CN115010498A - Forming method of SiC complex component - Google Patents
Forming method of SiC complex component Download PDFInfo
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- CN115010498A CN115010498A CN202210674196.7A CN202210674196A CN115010498A CN 115010498 A CN115010498 A CN 115010498A CN 202210674196 A CN202210674196 A CN 202210674196A CN 115010498 A CN115010498 A CN 115010498A
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Abstract
The invention belongs to the field of 3D printing, and relates to a material increase manufacturing process of a SiC complex component, which comprises the following steps: 1) selecting nano SiC powder and a submicron additive, carrying out wet milling by taking deionized water as a medium, and screening after dry-pressing granulation to obtain granulated powder with the particle size of less than 15 um; 2) preparing a photo-curing slurry based on the granulated powder obtained in the step 1); 3) forming the photocuring slurry prepared in the step 2) into a complex blank by adopting an upper projection type photocuring indirect additive manufacturing device; 4) degreasing and sintering the complex blank prepared in the step 3) to obtain the SiC complex component, wherein the sintering is reaction sintering, liquid phase sintering or solid phase sintering. The invention provides a forming method of a SiC complex component, which can improve the compactness of a finished piece and reduce the forming energy consumption.
Description
Technical Field
The invention belongs to the field of 3D printing, relates to a complex component forming method, and particularly relates to a SiC complex component forming method.
Background
Although silicon carbide is a new material which is developed only in recent industry, it has been widely used in many occasions, such as high-temperature and wear-resistant protective parts, acid and alkali resistant sealing parts, heat insulation and heat dissipation heat exchange parts, heat insulation and insulation circuit parts and other structures, heat engines, electric power and the like, due to its advantages of high strength, high hardness, good high temperature resistance, excellent thermal shock resistance, reliable chemical corrosion resistance and the like, after being developed for a short period of several decades.
As a ceramic material with extremely strong covalent bonds, the traditional silicon carbide can be formed only by adopting a powder metallurgy process, namely, a blank is manufactured by utilizing a die at first, and then a final finished piece is obtained by the processes of pressureless sintering, hot-pressing sintering, reaction sintering, hot isostatic pressing sintering and the like, so that the cost is high, the period is long, and the ceramic material cannot be used for parts with slightly complex shapes and structures; however, due to a series of problems of easy agglomeration, insensitivity to laser action, low diffusion coefficient and the like of silicon carbide powder, barriers which hinder engineering application of the process are caused by difficulty in obtaining raw materials meeting forming requirements, single structure of a formed product, low density of the formed product, high energy consumption in the forming process and the like.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a method for forming a SiC complex component, which can solve the problems of raw material supply, improve the fineness and density of a workpiece and reduce the forming energy consumption.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for forming a SiC complex component is characterized by comprising the following steps: the SiC complex component forming method comprises the following steps:
1) selecting nano SiC powder and a submicron additive, carrying out wet milling by taking deionized water as a medium, and screening after dry-pressing granulation to obtain granulated powder with the particle size of less than 15 um;
2) preparing a photo-curing slurry based on the granulated powder obtained in the step 1);
3) forming the photocuring slurry prepared in the step 2) into a blank by adopting upper projection type photocuring indirect additive manufacturing equipment;
4) degreasing and sintering the blank prepared in the step 3) to obtain the SiC complex component, wherein the sintering is reaction sintering, liquid phase sintering or solid phase sintering.
The step 1) is specifically as follows:
taking nano SiC powder and a submicron additive, wet-milling for 24-48h in a ball milling tank by taking deionized water as a medium, and screening after dry-pressing granulation to obtain granulated powder with the particle size of less than 15 um; the submicron additive is C, B 4 C、B、Al 2 O 3 、Y 2 O 3 One or more mixtures of raw materials such as rare earth oxide and the like; the pressure of the dry-pressing granulation is 80-150 MPa.
When the sintering in the step 4) adopts reaction sintering, the submicron additive in the step 1) is C;
when the sintering in the step 4) adopts liquid phase sintering, the submicron additive in the step 1) is Al 2 O 3 、Y 2 O 3 Or a rare earth oxide;
when the sintering in the step 4) adopts solid-phase sintering, the submicron additive in the step 1) is B 4 C. B or C.
