CN116332655A - Ceramic arm and preparation method and application thereof - Google Patents

Ceramic arm and preparation method and application thereof Download PDF

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Publication number
CN116332655A
CN116332655A CN202310314481.2A CN202310314481A CN116332655A CN 116332655 A CN116332655 A CN 116332655A CN 202310314481 A CN202310314481 A CN 202310314481A CN 116332655 A CN116332655 A CN 116332655A
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China
Prior art keywords
ceramic
powder
arm
degreasing
blank body
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陈文彬
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Hunan Sheng Ci Technology Co ltd
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Hunan Sheng Ci Technology Co ltd
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    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B65CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65GTRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
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Abstract

The invention provides a ceramic arm, a preparation method and application thereof, and relates to the technical field of ceramic arms. According to the preparation method of the ceramic arm, the first blank body and the second blank body are directly pressed out by using the first die and the second die, and then the first blank body and the second blank body are covered and then are hot-pressed to form a closed air passage; the invention also provides a ceramic arm, which is prepared by adopting the preparation method of the ceramic arm, and the prepared ceramic arm has high strength, and the formed airway has the advantages of smooth and level surface, high precision, small error, uniform airway flow and longer service life.

Description

Ceramic arm and preparation method and application thereof
Technical Field
The invention belongs to the technical field of ceramic arms, and relates to a ceramic arm, a preparation method and application thereof.
Background
Ceramic arms currently rely mainly on a combination of ceramic plates to form the airway, typically secured between the plates by an organic or inorganic adhesive. However, as the service life of the ceramic arm increases, the adhesive ages, resulting in poor air tightness of the air passage of the ceramic arm, and further shortened service life. The temperature of the adhesive is greatly affected, the organic adhesive is generally used below 300 ℃, the high-temperature inorganic adhesive is generally used below 800 ℃, and if the use temperature exceeds the temperature of the organic adhesive or the inorganic adhesive, air leakage is inevitably generated, so that the normal use of a ceramic arm is affected.
In order to avoid the influence of the binder on the ceramic arm, the prior art also provides a preparation method of the ceramic arm, specifically, ceramic raw materials and an air passage model prepared by adopting low-melting-point substances (such as paraffin) are molded together, and the air passage model is directly pressed inside to obtain a blank body with the air passage model; and then burning the air passage model, and sintering the blank body with the air passage model removed to obtain the ceramic arm with the air passage. Compared with a ceramic arm formed by combining ceramic plates, the ceramic arm manufactured by the manufacturing method does not need to be bonded and fixed, and the problem of air leakage of an air passage cannot occur in the follow-up process. However, in practice, it is found that powder particles adhere to the air passage model, uneven air passages can occur in the pressing process, pits are formed in the air passage wall, the arm is difficult to clean, the air passage phenomenon can be adhered due to dust particle sintering, and the product is polluted, so that the use is affected.
In view of this, the present invention has been made.
Disclosure of Invention
Aiming at the defects and defects existing in the prior art, the invention aims to provide a preparation method of a ceramic arm, which directly utilizes a first die and a second die to heat and press air passages of a first blank body and a second blank body, and then covers the first blank body and the second blank body and then thermally presses the first blank body and the second blank body to form a closed air passage.
In order to achieve the above purpose, the following technical scheme is adopted:
the invention provides a preparation method of a ceramic arm, which comprises the following steps:
(a) Providing granulated powder formed by ceramic powder and an auxiliary agent;
providing a first mold and a second mold for molding a ceramic arm to be prepared, wherein one of the first mold and the second mold has the same air passage structure as the ceramic arm to be prepared;
(b) Adding the granulated powder into a first die and a second die respectively, then heating and pressurizing, cooling and demolding to obtain a first blank body and a second blank body, wherein one of the first blank body and the second blank body has the air passage structure;
(c) Covering the first blank body and the second blank body, and then performing heating and pressurizing treatment to bond the first blank body and the second blank body to obtain an arm blank body with a closed air passage structure;
(d) Degreasing and sintering the arm blank to obtain the ceramic arm.
Furthermore, on the basis of the above technical solution of the present invention, in the step (a), the ceramic powder includes at least one of high-purity alumina powder, alumina antistatic composite ceramic powder, zirconia antistatic composite ceramic powder, or silicon carbide composite ceramic powder.
Further, on the basis of the above technical solution of the present invention, in the step (a), the auxiliary agent includes at least two of a plasticizer, a flux, a lubricant or a coupling agent;
preferably, the plasticizer comprises at least one of polypropylene, dibutyl phthalate, or polyvinyl butyral;
preferably, the flux comprises paraffin wax and/or polyethylene glycol;
preferably, the lubricant comprises at least one of stearic acid, stearyl alcohol, or polyethylene wax;
preferably, the coupling agent comprises an aluminate and/or titanate.
