CN109678524A - A kind of silicon nitride ceramics implantation material and preparation method thereof that performance is controllable - Google Patents
A kind of silicon nitride ceramics implantation material and preparation method thereof that performance is controllable Download PDFInfo
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Abstract
The present invention relates to a kind of silicon nitride ceramics implantation materials and preparation method thereof that performance is controllable, and the raw material components of implantation material include silicon nitride and additive；Additive includes the first additive, Second addition and third additive；First additive is selected from one of magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride or a variety of mixtures；Second addition is selected from one of erbium oxide, thulium oxide, ytterbium oxide and three two lutetiums of oxidation or a variety of mixtures；Third additive is selected from one of praseodymium oxide, samarium oxide, ceria, neodymium oxide and titanium oxide calcium or a variety of mixtures.Implantation material outer layer provided by the invention is opposite based on alpha phase silicon nitride, internal opposite based on beta phase silicon nitride, so that it is hard to reach appearance, internal tough effect, hardness and wearability can be improved and improve its fracture toughness and intensity, resist crackle and reduce the risk accordingly destroyed.
Description
Technical field
The present invention relates to bio-medical implantation material technical field, in particular to a kind of silicon nitride ceramics that performance is controllable implantation
Object and preparation method thereof.
Background technique
It is some relevant to prosthetic material to ask although artificial joint replacement is one of most successful surgical intervention operation
Topic is not finalized yet.According to the data of 2018 annual report of joint replacement Register, the U.S., revision procedure more than 70%
Reason is bone dissolution, is worn, infection, aseptic loosening and dislocation.And it is overhauled in reason above-mentioned, articular surface used in prosthese
The quantity of material and its wear particle, size and biological effect have conclusive effect.
In industrialized country in the world, quick and anaphylactoid incidence super to metal is increasing.Receive
The patient of the metal to metal Using prosthesis secondary as friction, a possibility that metal is super quick occurs in they can not be complete in the preoperative
It is complete to exclude.And postoperative inspection and diagnosis to metal allergy, increase additional burden to patient and medical insurance person.Therefore, it adopts
The ceramic implants material being excellent in used in vivo biodistribution compatibility just seems even more important.
Discovered in recent years simultaneously, the corrosion of bulb-handle cone junction is one for influencing artificial full hip-joint replacement result
Major reason, and the severity of this corrosion is determined by many factors.There is increasing evidence that except can be reduced poly- second
Outside alkene or high crosslinked polyethylene joint surface wear, ceramic bulb also functions to most important in the metal erosion for mitigating handle cervical vertebra portion
Effect, and itself then never corrodes.
Fretting wear and the above-mentioned bone referred to since the functional characteristic of joint prosthesis makes so, between each component part
Dissolution, joint instability, hypersensitivity, joint liquid-film lubrication and handle taper thread grinding damage etc. are studied to be proved to be the influence orthopaedics implant service life
And the key factor of operation success or failure, and biomedical ceramics investment orthopaedics market is during the last ten years, verifies through clinical effectiveness, ceramics
Implantation material is the ideal substitution of conventional metals or high molecular material implantation material.
In bio-medical type ceramic field, mainly there is aluminium oxide ceramics (being commonly called as yellow pottery) at present, zirconia ceramics (is commonly called as white
Pottery) and Zirconium oxide plasticizing aluminium oxide ceramics (be commonly called as powder make pottery).But the main problem of Huang pottery is that its toughness is lower, to be easy
Fragmentation.
The toughness ratio Huang Taohao of white pottery, but zirconium oxide is a kind of metastable phase material, ageing of performance is a significant scarce
It falling into, the aging of zirconium oxide refers to that tetragonal phase leads to rough surface from monoclinic phase transformation, volume expansion in transition process is sent to, from
And increase abrasion, in addition, micro-crack even macroscopic cracking can be generated, it is remarkably decreased material mechanical performance.