The step 2) is specifically: mixing the photocuring binder with the granulation powder obtained in the step 1), and stirring for 5-20min to prepare photocuring slurry; the volume ratio of the light-cured binder to the granulated powder is 1: 4-1: 1.
the photo-curing adhesive comprises a matrix and a component which is soluble in water after being cured; the water-soluble component after curing is one or the combination of polyethylene glycol acrylate monoester and water-based polyurethane acrylate.
The volume of the water-soluble component after curing is A; the total volume of the cured water-soluble component and the matrix is B; and A is (10% -25%) B.
The thickness of the layers adopted in the step 3) is 20-40 um; the curing parameters of the binder are selected during forming according to the fact that the powder consolidation thickness is 1.2-2 times of the layering thickness.
Degreasing in the step 4) is to soak the complex blank obtained in the step 3) in distilled water at the temperature of 40-80 ℃ for 2-6h, and remove the water-soluble components in the photo-curing adhesive after curing; and then drying at 80 ℃, raising the temperature to 900 ℃ at the heating rate of 0.1-5 ℃/min under the argon protective atmosphere, preserving the temperature for 1-5h, removing the residual photocuring binder, and finishing degreasing to form a degreased part.
After degreasing in the step 4), the whole carbon residue of the light-cured binder is 0-6.5% of the mass fraction of the SiC powder in the light-cured slurry, and the carbon residue in the light-cured binder participates in sintering after degreasing.
When the sintering in step 4) is reaction sintering, the sintering process is as follows: raising the temperature of the silicon powder and the degreased part to 1400-1700 ℃ at the heating rate of 6-10 ℃/min under the vacuum condition, and preserving the heat for 30-60min to finish sintering to obtain a SiC complex component;
when the sintering in the step 4) is liquid phase sintering, the sintering process is as follows: raising the temperature to 1300 ℃ and 1900 ℃ at the heating rate of 5-8 ℃/min under the argon environment, and preserving the heat for 30-120min to finish sintering to obtain the SiC complex component;
when the sintering in the step 4) is solid-phase sintering, the sintering process comprises the following steps: raising the temperature to 1900 ℃ at the heating rate of 5-8 ℃/min in the argon or vacuum environment, preserving the heat for 30min, raising the temperature to 2000-2100 ℃ at the heating rate of 1-3 ℃/min, preserving the heat for 20-90min, and completing sintering to obtain the SiC complex component.
The invention has the advantages that:
according to the invention, the nanoscale powder is formed into a micron-sized raw material with certain fluidity at a higher bulk density through dry-pressing granulation, so that the problems of powder agglomeration, poor slurry fluidity, low solid content of a blank and the like in the forming process are solved; meanwhile, the powder pretreatment is carried out by selecting the nano SiC powder and the submicron additive, so that the powder acquisition cost is reduced, and the mixing uniformity can be improved; in addition, the components capable of being pre-degreased by water are added into the binder, so that the blank cleaning process can be simplified, the forming period can be shortened, and the energy consumption can be reduced; moreover, the invention controls the components of the binder to realize the regulation and control of the carbon residue of the degreased green body, reduce the content of the additive, and realize the reduction of the cost and the improvement of the solid content; the upper projection type photocuring indirect additive manufacturing equipment is used for forming a complex blank, the stacking density of SiC is improved through the compaction of the scraper, and the density of a final product is improved.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention provides a method for forming a SiC complex component, which specifically comprises the following steps:
1) pretreating powder;
taking nano SiC powder and a submicron additive, wet-milling for 24-48h in a ball milling tank by taking deionized water as a medium, and then screening granulation powder smaller than 15um after dry-pressing granulation.
