CN108892515A - A kind of photocuring silicon nitride ceramics slurry, silicon nitride ceramics and preparation method thereof - Google Patents
A kind of photocuring silicon nitride ceramics slurry, silicon nitride ceramics and preparation method thereof Download PDFInfo
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- CN108892515A CN108892515A CN201810877840.4A CN201810877840A CN108892515A CN 108892515 A CN108892515 A CN 108892515A CN 201810877840 A CN201810877840 A CN 201810877840A CN 108892515 A CN108892515 A CN 108892515A
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Abstract
The application belongs to technical field more particularly to a kind of photocuring silicon nitride ceramics slurry, silicon nitride ceramics of ceramic material and preparation method thereof.This application provides a kind of photocuring silicon nitride ceramics slurry, silicon nitride ceramics and preparation method thereof, the technological deficiency that solid concentration is low and the monolayer immobilization thickness of its Stereolithography is low of traditional silicon nitride ceramics slurry can effectively solve.A kind of preparation method of photocuring silicon nitride ceramics slurry of the application, includes the following steps：Step 1: silicon nitride powder liquid solution, sintering aid solution, dispersing agent and precipitant mix are obtained precipitation solution, and hybrid solid is obtained by filtration to the precipitation solution；Step 2: after being cleaned to the hybrid solid calcining and ball milling after, obtain coated powder；Step 3: the coated powder, light-cured resin, photoinitiator and dispersant are obtained photocuring silicon nitride ceramics slurry.
Description
Technical field
The application belongs to the technical field more particularly to a kind of photocuring silicon nitride ceramics slurry, silicon nitride of ceramic material
Ceramics and preparation method thereof.
Background technique
Silicon nitride ceramics is one of current most potential structural ceramics, excellent high-temperature behavior, chemical stability etc.
Characteristic plays an important role it in high-temperature field.With the development of science and technology, the application field of silicon nitride ceramics, make
It is also more and more harsh with requiring.Currently, classical production process is all to be molded beta-silicon nitride powder or slurry, using
The post-processings such as sintering cooperation machining obtains required ceramic component, this mould-forming process allow for member processing cost compared with
Height is difficult to prepare the complicated part such as radian, hollow out, seriously limits the application and development of silicon nitride ceramics.
For this problem, numerous scholars propose dead size forming methods, by increasing material manufacturing method (solid without mold at
Type technology) shape needed for straight forming component, this technology can prepare the silicon nitride ceramics with labyrinth, this makes
Preparation cost decline, that widens silicon nitride ceramics uses field.Quick molding method currently used for ceramics has：3 D-printing at
Type (3DP), selective laser fusing (SLM) and Stereolithography (SLA/DLP).Stereolithography method is compared with other two kinds of mainstreams
Method is easier to prepare ceramic of compact part.But Stereolithography method needs a kind of suitable silicon nitride ceramics slurry.Scholar grinds
The silicon nitride ceramics slurry for Stereolithography is studied carefully, has had the following problems：(1) solid phase of traditional silicon nitride ceramics slurry
Content is low；(2) the monolayer immobilization thickness of traditional silicon nitride ceramics slurry is low.The two main problems limit silicon nitride ceramics
It is formed using Stereolithography technology.
Apply for content
In view of this, this application provides a kind of photocuring silicon nitride ceramics slurry, silicon nitride ceramics and preparation method thereof,
Can effectively solve traditional silicon nitride ceramics slurry solid concentration is low and the monolayer immobilization thickness of its Stereolithography is low
Technological deficiency.
A kind of preparation method of photocuring silicon nitride ceramics slurry of the application, includes the following steps：
Step 1: silicon nitride powder liquid solution, sintering aid solution, the first dispersing agent and precipitant mix are precipitated
Solution, and hybrid solid is obtained by filtration to the precipitation solution；
Step 2: after being cleaned to the hybrid solid calcining and ball milling after, obtain coated powder；
Step 3: the coated powder, light-cured resin, photoinitiator and the second dispersant are obtained photocuring
Silicon nitride ceramics slurry.
