Method for producing a chemical vapor deposition substrate and chemical vapor deposition method

Abstract

Provided are a chemical vapor deposition substrate preparation method and a chemical vapor deposition method. The chemical vapor deposition substrate preparation method comprises: providing a graphite plate, surface cleaning, the graphite plate being provided with a plurality of through holes spaced apart, the hole diameter of the through holes being not greater than 10 mm, the spacing being not greater than 20 cm, the length direction size of the graphite plate being ≤2000 mm, the width direction size being ≤1000 mm, and the thickness direction size being 20-40 mm; providing a graphite paper with a thickness of 0.5-2.0 mm; brushing an adhesive on the graphite plate with a thickness of 0.1-0.5 mm; laying the graphite paper on the graphite plate; pushing the graphite paper flat; cleaning the adhesive discharged from the through holes and the periphery of the graphite plate; covering the graphite paper with a soft pad, placing a plate on the soft pad, and standing at room temperature for not less than 10 h; after standing, taking out the graphite plate with the graphite paper, and trimming the periphery corners; and putting the graphite plate with the graphite paper into a high-temperature device, heating to 200-600 ℃ at not higher than 50 ℃ / h under vacuum or a protective atmosphere, keeping the temperature for not less than 3 h, naturally cooling after keeping the temperature, and obtaining a chemical vapor deposition substrate.

Description

TECHNICAL FIELD

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

[0002] Chemical vapor deposition (CVD) is a process in which gaseous or vapor state substances react on the gas phase or gas-solid interface to form solid deposition. 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 multi-element intercompounds in groups III-V, II-IV, and IV-VI, and their physical functions can be precisely controlled through the deposition process of gas phase doping. Chemical vapor deposition has become a new field of inorganic synthesis chemistry. It is currently widely used in the production of infrared optical materials such as zinc selenide, zinc sulfide, and silicon carbide.

[0003] In the chemical vapor deposition production of infrared optical materials, due to the large scale of the growth of infrared optical materials (i.e. the length, width and thickness are large, and after growth, it is a block product, and the block product usually has a thickness of more than 10 mm), the substrate commonly used for the growth of infrared optical materials is made of graphite material (i.e. graphite plate). Due to the advantages of graphite material such as high temperature resistance, corrosion resistance, easy processing, and low cost, it is widely used in the field of chemical vapor deposition as a substrate for the growth of block products.

[0004] Since the graphite material is a porous structure under the microscope, in chemical vapor deposition, the molecules of the block product generated by the reaction will be deposited on the substrate, and the gas molecules will penetrate into each hole of the porous structure of the substrate. Finally, when the product is separated, the substrate and the block product will be torn to different degrees; therefore, the deposition substrate must be pretreated. The methods for pretreating the substrate usually include spraying a release agent and polishing the substrate. Spraying a release agent (usually liquid graphite) on the substrate can easily separate the block product formed by deposition from the substrate and will not cause tearing damage to the block product formed by deposition, but even after spraying the release agent and polishing, chemical vapor deposition at high temperature will form a coarse particle layer at the bottom of the block product. This coarse particle product cannot be used directly, and during the processing of the block product, the coarse particle layer needs to be ground off, which will reduce the utilization rate of the block product. Polishing the substrate directly, although it can be used on the surface of the substrate to form a block product without a coarse particle layer, but 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 block product formed by deposition will penetrate into the scratched part, which will easily cause the block product to crack and damage.

[0005] Therefore, there is a need for further improvement on a chemical vapor deposition substrate. SUMMARY

[0006] In view of the problems in the background art, 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 applied to chemical vapor deposition growth of a large-scale bulk product.

[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 formation of a coarse grain layer at the bottom of a bulk product formed by chemical vapor deposition.

[0008] 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 can avoid the risk of scratching of a polished surface formed by directly polishing a graphite plate and the problem of cracking damage of a bulk product caused by reuse.

[0009] 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 can reduce growth costs.

[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 can be applied to mass production.