Wherein the submicron additive is C, B 4 C、B、Al 2 O 3 、Y 2 O 3 One or more mixtures (optionally not added) of raw materials such as rare earth oxide, wherein the submicron additive is C when the reaction sintered silicon carbide is prepared, and the submicron additive is B when the solid phase sintered silicon carbide is prepared 4 C or B, C, if preparing liquid phase sintered silicon carbide, the submicron additive is Al 2 O 3 、Y 2 O 3 Rare earth oxides and the like; the briquetting pressure of the dry-pressing granulation is 80-150 MPa.
It should be noted that, because the additive ratio of different types of silicon carbide is greatly different, the ratio of the additive is determined by the skilled person according to the actual needs, and the application does not limit the additive ratio. Illustratively, the mass of the submicron additive is 0.4% to 10% of the mass of the nanoscale SiC powder.
2) Preparing forming slurry;
taking the photocuring binder and the SiC granulated powder obtained in the step 1) according to the following binder: silicon carbide granulation powder 1: 4-1: 1 for 5-20min on a gravity mixer, then adding a dispersant, a photoinitiator, a defoaming agent and the like, and uniformly stirring to prepare the photocuring slurry, wherein in the selection of the proportion of the binder and the silicon carbide granulation powder, the higher solid content can reduce the post-sintering shrinkage rate and improve the density of the final finished piece.
The photocurable adhesive contains a component soluble in water after curing, such as polyethylene glycol acrylate monoester or aqueous urethane acrylate, in addition to a commercially available photocurable adhesive (the same will be described in examples). Preferably, the volume fraction of the water-soluble component in the photo-curable adhesive after curing is 10 to 25%. By controlling the proportion of water-soluble components in the photocuring binder, the forming ligand can be dissolved and degreased in water to form pores, and the functions of not damaging the strength of a blank, not changing the dimensional stability of the blank, not introducing impurity elements and the like are achieved after water-soluble degreasing.
In addition, the whole carbon residue after degreasing of the subsequent light-cured binder is 0-6.5% of the mass fraction of the SiC powder in the slurry, wherein the residual carbon can participate in the subsequent SiC sintering.
It will be appreciated that the forming apparatus can be cleaned and brought into a ready-to-process condition while the forming slurry is being prepared. The device is particularly an up-projection type photocuring indirect additive manufacturing device which is used for forming the SiC fine component blank. Of course, the forming equipment may be prepared before the blank is formed, and the timing for preparing the forming equipment is not limited in the present application.
3) Forming a blank;
and (3) forming the complex blank by using the upper projection type photocuring indirect additive manufacturing equipment, and processing the part model according to a process rule before forming, such as performing process treatment on the part model, such as characteristic modification, auxiliary structure addition, size scaling and the like. In addition, printing parameters can be adjusted according to a process rule, illustratively, the laser spot is 15um, the used layering thickness is 20-40um, and the light-cured binder curing parameter is selected according to the condition that the powder consolidation thickness is 1.2-2 times of the layering thickness.
It can be understood that after the forming is finished, the blank is taken out from the equipment, and the excess substances such as unformed powder, adhesive powder and the like in the blank and on the surface are removed. In some cases, in which the surface quality of the finished part is particularly critical, the blank may be subjected to a post-treatment, such as grinding, polishing, etc., during the process.
4) Degreasing and sintering.
Degreasing, namely soaking the blank formed in the step 3) in distilled water at the temperature of 40-80 ℃ for 2-6h, and removing components which can be dissolved in water in the photocuring binder to form communicated micropores; and then drying the mixture in a drying box at the temperature of 80 ℃, raising the temperature to 900 ℃ at the heating rate of 0.1-5 ℃/min under the argon protective atmosphere, and preserving the heat for 1-5h to remove the residual photocuring binder to form a degreased part.
The final part is obtained using reactive sintering, liquid or solid phase sintering processes.
The reaction sintering process comprises the steps of raising the temperature of the silicon powder and the degreased part to 1400-1700 ℃ at the heating rate of 6-10 ℃/min and preserving the heat for 30-60min under the vacuum condition; the liquid phase sintering process is that the temperature is raised to 1300 ℃ and 1900 ℃ at the heating rate of 5-8 ℃/min under the argon environment and is preserved for 30-120 min; the solid phase sintering process includes raising the temperature to 1900 deg.c in argon or vacuum at 5-8 deg.c/min for 30min, raising the temperature to 2100 deg.c at 1-3 deg.c/min, and maintaining for 20-90 min.