Preferably, the partial size of the beta-silicon nitride powder in the silicon nitride powder liquid solution is 0.2-1 μm.
Preferably, the concentration of the silicon nitride powder liquid solution is 0.1-1mol/L.
Preferably, the sintering aid solution includes Aluminium chloride hexahydrate solution, ANN aluminium nitrate nonahydrate solution, six hydrations
Yttrium nitrate solution, magnesium chloride hexahydrate solution and magnesium nitrate hexahydrate solution it is one or more.
Preferably, the concentration of the sintering aid solution is 0.01~0.5mol/L.
More preferably, the concentration of the sintering aid solution is 0.01~0.04mol/L.
Preferably, the precipitating reagent includes NaOH, KOH, NH3·H2O and CO (NH2)2One of or it is a variety of.
Preferably, the pH value of the precipitation solution is 8-12.
More preferably, the pH value of the precipitation solution is 9~11.
Disclosed herein as well is a kind of silicon nitride ceramics slurry, the system including photocuring silicon nitride ceramics slurry as mentioned
Preparation Method is made.
Disclosed herein as well is a kind of preparation methods of silicon nitride ceramics, include the following steps：
Step 1 is starched with photocuring silicon nitride ceramics made from the preparation method of the photocuring silicon nitride ceramics slurry
Material or the photocuring silicon nitride ceramics slurry are raw material, are carried out at successively solidification superposition according to the slicing profile of part drawing
Reason, obtains molding blank；
The molding blank is carried out dumping and sintering by step 2, obtains silicon nitride ceramics.
Disclosed herein as well is a kind of silicon nitride ceramics, the preparation method including the silicon nitride ceramics is made.
The application to by the chemistry of silicon nitride powder liquid solution, sintering aid solution, dispersing agent and precipitant mix by sinking
The method in shallow lake realizes the surface cladding of beta-silicon nitride powder, changes the surface characteristic of beta-silicon nitride powder.The application has following excellent
Point：(1) surface characteristic for changing beta-silicon nitride powder, reduces the refringence of powder and resin, improves photocuring silicon nitride
The solid content and photocuring silicon nitride ceramics slurry curing depth of ceramic slurry；(2) the evenly dispersed of sintering aid is realized.
From experimental data it is found that the photocuring silicon nitride ceramics slurry system coated by surface of the chemical precipitation to beta-silicon nitride powder
The curing depth of the silicon nitride ceramics obtained is significantly improved, and consistency is also in acceptability limit.This application provides one kind
Silicon nitride ceramics slurry suitable for Stereolithography and the method for preparing silicon nitride ceramics with it, further improve and pass through 3d
The feasibility for printing silicon nitride ceramics, will widen the application field of silicon nitride ceramics.
Specific embodiment
This application provides a kind of silicon nitride ceramics slurry and silicon nitride ceramics and its preparation method and application, for solving
The solid concentration of traditional silicon nitride ceramics slurry is low and the time for exposure of its Stereolithography is long and it is existing to be easy to produce scattering
The technological deficiency of elephant.
Below by the technical scheme in the embodiment of the application is clearly and completely described, it is clear that described implementation
Example is merely a part but not all of the embodiments of the present application.Based on the embodiment in the application, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model of the application protection
It encloses.
This application provides a kind of specific embodiment of the preparation method of photocuring silicon nitride ceramics slurry, preparation steps
It is rapid as follows：
(a) the beta-silicon nitride powder aqueous solution of 0.1-1mol/L, the sintering aid solution of 0.01~0.5mol/L are prepared, by nitrogen
Beta-silicon nitride powder is carried out chemical precipitation packet by SiClx powder solution, sintering aid solution, the first dispersing agent and precipitant mix
It covers, obtains precipitation solution, and solid-liquid filtration is carried out to precipitation solution and obtains hybrid solid, wherein the PH of precipitation solution is 8-12；
(b) it by hybrid solid, is cleaned multiple times with deionized water and alcohol isolated after removing residual ion to go
Powder, after carrying out calcining and ball milling after powder drying, wherein method for calcinating is：Powder is under air with the rate of 1~3 DEG C/min
It is warming up to 500-800 DEG C of 1~3h of heat preservation, ball grinding method sieves with 100 mesh sieve after being ball milling 6h, obtains coated powder；
(c) by coated powder, light-cured resin, photoinitiator and the second dispersant, photocuring silicon nitride pottery is obtained
Porcelain slurry.