Furthermore, on the basis of the technical scheme of the invention, in the step (a), the preparation method of the granulating powder comprises the following steps:
mixing ceramic powder and an auxiliary agent, then carrying out high-temperature kneading, cooling and solidifying the kneaded material, and then crushing to obtain granulated powder;
preferably, the high temperature kneading is carried out at a temperature of 160 to 220℃for a period of 2 to 6 hours.
Furthermore, on the basis of the technical scheme, in the step (b), the heating temperature is 140-190 ℃;
and/or the pressurizing pressure is 5-30MPa, and the pressure is maintained for 5-10min.
Further, on the basis of the technical scheme, in the step (c), the heating temperature is 120-160 ℃;
and/or the pressurizing pressure is 3-50MPa, and the pressure is maintained for 3-10min.
Furthermore, on the basis of the technical scheme, in the step (d), the degreasing comprises the steps of degreasing by a solvent and then degreasing by embedding powder;
preferably, the solvent used for degreasing comprises at least one of deionized water, acetone, petroleum ether, kerosene or heptane;
preferably, the temperature of the solvent degreasing is 40-50 ℃, and the time of the solvent degreasing is 6-36h;
preferably, the embedding powder used for embedding powder degreasing comprises alumina;
preferably, the temperature of the powder burying degreasing is 400-600 ℃, and the temperature of the powder burying degreasing is 40-60h.
Furthermore, on the basis of the technical scheme, in the step (d), the sintering temperature is 1300-1700 ℃, the time required for heating to the sintering temperature is 75-85h, and the heat preservation time at the sintering temperature is 5-15h.
The invention also provides a ceramic arm, which is prepared by adopting the preparation method of the ceramic arm.
The invention also provides application of the ceramic arm in the field of semiconductor chip wafer handling equipment.
Compared with the prior art, the technical scheme of the invention has at least the following technical effects:
(1) The invention provides a preparation method of a ceramic arm, which comprises the steps of adding granulated powder formed by ceramic powder and an auxiliary agent into a first die and a second die respectively, heating and pressurizing, cooling and demolding to obtain a first blank body and a second blank body, covering the blank bodies, heating and pressurizing to bond the first blank body and the second blank body to obtain an arm blank body with a closed air passage structure, degreasing and sintering the arm blank body to obtain the ceramic arm; the preparation method directly utilizes the first die and the second die to heat and extrude the first blank body and the second blank body, and then the first blank body and the second blank body are covered and then thermally pressed to form a closed air passage.
(2) The invention also provides a ceramic arm, which is prepared by adopting the preparation method of the ceramic arm. In view of the advantages of the preparation method, the prepared ceramic arm has high strength, and the formed airway has the advantages of smooth and level surface, high precision, small error, uniform airway flow and longer service life.
(3) The invention also provides application of the ceramic arm, and has good application prospect in the field of semiconductor chip wafer handling equipment in view of the advantages of the ceramic arm.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention. It will be apparent to those skilled in the art that the examples are merely to aid in understanding the invention and are not to be construed as a specific limitation thereof. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The process parameters for the specific conditions not noted in the examples below are generally as usual.
The endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be obtained in combination with each other between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point values, and are to be considered as specifically disclosed in the present invention.
According to a first aspect of the present invention, there is provided a method of manufacturing a ceramic arm, comprising the steps of:
(a) Providing granulated powder formed by ceramic powder and an auxiliary agent;
providing a first die and a second die for molding a ceramic arm to be prepared, wherein one of the first die and the second die has the same air passage structure as the ceramic arm to be prepared;
(b) Adding the granulated powder into a first die and a second die respectively, then heating and pressurizing, cooling and demolding to obtain a first blank body and a second blank body, wherein one of the first blank body and the second blank body has the air passage structure;
(c) Covering the first blank body and the second blank body, and then performing heating and pressurizing treatment to bond the first blank body and the second blank body to obtain an arm blank body with a closed air passage structure;
(d) Degreasing and sintering the arm blank to obtain the ceramic arm.
Specifically, in the step (a), the ceramic powder may be formed by compounding a single kind of ceramic raw material or different kinds of ceramic raw materials. The addition of the auxiliary agent is helpful for ensuring that the blank has certain strength and toughness and different glue mixing temperatures, so that the step degreasing is realized, and the blank cracking caused by centralized degreasing at a single temperature is avoided.
As the forming die for the ceramic arm to be prepared, two blanks can be prepared by adopting the first die and the second die, and the structure of the two blanks after being covered is the same as that of the ceramic arm to be prepared.
Step (b) and step (c) are forming processes of the ceramic arm to be prepared.
In the step (b), after the granulated powder is added into the first die and the second die, the two dies are heated to enable the granulated powder to be melted, then the pressure treatment is carried out for pressure pressing, after the pressurization is finished, the temperature is reduced, the first die is demolded to obtain a first blank body, and the second die is demolded to obtain a second blank body.