The technical solution provided by the present invention will be described in detail with reference to the following embodiments:
example 1 reaction sintering SiC Complex Member Forming method
1) Powder pretreatment
Taking nano SiC powder and submicron carbon black with the mass fraction of 1 percent, wet-milling for 24 hours in a ball milling tank by taking deionized water as a medium, and then screening granulated powder with the particle size of less than 15um after dry-pressing granulation. The briquetting pressure of the dry-pressing granulation is 100 MPa.
2) Formation slurry preparation
Preparing equipment, cleaning up the upper projection type photocuring indirect additive manufacturing equipment and enabling the equipment to enter a state to be processed.
Preparing raw materials, namely taking a photocuring binder and the SiC powder obtained in the step 1) according to the photocuring binder: silicon carbide granulated powder 1:1, stirring for 5min on a gravity stirrer, and then adding the dispersing agent, the photoinitiator, the defoaming agent and the like, and uniformly stirring to prepare the photocuring slurry. The volume fraction of polyethylene glycol acrylate monoester in the photocuring binder is 25%, and the whole carbon residue after the binder is degreased is 6.5% of the mass fraction of SiC powder in the slurry.
3) Shaping of the blank
And forming the complex blank by using the upper projection type photocuring indirect additive manufacturing equipment, and performing process treatment such as feature modification, auxiliary structure addition, size scaling and the like on the part model according to a process rule before forming. The layering thickness used was 40um and the binder curing parameters were chosen so that the powder consolidation thickness was 1.2 times the layering thickness. And after the forming is finished, taking the blank out of the equipment, and removing redundant substances such as unformed powder, adhesive powder and the like in the blank and on the surface of the blank, wherein the blank can be subjected to operations such as grinding, polishing and the like in the process if the requirement on the surface quality of the final product is particularly high.
4) Degreasing and sintering
Degreasing, namely soaking the blank in distilled water at the temperature of 80 ℃ for 2 hours, and removing the water-soluble polyethylene glycol acrylate monoester in the binder; and then drying the mixture in a drying oven at the temperature of 80 ℃, raising the temperature to 600 ℃ at the heating rate of 5 ℃/min under the argon protective atmosphere, and preserving the heat for 5 hours to remove the residual binder to form a degreased part.
And (3) sintering, namely raising the silicon powder and the degreased part to 1700 ℃ at the heating rate of 6 ℃/min under the vacuum condition, and preserving the heat for 30min to obtain the required part.
Example 2 method for Forming liquid phase sintered SiC Complex Member
1) Powder pretreatment
Taking nano SiC powder and submicron additives with the mass fraction of 10 percent; the submicron additive is Al 2 O 3 And Y 2 O 3 The two are added according to the weight ratio of 1: 1; wet grinding for 24h in a ball milling tank by using deionized water as a medium, then screening granulation powder with the particle size of less than 10um after dry-pressing granulation, wherein the briquetting pressure of the dry-pressing granulation is 80 MPa.
2) Formation slurry preparation
Preparing equipment, cleaning up the upper projection type photocuring indirect additive manufacturing equipment and enabling the upper projection type photocuring indirect additive manufacturing equipment to enter a to-be-processed state.
Preparing raw materials, namely taking a photocuring binder and the SiC powder obtained in the step 1) according to the photocuring binder: silicon carbide granulation powder 1: 4, stirring for 20min on a gravity stirrer, and then adding the dispersing agent, the photoinitiator, the defoaming agent and the like, and uniformly stirring to prepare the photocuring slurry. The volume fraction of the waterborne polyurethane acrylate in the photocuring binder is 25%, and the mass fraction of the SiC powder in the slurry is 0.3% of the whole carbon residue after the binder is degreased.
