CN113277853A - Laser additive manufacturing method of silicon carbide composite large-size ultra-light optical reflector - Google Patents
Laser additive manufacturing method of silicon carbide composite large-size ultra-light optical reflector Download PDFInfo
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Abstract
The invention discloses a laser additive manufacturing method of a silicon carbide composite material large-size ultra-light optical reflector, which comprises the following steps: designing an optical reflector support body structure meeting a lightweight target and a reflector service condition; preparing a high-performance silicon carbide ceramic-resin composite powder material; forming a large-size ultra-light optical reflector preform made of silicon carbide ceramic composite material; carrying out pyrolytic carbonization and reactive infiltration silicon densification treatment; growing a silicon carbide compact coating on the surface of the side of the large-size optical reflector after reaction infiltration sintering by adopting CVD; and finally, carrying out optical processing and verification. The invention has the advantages of high production efficiency, high manufacturing precision, good designability, high material utilization rate and the like, is more suitable for the efficient integral manufacturing of the large-size ultra-light optical reflector made of the silicon carbide composite material, and can overcome the limitation of manufacturing the light-weight structure of the large-size ultra-light optical reflector in the prior art.
Description
Technical Field
The invention relates to the technical field of laser additive manufacturing, in particular to a laser additive manufacturing method of a silicon carbide composite large-size ultra-light optical reflector.
Background
The demand of the modern remote sensing field for continuously improving the resolution of the space optical remote sensor enables the caliber of the reflective space optical primary mirror to be continuously increased, but the large-size optical reflector brings the problem of difficulty in the day, and therefore the demand of light weight development of the space optical reflector is generated. At present, the reflecting mirror is mostly made of metal materials such as aluminum, beryllium, nickel and the like, or various optical glasses are adopted. The aluminum and the aluminum alloy have poor thermal properties and are difficult to adapt to the space environment; beryllium and its alloys are toxic and too expensive; nickel and its alloy have poor low-temperature performance and high density; optical glass also has problems of poor rigidity and low thermal diffusivity. In recent years, silicon carbide has become one of the first choice materials for the space mirror by virtue of its advantages of high mechanical strength, low density, excellent thermal shock resistance, stable chemical properties, etc. However, silicon carbide ceramic materials are hard and brittle, and are difficult to process into complex structures required by lightweight design, such as single arch, meniscus, reverse flat, double concave and other external structures, and triangular, square, hexagonal, fan-shaped, circular, anisotropic honeycomb and other reinforcing rib structures. The lightweight structure can ensure the rigidity of the structure with lower mass, but also leads to complication of the shape of the mirror blank. If the traditional process is adopted, not only are the processing steps complicated and long in time consumption, but also most of the traditional processes can only realize open lightweight design, so that the complexity of a lightweight structure is limited. Therefore, it is urgent to find a forming method capable of satisfying the requirements of large-size silicon carbide ceramics on high precision and complex structure so as to satisfy the requirements of the silicon carbide ceramics for processing and manufacturing large-size space reflectors.
Disclosure of Invention
Based on the defects of the prior art, the technical problem to be solved by the invention is to provide the laser material additive manufacturing method of the silicon carbide composite material large-size ultra-light optical reflector, which has the advantages of high production efficiency, high manufacturing precision, good designability, high material utilization rate and the like, is more suitable for the efficient integral manufacturing of the silicon carbide composite material large-size ultra-light optical reflector, and overcomes the limitation of manufacturing a light-weight structure of the large-size ultra-light optical reflector in the prior art.
In order to solve the technical problem, the invention provides a laser additive manufacturing method of a silicon carbide composite material large-size ultra-light optical reflector, which comprises the following steps:
(1) designing an optical reflector support body structure meeting a lightweight target and a reflector service condition;
(2) preparing a high-performance silicon carbide ceramic-resin composite powder material;
(3) adopting a large-table-board powder bed selective laser sintering additive manufacturing process to form a large-size ultra-light optical reflector preform made of a silicon carbide ceramic composite material;
(4) carrying out pyrolysis carbonization and reaction melt siliconizing densification treatment on the large-size optical reflector silicon carbide ceramic composite material prefabricated body;
(5) growing a silicon carbide compact coating on the surface of the side of the large-size optical reflector after reaction infiltration sintering by adopting a Chemical Vapor Deposition (CVD) technology, wherein the thickness of the coating is more than 100 mu m;
(6) and (3) carrying out optical processing and verification on the mirror surface of the large-size optical reflector after Chemical Vapor Deposition (CVD).
