conditions are of high cost, and the crystallite dimension finally obtained is generally large.As can adopt
With traditional normal pressure-sintered calcium silicates prepared mechanical property and increased substantially, this by calcium silicates in technical field of biological material
Using hewing out new world.
The content of the invention
In view of the problems of the existing technology and demand, the purpose of the present invention is pass through simple, the of low cost side of technique
Method prepares low porosity, good mechanical performance and the calcium silicates bioceramic material applied suitable for biological load-bearing.
The present invention provides a kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic, the system
Preparation Method includes the following steps：
A) in mass ratio 0:100~30:70 weigh silicon dioxide gel and calcium silicate powder, add binding agent, and mixing is equal
Even, dry aftershaping obtains ceramic body；
B) it is normal pressure-sintered in 800~1300 DEG C of progress to obtained ceramic body, obtain calcium silicates ceramics.
Compared with prior art, it is provided by the invention to be given birth to by the calcium silicates that sintering aid is prepared of silicon dioxide gel
Thing ceramic sintering temperature is low, porosity is low, and mechanical property is good.Calcium silicates ceramics bending strength prepared in accordance with the present invention is up to
186.6MPa, the perforate porosity as low as 3.7%.On the basis of conventional atmospheric sintering process defect is overcome, solves calcium silicates
The problem of bioceramic hard-to-sinter, poor mechanical property.
It is preferred that the calcium silicate powder is β phase calcium silicate powders.
It is preferred that in step a), the mass percent shared by the silicon dioxide gel is 1~10wt%, the silicic acid
Mass percent shared by calcium powder body is 99~90wt%.
It is preferred that in step a), the binding agent is organic binder bond, is preferably alcohol based binder, and additive amount accounts for powder
The 0~5% of body total amount.
It is preferred that in step a), using alcohol as ball-milling medium, ball milling mixing is uniform, it is preferable that powder mixture, ball milling
Medium, the mass ratio of abrading-ball are (1~3)：(2~6)：(3~6), when Ball-milling Time is 2~12 small.
It is preferred that in step b), molding mode is dry-pressing and isostatic cool pressing.
It is preferred that in step b), 800 DEG C are warming up to 5~10 DEG C/min, then final burning is warming up to 1~5 DEG C/min
Junction temperature, temperature-fall period are furnace cooling.
It is preferred that in step b), final sintering temperature is 900~1200 DEG C, is preferably 1000~1150 DEG C, soaking time
For 30 minutes~5 it is small when, be preferably 1~4 it is small when.
The present invention provides a kind of simple, the of low cost method of technique, it can prepare that porosity is low, mechanical property is excellent
It is different, and suitable for the silicic acid calcium ceramic material of biological load-bearing application.The present invention uses normal pressure-sintered technique, molten using silica
Glue is sintering aid, has obtained that porosity is low, the calcium silicates ceramics of high mechanical properties.Meanwhile the present invention uses normal pressure-sintered temperature
Spend low, raw material sources enrich.It is a kind of method for being suitable for preparing strong mechanical performance calcium silicates bioceramic material on a large scale.
Brief description of the drawings
Fig. 1：Calcium silicates bioceramic cross-section morphology figure made from embodiment 1；
Fig. 2：Calcium silicates bioceramic cross-section morphology figure obtained by comparative example；
Fig. 3：Calcium silicates bioceramic cross-section morphology figure made from embodiment 2；
Fig. 4：Calcium silicates bioceramic cross-section morphology figure made from embodiment 3；
Fig. 5：Calcium silicates bioceramic cross-section morphology figure made from embodiment 4.
Embodiment
Lower combination attached drawing and following embodiments further illustrate the present invention, it should be appreciated that attached drawing and following embodiments are only
For illustrating the present invention, it is not intended to limit the present invention.
The present invention provides a kind of preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic.Using two
Silica is sintering aid, calcium silicates is principal phase, adds binding agent, and uniformly, after shaping normal pressure-sintered system is carried out through ball milling mixing
It is standby and obtain.It is sintering aid by using silicon dioxide gel, the silica energy added in liquid form in blending process
More uniformly mixed with calcium silicate powder；After mixed powder shaping after drying in sintering range, it may occur that unformed
Crystallization and phase transition process of the silica dioxide gel to silica crystals；This chemical transformation to be dispersed in calcium silicate powder
Silica in body has good activity, so that the sintering process between promoting calcium silicate particle, promotes densification, prepare
Porosity is low, excellent in mechanical performance, and suitable for the silicic acid calcium ceramic material of biological load-bearing application.