Wherein, the partial size of the beta-silicon nitride powder in silicon nitride powder liquid solution is 0.2-1 μm.
Wherein, the concentration of silicon nitride powder liquid solution is 0.1-1mol/L.
Wherein, silicon nitride powder liquid solution is the aqueous solution of beta-silicon nitride powder.
Wherein, sintering aid solution includes Aluminium chloride hexahydrate solution (AlCl3·H2O), ANN aluminium nitrate nonahydrate solution (Al
(NO3)3·9H2O), six nitric hydrate yttrium solution (Y (NO3)3·6H2O), magnesium chloride hexahydrate solution (MgCl2·6H2) and six water O
Magnesium nitrate solution (Mg (NO3)2·6H2O) one or more.
Wherein, the concentration of each sintering aid solution is 0.01~0.5mol/L.
More preferably, the concentration of each sintering aid solution is 0.01~0.04mol/L.
Wherein, the first dispersing agent includes one of Sodium Polyacrylate, ammonium polyacrylate or methylcellulose or a variety of.
Wherein, the additive amount of the first dispersing agent is 0.5~1.5wt% of beta-silicon nitride powder, and beta-silicon nitride powder is silicon nitride
Beta-silicon nitride powder in powder solution, the first dispersing agent are to disperse beta-silicon nitride powder in water, are conducive to coat, and with second
The effect of dispersing agent is different.
Wherein, the mixing condition of step (a) is the one or more of magnetic agitation, mechanical stirring or heating.
Wherein, the revolving speed of magnetic agitation is 0~1250rpm, and churned mechanically revolving speed is 0~2000rpm, and heating temperature is
50~80 DEG C.
Wherein, precipitating reagent NaOH, KOH, NH3·H2O or CO (NH2)2One of.
More preferably, the pH value of precipitation solution is 9~11.
Wherein, step (a) filter method is vacuum filtration or rotating centrifugal, vacuum degree 0.09MPa, rotation speed are
8000-12000rpm。
Wherein, the method for step (b) calcining is：Powder is warming up to 500-800 under air with the rate of 1~3 DEG C/min
DEG C heat preservation 1~3h.
Wherein, light-cured resin includes 1,6- hexanediyl ester (HDDA), pentaerythritol tetraacrylate
(PETTA) and one of trimethylolpropane trimethacrylate (TMPTA) or a variety of.
Wherein, the mass percent of the addition of light-cured resin is the 40~60% of photocuring silicon nitride ceramics slurry.
Wherein, it includes 2- hydroxy-2-methyl -1- phenyl -1- acetone (1173), phenyl bis- (2,4,6- that photoinitiator, which is selected from,
Trimethylbenzoyl) phosphine oxide (819), (2,4,6- trimethylbenzoyl) diphenyl phosphine oxide (TPO) and 2 isopropyl sulphur
One of miscellaneous anthrone (ITX) is a variety of.
Wherein, the addition quality of photoinitiator is 1~2wt% of light-cured resin.
Specifically, the second dispersing agent includes one of BYK-9076, BYK-163 and BYK-9077 or a variety of.
Specifically, the additive amount of the second dispersing agent is 1~2wt% of coated powder, the effect of the second dispersing agent is will to wrap
Whiting body is fully dispersed in slurry preparation to be opened, and the viscosity of product is advantageously reduced.
A kind of forming method of silicon nitride ceramics provided by the present application, the preparation step are as follows：
Step 1, using above-mentioned photocuring silicon nitride ceramics slurry as raw material, carried out according to the slicing profile of part drawing layer-by-layer
Solidify superposition processing, obtains molding blank；
The molding blank is carried out dumping and sintering by step 2, obtains silicon nitride ceramics.