Preferably, the laser additive manufacturing method of the silicon carbide composite material large-size ultra-light optical reflector provided by the invention further comprises part or all of the following technical characteristics:
as an improvement of the technical scheme, in the step (1), the optical reflector support structure is designed by using three-dimensional modeling software such as UG, Pro/E and the like.
As an improvement of the above technical solution, in the step (2), the high-performance silicon carbide ceramic-resin composite powder material comprises the following components in percentage by mass: 82-92 wt% of silicon carbide ceramic powder, 8-18 wt% of adhesive and 2-4 wt% of curing agent in mass fraction of the adhesive;
the preparation steps of the high-performance silicon carbide ceramic-resin composite powder material are as follows: dissolving an adhesive containing a certain curing agent into a methanol solution at 45-55 ℃, adding silicon carbide ceramic powder, gradually cooling the solution under stirring, separating out the adhesive on the surfaces of silicon carbide ceramic powder particles under the action of heterogeneous nucleation, taking out a thick powder aggregate, drying the thick powder aggregate at the backlight position below 40 ℃ for 12-24 hours to obtain a dry composite powder block, and grinding the dry composite powder block through a 100-mesh sieve to obtain the silicon carbide ceramic composite powder.
As an improvement of the above technical solution, the adhesive is phenolic resin or epoxy resin; the curing agent is urotropin.
As an improvement of the above technical solution, in the step (3), the parameters of the selective laser sintering additive manufacturing process are as follows: the laser power is set to 6-9W, the layering thickness is set to 0.1-0.2 mm, the printing speed is set to 1500-2000 mm/s, and the scanning interval is set to 0.1-0.2 mm.
As an improvement of the above technical solution, in the step (4), the step of pyrolysis carbonization comprises: and heating the printed large-size ultra-light optical reflector preform made of the silicon carbide ceramic composite material to 800 ℃ at a heating rate of 2 ℃/min in an argon atmosphere, and then preserving heat for 3 hours for carbonization treatment.
As an improvement of the above technical solution, in the step (4), the reaction infiltration silicon densification treatment comprises the following steps: placing silicon wafers on the upper surface and the lower surface of the carbonized large-size optical reflector preform, heating to 1500 ℃ at a heating rate of 5 ℃/min under an argon atmosphere, heating to 1650 ℃ at a heating rate of 2 ℃/min, and preserving heat for 1 hour.
As an improvement of the above technical solution, in the step (5), the process parameters of the Chemical Vapor Deposition (CVD) process are: silicon tetrachloride (SiCl)4) Being a silicon source, methane (CH)4) As a carbon source, H2As carrier gas, the deposition temperature is 1300-1600 ℃, and the deposition is carried outThe pressure is 4-10 kPa, and the deposition time is 5-20 min; SiCl4Carrying in by adopting a bubbling mode; h2The flow rate of (1) is 1500-2000 sccm; CH (CH)4The flow rate of (2) is 100-200 sccm; the molar ratio of carbon to silicon of the precursor RC to Si is 0.5-2.
As an improvement of the above technical solution, in the step (6), the optical processing method is to perform efficient grinding and polishing by an online electrolytic grinding and polishing dressing process.
As an improvement of the above technical solution, in the step (6), the verification method is to measure the mirror surface profile by using a three-dimensional profiler and calculate the roughness; measuring the surface shape precision by using a laser interferometer; the reflectance was measured using a reflectance tester. The final product has surface roughness Ra not more than 1nm, surface shape precision RMS not more than lambda/40 (lambda being 632.8nm), mirror surface with average reflectivity not less than 96% in 500-800nm wave band, integral light weight ratio not less than 80% and surface density not more than 20kg/m2。
Compared with the prior art, the technical scheme of the invention has the following beneficial effects: the method has the advantages of high production efficiency, high manufacturing precision, good designability, high material utilization rate and the like, is more suitable for the efficient integral manufacturing of the silicon carbide composite material large-size ultra-light optical reflector, can overcome the limitation of manufacturing the light-weight structure of the large-size ultra-light optical reflector in the prior art, carries out the forming of the multilayer topological structure reflector by the SLS technology, further reduces the surface density of the reflector on the premise of ensuring the rigidity and the surface shape precision, and improves the light-weight rate of the reflector to more than 80 percent.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the contents of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, the following detailed description is given in conjunction with the preferred embodiments.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings of the embodiments will be briefly described below.