[0011] Thus, a chemical vapor deposition substrate preparation method includes steps of: 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 plurality of through holes having a hole diameter not greater than 10 mm, the plurality of through holes having a spacing not greater than 20 cm, the graphite plate having a length direction size ≤2000 mm, the graphite plate having a width direction size ≤1000 mm, and the graphite plate having a thickness direction size of 20-40 mm; S2, providing a graphite paper, the graphite paper having a size covering the upper surface of the graphite plate, and the graphite paper having a thickness of 0.5-2.0 mm; S3, brushing an adhesive on the entire upper surface of the graphite plate, the adhesive being a glue capable of being used in chemical vapor deposition, and the adhesive having a thickness of 0.1-0.5 mm; S4, laying the graphite paper on the graphite plate; S5, using a tool to push the graphite paper flat, and discharging excess adhesive and gas from the through holes of the graphite plate and the periphery of the graphite plate; S6, using a scraper to clean the excess adhesive discharged from the through holes of the graphite plate and the periphery of the graphite plate; S7, using a soft pad to entirely cover the adhered graphite paper, and then covering the entire soft pad with a plate, and standing at room temperature for not less than 10 h; S8, after standing, removing the soft pad and the plate, taking out the graphite plate with the adhered graphite paper, and trimming the four corners of the graphite plate; and S9, putting the graphite plate with the adhered graphite paper into a high-temperature device for hardening treatment, heating to 200-600 ℃ at a temperature rising speed not higher than 50 ℃ / h under vacuum or protective atmosphere, and keeping at the temperature for not less than 3 h, and then naturally cooling, to obtain a chemical vapor deposition substrate.

[0012] A chemical vapor deposition method is provided, which uses the chemical vapor deposition substrate prepared by the aforementioned chemical vapor deposition substrate preparation method, and entirely deposits and grows a bulk product on the graphite paper of the chemical vapor deposition substrate.

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

[0014] In the chemical vapor deposition substrate preparation method 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 a 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 on the upper surface of the graphite plate is smooth, and there is no blistering and adhesive peeling phenomenon, and the graphite paper with the smooth surface without blistering and adhesive peeling firmly bonded on the upper surface of the graphite plate will be very suitable for chemical vapor deposition to grow a large-scale bulk product, especially an infrared optical material.

[0015] In the chemical vapor deposition substrate preparation method and the chemical vapor deposition method according to the present disclosure, the chemical vapor deposition substrate prepared through steps S1 to S9 is used for deposition of large-scale bulk products by using the surface-smoothed graphite paper that is firmly bonded on the upper surface of the graphite plate without blistering and peeling, thus avoiding the pretreatment of directly using the graphite plate for deposition of large-size bulk products in the background art, specifically, avoiding the formation of a coarse particle layer at the bottom of the bulk product formed by chemical vapor deposition in the case of using a release agent in the background art, thereby improving the utilization rate of the bulk product, avoiding the risk of scratching of the polished surface formed by directly polishing the graphite plate and the problem of cracking damage of the bulk product caused by reusing, and thus enabling the graphite plate to be repeatedly and long-term used, thereby reducing the growth cost.

[0016] In the chemical vapor deposition substrate preparation method and the chemical vapor deposition method according to the present disclosure, the chemical vapor deposition substrate prepared through steps S1 to S9 is used for deposition of large-scale bulk products by using the surface-smoothed graphite paper that is firmly bonded on the upper surface of the graphite plate without blistering and peeling, thus avoiding the pretreatment of directly using the graphite plate for deposition of large-size bulk products in the background art, specifically, avoiding the formation of a coarse particle layer at the bottom of the bulk product formed by chemical vapor deposition in the case of using a release agent in the background art, thereby improving the utilization rate of the bulk product, avoiding the risk of scratching of the polished surface formed by directly polishing the graphite plate and the problem of cracking damage of the bulk product caused by reusing, and thus enabling the graphite plate to be repeatedly and long-term used, thereby reducing the growth cost. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 is an exploded view of part of the components involved in the preparation method of the chemical vapor deposition substrate according to the present disclosure, in which the adhesive is schematically shown in the form of a plate.