In the step (c), the first green body and the second green body are covered and then have the same structure as the ceramic arm to be prepared. Different from the mode of bonding by adopting the adhesive in the prior art, the first green body and the second green body are not bonded by adopting the adhesive, but the first green body and the second green body after being covered are heated and pressurized, and under the action of certain temperature and pressure, the first green body and the second green body are slightly melted and bonded together, so that the air passage structure on the first green body and the second green body is closed, and the arm green body is obtained.
In the step (d), since part of the organic auxiliary agent remains in the arm blank, degreasing treatment is required to be performed on the arm blank. And (5) sintering after degreasing to obtain the ceramic arm.
The invention provides a preparation method of a ceramic arm, which comprises the steps of adding granulated powder formed by ceramic powder and an auxiliary agent into a first die and a second die respectively, heating and pressurizing, cooling and demolding to obtain a first blank body and a second blank body, covering the blank bodies, heating and pressurizing to bond the first blank body and the second blank body to obtain an arm blank body with a closed air passage structure, degreasing and sintering the arm blank body to obtain the ceramic arm; the preparation method directly utilizes the first die and the second die to heat and press the air passage of the first blank body or the second blank body, and then the first blank body and the second blank body are covered and then are hot pressed to form a closed air passage.
There is a further optimization for the kind of ceramic powder.
As an optional embodiment of the present invention, in step (a), the ceramic powder includes at least one of high-purity alumina powder, alumina antistatic composite ceramic powder, zirconia antistatic composite ceramic powder, or silicon carbide composite ceramic powder.
In the present invention, the high purity alumina powder means alumina powder having a purity of 99.8% or more.
As the alumina antistatic composite ceramic powder or the zirconia antistatic composite ceramic powder is used as the raw material of the ceramic arm, the ceramic arm has good and long-term antistatic performance, and the problem that the antistatic performance is reduced due to the fact that an antistatic coating arranged on the surface of the ceramic arm is easy to age and abrade in the prior art is solved.
As an alternative embodiment of the invention, the alumina antistatic composite ceramic powder comprises the following raw materials in percentage by mass:
65-95% of aluminum oxide, 3-30% of titanium dioxide, 0.2-1.5% of silicon dioxide, 0.2-3% of sintering aid, 0-5% of tin oxide and 0-1% of nickel oxide; wherein the sintering aid comprises at least one of yttrium oxide, calcium oxide, niobium oxide or cerium oxide.
Alumina typically, but not limitatively, has a mass fraction of 65%, 68%, 70%, 75%, 78%, 80%, 85%, 88%, 90% or 95%; titanium dioxide typically, but not limited to, 3%, 5%, 10%, 12%, 15%, 20%, 22%, 25%, 28% or 30% by mass; silica typically, but not limitatively, has a mass fraction of 0.2%, 0.5%, 1.0% or 1.5%; the burn aid is typically, but not limited to, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5% or 3.0% by mass; tin oxide typically, but not limited to, is 0%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0% by mass; nickel oxide typically, but not by way of limitation, is 0%, 0.2%, 0.5%, 0.8% or 1.0% by mass.
As an alternative embodiment of the invention, the zirconia antistatic composite ceramic powder comprises the following raw materials in percentage by mass:
10-90% of cerium-yttrium stabilized zirconia, 1-5% of aluminum oxide, 5-85% of zinc oxide, 0.05-5% of nickel monoxide, 0.02-5% of titanium dioxide, 0.1-5% of silicon dioxide, 0.02-5% of calcium oxide and 0.1-3% of strontium oxide.
Cerium yttrium-stabilized zirconia refers to ceria and yttria-stabilized zirconia, the mass ratio of ceria and yttria in zirconia is not particularly limited, and typical but non-limiting mass fractions of ceria-stabilized zirconia are 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% or 90%; typical but non-limiting mass fractions of aluminum oxide are 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0%; zinc oxide typically, but not limited to, is 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% or 85% by mass; typical but non-limiting mass fractions of nickel monoxide are 0.05%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0%; titanium dioxide typically, but not limited to, is 0.02%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0% by mass; silica typically, but not limited to, has a mass fraction of 0.1%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0%; typical, but non-limiting, mass fractions of calcium oxide are 0.02%, 0.2%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5% or 5.0%; strontium oxide typically, but not by way of limitation, is 0.1%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5% or 3.0% by mass.
As an alternative embodiment of the invention, the silicon carbide composite ceramic powder comprises the following raw materials in percentage by mass:
90-99.5% of silicon carbide, 0.1-1% of yttrium oxide, 0.1-1.5% of calcium fluoride, 0.1-5.5% of boron carbide and 0.2-2% of aluminum oxide.