Powder pottery is the upgrading products of yellow pottery, toughening mechanism first is that oxygen using disperse in stable alumina substrate
Change the stable nanometer grade tetragonal zirconia particles (Y-TZP) of yttrium.This Y-TZP crystal dispersed distribution, it is possible to reduce structure changes,
Potential crack propagation can be prevented simultaneously.Another enhancing mechanism is the strontium oxide strontia and oxygen that platelike crystal is formed by adding
Change chromium to realize.This platelike crystal consumes energy when stopping crackle, improves the intensity and toughness of powder pottery.It is either logical
The powder pottery of crossing transformation toughening or platelike crystal toughening is all to improve toughness by addition impurity, is especially added to
10%~30% zirconium oxide has the problem of aging, and aging gradually internally develops generally since surface, in wet condition
Aging is more serious, and in human body under complicated physiological environment, what kind of variation is performance have, and still not can determine that at present is
No is intracorporal time bomb.In spite of the marketing energetically of trade monopoly giant Germany Sai Lang Tyke (CeramTec) company, face
Still having the report of powder pottery failure on bed can be disclosed out.
From the point of view of the development trend of structural ceramics, the silicon nitride ceramics for being known as the all-round champion of ceramics is final liter
Grade, which is regenerated, to be selected, and silicon nitride ceramics not only possesses all known advantages of above-mentioned general ceramic implants, while compared to aforementioned
Three kinds of oxide ceramics, also possess unrivaled advantage, especially as bio-medical type ceramics.
Every mechanical performance index of silicon nitride ceramics implantation material is better than oxide ceramics currently on the market, has
High rigidity, high bending strength, excellent frictional behaviour, especially fracture toughness are increased substantially, and furthermore silicon nitride is made
For a kind of chemically stable material, there is no the problem of aging of zirconium oxide, and also there is the long upper and Bone Ingrowth ability of good bone (to be formed
The ability of biological fixation) and anti-infection ability and good developability.
Currently, domestic ceramic implants are mainly or based on aluminium oxide ceramics and zirconia ceramics, it is only minimal amount of
Work starts to be related to more excellent performance of silicon nitride ceramics, and there are no silicon nitride ceramics implantation materials to put goods on the market up to now,
Corresponding material application study is also in bio-medical implantation material field with respect to early stage, by retrieval, is related to silicon nitride
The patent of ceramic bulb only has following two.
Patent CN103435356B (2013-08-09 application, 2015-02-11 authorization) disclose a kind of gel casting at
The method that type, pressureless sintering prepare silicon nitride Artificial Ceramic joint.The invention be by two kinds of granularity d50 0.2 μm~0.9 μm it
Between different-grain diameter submicron order α-siliconnitride and dopant be mixed in a certain ratio, then through gel casting moulding process, row
Glue, sintering, polishing and surface polishing have obtained bending strength greater than 700MPa, and fracture toughness is greater than 6MPam1/2, volume abrasion
Rate is less than 1mm3The Artificial Ceramic joint in/1,000 ten thousand periods, compared with Artificial Ceramic joint prepared by aluminium oxide or zirconium oxide, tool
There is higher reliability, is suitble to be used for a long time in human body.
Patent CN108585880A (2018-01-22 application, 2018-09-28 are announced, and are not yet authorized) discloses a kind of nitrogen
The preparation method of SiClx ceramics hip joint bulb, including silicon nitride, silicon nitride ceramics microballon, solvent is used to carry out ball for raw material
Mill, later as being granulated, obtained by forming and sintering.The invention is manufactured compared with traditional technology using binary or ternary sintering aid
Ceramic hip joint ceramics bulb more has reasonability, operability, and firing range is wider, and performance is more excellent, and wearability is more
Good, abrasion are less, are implanted into less side effects, longer life expectancy after human body；Using etc. static pressure, green body is finer and close and is evenly distributed；
Reasonable sintering curve and gap vacuum take out impurity and are to maintain product quality and purity.