[0018] Figure 2 is an assembled view of part of the components before the end of the standing period in the preparation method of the chemical vapor deposition substrate according to the present disclosure, in which the adhesive is schematically shown in the form of a plate.

[0019] Figure 3 is a perspective cutaway view along the A-A line of Figure 2

[0020] Figure 4 is a perspective cutaway view of the graphite plate with the graphite paper bonded thereto after removal of the soft pad and the plate in Figure 3

[0021] Figure 5 is a perspective cutaway view of the graphite plate with the graphite paper bonded thereto after trimming of the four corner edges in Figure 4

[0022] Figure 6 ​​​is with Figure 5 A perspective sectional view of a bulk product formed by chemical vapor deposition on a graphite paper to which a corresponding chemical vapor deposition substrate is bonded on a graphite plate.

[0023] Figure 7 A photograph taken from above of a chemical vapor deposition substrate prepared in Example 1, in which the holes at the upper and lower edges in the photograph are holes installed in a deposition chamber.

[0024] Figure 8 and Figure 9 Photographs taken from the side of bulk products formed by chemical vapor deposition prepared in Example 4 and Example 5, respectively, after the remaining graphite paper was removed by grinding.

[0025] In which the 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 soft pad

[0029] T thickness direction 5 plate

[0030] 1 graphite plate 200 bulk product

[0031] 11 through hole DETAILED DESCRIPTION

[0032] The accompanying drawings illustrate embodiments of the present disclosure, and it is 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 a basis for the claims and as a basis for teaching a person of ordinary skill in the art to implement the present disclosure in various ways.

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

[0034] Referring to Figures 1 to 6 , the method for preparing a chemical vapor deposition substrate according to the present disclosure includes the steps of:

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

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

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

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

[0039] S5, using a tool (not shown) to push the graphite paper 2 flat, and discharging the excess adhesive 3 and gas from the through hole 11 of the graphite plate 1 and the periphery of the graphite plate 1;

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

[0041] S7, using a soft pad 4 to cover the graphite paper 2 that has been pasted, and then covering the entire soft pad 4 with a plate 5, and standing at room temperature for not less than 10h;

[0042] S8, after standing, removing the soft pad 4 and the plate 5, taking out the graphite plate 1 with the graphite paper 2 pasted, and trimming the corners around the graphite plate 1;

[0043] S9, putting the graphite plate 1 with the graphite paper 2 pasted into a high-temperature device (not shown) for hardening treatment, heating to 200-600℃ at a temperature rising speed of not more than 50℃ / h under vacuum or protective atmosphere, and keeping the temperature for not less than 3h, and then naturally cooling down, thereby obtaining 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 composed 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 on the upper surface of the graphite plate 1 is smooth without blistering and delamination, and the graphite paper 2 firmly bonded on the upper surface of the graphite plate 1 without blistering and delamination and with a smooth surface will be very suitable for chemical vapor deposition growth of large-scale bulk products 200, especially infrared optical materials.

[0045] In the method for preparing a chemical vapor deposition substrate according to the present disclosure, the chemical vapor deposition substrate 100 prepared through steps S1 to S9 is used for depositing the large-scale bulk product 200 by using the surface-smoothed graphite paper 2 firmly bonded on the upper surface of the graphite plate 1 without blistering and debonding, thus avoiding the pretreatment of directly using the graphite plate for depositing the large-size bulk product 200 in the background art, specifically, avoiding the formation of a coarse-grained layer at the bottom of the bulk product formed by chemical vapor deposition in the case of using a release agent in the background art, thereby improving the utilization rate of the bulk product, avoiding the risk of scratching the polished surface formed by directly polishing the graphite plate and the problem of cracking and damage of the bulk product caused by reusing, and thereby enabling the graphite plate 1 to be repeatedly and long-term used, thereby reducing the growth cost.