Silicon carbide typically but not limited to 90%, 92%, 94%, 95%, 96%, 98%, 99% or 99.5% by mass, yttria typically but not limited to 0.1%, 0.2%, 0.5%, 0.6%, 0.8% or 1.0% by mass, calcium fluoride typically but not limited to 0.1%, 0.2%, 0.5%, 0.6%, 0.8%, 1.0%, 1.2% or 1.5% by mass, and boron carbide typically but not limited to 0.1%, 0.5%, 1.0%, 1.5%, 2.0%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%, 5.0% or 5.5% by mass; typical, but non-limiting, mass fractions of alumina are 0.2%, 0.5%, 1.0%, 1.5% or 2.0%.
As an alternative embodiment of the present invention, in step (a), the auxiliary agent comprises at least two of a plasticizer, a flux, a lubricant or a coupling agent, preferably comprises a plasticizer, a flux, a lubricant and a coupling agent.
The plasticizer is mainly used for improving the strength of the blank. As an alternative embodiment of the present invention, the plasticizer comprises at least one of polypropylene, polyethylene, dibutyl phthalate, or polyvinyl butyral.
Preferably, the mass of plasticizer is 0.3-10% (e.g., 0.3%, 0.5%, 1.0%, 2.0%, 3.0%, 4.0%, 5.0%, 6.0%, 7.0%, 8.0%, 9.0%, or 10.0%) of the mass of the ceramic powder.
As an alternative embodiment of the present invention, the flux comprises paraffin wax and/or polyethylene glycol, preferably paraffin wax and polyethylene glycol. Paraffin is used as a low-temperature flux, polyethylene glycol is used as a high-temperature flux, and the paraffin and the polyethylene glycol are matched to realize the glue discharging degreasing of different fluxes at different temperatures.
Preferably, the flux is 2-8% (e.g., 2%, 3%, 4%, 5%, 6%, 7%, or 8%) of the mass of the ceramic powder.
The lubricant can improve the lubricity of the ceramic powder. As an alternative embodiment of the present invention, the lubricant comprises at least one of stearic acid, stearyl alcohol, or polyethylene wax.
Preferably, the lubricant comprises 0.1-1.5% (e.g., 0.1%, 0.2%, 0.4%, 0.5%, 0.6%, 0.8%, 1%, 1.2%, 1.4%, or 1.5%) of the ceramic powder mass.
The coupling agent may improve the fluidity of the ceramic powder and the flux, and as an alternative embodiment of the present invention, the coupling agent includes aluminate and/or titanate.
Preferably, the mass of the coupling agent is 0.1-1% (e.g., 0.1%, 0.2%, 0.4%, 0.5%, 0.6%, 0.8%, or 1%) of the mass of the ceramic powder.
As an alternative embodiment of the present invention, in the step (a), the method for preparing the granulated powder comprises the steps of:
mixing ceramic powder and an auxiliary agent, then carrying out high-temperature kneading, cooling and solidifying the kneaded material, and then crushing to obtain granulated powder.
As an alternative embodiment of the invention, the high temperature kneading is carried out at a temperature of 160-220℃for a period of 2-6 hours. Typical but non-limiting high temperature kneading temperatures are 160 ℃, 170 ℃, 180 ℃, 190 ℃,200 ℃, 210 ℃ or 220 ℃, and typical but non-limiting high temperature kneading times are 2 hours, 3 hours, 4 hours, 5 hours or 6 hours.
As an alternative embodiment of the present invention, in step (b), the heating temperature is 140-190 ℃; and/or the pressurizing pressure is 5-30MPa, and the pressure maintaining time is 5-10min. Typical but non-limiting heating temperatures are 140 ℃, 150 ℃, 160 ℃, 170 ℃, 180 ℃, or 190 ℃; typical but non-limiting heating pressures are 5MPa, 6MPa, 8MPa, 10MPa, 15MPa, 18MPa, 20MPa, 22MPa, 25MPa, 28MPa or 30MPa; typical, but non-limiting, dwell times are 5, 6, 8, 9 or 10 minutes.
As an alternative embodiment of the present invention, in step (c), the heating temperature is 120-160 ℃; and/or the pressurizing pressure is 3-50MPa, and the pressure maintaining time is 3-10min. Typical but non-limiting heating temperatures are 120 ℃, 130 ℃, 140 ℃, 150 ℃ or 160 ℃; typical but non-limiting heating pressures are 3MPa, 5MPa, 10MPa, 15MPa, 18MPa, 20MPa, 22MPa, 25MPa, 28MPa, 30MPa, 32MPa, 35MPa, 40MPa, 42MPa, 45MPa or 50MPa; typical, but non-limiting, dwell times are 3min, 4min, 5min, 6min, 8min, or 10min.
In an alternative embodiment of the present invention, in step (d), degreasing includes degreasing with a solvent followed by degreasing with buried powder. Soaking the blank body with solvent (such as kerosene or heptane) to remove partial paraffin and stearic acid, burying powder for degreasing, removing PEG at low temperature, and removing the rest organic matters at 200-500 ℃ to avoid the concentrated decomposition of the organic matters and the cracking of the volume-expanded blank body.
