Preparation method of chemical vapor deposition substrate and chemical vapor deposition method

Abstract

The invention provides a preparation method of a chemical vapor deposition substrate and a chemical vapor deposition method.The preparation method of the chemical vapor deposition substrate comprises the steps that a graphite plate is provided, the surface of the graphite plate is clean, the graphite plate is provided with a plurality of through holes which are communicated at intervals, the hole diameter of the through holes is not larger than 10 mm, and the distance between the through holes is not larger than 20 cm; the size of the graphite plate in the length direction is less than or equal to 2000 mm, the size in the width direction is less than or equal to 1000 mm, and the size in the thickness direction is 20-40 mm; graphite paper is provided, and the thickness of the graphite paper is 0.5-2.0 mm; the graphite plate is coated with an adhesive with the thickness of 0.1-0.5 mm; the graphite paper is flatly laid on the graphite plate; flattening the graphite paper; the adhesive discharged from the through holes and the periphery of the graphite plate is cleared away; covering the soft cushion with graphite paper, covering the soft cushion with the plate, and standing at normal temperature for not less than 10 hours; after standing, taking out the graphite plate adhered with the graphite paper, and trimming the peripheral corners; and putting the graphite plate adhered with the graphite paper into high-temperature equipment, heating to 200-600 DEG C at a speed of not higher than 50 DEG C / h under a vacuum or protective atmosphere condition, keeping the temperature for not less than 3 hours, and naturally cooling after keeping the temperature, thereby obtaining the chemical vapor deposition substrate.

Description

Technical Field

[0001] The present disclosure relates to the field of chemical vapor deposition, and more specifically to a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method. Background Art

[0002] Chemical Vapor Deposition (CVD) is a process in which gaseous or vaporous substances react in the gas phase or at the gas-solid interface to form solid deposits. Chemical vapor deposition is a new technology for preparing inorganic materials developed in recent decades. These inorganic materials can be oxides, sulfides, nitrides, carbides, or binary or multinary inter-element compounds in groups III-V, II-IV, and IV-VI, and their physical functions can be precisely controlled by the deposition process of gas phase doping. Chemical vapor deposition has become a new field of inorganic synthetic chemistry. It is currently widely used in the production of infrared materials such as zinc selenide, zinc sulfide, silicon carbide, etc.

[0003] In the chemical vapor deposition production of infrared optical materials, due to the large scale of infrared optical materials (i.e., large length, width and thickness, and bulk products after growth, the thickness of bulk products is usually more than 10mm), the commonly used substrate for the growth of infrared optical materials is currently made of graphite materials (i.e., graphite plates). Graphite materials are widely used in the field of chemical vapor deposition as substrates for the growth of bulk products because of their high temperature resistance, corrosion resistance, easy processing and low cost.

[0004] Since graphite materials are porous in microscopic structure, during chemical vapor deposition, the molecules of the bulk product generated by the reaction will be deposited on the substrate, and the gas molecules will penetrate into every hole of the porous structure of the substrate. When the products are finally separated, the substrate and the bulk product will be torn to varying degrees; therefore, the deposited substrate must be pretreated. There are usually two methods for substrate pretreatment: spraying release agent and substrate polishing. Spraying release agent (usually liquid graphite) on the substrate can make it easy to separate the bulk product formed by deposition from the substrate and will not cause tearing damage to the bulk product formed by deposition. However, even if polishing is performed after spraying the release agent, chemical vapor deposition at high temperature will form a coarse particle layer at the bottom of the bulk product. This coarse particle product cannot be used directly. When processing the bulk product, the coarse particle layer needs to be ground off, which will reduce the utilization rate of the bulk product. Directly polishing the substrate can ensure that the bulk product deposited on its surface will not have a coarse particle layer. However, the polished surface of the substrate is very easy to be scratched during use. When the scratched substrate is used again, the molecules of the deposited bulk product will penetrate into the scratched area, which can easily cause cracking and damage to the bulk product.

[0005] Therefore, further improvements are needed in chemical vapor deposition substrates. Summary of the invention

[0006] In view of the problems existing in the background technology, an object of the present disclosure is to provide a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method, which can be applicable to growing large-scale bulk products by chemical vapor deposition.