As calcium silicate powder, commercialization can be purchased from, can also voluntarily be prepared.Its preparation method for example can be：Respectively
The sodium metasilicate and calcium nitrate solution of same concentrations are prepared, sodium silicate solution is added dropwise in calcium nitrate solution and stirred obtains silicon
Sour calcium suspension.Suspension is filtered respectively 2~3 times, disperseed with distilled water, absolute ethyl alcohol by the way of vacuum filtration
The white solid of free from admixture.White solid is placed in 80 DEG C of baking ovens and keeps the temperature 12h, obtains white powder.White powder is put into
2~3h is calcined in Muffle furnace under the conditions of 800 DEG C, finally obtains calcium silicate powder.Obtained calcium silicate powder is β phase calcium silicates
Powder.By using β phase calcium silicate powders, it is better than other phases because β phases obtain mechanical property, such as α phases, it is ensured that final sample has
There is the mechanical property of higher.In addition, the particle diameter of calcium silicate powder can be 0.5~2 μm, in this particle size range, β phase powders both had
There is certain activity, and can be mixed uniformly with second.
The particle diameter of silica can be 10~20nm in silicon dioxide gel, in this particle size range, silicon dioxide granule
Active higher, can more promote the sintering of ceramic particle.
By silicon dioxide gel with and calcium silicate powder mix when, the mass percent of the two can be 0:100~30:70,
Preferably, the mass percent shared by silicon dioxide gel is 1~10wt, the mass percent shared by calcium silicate powder for 99~
90wt%.It is highly preferred that in the range of 1~5wt%, the mass percent shared by silicon dioxide gel is the higher the better.With
The increase of silicon dioxide gel additive amount, has more amorphous silicas to be changed into crystalline silicon dioxide and phase turn occurs
Become, so as to can more promote the sintering character between calcium silicate particle.If but silicon dioxide gel adding too much, in ceramic matrix
Silica volume is more, and the thermal coefficient of expansion and calcium silicates difference of thermal expansion coefficients of silica are larger, can be led in sintering process
Ceramic particle is caused to crack because shrinking uneven, stomatal number increases in ceramic matrix, so as to influence the mechanical property of calcium silicates ceramics.
It is preferably organic binder bond as binding agent, such as the alcohol based binders such as polyvinyl butyral resin can be used.
The additive amount of binding agent can account for the 0~5% of powder total amount, be preferably 0~2%.Binding agent can add as a solution, its
Concentration may be, for example, 1~7%.
In one example, silicon dioxide gel and calcium silicate powder are weighed by proportioning, using alcohol as ball-milling medium, added
Organic binder bond, ball milling mixing is uniform, and drying, obtains finely dispersed silica dioxide gel/calcium silicate powder mixture.Abrading-ball
Planetary ball mill can be used.Powder, ball-milling medium, the mass ratio of abrading-ball can be (1~3)：(2~6)：(3~6).Ball-milling Time can
For 2~12 it is small when.
After powder mixture is made, make powder mixing body formed.In one preferred embodiment, to mixed powder into
Row dry-pressing, isostatic cool pressing obtain ceramic body.It is molded by using such mode, can makes green compact that there is certain intensity.
It is it should be understood that also possible using other common molding modes.
Carried out after shaping normal pressure-sintered.It can be that final sintering temperature is warming up to 5~10 DEG C/min, or can also be
A certain medium temperature (such as 800 DEG C) is warming up to 5~10 DEG C/min, then final sintering temperature is warming up to 1~5 DEG C/min.
Temperature-fall period can be furnace cooling.In one example, final sintering temperature is 800~1300 DEG C, and soaking time is 30 minutes
~5 it is small when.In a preferable example, final sintering temperature is 900~1200 DEG C, when soaking time is 1~4 small.One
In a preferred example, final sintering temperature is 1000~1150 DEG C, and in this temperature range, silicon dioxide gel is as burning
Knot auxiliary agent can give full play to its effect, can fully be sintered between ceramic particle and crystallite dimension will not be because of temperature mistake
It is high and excessive.