As an alternative embodiment of the present invention, the solvent used for solvent degreasing includes at least one of deionized water, acetone, petroleum ether, kerosene, or heptane.
As an alternative embodiment of the invention, the temperature of the solvent degreasing is 40-50 ℃ and the time of the solvent degreasing is 6-36h; typical, but non-limiting, solvent degreasing temperatures are 40 ℃, 42 ℃, 44 ℃, 45 ℃, 48 ℃, or 50 ℃; typical, but non-limiting, solvent degreasing times are 6h, 10h, 12h, 18h, 24h, 28h, 32h, or 36h.
As an alternative embodiment of the present invention, the embedding powder used for embedding powder degreasing includes alumina embedding powder.
As an alternative embodiment of the invention, the temperature of the powder burying degreasing is 400-600 ℃, and the temperature of the powder burying degreasing is 40-60h. Typical, but non-limiting, temperatures for powder embedding degreasing are 400 ℃, 420 ℃, 440 ℃, 450 ℃, 480 ℃, 500 ℃, 520 ℃, 540 ℃, 550 ℃, 580 ℃, or 600 ℃; typical, but non-limiting, solvent degreasing times are 40h, 42h, 45h, 48h, 50h, 52h, 55h, 58h, or 60h.
As an alternative embodiment of the invention, in the step (d), the sintering temperature is 1300-1700 ℃, the time required for heating to the sintering temperature is 75-85h, and the time for maintaining at the sintering temperature is 5-15h. Typical but non-limiting sintering temperatures are 1300 ℃, 1350 ℃, 1400 ℃, 1550 ℃, 1500 ℃, 1550 ℃, 1600 ℃, 1650 ℃ or 1700 ℃, and typical but non-limiting times required to raise the temperature to the sintering temperature are 75h, 78h, 80h, 82h or 85h. The sintering time required at the sintering temperature (1300-1700 ℃) is, for example, 5h, 6h, 8h, 10h, 12h or 15h.
As an alternative embodiment of the present invention, the step of finishing the sintered product after sintering in step (d) is further included to obtain the ceramic arm.
The finishing comprises the steps of grinding, polishing and the like.
According to a second aspect of the present invention, there is also provided a ceramic arm manufactured by the above-mentioned manufacturing method of the ceramic arm.
In view of the advantages of the preparation method, the ceramic arm has high strength, and the formed airway has the advantages of smooth and level surface, high precision, small error, uniform airway flow, difficult air leakage and long service life.
According to a third aspect of the present invention, there is also provided the use of the ceramic arm described above in the field of semiconductor chip wafer handling equipment.
In view of the advantages of the ceramic arm, the ceramic arm has good application prospect in the field of semiconductor chip wafer handling equipment.
The present invention will be described in further detail with reference to specific examples and comparative examples.
Example 1
The embodiment provides a preparation method of a ceramic arm, which comprises the following steps:
(a) Providing granulated powder formed by ceramic powder (high-purity alumina powder) and an auxiliary agent;
83.5% of high-purity alumina powder (purity is 99.8%), 16.5% of auxiliary agent (wherein, 5% of Paraffin (PW), 8% of Polyethylene (PE), 2% of polyethylene glycol (PEG), 1% of stearic acid and 0.5% of aluminate) are mixed and melted, the mixture is placed in a mixing mill and stirred uniformly, the mixture is heated to 200 ℃ to melt the auxiliary agent, and is kneaded and sheared uniformly with the high-purity alumina powder at a speed of 160 revolutions per minute for 4 hours, the uniformly mixed material is taken out in a heated state, cooled and solidified in a container, the solidified material is crushed into a mixture by a jaw crusher, and the mixture is sieved to ensure that particles are below 4 meshes, so that the granulated powder is obtained.
A first mold and a second mold for molding a ceramic arm to be prepared are provided, the first mold having the same airway structure as the ceramic arm to be prepared.
(b) And adding the granulated powder into a first die and a second die respectively, heating the first die and the second die at 190 ℃ for 15min to uniformly melt the granulated powder, pressurizing the granulated powder for pressure pressing at 8MPa, maintaining the pressure for 5min after pressing, cooling to 100 ℃, and demolding to obtain a first blank body and a second blank body with air passage structures.
(c) And (3) covering (superposing) the first blank body and the second blank body, then placing into a mold, heating and pressurizing to bond the first blank body and the second blank body, keeping the pressure for 10min after pressing at the heating temperature of 150 ℃ and the pressure of 3MPa, and taking out the mold after cooling to obtain the arm blank body with the closed air passage structure.