Specifically, step 1 is the step of molding：Model 3 d part is desired to make money or profit to be sliced with software and imports Stereolithography machine
In, then the photocuring silicon nitride ceramics slurry of preparation is added in Stereolithography machine, according to program setting, ceramic slurry by
Layer solidification successively adds up, and finally obtains molding blank.
Specifically, the method for dumping is：Molding blank is heated up in vacuum or air with the rate of 0.5-2 DEG C/min
600 DEG C of 1~3h of heat preservation are warming up to 300 DEG C of 1~3h of heat preservation, then with the rate of 0.5-2 DEG C/min.
Specifically, sintering method is：Green body after dumping is under nitrogen or vacuum atmosphere, with the speed of 0.5~3 DEG C/min
Rate is warming up to 1700~1850 DEG C of heat preservations 1~3h, air pressure 0.1-10MPa.
Wherein, it is commercially available or self-control that following embodiment is raw materials used.
Embodiment 1
The embodiment of the present application provides the preparation method of the first photocuring silicon nitride ceramics slurry, and its step are as follows：
(a) magnetic stirring apparatus (revolving speed 1250rpm) is used, in the silicon nitride deionized water solution of 0.1mol/L, be added
0.8wt% Sodium Polyacrylate (0.8wt% that Sodium Polyacrylate is beta-silicon nitride powder), by 0.03mol/L ANN aluminium nitrate nonahydrate
Water solution A l (NO3)3·9H2O、NH3·H2Six nitric hydrate yttrium aqueous solution Y (NO of O and 0.01mol/L3)3·6H2O instills nitridation
It in silicon deionized water solution, is stirred, obtains precipitation solution；The PH for adjusting precipitation solution is 10.5, is stood；
(b) precipitation solution is separated powder liquid using centrifuge, the powder isolated makes to be washed with deionized 3 times, wine
Fine purifiation is washed 1 time, and after powder drying for 24 hours, by the calcining of powder under air, calcination condition is that the rate of 1 DEG C/min is warming up to
500 DEG C of heat preservation 3h, ball milling 6h after calcining sieve with 100 mesh sieve to obtain coated powder；
(c) by the 50g coated powder and 23g 1,6 hexanediol diacrylate (HDDA), 0.4g phenyl pair after sieving
(2,4,6- trimethylbenzoyl) phosphine oxide (819) and 0.5g BYK-9076 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of the first silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in air of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 3h are warming up to 300 DEG C of heat preservation 1h, then with the rate of 1 DEG C/min；Green body after dumping is sintered under a nitrogen with 3
DEG C/rate of min is warming up to 1820 DEG C of heat preservations 2h, air pressure 0.1MPa and obtains the silicon nitride ceramics for having complicated shape.
Embodiment 2
The embodiment of the present application provides the preparation method of second of silicon nitride ceramics slurry, and its step are as follows：
(a) by the silicon nitride deionized water solution of 0.1mol/L, 0.8wt% Sodium Polyacrylate, nine water of 0.03mol/L is added
Close aluminum nitrate Al (NO3)3·9H2O, six nitric hydrate yttrium (Y (NO of NaOH and 0.01mol/L3)3·6H2O) aqueous solution uses mechanical
Blender stirs (revolving speed 1500rpm) mixing, obtains precipitation solution；The PH for adjusting precipitation solution is 11.5, is heated to 60 DEG C,
It stands；
(b) precipitation solution is separated powder liquid using vacuum filtration (vacuum degree 0.09MPa), the powder isolated uses
Deionized water is washed 4 times, and ethanol wash 1 time, for 24 hours by powder drying, the calcining of rear powder under vacuum is with the rate of 2 DEG C/min
500 DEG C of heat preservation 2h are warming up to, ball milling 6h after calcining sieves with 100 mesh sieve to obtain coated powder；
(c) by the 50g coated powder and 23g pentaerythritol tetraacrylate (PETTA), 0.4g 2- hydroxyl -2- after sieving
Methyl-1-phenyl-1- acetone (1173) and 0.5g BYK-9077 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of second of silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, it is warming up to the rate of 1 DEG C/min
300 DEG C of heat preservation 1.5h, then 600 DEG C of heat preservation 2h are warming up to the rate of 1 DEG C/min；Green body after dumping is sintered under a nitrogen with 2
DEG C/rate of min is warming up to 1820 DEG C of heat preservations 2h, air pressure 8MPa and obtains the silicon nitride ceramics for having complicated shape.