[0007] Another object of the present disclosure is to provide a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method, which can avoid the formation of a coarse particle layer at the bottom of a bulk product formed by chemical vapor deposition.

[0008] Another object of the present disclosure is to provide a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method, which can avoid the risk of scratching the polished surface formed by directly polishing the graphite plate and the problem of cracking and damage of the block product caused by reuse.

[0009] Another object of the present disclosure is to provide a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method, which can reduce the growth cost.

[0010] Still another object of the present disclosure is to provide a method for preparing a chemical vapor deposition substrate and a chemical vapor deposition method, which are applicable to large-scale production.

[0011] Thus, a method for preparing a chemical vapor deposition substrate includes the following steps: S1, providing a graphite plate, cleaning the surface of the graphite plate, the graphite plate being provided with a plurality of through holes spaced apart in the length direction and the width direction and penetrating in the thickness direction, the aperture of the plurality of through holes being no greater than 10 mm, the spacing between the plurality of through holes being no greater than 20 cm, the dimension of the graphite plate in the length direction being ≤2000 mm, the dimension of the graphite plate in the width direction being ≤1000 mm, and the dimension of the graphite plate in the thickness direction being 20-40 mm; S2, providing graphite paper, the dimension of the graphite paper covering the upper surface of the graphite plate, the thickness of the graphite paper being 0.5-2.0 mm; S3, brushing an adhesive on the entire upper surface of the graphite plate, the adhesive being an adhesive that can be used in chemical vapor deposition, and the thickness of the adhesive being 0.1-0.5 mm; S4, Spread the graphite paper flat on the graphite plate; S5, use a tool to flatten the graphite paper, and discharge the excess adhesive and gas from the through holes of the graphite plate and the surrounding areas of the graphite plate; S6, use a scraper to clean up the excess adhesive discharged from the through holes of the graphite plate and the surrounding areas of the graphite plate; S7, use a soft pad to cover the entire pasted graphite paper, and then cover the entire soft pad with a plate, and let it stand at room temperature for not less than 10 hours; S8, after the standing period, remove the soft pad and the plate, take out the graphite plate pasted with graphite paper, and trim the four corners along the graphite plate; S9, put the graphite plate pasted with graphite paper into a high-temperature device for hardening treatment, and heat it to 200-600℃ at a heating rate of not more than 50℃ / h under vacuum or protective atmosphere conditions, and keep it warm at this temperature for not less than 3 hours. After the insulation period, cool it down naturally to obtain a chemical vapor deposition substrate.

[0012] A chemical vapor deposition method is provided. The chemical vapor deposition method uses a chemical vapor deposition substrate prepared by the above-mentioned method for preparing a chemical vapor deposition substrate, and deposits a growth block product entirely on graphite paper of the chemical vapor deposition substrate.

[0013] The beneficial effects of the present disclosure are as follows.

[0014] In the preparation method of the chemical vapor deposition substrate and the chemical vapor deposition method according to the present disclosure, through steps S1 to S9, a chemical vapor deposition substrate composed of a graphite plate and graphite paper firmly bonded together via the adhesive in the through holes of the graphite plate and the adhesive between the upper surface of the graphite plate and the graphite paper can be prepared. The surface of the graphite paper firmly bonded to the upper surface of the graphite plate is smooth without bubbling or debonding. The smooth graphite paper firmly bonded to the upper surface of the graphite plate without bubbling or debonding will be very suitable for chemical vapor deposition to grow large-scale bulk products, especially infrared optical materials.

[0015] In the preparation method of the chemical vapor deposition substrate and the chemical vapor deposition method according to the present disclosure, when the chemical vapor deposition substrate prepared by steps S1 to S9 grows a large-scale bulk product by chemical vapor deposition, the chemical vapor deposition substrate uses a smooth graphite paper with no bubbling or degumming firmly bonded to the upper surface of the graphite plate for the deposition of large-scale bulk products. This avoids the pretreatment of the graphite plate directly used to deposit large-sized bulk products in the background technology. Specifically, it avoids the formation of a coarse particle layer at the bottom of the bulk product formed by chemical vapor deposition using a release agent in the background technology, thereby improving the utilization rate of the bulk product and avoiding the risk of scratches on the polished surface formed by directly polishing the graphite plate in the background technology and the problem of cracking and damage to the bulk product caused by reuse, thereby enabling the graphite plate to be used repeatedly and for a long time, thereby reducing the growth cost.