3) Shaping of the blank
And forming the complex blank by using the upper projection type photocuring indirect additive manufacturing equipment, and performing process treatment such as feature modification, auxiliary structure addition, size scaling and the like on the part model according to a process rule before forming. The layering thickness used was 40um and the binder curing parameters were chosen so that the powder consolidation thickness was 1.2 times the layering thickness. And after the forming is finished, taking the blank out of the equipment, and removing redundant substances such as unformed powder, adhesive powder and the like in the blank and on the surface of the blank, wherein the blank can be subjected to operations such as grinding, polishing and the like in the process if the requirement on the surface quality of the final product is particularly high.
4) Degreasing and sintering.
Degreasing, namely soaking the blank body in distilled water at 40 ℃ for 6 hours, and removing the aqueous polyurethane acrylate in the binder; and then drying the mixture in a drying oven at the temperature of 80 ℃, raising the temperature to 700 ℃ at the heating rate of 3 ℃/min under the argon protective atmosphere, and preserving the heat for 2 hours to remove the residual binder to form a degreased part.
Sintering, raising the temperature to 1750 ℃ at the heating rate of 5 ℃/min under the argon environment, and keeping the temperature for 120min to obtain the required product.
EXAMPLE 3 Forming method of solid-phase sintered SiC Complex Member
1) Powder pretreatment
Taking nano SiC powder and submicron B with the mass fraction of 0.4 percent 4 And C, wet-milling for 24 hours in a ball milling tank by using deionized water as a medium, and screening granulation powder with the particle size of less than 5um after dry-pressing granulation. The briquetting pressure for dry-pressing granulation is 150 MPa.
2) Formation slurry preparation
Preparing equipment, cleaning up the upper projection type photocuring indirect additive manufacturing equipment and enabling the upper projection type photocuring indirect additive manufacturing equipment to enter a to-be-processed state.
Preparing raw materials, namely taking a photocuring binder and the SiC powder obtained in the step 1 according to the photocuring binder: silicon carbide granulation powder 2: 3, stirring for 5min on a gravity stirrer, and then adding the dispersing agent, the photoinitiator, the defoaming agent and the like, and uniformly stirring to prepare the photocuring slurry. The total volume of the polyethylene glycol acrylate monoester and the waterborne polyurethane acrylate in the adhesive accounts for 10 percent, and the whole carbon residue after the adhesive is degreased is 0 percent.
3) Shaping of the blank
And forming the complex blank by using the upper projection type photocuring indirect additive manufacturing equipment, and performing process treatment such as feature modification, auxiliary structure addition, size scaling and the like on the part model according to a process rule before forming. The layering thickness used is 20um, and the curing parameters of the adhesive are selected according to the condition that the powder consolidation thickness is 2 times of the layering thickness.
And after the forming is finished, taking the blank out of the equipment, and removing redundant substances such as unformed powder, adhesive powder and the like in the blank and on the surface of the blank, wherein the blank can be subjected to operations such as grinding, polishing and the like in the process if the requirement on the surface quality of the final product is particularly high.
4) Degreasing and sintering.
Degreasing, namely soaking the blank in distilled water at the temperature of 80 ℃ for 6h, and removing polyethylene glycol acrylate monoester and waterborne polyurethane acrylate in the binder; and then drying the mixture in a drying oven at the temperature of 80 ℃, raising the temperature to 900 ℃ at the heating rate of 0.1 ℃/min under the protection of argon, and preserving the heat for 1h to remove the residual binder to form a degreased part.
Sintering, raising the temperature to 1900 ℃ at the heating rate of 5 ℃/min under the argon environment, preserving the heat for 30min, then raising the temperature to 2050 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 90min to obtain the required product.
Claims (10)
1. A method for forming a SiC complex component is characterized by comprising the following steps: the SiC complex component forming method comprises the following steps:
1) selecting nano SiC powder and a submicron additive, carrying out wet milling by taking deionized water as a medium, and screening after dry-pressing granulation to obtain granulated powder with the particle size of less than 15 um;
2) preparing a photo-curing slurry based on the granulated powder obtained in the step 1);
3) forming the photocuring slurry prepared in the step 2) into a blank by adopting an upper projection type photocuring indirect additive manufacturing device;
4) degreasing and sintering the blank prepared in the step 3) to obtain the SiC complex component, wherein the sintering is reaction sintering, liquid phase sintering or solid phase sintering.