FIG. 1 is a schematic flow chart of a laser additive manufacturing method of a silicon carbide composite material large-size ultra-light optical reflector according to the invention;
FIG. 2 is a three-dimensional model of a topologically optimized large-size optical reflector established in an embodiment of a laser additive manufacturing method of a large-size ultra-light optical reflector made of a silicon carbide composite material.
Detailed Description
Other aspects, features and advantages of the present invention will become apparent from the following detailed description, which, when taken in conjunction with the drawings, illustrate by way of example the principles of the invention.
A laser additive manufacturing method of a silicon carbide composite material large-size ultra-light optical reflector is shown in the attached figure 1, and comprises the following specific steps:
and designing a large-size optical reflector three-dimensional model. And carrying out lightweight design by using UG, Pro/E and other three-dimensional modeling software, establishing a topology optimization large-size optical reflector three-dimensional model as shown in figure 2, and exporting an STL format file for later use.
Preparing the silicon carbide ceramic-resin composite powder material. Firstly, dissolving 36g of adhesive (comprising 35.28g of phenolic resin and 0.72g of urotropine) into a methanol solution at 55 ℃, then adding 164g of silicon carbide powder, gradually cooling the solution under stirring, utilizing heterogeneous nucleation to separate out the adhesive and cover the surfaces of silicon carbide ceramic powder particles, then taking out thick powder aggregates, drying the thick powder aggregates at a low-temperature backlight position for 12-24 hours to obtain dry composite powder blocks, and then grinding and sieving to obtain the silicon carbide ceramic-resin composite powder material.
And printing the silicon carbide large-size optical reflector blank. Firstly, the previous large-size optical reflector three-dimensional model is led into an SLS 3D printer, the preheating temperature is set to be 65 ℃, the filling power is set to be 6.5w, the profile power is set to be 4w, the scanning speed is 1750mm/s, the layering thickness is 0.15mm, and the scanning distance is 0.15 mm. And putting the prepared composite powder into powder cylinders at two sides, and starting printing. And preheating, printing and cooling to obtain a large-size optical reflector blank. And (3) removing powder by using blast air flow to obtain a final silicon carbide large-size optical reflector blank, wherein the bending strength of the final silicon carbide large-size optical reflector blank is more than or equal to 2MPa, and the strength of the final silicon carbide large-size optical reflector blank is enough for carrying out carbonization and melt siliconizing processes.
And carbonizing the silicon carbide large-size optical reflector blank. And (3) placing the prepared silicon carbide large-size optical reflector blank in a boron carbide crucible, then placing the silicon carbide large-size optical reflector blank in a tubular furnace, heating the silicon carbide large-size optical reflector blank to 800 ℃ (higher than the pyrolysis temperature of phenolic resin) at the heating rate of 2 ℃/min in the argon atmosphere, and then preserving the heat for 3 hours for carbonization treatment.
And (3) melting and siliconizing the silicon carbide large-size optical reflector blank. Placing the carbonized large-size optical reflector blank in a boron carbide crucible, placing silicon wafers on the upper surface and the lower surface of the silicon carbide blank, heating to 1500 ℃ at a heating rate of 5 ℃/min under an argon atmosphere, heating to 1650 ℃ at a heating rate of 2 ℃/min, and carrying out heat preservation for 1 hour to carry out melt siliconizing treatment to obtain a large-size optical reflector preform, wherein the bending strength of the large-size optical reflector preform is more than or equal to 250MPa, and the elastic modulus of the large-size optical reflector preform is more than or equal to 250 GPa.
CVD treatment is carried out on the silicon carbide large-size optical reflector blank. The technological parameters of CVD treatment on the sintered silicon carbide large-size optical reflector are as follows: silicon tetrachloride (SiCl)4) Being a silicon source, methane (CH)4) As a carbon source, H2As carrier gas, deposition temperature is 1500 deg.C, deposition pressure is 10kPa, and deposition time is 20 min; SiCl4Carrying in by adopting a bubbling mode; the flow rate of H2 was 2000 sccm; CH (CH)4The flow rate of (2) is 200 sccm; the precursor carbon/silicon molar ratio RC/Si molar ratio is 1.