[0046] In the method for preparing a chemical vapor deposition substrate according to the present disclosure, the chemical vapor deposition substrate 100 prepared through steps S1 to S9 is used for depositing the large-scale bulk product 200 by using the surface-smoothed graphite paper 2 firmly bonded on the upper surface of the graphite plate 1 without blistering and debonding, thus facilitating the debonding between the bulk product 200 and the graphite plate 1 without damaging the bulk product 200 and the graphite plate 1, thereby improving the yield of the product bulk 200 and enabling it to be repeatedly and long-term used, thereby improving the production efficiency and reducing the cost, and being suitable for large-scale production.

[0047] In step S1, the graphite plate 1 is cleaned. Figure 1 In the example shown, a plurality of through holes 11 are arranged at equal intervals in the length direction L and the width direction W. In step S1, in an example, the hole diameter of the through holes 11 is in the range of 3-5 mm, and the pitch is in the range of 10-15 cm. In step S1, for example, the graphite plate 1 is a graphite plate of Japan Oriental Carbon brand IG-12.

[0048] In step S1, for example, cleaning can be performed by wiping with an organic solvent such as ethanol or acetone, and 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 an example, the thickness of the graphite paper 2 is in the range of 0.5-1.5 mm. For example, the graphite paper 2 is a graphite paper with a carbon content ≥99.5%, a sulfur content ≤200 PPM, a chlorine content ≤30 PPM, a density deviation ±0.5 g / cm 3Tensile strength ≥ 4.5 MPa, compression rate 35-45%, resilience ≥ 9%, thermal weight loss at 450℃ ≤ 5%, stress relaxation rate ≤ 10%. For example, graphite paper 2 is commercially available 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 filling the plurality of through holes 11 of the graphite plate 1 and being flat on the entire upper surface of the graphite plate 1 during the brushing of the adhesive 3. In step S3, for example, the adhesive 3 is SL8308 high-temperature-resistant glue of 1200℃ from Zhuzhou Shilin Polymer Co., Ltd. Of course, it is not limited thereto, as long as the adhesive 3 can be suitable for the glue 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 can apply a certain pressure to the pasted graphite paper 2, so that the graphite paper 2 can be better adhered to the upper surface of the graphite plate 1 during the normal temperature standing. In step S7, the soft pad 4 is a silica gel pad or a PVC rubber pad; the plate 5 is a light plastic material, specifically, it can be a PP plate or a PVC plate or an acrylic plate. In step S7, for example, the normal temperature standing is 15-20h.

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

[0055] In the hardening treatment of the high-temperature equipment in step S9, the vacuum or the protective atmosphere condition can avoid the oxidation of the graphite plate 1 and the graphite paper 2. The protective atmosphere is, for example, nitrogen. In the hardening treatment of the high-temperature equipment in step S9, the solvent in the adhesive 3 will be discharged along the corresponding through hole 11. In step S9, in an example, the heating rate is 20-30℃ / h, the temperature heated to is 400-500℃, and the holding time is 3-4h.

[0056] [Chemical vapor deposition method]

[0057] With reference to Figure 6 According to the chemical vapor deposition method of the present disclosure, the chemical vapor deposition substrate 100 prepared by the aforementioned method for preparing a chemical vapor deposition substrate is used to deposit and grow a bulk product 200 on the graphite paper 2 of the chemical vapor deposition substrate 100.

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

[0059] The features, effects, preparation and operation of the chemical vapor deposition substrate 100 employed by the chemical vapor deposition method according to the present disclosure can refer to the foregoing, which will not be repeated here.