Summary of the invention
The purpose of the present invention is preparing a kind of silicon nitride ceramics implantation material that performance is controllable, outer layer is opposite with alpha phase
Based on silicon nitride, and it is internal then opposite based on beta phase silicon nitride, it can thus reach the effect that appearance is hard, and inside is tough
Fruit can improve the hardness of silicon nitride ceramics implantation material and wearability and improve its fracture toughness and intensity, resist crackle and
Reduce the risk accordingly destroyed.
To achieve the above object, the present invention provides a kind of silicon nitride ceramics implantation materials that performance is controllable, comprising: implantation material
Raw material components include silicon nitride and additive；Additive includes the first additive, Second addition and third additive；First
Additive is in magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride
One or more mixtures, preferably 1~2 kind；Second addition is selected from erbium oxide, thulium oxide, ytterbium oxide and three oxidations two
One of lutetium or a variety of mixtures, preferably 1~2 kind；Third additive is selected from praseodymium oxide, samarium oxide, ceria, three
Aoxidize one of two neodymiums and titanium oxide calcium or a variety of mixtures, preferably 1~2 kind.
In the raw material components that the present invention uses, the mass ratio of silicon nitride and additive is (60~95): (5~40).
Implantation material provided by the invention includes internal and surface layer；Internal raw material components include silicon nitride and additive；Add
Adding agent includes the first additive and Second addition；The raw material components on surface layer include silicon nitride and additive；Additive includes the
One additive and third additive.In the raw material components of the inside of implantation material provided by the invention, the matter of silicon nitride and additive
Amount is than being (60~95): (5~40)；The mass ratio of first additive and Second addition is (60~95): (5~40)；Surface layer
Raw material components in, the mass ratio of silicon nitride and additive is (60~95): (5~40)；First additive and third additive
Mass ratio be (60~95): (5~40).
As a preferred embodiment, in the raw material components that the present invention uses, the first additive is magnesia and aluminium oxide
Mixture；The mass ratio of magnesia and aluminium oxide is (60~95): (5~40).
The present invention also provides a kind of preparation methods of silicon nitride ceramics implantation material, comprising steps of S1: by silicon nitride and adding
Add agent to mix, successively carries out ball-milling treatment, granulation, drying process later, obtain first chamber；Wherein, additive includes the
One additive and Second addition, the first additive be selected from magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide,
One of titanium carbide, titanium nitride and boron nitride or a variety of mixtures；Second addition is selected from erbium oxide, thulium oxide, oxidation
One of ytterbium and three two lutetiums of oxidation or a variety of mixtures；S2: first chamber is subjected to layer-by-layer pre-molding, obtains first
Green body；S3: nitridation silicon additive is mixed, ball-milling treatment, granulation and drying process is successively carried out later, obtains the second combination
Object；Wherein, additive include the first additive and third additive, the first additive be selected from magnesia, aluminium oxide, yttrium oxide,
One of strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride or a variety of mixtures；The choosing of third additive
One of autoxidation praseodymium, samarium oxide, ceria, neodymium oxide and titanium oxide calcium or a variety of mixtures；S4:
One billet surface carries out layer-by-layer pre-molding by raw material of second chamber, obtains green body part；Green body part is machined out into
Type and/or manual processing molding, obtain part to be sintered；S5: part to be sintered is sintered, sintered part is obtained；S6: it will burn
Knot part is post-processed, and the controllable silicon nitride ceramics implantation material of performance is obtained.
In the S2 and S4 of the preparation method of silicon nitride ceramics implantation material provided by the invention, pre-molding includes being cold-pressed into
At least one of type, cold isostatic compaction, hot-forming, pre-sintering molding.
In the S5 of the preparation method of silicon nitride ceramics implantation material provided by the invention, treat sintered part be sintered for
According to the demand of final implantation material, the surface for treating sintered part is sintered pore-creating processing, so that the surface of gained sintered part has
There is porous coarse structure；As a preferred embodiment, treating sintered part and be sintered includes: in nitrogen or other indifferent gas
It under body protection, treats sintered part and carries out gas pressure sintering, the temperature of sintering is 1700~2500 DEG C, and the time of sintering is 3~48 small
When.