[0016] In the preparation method of the chemical vapor deposition substrate and the chemical vapor deposition method according to the present disclosure, when the chemical vapor deposition substrate is prepared through steps S1 to S9, when a large-scale bulk product is grown by chemical vapor deposition, because the chemical vapor deposition substrate utilizes a smooth graphite paper with no bubbling or debonding firmly bonded to the upper surface of the graphite plate for the deposition of large-scale bulk products, it is convenient to demold the bulk product and the graphite plate without damaging the bulk product and the graphite plate, thereby improving the yield of the product block and enabling repeated and long-term use, thereby improving production efficiency and reducing costs, and is suitable for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is an exploded view of some components involved in the method for preparing a chemical vapor deposition substrate according to the present disclosure, wherein the adhesive is schematically shown in a plate shape.

[0018] Figure 2 It is an assembly diagram of some parts of the preparation method of the chemical vapor deposition substrate disclosed in the present invention before the static state is completed, wherein the adhesive is schematically shown in a plate shape.

[0019] Figure 3 is along Figure 2 The 3D cutaway diagram made by the AA line,

[0020] Figure 4 yes Figure 3 A three-dimensional cutaway view of a graphite plate bonded with graphite paper after the cushion and the plate have been removed after standing.

[0021] Figure 5 yes Figure 4 A three-dimensional cross-sectional view of a graphite plate bonded with graphite paper after trimming the four corners.

[0022] Figure 6is with Figure 5 A three-dimensional cross-sectional view of a block product formed by chemical vapor deposition on a graphite paper bonded to a graphite plate, of a corresponding chemical vapor deposition substrate.

[0023] Figure 7 A top view photograph of the chemical vapor deposition substrate prepared in Example 1 taken from the graphite paper side is given, wherein the holes at the upper and lower edges in the photograph are holes installed in the deposition chamber.

[0024] Figure 8 and Fig. 9 Photos taken from the side of the block products formed by chemical vapor deposition prepared in Example 4 and Example 5 are respectively given after grinding to remove the residual graphite paper.

[0025] The accompanying drawings are described as follows:

[0026] 100 Chemical Vapor Deposition Substrate 2 Graphite Paper

[0027] L Length direction 3 adhesive

[0028] W width direction 4 cushions

[0029] T thickness direction 5 plate

[0030] 1 graphite plate 200 pieces

[0031] 11 Through Holes DETAILED DESCRIPTION

[0032] The accompanying drawings show embodiments of the present disclosure, and it will be understood that the disclosed embodiments are merely examples of the present disclosure, and the present disclosure can be implemented in various forms. Therefore, the specific details disclosed herein should not be interpreted as limiting, but merely as the basis for the claims and as a representative basis for teaching ordinary technicians in the field to implement the present disclosure in various ways.

[0033] [Method for preparing chemical vapor deposition substrate]

[0034] Reference Figures 1 to 6 According to the present invention, the method for preparing a chemical vapor deposition substrate comprises the following steps:

[0035] S1, providing a graphite plate 1, cleaning the surface of the graphite plate 1, wherein the graphite plate 1 is provided with a plurality of through holes 11 spaced apart in the length direction L and the width direction W and penetrating in the thickness direction T, wherein the aperture of the plurality of through holes 11 is not greater than 10 mm, and the spacing between the plurality of through holes 11 is not greater than 20 cm, the dimension of the graphite plate 1 in the length direction L is ≤2000 mm, the dimension of the graphite plate 1 in the width direction W is ≤1000 mm, and the dimension of the graphite plate 1 in the thickness direction T is 20-40 mm;

[0036] S2, providing graphite paper 2, the size of the graphite paper 2 covers the upper surface of the graphite plate 1, and the thickness of the graphite paper 2 is 0.5-2.0 mm;

[0037] S3, brushing adhesive 3 on the entire upper surface of the graphite plate 1, the adhesive 3 is an adhesive that can be used in chemical vapor deposition, and the thickness of the adhesive 3 is 0.1-0.5 mm;

[0038] S4, laying the graphite paper 2 flat on the graphite plate 1;