[0060] [TEST]

[0061] Embodiment 1

[0062] The preparation method of the chemical vapor deposition substrate of embodiment 1 employs the following steps:

[0063] S1, provide a graphite plate 1, clean the surface of the graphite plate 1, clean with ethanol wiping, and then air dry, place the air-dried graphite plate 1 flat on the workbench, the graphite plate 1 is a graphite plate of Japan Toyo Carbon brand IG-12, 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 along the thickness direction T by processing, 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 3mm, the spacing between the plurality of through holes 11 is 10cm, the size of the length direction L of the graphite plate 1 is 2000mm, the size of the width direction W of the graphite plate 1 is 1000mm, and the size of the thickness direction T of the graphite plate 1 is 30mm;

[0064] S2, provide a graphite paper 2, cut 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 0.5mm, the graphite paper 2 is commercially available from Qingdao Juzhengyuan Graphite Technology Co., Ltd., and has a carbon content ≥99.5%, a sulfur content ≤200PPM, a chlorine content ≤30PPM, a density deviation ±0.5g / cm 3 , a tensile strength ≥4.5MPa, a compression rate of 35-45%, a resilience rate ≥9%, a thermal weight loss at 450℃ ≤55%, and a stress relaxation rate ≤510%;

[0065] S3, brush the adhesive 3 on the entire upper surface of the graphite plate 1 with a brush, the adhesive 3 is SL8308 high-temperature-resistant adhesive of 1200℃ from Zhuzhou Shilin Polymer Co., Ltd., and the adhesive 3 flows into and fills the plurality of through holes 11 of the graphite plate 1 during the brushing process, and the thickness of the adhesive 3 on the entire upper surface of the graphite plate 1 is 0.5mm;

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

[0067] S5, use a rubber squeegee to push the graphite paper 2 flat, and push out the excess adhesive 3 and gas from the through holes 11 of the graphite plate 1 and the four sides of the graphite plate 1;

[0068] S6, use a rubber squeegee to clean away the excess adhesive 3 pushed out from the through holes 11 of the graphite plate 1 and the four sides of the graphite plate 1;

[0069] S7, the soft pad 4 of the silica gel pad is used to cover and paste the graphite paper 2, and then the plate 5 of PP is used to cover the soft pad 4, and the temperature is kept at room temperature for 20 hours;

[0070] S8, after the temperature is kept, the soft pad 4 and the plate 5 are removed, the graphite plate 1 with the graphite paper 2 is taken out, and the art knife is used to trim the four corners of the graphite plate 1;

[0071] S9, the graphite plate 1 with the graphite paper 2 is put into the high-temperature equipment for hardening treatment, the high-temperature equipment is vacuumized to discharge oxygen, then the high-temperature equipment is filled with nitrogen for protection, the temperature is increased to 500 DEG C at a speed of 20 DEG C / h, the temperature is kept at the temperature for 4 hours, and then the temperature is naturally decreased, so that the chemical vapor deposition substrate 100 is obtained.

[0072] Example 2

[0073] The preparation method of the chemical vapor deposition substrate in Example 2 is different from that in Example 1 except the following points:

[0074] In step S1, the aperture of each through hole 11 is 5 mm, and the spacing between the plurality of 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 temperature is kept at room temperature for 15 hours;

[0078] In step S9, the temperature is increased to 400 DEG C at a speed of 25 DEG C / h, and the temperature is kept at the temperature for 3 hours.

[0079] Example 3

[0080] The preparation method of the chemical vapor deposition substrate in Example 3 is different from that in Example 1 except the following points:

[0081] In step S1, the aperture of each through hole 11 is 4 mm, and the spacing between the plurality of 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 temperature is kept at room temperature for 17 hours;

[0085] In step S9, the temperature is increased to 450 DEG C at a speed of 30 DEG C / h, and the temperature is kept at the temperature for 3.5 hours.