In the S5 of the preparation method of silicon nitride ceramics implantation material provided by the invention, treats sintered part and be sintered it
Afterwards further include: hip treatment is carried out to sintered part, the temperature of hip treatment is 1500~2400 DEG C, pressure 100
~300MPa, time are 3~48 hours.
In the S6 of the preparation method of silicon nitride ceramics implantation material provided by the invention, post-processing is carried out for burning to sintered part
Knot part is surface-treated, laser marking, at least one of cleaning；As a preferred embodiment, surface treatment includes pore-creating
At least one of post-processing, polishing treatment, surface acid-washing processing；Wherein, polishing treatment includes grinding processing and/or grinds
Mill processing；Surface acid-washing processing includes: that sintered part is statically placed in acidic oxidation electrolyte solution to react；Acidic oxidation electrolyte
Solution is the mixed aqueous solution of hydrofluoric acid, aqueous hydrogen peroxide solution or hydrofluoric acid and hydrogen peroxide.
In the S1 of the preparation method of silicon nitride ceramics implantation material provided by the invention, the mass ratio of silicon nitride and additive is
(60~95): (5~40)；The mass ratio of first additive and Second addition is (60~95): (5~40)；In S3, silicon nitride
Mass ratio with additive is (60~95): (5~40)；The mass ratio of first additive and third additive is (60~95):
(5~40).
Technical solution provided by the invention, have it is following the utility model has the advantages that
(1) ceramic implants are as conventional metals or the ideal substitution of high molecular material implantation material；Nitrogen provided by the invention
SiClx ceramic implants not only possess all known advantages of general ceramic implants, while compared to existing three kinds of oxides
Ceramics also possess unrivaled advantage, especially as bio-medical type ceramics；Silicon nitride ceramics provided by the invention is planted
Enter the oxide ceramics of every mechanical performance index of object better than currently on the market, with high rigidity, high bending strength is excellent
Different frictional behaviour, especially fracture toughness, are increased substantially, and furthermore silicon nitride is as a kind of chemically stable material,
There is no the problem of aging of zirconium oxide, also have the long upper and Bone Ingrowth ability of good bone (ability for forming biological fixation) and resist
Infection ability and good developability.
(2) present invention promotes or inhibits alpha phase to arrive the complete transformation of beta phase by sintering aid, by successively at
Type, reaches that appearance is hard, internal tough effect, can improve the hardness of silicon nitride ceramics implantation material and wearability and mention
Its high fracture toughness and intensity resist crackle and reduce the risk accordingly destroyed.
Additional aspect and advantage of the invention will be set forth in part in the description, and will partially become from the following description
Obviously, or practice through the invention is recognized.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the controllable silicon nitride ceramics implantation material of the performance of the invention being prepared.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.The following examples are only intended to illustrate the technical solution of the present invention more clearly, therefore is intended only as example, without
It can be limited the scope of the invention with this.
Experimental method in following embodiments is unless otherwise specified conventional method.Examination as used in the following examples
Material is tested, is to be commercially available from regular shops unless otherwise specified.Quantitative test in following embodiment, is respectively provided with three
Secondary to repeat to test, data are the average value or mean+SD of three repeated experiments.
Based on the patent (application number 201711177603.9) applied before, the present invention provides a kind of nitridation that performance is controllable
Silicon ceramic implants, the raw material components of the implantation material include that mass ratio is (60~95): the silicon nitride and additive of (5~40)；
Additive includes the first additive, Second addition and third additive；First additive is selected from magnesia, aluminium oxide, oxidation
One of yttrium, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride or a variety of mixtures, preferably 1~
2 kinds, more preferably mass ratio is (60~95): the magnesia of (5~40) and the mixture of aluminium oxide；Second addition is selected from oxygen
One of change erbium, thulium oxide, ytterbium oxide and three two lutetiums of oxidation or a variety of mixtures, preferably 1~2 kind；Third additive
Selected from one of praseodymium oxide, samarium oxide, ceria, neodymium oxide and titanium oxide calcium or a variety of mixtures, preferably
It is 1~2 kind.The Second addition that the present invention uses has the function of promotion silicon nitride phase transformation, and the third additive of use has
Inhibit the effect of silicon nitride phase transformation.