[0039] S5, using a tool (not shown) to flatten the graphite paper 2, and discharge the excess adhesive 3 and gas from the through holes 11 of the graphite plate 1 and around the graphite plate 1;

[0040] S6, using a scraper (not shown) to clean up the excess adhesive 3 discharged from the through hole 11 of the graphite plate 1 and around the graphite plate 1;

[0041] S7, using a soft pad 4 to completely cover the pasted graphite paper 2, and then using a plate 5 to cover the entire soft pad 4, and leaving it at room temperature for no less than 10 hours;

[0042] S8, after the standing is completed, the cushion 4 and the plate 5 are removed, the graphite plate 1 with the graphite paper 2 attached thereto is taken out, and the four corners of the graphite plate 1 are trimmed;

[0043] S9, putting the graphite plate 1 pasted with graphite paper 2 into a high-temperature device (not shown) for hardening treatment, heating it to 200-600°C at a heating rate not higher than 50°C / h under vacuum or protective atmosphere conditions, and keeping it at this temperature for not less than 3h. After the insulation is completed, the temperature is naturally cooled to obtain a chemical vapor deposition substrate 100.

[0044] In the preparation method of the chemical vapor deposition substrate according to the present disclosure, through steps S1 to S9, a chemical vapor deposition substrate 100 consisting of a graphite plate 1 and a graphite paper 2 firmly bonded together via the adhesive 3 in the through hole 11 of the graphite plate 1 and the adhesive 3 between the upper surface of the graphite plate 1 and the graphite paper 2 can be prepared. The surface of the graphite paper 2 firmly bonded to the upper surface of the graphite plate 1 is smooth without bubbling or debonding. The smooth graphite paper 2 firmly bonded to the upper surface of the graphite plate 1 without bubbling or debonding will be very suitable for chemical vapor deposition growth of large-scale bulk products 200, especially infrared optical materials.

[0045] In the preparation method of the chemical vapor deposition substrate according to the present disclosure, the chemical vapor deposition substrate 100 prepared by steps S1 to S9, when growing a large-scale bulk product 200 by chemical vapor deposition, because the chemical vapor deposition substrate 100 uses the smooth graphite paper 2 with no bubbling and degumming firmly bonded to the upper surface of the graphite plate 1 for the deposition of the large-scale bulk product 200, thereby avoiding the pretreatment of the graphite plate directly used to deposit the large-sized bulk product 200 in the background technology. Specifically, it avoids the formation of a coarse particle layer at the bottom of the bulk product formed by chemical vapor deposition using a release agent in the background technology, thereby improving the utilization rate of the bulk product, avoiding the risk of scratches on the polished surface formed by directly polishing the graphite plate in the background technology and the problem of cracking and damage of the bulk product caused by reuse, thereby enabling the graphite plate 1 to be used repeatedly and for a long time, thereby reducing the growth cost.

[0046] In the preparation method of the chemical vapor deposition substrate according to the present disclosure, the chemical vapor deposition substrate 100 prepared by steps S1 to S9, when growing a large-scale block product 200 by chemical vapor deposition, because the chemical vapor deposition substrate 100 uses the smooth graphite paper 2 with no bubbling or debonding firmly bonded to the upper surface of the graphite plate 1 for the deposition of the large-scale block product 200, it is convenient to demold the block product 200 and the graphite plate 1 without damaging the block product 200 and the graphite plate 1, thereby improving the yield of the product block 200 and enabling it to be used repeatedly and for a long time, thereby improving production efficiency and reducing costs, and is suitable for large-scale production.

[0047] In step S1, Figure 1 In the example shown, the plurality of through holes 11 are arranged at equal intervals in the length direction L and the width direction W. In step S1, in one example, the aperture of the through holes 11 is in the range of 3-5 mm, and the spacing is in the range of 10-15 cm. In step S1, for example, the graphite plate 1 is a graphite plate of Toyo Tanso brand IG-12 of Japan.

[0048] In step S1, for example, the cleaning can be done by wiping with an organic solvent such as ethanol or acetone and then air-drying. The cleaned graphite plate 1 is placed flat on a workbench.