Embodiment 3
The embodiment of the present application provides the preparation method of the third silicon nitride ceramics slurry, and its step are as follows:
(a) by the silicon nitride deionized water solution of 0.2mol/L, 0.8wt% Sodium Polyacrylate, nine water of 0.05mol/L is added
Close aluminum nitrate Al (NO3)3·9H2O, KOH and 0.03mol/L magnesium chloride hexahydrate MgCl2·6H2O aqueous solution uses mechanical agitator
(revolving speed 1800rpm) is stirred, and obtains precipitation solution；The PH for adjusting precipitation solution is 10.5, is heated to 60 DEG C, stands；
(b) precipitation solution is separated powder liquid using vacuum filtration (vacuum degree 0.09MPa), the powder isolated uses
Deionized water is washed 3 times, and ethanol wash 1 time, for 24 hours by powder drying, the calcining of rear powder under air is with the rate of 2 DEG C/min
500 DEG C of heat preservation 2h are warming up to, ball milling 6h after calcining sieves with 100 mesh sieve to obtain coated powder；
(c) by the 50g coated powder and 35g trimethylolpropane trimethacrylate (TMPTA), 0.35g 2- hydroxyl after sieving
Base-2- methyl-1-phenyl-1- acetone (1173) and 1g BYK-9075 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of the third silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 3h are warming up to 300 DEG C of heat preservation 0.5h, then with the rate of 0.5 DEG C/min；Green body after dumping is sintered under a nitrogen
1820 DEG C of heat preservations 2h, air pressure 0.1MPa, which are warming up to, with the rate of 2 DEG C/min obtains the silicon nitride ceramics for having complicated shape.
Embodiment 4
The embodiment of the present application provides the preparation method of the 4th kind of photocuring silicon nitride ceramics slurry, and its step are as follows：
(a) by the silicon nitride deionized water solution of 0.1mol/L, 1.2wt% Sodium Polyacrylate, nine water of 0.5mol/L is added
Close aluminum nitrate Al (NO3)3·9H2O, KOH and 0.03mol/L magnesium nitrate hexahydrate Mg (NO3)2·6H2O aqueous solution uses mechanical stirring
Device (revolving speed 1000rpm) is stirred, and obtains precipitation solution；The PH for adjusting precipitation solution is 9.5, is heated to 50 DEG C, stands；
(b) precipitation solution is separated powder liquid using centrifuge (revolving speed 8000rpm), the powder use isolated go from
Sub- water washing 3 times, ethanol wash 1 time, for 24 hours by powder drying, the calcining of rear powder under air is heated up with the rate of 2 DEG C/min
To 500 DEG C of heat preservation 2h, ball milling 6h after calcining sieves with 100 mesh sieve to obtain coated powder；
(c) by the 50g coated powder and 35g trimethylolpropane trimethacrylate (TMPTA), 0.35g 2- hydroxyl after sieving
Base-2- methyl-1-phenyl-1- acetone (1173) and 1.5g BYK-9077 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of the 4th kind of silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 3h are warming up to 300 DEG C of heat preservation 0.5h, then with the rate of 0.5 DEG C/min；Green body after dumping is sintered under a nitrogen
1850 DEG C of heat preservations 2h, air pressure 0.1MPa, which are warming up to, with the rate of 1 DEG C/min obtains the silicon nitride ceramics for having complicated shape.