As shown in Figure 1, implantation material provided by the invention includes internal and surface layer；Internal raw material components include that mass ratio is
(60~95): the silicon nitride and additive of (5~40)；Additive includes that mass ratio is (60~95): first addition of (5~40)
Agent and Second addition；The raw material components on surface layer include that mass ratio is (60~95): the silicon nitride and additive of (5~40)；Add
Adding agent to include mass ratio is (60~95): first additive and third additive of (5~40).The present invention is by adjusting additive
Ingredient and additive amount, can be improved gained silicon nitride ceramics implantation material performance.
The present invention also provides a kind of preparation methods of silicon nitride ceramics implantation material, comprising steps of
S1: be (60~95) by mass ratio: the silicon nitride and additive of (5~40) mix, and successively carry out at ball milling later
Reason is granulated, is dried, and obtains first chamber；The mass ratio of silicon nitride and additive can be 60:40,70:30,80:
20,90:10,95:5；
Wherein, additive include mass ratio be (60~95): first additive and Second addition of (5~40), first
Additive is in magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride
One or more mixtures；Second addition is selected from one of erbium oxide, thulium oxide, ytterbium oxide and three two lutetiums of oxidation or more
The mixture of kind；The mass ratio of first additive and Second addition can be 60:40,70:30,80:20,90:10,95:5.
The present invention can according to the demand of final implantation material, select adapt to mold, inside implantation material add magnesia,
Aluminium oxide, ytterbium oxide, erbium oxide, thulium oxide, three at least three kinds aoxidized in two lutetiums are used as sintering aid, promote follow-up sintering mistake
Cheng Zhong, the alpha phase inside implantation material arrives the complete transformation of beta phase, so that inside implantation material based on beta phase silicon nitride.
S2: first chamber is subjected to layer-by-layer pre-molding, obtains the first green body；Wherein, pre-molding includes being cold-pressed into
At least one of type, cold isostatic compaction, hot-forming, pre-sintering molding.
S3: be (60~95) by mass ratio: the silicon nitride and additive of (5~40) mix, and successively carry out at ball milling later
Reason is granulated and is dried, and obtains second chamber；The mass ratio of silicon nitride and additive can be 60:40,70:30,80:
20,90:10,95:5；
Wherein, additive include mass ratio be (60~95): first additive and third additive of (5~40), first
Additive is in magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride
One or more mixtures；Third additive is selected from praseodymium oxide, samarium oxide, ceria, neodymium oxide and titanium oxide
One of calcium or a variety of mixtures；The mass ratio of first additive and third additive can be 60:40,70:30,80:
20,90:10,95:5.
The present invention can add magnesia, aluminium oxide, praseodymium oxide, samarium oxide, ceria, three oxidations in implantation material outer layer
At least three kinds in two neodymiums, titanium oxide calcium are used as sintering aid, in the subsequent sintering process, alpha phase are inhibited to arrive beta phase
Complete transformation so that implantation material outer layer is based on alpha phase silicon nitride.
S4: layer-by-layer pre-molding is carried out by raw material of second chamber in the first billet surface, obtains green body part；By green body
Part is machined out molding and/or manual processing molding, obtains part to be sintered；
Wherein, pre-molding include cold moudling, cold isostatic compaction, it is hot-forming, be pre-sintered molding at least one
Kind.
S5: part to be sintered is sintered, sintered part is obtained；
Specifically, according to the demand of final implantation material, the surface for treating sintered part is sintered pore-creating processing, so that gained
The surface of sintered part has porous coarse structure；Specifically include: under nitrogen or other inert gas shieldings, treat sintered part into
Row gas pressure sintering, the temperature of sintering are 1700~2500 DEG C, can be 1700 DEG C, 1800 DEG C, 1900 DEG C, 2000 DEG C, 2100 DEG C,
2200 DEG C, 2300 DEG C, 2400 DEG C, 2500 DEG C, time of sintering are 3~48 hours, can be 3 hours, 10 hours, 20 hours,
30 hours, 40 hours, 48 hours.