[0049] The graphite paper 2 of step S2 can be cut to a suitable size so that the size of the graphite paper 2 covers the upper surface of the graphite plate 1. In one example, the thickness of the graphite paper 2 is in the range of 0.5-1.5 mm. For example, the graphite paper 2 has a carbon content of ≥99.5%, a sulfur content of ≤200 PPM, a chlorine content of ≤30 PPM, and a density deviation of ±0.5 g / cm 3, tensile strength ≥ 4.5 MPa, compression rate 35-45%, rebound rate ≥ 9%, thermal weight loss at 450°C ≤ 5%, stress relaxation rate ≤ 10%. For example, graphite paper 2 is purchased from Qingdao Jiuzhengyuan Graphite Technology Co., Ltd.

[0050] In step S3, the thickness of the adhesive 3 refers to the thickness of the adhesive 3 flowing into and fully filling the multiple through holes 11 of the graphite plate 1 and on the entire upper surface of the graphite plate 1 during the process of brushing the adhesive 3. In step S3, for example, the adhesive 3 is SL8308 1200°C high temperature resistant adhesive produced by Zhuzhou Shilin Polymer Co., Ltd. Of course, it is not limited to this, as long as the adhesive 3 can be used in chemical vapor deposition.

[0051] In step S5 , for example, the tool is a rubber scraper.

[0052] In step S6 , for example, the scraper is a rubber scraper.

[0053] In step S7, the soft pad 4 and the plate 5 are capable of applying a certain pressure to the pasted graphite paper 2, so that the graphite paper 2 can be better attached to the upper surface of the graphite plate 1 through the adhesive 3 during the standing process at room temperature. In step S7, the soft pad 4 is a silicone pad or a PVC pad; the plate 5 is a light plastic material, specifically, a PP board or a PVC board or an acrylic board. In step S7, for example, the graphite paper 2 is standing at room temperature for 15-20 hours.

[0054] In step S8, trimming the four corners can be performed using a utility knife.

[0055] In the hardening process of the high temperature equipment in step S9, the vacuum or protective atmosphere conditions can prevent the graphite plate 1 and the graphite paper 2 from being oxidized. The protective atmosphere is, for example, nitrogen. In the hardening process of the high temperature equipment in step S9, the solvent in the adhesive 3 is discharged along the corresponding through hole 11. In step S9, in one example, the heating rate is 20-30°C / h, the heated temperature is 400-500°C, and the holding time is 3-4h.

[0056] [Chemical Vapor Deposition Method]

[0057] Reference Figure 6 According to the chemical vapor deposition method disclosed in the present invention, a chemical vapor deposition substrate 100 prepared by the aforementioned method for preparing a chemical vapor deposition substrate is used, and a bulk product 200 is deposited and grown entirely on the graphite paper 2 of the chemical vapor deposition substrate 100 .

[0058] The block product 200 may be, but is not limited to, zinc selenide or zinc sulfide. As mentioned above, the thickness of the block product 200 is above 10 mm. For example, the thickness of the block product 200 is up to 50 mm.

[0059] The characteristics, effects, preparation and operation of the chemical vapor deposition substrate 100 used in the chemical vapor deposition method according to the present disclosure can be found in the foregoing description and will not be repeated here.

[0060] [test]

[0061] Example 1

[0062] The method for preparing the chemical vapor deposition substrate of Example 1 adopts the following steps:

[0063] S1, providing a graphite plate 1, cleaning the surface of the graphite plate 1, wiping with ethanol and then drying, placing the dried graphite plate 1 flat on a workbench, the graphite plate 1 is a graphite plate of Toyo Tanso grade IG-12 of Japan, the graphite plate 1 is processed to have a plurality of through holes 11 spaced apart in the length direction L and the width direction W and penetrating in the thickness direction T, the plurality of through holes 11 are arranged at equal intervals in the length direction L and the width direction W, the aperture of the plurality of through holes 11 is 3 mm, the spacing between the plurality of through holes 11 is 10 cm, the size of the graphite plate 1 in the length direction L is 2000 mm, the size of the graphite plate 1 in the width direction W is 1000 mm, and the size of the graphite plate 1 in the thickness direction T is 30 mm;