Embodiment 5
The embodiment of the present application provides the preparation method of the 5th kind of photocuring silicon nitride ceramics slurry, and its step are as follows:
(a) by the silicon nitride deionized water solution of 1mol/L, 1.2wt% Sodium Polyacrylate is added, 0.5mol/L nine is hydrated
Aluminum nitrate Al (NO3)3·9H2O、CO(NH2)2With 0.2mol/L magnesium nitrate hexahydrate Mg (NO3)2·6H2O aqueous solution is stirred, and is obtained
To precipitation solution；The PH for adjusting precipitation solution is 9.5, is heated to 60 DEG C, stands；
(b) precipitation solution is separated powder liquid using centrifuge (revolving speed 10000rpm), the powder use isolated is gone
Ion water washing 3 times, ethanol wash 1 time, for 24 hours by powder drying, the calcining of rear powder under air is with the rate liter of 2 DEG C/min
To 500 DEG C of heat preservation 2h, ball milling 6h after calcining sieves with 100 mesh sieve to obtain coated powder temperature；
(c) by the 50g coated powder and 40g pentaerythritol tetraacrylate (PETTA), 0.4g (2,4,6- tri- after sieving
Methyl benzoyl) diphenyl phosphine oxide (TPO) and 1.5g BYK-9077 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of the 5th kind of silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 3h are warming up to 300 DEG C of heat preservation 0.5h, then with the rate of 0.5 DEG C/min；Green body after dumping is sintered under a nitrogen
1820 DEG C of heat preservations 2h, air pressure 0.1MPa, which are warming up to, with the rate of 2 DEG C/min obtains the silicon nitride ceramics for having complicated shape.
Embodiment 6
The embodiment of the present application provides the preparation method of the 6th kind of photocuring silicon nitride ceramics slurry, and its step are as follows:
(a) magnetic stirring apparatus (revolving speed 1500rpm) is used, the silicon nitride deionized water solution of 0.2mol/L is added
1.2wt% Sodium Polyacrylate, 0.1mol/L ANN aluminium nitrate nonahydrate Al (NO3)3·9H2O、CO(NH2)2With six water nitre of 0.08mol/L
Sour magnesium Mg (NO3)2·6H2O aqueous solution is stirred, and obtains precipitation solution；The PH for adjusting precipitation solution is 9, is stood；
(b) precipitation solution is separated powder liquid using centrifuge (revolving speed 12000rpm), the powder use isolated is gone
Ion water washing 2 times, ethanol wash 2 times, for 24 hours by powder drying, the calcining of rear powder under air is with the rate liter of 1 DEG C/min
To 500 DEG C of heat preservation 2h, ball milling 6h after calcining sieves with 100 mesh sieve to obtain coated powder temperature；
(c) by the 50g coated powder and 40g pentaerythritol tetraacrylate (PETTA), 0.4g (2,4,6- tri- after sieving
Methyl benzoyl) diphenyl phosphine oxide (TPO) and 1g BYK-9076 mixing, obtain photocuring silicon nitride ceramics slurry.
The embodiment of the present application provides the forming method of the 6th kind of silicon nitride ceramics, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 2h are warming up to 300 DEG C of heat preservation 0.5h, then with the rate of 1 DEG C/min；Green body after dumping be sintered under a nitrogen with
The rate of 2 DEG C/min is warming up to 1850 DEG C of heat preservations 3h, air pressure 10MPa and obtains the silicon nitride ceramics for having complicated shape.
Comparative example
Present invention also provides a kind of comparative example, comparative example is the silicon nitride ceramics that uncoated beta-silicon nitride powder is prepared
The specific preparation method of slurry, the silicon nitride ceramics which is prepared is as follows：
(1) by aluminium oxide, yttrium oxide and beta-silicon nitride powder according to 4:6:90 ratio ball milling mixing, obtains mixed powder；
(2) by 50g mixed powder and 40g pentaerythritol tetraacrylate (PETTA), 0.4g (2,4,6- trimethylbenzene first
Acyl group) diphenyl phosphine oxide (TPO) and 1gBYK-9076 mixing, obtain photocuring silicon nitride ceramics slurry.