(d) Soaking the arm blank in n-heptane for degreasing at 50 ℃ for 9 hours, removing part of PW and PEG, taking out the blank, putting the blank into an alumina crucible, putting alumina embedded powder (particle size is 3-5 mu m), heating to 60 ℃ -120 ℃ -200 ℃ -260 ℃ -330 ℃ -600 ℃, and preserving the temperature for 5 hours at each temperature point, wherein the total degreasing time is 60 hours (comprising the heating time and the preserving time of each temperature point) so as to remove the rest PW, PEG, PE, stearic acid and aluminate;
and (3) placing the degreased arm blank body into a sintering furnace for sintering, heating to the sintering temperature of 1620 ℃, keeping the temperature for 80 hours at the sintering temperature, processing the sintered product for 6 hours at the temperature of 1620 ℃, performing cutting flat grinding, peripheral grinding, CNC (computerized numerical control) processing and polishing to obtain the ceramic arm.
Example 2
The present example provides a method for manufacturing a ceramic arm, and the remaining steps and process parameters are the same as those of example 1, except that the ceramic powder in step (a) is replaced with zirconia antistatic composite ceramic powder from high-purity alumina powder.
The zirconia antistatic composite ceramic powder comprises the following components in percentage by mass:
81% of cerium yttrium stabilized zirconia, 14% of zinc oxide, 1.5% of aluminum oxide, 1% of silicon dioxide, 1.5% of titanium dioxide, 0.5% of calcium oxide, 0.2% of strontium oxide and 0.3% of nickel monoxide.
The batching method of the zirconia antistatic composite ceramic powder comprises the following steps:
(1) Weighing cerium-yttrium stabilized zirconia, zinc oxide, aluminum oxide, silicon dioxide, titanium dioxide, calcium oxide, strontium oxide and nickel monoxide according to a proportion, putting the mixture into a ball milling tank, adding zirconia grinding balls, deionized water and a dispersing agent (ammonium citrate, the mass of which accounts for 0.3 percent of that of the zirconia antistatic composite ceramic powder), and mixing: ball: the water mass ratio is 1:3:0.9, the ball mill grinds for 60 hours at the rotating speed of 360r/min, then an adhesive (with the brand of PB-72 and the mass of 0.5 percent of the zirconia antistatic composite ceramic powder) is added into the ball-milled material, ball-milling and mixing are continued for 4 hours, and the slurry is taken out to finish the batching;
(2) And (3) pumping the ingredients obtained in the step (1) into a spray granulation tower by a peristaltic pump for drying and granulating, wherein the drying and granulating temperature is 110 ℃, sieving the granulated powder by a 100-mesh sieve, and taking undersize products to obtain the zirconia antistatic composite ceramic powder.
Example 3
The present example provides a method for manufacturing a ceramic arm, and the remaining steps and process parameters are the same as those of example 1, except that the ceramic powder in step (a) is replaced with alumina antistatic composite ceramic powder.
The alumina antistatic composite ceramic powder comprises the following components in percentage by mass:
93% of aluminum oxide, 5% of titanium dioxide, 0.5% of silicon dioxide, 0.5% of sintering aid calcium oxide, 0.8% of tin oxide and 0.2% of nickel oxide.
The batching method of the alumina antistatic composite ceramic powder comprises the following steps:
(1) Placing the alumina antistatic composite ceramic powder into a ball milling tank, adding water and a dispersing agent, ball milling for 60 hours at a rotating speed of 260r/min, adding an adhesive, and continuing ball milling for 5-15 hours to obtain slurry;
wherein the dispersing agent is ammonium citrate, the mass of the ammonium citrate is 0.3wt% of the total amount of all components in the alumina antistatic composite ceramic powder, the adhesive is PB-72, the mass of PB-72 is 0.5wt% of the total amount of all components in the alumina antistatic composite ceramic powder, and the volume ratio of the balls, the materials and the water is 3:1:0.5.
(2) Sieving the slurry with 160 mesh sieve, spray granulating, and sieving the powder obtained by spray granulating with double-layer sieve to obtain aluminum oxide antistatic composite ceramic powder;
wherein, the upper layer screen mesh number of the double-layer screen is 60 meshes, and the lower layer screen mesh number is 120 meshes;
the spray granulation process comprises the following steps: the inlet temperature is 300 ℃, the outlet temperature is 120 ℃, the negative pressure is 60Pa, the frequency of the atomizer is 20HZ, the rotating speed of the atomizer is 9000r/min, and the feeding pump speed is 25mL/min.
Example 4
The present example provides a method for manufacturing a ceramic arm, and the remaining steps and process parameters are the same as those of example 1, except that the ceramic powder in step (a) is replaced by a silicon carbide composite ceramic powder.
The silicon carbide composite ceramic powder comprises the following components in percentage by mass: 96% of silicon carbide, 1% of yttrium oxide, 0.2% of calcium fluoride, 1.3% of boron carbide and 1.5% of aluminum oxide.