[0064] S2, providing graphite paper 2, cutting the graphite paper 2 to a suitable size so that the size of the graphite paper 2 covers the upper surface of the graphite plate 1, the thickness of the graphite paper 2 is 0.5 mm, the carbon content of the graphite paper 2 is ≥ 99.5%, the sulfur content is ≤ 200 PPM, the chlorine content is ≤ 30 PPM, and the density deviation is ± 0.5 g / cm 3 , tensile strength ≥ 4.5 MPa, compression rate 35-45%, rebound rate ≥ 9%, thermal weight loss at 450°C ≤ 55%, stress relaxation rate ≤ 510%, graphite paper 2 was purchased from Qingdao Jiuzhengyuan Graphite Technology Co., Ltd.;

[0065] S3, using a brush to apply adhesive 3 on the entire upper surface of the graphite plate 1, the adhesive 3 is SL8308 1200°C high temperature resistant adhesive produced by Zhuzhou Shilin Polymer Co., Ltd., during which the adhesive 3 flows into and fully fills the multiple through holes 11 of the graphite plate 1, and the thickness of the adhesive 3 on the entire upper surface of the graphite plate 1 is 0.5 mm;

[0066] S4, laying the graphite paper 2 flat on the graphite plate 1;

[0067] S5, using a rubber scraper to flatten the graphite paper 2, and discharge the excess adhesive 3 and gas from the through holes 11 of the graphite plate 1 and around the graphite plate 1;

[0068] S6, using a rubber scraper to clean up the excess adhesive 3 discharged from the through hole 11 of the graphite plate 1 and around the graphite plate 1;

[0069] S7, use a silicone pad soft pad 4 to completely cover the pasted graphite paper 2, and then use a PP plate 5 to cover the entire soft pad 4, and let it stand at room temperature for 20 hours;

[0070] S8, after the standing is completed, the cushion 4 and the plate 5 are removed, the graphite plate 1 with the graphite paper 2 attached thereto is taken out, and the four corners of the graphite plate 1 are trimmed with a utility knife;

[0071] S9, putting the graphite plate 1 pasted with graphite paper 2 into a high-temperature device for hardening treatment, vacuuming the high-temperature device to expel oxygen, and then filling the high-temperature device with nitrogen for protection, heating to 500°C at a heating rate of 20°C / h, keeping the temperature for 4h, and cooling naturally after the end of the keeping, thereby obtaining a chemical vapor deposition substrate 100.

[0072] Example 2

[0073] The method for preparing the chemical vapor deposition substrate of Example 2 is the same as that of Example 1 except for the following differences:

[0074] In step S1, the diameter of each through hole 11 is 5 mm, and the spacing between the multiple through holes 11 is 15 cm;

[0075] In step S2, the thickness of the graphite paper 2 is 1.0 mm;

[0076] In step S3, the thickness of the adhesive 3 is 0.3 mm;

[0077] In step S7, the mixture is allowed to stand at room temperature for 15 hours;

[0078] In step S9, the temperature is increased to 400°C at a rate of 25°C / h and maintained at this temperature for 3 hours.

[0079] Example 3

[0080] The method for preparing the chemical vapor deposition substrate of Example 3 is the same as that of Example 1 except for the following differences:

[0081] In step S1, the diameter of each through hole 11 is 4 mm, and the spacing between the multiple through holes 11 is 12 cm;

[0082] In step S2, the thickness of the graphite paper 2 is 1.5 mm;

[0083] In step S3, the thickness of the adhesive 3 is 0.1 mm;

[0084] In step S7, the mixture is allowed to stand at room temperature for 17 hours;

[0085] In step S9, the temperature is increased to 450°C at a rate of 30°C / h and maintained at this temperature for 3.5 hours.

[0086] Example 4

[0087] Example 4 Using the chemical vapor deposition substrate 100 prepared in Example 1, a chemical vapor deposition method is used to deposit zinc selenide with a thickness of 50 mm on the graphite paper 2 of the chemical vapor deposition substrate 100. The chemical vapor deposition process of zinc selenide adopts the following process:

[0088] Into the chemical vapor deposition furnace, the chemical vapor deposition substrate 100 prepared in Example 1 is loaded, and a zinc ingot with a purity of 99.999% is loaded into the crucible. The furnace is evacuated and leak-checked. The pressure rise rate of the furnace body is required to be less than 8Pa / h. After passing the test, the temperature is programmed to control the pressure in the furnace at 5KPa, the crucible heating rate is 0.3℃ / min, the deposition chamber heating rate is 0.5℃ / min, the crucible is heated to 650℃, the deposition chamber is heated to 710℃, and then argon carrier gas is introduced into the crucible and argon carrier gas and hydrogen selenide are introduced into the deposition chamber. The argon flow rate introduced into the crucible is 30L / m in, the evaporation rate of zinc vapor in the crucible is 5 L / min; the flow rate of 5N hydrogen selenide introduced into the deposition chamber is 5.5 L / min, the flow rate of argon mixed with hydrogen selenide introduced into the deposition chamber is 55 L / min, the deposition rate is controlled to 80 μm / h, zinc selenide is deposited, and after the deposition is completed, the same pressure as that in the deposition process is maintained, the introduction of carrier gas and hydrogen selenide is stopped, the temperature in the deposition chamber is cooled to 600°C at a cooling rate of 0.2°C / min, and the temperature is maintained at 600°C for 10 hours, and then cooled to room temperature at a cooling rate of 0.2°C / min, and a zinc selenide block product is obtained.

[0089] Example 5

[0090] Example 5 Using the chemical vapor deposition substrate 100 prepared in Example 2, a chemical vapor deposition method is used to deposit zinc sulfide with a thickness of 53 mm on the graphite paper 2 of the chemical vapor deposition substrate 100. The chemical vapor deposition process of zinc sulfide adopts the following process:

[0091] Into the chemical vapor deposition furnace, the chemical vapor deposition substrate 100 prepared in Example 2 was loaded, and a zinc ingot with a purity of 99.999% was loaded into the crucible. The furnace was evacuated and leak-checked. The pressure rise rate of the furnace body was required to be less than 8Pa / h. After passing the test, the temperature was programmed to control the pressure in the furnace at 6KPa, the crucible heating rate was 0.5℃ / min, and the deposition chamber heating rate was 0.8℃ / min. The crucible was heated to 630℃, and the deposition chamber was heated to 660℃. Then, argon gas was introduced into the crucible, and argon gas and hydrogen sulfide were introduced into the deposition chamber. The argon flow rate introduced into the crucible was The temperature of the deposition chamber was controlled at 50 L / min, the evaporation rate of zinc vapor was 6 L / min, the flow rate of 4N hydrogen sulfide introduced into the deposition chamber was 5.2 L / min, the flow rate of argon mixed with hydrogen sulfide introduced into the deposition chamber was 90 L / min, the deposition rate was controlled at 60 μm / h, and zinc sulfide was deposited. After the deposition was completed, the same pressure as that during the deposition process was maintained, the introduction of carrier gas argon and hydrogen sulfide was stopped, the deposition chamber was heated to 700 ° C at a heating rate of 0.5 ° C / min, and the temperature was kept constant for 20 hours; then the temperature was cooled to room temperature at a cooling rate of 0.2 ° C / min, and a zinc sulfide block product was obtained from the furnace.

[0092] After the block product of Example 4-5 is taken out of the furnace, a metal wire or iron wire with a wire diameter smaller than the sum of the thickness of the graphite paper 2 and the thickness of the adhesive 3 is used to perform wire cutting on the graphite paper 2 between the block product 200 and the graphite plate 1 to de-mold the block product 200 and the graphite plate 1. After de-molding, the graphite plate 1 is subsequently cleaned of the glue and reused, and the block product 200 after de-molding is ground to remove the graphite paper remaining after wire cutting.

[0093] The graphite paper of the chemical vapor deposition substrate prepared in Examples 1-3 has a smooth surface without bubbling or degumming. Figure 7 A top view photograph of the chemical vapor deposition substrate prepared in Example 1 taken from the graphite paper 1 side is given.

[0094] Figure 8 and Fig. 9 Photos taken from the side of the block products formed by chemical vapor deposition prepared in Example 4 and Example 5 after grinding to remove the residual graphite paper are respectively given, wherein the block products except the bottom are all surface processed. Figure 8 and Fig. 9 It can be seen that there is no coarse particle layer at the bottom of the block product.

[0095] The above detailed description is used to describe multiple exemplary embodiments, but this document is not intended to be limited to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined together to form multiple additional combinations that are not shown for the sake of simplicity.