Test result indicates that：Calcium silicates bioceramic three-point bending resistance intensity prepared by the present invention is up to 186.6MPa, opens
The hole porosity as low as 3.7%.Compared to the calcium silicates bioceramic prepared under similarity condition, the porosity is decreased obviously, bending resistance is strong
Degree significantly improves.Solve hard-to-sinter, poor mechanical property under calcium silicates normal pressure by adding silicon dioxide gel for sintering aid
The problem of.The preparation method has the characteristics that preparation process is simple, technique is controllable, cost is low, can significantly extend calcium silicates in bone
Substitute the application in terms of bioceramic.Therefore, the calcium silicates ceramics prepared by the present invention can be applied to technical field of biological material.
Embodiment is enumerated further below so that the present invention will be described in detail.It will similarly be understood that following embodiments are served only for this
Invention is further described, it is impossible to is interpreted as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary concrete numerical value.
Embodiment 1
1 is pressed first:99:100 proportionings weigh silicon dioxide gel (solid-liquid mass percent 30%, Shanghai Ha Lingsheng respectively
Thing Science and Technology Ltd.), calcium silicate powder, absolute ethyl alcohol, and add suitable alcohol-based polyvinylbutyral binder.OK
When celestial body mill 3 is small, dispersed mixed powder is made；Then when drying 3 is small at 50~80 DEG C, sieving, obtains powder and mixes
It is fit；Obtained powder is subjected to dry-pressing again, isostatic pressed handles to obtain the strip that length is 3 × 4 × 40mm.By strip
It is put into alumina crucible and carries out normal pressure-sintered, when 1100 DEG C of insulations 3 are small, that is, it is 1% that silicon dioxide gel additive amount, which is made,
Calcium silicates ceramics.
The microscopic appearance of calcium silicates bioceramic obtained by the present embodiment is as shown in Figure 1.The ceramic physical property with
Mechanical property is shown in Table 1.Wherein bending strength uses three-point bending method (Instron 5566, INSTRON, Norwood, MA)
Test, sintering shrinkage using measurement sintering before and after ceramics sample change in size be calculated, test, the perforate porosity using Ah
Base Mead drainage (national standard GB-T 1966-1996) is tested.In contrast to not adding silicon dioxide gel, calcium silicates ceramics pattern
Too big difference is had no, the perforate porosity is declined slightly, and bending strength also slightly increases.Illustrate that silica additive amount is very few to silicon
The pattern and bending strength of sour calcium bioceramic influence not notable.
Comparative example
This comparative example is differed only in embodiment 1：Be free of silicon dioxide gel in raw material, remaining content with implementation
It is identical shown in example 1.Calcium silicates bioceramic obtained by this comparative example to surround and watch pattern as shown in Figure 2.Obtained by this comparative example
Calcium silicates ceramics strength be 41.1MPa, the perforate porosity is 31.7%.
Embodiment 2
5 are pressed first:95:100 proportionings weigh silicon dioxide gel (solid-liquid mass percent 30%, Shanghai Ha Lingsheng respectively
Thing Science and Technology Ltd.), calcium silicate powder, absolute ethyl alcohol, suitable binding agent.When planetary ball mill 3 is small, it is made dispersed
Mixed powder；Then when drying 3 is small at 50~80 DEG C, sieving, obtains powder mixture；Obtained powder is done again
Pressure, isostatic pressed handle to obtain the strip that length is 3 × 4 × 40mm.Strip is put into progress normal pressure burning in alumina crucible
Knot, when 1100 DEG C of insulations 3 are small, that is, is made the calcium silicates ceramics that silicon dioxide gel additive amount is 5%.
The microscopic appearance of calcium silicates ceramics obtained by the present embodiment is as shown in Figure 3.The ceramic physical property and mechanics
Performance is shown in Table 1.As can be seen from the figure with the increase of silica additive amount, densification degree rise, crystallite dimension
Also bigger, the perforate porosity significantly reduces, and bending strength significantly increases, its bending strength is up to 186.6MPa.
Embodiment 3
5 are pressed first:95:100 proportionings weigh silicon dioxide gel (solid-liquid mass percent 30%, Shanghai Ha Lingsheng respectively
Thing Science and Technology Ltd.), calcium silicate powder, absolute ethyl alcohol, suitable binding agent.When planetary ball mill 3 is small, it is made dispersed
Mixed powder；Then when drying 3 is small at 50~80 DEG C, sieving, obtains powder mixture；Obtained powder is done again
Pressure, isostatic pressed handle to obtain the strip that length is 3 × 4 × 40mm.Strip is put into progress normal pressure burning in alumina crucible
Knot, when 1150 DEG C of insulations 3 are small, that is, is made the calcium silicates ceramics that silicon dioxide gel additive amount is 5%.