[0086] Example 4

[0087] Example 4 utilizes the chemical vapor deposition substrate 100 prepared in Example 1 to deposit zinc selenide on the graphite paper 2 of the chemical vapor deposition substrate 100 by a chemical vapor deposition method. The chemical vapor deposition process of zinc selenide utilizes the following process:

[0088] In the chemical vapor deposition furnace, the chemical vapor deposition substrate 100 prepared in Example 1 is loaded, a zinc ingot with purity of 99.999% is loaded into the crucible, the furnace is vacuumized, leak tested, and the pressure rise rate of the furnace body is required to be less than 8 Pa / h, after passing the test, the program temperature is started, the pressure in the furnace is controlled at 5 KPa, the temperature rising rate of the crucible is 0.3°C / min, and the temperature rising rate of the deposition chamber is 0.5°C / min, the crucible is heated to 650°C, and the deposition chamber is heated to 710°C, then the carrier gas argon is introduced into the crucible and the carrier gas argon and hydrogen selenide are introduced into the deposition chamber, the argon flow introduced into the crucible is 30 L / min, the evaporation rate of zinc vapor in the crucible is 5 L / min, the 5N hydrogen selenide flow introduced into the deposition chamber is 5.5 L / min, the argon flow mixed with the hydrogen selenide introduced into the deposition chamber is 55 L / min, the deposition rate is controlled at 80 μm / h, and the zinc selenide is deposited, after the deposition is completed, the same pressure as in the deposition process is maintained, the carrier gas and hydrogen selenide are stopped, the temperature in the deposition chamber is lowered to 600°C at a rate of 0.2°C / min, the temperature is kept constant at 600°C for 10 h, then the temperature is lowered to room temperature at a rate of 0.2°C / min, and the zinc selenide bulk product is obtained after the furnace is discharged.

[0089] Example 5

[0090] Example 5 utilizes the chemical vapor deposition substrate 100 prepared in Example 2 to deposit zinc sulfide on the graphite paper 2 of the chemical vapor deposition substrate 100 by a chemical vapor deposition method. The chemical vapor deposition process of zinc sulfide utilizes the following process:

[0091] In a chemical vapor deposition furnace, the chemical vapor deposition substrate 100 prepared in Example 2 was loaded, a zinc ingot with a purity of 99.999% was loaded into a crucible, the furnace was vacuumized, leak tested, and the pressure rise rate of the furnace body was required to be less than 8 Pa / h, after which the program temperature was started, the pressure in the furnace was controlled at 6 KPa, the temperature rising rate of the crucible was 0.5°C / min, and the temperature rising rate of the deposition chamber was 0.8°C / min, the crucible was heated to 630°C, and the deposition chamber was heated to 660°C, then the carrier gas argon was introduced into the crucible and the carrier gas argon and hydrogen sulfide were introduced into the deposition chamber, the argon flow rate introduced into the crucible was 50 L / min, the evaporation rate of zinc vapor was 6 L / min, the 4N hydrogen sulfide flow rate introduced into the deposition chamber was 5.2 L / min, the argon flow rate mixed with the hydrogen sulfide introduced into the deposition chamber was 90 L / min, the deposition rate was controlled at 60 μm / h, and the zinc sulfide was deposited, after the deposition was completed, the same pressure as in the deposition process was maintained, the introduction of the carrier gas argon and the hydrogen sulfide was stopped, the temperature of the deposition chamber was raised to 700°C at a temperature rising rate of 0.5°C / min, and the temperature was kept constant for 20 h, then the temperature was lowered to room temperature at a temperature lowering rate of 0.2°C / min, and the zinc sulfide bulk product was obtained after the furnace was discharged.

[0092] After the bulk products of Examples 4-5 were discharged from the furnace, a metal wire, iron wire, with a wire diameter less than the sum of the thickness of the graphite paper 2 and the thickness of the adhesive 3 was used to perform wire cutting along the graphite paper 2 aligned between the bulk product 200 and the graphite plate 1, so as to separate the bulk product 200 from the graphite plate 1, the separated graphite plate 1 was cleaned of the adhesive and reused, and the separated bulk product 200 was ground to remove the residual graphite paper after the wire cutting.