Claims

1. A method for preparing a chemical vapor deposition substrate, characterized in that: Includes steps: S1, providing a graphite plate (1), cleaning the surface of the graphite plate (1), wherein the graphite plate (1) is provided with a plurality of through holes (11) spaced apart in the length direction (L) and the width direction (W) and penetrating in the thickness direction (T), wherein the aperture of the plurality of through holes (11) is not greater than 10 mm, and the spacing between the plurality of through holes (11) is not greater than 20 cm, the size of the graphite plate (1) in the length direction (L) is ≤2000 mm, the size of the graphite plate (1) in the width direction (W) is ≤1000 mm, and the size of the graphite plate (1) in the thickness direction (T) is 20-40 mm; S2, providing graphite paper (2), wherein the size of the graphite paper (2) covers the upper surface of the graphite plate (1), and the thickness of the graphite paper (2) is 0.5-2.0 mm; S3, brushing adhesive (3) on the entire upper surface of the graphite plate (1), the adhesive (3) is an adhesive that can be used in chemical vapor deposition, and the thickness of the adhesive (3) is 0.1-0.5 mm; S4, laying the graphite paper (2) flat on the graphite plate (1); S5, using a tool (not shown) to flatten the graphite paper (2), and discharge the excess adhesive (3) and gas from the through holes (11) of the graphite plate (1) and around the graphite plate (1); S6, using a scraper (not shown) to clean up the excess adhesive (3) discharged from the through hole (11) of the graphite plate (1) and around the graphite plate (1); S7, using a soft pad (4) to completely cover the pasted graphite paper (2), and then using a plate (5) to cover the entire soft pad (4), and leaving it at room temperature for no less than 10 hours; S8, after the standing still is completed, the soft pad (4) and the plate (5) are removed, the graphite plate (1) with the graphite paper (2) attached thereto is taken out, and the four corners of the graphite plate (1) are trimmed; S9, putting the graphite plate (1) pasted with graphite paper (2) into a high-temperature device (not shown) for hardening treatment, heating to 200-600°C at a heating rate of no more than 50°C / h under vacuum or protective atmosphere conditions, and keeping the temperature at this temperature for no less than 3h. After the insulation is completed, the temperature is naturally cooled to obtain a chemical vapor deposition substrate (100).

2. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S1, a plurality of through holes (11) are arranged at equal intervals in the length direction (L) and the width direction (W).

3. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S1, the aperture of the through hole (11) is in the range of 3-5 mm, and the spacing is in the range of 10-15 cm; In step S1, the surface is cleaned by wiping with an organic solvent such as ethanol or acetone and then dried.

4. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S2, the thickness of the graphite paper (2) is in the range of 0.5-1.5 mm; In step S2, the graphite paper (2) has a carbon content of ≥99.5%, a sulfur content of ≤200 PPM, a chlorine content of ≤30 PPM, and a density deviation of ±0.5 g / cm 3 , tensile strength ≥4.5MPa, compression rate 35-45%, rebound rate ≥9%, thermal weight loss at 450℃ ≤5%, stress relaxation rate ≤10%.

5. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S3, the adhesive (3) is SL8308 1200°C high temperature resistant adhesive produced by Zhuzhou Shilin Polymer Co., Ltd.

6. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S3, using a brush or a roller, brush the adhesive (3) on the entire upper surface of the graphite plate (1); In step S5, the tool is a rubber scraper; In step S6, the scraper is a rubber scraper; In step S7, the soft pad (4) is a silicone pad or a PVC pad, and the plate (5) is a light plastic material, which is a PP plate, a PVC plate, or an acrylic plate.

7. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S7, the mixture is left to stand at room temperature for 15-20 hours.

8. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that: In step S9, the heating rate is 20-30°C / h, the heated temperature is 400-500°C, and the insulation time is 3-4h.

9. A chemical vapor deposition method, characterized in that: The chemical vapor deposition method adopts a chemical vapor deposition substrate (100) prepared by the method for preparing a chemical vapor deposition substrate according to any one of claims 1 to 8, and deposits a growth block product (200) entirely on the graphite paper (2) of the chemical vapor deposition substrate (100).

10. The chemical vapor deposition method according to claim 9, characterized in that: The bulk product (200) is zinc selenide or zinc sulfide.

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