The present invention, which treats to further comprise the steps of: after sintered part is sintered, carries out hip treatment to sintered part,
The temperature of hip treatment be 1500~2400 DEG C, can be 1500 DEG C, 1600 DEG C, 1700 DEG C, 1800 DEG C, 1900 DEG C,
2000 DEG C, 2100 DEG C, 2200 DEG C, 2300 DEG C, 2400 DEG C, pressure be 100~300MPa, can be 100MPa, 150MPa,
200MPa, 250MPa, 300MPa, time are 3~48 hours, can be 3 hours, 10 hours, 20 hours, and 30 hours, 40 hours,
48 hours.
S6: sintered part is post-processed, and obtains the controllable silicon nitride ceramics implantation material of performance；
Specifically, sintered part is surface-treated, laser marking, at least one of cleaning；Surface treatment includes making
At least one of hole post-processing, polishing treatment, surface acid-washing processing；Wherein, polishing treatment include grinding processing and/or
Milled processed；Surface acid-washing processing includes: that sintered part is statically placed in acidic oxidation electrolyte solution to react；Acidic oxidation electrolysis
Matter solution is the mixed aqueous solution of hydrofluoric acid, aqueous hydrogen peroxide solution or hydrofluoric acid and hydrogen peroxide.
Studies have shown that the product of the wearability of silicon nitride ceramics and its fracture toughness and hardness is in a certain proportion of linear pass
System.In view of silicon nitride ceramics implantation material is in bio-medical field, application scenarios especially in terms of orthopaedics, the nitridation of target
It is necessary to have fracture toughnesses as high as possible and intensity to resist crackle and to reduce the risk accordingly destroyed for silicon ceramic implants,
It also needs that there is hardness as high as possible simultaneously, to improve the wearability of silicon nitride ceramics implantation material together.The present invention considers
To itself unique crystalline structure of silicon nitride ceramic material, during the sintering process, the silicon nitride of alpha phase can be changed into beta
Phase, in-situ preparation long column shape crystal, such long column shape crystal has the ability of Anticrack, to improve the fracture of material
Toughness realizes the self toughening of silicon nitride ceramics.But the hardness number of beta phase silicon nitride is lower than alpha phase, during the sintering process,
The complete transformation of beta phase is arrived in case of alpha phase, the fracture toughness and intensity of silicon nitride ceramics can increase, still
Its hardness is lower with respect to the silicon nitride of alpha phase, thus the relatively blunt raising in silicon nitride ceramics wearability.
The silicon nitride ceramics implantation material controllable to performance provided by the invention and its preparation side combined with specific embodiments below
Method is described further.
The present embodiment provides a kind of silicon nitride ceramics implantation material, preparation method comprising steps of
S1: silicon nitride and additive that mass ratio is 75:25 are mixed, successively carry out ball-milling treatment, granulation, drying later
Processing, obtains first chamber；Wherein, additive is the first additive and Second addition that mass ratio is 70:30, and first adds
Adding agent is the mixture of magnesia and aluminium oxide that mass ratio is 70:30；Second addition is the erbium oxide that mass ratio is 70:30
And thulium oxide.
S2: first chamber is subjected to layer-by-layer pre-molding, obtains the first green body；Wherein, pre-molding is hot-forming.
S3: silicon nitride and additive that mass ratio is 75:25 are mixed, and are successively carried out ball-milling treatment later, are granulated and do
Dry processing, obtains second chamber；Wherein, additive is the first additive and Second addition that mass ratio is 70:30, first
Additive is the mixture of the magnesia that mass ratio is 70:30 and aluminium oxide；Third additive is the oxidation that mass ratio is 70:30
The mixture of praseodymium and samarium oxide.