The batching method of the silicon carbide composite ceramic powder comprises the following steps:
(1) Drying the magnesium silicide powder in a vacuum oven at 120 ℃ for 12 hours;
(2) Under the protection of argon atmosphere, firstly loading 1g of magnesium silicide into a ball milling tank, then placing grinding balls into the ball milling tank and sealing, wherein the mass ratio of the grinding balls to the materials is 30:1; after vacuuming, 5bar CO is introduced into the ball milling tank 2 And (3) continuously ball-milling the ball-milling tank at a rotating speed of 300rpm for 6 hours under the condition of room temperature by using gas. After the reaction is finished, taking out a solid product, sequentially soaking the solid product in 0.5mol/L dilute hydrochloric acid and 0.1mol/L hydrofluoric acid, filtering the solid product, washing the solid product with deionized water until the solution is neutral, and drying and cooling the solid product at 120 ℃ to obtain silicon carbide powder;
(3) Weighing the prepared silicon carbide, yttrium oxide, calcium fluoride, boron carbide and aluminum oxide according to the weight ratio, ball-milling and mixing, adding dispersant polyacrylamide (the dosage of which is 0.5 percent of the mass of the silicon carbide composite ceramic powder), and performing spray granulation to obtain the silicon carbide composite ceramic powder.
Comparative example 1
The comparative example provides a preparation method of a ceramic arm, comprising the following steps:
(1) Placing commercial high-purity alumina granulated powder with the concentration of more than 99.98% into a die for compression molding to obtain a pressed plate;
(2) Placing the pressed board obtained in the step (1) into a high-temperature sintering furnace for sintering, heating the sintering system to 1600 ℃ for 0.80h, and preserving heat for 6h to obtain a ceramic board;
(3) Firstly, flatly grinding two planes of the ceramic plate obtained in the step (2), then cutting the ceramic plate into plates with the thickness required by arms, then CNC processing an air outlet channel shape A plate, and flatly grinding a patch B plate with the same shape as the air outlet channel to obtain an arm A plate and an arm B plate respectively;
(4) And (3) bonding the processed arm A plate and the arm B plate together by using high-temperature glue (the high-temperature resistant temperature is about 600 ℃), drying and roasting, checking the air tightness of the obtained product, and spraying an antistatic polytetrafluoroethylene coating (the coating thickness is 60 mu m) after the air tightness is qualified to obtain the ceramic arm.
Comparative example 2
This comparative example provides a ceramic arm prepared in the same manner as comparative example 1 except that the antistatic polytetrafluoroethylene coating was not sprayed.
In order to compare technical effects of the above examples and comparative examples, the following experimental examples were specially set.
Experimental example 1
The ceramic arm provided in each of the examples and comparative examples of the present invention was tested for air tightness, strength, maximum use temperature, antistatic property, etc., and specific results are shown in table 1.
Wherein, intensity is detected according to ASTM C1161, the highest use temperature is measured by a thermometer, and antistatic performance is detected according to ANSI/ESDS 7.1.
The air tightness detection adopts enterprise standards, and specifically comprises the following steps:
(1) After the helium detector is started up, correcting the equipment according to the operation requirement;
(2) Except for the air passage inlet of the ceramic arm, the air passage is sealed by using Teflon adhesive tape;
(3) The air passage inlet is connected and sealed with the detection port of the helium detector, and when a start button is pressed, the equipment displays leakage quality smaller than 6.0x10 -8 The joint was purged with helium. The device showed less than 6.0 x 10 on purging -8 The alarm is NO, otherwise, the alarm is OK;
(4) Recording a test result;
(5) Sealing the air holes on the ceramic arm, pumping to-100 KPa, and pumping time can not be more than 1 minute. Closing the valve, wherein the pressure is not changed after 1 hour, releasing the seal, and releasing the pressure to 0 within 5 seconds;
(6) Matching the wafer to seal the air holes;
(7) Pumping to-90 KPa, wherein the pumping time is not more than 1 minute, standing for 10 seconds, and immediately observing the value of an air hole barometer to be a vacuum value, wherein the standard is-80 to-100 KPa;
(8) Sealing the air hole, pumping to-100 KPa, pumping for not more than 1 minute, closing the valve, and releasing the deblocking after 1 hour, wherein the pressure release is 0 within 5 seconds;
(9) Pumping to-90 KPa, wherein the pumping time is not more than 1 minute, sealing is released, pressure is released for 5 seconds, and then the barometer value is observed and is the airway air pumping value, and the standard is 0 to-6;
(10) Matching the wafer to seal the air holes;
(11) Pumping to-90 to-100 KPa, stabilizing the pressure for 10 seconds, closing the valve, and pumping for not more than 1 minute;
(12) After closing the valve, timing, maintaining the pressure for 30 seconds, wherein the pressure release value is not more than-10 KPa (general test);
(13) And (3) timing after closing the valve, maintaining the pressure for 30 seconds, wherein the pressure release value does not exceed-6 KPa (special requirement).
TABLE 1
Figure BDA0004149796640000171
As can be seen from table 1, the ceramic arms provided by the examples of the present invention are superior in all aspects to the ceramic arms provided by the comparative examples.