And (3) polishing the mirror surface of the large-size silicon carbide optical reflector. Carrying out on-line electrolytic polishing and finishing and other process treatments on the mirror surface of the silicon carbide large-size optical reflector after CVD treatment, and finally obtaining the mirror surface with the surface roughness Ra of less than or equal to 1nm, the surface shape precision RMS of less than or equal to lambda/40 (lambda is 632.8nm), the 500-plus 800-nm wave band average reflectivity of more than or equal to 96 percent, the integral lightweight rate of the reflector of more than or equal to 80 percent, and the surface density of less than or equal to 20kg/m2。
The raw materials listed in the invention, the upper and lower limits and interval values of the raw materials of the invention, and the upper and lower limits and interval values of the process parameters (such as temperature, time and the like) can all realize the invention, and the examples are not listed.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (10)
1. A laser additive manufacturing method of a silicon carbide composite material large-size ultra-light optical reflector is characterized by comprising the following steps:
(1) designing an optical reflector support body structure meeting a lightweight target and a reflector service condition;
(2) preparing a high-performance silicon carbide ceramic-resin composite powder material;
(3) adopting a large-table-board powder bed selective laser sintering additive manufacturing process to form a large-size ultra-light optical reflector preform made of a silicon carbide ceramic composite material;
(4) carrying out pyrolytic carbonization and reactive infiltration silicon densification treatment on the large-size optical reflector silicon carbide ceramic composite material preform;
(5) growing a silicon carbide compact coating on the surface of the large-size optical reflector on the mirror surface side after reaction infiltration sintering by adopting a chemical vapor deposition technology, wherein the thickness of the coating is more than 100 mu m;
(6) and (4) carrying out optical processing and verification on the mirror surface of the large-size optical reflector after chemical vapor deposition.
2. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: and (1) designing the optical reflector support body structure by using UG, Pro/E and other three-dimensional modeling software.
3. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (2), the high-performance silicon carbide ceramic-resin composite powder material comprises the following components in percentage by mass: 82-92 wt% of silicon carbide ceramic powder, 8-18 wt% of adhesive and 2-4 wt% of curing agent in mass fraction of the adhesive;
the preparation steps of the high-performance silicon carbide ceramic-resin composite powder material are as follows: dissolving an adhesive containing a certain curing agent into a methanol solution at 45-55 ℃, adding silicon carbide ceramic powder, gradually cooling the solution under stirring, separating out the adhesive on the surfaces of silicon carbide ceramic powder particles under the action of heterogeneous nucleation, taking out a thick powder aggregate, drying the thick powder aggregate at the backlight position below 40 ℃ for 12-24 hours to obtain a dry composite powder block, and grinding the dry composite powder block through a 100-mesh sieve to obtain the silicon carbide ceramic composite powder.
4. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 3, characterized in that: the adhesive is phenolic resin or epoxy resin; the curing agent is urotropin.
5. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (3), the parameters of the selective laser sintering additive manufacturing process are as follows: the laser power is set to 6-9W, the layering thickness is set to 0.1-0.2 mm, the printing speed is set to 1500-2000 mm/s, and the scanning interval is set to 0.1-0.2 mm.
6. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (4), the step of pyrolysis and carbonization comprises the following steps: and heating the printed large-size ultra-light optical reflector preform made of the silicon carbide ceramic composite material to 800 ℃ at a heating rate of 2 ℃/min in an argon atmosphere, and then preserving heat for 3 hours for carbonization treatment.
7. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (4), the reaction infiltration silicon densification treatment comprises the following steps: placing silicon wafers on the upper surface and the lower surface of the carbonized large-size optical reflector preform, heating to 1500 ℃ at a heating rate of 5 ℃/min under an argon atmosphere, heating to 1650 ℃ at a heating rate of 2 ℃/min, and preserving heat for 1 hour.
8. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (5), the process parameters of the chemical vapor deposition treatment are as follows: silicon tetrachloride as silicon source, methane as carbon source, and H2The carrier gas is used, the deposition temperature is 1300-1600 ℃, the deposition pressure is 4-10 kPa, and the deposition time is 5-20 min; SiCl4Carrying in by adopting a bubbling mode; h2The flow rate of (1) is 1500-2000 sccm; CH (CH)4The flow rate of (2) is 100-200 sccm; the molar ratio of carbon to silicon of the precursor RC to Si is 0.5-2.
9. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (6), the optical processing method is to perform efficient grinding and polishing by an online electrolytic grinding and polishing finishing process.
10. The laser additive manufacturing method of the silicon carbide composite large-size ultra-light optical reflector according to claim 1, characterized in that: in the step (6), the verification method is to measure the mirror surface profile by using a three-dimensional profile meter and calculate the roughness; measuring the surface shape precision by using a laser interferometer; the reflectance was measured using a reflectance tester.
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| CN117735992A (en) * | 2023-12-20 | 2024-03-22 | 扬州北方三山工业陶瓷有限公司 | Preparation method of lightweight ceramic reflector |
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