S4: layer-by-layer pre-molding is carried out by raw material of second chamber in the first billet surface, obtains green body part；By green body
Part is machined out molding, obtains part to be sintered；Wherein, pre-molding is hot-forming.
S5: carrying out gas pressure sintering for part to be sintered, and the temperature of sintering is 1800 DEG C, and the time of sintering is 24 hours, is obtained
Sintered part；Hip treatment is carried out to sintered part, the temperature of hip treatment is 1900 DEG C, pressure 200MPa, the time
It is 20 hours.
S6: the product that S5 is obtained is surface-treated, laser marking, cleaning, obtains the controllable silicon nitride ceramics of performance
Implantation material；Wherein, surface treatment includes pore-creating post-processing, polishing treatment, surface acid-washing processing；Polishing treatment includes grinding
Processing；Surface acid-washing processing includes: that sintered part is statically placed in acidic oxidation electrolyte solution to react；Acidic oxidation electrolyte is molten
Liquid is hydrofluoric acid.
The performance indicator result for the silicon nitride ceramics implantation material that the present invention is prepared can achieve:
(1) hardness: HV101400~1600；
(2) bending strength: 800~1000MPa；
(3) fracture toughness: 6~8MPa*m1/2；
(4) wear rate: < 1mm3/107Period.
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.Unless specifically stated otherwise, it otherwise illustrates in these embodiments
Component and opposite step, numerical expression and the numerical value of step are not limit the scope of the invention.It is illustrated and described herein
In all examples, unless otherwise prescribed, any occurrence should be construed as merely illustratively, not as limitation, because
This, other examples of exemplary embodiment can have different values.
In the description of the present invention, it is to be understood that, term " first ", " second " are used for description purposes only, and cannot
It is interpreted as indication or suggestion relative importance or implicitly indicates the quantity of indicated technical characteristic.Define as a result, " the
One ", the feature of " second " can explicitly or implicitly include one or more of the features.In the description of the present invention,
" a variety of " are meant that two or more, unless otherwise specifically defined.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover in protection scope of the present invention.
Claims (10)
1. a kind of silicon nitride ceramics implantation material, it is characterised in that:
The raw material components of the implantation material include silicon nitride and additive；
The additive includes the first additive, Second addition and third additive；
First additive is selected from magnesia, aluminium oxide, yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride
With one of boron nitride or a variety of mixtures；
The Second addition is selected from one of erbium oxide, thulium oxide, ytterbium oxide and three two lutetiums of oxidation or a variety of mixtures；
The third additive be selected from one of praseodymium oxide, samarium oxide, ceria, neodymium oxide and titanium oxide calcium or
A variety of mixtures.
2. silicon nitride ceramics implantation material according to claim 1, it is characterised in that:
The mass ratio of the silicon nitride and the additive is (60~95): (5~40).
3. silicon nitride ceramics implantation material according to claim 1, it is characterised in that:
The implantation material includes internal and surface layer；
The raw material components of the inside include silicon nitride and additive；The additive includes the first additive and the second addition
Agent；
The raw material components on the surface layer include silicon nitride and additive；The additive includes that the first additive and third are added
Agent.
4. silicon nitride ceramics implantation material according to claim 3, it is characterised in that:
In the raw material components of the inside, the mass ratio of the silicon nitride and the additive is (60~95): (5~40)；Institute
The mass ratio for stating the first additive and the Second addition is (60~95): (5~40)；
In the raw material components on the surface layer, the mass ratio of the silicon nitride and the additive is (60~95): (5~40)；Institute
The mass ratio for stating the first additive and the third additive is (60~95): (5~40).
5. silicon nitride ceramics implantation material according to claim 1, it is characterised in that:
First additive is the mixture of magnesia and aluminium oxide；
The mass ratio of the magnesia and the aluminium oxide is (60~95): (5~40).