[0093] The surface of the graphite paper of the chemical vapor deposition substrate prepared in Examples 1-3 was smooth, and no blistering and peeling occurred. Figure 7 A photograph of the top view of the chemical vapor deposition substrate prepared in Example 1 taken from the side of the graphite paper 1 is given.

[0094] Figure 8 and Figure 9 Photographs of the bulk products prepared in Examples 4 and 5 taken from the side after the residual graphite paper was removed by grinding are given, respectively, wherein the bulk products were surface processed except for the bottom. From Figure 8 and Figure 9 It can be seen that the bottom of the bulk product has no coarse particle layer.

[0095] A plurality of exemplary embodiments are described using the above detailed description, but the present text is not intended to be limited to the explicitly disclosed combinations. Therefore, unless otherwise specified, various features disclosed herein can be combined together to form a plurality of additional combinations which are not shown for the sake of simplicity.

Claims

1. A method for preparing a chemical vapor deposition substrate, characterized in that, Including the following steps: S1, a graphite plate (1) is provided, the surface of the graphite plate (1) is cleaned, the graphite plate (1) is provided with a plurality of through holes (11) spaced apart in the length direction (L) and width direction (W) and extending along the thickness direction (T), the diameter of the plurality of through holes (11) is not greater than 10mm, the spacing between the plurality of through holes (11) is not greater than 20cm, the length direction (L) dimension of the graphite plate (1) is ≤2000mm, the width direction (W) dimension of the graphite plate (1) is ≤1000mm, and the thickness direction (T) dimension of the graphite plate (1) is 20-40mm; S2, providing graphite paper (2), the size of graphite paper (2) covers the upper surface of graphite plate (1), and the thickness of graphite paper (2) is 0.5-2.0mm; S3, apply adhesive (3) to the entire upper surface of the graphite plate (1). The adhesive (3) is a glue that can be used in chemical vapor deposition. The thickness of the adhesive (3) is 0.1-0.5 mm. S4, lay the graphite paper (2) flat on the graphite plate (1); S5, use a tool to flatten the graphite paper (2) and expel excess adhesive (3) and gas from the through holes (11) of the graphite plate (1) and around the graphite plate (1); S6, use a scraper to remove the excess adhesive (3) that has been discharged from the through hole (11) of the graphite plate (1) and around the graphite plate (1); S7, use a soft pad (4) to completely cover the pasted graphite paper (2), then cover the entire soft pad (4) with a board (5), and let it stand at room temperature for no less than 10 hours; S8. After the resting period, remove the pad (4) and the board (5), take out the graphite board (1) with the graphite paper (2) pasted on it, and trim the four corners along the graphite board (1). S9, the graphite plate (1) with graphite paper (2) attached is placed in a high-temperature equipment for hardening treatment. Under vacuum or protective atmosphere conditions, it is heated to 200-600°C at a heating rate of no more than 50°C / h and kept at this temperature for no less than 3 hours. After the heat preservation is completed, it is cooled naturally 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 diameter 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, cleaning is performed by wiping with organic solvents such as ethanol or acetone, followed by air drying.

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 ≥99.5%, a sulfur content ≤200PPM, a chlorine content ≤30PPM, and a density deviation of ±0.5g / cm³. 3 Tensile strength ≥ 4.5 MPa, compression ratio 35-45%, resilience ≥ 9%, thermal weight loss at 450°C ≤ 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 high-temperature adhesive resistant to 1200℃ from 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, an adhesive (3) is applied to the entire upper surface of the graphite plate (1) using a brush or roller. 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 board (5) is made of lightweight plastic material, which is PP board, PVC board or acrylic board.

7. The method for preparing a chemical vapor deposition substrate according to claim 1, characterized in that, In step S7, let it 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 temperature reached is 400-500°C, and the holding time is 3-4h.

9. A chemical vapor deposition method, characterized in that, The chemical vapor deposition method employs a chemical vapor deposition substrate (100) prepared by the chemical vapor deposition substrate preparation method according to any one of claims 1-8, and deposits and grows a bulk product (200) on 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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