The following provide the forming methods of the silicon nitride ceramics of comparative example, and its step are as follows：
The first step, molding：Model 3 d part is desired to make money or profit to be sliced with software and is imported in Stereolithography machine, then by preparation
Photocuring silicon nitride ceramics slurry is added in Stereolithography machine, according to program setting, photocuring silicon nitride ceramics slurry by
Layer solidification successively adds up, and finally obtains molding blank；
Second step：Post-processing：By the dumping in a vacuum of the molding blank in the first step, heated up with the rate of 0.5 DEG C/min
600 DEG C of heat preservation 2h are warming up to 300 DEG C of heat preservation 0.5h, then with the rate of 1 DEG C/min；Green body after dumping be sintered under a nitrogen with
The rate of 2 DEG C/min is warming up to 1820 DEG C of heat preservations 2h, air pressure 8MPa and obtains the silicon nitride ceramics for having complicated shape.
The curing depth and consistency for detecting the silicon nitride ceramics of above embodiments 1-6 and comparative example, as a result such as 1 institute of table
Show.
The test result of table 1 embodiment 1-6 and comparative example
| Sample | Curing depth (micron) | Consistency (%) |
| Comparative example | 20 | 92 |
| Embodiment 1 | 22 | 95 |
| Embodiment 2 | 22 | 97 |
| Embodiment 3 | 24 | 85 |
| Embodiment 4 | 25 | 85 |
| Embodiment 5 | 35 | 80 |
| Embodiment 6 | 27 | 82 |
As known from Table 1, embodiment 1-6 and comparative example can be seen that coat sintering aid by chemical precipitation method and nitrogenize
Silicon can effectively improve the thickness of silicon nitride ceramics slurry monolayer immobilization in Light Curing, Neng Goubao to silicon nitride surface
Demonstrate,prove inter-layer bonding force.Furthermore suitable cladding process facilitates the raising of consistency, and cladding processing effectively increases sintering aid
Dispersion in beta-silicon nitride powder；From embodiment 1-6 it is found that the concentration of each sintering aid is when telling somebody what one's real intentions are concentration that is, 0.01
When~0.04mol/L, the curing depth and consistency performance of silicon nitride ceramics are more superior.
The above is only the preferred embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (10)
1. a kind of preparation method of photocuring silicon nitride ceramics slurry, which is characterized in that include the following steps：
Step 1: silicon nitride powder liquid solution, sintering aid solution, the first dispersing agent and precipitant mix are obtained into precipitation solution,
And hybrid solid is obtained by filtration to the precipitation solution；
Step 2: after being cleaned to the hybrid solid calcining and ball milling after, obtain coated powder；
Step 3: the coated powder, light-cured resin, photoinitiator and the second dispersant are obtained photocuring nitridation
Silicon ceramic slurry.
2. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the silicon nitride
The partial size of beta-silicon nitride powder in powder solution is 0.2-1 μm.
3. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the silicon nitride
The concentration of powder solution is 0.1-1mol/L.
4. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the sintering helps
Agent solution include Aluminium chloride hexahydrate solution, ANN aluminium nitrate nonahydrate solution, six nitric hydrate yttrium solution, magnesium chloride hexahydrate solution and
Magnesium nitrate hexahydrate solution it is one or more.
5. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the sintering helps
The concentration of agent solution is 0.01~0.5mol/L.
6. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the precipitating reagent
Including NaOH, KOH, NH3·H2O and CO (NH2)2One of or it is a variety of.
7. the preparation method of photocuring silicon nitride ceramics slurry according to claim 1, which is characterized in that the precipitating is molten
The pH value of liquid is 8-12.
8. a kind of silicon nitride ceramics slurry, which is characterized in that including photocuring nitrogen as claimed in any one of claims 1 to 7
The preparation method of SiClx ceramic slurry is made.
9. a kind of preparation method of silicon nitride ceramics, which is characterized in that include the following steps：
Step 1, made from the preparation method of the photocuring silicon nitride ceramics slurry as described in claim 1 to 6 any one
Photocuring silicon nitride ceramics slurry or photocuring silicon nitride ceramics slurry as claimed in claim 7 are raw material, according to part drawing
Slicing profile carry out successively solidification superposition processing, obtain molding blank；
The molding blank is carried out dumping and sintering by step 2, obtains silicon nitride ceramics.
10. a kind of silicon nitride ceramics, which is characterized in that the preparation method system including silicon nitride ceramics as claimed in claim 9
?.
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