6. a kind of preparation method of silicon nitride ceramics implantation material, which is characterized in that comprising steps of
S1: silicon nitride and additive are mixed, and are successively carried out ball-milling treatment, granulation, drying process later, are obtained the first combination
Object；Wherein, the additive include the first additive and Second addition, first additive be selected from magnesia, aluminium oxide,
One of yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride or a variety of mixtures；It is described
Second addition is selected from one of erbium oxide, thulium oxide, ytterbium oxide and three two lutetiums of oxidation or a variety of mixtures；
S2: the first chamber is subjected to layer-by-layer pre-molding, obtains the first green body；
S3: silicon nitride and additive are mixed, and are successively carried out ball-milling treatment, granulation and drying process later, are obtained the second combination
Object；Wherein, the additive include the first additive and third additive, first additive be selected from magnesia, aluminium oxide,
One of yttrium oxide, strontium oxide strontia, cerium oxide, chromium oxide, titanium carbide, titanium nitride and boron nitride or a variety of mixtures；It is described
Third additive is selected from one of praseodymium oxide, samarium oxide, ceria, neodymium oxide and titanium oxide calcium or a variety of mixed
Close object；
S4: layer-by-layer pre-molding is carried out by raw material of the second chamber in first billet surface, obtains green body part；It will
The green body part is machined out molding and/or manual processing molding, obtains part to be sintered；
S5: the part to be sintered is sintered, sintered part is obtained；
S6: the sintered part is post-processed, and obtains the controllable silicon nitride ceramics implantation material of performance.
7. the preparation method of silicon nitride ceramics implantation material according to claim 6, it is characterised in that:
In S2 and S4, the pre-molding include cold moudling, cold isostatic compaction, it is hot-forming, be pre-sintered molding in extremely
Few one kind.
8. the preparation method of silicon nitride ceramics implantation material according to claim 6, it is characterised in that:
In S5, the part to be sintered is sintered as according to the demand of final implantation material, to the table of the part to be sintered
Face is sintered pore-creating processing, so that the surface of gained sintered part has porous coarse structure；
Preferably, the part to be sintered is sintered include: under nitrogen or other inert gas shieldings, to it is described to
Sintered part carries out gas pressure sintering, and the temperature of sintering is 1700~2500 DEG C, and the time of sintering is 3~48 hours；
Preferably, after being sintered to the part to be sintered further include: hip treatment is carried out to the sintered part,
The temperature of the hip treatment is 1500~2400 DEG C, and pressure is 100~300MPa, and the time is 3~48 hours.
9. the preparation method of silicon nitride ceramics implantation material according to claim 6, it is characterised in that:
In S6, to the sintered part carry out post-processing to be surface-treated to the sintered part, laser marking, in cleaning extremely
Few one kind；
Preferably, the surface treatment includes at least one of pore-creating post-processing, polishing treatment, surface acid-washing processing；
Wherein, the polishing treatment includes grinding processing and/or milled processed；
The surface acid-washing processing includes: that the sintered part is statically placed in acidic oxidation electrolyte solution to react；The acidity
Oxidization electrolysis matter solution is the mixed aqueous solution of hydrofluoric acid, aqueous hydrogen peroxide solution or hydrofluoric acid and hydrogen peroxide.
10. the preparation method of silicon nitride ceramics implantation material according to claim 6, it is characterised in that:
In S1, the mass ratio of the silicon nitride and the additive is (60~95): (5~40)；First additive and institute
The mass ratio for stating Second addition is (60~95): (5~40)；
In S3, the mass ratio of the silicon nitride and the additive is (60~95): (5~40)；First additive and institute
The mass ratio for stating third additive is (60~95): (5~40).
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| CN111517806B (en) * | 2020-04-26 | 2021-12-07 | 中国科学院上海硅酸盐研究所 | High-toughness silicon nitride ceramic and preparation method thereof |
| CN115196973A (en) * | 2022-06-29 | 2022-10-18 | 苏州玄陶商务咨询有限公司 | Multilayer silicon nitride ceramic implant and method of making same |
| CN115196973B (en) * | 2022-06-29 | 2023-10-17 | 苏州玄陶商务咨询有限公司 | Multilayer silicon nitride ceramic implant and method for making same |
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