The microscopic appearance of calcium silicates ceramics obtained by the present embodiment is as shown in Figure 4.The ceramic physical property and mechanics
Performance is shown in Table 1.Comparative example 2 understands that sintering temperature is higher, and ceramic crystalline grain size is bigger, and pattern is finer and close, but bending resistance
Intensity declines, this is because big crystallite dimension reduces the bending strength of ceramics.
Embodiment 4
10 are pressed first:90:100 proportionings weigh silicon dioxide gel (solid-liquid mass percent 30%, Shanghai Ha Lingsheng respectively
Thing Science and Technology Ltd.), calcium silicate powder, absolute ethyl alcohol, and add suitable binding agent.When planetary ball mill 3 is small, it is made uniform
Scattered mixed powder；Then when drying 3 is small at 50~80 DEG C, sieving, obtains powder mixture；Again by obtained powder
Carry out dry-pressing, isostatic pressed handles to obtain the strip that length is 3 × 4 × 40mm.Strip is put into alumina crucible and is carried out
It is normal pressure-sintered, when 1100 DEG C of insulations 3 are small, that is, the calcium silicates ceramics that silicon dioxide gel additive amount is 10% are made.
The microscopic appearance of calcium silicates ceramics obtained by the present embodiment is as shown in Figure 5.The ceramic physical property and mechanics
Performance is shown in Table 1.Comparative example 3 understands that silicon dioxide gel additive amount is excessive, can exist on the contrary in ceramic matrix more
Stomata, and ceramic crystalline grain size bigger, thus bending strength is lower.
The physical property and mechanical property of the ceramics of table 1
Industrial applicability：The preparation method of the present invention has the characteristics that preparation process is simple, technique is controllable, cost is low, can
Significantly application of the extension calcium silicates in terms of bone substitutes bioceramic.
Claims (9)
- A kind of 1. preparation method using silicon dioxide gel as sintering aid calcium silicates bioceramic, it is characterised in that the system Preparation Method includes the following steps：a）Weigh silicon dioxide gel and calcium silicate powder, the mass percent shared by the silicon dioxide gel for 1~ 10wt%, the mass percent shared by the calcium silicate powder are 99~90wt%, add binding agent polyvinyl butyral resin, mixing Uniformly, dry aftershaping obtains ceramic body；b）It is normal pressure-sintered in 800~1300 DEG C of progress to obtained ceramic body, calcium silicates ceramics are obtained, obtained calcium silicates pottery The bending strength of ceramic material is up to 186.6MPa, the perforate porosity as low as 3.7%.
- 2. preparation method according to claim 1, it is characterised in that the calcium silicate powder is β phase calcium silicate powders.
- 3. preparation method according to claim 1, it is characterised in that step a）In, the additive amount of the binding agent accounts for powder The 0~5% of body total amount.
- 4. preparation method according to claim 1, it is characterised in that step a）In, using alcohol as ball-milling medium, ball milling It is uniformly mixed.
- 5. preparation method according to claim 4, it is characterised in that powder mixture, ball-milling medium, the mass ratio of abrading-ball For（1~3）：（2~6）：（3~6）, when Ball-milling Time is 2~12 small.
- 6. preparation method according to claim 1, it is characterised in that step b）In, molding mode is dry-pressing and cold etc. quiet Pressure.
- 7. preparation method according to claim 1, it is characterised in that step b）In, it is warming up to 800 with 5~10 DEG C/min DEG C, then final sintering temperature is warming up to 1~5 DEG C/min, temperature-fall period is furnace cooling.
- 8. preparation method according to any one of claim 1 to 7, it is characterised in that step b）In, final sintering temperature For 900~1200 DEG C, when soaking time is 30 minutes~5 small.
- 9. preparation method according to claim 8, it is characterised in that step b）In, final sintering temperature for 1000~ 1150 DEG C, when soaking time is 1~4 small.
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| CN115196953A (en) * | 2021-04-12 | 2022-10-18 | 中国科学院上海硅酸盐研究所 | In-situ rod-shaped crystal self-toughening porous calcium silicate biological ceramic and preparation method thereof |
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| CN1686793A (en) * | 2005-04-08 | 2005-10-26 | 中国科学院上海硅酸盐研究所 | Method for preparing porous bracket of calcium silicate |
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