Specifically, unlike the preparation method of the ceramic arm according to the embodiment of the present invention, the ceramic arms of comparative examples 1 and 2 were prepared using a conventional preparation method (ceramic plates are combined to form air passages, and high-temperature adhesive is used between the ceramic plates). As can be seen from the data in Table 1, the strength of the integrally formed ceramic arm prepared by the preparation method of each embodiment of the invention is high, can reach about 400MPa, the tightness is good, the ceramic arm can be normally used even when the ceramic arm is resistant to high temperature to about 1000 ℃, the strength of each of comparative example 1 and comparative example 2 is much lower than that of each embodiment of the invention, the sealing performance is poorer than that of each embodiment, and the highest use temperature is also lower.
The ceramic arms of examples 2, 3 and 4 were prepared using different kinds of antistatic materials as ceramic powders, respectively, and comparative example 1 was prepared by providing an antistatic coating layer on the ceramic arm. As can be seen from the data in Table 1, the antistatic properties of examples 2 to 4 are substantially equivalent to those of comparative example 1, but since the antistatic coating of comparative example 1 is applied on the surface of the ceramic arm, the antistatic coating is easy to age and wear after long-term use, thereby causing the problem of deterioration of the antistatic properties of the ceramic arm. The inventors have compared the abrasion resistance of comparative example 1 with that of example 3, and the ceramic arm with antistatic coating of comparative example 1 has the abrasion loss of antistatic effect of the coating after about 1000 times of abrasion test, while the antistatic effect of the present invention is not changed by 1000 times of use of the present invention.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The preparation method of the ceramic arm is characterized by comprising the following steps of:
(a) Providing granulated powder formed by ceramic powder and an auxiliary agent;
providing a first mold and a second mold for molding a ceramic arm to be prepared, wherein one of the first mold and the second mold has the same air passage structure as the ceramic arm to be prepared;
(b) Adding the granulated powder into a first die and a second die respectively, then heating and pressurizing, cooling and demolding to obtain a first blank body and a second blank body, wherein one of the first blank body and the second blank body has the air passage structure;
(c) Covering the first blank body and the second blank body, and then performing heating and pressurizing treatment to bond the first blank body and the second blank body to obtain an arm blank body with a closed air passage structure;
(d) Degreasing and sintering the arm blank to obtain the ceramic arm.
2. The method for manufacturing a ceramic arm according to claim 1, wherein in the step (a), the ceramic powder comprises at least one of high-purity alumina powder, alumina antistatic composite ceramic powder, zirconia antistatic composite ceramic powder, or silicon carbide composite ceramic powder;
and/or the auxiliary agent comprises at least two of a plasticizer, a flux, a lubricant or a coupling agent.
3. The method of producing a ceramic arm according to claim 2, wherein the plasticizer comprises at least one of polypropylene, dibutyl phthalate, or polyvinyl butyral;
and/or, the flux comprises paraffin and/or polyethylene glycol;
and/or the lubricant comprises at least one of stearic acid, stearyl alcohol, or polyethylene wax;
and/or the coupling agent comprises an aluminate and/or titanate.
4. The method of claim 1, wherein in step (a), the method of preparing the granulated powder comprises the steps of:
mixing ceramic powder and an auxiliary agent, then carrying out high-temperature kneading, cooling and solidifying the kneaded material, and then crushing to obtain granulated powder;
preferably, the high temperature kneading is carried out at a temperature of 160 to 220℃for a period of 2 to 6 hours.
5. The method of claim 1, wherein in step (b), the heating temperature is 140-190 ℃;
and/or the pressurizing pressure is 5-30MPa, and the pressure is maintained for 5-10min.
6. The method of claim 1, wherein in step (c), the heating temperature is 120-160 ℃;
and/or the pressurizing pressure is 3-50MPa, and the pressure is maintained for 3-10min.
7. The method of claim 1-6, wherein in step (d), the degreasing comprises degreasing with a solvent followed by degreasing with embedded powder;
and/or in the step (d), the sintering temperature is 1300-1700 ℃, the time required for heating to the sintering temperature is 75-85h, and the heat preservation time at the sintering temperature is 5-15h.
8. The method for preparing a ceramic arm according to claim 7, wherein the degreasing comprises degreasing with a solvent including at least one of deionized water, acetone, petroleum ether, kerosene, and heptane, followed by degreasing with buried powder;
and/or the degreasing temperature of the solvent is 40-50 ℃, and the degreasing time of the solvent is 6-36h;
and/or the embedding powder adopted by the embedding powder degreasing comprises alumina;
and/or the temperature of the degreasing of the buried powder is 400-600 ℃, and the temperature of the degreasing of the buried powder is 40-60h.
9. A ceramic arm obtainable by the method of any one of claims 1 to 8.
10. Use of the ceramic arm of claim 9 in the field of semiconductor die wafer handling equipment.
CN202310314481.2A 2023-03-28 2023-03-28 Ceramic arm and preparation method and application thereof Pending CN116332655A (en)

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