2. The SiC complex member forming method according to claim 1, characterized in that: the step 1) is specifically as follows:
taking nano SiC powder and a submicron additive, wet-milling for 24-48h in a ball milling tank by taking deionized water as a medium, and screening after dry-pressing granulation to obtain granulated powder with the particle size of less than 15 um; the submicron additive is C, B 4 C、B、Al 2 O 3 、Y 2 O 3 One or more mixtures of raw materials such as rare earth oxide and the like; the pressure of the dry-pressing granulation is 80-150 MPa.
3. The SiC complex member forming method according to claim 2, characterized in that:
when the sintering in the step 4) adopts reaction sintering, the submicron additive in the step 1) is C;
when the sintering in the step 4) adopts liquid phase sintering, the submicron additive in the step 1) is Al 2 O 3 、Y 2 O 3 Or a rare earth oxide;
when the sintering in the step 4) adopts solid-phase sintering, the submicron additive in the step 1) is B 4 C. B or C.
4. The SiC complex member forming method according to claim 3, characterized in that: the step 2) is specifically as follows: mixing the photocuring binder with the granulation powder obtained in the step 1), and uniformly stirring for 5-20min to prepare photocuring slurry; the volume ratio of the light-cured binder to the granulated powder is 1: 4-1: 1.
5. the SiC complex member forming method according to claim 4, characterized in that: the light-cured adhesive comprises a matrix and a component which is soluble in water after being cured; the water-soluble component after curing is one or the combination of polyethylene glycol acrylate monoester and water-based polyurethane acrylate.
6. The SiC complex member forming method according to claim 5, characterized in that: the volume of the cured water-soluble component is A; the total volume of the cured water-soluble component and the matrix is B; and A is (10% -25%) B.
7. The SiC complex member forming method according to claim 6, characterized in that: the thickness of the layers adopted in the step 3) is 20-40 um; the curing parameters of the binder are selected during forming according to the fact that the powder consolidation thickness is 1.2-2 times of the layering thickness.
8. The SiC complex member forming method according to claim 7, characterized in that: degreasing in the step 4) is to soak the complex blank obtained in the step 3) in distilled water at the temperature of 40-80 ℃ for 2-6h, and remove water-soluble components in the photo-curing adhesive after curing; and then drying at 80 ℃, raising the temperature to 900 ℃ at the heating rate of 0.1-5 ℃/min under the argon protective atmosphere, preserving the temperature for 1-5h, removing the residual photocuring binder, and finishing degreasing to form a degreased part.
9. The SiC complex member forming method according to claim 7, characterized in that: after degreasing in the step 4), the whole carbon residue of the light-cured binder is 0-6.5% of the mass fraction of the SiC powder in the light-cured slurry, and the carbon residue in the light-cured binder participates in sintering after degreasing.
10. The SiC complex member forming method according to claim 9, characterized in that:
when the sintering in the step 4) is reaction sintering, the sintering process comprises the following steps: raising the temperature of the silicon powder and the degreased part to 1400-1700 ℃ at the heating rate of 6-10 ℃/min under the vacuum condition, and preserving the heat for 30-60min to finish sintering to obtain a SiC complex component;
when the sintering in the step 4) is liquid phase sintering, the sintering process comprises the following steps: raising the temperature to 1300 ℃ and 1900 ℃ at the heating rate of 5-8 ℃/min under the argon environment, and preserving the heat for 30-120min to finish sintering to obtain the SiC complex component;
when the sintering in the step 4) is solid-phase sintering, the sintering process comprises the following steps: raising the temperature to 1900 ℃ at the heating rate of 5-8 ℃/min under the argon or vacuum environment, preserving the heat for 30min, then raising the temperature to 2100 ℃ at the heating rate of 1-3 ℃/min, preserving the heat for 20-90min, and finishing sintering to obtain the SiC complex component.
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